PRIORITY CLAIM

This application is a continuation of U.S. Non-provisional application Ser. No. 15/059,995, filed Mar. 3, 2016, which claims priority under 35 U.S.C. § 119(e) to U.S. Provisional Application No. 62/128,195, filed Mar. 4, 2015, and U.S. Provisional Application No. 62/279,177, filed Jan. 15, 2016, each of which are expressly incorporated by reference herein.

BACKGROUND

The present disclosure relates to polymeric materials that can be formed to produce a container, and in particular, polymeric materials that insulate. More particularly, the present disclosure relates to polymer-based formulations that can produce an insulated non-aromatic polymeric material.

SUMMARY

According to the present disclosure, a polymeric material includes a polymeric resin and at least one cell-forming agent. In illustrative embodiments, a blend of polymeric resins and cell-forming agents is mixed and extruded or otherwise formed to produce an insulated cellular non-aromatic polymeric material. The insulated cellular non-aromatic polymeric material has a low density but is resistant to and/or can withstand impact forces. The low density, insulated cellular non-aromatic polymeric material can be used for improved containers.

In illustrative embodiments, an insulative cellular non-aromatic polymeric material comprises a cell-forming agent and at least one high-density polyethylene-based base resin. The cell-forming agent can include a chemical nucleating agent and a physical blowing agent. In an embodiment, a base resin can be HDPE, which can be virgin HDPE, regrind, or mixtures thereof.

In illustrative embodiments, the insulative cellular non-aromatic polymeric material has a density of less than about 0.9 grams per cubic centimeter. In illustrative embodiments, the insulative cellular non-aromatic polymeric material has a density in a range of about 0.1 grams per cubic centimeter to about 0.5 grams per cubic centimeter. In illustrative embodiments, the insulative cellular non-aromatic polymeric material has a density in a range of about 0.15 grams per cubic centimeter to about 0.4 grams per cubic centimeter. In illustrative embodiments, the insulative cellular non-aromatic polymeric material has a density of about 0.2 grams per cubic centimeter.

Additional features of the present disclosure will become apparent to those skilled in the art upon consideration of illustrative embodiments exemplifying the best mode of carrying out the disclosure as presently perceived.

BRIEF DESCRIPTION OF THE DRAWINGS

The detailed description particularly refers to the accompanying figures in which:

FIG. 1 is a perspective and diagrammatic view of the co-extrusion system used to prepare the insulative cellular non-aromatic polymeric material, showing that the co-extrusion system includes an outer-layer extruder configured to receive an outer-layer formulation and provide an outer-layer parison, an inner-layer extruder configured to receive an inner-layer formulation and provide an inner-layer parison, a core-layer extruder configured to receive a core-layer formulation and provide a core-layer parison, and a co-extrusion die coupled to each of the extruders to receive the associated parisons and configured to extrude the inner-layer, the core-layer, and the outer-layer parisons to establish a multi-layer tube;

FIG. 2 is a partial perspective view taken from below the co-extrusion die of the co-extrusion system of FIG. 1 showing that the co-extrusion die includes an annular aperture configured to extrude the multi-layer tube;

FIG. 3 is a view similar to FIG. 2 after co-extrusion of the insulative cellular non-aromatic polymeric material as a multi-layer tube has begun with portions of the multi-layer tube broken away to reveal that the inner layer is spaced apart from the outer layer and that the core layer is located therebetween;

FIG. 4 is a perspective view of an unassembled density determination apparatus showing the components (clockwise starting in the upper left) gem holder, platform, suspension bracket, and suspension spacer;

FIG. 5 is a perspective view of the multi-layer container formed from the insulative cellular non-aromatic polymeric material using a container-molding process;

FIG. 6 is a sectional view taken along line 6-6 of FIG. 5 showing that the multi-layer container includes a side wall including the inner layer, the outer layer spaced apart from the inner layer, and a compressed core layer located therebetween and showing that some of the expanded cells have collapsed along the inner and outer layers to cause the compressed core layer to have a relatively greater density than the core layer of the multi-form tube;

FIG. 7 is a perspective view of a multi-layer container made from insulative cellular non-aromatic material in accordance with the present disclosure with portions broken away to reveal that the multi-layer container includes an inner layer, a core layer, and an outer layer; and

FIG. 8 is a perspective view of another embodiment of a multi-layer container made insulative cellular non-aromatic material in accordance with the present disclosure with portions broken away to reveal that the multi-layer container includes an inner layer, a core layer, and an outer layer.

DETAILED DESCRIPTION

A polymeric material 10 according to the present disclosure can be used to form insulative multi-layer containers 14, 214, 314 as shown for example, in FIGS. 1, 5, 7, and 8. As described herein, a core polymeric material 10B, sometimes called an insulative cellular non-aromatic polymeric material, includes at least one cell-forming agent and a polymeric resin (i.e., a thermoplastic polyolefin). To form core polymeric material 10B, a blend of polymeric resins and cell-forming agents are combined via blending and extruded, as shown for example as extrusion process 100 in FIG. 1. Polymeric material 10 can be co-extruded, as shown in FIG. 1, to form a multi-layer tube 12, which can then be blow molded to form insulative multi-layer containers 14, 214, 314.

Co-extrusion process 100 can be used to form multi-layer tubes 12, sometimes called a parison, that include an inner layer 12A, a core layer 12B, and an outer layer 12C, each formed of a polymeric material 10A, 10B, 10C, as shown in FIG. 1. The molten formulations 42, 46, 50 for each of inner layer 12A, core layer 12B, and outer layer 12C pass through the extruders 20, 22, 36 to an annular extrusion die 38, as shown in FIGS. 1 and 3. The annular extrusion die 38 is configured to locate inner layer 12A around an interior space 23 and to locate core layer 12B between inner layer 12A and outer layer 12C through an annular aperture 39, as shown in FIG. 2. While three formulations are discussed herein, more or less formulations may be fed to associated extruders to produce a multiple layer tube having more or less layers. Reference is hereby made to U.S. patent application Ser. No. 14/475,411, filed Sep. 2, 2014 and titled MULTI-LAYER TUBE AND PROCESS OF MAKING THE SAME for disclosure relating to co-extrusion and multi-layer tube formation, which application is hereby incorporated in its entirety

Multi-layer tube 12 can be blow molded to form multi-layer containers 14, 214, 314 as shown in FIGS. 5-8. As an example, multi-layer tube 12 can be inserted into a mold and have air forced into interior space 23 to cause the multi-layer tube 12 to expand to fit an interior surface of the mold. Throughout this process, the relative locations of polymeric material 10A, 10B, 10C of multi-layer tube 12 are maintained and form the inner layer 14A, core layer 14B, and outer layer 14C of multi-layer container 14 once blow molded, as shown in FIG. 6. Reference is hereby made to U.S. patent application Ser. No. 14/475,266, filed Sep. 2, 2014 and titled CONTAINER AND PROCESS FOR MAKING THE SAME for disclosure relating to container forming processes, which application is hereby incorporated in its entirety.

In one exemplary embodiment, polymeric material 10 comprises a formulation that includes at least one polymeric resin. The polymeric material 10 may include one or more base resins. As an example, core polymeric material 10B comprises at least one polyethylene base resin and one or more cell-forming agents. As described herein, the core polymeric material 10B may be called an insulative cellular non-aromatic polymeric material. Reference is hereby made to U.S. patent application Ser. No. 14/331,066, filed Jul. 14, 2014 and titled POLYMERIC MATERIAL FOR CONTAINER for disclosure relating to possible formulation options, which application is hereby incorporated in its entirety.

Cell-forming agents provide a means for decreasing the density of the polymeric material while maintaining advantageous physical properties. Cell-forming agents can be chemical agents, physical agents, or combinations of both. Cell-forming agents can be physical blowing agents, chemical blowing agents, or combinations of both. Cell-forming agents can include nucleating agents.

Insulative cellular material can be co-extruded with additional layers that have advantageous properties. For example, inner layer polymeric material 10A and outer-layer polymeric material 10C can contain a reinforcing fiber, a hardener, a color, or a combination thereof.

In one example, the base resin is high-density polyethylene (HDPE). A HDPE base resin can be a HDPE homopolymer or a HDPE copolymer. In another example, the base resin is a unimodal HDPE. In yet another example, the base resin is unimodal, high-melt strength HDPE. In still yet another example, the base resin is unimodal, high-melt strength HDPE such as DOW® DOWLEX™ IP 41 HDPE (available from The Dow Chemical Company) that has been electron-beam modified to provide long-chain branching and a melt index of about 0.25 g/10 min. Another example of a unimodal, high-melt strength HDPE is EQUISTAR® ALATHON® H5520 HDPE copolymer (available from Lyondell Chemical Company) that has been electron-beam modified to have long-chain branching and a melt index of about 0.25 g/10 min. Another example of a suitable unimodal HDPE is FORMOLENE® HB5502F HDPE hexene copolymer (available from Formosa Plastics Corporation). In another suitable embodiment of a HDPE hexene copolymer, the HDPE is Marlex® HHM 5502BN HDPE hexene copolymer (Chevron Phillips Chemical Company, The Woodlands, Tex.). In some embodiments, the HDPE has a melt index from about 0.1 g/10 min to about 0.4 g/10 min. In an example the HDPE has a melt index between 0.7 g/10 min and 0.9 g/10 min. In another example, the HDPE resin is DOW DMDA 6400 NT7.

Long-chain branching refers to the presence of polymer side chains (branches) that have a length that is comparable or greater than a length of the backbone which is coupled to the polymer side chains. Long-chain branching creates viscoelastic chain entanglements (polymer entanglements) that hamper flow during extensional or oriented stretching and provide for a strain hardening phenomenon.

The strain hardening phenomenon may be observed through two analytical methods. The first analytical method used to observe the presence of strain hardening on an extensional rheometer. During extensional or oriented flow on an extensional rheometer, strain hardening will occur when polymer entanglements do not allow the polymer to flow under Linear Viscoelastic (LVE) conditions. As a result, these polymer entanglements hamper flow and create a deviation from the LVE conditions as observed as a hook formation. The strain hardening phenomenon becomes more severe as strain and strain rate increase due to faster and more severe polymer chain entanglement motion. Virgin polymers without long-chain branching will exhibit LVE flow characteristics. In comparison, long-chain branched polymers will exhibit strain hardening and which causes a deviation from the LVE flow characteristics of the virgin polymer providing the hook formation under the same test conditions.

The second analytical method used to observe the presence of long-chain branching is evaluating melt strength data as tested per ISO 16790 which is incorporated by reference herein in its entirety. An amount of melt strength is known to be directly related to the presence of long-chain branching when compared to similar virgin polymers lacking long-chain branching. By way of example, Borealis DAPLOY™ WB140HMS Polypropylene (PP) (available from Borealis AG) is compared to other polymers having similar molecular weight, polydispersity index, and other physical characteristics. The DAPLOY™ WB140HMS PP has a melt strength which exceeds about 36 cN while other similar PP resins lacking long-chain branching have a melt strength of less than about 10 cN.

Melt flow index (MFI) is an indirect measure of the viscosity of a polymer when molten. The index is defined as the mass of polymer melt that will flow through a capillary of a specific diameter and length by a pressure applied in 10 minutes, as described in ASTM D1238. For example, the Marlex® HHM 5502BN HDPE hexene copolymer (Chevron Phillips) has a melt flow index of 0.35 g/10 min per ASTM D1238. A larger melt index value indicates a lower viscosity. Higher molecular weight polymers will be more viscous and less will flow under the same conditions so the melt index will be a smaller number.

In certain exemplary embodiments, the formulation may include two base resins that are HDPE. In some embodiments the HDPE base resin may include multiple HDPE resins. One illustrative example of the formulation includes a first base resin of FORMOLENE® HB5502F HDPE hexene copolymer (available from Formosa Plastics Corporation) and a second base resin of EQUISTAR® ALATHON® H5520 HDPE copolymer (available from Lyondell Chemical Company). In embodiments with more than one HDPE copolymer, different HDPE copolymers can be used depending on the attributes desired in the formulation. For example, a formulation may include both electron-beam modified EQUISTAR® ALATHON® H5520 and FORMOLENE® HB5502F HDPE. In such an embodiment, the EQUISTAR® ALATHON® H5520 provides higher melt strength which increases foaming potential, and has less flexural modulus or brittleness. The FORMOLENE® HB5502F HDPE provides wide unimodal polydispersity index of the molecular weight distribution and maximizes economic advantage.

In another example, a formulation includes about 50% electron-beam modified EQUISTAR® ALATHON® H5520 and about 50% FORMOLENE® HB5502F HDPE. The combination provides a material having drop resistance capability associated with a non-modified HDPE resin and increased melt strength of an electron-beam modified long-chain branched HDPE. Depending on the desired characteristics, the percentage of the HDPE base resin between the two HDPE base resins may be varied, e.g., 25%/75%, 30%/70%, 35%/65%, 40%/60%, 45%/55%, 50%/50%, etc., by weight of the base resins. In an embodiment, a formulation includes three HDPE base resins. Again, depending on the desired characteristics, the percentage of three HDPE copolymers can be varied, 33%/33%/33%, 30%/30%/40%, 25%/25%/50%, etc., by weight of the base resins.

In certain exemplary embodiments, the formulation may include two base resins wherein the first base resin is an HDPE resin and the second base resin is a Low-Density Polyethylene (LDPE). In an example the LDPE resin has a melt index between 0.7 g/10 min and 0.9 g/10 min as measured by ASTM D1238. In another example, the LDPE resin is DOW™ LDPE 692 LDPE HEALTH+™ available from The Dow Chemical Company®.

In certain exemplary embodiments, the formulation may include two base resins wherein the first base resin is an HDPE resin and the second base resin is a Low-Density Polyethylene (LDPE) resin. Without being bound by theory, LDPE may be added to improve the compression resistance of the core layer during container-molding process 100. In an example the HDPE has a melt index between 0.7 g/10 min and 0.9 g/10 min. In another example, the HDPE resin is DOW DMDA 6400 NT7. In an example the LDPE resin has a melt index between 0.7 g/10 min and 0.9 g/10 min as measured by ASTM D1238. In another example, the LDPE resin is DOW™ LDPE 692 LDPE HEALTH+™ available from The Dow Chemical Company®.

In an illustrative example, the formulation comprises a blend of a certain percentage by weight of an HDPE resin and the remainder of the blend is an LDPE resin. In embodiments described herein, the percentage amount of HDPE in the blend may be 100%, 90%, 80%, 70%, 60%, 50%, 40%, 30%, 20%, 10% or 0 and the remainder of the blend is LDPE. It is within the present disclosure for the amount of HDPE in the blend to fall within one of many different ranges. In a set of ranges, the amount of HDPE in the blend can be about 0% to about 100%, about 20% to about 100%, about 40% to about 100%, about 60% to about 100%, about 70% to about 100%, about 80% to about 100%, about 80% to about 95%, and about 85% to about 95% of the blend. Polymeric material as disclosed herein includes at least one base resin. In illustrative embodiments, the at least one base resin can be HDPE. The amount of a base resin may be one of several different values or fall within one of several different ranges. It is within the scope of the present disclosure to select an amount of base resin to be one of the following values: about 20%, about 25%, about 30%, about 35%, about 40%, about 45%, about 50%, about 55%, about 60%, about 65%, about 70%, about 75%, about 80%, about 85%, about 86%, about 87%, about 88%, about 89%, about 90%, about 91%, about 92%, about 93%, about 94%, about 95%, about 96%, about 97%, about 98%, about 99%, about 99.5%, about 99.9%, and about 100% of the total formulation of the polymeric layer by weight percentage. It is within the present disclosure for the amount of base resin in the formulation to fall within one of many different ranges. In a first set of ranges, the range of base resin is one of the following ranges: about 20% to about 99.9%, about 25% to about 99.9%, about 50% to about 99.9%, about 85% to about 99.9%, about 90% to about 99.9%, about 95% to about 99.9%, about 98% to about 99.9%, and about 99% to about 99.9% of the total formulation of the polymeric layer by weight percentage. In a second set of ranges, the range of base resin is one of the following ranges: about 85% to about 99%, about 85% to about 98%, about 85% to about 95%, and about 85% to about 90% of the total formulation of the polymeric layer by weight percentage. In a third set of ranges, the range of base resin is one of the following ranges: about 90% to about 99%, and about 95% to about 98% of the total formulation by weight percentage. Each of these values and ranges is embodied in Examples 1 to 33.

In some embodiments, the core-layer formulation comprises an impact modifier to improve the performance of the container. In an embodiment the core-layer formulation comprises about 5% of an impact modifier. In some embodiments, the core-layer formulation comprises Vistamaxx™ available from the ExxonMobil™ Corporation.

In an embodiment, the base resin can be 100% virgin base resin. In an embodiment, the base resin can be a mixture of virgin base resin and regrind base resin. For example, the base resin can be about 100%, about 90%, about 80%, about 75%, about 70%, about 60%, about 50%, about 40%, about 30%, about 25%, about 20%, or about 10% virgin base resin with the remainder being a regrind. In an exemplary embodiment, the base resin is about 50% virgin HDPE and about 50% regrind.

In some embodiments, the HDPE base resin comprises up to about 90% regrind, up to about 80% regrind, up to about 60% regrind, up to about 40% regrind, up to about 20% regrind, about 20% to about 90% regrind, about 30% to about 90% regrind, about 40% to about 90% regrind, about 50% to about 90% regrind, about 20% to about 75% regrind, about 30% to about 75% regrind, about 40% to about 75% regrind, about 50% to about 75% regrind, about 20% to about 60% regrind, about 30% to about 60% regrind, about 40% to about 60% regrind, or about 50% to about 60% regrind. The regrind may be first pass regrind, second pass regrind, third pass regrind, and the like.

The term polymeric layer refers to a polymeric monolayer, a polymeric core layer in a multi-layer material, or a non-core polymeric layer in a multi-layer material.

