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  Stable polyamides for simultaneous solid phase polymerization of polyesters and polyamidesUSPTO Application #: 20070093616Title: Stable polyamides for simultaneous solid phase polymerization of polyesters and polyamides Abstract: This specification discloses polyamides which remain stable and do not form gels when the polyamides are exposed to solid phase polymerization conditions associated with the polyester. (end of abstract) Agent: M&g Usa, Corporation - Sharon Center, OH, US Inventors: Joachim Strauch, Maria Teresa Scrivani, Simone Ferrero, Gianluca Ferrari, Douglas David Callander, Arianna Giovannini USPTO Applicaton #: 20070093616 - Class: 525425000 (USPTO) Related Patent Categories: Synthetic Resins Or Natural Rubbers -- Part Of The Class 520 Series, Natural Rubber Compositions Having Nonreactive Materials (dnrm) Other Than: Carbon, Silicon Dioxide, Glass Titanium Dioxide, Water, Hydrocarbon, Halohydrocarbon, Ethylenically Unsaturated Reactant Admixed With A Preformed Reaction Product Derived From: (a) At Least One Polycarboxylic Acid, Ester, Or Anhydride; (b) At Least One Polyhydroxy Compound; And (c) At Least One Fatty Acid Glycerol Ester, Or A Fatty Acid Or Salt Derived From A Naturally Occurring Glyceride, Tall Oil, Or A Tall Oil Fatty Acid, Solid Polymer Derived From At Least One Carboxylic Acid Or Derivative, Solid Polymer Derived From At Least One Lactam; From An Amino Carboxylic Acid Or Derivative; Or From A Polycarboxylic Acid Or Derivative, Solid Polymer Derived From An Amino Carboxylic Acid Or Derivative; From A Polyamine And A Polycarboxylic Acid Or Derivative; From At Least One Lactam; Or From A Polyamine Salt Of A Polycarboxylic Acid, Mixed With Polycarboxylic Acid Or Derivative And Polyhydroxy Reactant Or Polymer Therefrom The Patent Description & Claims data below is from USPTO Patent Application 20070093616. Brief Patent Description - Full Patent Description - Patent Application Claims
PRIORITIES AND CROSS REFERENCE [0001] This patent application claims the benefit of the priority of U.S. Provisional Patent Application Ser. No. 60/730,197 filed Oct. 25, 2005 and U.S. Provisional Patent Application Ser. No. 60/730,198 filed Oct. 25, 2005. The teachings of these provisional patent applications are incorporated in their entirety herein by reference. FIELD OF THE INVENTION [0002] This invention relates to polyamides suitable for the simultaneous solid phase polymerization of polyesters and polyamides at polyester conditions. BACKGROUND OF THE INVENTION [0003] Many industrial articles are comprised of multiple components to economically improve their properties. Multi-component articles made from thermoplastic and thermoset materials are generally manufactured with a final melt-mixing extruder that homogenously combines the various components into an article such as a sheet, film, fiber, a bottle or an injection molded part, frequently called a preform. The article, particularly the preform, is often further processed to make another article such as a bottle, tray, jar, or bag. [0004] Many packages integrate the materials into a separate layer in the wall of the container. This is accomplished by using one extruder to melt a major component and form the article while a second extruder melts the barrier material and injects the barrier material in a separate layer of the article that forms the wall of the container. U.S. Pat. No. 4,501,781, for example, describes improving passive barrier properties of the container by incorporating a polyamide layer and a polyester layer to make a multi-layer container. [0005] U.S. Pat. No. 4,501,781 also teaches that the polyamide can be homogeneously blended with the polyester in the container wall as opposed to the polyamide being placed in a separate layer. When using homogeneously combined materials, manufacturing economies are maximized the earlier the materials are combined. In the case of polyamides and polyesters, both benefit from the thermal process known as solid phase polymerization. [0006] Solid phase polymerization efficiently increases the number average molecular weight of both polyesters and polyamides. The increase in number average molecular weight can be measured with many techniques such as inherent viscosity (Inh. V.) and intrinsic viscosity (I.V.), relative viscosity (R.V.), and the total number of end groups (TEG). In the solid phase polymerization process the pellets are exposed to temperatures less than the temperature at which the pellets become liquid. This temperature exposure occurs in the presence of a driving force such as an inert gas or vacuum. The by-products of the polymerization reaction are removed from the pellet thus forcing an equilibrium increase in the molecular weight of the polymer. The thermal processing can occur from 40.degree. C. to a temperature slightly less than the temperature at which the pellet becomes liquid, such as 1.degree. C., or for more typically for commercial reasons, 5.degree. C. below the temperature at which the pellet becomes liquid. [0007] Because polyesters and polyamides are both pelletized during their respective manufacture, U.S. Pat. No. 5,340,884 advocates combining the polyester and polyamide at the first cutting step after polycondensation to eliminate additional and/or subsequent extrusion and cutting steps. But, U.S. Pat. No. 5,340,884 also cautions against blending the polyamide and polyester as they are removed from the polycondensation reactor if the polyester/polyamide blend will be subjected to further thermal processing such as solid state polymerization. Subsequent thermal processing may create undesirable color and/or haze and alter the molecular weight of the polyamide during extended time at elevated temperatures. [0008] U.S. Pat. No. 6,238,233 teaches blending acid terminated polyamides with polyester. However, U.S. Pat. No. 6,238,233 cautions against blending the molten polyester with acid terminated polyamide as it is removed from the polycondensation reactor before it is pelletized if the polyester/polyamide blend will be subjected to solid state [phase] polymerization since undesirable color and/or haze may