The formulation used to produce the insulative cellular non-aromatic polymeric material may further include one or more cell-forming agents. Cell-forming agents include nucleating agents and blowing agents. A nucleating agent is used to provide and control nucleation sites within a molten formulation to promote formation of cells, bubbles, or voids in the molten formulation during extrusion. A blowing agent is used to grow cells in the molten material at nucleation sites. Blowing agents may be used alone in the formulation or with nucleating agents.

Nucleating agent means a chemical or physical agent that provides sites for cells to form in a molten material. Nucleating agents may include chemical nucleating agents and physical nucleating agents. The nucleating agent may be blended with the formulation that is introduced into the hopper of the extruder. Alternatively, the nucleating agent may be added to the molten resin mixture in the extruder.

Formulations used to produce insulative cellular non-aromatic polymeric materials may include one or more cell-forming agents. The amount of a nucleating agent may be one of several different values or fall within one of several different ranges. It is within the scope of the present disclosure to select an amount of a nucleating agent to be one of the following values: about 0%, about 0.05%, about 0.1%, about 0.2%, about 0.3%, about 0.5%, about 1%, about 1.5%, about 2%, about 3%, about 4%, about 5%, about 6%, about 7%, about 8%, about 9%, about 10%, about 11%, about 12%, about 13%, about 14%, and about 15%, of the total formulation of the polymeric layer by weight percentage. It is within the scope of the present disclosure for the amount of a nucleating agent in the formulation to fall within one of many different ranges. In a first set of ranges, the percentage (w/w) range of a nucleating agent is one of the following ranges: about 0% to about 15%, about 0.05% to about 15%, about 0.1% to about 15%, about 0.25% to about 15%, about 0.5% to about 15%, about 0.75% to about 15%, about 1% to about 15%, about 2% to about 15%, about 3% to about 15%, about 4% to about 15%, and about 5% to about 15% of the total formulation of the polymeric layer by weight percentage. In a second set of ranges, the percentage (w/w) range of a nucleating agent is one of the following ranges: about 0.05% to about 10%, about 0.1% to about 10%, about 0.25% to about 10%, about 0.5% to about 10%, about 0.75% to about 10%, about 1% to about 10%, about 2% to about 10%, about 3% to about 10%, about 4% to about 10%, and about 5% to about 10% of the total formulation of the polymeric layer by weight percentage. In a third set of ranges, the percentage (w/w) range of a nucleating agent is one of the following ranges: about 0.05% to about 5%, about 0.1% to about 5%, about 0.25% to about 5%, about 0.5% to about 5%, about 0.75% to about 5%, about 1% to about 5%, about 1.5% to about 5%, about 2% to about 5%, about 2.5% to about 5%, about 3% to about 5%, about 3.5% to about 5%, about 4% to about 5%, and about 4.5% to about 5% of the total formulation of the polymeric layer by weight percentage.

Suitable physical nucleating agents have desirable particle size, aspect ratio, and top-cut properties. Examples include, but are not limited to, talc, CaCO₃, mica, and mixtures of at least two of the foregoing. One representative example is Heritage Plastics HT6000 Linear Low Density Polyethylene (LLDPE) Based Talc Concentrate.

Formulations used to produce insulative cellular non-aromatic polymeric materials may include one or more cell-forming agents. The amount of a physical nucleating agent may be one of several different values or fall within one of several different ranges. It is within the scope of the present disclosure to select an amount of physical nucleating agent, such as talc, to be one of the following values: about 0%, about 0.05%, about 0.1%, about 0.3%, about 0.5%, about 1%, about 2%, about 3%, about 4%, about 5%, about 6%, and about 7% of the total formulation of the polymeric layer by weight percentage. It is within the scope of the present disclosure for the amount of a physical nucleating agent in the formulation to fall within one of many different ranges. In a first set of ranges, the range of a physical nucleating agent is one of the following ranges: about 0% to about 7% (w/w), about 0.1% to about 7%, about 0.25% to about 7%, about 0.5% to about 7%, about 0.75% to about 7%, about 1.0% to about 7%, about 1.25% to about 7%, about 1.5% to about 7%, about 1.75% to about 7%, about 2.0% to about 7%, about 2.25% to about 7%, about 2.5% to about 7%, about 3% to about 7%, about 4% to about 7%, about 5% to about 7%, and about 6% to about 7% of the total formulation of the polymeric layer. In a second set of ranges, the range of a physical nucleating agent is one of the following ranges: about 0% to about 6%, about 0% to about 5%, about 0% to about 4%, about 0% to about 3%, about 0% to about 2.5%, about 0% to about 2.25%, about 0% to about 2%, about 0% to about 1.75%, about 0% to about 1.5%, about 0% to about 1.25%, about 0% to about 1%, about 0% to about 0.75%, and about 0% to about 0.5% of the total formulation of the polymeric layer. In a third set of ranges, the range of a physical nucleating agent is one of the following ranges: about 0.1% to about 6%, about 0.5% to about 5%, about 1% to about 4%, and about 2% to about 3% of the total formulation of the polymeric layer. In an embodiment, the formulation lacks talc.

Suitable chemical nucleating agents decompose to create cells in the molten formulation when a chemical reaction temperature is reached. These small cells act as nucleation sites for larger cell growth from a physical or other type of blowing agent. In one example, the chemical nucleating agent is citric acid or a citric acid-based material. One representative example is HYDROCEROL™ CF-40E (available from Clariant Corporation), which contains citric acid and a crystal nucleating agent.

Formulations used to produce insulative cellular non-aromatic polymeric materials can include a chemical nucleating agent. The amount of a chemical nucleating agent may be one of several different values or fall within one of several different ranges. It is within the scope of the present disclosure to select an amount of a chemical nucleating agent and be one of the following values: about 0.1%, about 0.25%, about 0.5%, about 0.75%, about 1%, about 1.5%, about 2%, about 2.5%, about 3%, about 3.5%, about 4%, about 5%, 1 about 0%, and about 15% of the total formulation by weight percentage. It is within the scope of the present disclosure for the amount of a chemical nucleating agent in the formulation to fall within one of many different ranges. In a first set of ranges, the range of a chemical nucleating agent is one of the following ranges: about 0.1% to about 15%, about 0.25% to about 15%, about 0.5% to about 15%, about 1% to about 15%, about 1.5% to about 15%, about 2% to 1 about 5%, about 2.5% to about 15%, about 3% to about 15%, about 3.5% to about 15%, about 4% to about 15%, about 4.5% to about 15%, and about 5% to about 15% of the total formulation by weight percentage. In a second set of ranges, the range of a chemical nucleating agent is one of the following ranges: about 0.1% to about 10%, about 0.25% to about 10%, about 0.5% to about 10%, about 0.75% to about 10%, about 1% to about 10%, about 1.5% to about 10%, about 2% to about 10%, about 2.5% to about 10%, about 3% to about 10%, about 3.5% to about 10%, about 4% to about 10%, about 4.5% to about 10%, and about 5% to about 10% of the total formulation by weight percentage. In a third set of ranges, the range of a chemical nucleating agent is one of the following ranges: about 0.1% to about 5%, about 0.25% to about 5%, about 0.5% to about 5%, about 0.75% to about 5%, about 1% to about 5%, about 1.5% to about 5%, about 2% to about 5%, about 2.5% to about 5%, about 3% to about 5%, about 3.5% to about 5%, about 4% to about 5%, and about 4.5% to about 5% of the total formulation by weight percentage. Each of these values and ranges is embodied in the Examples.

A blowing agent refers to a physical or a chemical material (or combination of materials) that acts to expand nucleation sites. Blowing agents may include only chemical blowing agents, only physical blowing agents, combinations thereof, or several types of chemical and physical blowing agents. The blowing agent acts to reduce density by forming cells in the molten formulation at the nucleation sites. The blowing agent may be added to the molten resin mixture in the extruder.

Chemical blowing agents are materials that degrade or react to produce a gas. Chemical blowing agents may be endothermic or exothermic. Chemical blowing agents typically degrade at a certain temperature to decompose and release gas. One example of a chemical blowing agent is citric acid or citric-based material. One representative example is HYDROCEROL™ CF-40E (available from Clariant Corporation), which contains citric acid and a crystal nucleating agent. Here, the citric acid decomposes at the appropriate temperature in the molten formulation and forms a gas which migrates toward the nucleation sites and grows cells in the molten formulation. If sufficient chemical blowing agent is present, the chemical blowing agent may act as both the nucleating agent and the blowing agent. However, a chemical blowing agent does not always act as a nucleating agent.

In another example, chemical blowing agents may be selected from the group consisting of azodicarbonamide; azodiisobutyro-nitrile; benzenesulfonhydrazide; 4,4-oxybenzene sulfonylsemicarbazide; citric acid; citric-based material; p-toluene sulfonyl semi-carbazide; barium azodicarboxylate; N,N′-dimethyl-N,N′-dinitrosoterephthalamide; trihydrazino triazine; methane; ethane; propane; n-butane; isobutane; n-pentane; isopentane; neopentane; methyl fluoride; perfluoromethane; ethyl fluoride; 1,1-difluoroethane; 1,1,1-trifluoroethane; 1,1,1,2-tetrafluoro-ethane; pentafluoroethane; perfluoroethane; 2,2-difluoropropane; 1,1,1-trifluoropropane; perfluoropropane; perfluorobutane; perfluorocyclobutane; methyl chloride; methylene chloride; ethyl chloride; 1,1,1-trichloroethane; 1,1-dichloro-1-fluoroethane; 1-chloro-1,1-difluoroethane; 1,1-dichloro-2,2,2-trifluoroethane; 1-chloro-1,2,2,2-tetrafluoroethane; trichloromonofluoromethane; dichlorodifluoromethane; trichlorotrifluoroethane; dichlorotetrafluoroethane; chloroheptafluoropropane; dichlorohexafluoropropane; methanol; ethanol; n-propanol; isopropanol; sodium bicarbonate; sodium carbonate; ammonium bicarbonate; ammonium carbonate; ammonium nitrite; N,N′-dimethyl-N,N′-dinitrosoterephthalamide; N,N′-dinitrosopentamethylene tetramine; azodicarbonamide; azobisisobutylonitrile; azocyclohexylnitrile; azodiaminobenzene; bariumazodicarboxylate; benzene sulfonyl hydrazide; toluene sulfonyl hydrazide; p,p′-oxybis(benzene sulfonyl hydrazide); diphenyl sulfone-3,3′-disulfonyl hydrazide; calcium azide; 4,4′-diphenyl disulfonyl azide; p-toluene sulfonyl azide, and combinations thereof.

In one aspect of the present disclosure, where a chemical blowing agent is used, the chemical blowing agent may be introduced into the material formulation that is added to the hopper.

Formulations used to produce insulative cellular non-aromatic polymeric materials may include one or more chemical blowing agents. The amount of a chemical blowing agent may be one of several different values or fall within one of several different ranges. It is within the scope of the present disclosure to select an amount of a chemical blowing agent to be one of the following values: about 0%, about 0.05%, about 0.1%, about 0.5%, about 0.75%, about 1%, about 1.5%, about 2%, about 3%, about 4%, and about 5%, of the total formulation of the polymeric layer by weight percentage. It is within the scope of the present disclosure for the amount of a chemical blowing agent in the formulation to fall within one of many different ranges. In a first set of ranges, the range of a chemical blowing agent is one of the following ranges: about 0.1% to about 5% (w/w), about 0.25% to about 5%, about 0.5% to about 5%, about 0.75% to about 5%, about 1% to about 5%, about 1.5% to about 5%, and about 2% to 5 about % of the total formulation of the polymeric layer by weight percentage. In a second set of ranges, the range of a chemical blowing agent is one of the following ranges: about 0.1% to about 2%, about 0.1% to about 3%, about 0.25% to about 2%, about 0.5% to about 2%, about 0.75% to about 2%, about 1% to about 2%, and about 1.5% to about 2% of the total formulation by weight percentage. In a third set of ranges, the range of a chemical blowing agent is one of the following ranges: about 0.1% to about 1%, about 0.25% to about 1%, about 0.5% to about 1%, and about 0.75% to about 1%, of the total formulation of the polymeric layer by weight percentage.

One example of a physical blowing agent is nitrogen (N₂). The N₂is pumped into the molten formulation via a port in the extruder as a supercritical fluid. The molten material with the N₂in suspension then exits the extruder via a die where a pressure drop occurs. As the pressure drop happens, N₂moves out of suspension toward the nucleation sites where cells grow. Excess gas blows off after extrusion with the remaining gas trapped in the cells formed in the extrudate. Other suitable examples of physical blowing agents include, but are not limited to, carbon dioxide (CO₂), helium, argon, air, pentane, butane, or other alkane mixtures of the foregoing and the like.

In an illustrative example, a physical blowing agent may be introduced at a rate of about 0.02 pounds per hour (lbs/h) to about 1.3 (lbs/h). In another illustrative example, the physical blowing agent may be introduced at a rate of about 0.03 (lbs/h) to about 1.25 (lbs/h). In another illustrative example, the physical blowing agent may be introduced at a rate of about 0.02 (lbs/h) to about 0.15 (lbs/h). In another illustrative example, the physical blowing agent may be introduced at a rate of about 0 (lbs/h) to about 0.15 (lbs/h). In another illustrative example, the physical blowing agent may be introduced at a rate of about 0.02 (lbs/h) to about 0.22 (lbs/h). In another illustrative example, the physical blowing agent may be introduced at a rate of about 0.02 (lbs/h) to about 0.25 (lbs/h). In still yet another illustrative example the physical blowing agent may be introduced at a rate of about 0.07 (lbs/h) to about 0.27 (lbs/h). In some embodiments, the physical blowing agent is used between about 0.01 lbs/h to about 0.2 lbs/h, about 0.01 lbs/h to about 0.17 lbs/h, about 0.01 lbs/h to about 0.15 lbs/h, about 0.01 lbs/h to about 0.1 lbs/h, about 0.05 lbs/h to about 0.2 lbs/h, about 0.05 lbs/h to about 0.17 lbs/h, about 0.05 lbs/h to about 0.15 lbs/h, about 0.05 lbs/h to about 0.1 lbs/h, about 0.1 lbs/h to about 0.2 lbs/h, about 0.1 lbs/h to about 0.17 lbs/h, or about 0.1 lbs/h to about 0.15 lbs/h.

In further embodiments, the physical blowing agent is measured in saturation percentage (%). In exemplary embodiments, physical blowing agent saturation can have a range that is about 0.1% to about 0.4%, about 0.1% to about 0.35%, about 0.1% to about 0.3%, about 0.1% to about 0.25%, 0.15% to about 0.4%, about 0.15% to about 0.35%, about 0.15% to about 0.3%, about 0.15% to about 0.25%, 0.2% to about 0.4%, about 0.2% to about 0.35%, about 0.2% to about 0.3%, or about 0.2% to about 0.25%.

In one aspect of the present disclosure, at least one slip agent may be incorporated into the formulation to aid in increasing production rates. Slip agent (also known as a process aid) is a term used to describe a general class of materials that is added to a formulation to provide surface lubrication to the polymer during and after conversion. Slip agents may also reduce or eliminate die drool. Representative examples of slip agents include amides of fats or fatty acids, such as, but not limited to, erucamide and oleamide. In one exemplary aspect, amides from oleyl (single unsaturated C-18) through erucyl (C-22 single unsaturated) may be used. Other representative examples of a slip agent include low molecular weight amides and fluoroelastomers. Combinations of two or more slip agents can be used. Slip agents may be provided in a master batch pellet form and blended with the resin formulation. One example of a suitable slip agent is Ampacet 102823 Process Aid PE MB LLDPE.

Formulations used to produce insulative cellular non-aromatic polymeric materials may include one or more slip agents. The amount of a slip agent may be one of several different values or fall within one of several different ranges. It is within the scope of the present disclosure to select an amount of a slip agent to be one of the following values: about 0%, about 0.1%, about 0.25%, about 0.5%, about 0.75%, about 1%, about 1.25%, about 1.5%, about 1.75%, about 2%, about 2.25%, about 2.5%, about 2.75%, about 3%, and about 4% of the total formulation of the polymeric layer by weight percentage. It is within the scope of the present disclosure for the amount of a slip agent in the formulation to fall within one of many different ranges. In a first set of ranges, the range of a slip agent is one of the following ranges: about 0% to about 4% (w/w), about 0.1% to about 4%, about 0.25% to about 4%, about 0.5% to about 4%, about 0.75% to about 4%, about 1% to about 4%, about 1.25% to about 4%, about 1.5% to about 4%, about 1.75% to about 4%, about 2% to about 4%, about 2.25% to about 4%, and about 2.5% to about 4% of the total formulation of the polymeric layer by weight percentage. In a second set of ranges, the range of a slip agent is one of the following ranges: about 0% to about 3%, about 0% to about 2.5%, about 0% to about 2.25%, about 0% to about 2%, about 0% to about 1.75%, about 0% to about 1.5%, about 0% to about 1.25%, about 0% to about 1%, about 0% to about 0.75%, and about 0% to about 0.5% of the total formulation of the polymeric layer by weight percentage. In a third set of ranges, the range of a slip agent is one of the following ranges: about 0.1% to about 2.5%, about 0.25% to about 2.25%, about 0.5% to about 2%, about 0.75%, to about 1.75%, and 1 about % to about 1.5% of the total formulation by weight percentage. In an embodiment, the formulation lacks a slip agent.

In another aspect of the present disclosure, an impact modifier may be incorporated into a formulation to minimize fracturing of the insulative cellular non-aromatic polymeric material when subjected to an impact such as a drop test. One representative example of a suitable impact modifier is DOW® AFFINITY™ PL 1880G polyolefin plastomer.

Formulations used to produce insulative cellular non-aromatic polymeric materials may include one or more colorants. The colorants can be supplied in a masterbatch mixture and combined via blending with the formulation. In an example, Ampacet 112761 White Polyethylene Masterbatch is used as a colorant. The amount of a colorant may be one of several different values or fall within one of several different ranges. It is within the scope of the present disclosure to select an amount of a colorant to be one of the following values: about 0%, about 0.1%, about 0.25%, about 0.5%, about 0.75%, about 1%, about 2%, about 3%, about 4% about 5%, about 6%, and about 7% of the total formulation of the polymeric layer by weight percentage. It is within the scope of the present disclosure for the amount of a colorant in the formulation to fall within one of many different ranges. In a first set of ranges, the range of a colorant is one of the following ranges: about 0% to about 5% (w/w), about 0.1% to about 5%, about 0.25% to about 5%, about 0.5% to about 5%, about 0.75% to about 5%, about 1% to about 5%, about 1.25% to about 5%, about 1.5% to about 5%, about 1.75% to about 5%, about 2% to about 5%, about 2.25% to about 5%, about 2.5% to about 5%, about 3% to about 5%, and about 4% to about 5% of the total formulation of the polymeric layer by weight percentage. In a second set of ranges, the range of a colorant is one of the following ranges: about 0% to about 3%, about 0% to about 2.5%, about 0% to about 2.25%, about 0% to about 2%, about 0% to about 1.75%, about 0% to about 1.5%, about 0% to about 1.25%, about 0% to about 1%, about 0% to about 0.75%, and about 0% to about 0.5% of the total formulation of the polymeric layer by weight percentage. In a third set of ranges, the range of a colorant is one of the following ranges: about 0.1% to about 3.5%, about 0.5% to about 3%, about 0.75% to about 2.5%, and about 1% to about 2% of the total formulation by weight percentage. In an embodiment, the formulation lacks a colorant.

A material-formulation process in accordance with the present disclosure uses a polyethylene-based formulation to produce a strip of insulative cellular non-aromatic polymeric material. Raw material according to the polyethylene-based material is gravity fed into the barrel of an extruder where it is heated to produce a molten material. A cell-forming agent is then introduced into the molten material prior to extrusion. As the molten materials exit the extruder, cells nucleate in the molten material, and the molten material expands and cools to form a sheet of insulative cellular non-aromatic polymeric material.

An insulative cellular non-aromatic polymeric material produced in accordance with the present disclosure can be formed to produce an insulative cup or an insulative container. In another illustrative example, the insulative cellular non-aromatic polymeric material produces a monolayer tube or monolayer parison that is blow molded to form an insulative container (e.g., bottle). In an embodiment, a monolayer foamed bottle further includes an extruded second layer (i.e., skin layer). In illustrative embodiments, a second layer can be linear low density polyethylene (LLDPE), low density polyethylene (LDPE), medium density polyethylene (MDPE), high density polyethylene (HDPE), polypropylene homopolymer, polypropylene impact copolymer, polypropylene random polymer, polystyrene, polyethylene terephthalate (PET), or polyvinyl chloride (PVC).

In an example, multi-layer container 14, 214, 314 includes a core layer 14B and at least one non-core layer. In an illustrative example, a core layer 14B is sandwiched between an inner polymeric layer 14A and an outer polymeric layer 14C. In an example, each layer (core and non-core layers) of multi-layer container 14, 214, 314 includes at least one HDPE base resin. In an embodiment, a non-core layer can include fiber. A suitable fiber can be a synthetic fiber that reinforces polyolefin formulations to provide, e.g., higher stiffness to the material and better feeding and handling during extrusion or blow molding process. A suitable fiber for a polymeric layer includes a synthetic, mineral based fiber, such as Hyperform® HPR-803i (Milliken & Co., Spartanburg, S.C.). Another suitable fiber blend contains about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem). In an embodiment, one or more non-core polymeric layers includes fiber. In an illustrative embodiment, a multi-layer container has fiber in an outer polymeric layer but an inner polymeric layer does not include fiber.

The amount of fiber may be one of several different values or fall within one of several different ranges. It is within the scope of the present disclosure to select an amount of fiber to be one of the following values: about 5%, about 10%, about 15%, about 20%, and about 25% of the layer by weight percentage. It is within the scope of the present disclosure for the amount of fiber in the layer to fall within one of many different ranges. In a first set of ranges, the range of fiber is one of the following ranges: about 0% to about 25% (w/w), about 5% to about 25%, about 10% to about 25%, about 15% to about 25%, and about 20% to about 25 of the total layer by weight percentage. In a second set of ranges, the range of fiber is one of the following ranges: about 0% to about 25%, about 0% to about 20%, about 0% to about 15%, about 0% to about 10%, and about 0% to about 5% of the total layer by weight percentage. In a third set of ranges, the range of a colorant is one of the following ranges: about 5% to about 20%, about 5% to about 15%, and about 5% to about 10%. In a fourth set of ranges, the range of fiber is one of the following ranges: about 10% to about 20%, and about 10% to about 15% of the total layer by weight percentage. In an embodiment, non-core layers lack fiber.

In an embodiment, one of the non-core layers can include a colorant. The colorants can be supplied in a masterbatch mixture and combined via blending with the formulation. In an example, Ampacet 112761 White Polyethylene Masterbatch is used as a colorant. The amount of a colorant may be one of several different values or fall within one of several different ranges. It is within the scope of the present disclosure to select an amount of a colorant to be one of the following values: about 0%, about 0.1%, about 0.25%, about 0.5%, about 0.75%, about 1%, about 2%, about 3%, about 4% about 5%, about 6%, and about 7% of the total formulation of the polymeric layer by weight percentage.

It is within the scope of the present disclosure for the amount of a colorant in the formulation to fall within one of many different ranges. In a first set of ranges, the range of a colorant is one of the following ranges: about 0% to about 7% (w/w), about 0.1% to about 7%, about 0.25% to about 7%, about 0.5% to about 7%, about 0.75% to about 7%, about 1% to about 7%, about 1.25% to about 7%, about 1.5% to about 7%, about 1.5% to about 6%, about 1.5% to about 5%, about 1.75% to about 5%, about 2% to about 5%, about 2.25% to about 5%, about 2.5% to about 5%, about 3% to about 5%, and about 4% to about 5% of the total formulation of the polymeric layer by weight percentage. In a second set of ranges, the range of a colorant is one of the following ranges: about 0% to about 3%, about 0% to about 2.5%, about 0% to about 2.25%, about 0% to about 2%, about 0% to about 1.75%, about 0% to about 1.5%, about 0% to about 1.25%, about 0% to about 1%, about 0% to about 0.75%, and about 0% to about 0.5% of the total formulation of the polymeric layer by weight percentage. In a third set of ranges, the range of a colorant is one of the following ranges: about 0.1% to about 3.5%, about 0.5% to about 3%, about 0.75% to about 2.5%, and about 1% to about 2% of the total formulation by weight percentage. In an embodiment, the formulation lacks a colorant.

In an illustrative example, multi-layer container 14, 214, 314 is a bottle having a) a core layer comprising HDPE, a chemical blowing agent, and talc; b) an outer polymeric layer comprising HDPE, a colorant, and fiber; and c) an inner polymeric layer comprising HDPE and fiber. In one example, the density of multi-layer container 14 is less than about 0.75 g/cm³. In one example, the density of multi-layer container 14 is less than about 0.7 g/cm³. In one example, the density of multi-layer container 14 is less than about 0.75 g/cm³. In one example, the density of multi-layer container 14 is less than about 0.7 g/cm³. In one example, the density of multi-layer container 14 is less than about 0.65 g/cm³. In one example, the density of multi-layer container 14 is less than about 0.6 g/cm³. In another example, the density of multi-layer container 14 is less than about 0.55 g/cm³. In another example, the density of multi-layer container 14 is less than about 0.5 g/cm³. In another example, the density of multi-layer container 14 is less than about 0.45 g/cm³. In another example, the density of multi-layer container 14 is less than about 0.4 g/cm³. In one example, the density of multi-layer container 14 is one of the following ranges: about 0.4 g/cm³to about 0.8 g/cm³, about 0.4 g/cm³to about 0.7 g/cm³, about 0.4 g/cm³to about 0.55 g/cm³, about 0.4 g/cm³to about 0.5 g/cm³, or about 0.4 g/cm³to about 0.45 g/cm³.

In an embodiment, the insulative cellular non-aromatic polymeric material is located between and coupled to an inner polymeric layer and an outer polymeric layer to produce a multi-layer tube 12. The density of the multi-layer tube 12 may be one of several different values or fall within one several different ranges. It is within the scope of the present disclosure for the density of the multi-layer tube 12 to fall within one of many different ranges. In a first set of ranges, the density is one of the following ranges: about 0.5 g/cm³to about 0.92 g/cm³, about 0.6 g/cm³to about 0.92 g/cm³, about 0.65 g/cm³to about 0.92 g/cm³, about 0.7 g/cm³to about 0.92 g/cm³, about 0.75 g/cm³to about 0.92 g/cm³, about 0.8 g/cm³to about 0.92 g/cm³, about 0.85 g/cm³to about 0.92 g/cm³, and about 0.9 g/cm³to about 0.92 g/cm³. In a second set of ranges, the density is one of the following ranges: about 0.5 g/cm³to about 0.9 g/cm³, about 0.6 g/cm³to about 0.9 g/cm³, about 0.65 g/cm³to about 0.9 g/cm³, about 0.7 g/cm³to about 0.9 g/cm³, about 0.75 g/cm³to about 0.9 g/cm³, about 0.8 g/cm³to about 0.9 g/cm³, and about 0.85 g/cm³to about 0.9 g/cm³. In a third set of ranges, the density is one of the following ranges: about 0.6 g/cm³to about 0.85 g/cm³, about 0.65 g/cm³to about 0.8 g/cm³, and about 0.7 g/cm³to about 0.75 g/cm³.

In an embodiment, the insulative cellular non-aromatic polymeric material is located between and coupled to an inner polymeric layer 12A and an outer polymeric 12C layer to produce a multi-layer parison. The density of the multi-layer parison 12 may be one of several different values or fall within one several different ranges. It is within the scope of the present disclosure for the density of the multi-layer parison 10 to fall within one of many different ranges. In a first set of ranges, the density is one of the following ranges: about 0.4 g/cm³to about 0.8 g/cm³, about 0.45 g/cm³to about 0.8 g/cm³, about 0.5 g/cm³to about 0.8 g/cm³, about 0.55 g/cm³to about 0.8 g/cm³, about 0.6 g/cm³to about 0.8 g/cm³, about 0.65 g/cm³to about 0.8 g/cm³, about 0.7 g/cm³to about 0.8 g/cm³, and about 0.75 g/cm³to about 0.8 g/cm³. In a second set of ranges, the density of a multi-layer parison is one of the following ranges: about 0.4 g/cm³to about 0.75 g/cm³, about 0.4 g/cm³to about 0.7 g/cm³, about 0.4 g/cm³to about 0.65 g/cm³, about 0.4 g/cm³to about 0.6 g/cm³, about 0.4 g/cm³to about 0.55 g/cm³, about 0.4 g/cm³to about 0.5 g/cm³, and about 0.4 g/cm³to about 0.45 g/cm³. In a third set of ranges, the density of a multi-layer parison is one of the following ranges: about 0.45 g/cm³to about 0.7 g/cm³, about 0.5 g/cm³to about 0.65 g/cm³, and about 0.55 g/cm³to about 0.6 g/cm³. Density was determined according to the density test procedure outlined in Example 14 using the apparatus in FIG. 4.

In an embodiment, the density of multi-layer tube 12 may be one of several different values or fall within one of several different ranges. It is within the scope of the present disclosure to select a density and be one of the following values: about 0.1 g/cm³, about 0.15 g/cm³, about 0.2 g/cm³, about 0.25 g/cm³, about 0.3 g/cm³, about 0.35 g/cm³, about 0.4 g/cm³about 0.45 g/cm³, about 0.5 g/cm³, about 0.55 g/cm³, about 0.6 g/cm³, about 0.65 g/cm³, about 0.7 g/cm³, about 0.75 g/cm³, about 0.785 g/cm³, and about 0.8 g/cm³. It is within the scope of the present disclosure for the density of the formulation to fall within one of many different ranges. In a first set of ranges, the range of density is one of the following ranges: about 0.1 g/cm³to about 0.8 g/cm³, about 0.15 g/cm³to about 0.8 g/cm³, about 0.2 g/cm³to about 0.8 g/cm³, about 0.25 g/cm³to about 0.8 g/cm³, about 0.3 g/cm³to about 0.8 g/cm³, about 0.35 g/cm³to about 0.8 g/cm³, about 0.4 g/cm³to about 0.8 g/cm³, about 0.45 g/cm³to about 0.8 g/cm³, about 0.5 g/cm³to about 0.8 g/cm³, about 0.55 g/cm³to about 0.8 g/cm³, about 0.6 g/cm³to about 0.8 g/cm³, about 0.65 g/cm³to about 0.8 g/cm³, about 0.7 g/cm³to about 0.8 g/cm³, and about 0.75 g/cm³to about 0.8 g/cm³. In a second set of ranges, the range of density is one of the following ranges: about 0.1 g/cm³to about 0.75 g/cm³, about 0.1 g/cm³to about 0.7 g/cm³, about 0.1 g/cm³to about 0.65 g/cm³, about 0.1 g/cm³to about 0.6 g/cm³, about 0.1 g/cm³to about 0.55 g/cm³, about 0.1 g/cm³to about 0.5 g/cm³, about 0.1 g/cm³to about 0.45 g/cm³, about 0.1 g/cm³to about 0.4 g/cm³, about 0.1 g/cm³to about 0.35 g/cm³, about 0.1 g/cm³to about 0.3 g/cm³, about 0.1 g/cm³to about 0.25 g/cm³, about 0.1 g/cm³to about 0.2 g/cm³, and about 0.1 g/cm³to about 0.15 g/cm³. In a third set of ranges, the range of density is one of the following ranges: about 0.3 g/cm³to about 0.8 g/cm³, about 0.35 g/cm³to about 0.8 g/cm³, about 0.35 g/cm³to about 0.75 g/cm³, about 0.4 g/cm³to about 0.75 g/cm³, about 0.4 g/cm³to about 0.7 g/cm³, about 0.4 g/cm³to about 0.65 g/cm³, and about 0.4 g/cm³to about 0.6 g/cm³. Each of these values and ranges is embodied in the Examples. Density was determined according to the density test procedure outlined in Example 14 using the apparatus in FIG. 4.

In an embodiment, the density of the insulative cellular non-aromatic polymeric material may be one of several different values or fall within one of several different ranges. It is within the scope of the present disclosure to select a density and be one of the following values: about 0.1 g/cm³, about 0.15 g/cm³, about 0.2 g/cm³, about 0.25 g/cm³, about 0.3 g/cm³, about 0.35 g/cm³, about 0.4 g/cm³about 0.45 g/cm³, about 0.5 g/cm³, about 0.55 g/cm³, about 0.6 g/cm³, about 0.65 g/cm³, about 0.7 g/cm³, about 0.75 g/cm³, about 0.785 g/cm³, and about 0.8 g/cm³. It is within the scope of the present disclosure for the density of the insulative cellular non-aromatic polymeric material to fall within one of many different ranges. In a first set of ranges, the range of density is one of the following ranges: about 0.1 g/cm³to about 0.8 g/cm³, about 0.15 g/cm³to about 0.8 g/cm³, about 0.2 g/cm³to about 0.8 g/cm³, about 0.25 g/cm³to about 0.8 g/cm³, about 0.3 g/cm³to about 0.8 g/cm³, about 0.35 g/cm³to about 0.8 g/cm³, about 0.4 g/cm³to about 0.8 g/cm³, about 0.45 g/cm³to about 0.8 g/cm³, about 0.5 g/cm³to about 0.8 g/cm³, about 0.55 g/cm³to about 0.8 g/cm³, about 0.6 g/cm³to about 0.8 g/cm³, about 0.65 g/cm³to about 0.8 g/cm³, about 0.7 g/cm³to about 0.8 g/cm³, and about 0.75 g/cm³to about 0.8 g/cm³. In a second set of ranges, the range of density is one of the following ranges: about 0.1 g/cm³to about 0.75 g/cm³, about 0.1 g/cm³to about 0.7 g/cm³, about 0.1 g/cm³to about 0.65 g/cm³, about 0.1 g/cm³to about 0.6 g/cm³, about 0.1 g/cm³to about 0.55 g/cm³, about 0.1 g/cm³to about 0.5 g/cm³, about 0.1 g/cm³to about 0.45 g/cm³, about 0.1 g/cm³to about 0.4 g/cm³, about 0.1 g/cm³to about 0.35 g/cm³, about 0.1 g/cm³to about 0.3 g/cm³, about 0.1 g/cm³to about 0.25 g/cm³, about 0.1 g/cm³to about 0.2 g/cm³, and about 0.1 g/cm³to about 0.15 g/cm³. In a third set of ranges, the range of density is one of the following ranges: about 0.1 g/cm³to about 0.8 g/cm³, about 0.15 g/cm³to about 0.75 g/cm³, about 0.2 g/cm³to about 0.6 g/cm³, about 0.2 g/cm³to about 0.5 g/cm³, about 0.2 g/cm³to about 0.45 g/cm³, about 0.25 g/cm³to about 0.45 g/cm³, and about 0.25 g/cm³to about 0.4 g/cm³. Each of these values and ranges is embodied in the Examples. Density of the insulative cellular non-aromatic polymeric material may be determined by any suitable method. One example of determining density includes measuring a density of the multi-layer tube or multi-layer container, determining relative thicknesses of each layer, and calculating the density of the insulative cellular non-aromatic polymeric material using the relative thicknesses of the layers, the known density of the other layers, and the known density of the multi-layer tube or container.