develop during extended time at elevated temperatures. [0009] WO 2005/110694 A1 teaches the use of the compartmentalized pellet to reduce the color caused by simultaneously thermally treating a polyester-polyamide blend. According to WO 2005/110694 A1, the polyester-polyamide composition does not exhibit increased color during thermal processing when the majority of the polyester is placed in one compartment or zone of the pellet and the majority of the polyamide is placed in another compartment or zone prior to thermal processing. WO 2005/110694 A1 acknowledges that certain compounds are not stable at high processing temperatures and extended processing times. WO 2005/110694 A1 teaches to use a reaction enhancer or raise the starting molecular weight to allow the pellet to solid phase polymerized at a lower temperature and shorter time if one of the components cannot withstand the higher process temperatures. These approaches increase the cost to thermally process the materials together. [0010] There exists therefore, the need for a polyamide composition which allows a pellet containing polyester and polyamide to be solid phase polymerized without detrimental impact on the properties of either material. SUMMARY OF THE INVENTION [0011] Disclosed in this invention is a resin composition comprising a polyester selected from the group consisting of crystallizable polyesters that have at least 85% of the crystallizable polyester acid moieties derived from the group consisting of terephthalic acid, 2,6 naphthalene dicarboxylic acid and their diesters and a polyamide comprising a residue selected from the group consisting of the repeating unit of amino caproic acid and the repeating unit of A-D, wherein A is the residue of a dicarboxylic acid comprising adipic acid, isophthalic acid, terephthalic acid, 1,4-cyclohexanedicarboxylic acid, or naphthalenedicarboxylic acid, or a mixture thereof, and D is a residue of a diamine comprising m-xylylene diamine, p-xylylene diamine, hexamethylene diamine, ethylene diamine, or 1,4 cyclohexanedimethylamine, or a mixture thereof, wherein the polyamide has a triamine content after hydrolysis of less than 0.22 and a carboxyl content of outside the range of 20 to 80 percent of the total number of end groups. It is further disclosed that the resin composition can have at least 90% of the crystallizable polyester's acid moieties derived from terephthalic acid and at least 90% of the crystallizable polyester's glycol moieties are derived from ethylene glycol. A preferred polyamide, MXD6 is also disclosed. It is also disclosed that the composition may exist as a resin pellet with the polyamide dispersed into the polyester or as a compartmentalized pellet comprising a first compartmentalized zone and a second compartmentalized zone, wherein the first compartmentalized zone is comprised of the polyester and the second compartmentalized zone is comprised of the polyamide. [0012] A process for solid phase polymerizing a polyester and a polyamide at the same temperature for the same amount of time is also disclosed, wherein said process comprises the steps of A) Selecting a polyester from the group consisting of crystallizable polyesters that have at least 85% of the crystallizable polyester acid moieties derived from the group consisting of terephthalic acid, 2,6 naphthalene dicarboxylic acid and their diesters and a polyamide comprising a residue selected from the group consisting of the repeating unit of amino caproic acid and the repeating unit of A-D, wherein A is the residue of a dicarboxylic acid comprising adipic acid, isophthalic acid, terephthalic acid, 1,4-cyclohexanedicarboxylic acid, or naphthalenedicarboxylic acid, or a mixture thereof, and D is a residue of a diamine comprising m-xylylene diamine, p-xylylene diamine, hexamethylene diamine, ethylene diamine, or 1,4 cyclohexanedimethylamine, or a mixture thereof, wherein the polyamide has a triamine content after hydrolysis of less than 0.22 and a carboxyl content outside the range of 20 to 80 percent of the total number of end groups; B) Combining the polyester and polyamide into resin pellets so that the resin pellets comprise both the polyester and polyamide; C) Heating the resin pellets to a temperature in the range of 40.degree. C. to 1.degree. C. below which the pellets become liquid; and D) Maintaining the resin pellets in the temperature range for sufficient time to increase the intrinsic viscosity of the polyester by at least 0.05 dl/g. [0013] It is further disclosed that that at least 90% of the crystallizable polyester's acid moieties can be derived from terephthalic acid and 90% of the crystallizable polyester's glycol moieties can be derived from ethylene glycol. Again, the preferred polyamide for the process is MXD6 nylon. [0014] It is also disclosed that the polyamide and polyester may be combined into the pellets so that the polyamide is dispersed into the polyester or combined into compartmentalized pellets comprising a first compartmentalized zone and a second compartmentalized zone, wherein the first compartmentalized zone is comprised of the polyester and the second compartmentalized zone is comprised of the polyamide. It is further disclosed to heat the pellets to a temperature in the range of 165.degree. C. and 235.degree. C. wherein at least 90% of the crystallizable polyester's acid moieties are derived from terephthalic acid and at least 90% of crystallizable polyester's glycol moieties are derived from ethylene glycol. Also disclosed is that the crystallizable polyester comprises lithium sulfoisophthalate. BRIEF DESCRIPTION OF THE DRAWINGS [0015] FIG. 1 depicts a resin pellet with two compartments or zones in the core-sheath configuration. [0016] FIG. 2 depicts a resin pellet with two compartments or zones in the core-sheath configuration where the core is encapsulated, surrounded, or enclosed by an outer sheath layer. [0017] FIG. 3 depicts a resin pellet with three compartments or zones in a multi-layered or sandwich configuration. [0018] FIG. 4 depicts a resin pellet of three compartmentalized zones configured in two concentric layers surrounding a core. 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