In an embodiment, the insulative cellular non-aromatic polymeric material is located between and coupled to an inner polymeric layer and an outer polymeric layer to produce a multi-layer parison. The outer layer thickness of the multi-layer parison may be one of several different values or fall within one several different ranges. It is within the scope of the present disclosure for the thickness of the outer layer of the multi-layer parison to fall within one of many different ranges. In a first set of ranges, the thickness of the outer layer is one of the following ranges: about 5 mils to about 26 mils, about 6 mils to about 24 mils, about 8 mils to about 24 mils, and about 10 mils to about 24 mils. In a second set of ranges, the thickness of the outer layer of a multi-layer parison is one of the following ranges: about 5 mils to about 26 mils, about 6 mils to about 24 mils, about 8 mils to about 24 mils, and about 10 mils to about 24 mils. In another set of ranges, the outer layer thickness can be a percentage of the overall thickness of the multi-layer parison. In a set of ranges, the percentage thickness of the outer layer can be about 4% to about 9%, about 5% to about 9%, about 5% to about 8%, about 5.5% to about 8%, and about 5.5% to about 7% of the overall thickness of the multi-layer parison.

In an embodiment, the insulative cellular non-aromatic polymeric material is located between and coupled to an inner polymeric layer and an outer polymeric layer to produce a multi-layer parison. The core layer thickness of the multi-layer parison may be one of several different values or fall within one several different ranges. It is within the scope of the present disclosure for the thickness of the core layer of the multi-layer parison to fall within one of many different ranges. In a first set of ranges, the thickness is one of the following ranges: about 14 mils to 130 mils, about 20 mils to about 130 mils, about 40 mils to about 130 mils, and about 50 mils to about 130 mils. In a second set of ranges, the thickness of the core layer is one of the following ranges: about 60 mils to about 130 mils, about 70 mils to about 130 mils, about 80 mils to about 130 mils, about 90 mils to about 130 mils, and about 100 mils to about 130 mils, and about 6.5 mils to about 8 mils. In another set of ranges, the core layer thickness can be a percentage of the overall thickness of the multi-layer parison. In a first set of ranges, the percentage thickness of the outer layer can be about 4% to about 9%, about 5% to about 9%, about 5% to about 8%, about 5.5% to about 8%, and about 5.5% to about 7% of the overall thickness of the multi-layer parison.

In an embodiment, the insulative cellular non-aromatic polymeric material is located between and coupled to an inner polymeric layer and an outer polymeric layer to produce a multi-layer parison. The inner layer thickness of the multi-layer parison may be one of several different values or fall within one several different ranges. It is within the scope of the present disclosure for the thickness of the inner layer of the multi-layer parison to fall within one of many different ranges. In a first set of ranges, the thickness is one of the following ranges: about 3.0 mils to about 15.5 mils.

In an embodiment, a throughput system includes a multi-parison drop. For example, an extrusion line starts as a single line and then splits into 2, 3, 4, 5, or more lines for multiple parison drops. In an embodiment, the RPMs for the extrusion stream start at a particular level (e.g., 48 RPM) and splits evenly into 2 (e.g., 24 RPM each), 3 (e.g., 16 RPM each), 4 (12 RPM each), or more multi-parison drops splitting the RPMs. A more efficient output can be achieved by splitting the extrusion stream into multiple parison drop streams. Thereby, an embodiment includes a system comprising an extrusion stream that splits into multiple parison streams. In an embodiment, the system provides multiple foamed parison drops. Such a system that splits the extrusion line into multiple parison drops can produce foamed bottle. In an embodiment, the foamed bottles have densities as described herein.

Containers (e.g., bottles) can be subjected to a drop test, which is a test to determine a container's ability to withstand free-fall impact forces. Containers that do not pass the drop test are not suitable for commercial applications. In an illustrative embodiment, the insulative cellular non-aromatic polymeric material is coupled and located between two polymeric layers to form a multi-layer parison. The multi-layer parison is then formed, for example, via blow molding into container 14, 214, 314. The container is then filled with water and closed off with, for example, a lid. The sample container is then held at about 73 degrees Fahrenheit (22.8 degrees Celsius) and about 50% relative humidity. The filled, capped containers are then subjected to the following drop test procedure: (a) the filled, capped container is located at about five feet above a hard surface such as concrete or tile; (b) the filled, capped container is then oriented such that a bottom of the filled, capped container is arranged to lie in substantially parallel relation to the hard surface; (c) each of ten capped, filled containers are dropped; (d) upon impact, each filled, capped container is examined for any break or shattering of the wall that causes water to leak out of the bottle; and (e) the total number of bottles showing any sign of leakage after the drop test are counted as failures.

A method of producing a container or parison as described herein includes extruding or blow-molding any of the formulations described herein. An illustrative embodiment of a blow molded container 14 is FIG. 5. Another illustrative embodiment of a blow molded container 214 is FIG. 7. Another illustrative embodiment of a blow molded container 314 is FIG. 8.

In an illustrative embodiment, a formulation for producing an insulative cellular non-aromatic polymeric material includes about 98% HDPE, about 0.5% chemical blowing agent (CBA), and about 1.5% nucleating agent (e.g., talc). The formulation can be used to produce a material that is a) a monolayer forming a container or parison or b) the core layer in a multi-layer container or parison. In an illustrative multi-layer embodiment, a core layer of about 98% HDPE, about 0.5% CBA, and about 1.5% nucleating agent can be sandwiched between at least one inner polymeric layer and at least one outer polymeric layer. An illustrative outer polymeric layer includes i) about 80% HDPE, ii) 5 about % colorant, and iii) about 15% fiber. An illustrative inner polymeric layer includes about 85% HDPE and about 15% fiber.

In an illustrative embodiment, a formulation for producing an insulative cellular non-aromatic polymeric material includes about 98.75% HDPE, about 0.75% chemical blowing agent (CBA), and about 0.2% nucleating agent (e.g., talc).

In an illustrative embodiment, a formulation for producing an insulative cellular non-aromatic polymeric material includes about 98% HDPE and about 2.0% chemical blowing agent (CBA).

In an illustrative embodiment, a formulation for producing an insulative cellular non-aromatic polymeric material includes about 96.5% HDPE, about 0.5% chemical blowing agent (CBA), about 2% slip agent, and about 1% colorant.

In an illustrative embodiment, a formulation for producing an insulative cellular non-aromatic polymeric material includes about 95% HDPE, about 1.5% chemical blowing agent (CBA), about 2% slip agent, about 0.5% nucleating agent (e.g., talc) and about 1% colorant, wherein the about 95% is about a 50%/50% blend of two separate HDPE resins. Thus, each HDPE resin is about 47.5% of the total formulation of the polymeric layer by weight percentage.

In an illustrative embodiment, a formulation for producing an insulative cellular non-aromatic polymeric material includes about 82.54% HDPE, about 62% chemical blowing agent (CBA), about 2.49% slip agent, about 11.16% nucleating agent (e.g., talc) and 3.19% colorant.

In illustrative embodiments the formulation may be used to form a multi-layer container 314, as shown in FIG. 8. Multi-layer container 314 includes a floor 388, a cylindrical container wall 390, and cylindrical neck 392 as shown in FIG. 8. Multi-layer container 314 is formed of an outer layer 390A, an inner layer 390C, and a core layer 390B located therebetween that has a thickness 390D.

The following numbered paragraphs define particular embodiments of the insulative cellular non-aromatic polymeric material formulation of the invention:

- 1) about 80-about 99.9 wt % of at least one HDPE polymeric resin;
- about 0.1-about 12 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents; and
- optionally, the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 2) about 80-about 99.9 wt % of at least one HDPE polymeric resin;
- about 0.1-about 12 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents;
- about 0.5-about 3 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 3) about 84-about 99.9 wt % of at least one HDPE polymeric resin;
- about 0.1-about 3 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents; and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 4) about 84-99.9 wt % of at least one HDPE polymeric resin;
- about 0.1-about 3 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents;
- about 0.5-about 3 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 5) about 85-about 99.9 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents; and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 6) about 85-about 99.9 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents;
- about 0.5-about 3 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 7) about 85-about 99.7 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents; and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 8) about 85-about 99.7 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents;
- about 0.5-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 9) about 87-about 99.7 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents; and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 10) about 87-about 99.7 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents;
- about 0.8-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 11) about 90-about 99.7 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents; and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 12) about 90-about 99.7 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents;
- about 0.8-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 13) about 90-about 99.7 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.2 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents; and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 14) about 90-about 99.7 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.2 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents;
- about 0.8-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 15) about 92-about 99.7 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.2 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents; and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 16) about 92-about 99.7 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.2 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents;
- about 0.8-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 17) about 95-about 99.7 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.0 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents; and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 18) about 95-about 99.7 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.0 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents;
- about 0.8-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 19) about 95-about 99.5 wt % of at least one HDPE polymeric resin;
- 0.1-2.0 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents; and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 20) about 95-about 99.5 wt % of at least one HDPE polymeric resin;
- about 0.1-about 2.0 wt % of at least one nucleating agent selected from physical nucleating agents and chemical nucleating agents;
- about 0.8-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.

In any of the numbered paragraphs (1)-(20) above, the one or more HDPE polymeric resin may be selected from HDPE homopolymer or HDPE copolymer. Suitably, the one or more HDPE polymeric resin is selected from DOW® DOWLEX™ IP 41 HDPE (available from The Dow Chemical Company) that has been electron-beam modified to provide long-chain branching and a melt index of about 0.25 g/10 min, EQUISTAR® ALATHON® H5520 HDPE copolymer (available from Lyondell Chemical Company) that has been electron-beam modified to have long-chain branching and a melt index of about 0.25 g/10 min, FORMOLENE® HB5502F HDPE hexene copolymer (available from Formosa Plastics Corporation), and Marlex® HHM 5502BN HDPE hexene copolymer. In one embodiment, the one or more HDPE polymeric resin is DOW® DOWLEX™ IP 41 HDPE. In another embodiment, the one or more HDPE polymeric resin is DOW® DOWLEX™ IP 41 HDPE and FORMOLENE® HB5502F HDPE hexene copolymer. In another embodiment, the one or more HDPE polymeric resin is FORMOLENE® HB5502F HDPE hexene copolymer and EQUISTAR® ALATHON® H5520 HDPE copolymer. In one embodiment, the one or more HDPE polymeric resin is DOW® DOWLEX™ IP 41 HDPE and Marlex® HHM 5502BN HDPE hexene copolymer.

In any of the numbered paragraphs (1)-(20) above, the at least one nucleating agent may be a physical nucleating agent selected from talc, CaCO₃and/or mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E, available from Clariant Corporation). In one embodiment, the at least one nucleating agent is a mixture of talc and HYDROCEROL™ CF-40E. In another embodiment, the at least one nucleating agent is talc. In another embodiment, the at least one nucleating agent is HYDROCEROL™ CF-40E.

In any of the numbered paragraphs (1)-(20) above, the at least one slip agent may be selected from amides, fluoroelastomers, amides of fats or fatty acids, such as erucamide and oleamide, and amides from oleyl (single unsaturated C-18) through erucyl (C-22 single unsaturated). In one embodiment, the at least one slip agent is Ampacet 102823 Process Aid PE MB LLDPE.

In any of the numbered paragraphs (1)-(20) above, the colorant(s) may be selected from any suitable colorant. In one embodiment, the colorant is COLORTECH® 11933-19 Titanium Oxide Colorant.

In any of the numbered paragraphs (1)-(20) above, the impact modifier(s) may be selected from any suitable impact modifier. In one embodiment, the impact modifier is DOW® AFFINITY™ PL 1880G polyolefin plastomer.

The following numbered paragraphs define particular embodiments of the insulative cellular non-aromatic polymeric material formulation of the invention:

- 21) about 80-about 99.9 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 7 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E); and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 22) about 80-about 99.9 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 7 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E);
- about 0.5-about 3 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 23) about 84-about 99.9 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 3 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E); and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 24) about 84-about 99.9 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 3 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E);
- about 0.5-about 3 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 25) about 85-about 99.9 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E); and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 26) about 85-about 99.9 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E);
- about 0.5-about 3 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 27) about 85-about 99.7 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E); and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 28) about 85-about 99.7 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E);
- about 0.5-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 29) about 87-about 99.7 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E); and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 30) about 87-about 99.7 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E);
- about 0.8-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 31) about 90-about 99.7 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E); and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 32) about 90-about 99.7 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.5 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E);
- about 0.8-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 33) about 90-about 99.7 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.2 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E); and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 34) about 90-about 99.7 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.2 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E);
- about 0.8-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 35) about 92-about 99.7 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.2 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E); and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 36) about 92-about 99.7 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.2 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E);
- about 0.8-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 37) about 95-about 99.7 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.0 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E); and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 38) about 95-about 99.7 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.0 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E);
- about 0.8-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.
- 39) about 95-about 99.5 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.0 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E); and
- optionally the balance of the formulation comprising one or more additives selected from slip agents, colorants and impact modifiers.
- 40) about 95-about 99.5 wt % of at least one HDPE polymeric resin selected from DOW® DOWLEX™ IP 41 HDPE, EQUISTAR® ALATHON® H5520 HDPE copolymer, and FORMOLENE® HB5502F HDPE hexene copolymer, and Marlex® HHM 5502BN HDPE hexene copolymer;
- about 0.1-about 2.0 wt % of at least one nucleating agent selected from talc, CaCO₃, mica, and/or a chemical nucleating agent selected from citric acid or a citric acid-based material (e.g. HYDROCEROL™ CF-40E);
- about 0.8-about 2.5 wt % of at least one slip agent; and
- optionally the balance of the formulation comprising one or more additives selected from colorants and impact modifiers.

In any of the numbered paragraphs (21)-(40) above, the at least one slip agent may be selected from amides, fluoroelastomers, amides of fats or fatty acids, such as erucamide and oleamide, and amides from oleyl (single unsaturated C-18) through erucyl (C-22 single unsaturated). In one embodiment, the at least one slip agent is Ampacet 102823 Process Aid PE MB LLDPE.

In any of the numbered paragraphs (21)-(40) above, the colorant(s) may be selected from any suitable colorant. In one embodiment, the colorant is COLORTECH® 11933-19 Titanium Oxide Colorant.

In any of the numbered paragraphs (21)-(40) above, the impact modifier(s) may be selected from any suitable impact modifier. In one embodiment, the impact modifier is DOW® AFFINITY″ PL 1880G polyolefin plastomer.

One or more additional components and additives optionally may be incorporated, such as, but not limited to, colorants (such as, but not limited to, titanium dioxide), and compound regrind.

EXAMPLES
Example 1

Formulation and Extrusion

DOW® DOWLEX™ IP 41 HDPE was used as the polyethylene base resin. The polyethylene base resin was blended with HYDROCEROL® CF 40E as a nucleating agent and N₂as a blowing agent. Ampacet 102823 Process Aid PE MB LLDPE was added as a slip agent and COLORTECH® 11933-19 was added as a colorant. The percentages were about:

96.5%
DOW ® DOWLEX ™ IP 41 HDPE

0.5%
HYDROCEROL ® CF 40E

2.0%
Ampacet 102823 Process Aid PE MB LLDPE

1.0%
COLORTECH ® 11933-19 Titanium Oxide Colorant

The HDPE, nucleating agents, slip agent, and colorant were added to an extruder hopper and blended to provide a formulation. The formulation was then heated in the extruder to form a molten material. The blowing agent was then added to the molten material at a rate of about:

0.092
lbs/hr N₂

The N₂was injected into the molten material to expand the molten material and reduce density of the insulative cellular non-aromatic polymeric material. The resulting mixture was then extruded through a die head to establish a parison. Inner and outer polymeric layers were also extruded to locate the insulative cellular non-aromatic polymeric material therebetween to form a multi-layer parison which was then blow molded to form the insulative container.

Test Results

The insulative cellular non-aromatic polymeric material was mated to inner and outer polymeric layers to form a multi-layer parison having a density of about 0.480 grams per cubic centimeter. The multi-layer parison was then blow molded to establish an insulative container having a density of about 0.695 grams per cubic centimeter.

Example 2

Formulation and Extrusion

DOW® DOWLEX™ IP 41 HDPE was used as the polyethylene base resin. The polyethylene base resin was blended with Heritage Plastics HT6000 LLDPE talc as a nucleating agent, HYDROCEROL® CF 40E as another nucleating agent, and N₂as a blowing agent. Ampacet 102823 Process Aid PE MB LLDPE was added as a slip agent and COLORTECH® 11933-19 was added as a colorant. The percentages were about:

87.4%
DOW ® DOWLEX ™ IP 41 HDPE

5.33%
Heritage Plastics HT6000 LLDPE Based Talc Concentrate

3.88%
COLORTECH ® 11933-19 Titanium Oxide Colorant

1.45%
HYDROCEROL ® CF 40E

1.94%
Ampacet 102823 Process Aid PE MB LLDPE

The HDPE, nucleating agents, slip agent, and colorant were added to an extruder hopper and blended to provide a formulation. The formulation was then heated in the extruder to form a molten material. The blowing agent was then added to the molten material at a rate of about:

0.092
lbs/hr N₂

The N₂was injected into the molten material to expand the molten material and reduce density of the insulative cellular non-aromatic polymeric material. The resulting mixture was then extruded through a die head to establish a parison. Inner and outer polymeric layers were also extruded to locate the insulative cellular non-aromatic polymeric material therebetween to form a multi-layer parison which is then blow molded to form the insulative container.

Test Results

The insulative cellular non-aromatic polymeric material was mated to inner and outer polymeric layers and blow molded to establish an insulative container. The insulative container has a density of about 0.770 grams per cubic centimeter.

Example 3

Formulation and Extrusion

DOW® DOWLEX™ IP 41 HDPE was used as the polyethylene base resin. The polyethylene base resin was blended with Heritage Plastics HT6000 LLDPE talc as a nucleating agent, HYDROCEROL® CF 40E as another nucleating agent, and N₂as a blowing agent. Ampacet 102823 Process Aid PE MB LLDPE was added as a slip agent and COLORTECH® 11933-19 was added as a colorant. The percentages were about:

87.4%
DOW ® DOWLEX ™ IP 41 HDPE

6.3%
Heritage Plastics HT6000 LLDPE Based Talc Concentrate

3.19%
COLORTECH ® 11933-19 Titanium Oxide Colorant

0.62%
HYDROCEROL ® CF 40E

2.49%
Ampacet 102823 Process Aid PE MB LLDPE

The HDPE, nucleating agents, slip agent, and colorant were added to an extruder hopper and blended to provide a formulation. The formulation was then heated in the extruder to form a molten material. The blowing agent was then added to the molten material at a rate of about:

0.092
lbs/hr N₂

The N₂was injected into the molten material to expand the molten material and reduce density of the insulative cellular non-aromatic polymeric material. The resulting mixture was then extruded through a die head to establish a parison. Inner and outer polymeric layers were also extruded to locate the insulative cellular non-aromatic polymeric material therebetween to form a multi-layer parison which is then blow molded to form the insulative container.

Test Results

The insulative cellular non-aromatic polymeric material was mated to inner and outer polymeric layers and blow molded to establish an insulative container. The insulative container has a density of about 0.750 grams per cubic centimeter.

Example 4

Formulation and Extrusion

DOW® DOWLEX™ IP 41 HDPE was used as the polyethylene base resin. The polyethylene base resin was blended with HYDROCEROL® CF 40E as a nucleating agent and CO₂as a blowing agent. Ampacet 102823 Process Aid PE MB LLDPE was added as a slip agent and COLORTECH® 11933-19 was added as a colorant. The percentages were about:

98.25%
DOW ® DOWLEX ™ IP 41 HDPE

0.25%
HYDROCEROL ® CF 40E

0.5%
COLORTECH ® 11933-19 Titanium Oxide Colorant

1.0%
Ampacet 102823 Process Aid PE MB LLDPE

The HDPE, nucleating agent, slip agent, and colorant were added to an extruder hopper and blended to provide a formulation. The formulation was then heated in the extruder to form a molten material. The blowing agent was then added to the molten material at a rate of about:

0.09
lbs/hr CO₂

The CO₂was injected into the molten material to expand the molten material and reduce density of the insulative cellular non-aromatic polymeric material. The resulting mixture was then extruded through a die head to establish a parison. Inner and outer polymeric layers were also extruded to locate the insulative cellular non-aromatic polymeric material therebetween to form a multi-layer parison which is then blow molded to form the insulative container.

Test Results

The insulative cellular non-aromatic polymeric material was mated to inner and outer polymeric layers and blow molded to establish an insulative container. The insulative container has a density of about 0.794 grams per cubic centimeter.

Example 5

Formulation and Extrusion

FORMOSA PLASTICS® FORMOLENE™ HB5502F HDPE hexene copolymer was used as the polyethylene base resin. The polyethylene base resin was blended with HYDROCEROL® CF 40E as a nucleating agent, Heritage Plastics HT6000 LLDPE talc as another nucleating agent, and N₂as a blowing agent. The percentages were about:

98.75%
FORMOLENE(T) HB5502F HDPE hexene copolymer

0.2%
Heritage Plastics HT6000 LLDPE Based Talc Concentrate

0.75%
HYDROCEROL ® CF 40E

The HDPE and nucleating agents were added to an extruder hopper and blended to provide a formulation. The formulation was then heated in the extruder to form a molten material. The blowing agent was then added to the molten material at a rate of about:

0.125
lbs/hr N₂

The N₂was injected into the molten material to expand the molten material and reduce density of the insulative cellular non-aromatic polymeric material. The resulting mixture was then extruded through a die head to establish a parison. Inner and outer polymeric layers were also extruded to locate the insulative cellular non-aromatic polymeric material therebetween to form a multi-layer parison which is then blow molded to form the insulative container.

Test Results

The insulative cellular non-aromatic polymeric material was mated to inner and outer polymeric layers to form a multi-layer parison having a density of about 0.399 grams per cubic centimeter. The multi-layer parison was then blow molded to establish an insulative container having a density of about 0.610 grams per cubic centimeter.

Example 6

Formulations and Test Results

FORMOSA PLASTICS® FORMOLENE® HB5502F HDPE hexene copolymer was used as the polyethylene base resin. To that polyethylene base resin, one or more nucleating agents such as HYDROCEROL® CF 40E, Heritage Plastics HT6000 LLDPE talc, or Heritage Plastics HT4HP were added. In addition, N₂or CO₂were added as a blowing agent. Furthermore, in some examples, Ampacet 102823 Process Aid PE MB LLDPE was added as a slip agent and COLORTECH® 11933-19 was added as a colorant. The various formulations and resulting multi-layer parison and insulative container densities are shown below in Table 1.

TABLE 1

Comparison of different insulative cellular non-aromatic

polymeric material formulations to create various multi-layer parison and insulative

container densities

Formosa

Base
CF-

Bottle
Parison

Resin
40E

Colortech
HT4HP
Gas
Density
Density

Trial
[%]
[%]
Additive #2
[%]
[%]
[lbs/hr]
[g/cm³]
[g/cm³]

6.1
96.5
0.5
2% Ampacet
1
0
0.09 CO₂
0.797
0.481

6.2
95
1.5
2% Ampacet
1
0.5
0.08 CO₂
0.806
0.455

6.3
95
1.5
2% Ampacet
1
0.5
0.11 CO₂
0.753
0.451

6.4
95
1.5
2% Ampacet
1
0.5
0.09 N₂
0.690
0.455

6.5
95
1.5
2% Ampacet
1
0.5
0.09 N₂
0.693
0.447

6.6
95
1.5
2% Ampacet
1
0.5
0.09 N₂
0.718
0.467

6.7
96
0.5
2% Ampacet
1
0.5
0.09 N₂
0.785
0.503

6.8
96
0.5
2% Ampacet
1
0.5
0.09 N₂
0.788
0.516

6.9
96
0.5
2% Ampacet
1
0.5
0.09 N₂
0.736
0.495

6.10
96
0.5
2% Ampacet
1
0.5
0.09 N₂
0.752
0.496

6.11
96
0.5
2% Ampacet
1
0.5
0.09 N₂
0.749
0.473

6.12
96.5
0.5
2% Ampacet
1
0
0.09 N₂
0.779
0.498

6.13
99.9
0.1

0
0.03 N₂
0.918
0.785

6.14
99.4
0.1
0.5%

0
0.1 N₂
0.730
0.502

HT6000

6.15
97.4
0.1
2.5%

0
0.125 N₂
0.632
0.434

HT6000

6.16
99.25
0.75

0
0.1 N₂
0.723
0.688

6.17
98.75
0.75
0.5%

0
0.125 N₂
0.606
0.568

HT6000

6.18
96.75
0.75
2.5%

0
0.03 N₂
0.892
0.470

HT6000

6.19
98
2.0

0
0.125 N₂
0.481
0.416

6.20
97.5
2.0
0.5%

0
0.03 N₂
0.846
0.478

HT6000

6.21
95.5
2.0
2.5%

0
0.1 N₂
0.597
0.411

HT6000

6.22
98.75
0.75
0.4%

0
0.125 N₂
0.573
0.414

HT6000

Example 7

Formulations and Test Results

FORMOSA PLASTICS® FORMOLENE® HB5502F HDPE hexene copolymer was used as the polyethylene base resin. To that polyethylene base resin, HYDROCEROL® CF 40E and Heritage Plastics HT6000 LLDPE talc as nucleating agents were added. In addition, N₂was added as a blowing agent. The percentages were about:

98.75% FORMOLENE(T) HB5502F HDPE hexene copolymer

0.75% HYDROCEROL® CF 40E

0.3% Heritage Plastics HT6000 LLDPE Based Talc Concentrate

The HDPE and nucleating agents were added to an extruder hopper and blended to provide a formulation. The formulation was then heated in the extruder to form a molten material. A blowing agent was then added to the molten material at a rate of about:

0.12 lbs/hr N₂

The N₂was injected into the molten material to expand the molten material and reduce density of the insulative cellular non-aromatic polymeric material. The resulting mixture was then extruded through a die head to establish a parison. Inner and outer polymeric layers were also extruded to locate the insulative cellular non-aromatic polymeric material therebetween to form a multi-layer parison which is then blow molded to form the insulative container.

Test Results

The insulative cellular non-aromatic polymeric material was mated to inner and outer polymeric layers to form a multi-layer parison having a density of about 0.407 grams per cubic centimeter. The multi-layer parison was then blow molded to establish an insulative container having a density of about 0.577 grams per cubic centimeter.

Example 8

Formulation and Extrusion

FORMOSA PLASTICS® FORMOLENE® HB5502F HDPE hexene copolymer and EQUISTAR® ALATHON® H5520 HDPE copolymer were used as polyethylene base resins. The polyethylene base resins were blended with HYDROCEROL® CF 40E as a nucleating agent and Heritage Plastics HT6000 LLDPE talc as another nucleating agent, and N₂as a blowing agent. Ampacet 102823 Process Aid PE MB LLDPE was added as a slip agent and COLORTECH® 11933-19 was added as a colorant. The percentages were about:

47.5%
FORMOLENE ® HB5502F HDPE hexene copolymer

47.5%
EQUISTAR ® ALATHON ® H5520 HDPE copolymer

0.5%
Heritage Plastics HT4HP Talc

1.5%
HYDROCEROL ® CF 40E

2.0%
Ampacet 102823 Process Aid PE MB LLDPE

1.0%
COLORTECH ® 11933-19 Titanium Oxide Colorant

The HDPE, nucleating agents, slip agents, and colorants were added to an extruder hopper and blended to provide a formulation. The formulation was then heated in the extruder to form a molten material. The blowing agent was then added to the molten material at a rate of about:

0.12
lbs/hr N₂

The N₂was injected into the molten material to expand the molten material and reduce density of the insulative cellular non-aromatic polymeric material. The resulting mixture was then extruded through a die head to establish a parison. Inner and outer polymeric layers were also extruded to locate the insulative cellular non-aromatic polymeric material therebetween to form a multi-layer parison which is then blow molded to form the insulative container.

Test Results

The insulative cellular non-aromatic polymeric material was mated to inner and outer polymeric layers to form a multi-layer parison having a density of about 0.396 grams per cubic centimeter. The multi-layer parison was then blow molded to establish an insulative container having a density of about 0.519 grams per cubic centimeter.

Example 9

Formulations and Test Results

FORMOSA PLASTICS® FORMOLENE® HB5502F HDPE hexene copolymer and EQUISTAR® ALATHON® H5520 HDPE copolymer were used as polyethylene base resins. The polyethylene base resins were used in various percentages from about 23.875% to about 74.925% of the formulation. The polyethylene base resins were blended with HYDROCEROL® CF 40E as a nucleating agent and Heritage Plastics HT6000 LLDPE talc as another nucleating agent, and CO₂or N₂as a blowing agent. The blowing agent was used at levels between about 0.3 lbs/hr to about 1.25 lbs/hour. Ampacet 102823 Process Aid PE MB LLDPE was added as a slip agent and COLORTECH® 11933-19 was added as a colorant. In some examples, DOW® AFFINITY™ PL 1880G polyolefin elastomer was added as an impact modifier to the formulation. The various formulations and resulting multi-layer parison and insulative container densities are shown below in Table 2.

TABLE 2

Comparison of different insulative cellular non-aromatic

polymeric material formulations to create various multi-layer parison and insulative

container densities

Formosa

Base

Bottle
Parison

Resin
Base Resin
Additive
Additive
Additive
Additive
N₂
Density
Density

Trial
[%]
#2
#1
#2
#3
#4
[lbs/hr]
[g/cm³]
[g/cm³]

9.1
47.5
47.5% LBI
1.5% CF-
2%
1%
0.5%
0.092
0.649
0.423

40E
Ampacet
Colortech
HT4HP

9.2
24.98
74.925%
0.1% CF-

0.03
0.906
0.771

LBI
40E

0.25MI

9.3
24.7
74.0625%
0.75%
0.5%

0.1
0.668
0.611

LBI
CF-40E
HT6000

0.25MI

9.4
23.875
71.625%
2% CF-
2.5%

0.125
0.851
0.720

LBI
40E
HT6000

0.25MI

9.5
49.7
49.7% LBI
0.1% CF-
0.5%

0.125
0.668
0.436

0.25MI
40E
HT6000

9.6
48.375
48.375%
0.75%
2.5%

0.03
0.903
0.711

LBI
CF-40E
HT6000

0.25MI

9.7
49
49% LBI
2% CF-

0.1
0.626
0.425

0.25MI
40E

9.8
73.05
24.35%
0.1% CF-
2.5%

0.1
0.751
0.495

LBI
40E
HT6000

0.25MI

9.9
74.44
24.8125%
0.75%

0.125
0.578
0.422

LBI
CF-40E

0.25MI

9.10
73.125
24.375%
2% CF-
0.5%

0.03
0.858
0.566

LBI
40E
HT6000

0.25MI

9.11
42.25
42.25%
15% Dow
0.1%
0.4%

0.125
0.640
0.441

LBI
Impact
CF-40E
HT6000

0.25MI
Mod

9.12
42.25
42.25%
15% Dow
0.1%
0.4%

0.1
0.742
0.502

LBI
Impact
CF-40E
HT6000

0.25MI
Mod

9.13
42.25
42.25%
15% Dow
0.1%
0.4%

0.1
0.735
0.508

LBI
Impact
CF-40E
HT6000

0.25MI
Mod

9.14
42.25
42.25%
15% Dow
0.1%
0.4%

0.1
0.766
0.512

LBI
Impact
CF-40E
HT6000

0.25MI
Mod

Example 10

Formulations and Test Results

FORMOSA PLASTICS® FORMOLENE® HB5502F HDPE hexene copolymer was used as polyethylene base resin. The polyethylene base resin was used in various percentages from about 97.95% to about 100% of the formulation. In some examples, the polyethylene base resin was blended with HYDROCEROL® CF 40E as a nucleating agent and Heritage Plastics HT6000 LLDPE talc as another nucleating agent, and N₂as a blowing agent. The blowing agent was used at levels between about 0.05 lbs/hr to about 0.15 lbs/hour. COLORTECH® 11933-19 was added as a colorant in some examples. The various formulations and resulting multi-layer parison and insulative container densities are shown below in Table 3.

TABLE 3

Comparison of different insulative cellular non-aromatic

polymeric material formulations to create various multi-layer parison

and insulative container densities

For-

mosa

CF-

Bottle
Parison

5502F
Colortech
40E
HT6000
N₂
Density
Density

Trial
[%]
[%]
[%]
[%]
[lbs/hr]
[g/cm³]
[g/cm³]

10.1
97.95
1
0.75
0.3
0.1222
0.7183
*

10.2
98
0
2
0
0.0529
0.6950
*

10.3
99.25
0
0.75
0
0.0534
0.7296
*

10.4
99
0
1.0
0
0.0511
0.7404
0.4292

10.5
98.7
0
1.0
0.3
0.0514
0.7316
0.4272

10.6
98.45
0
1.25
0.3
0.0521
0.7309
0.4276

10.7
98.75
0
1.25
0
0.0529
0.7303
0.4236

10.8
98.75
0
1.25
0
0.0522
0.7136
0.4234

10.9
98.75
0
1.25
0
0.0538
0.7214
0.4304

10.10
100
0
0
0
0.1468
*
*

10.11
100
0
0
0
0.1392
*
*

10.12
99.9
0
0
0.1
0.1393
*
*

10.13
99.5
0
0
0.5
0.0656
*
*

10.14
99.4
0
0.1
0.5
0.0702
*
*

10.15
99.3
0
0.2
0.5
0.0692
*
*

10.16
99.7
0
0.1
0.2
0.0673
*
*

10.17
99.7
0
0.1
0.2
0.0892
*
*

10.18
99.7
0
0.1
0.2
0.105
*
*

10.19
99.7
0
0.1
0.2
0.1188
*
*

10.20
99.7
0
0.1
0.2
0.0915
*
*

10.21
99.05
0
0.75
0.2
0.0906
*
*

* Data not available

Example 11

Formulations and Test Results

Bottles were formed from 99.4 wt % FORMOSA PLASTICS® FORMOLENE® HB5502F HDPE hexene copolymer as the polyethylene base resin blended with 0.1 wt % HYDROCEROL® CF 40E as a nucleating agent and 0.5 wt % Heritage Plastics HT6000 LLDPE talc as another nucleating agent with 0.04 lbs/hr of N₂blowing agent. The resulting bottles and parisons were a single layer (i.e., monolayer). The resulting monolayer parison and monolayer container densities are shown under the various process conditions.

TABLE 4

Comparison of process parameters on bottle and parison densities.

Run
Cycle

Parison ρ
Bottle ρ

[#]
[s]
Air [psi]
Vacuum
[g/cm³]
[g/cm³]

1
14
40
Off
0.546
0.748

2
14
40
On
0.570
0.795

3
14
60
Off
0.542
0.706

4
14
60
On
0.538
0.724

5
15
40
Off
0.553
0.792

6
15
40
On
0.559
0.789

7
15
60
Off
0.542
0.844

8
15
60
On
0.550
0.798

9
16
40
Off
0.536
0.649

10
16
40
On
0.549
0.788

11
16
60
Off
0.540
0.825

12
16
60
On
0.555
0.840

13
17
40
Off
0.548
0.791

14
17
40
On
0.544
0.789

15
17
60
Off
0.543
0.716

16
17
60
On
0.548
0.707

17
18
40
Off
0.546
0.806

18
18
40
On
0.540
0.792

19
18
60
Off
0.533
0.833

20
18
60
On
0.547
0.829

Example 12

Formulations and Test Results

FORMOSA PLASTICS® FORMOLENE® HB5502F HDPE hexene copolymer was used as polyethylene base resin. The polyethylene base resin was used in 99.4 wt % of the formulation. The polyethylene base resin was either 100% virgin HDPE (i.e., the control) or a combination of virgin HDPE and regrind. The regrind was a foam bottle produced according to Example 11, ground up, and then put back into the system. The polyethylene base resin was blended with 0.1 wt % HYDROCEROL® CF 40E as a nucleating agent and 0.5 wt % Heritage Plastics HT6000 LLDPE talc as another nucleating agent, and N₂as a blowing agent. The blowing agent was used at about 0.04 lbs/hr. The various formulations and resulting monolayer parison and insulative container densities are shown below in Table 5.

TABLE 5

Comparison of percent virgin and percent regrind on bottle and

parison densities.

Virgin
Regrind
Cycle
Parison ρ
Bottle ρ

Run [#]
[%]
[%]
Time [s]
[g/cm³]
[g/cm³]

Control
100
0
15
0.617
0.757

1
80
20
14
0.524
0.769

2
80
20
15
0.493
0.728

3
80
20
16
0.499
0.747

4
60
40
14
0.519
0.747

5
60
40
15
0.531
0.751

6
60
40
16
0.523
0.742

7
40
60
14
0.493
0.718

8
40
60
15
0.435
0.697

9
40
60
16
0.444
0.682

10
20
80
14
0.442
0.690

11
20
80
15
0.483
0.726

12
20
80
16
0.493
0.728

The bottles produced with regrind as part of the base polyethylene maintained densities of about 80%.

Another set of bottles was produced as described immediately above except that the regrind was a 2nd pass regrind.

TABLE 6

Comparison of percent virgin and percent 2nd pass regrind on

bottle and parison densities.

Virgin
Regrind
Cycle
Parison ρ
Bottle ρ

Run [#]
[%]
[%]
Time [s]
[g/cm³]
[g/cm³]

1
80
20
14
0.536
0.773

2
80
20
15
0.502
0.764

3
80
20
16
0.496
0.778

Even with 2nd pass regrind, bottle characteristics were very similar to the characteristics of bottles produced with virgin HDPE.

Example 13

Effect of RPM on Bottle Formation

FORMOSA PLASTICS® FORMOLENE® HB5502F HDPE hexene copolymer was used as polyethylene base resin, at about 99.4%. The polyethylene base resin was blended with 0.1% HYDROCEROL® CF 40E as a nucleating agent and Heritage Plastics HT6000 LLDPE talc as another nucleating agent, and N₂as a blowing agent. The blowing agent was used at about 0.04 lbs/hr. This formulation was processed at various RPMs to produce bottles. Thus, the only variable in the bottle formation of these different runs was the RPMs of the throughput system.

TABLE 7

Effect of RPMs on Drop Test results.

Drop

Parison

Top
Test

ρ
Bottle ρ
Weight
Thickness
Load
[Pass

Run [#]
RPM
[g/cm³]
[g/cm³]
[g]
[mils]
[lbs-F]
%]

5
48
0.711
0.892
54.5
41.2
87.562
100

1
36
0.660
0.842
50.2
37.7
92.696
100

1A
36
0.638
0.780
51.5
43.6
89.578
100

2
27
0.577
0.817
53.4
42.1
105.806
100

3
18
0.495
0.756
45.0
37.0
73.94
20

4
11
0.396
0.601
32.0
30.7
36.764
0

Changing the RPM in the throughput system produced changes to bottle and parison characteristics. For example, higher RPMs produced a higher density parison and higher density bottle. Thereby, using a lower RPM in the throughput system produced lower density bottles. Although these systems utilized a single drop, this shows that a multi-parison drop system is possible. For example, a throughput system can start at a particular RPM (e.g., 48 RPM) for the extrusion stream and then and then split into multiple parison streams at lower RPMs. In an illustrative example, one extrusion stream can start at 48 RPM and split into 4 parison drop streams running at 12 RPM. This would produce a more efficient foaming system to produce bottles.

Example 14

Density Measurements

This Example demonstrates the test used to measure the density of filled and unfilled polymer parts.

Procedure

The density was determined by the apparatus shown, unassembled, in FIG. 4. Although not shown in FIG. 4, the apparatus also included a thermometer to measure the suspension liquid temperature. A suspension liquid is a fluid with a density lower than that of the sample to be measured. The sample must sink in the suspension fluid to determine the sample density. Water has a density of 1 g/cm³, so most unfilled polymers require some other suspension fluid such as isopropyl alcohol, density=0.8808 g/cm³. A Mettler AT400 balance (Mettler-Toledo LLC, Columbus, Ohio) was also used.

The density of a limestone-filled HDPE bottle was measured. After taring the balance to zero, the dry solid sample was weighed after placing it in the cup of the Mettler balance. The dry weight was 0.3833 g. After weighing the dry sample and before removing the sample from the cup, the balance was tared again. The sample was removed from the cup and placed on the gem holder in the suspension fluid. The sample was weighed providing the weight with a negative number (−0.3287 g). The number was converted to its absolute value (0.3287 g); the positive value is the sample buoyancy. The sample density was calculated by multiplying the dry weight (0.3833 g) by the sample buoyancy (0.3287 g) by the suspension fluid density (0.8808 g/cc), which equaled 1.0272 g/cc.

Example 15

Formulations and Test Results

Marlex® HHM 5502BN HDPE hexene copolymer (Chevron Phillips Chemical Company, The Woodlands, Tex.) was used as polyethylene base resin in the core layer. The polyethylene base resin was used in various percentages from about 98% to about 100% of the formulation. In some examples, the polyethylene base resin was blended with HYDROCEROL® CF 40E as a chemical blowing agent in all non-control samples and Heritage Plastics HT4HP talc as another nucleating agent, and N₂as a blowing agent. The blowing agent was used at about 11 kg/hr. The various formulations and resulting multi-layer parison and insulative container densities are shown below in Table 3.

The extruded material was a multi-layer material where the core layer was sandwiched between an outer and inner polymeric layer. The outer and inner layer were comprised of various amounts of Marlex® HHM 5502BN HDPE hexene copolymer (Chevron Phillips). The outer polymeric layer also included 5 wt % colorant (COLORTECH® 11933-19 titanium oxide). The inner polymeric layer did not include a colorant. Some embodiments of the formulations included inner and/or outer polymeric layers comprising a reinforcing fiber (Hyperform® HPR-803i, Milliken & Co., Spartanburg, S.C.).

TABLE 8

Comparison of different insulative cellular non-aromatic

polymeric material formulations to create various multi-layer parison and insulative

container densities

Core Layer
Outer Layer
Inner Layer

Sample
HDPE
CBA
Talc
HDPE
Color
Fiber
HDPE
Fiber

Control
100%
0%
0%
95%
5%
0%
100%
0%

1-1
100%
0.10%
0.30%
95%
5%
0%
100%
0%

1-2
100%
0.10%
0.30%
95%
5%
0%
100%
0%

1-3
100%
0.10%
0.30%
95%
5%
0%
100%
0%

1-4
98.4%
0.10%
1.50%
95%
5%
0%
100%
0%

1-5
98.4%
0.10%
1.50%
95%
5%
0%
100%
0%

1-6
98.4%
0.10%
1.50%
95%
5%
0%
100%
0%

1-7
99.2%
0.50%
0.30%
95%
5%
0%
100%
0%

1-8
99.2%
0.50%
0.30%
95%
5%
0%
100%
0%

1-9
99.2%
0.50%
0.30%
95%
5%
0%
100%
0%

1-10
98.0%
0.50%
1.50%
95%
5%
0%
100%
0%

1-10A
98.0%
0.50%
1.50%
80%
5%
15%
85%
15%

1-11
98.0%
0.50%
1.50%
95%
5%
0%
100%
0%

1-12
98.0%
0.50%
1.50%
95%
5%
0%
100%
0%

1-13
99.6%
0.10%
0.30%
85%
5%
10%
100%
0%

1-14
99.6%
0.10%
0.30%
80%
5%
15%
100%
0%

1-15
99.6%
0.10%
0.30%
75%
5%
20%
100%
0%

TABLE 9

Effect of formulation on Physical Characteristics, Bottle and

Parison Density, and Performance

Bottle ρ
Parison ρ
Weight
Density
Water Drop [%

Sample
[g/cm³]
[g/cm³]
[g]
[g/cm³]
passed test]

Control

23.0
0.934
100

1-1
0.58
0.46
17.1
0.710
70

1-2
0.655
0.46
16.9
0.734
80

1-3
0.79
0.46
17.1
0.760
70

1-4
0.58
0.45
17.7
0.644
90

1-5
0.70
0.45
17.2
0.685
100

1-6
0.80
0.45
16.8
0.744
80

1-7
0.60
0.5
17.4
0.612
60

1-8
0.69
0.5
17.3
0.697
100

1-9
0.74
0.5
17.1
0.760
100

1-10
0.61

17.0
0.625
100

1-10A
0.47

17.0
0.479
60

1-11
0.67

17.1
0.693
100

1-12
0.82

17.5
0.784
100

1-13
0.61

17.0
0.624
100

1-14
0.67

17.5
0.656
90

1-15
0.62

17.1
0.665
90

Example 16

Multi-Layer Tubes Comprising Various Amounts of Chemical Blowing Agent and Formed at Various Temperatures

Outer-layer formulation 44 comprised about 85% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 10% of a reinforcing fiber blend of about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company). Core-layer formulation 48 comprised between about 99.2% and about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), as shown in Table 10, which was used as a polyethylene base resin. The polyethylene base resin was blended with between about 0.1% and about 0.5% HYDROCEROL® CF 40E as a chemical blowing agent (CBA) and nucleating agent, as shown in Table 10, and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at a level of about 0.044 kg/h.

The extruder head temperature was varied between about 180° C. and about 190° C., and the core layer extruder barrel temperature was varied between about 180° C. and about 190° C., as shown in Table 10. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The layers were extruded such that the inner layer provided about 6% of the thickness of the entire tube, the outer layer provided about 6% of the thickness of the entire tube, and the core layer provided about 88% of the thickness of the entire tube. For each formulation, density was measured for six tubes according to the procedure of Example 2, as shown in Table 11 as Density. The average of the six densities for each formulation is shown as Average Density in Table 11. The melt temperature for each formulation was also determined and is reported in Table 11 as Melt Temp.

TABLE 10

Amount of CBA, amount of HDPE, head temperature, and barrel

temperature for tubes of Example 16.

Head Temp
Barrel Temp

Trial [#]
CBA [%]
HDPE [%]
[° C.]
[° C.]

12.A.0
0.10
99.6
180
180

12.A.1
0.50
99.2
180
180

12.A.2
0.10
99.6
190
180

12.A.3
0.50
99.2
190
180

12.A.4
0.10
99.6
180
190

12.A.5
0.50
99.2
180
190

12.A.6
0.10
99.6
190
190

12.A.7
0.50
99.2
190
190

TABLE 11

Density, average density, and melt temperature for tubes of

Example 16.

Average Density
Melt Temp

Trial [#]
Density [g/cm³]
[g/cm³]
[° C.]

12.A.0a
0.488
0.493
180

12.A.0b
0.499

12.A.0c
0.486

12.A.0d
0.495

12.A.0e
0.494

12.A.0f
0.498

12.A.1a
0.491
0.509
180

12.A.1b
0.514

12.A.1c
0.509

12.A.1d
0.517

12.A.1e
0.510

12.A.1f
0.511

12.A.2a
0.484
0.480
180

12.A.2b
0.486

12.A.2c
0.470

12.A.2d
0.486

12.A.2e
0.474

12.A.2f
0.482

12.A.3a
0.500
0.504
181

12.A.3b
0.499

12.A.3c
0.503

12.A.3d
0.508

12.A.3e
0.504

12.A.3f
0.509

12.A.4a
0.495
0.500
190

12.A.4b
0.505

12.A.4c
0.493

12.A.4d
0.507

12.A.4e
0.494

12.A.4f
0.505

12.A.5a
0.498
0.500
190

12.A.5b
0.506

12.A.5c
0.486

12.A.5d
0.507

12.A.5e
0.495

12.A.5f
0.510

12.A.6a
0.484
0.492
189

12.A.6b
0.494

12.A.6c
0.494

12.A.6d
0.494

12.A.6e
0.492

12.A.6f
0.493

12.A.7a
0.512
0.514
190

12.A.7b
0.523

12.A.7c
0.511

12.A.7d
0.520

12.A.7e
0.490

12.A.7f
0.526

Example 17

Multi-Layer Tubes Formed at Various N₂Flow Rates

Outer-layer formulation 44 comprised about 85% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 10% of a reinforcing fiber blend of about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company).

Core-layer formulation 48 comprised about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin. The polyethylene base resin was blended with about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at a level between about 0.034 kg/h and about 0.104 kg/h, as shown in Table 12.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The layers were extruded such that the inner layer provided about 6% of the thickness of the entire tube, the outer layer provided about 6% of the thickness of the entire tube, and the core layer provided about 88% of the thickness of the entire tube. In one embodiment, the inner layer provided about 5.8% of the thickness of the entire tube, the outer layer provided about 6.1% of the thickness of the entire tube, and the core layer provided about 88.2% of the thickness of the entire tube. In another embodiment, the inner layer provided about 5.9% of the thickness of the entire tube, the outer layer provided about 6.1% of the thickness of the entire tube, and the core layer provided about 88.0% of the thickness of the entire tube. The thicknesses for two tubes formed at each N₂flow rate were measured and are described in Table 13 as Outer Layer Thickness, Core Layer Thickness, Inner Layer Thickness, and Total Thickness. For each N₂flow rate, density was measured for four tubes according to the procedure of Example 14, as shown in Table 14 as Parison Density. The average of the four densities for each N₂flow rate is shown as Average Density in Table 14. The melt temperature for each formulation was also determined and is reported in Table 14 as Melt Temp.

TABLE 12

N₂flow rate for tubes of Example 17.

Trial [#]
N₂Flow Rate [kg/h]

12.B.0
0.034

12.B.1
0.044

12.B.2
0.054

12.B.3
0.064

12.B.4
0.074

12.B.5
0.084

12.B.6
0.094

12.B.7
0.104

TABLE 13

Outer layer thickness, core layer thickness, inner layer

thickness, and total thickness for tubes of Example 17.

Outer Layer
Core Layer
Inner Layer
Total

Thickness
Thickness
Thickness
Thickness

Trial [#]
[mils] [%]
[mils] [%]
[mils] [%]
[mils]

12.B.0a
7.18 (6.0)
104.24 (86.8)
8.63 (7.2)
120.05

12.B.0b
6.87 (6.1)
98.98 (87.4)
7.44 (6.6)
113.29

12.B.1a
5.46 (4.6)
106.51 (89.0)
7.67 (6.4)
119.64

12.B.1b
6.39 (5.4)
103.43 (87.7)
8.06 (6.8)
117.88

12.B.2a
6.93 (5.5)
110.55 (87.6)
8.76 (6.9)
126.24

12.B.2b
7.25 (5.5)
114.98 (87.9)
8.52 (6.5)
130.75

12.B.3a
7.77 (5.8)
119.12 (88.6)
7.54 (5.6)
134.43

12.B.3b
7.00 (5.2)
118.8 (88.7)
8.07 (6.0)
133.87

12.B.4a
8.79 (6.7)
115.64 (87.4)
7.28 (5.5)
131.71

12.B.4b
7.62 (5.5)
123.04 (89.5)
6.85 (5.0)
137.51

12.B.5a
8.03 (5.8)
122.68 (89.4)
6.56 (4.8)
137.27

12.B.5b
6.81 (5.1)
119.64 (89.8)
6.82 (5.1)
133.27

12.B.6a
7.07 (5.2)
120.52 (89.2)
7.50 (5.6)
135.09

12.B.6b
6.95 (4.9)
128.6 (91.2)
5.43 (3.9)
140.98

12.B.7a
6.60 (6.7)
84.9 (86.8)
6.33 (6.5)
97.83

12.B.7b
8.51 (9.1)
76.01 (81.6)
8.65 (9.3)
93.17

TABLE 14

Density, average density, and melt temp for tubes

of Example 17.

Density
Average Density
Melt Temp

Trial [#]
[g/cm³]
[g/cm³]
[° C.]

12.B.0a
0.554
0.542
180

12.B.0b
0.537

12.B.0c
0.538

12.B.0d
0.540

12.B.1a
0.506
0.508
180

12.B.1b
0.505

12.B.1c
0.513

12.B.1d
0.508

12.B.2a
0.466
0.470
180

12.B.2b
0.472

12.B.2c
0.472

12.B.2d
0.468

12.B.3a
0.425
0.431
180

12.B.3b
0.430

12.B.3c
0.434

12.B.3d
0.435

12.B.4a
0.401
0.408
180

12.B.4b
0.407

12.B.4c
0.411

12.B.4d
0.414

12.B.5a
0.379
0.374
180

12.B.5b
0.370

12.B.5c
0.372

12.B.5d
0.375

12.B.6a
0.393
0.398
180

12.B.6b
0.393

12.B.6c
0.401

12.B.6d
0.405

12.B.7a
0.559
0.544
180

12.B.7b
0.541

12.B.7c
0.537

12.B.7d
0.540

Example 18

Formulations and Test Results for Tubes with about 6% Inner/Outer Layer Thickness and Bottles Formed Therefrom

Outer-layer formulation 44 comprised about 85% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 10% of a reinforcing fiber blend of about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company).

Core-layer formulation 48 comprised about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin. The polyethylene base resin was blended with about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at levels between about 0.034 kg/h and about 0.104 kg/h as shown in Table 15.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The layers were extruded such that the inner layer provided about 6% of the thickness of the entire tube, the outer layer provided about 6% of the thickness of the entire tube, and the core layer provided about 88% of the thickness of the entire tube. In one embodiment, the inner layer provided about 6.1% of the thickness of the entire tube, the outer layer provided about 5.8% of the thickness of the entire tube, and the core layer provided about 88.2% of the thickness of the entire tube. For each N₂flow rate, the mean density of several tubes was measured according to the procedure of Example 14 and is shown below in Table 15 as Average Tube Density.

For tubes where tube density was not measured, a mold was closed around the tube and a blow needle was inserted into a space formed in the tube and a container was blow molded. For each N₂flow rate, the mean density of several bottles was measured according to the procedure of Example 14 and is shown below in Table 15 as Average Bottle Density.

TABLE 15

N₂flow rate, average tube density, and average bottle

density for tubes and bottles of Example 18.

Average

N₂Flow
Tube
Average Bottle

Rate
Density
Density

Trial [#]
[kg/h]
[g/cm³]
[g/cm³]

13.A.1
0.034
0.542
0.705

13.A.2
0.044
0.508
0.674

13.A.3
0.054
0.470
0.674

13.A.4
0.064
0.431
0.616

13.A.5
0.074
0.408
0.574

13.A.6
0.084
0.374
0.553

13.A.7
0.094
0.398
0.572

13.A.8
0.104
0.544
0.622

* Data not available

Example 19

Formulations and Test Results for Tubes with about 12% Inner/Outer Skin Thickness

Outer-layer formulation 44 comprised about 85% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 10% of a reinforcing fiber blend of about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company).

Core-layer formulation 48 comprised about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin. The polyethylene base resin was blended with about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at levels between about 0.044 kg/h and about 0.114 kg/h as shown in Table 16.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The layers were extruded such that the inner layer provided about 12% of the thickness of the entire tube, the outer layer provided about 12% of the thickness of the entire tube, and the core layer provided about 76% of the thickness of the entire tube. In one embodiment, the inner layer provided about 10.9% of the thickness of the entire tube, the outer layer provided about 11.1% of the thickness of the entire tube, and the core layer provided about 78.0% of the thickness of the entire tube. For each N₂flow rate, average outer, core, and inner layer thicknesses of the tubes were measured and are shown in Table 16. Also, for each of N₂flow rate, density was measured for four tubes according to the procedure of Example 14 and is shown in Table 17 as Density. The average of the four densities for each N₂flow rate is shown as Average Density in Table 17.

TABLE 16

N₂flow rate, outer layer thickness, core layer thickness, inner

layer thickness, and total thickness for tubes of Example 19.

N₂

Flow
Outer Layer
Core Layer
Inner Layer
Total

Rate
Thickness
Thickness
Thickness
Thickness

Trial [#]
[kg/h]
[mils] [%]
[mils] [%]
[mils] [%]
[mils]

13.B.0.1
0.044
14.29 (12.3)
86.21 (74.5)
15.29 (13.2)
115.79

13.B.1.1
0.054
13.79 (11.1)
98.07 (78.8)
12.54 (10.1)
124.4

13.B.2.1
0.064
13.04 (10.8)
93.23 (77.3)
14.29 (11.9)
120.56

13.B.3.1
0.074
13.37 (10.8)
97.92 (79.3)
12.2 (9.9)
123.49

13.B.4.1
0.084
13.12 (9.9)
105.76 (79.7)
13.79 (10.4)
132.67

13.B.5.1
0.094
13.70 (11.3)
94.82 (78.2)
12.7 (10.5)
121.22

13.B.6.1
0.104
13.62 (11.8)
90.23 (78.3)
11.36 (9.9)
115.21

13.B.7.1
0.114
13.46 (11.0)
95.15 (77.5)
14.13 (11.5)
122.74

TABLE 17

Density and average density for tubes of Example 19.

Trial [#]
Density [g/cm³]
Average Density [g/cm³]

13.B.0.1a
0.567
0.563

13.B.0.1b
0.553

13.B.0.1c
0.571

13.B.0.1d
0.559

13.B.1.1a
0.539
0.529

13.B.1.1b
0.534

13.B.1.1c
0.517

13.B.1.1d
0.526

13.B.2.1a
0.507
0.500

13.B.2.1b
0.503

13.B.2.1c
0.487

13.B.2.1d
0.502

13.B.3.1a
0.484
0.479

13.B.3.1b
0.479

13.B.3.1c
0.478

13.B.3.1d
0.476

13.B.4.1a
0.437
0.431

13.B.4.1b
0.428

13.B.4.1c
0.431

13.B.4.1d
0.427

13.B.5.1a
0.430
0.432

13.B.5.1b
0.421

13.B.5.1c
0.445

13.B.5.1d
0.433

13.B.6.1a
0.491
0.489

13.B.6.1b
0.466

13.B.6.1c
0.497

13.B.6.1d
0.502

13.B.7.1a
0.528
0.494

13.B.7.1b
0.525

13.B.7.1c
0.464

13.B.7.1d
0.460

Example 20

Formulations and Test Results for Bottles with about 12% Inner/Outer Skin Thickness

Outer-layer formulation 44 comprised about 85% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 10% of a reinforcing fiber blend of about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company).

Core-layer formulation 48 comprised about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin. The polyethylene base resin was blended with about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at levels between about 0.044 kg/h and about 0.114 kg/h as shown in Table 18.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The layers were extruded such that the inner layer provided about 12% of the thickness of the entire tube, the outer layer provided about 12% of the thickness of the entire tube, and the core layer provided about 76% of the thickness of the entire tube.

A mold was closed around the tube and a blow needle was inserted into a space formed in the tube and a container was blow molded. After molding, the inner layer of the bottle provided about 15% of the thickness of the entire bottle, the outer layer of the bottle provided about 15% of the thickness of the entire bottle, and the core layer of the bottle provided about 70% of the thickness of the entire bottle. In one embodiment, the inner layer of the bottle provided about 13.2% of the thickness of the entire bottle, the outer layer of the bottle provided about 17.5% of the thickness of the entire bottle, and the core layer of the bottle provided about 69.3% of the thickness of the entire bottle. In this embodiment, blow molding caused the inner layer's contribution to bottle thickness to increase by 20.9%, the outer layer's contribution to bottle thickness to increase by 57.4%, and the core layer's contribution to bottle thickness to decrease by 11.1%. The thicknesses for two tubes formed at each N₂flow rate were measured and are described in Table 18 as Outer Layer Thickness, Core Layer Thickness, Inner Layer Thickness, and Total Thickness. Also, for each of N₂flow rate, density was measured for three bottles according to the procedure of Example 14 and is shown in Table 19 as Bottle Density. The average of the four densities for each N₂flow rate is shown as Average Bottle Density in Table 19. Mean weight of several bottles was measured and is shown in Table 19.

TABLE 18

N₂flow rate, outer layer thickness, core layer thickness, inner

layer thickness, and total thickness for bottles of Example 20.

N₂Flow
Outer Layer
Core Layer
Inner Layer
Total

Rate
Thickness
Thickness
Thickness
Thickness

Trial [#]
[kg/h]
[mils] [%]
[mils] [%]
[mils] [%]
[mils]

13.B.0.2
0.044
8.98 (19.3)
30.5 (65.7)
6.94 (15.0)
46.42

13.B.1.2
0.054
7.39 (19.5)
25.07 (66.2)
5.4 (14.3)
37.86

13.B.2.2
0.064
5.73 (17.9)
21.28 (66.3)
5.08 (15.8)
32.09

13.B.3.2
0.074
7.59 (21.2)
22.59 (63.1)
5.64 (15.7)
35.82

13.B.4.2
0.084
4.79 (15.3)
23.16 (73.8)
3.45 (11.0)
31.4

13.B.5.2
0.094
6.6 (13.6)
37.47 (77.0)
4.6 (9.5)
48.67

13.B.6.2
0.104
8.65 (20.1)
28.1 (65.2)
6.38 (14.8)
43.13

13.B.7.2
0.114
8.27 (13.4)
47.55 (77.1)
5.85 (9.5)
61.67

TABLE 19

Bottle density, average bottle density, and bottle weight for

bottles of Example 20.

Bottle Density
Average Bottle
Bottle Weight

Trial [#]
[g/cm³]
density [g/cm³]
[g]

13.B.0.2a
0.748
0.758
20.30

13.B.0.2b
0.763

13.B.0.2c
0.762

13.B.1.2a
0.715
0.728
19.54

13.B.1.2b
0.737

13.B.1.2c
0.733

13.B.2.2a
0.718
0.716
18.89

13.B.2.2b
0.713

13.B.2.2c
0.717

13.B.3.2a
0.677
0.670
18.47

13.B.3.2b
0.659

13.B.3.2c
0.674

13.B.4.2a
0.624
0.636
17.71

13.B.4.2b
0.622

13.B.4.2c
0.662

13.B.5.2a
0.623
0.594
17.19

13.B.5.2b
0.585

13.B.5.2c
0.575

13.B.6.2a
0.593
0.576
16.69

13.B.6.2b
0.545

13.B.6.2c
0.590

13.B.7.2a
0.571
0.555
16.85

13.B.7.2b
0.522

13.B.7.2c
0.573

Example 21

Formulations and Test Results for Tubes with about 18% Inner/Outer Skin Thickness

Outer-layer formulation 44 comprised about 85% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 10% of a reinforcing fiber blend of about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company).

Core-layer formulation 48 comprised about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin. The polyethylene base resin was blended with about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at levels between about 0.044 kg/h and about 0.124 kg/h as shown in Table 20.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The layers were extruded such that the inner layer provided about 18% of the thickness of the entire tube, the outer layer provided about 18% of the thickness of the entire tube, and the core layer provided about 64% of the thickness of the entire tube. In one embodiment, the inner layer provided about 15.1% of the thickness of the entire tube, the outer layer provided about 17.1% of the thickness of the entire tube, and the core layer provided about 67.8% of the thickness of the entire tube. For each N₂flow rate, average outer, core, and inner layer thicknesses of the tubes were measured and are shown in Table 20. Also, for each of N₂flow rate, density was measured for four tubes according to the procedure of Example 14 and is shown in Table 21 as Density. The average of the four densities for each N₂flow rate is shown as Average Density in Table 21.

Table 20. N₂flow rate, outer layer thickness, core layer thickness, inner layer thickness, and total thickness for tubes of Example 21.

TABLE 20

N₂flow rate, outer layer thickness, core layer thickness, inner

layer thickness, and total thickness for tubes of Example 21.

N₂Flow
Outer Layer
Core Layer
Inner Layer
Total

Rate
Thickness [mils]
Thickness [mils]
Thickness [mils]
Thickness

Trial [#]
[kg/h]
[%]
[%]
[%]
[mils]

13.C.0.1
0.044
25.32 (20.5)
75.52 (61.2)
22.64 (18.3)
123.48

13.C.1.1
0.054
21.47 (16.8)
84.05 (65.8)
22.14 (17.3)
127.66

13.C.2.1
0.074
18.13 (14.5)
91.65 (73.1)
15.54 (12.4)
125.32

13.C.3.1
0.084
18.48 (14.5)
89.08 (69.8)
20.1 (15.7)
127.66

13.C.4.1
0.094
18.63 (15.6)
83.14 (69.7)
17.46 (14.6)
119.23

13.C.5.1
0.104
19.47 (17.3)
77.6 (68.8)
15.72 (13.9)
112.79

13.C.6.1
0.114
20.56 (19.3)
71.17 (66.9)
14.62 (13.7)
106.35

13.C.7.1
0.124
19.63 (23.0)
49.96 (58.6)
15.71 (18.4)
85.3

13.C.8.1
0.064
19.55 (15.5)
87.64 (69.6)
18.8 (14.9)
125.99

TABLE 21

Density and average density for tubes of Example 21.

Trial [#]
Density [g/cm³]
Average Density [g/cm³]

13.C.0.1a
0.601
0.605

13.C.0.1b
0.599

13.C.0.1c
0.608

13.C.0.1d
0.610

13.C.1.1a
0.582
0.575

13.C.1.1b
0.561

13.C.1.1c
0.579

13.C.1.1d
0.579

13.C.2.1a
0.514
0.512

13.C.2.1b
0.533

13.C.2.1c
0.500

13.C.2.1d
0.500

13.C.3.1a
0.490
0.482

13.C.3.1b
0.491

13.C.3.1c
0.477

13.C.3.1d
0.468

13.C.4.1a
0.442
0.504

13.C.4.1b
0.517

13.C.4.1c
0.501

13.C.4.1d
0.555

13.C.5.1a
0.474
0.518

13.C.5.1b
0.581

13.C.5.1c
0.460

13.C.5.1d
0.555

13.C.6.1a
0.503
0.576

13.C.6.1b
0.627

13.C.6.1c
0.531

13.C.6.1d
0.644

13.C.7.1a
0.610
0.506

13.C.7.1b
0.469

13.C.7.1c
0.538

13.C.7.1d
0.406

13.C.8.1a
0.496
0.496

13.C.8.1b
0.494

13.C.8.1c
0.485

13.C.8.1d
0.508

Example 22

Formulations and Test Results for Bottles with about 18% Inner/Outer Skin Thickness

Outer-layer formulation 44 comprised about 85% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 10% of a reinforcing fiber blend of about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company).

Core-layer formulation 48 comprised about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin. The polyethylene base resin was blended with about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at levels between about 0.044 kg/h and about 0.124 kg/h as shown in Table 22.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The layers were extruded such that the inner layer provided about 18% of the thickness of the entire tube, the outer layer provided about 18% of the thickness of the entire tube, and the core layer provided about 64% of the thickness of the entire tube.

A mold was closed around the tube and a blow needle was inserted into a space formed in the tube and a container was blow molded. After molding, the inner layer of the bottle provided about 22% of the thickness of the entire bottle, the outer layer of the bottle provided about 22% of the thickness of the entire bottle, and the core layer of the bottle provided about 56% of the thickness of the entire bottle. In one embodiment, the inner layer of the bottle provided about 20.1% of the thickness of the entire bottle, the outer layer of the bottle provided about 24.2% of the thickness of the entire bottle, and the core layer of the bottle provided about 55.7% of the thickness of the entire bottle. In this embodiment, blow molding caused the inner layer's contribution to bottle thickness to increase by 32.7%, the outer layer's contribution to bottle thickness to increase by 41.7%, and the core layer's contribution to bottle thickness to decrease by 17.8%. The thicknesses for two tubes formed at each N₂flow rate were measured and are described in Table 21 as Outer Layer Thickness, Core Layer Thickness, Inner Layer Thickness, and Total Thickness. Also, for each of N₂flow rate, density was measured for three bottles according to the procedure of Example 14 and is shown in Table 23 as Bottle density. The average of the four densities for each N₂flow rate is shown as Average Bottle Density in Table 23. Mean weight of several bottles was measured and is shown in Table 46.

TABLE 22

N₂flow rate, outer layer thickness, core layer thickness, inner

layer thickness, and total thickness for bottles of Example 22.

N₂Flow
Outer Layer
Core Layer
Inner Layer
Total

Rate
Thickness
Thickness
Thickness
Thickness

Trial [#]
[kg/h]
[mils] [%]
[mils] [%]
[mils] [%]
[mils]

13.C.0.2
0.044
11.45 (28.6)
20.86 (52.1)
7.72 (19.3)
40.03

13.C.1.2
0.054
7.72 (26.3)
14.01 (47.7)
7.64 (26.0)
29.37

13.C.2.2
0.074
10.03 (24.8)
22.72 (56.1)
7.76 (19.2)
40.51

13.C.3.2
0.084
9.55 (24.9)
21.59 (56.4)
7.15 (18.7)
38.29

13.C.4.2
0.094
8.73 (26.0)
17.42 (51.8)
7.47 (22.2)
33.62

13.C.5.2
0.104
9.91 (29.1)
16.29 (47.8)
7.88 (23.1)
34.08

13.C.6.2
0.114
7.51 (19.8)
22.54 (59.4)
7.92 (20.9)
37.97

13.C.7.2
0.124
10.03 (14.1)
52.99 (74.3)
8.27 (11.6)
71.29

13.C.8.2
0.064
10.4 (28.5)
19.1 (52.4)
6.98 (19.1)
36.48

TABLE 23

Density and average density for tubes of Example 22.

Trial [#]
Density [g/cm³]
Average Density [g/cm³]

13.C.0.1a
0.601
0.605

13.C.0.1b
0.599

13.C.0.1c
0.608

13.C.0.1d
0.610

13.C.1.1a
0.582
0.575

13.C.1.1b
0.561

13.C.1.1c
0.579

13.C.1.1d
0.579

13.C.2.1a
0.514
0.512

13.C.2.1b
0.533

13.C.2.1c
0.500

13.C.2.1d
0.500

13.C.3.1a
0.490
0.482

13.C.3.1b
0.491

13.C.3.1c
0.477

13.C.3.1d
0.468

13.C.4.1a
0.442
0.504

13.C.4.1b
0.517

13.C.4.1c
0.501

13.C.4.1d
0.555

13.C.5.1a
0.474
0.518

13.C.5.1b
0.581

13.C.5.1c
0.460

13.C.5.1d
0.555

13.C.6.1a
0.503
0.576

13.C.6.1b
0.627

13.C.6.1c
0.531

13.C.6.1d
0.644

13.C.7.1a
0.610
0.506

13.C.7.1b
0.469

13.C.7.1c
0.538

13.C.7.1d
0.406

13.C.8.1a
0.496
0.496

13.C.8.1b
0.494

13.C.8.1c
0.485

13.C.8.1d
0.508

Example 23

Formulations and Test Results for Tubes with Varying N₂Saturation

Outer-layer formulation 44 comprised about 75% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 20% of a reinforcing fiber blend of about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company).

Core-layer formulation 48 comprised about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin. The polyethylene base resin was blended with about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at a level between about 0.045 kg/h and about 0.070 kg/h, corresponding to between about 0.20% and about 0.30% as shown in Table 24.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. The core layer extruder was operated at 13 RPM. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The layers were extruded such that the inner layer provided about 11% of the thickness of the entire tube, the outer layer provided about 14% of the thickness of the entire tube, and the core layer provided about 75% of the thickness of the entire tube. The layer thicknesses for several tubes of flow rate were measured and the mean values of these thicknesses for each tube are described in Table 24 as Inner Layer Thickness and Outer Layer Thickness.

TABLE 24

N₂saturation, N₂flow rate, inner layer thickness, and outer

layer thickness, and total thickness for tubes of Example 23.

N₂
N₂Flow
Inner Layer
Outer Layer

Saturation
Rate
Thickness
Thickness [mils]

Trial [#]
[%]
[kg/h]
[%]
[%]

14.A.1
0.20
0.045
11.65
16.55

14.A.2
0.22
0.0495
11.55
16.15

14.A.3
0.24
0.054
11.65
16.55

14.A.4
0.26
0.0585
*
*

14.A.5
0.28
0.0629
*
*

14.A.6
0.30
0.069
*
*

*Data not available

Example 24

Formulations and Test Results for Bottles with Varying N₂Saturation

Outer-layer formulation 44 comprised about 75% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 20% of a reinforcing fiber blend of about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company).

Core-layer formulation 48 comprised about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin. The polyethylene base resin was blended with about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at a level between about 0.045 kg/h and about 0.070 kg/h as shown in Table 25.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. The core layer extruder was operated at 13 RPM. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The layers were extruded such that the inner layer provided about 11% of the thickness of the entire tube, the outer layer provided about 14% of the thickness of the entire tube, and the core layer provided about 75% of the thickness of the entire tube.

A mold was closed around the tube and a blow needle was inserted into a space formed in the tube and a container was blow molded. For each N₂flow rate, the weight of three bottles was measured and is shown in Table 25 as Bottle Weight. The average of the three weights for each N₂flow rate is shown as Average Bottle Weight in Table 25. Also, for each N₂flow rate, density was measured for three bottles according to the procedure of Example 14 and is shown in Table 25 as Bottle Density. The mean of the three densities for each N₂flow rate is shown as Average Bottle Density in Table 25.

TABLE 25

N₂flow rate, bottle weight, average bottle weight, bottle

density, and average bottle density for bottles of Example 24.

N₂Flow
Bottle
Average
Bottle
Average

Rate
Weight
Bottle
density
Bottle density

Trial [#]
[kg/h]
[g]
Weight [g]
[g/cm³]
[g/cm³]

14.A.1a
0.045
17.21
17.3
0.710
0.710

14.A.1b

17.08

0.703

14.A.1c

17.61

0.718

14.A.2a
0.0495
17.01
16.9
0.694
0.700

14.A.2b

17.01

0.696

14.A.2c

16.7

0.697

14.A.3a
0.054
17.08
17.0
0.674
0.670

14.A.3b

16.96

0.671

14.A.3c

16.95

0.668

14.A.4a
0.0585
17.38
17.4
0.651
0.653

14.A.4b

17.5

0.655

14.A.4c

17.36

0.653

14.A.5a
0.0629
17.14
17.2
0.653
0.646

14.A.5b

17.17

0.642

14.A.5c

17.16

0.644

14.A.6a
0.069
16.84
16.9
0.640
0.642

14.A.6b

16.91

0.649

14.A.6c

16.81

0.637

Example 25

Formulations and Test Results for Tubes with Varying N₂Saturation

Outer-layer formulation 44 comprised about 75% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 20% of a reinforcing fiber blend of about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company). In some embodiments, the inner-layer formulation 40 comprises about 3% to about 7.5% reinforcing fiber.

Core-layer formulation 48 comprised about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin. The polyethylene base resin was blended with about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at a level between about 0.045 kg/h and about 0.070 kg/h, corresponding to between about 0.20% and about 0.30% as shown in Table 26.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. The core layer extruder was operated at 13 RPM. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The inner layer extruder was operated at 20 rpm and the outer layer extruded was operated at 34 rpm such that the inner layer provided about 8% of the thickness of the entire tube, the outer layer provided about 14% of the thickness of the entire tube, and the core layer provided about 78% of the thickness of the entire tube. The layer thicknesses for several tubes of flow rate were measured and the mean values of these thicknesses for each tube are described in Table 26 as Inner Layer Thickness and Outer Layer Thickness.

TABLE 26

N₂saturation, N₂flow rate, inner layer thickness, and outer

layer thickness, and total thickness for tubes of Example 25.

N₂
N₂Flow
Inner Layer
Outer Layer

Saturation
Rate
Thickness
Thickness

Trial [#]
[%]
[kg/h]
[%]
[%]

14.A.7
0.20
0.045
7.30
16.85

14.A.8
0.22
0.0495
9.05
15.15

14.A.9
0.24
0.054
8.85
17.2

14.A.10
0.26
0.0585
11.8
18.9

14.A.11
0.28
0.0629
*
*

14.A.12
0.30
0.069
*
*

*Data not available

Example 26

Formulations and Test Results for Bottles with Varying N₂Saturation

Outer-layer formulation 44 comprised about 75% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 20% of a reinforcing fiber blend of about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company).

Core-layer formulation 48 comprised about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin. The polyethylene base resin was blended with about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at a level between about 0.045 kg/h and about 0.070 kg/h as shown in Table 27.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. The core layer extruder was operated at 13 RPM. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The inner layer extruder was operated at 20 rpm and the outer layer extruded was operated at 34 rpm such that the inner layer provided about 8% of the thickness of the entire tube, the outer layer provided about 14% of the thickness of the entire tube, and the core layer provided about 78% of the thickness of the entire tube.

A mold was closed around the tube and a blow needle was inserted into a space formed in the tube and a container was blow molded. For each N₂flow rate, the weight of three bottles was measured and is shown in Table 27 as Bottle Weight. The average of the three weights for each N₂flow rate is shown as Average Bottle Weight in Table 27. Also, for each N₂flow rate, density was measured for three bottles according to the procedure of Example 14 and is shown in Table 27 as Bottle Density. The mean of the three densities for each N₂flow rate is shown as Average Bottle Density in Table 27.

TABLE 27

N₂flow rate, bottle weight, average bottle weight, bottle

density, and average bottle density for bottles of Example 26.

N₂Flow
Bottle
Average
Bottle
Average

Rate
Weight
Bottle
density
Bottle density

Trial [#]
[kg/h]
[g]
Weight [g]
[g/cm³]
[g/cm³]

14.A.7a
0.045
17.02
17.0
0.694
0.691

14.A.7b

17.13

0.700

14.A.7c

16.81

0.678

14.A.8a
0.0495
17.23
17.2
0.669
0.659

14.A.8b

17.2

0.652

14.A.8c

17.3

0.657

14.A.9a
0.054
17.26
17.2
0.606
0.618

14.A.9b

17.24

0.641

14.A.9c

17.18

0.607

14.A.10a
0.0585
16.85
16.9
0.617
0.600

14.A.10b

16.93

0.593

14.A.10c

16.9

0.590

14.A.11a
0.0629
17.31
17.2
0.562
0.569

14.A.11b

17.09

0.589

14.A.11c

17.21

0.557

14.A.12a
0.069
17
17.1
0.601
0.585

14.A.12b

17.31

0.577

14.A.12c

17.11

0.578

Example 27

Formulations and Test Results for Bottles with Varying Process Aid

Outer-layer formulation 44 comprised between about 72% and about 75% of a base resin blend of 50% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company) and 50% DOW LLDPE 5004I Polyethylene, Low Density (available from the Dow Chemical Company) about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, about 20% of a reinforcing fiber blend of about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem), and between about 0% and about 3% of an Ampacet 102823 as a process aid. Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company). The outer-layer formulation is further described in Table 28.

Core-layer formulation 48 comprised between about 99.6% and about 99.9% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin. The polyethylene base resin was blended with between about 0.1% and about 0.3% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent and between about 0.1% and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at a level between of about 0.060 kg/h. The core-layer formulation is further described in Table 28.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. The core layer extruder was operated at 13 RPM. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The inner layer extruder was operated at 20 rpm and the outer layer extruded was operated at 34 rpm such that the inner layer provided about 8% of the thickness of the entire tube, the outer layer provided about 14% of the thickness of the entire tube, and the core layer provided about 78% of the thickness of the entire tube.

A mold was closed around the tube and a blow needle was inserted into a space formed in the tube and a container was blow molded. For each N₂flow rate, the weight of ten bottles was measured. The average of the ten weights for each N₂flow rate is shown as Average Bottle Weight in Table 29. Also, for each N₂flow rate, density was measured for three bottles according to the procedure of Example 14 and is shown in Table 29 as Bottle Density. The mean of the three densities for each N₂flow rate is shown as Average Bottle Density in Table 29.

TABLE 28

Amounts base resin blend, process aid, HDPE, talc, and

chemical blowing agent for bottles of Example 27.

Outer Layer
Core Layer

Trial
Base resin
102823
5502BN
HT6000
CF 40E

[#]
blend [%]
[%]
[%]
[%]
[%]

14.B.1
75
0
99.6
0.3
0.1

14.B.2
75
0
99.9
0
0.1

14.B.3
75
0
99.7
0
0.3

14.B.4
72
3
99.6
0.3
0.1

14.B.5
72
3
99.9
0
0.1

14.B.6
72
3
99.7
0
0.3

14.B.7
75
0
99.9
0
0.1

TABLE 29

Average bottle weight, bottle density, and average

bottle density for bottles of Example 27.

Average
Bottle
Average

Trial
Bottle Weight
density
Bottle density

[#]
[g]
[g/cm³]
[g/cm³]

14.B.1a
17.1 ± 0.3
0.672
0.68

14.B.1b

0.683

14.B.1c

0.690

14.B.2a
17.0 ± 0.1
0.669
0.67

14.B.2b

0.678

14.B.2c

0.676

14.B.3a
17.1 ± 0.2
0.665
0.67

14.B.3b

0.675

14.B.3c

0.669

14.B.4a
17.0 ± 0.4
0.670
0.67

14.B.4b

0.676

14.B.4c

0.676

14.B.5a
17.2 ± 0.2
0.681
0.68

14.B.5b

0.670

14.B.5c

0.674

14.B.6a
17.0 ± 0.2
0.672
0.67

14.B.6b

0.665

14.B.6c

0.667

14.B.7a
17.1 ± 0.2
0.657
0.65

14.B.7b

0.655

14.B.7c

0.648

Example 28

Formulation and Test Results for Bottles with 50% Regrind

Outer-layer formulation 44 comprised about 75% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 20% of a reinforcing fiber blend of about 15% Hyperform® HPR-803i (available from Milliken Chemical) and about 85% Braskem F020HC High Crystallinity Polypropylene (available from Braskem). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company).

Core-layer formulation 48 comprised about 50% first-pass regrind material and about 50% of a formulation comprising about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin, blended with about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent, and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at a level between that led to 0.22% N₂saturation.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The layers were extruded such that the inner layer provided about 11% of the thickness of the entire tube, the outer layer provided about 14% of the thickness of the entire tube, and the core layer provided about 75% of the thickness of the entire tube.

A mold was closed around the tube and a blow needle was inserted into a space formed in the tube and a container was blow molded. The weights of three bottles were measured to be 17.25 g, 17.16 g, and 17.39 g leading to an average weight of 17.3 g. Also, density was measured for three bottles according to the procedure of Example 14 to be 0.689 g/cm³, 0.676 g/cm³, and 0.680 g/cm³leading to an average density of 0.682 g/cm³.

Example 29

Formulations and Test Results for Bottles with Various Amounts of Regrind

Outer-layer formulation 44 comprised about 75% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 12.5% Braskem Polypropylene Inspire 6025N (available from Braskem), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 7.5% Hyperform® HPR-803i (available from Milliken Chemical). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company).

Core-layer formulation 48 comprised between about 0% and about 50% first-pass regrind material, as shown in Table 28, and between about 0% and about 50% of a formulation comprising about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin, blended with about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent, and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at a level that led to 0.22% N₂saturation.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The layers were extruded such that the inner layer provided about 11% of the thickness of the entire tube, the outer layer provided about 14% of the thickness of the entire tube, and the core layer provided about 75% of the thickness of the entire tube.

A mold was closed around the tube and a blow needle was inserted into a space formed in the tube and a container was blow molded. The average of the weights for each N₂flow rate is shown as Average Bottle Weight in Table 30. Also, for each formulation, density was measured for several bottles according to the procedure of Example 14. The mean of the densities for each formulation is shown as Average Bottle Density in Table 30.

TABLE 30

Amount of regrind, average bottle weight, bottle density,

and average bottle density for bottles of Example 29.

Average

Trial
Regrind
Bottle Density

[#]
[%]
[g/cm³]

16.A.1
0
0.685 ± 0.008

16.B.1
25
0.690 ± 0.004

16.B.2
50
0.670 ± 0.015

Example 30

Formulations and Test Results for Bottles with Various Amounts of Regrind

Outer-layer formulation 44 comprised about 75% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), about 12.5% Braskem Polypropylene Inspire 6025N (available from Braskem), about 5% Ampacet 112761 White Polyethylene Masterbatch (available from Ampacet Corporation) as a coloring agent, and about 7.5% Hyperform® HPR-803i (available from Milliken Chemical). Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company).

Core-layer formulation 48 comprised between about 0% and about 50% regrind material, as shown in Table 31, and between about 0% and about 50% of a formulation comprising about 99.6% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company), which was used as a polyethylene base resin, blended with about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent, and about 0.3% Heritage Plastics HT6000 LLDPE talc as another nucleating agent. Several stages of bottles production were performed using different amounts of multiple-pass regrind, as shown in Table 31. First pass regrind was obtained from bottles made of virgin material (stage 0), second pass regrind was obtained from bottles made of material from stage 1, third pass regrind was obtained from bottles made of material from stage 2, fourth pass regrind was obtained from bottles made of material from stage 3, fifth pass regrind was obtained from bottles made of material from stage 4, and sixth pass regrind was obtained from bottles made of material from stage 5. N₂was used as a blowing agent and was injected into the rest of the molten core-layer formulation 48 at a level between that led to 0.22% N₂saturation.

The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The layers were extruded such that the inner layer provided about 14% of the thickness of the entire tube, the outer layer provided about 14% of the thickness of the entire tube, and the core layer provided about 72% of the thickness of the entire tube.

A mold was closed around the tube and a blow needle was inserted into a space formed in the tube and a container was blow molded.

TABLE 31

Pass level of regrind material used in different stages of

production of bottles of Example 30.

Regrind Stage

Stage 0
Stage 1
Stage 2
Stage 3
Stage 4
Stage 5
Stage 6

Virgin
100.00%
50.00%
50.00%
50.00%
50.00%
50.00%
50.00%

1st Pass

50.00%
25.00%
25.00%
25.00%
25.00%
25.00%

2nd Pass

25.00%
12.50%
12.50%
12.50%
12.50%

3rd Pass

12.50%
6.25%
6.25%
6.25%

4th Pass

6.25%
3.13%
3.13%

5th Pass

3.13%
1.56%

6th Pass

1.56%

Example 31

Top Load Measurement Method

Top Load Measurements

General Procedure

Top load testing determines how much force a container can withstand before the container fails or necks in to form an hourglass shape. Various containers 10 were subjected to top load testing. An Instron tester, such as and generally consistent with an Instron Series 5500 Load Frame, may be used to determine top load performance

The top load test was generally performed according to the following procedure. A container was placed on a flat surface such that the floor of the container was arranged to lie in a substantially parallel relation to the flat surface. A crosshead of the Instron tester applied a compressive force to the top of the neck of the container. A load transducer, mounted in series with the container, measured the applied load. Containers 10 were tested until they failed or necked in to form an hourglass shape. Once failure or necking was observed, the value shown on Instron tester was recorded.

Example 32

Parison Cell Counting Method

General Procedure

Parison cell counting is a measurement of the quality of the foam of the extruded material. The extruded material, for example a parison, is cut in cross sections and viewed with microscopy. The number of cells are counted in a given unit volume, for example cubic inches.

A square of the sample to be subjected to the parison cell counting method is cut out from the center of the parison. The excised square of the parison is then divided by cutting across the diagonal exposing the underlying cell structure. The cells are then visualized and counted using microscopy.

Example 33

Formulations and Test Results for Tubes with Varying LDPE

Outer-layer formulation 44 comprised about 95% Dow DMDA 6400 NT7 and about 5% Ampacet 11078 as a white colorant. Inner-layer formulation 40 comprised about 100% Marlex® HHM 5502BN HDPE (available from Chevron Phillips Chemical Company).

Core-layer formulation 48 comprised a percentage of DOW DMDA 6400 NT7 as shown in Table 32, a percentage of DOW™ LDPE 692 LDPE HEALTH+™ as shown in Table 32 to form a core masterbatch that was about 98.9% of the overall formulation, about 0.1% HYDROCEROL® CF 40E as a chemical blowing agent and nucleating agent, and about 1% Heritage Plastics HT4HP talc as another nucleating agent. The N₂was introduced at about 0.032 kg/h. The extruder head temperature was about 190° C., and the core layer extruder barrel temperature was about 180° C. The inner and outer layer extruder barrel temperatures were both 190° C. The resulting expanded core-layer formulation 48 was extruded through a die head to establish a core-layer parison. The core layer extruder was operated at 13 RPM. Inner and outer layers were extruded through the die head, locating the expanded formulation therebetween, to form a multi-layer tube. The inner layer extruder was operated at 20 rpm and the outer layer extruded was operated at 34 rpm such that the inner layer provided about 15% of the thickness of the entire tube, the outer layer provided about 15% of the thickness of the entire tube, and the core layer provided about 70% of the thickness of the entire tube. The multi-layer tube was blow molded to form a container, as shown for example in FIG. 8, to provide a multi-layer bottle wherein the inner layer is about 30%, the outer layer is about 30% and the core layer is about 40% of the total bottle thickness. The Top Load performance was measured according to the Top Load Method described in Example 31, and the results are shown in Table 32. The parison was analyzed using the Cell Count of Parison Method described in Example 32, and the results are shown in Table 32. Table 32 shows the parison densities, the cell count of the parison in the diagonal, the bottle density, and the top load measurement.

TABLE 32

Characteristics of the parison and bottles formed in Example 33.

Parison
Cell count of
Bottle
Top

Percentage
Density
parison in
Density
Load

LDPE
(g/cm³)
diagonal
(g/cm³)
(lbsF)

0
0.526
1,081,339
0.710
91.42

10
0.531
1,712,299
0.723
92.21

20
0.522
1,761,616
0.714
94.03

30
0.517
2,033,991
0.711
87.91

40
0.517
2,542,148
0.720
88.35

50
0.514
2,942,949
0.711
87.28

60
0.514
2,842,743
0.714
86.78

70
0.507
3,276,861
0.705
87.66

80
0.506
3,121,752
0.708
82.65

90
0.512
3,174,007
0.682
80.96

100
0.491
2,877,073
0.657
89.33