IPC분류정보
국가/구분 |
United States(US) Patent
등록
|
국제특허분류(IPC7판) |
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출원번호 |
US-0149248
(2011-05-31)
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등록번호 |
US-8791187
(2014-07-29)
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발명자
/ 주소 |
- Quillen, Donna Rice
- Armentrout, Rodney Scott
- Jernigan, Mary Therese
- Stafford, Steven Lee
- Xia, Zhiyong
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출원인 / 주소 |
- Grupo Petrotemex, S.A. de C.V.
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대리인 / 주소 |
Oblon, Spivak, McClelland, Maier & Neustadt, L.L.P.
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인용정보 |
피인용 횟수 :
0 인용 특허 :
186 |
초록
▼
A polyester composition containing: a) aluminum atoms; andb) alkaline earth atoms or alkali metal atoms or alkali compound residues such as lithium atoms; andc) particles comprising titanium, zirconium, vanadium, niobium, hafnium, tantalum, chromium, tungsten, molybdenum, iron, or nickel atoms or co
A polyester composition containing: a) aluminum atoms; andb) alkaline earth atoms or alkali metal atoms or alkali compound residues such as lithium atoms; andc) particles comprising titanium, zirconium, vanadium, niobium, hafnium, tantalum, chromium, tungsten, molybdenum, iron, or nickel atoms or combinations thereof, where the particles improve the reheat rate of the polyester composition. The polyester polymer compositions may also contain phosphorus catalyst deactivators/stabilizers. The polyester compositions and the articles made from the compositions such as bottle preforms and stretch blow molded bottles have improved reheat rate while maintaining low haze, high L*, a b* below 3, and have low levels of acetaldehyde. In the process for making the polyester polymer, the polymer melt is polycondensed in the presence of a) and b), with the particles c) added in a melt phase process or added to the polymer in an injection molding machine or extruder. The polyester polymer composition can be made to high IV from the melt phase while avoiding solid state polymerization.
대표청구항
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1. A process for the manufacture of a polyester polymer, comprising: polyesterifying a monomer mixture comprising at least one diol and at least one alkylene terephthalate to form a polyesterified melt;polycondensing the polyesterified melt in the absence of titanium catalysts and in the presence of
1. A process for the manufacture of a polyester polymer, comprising: polyesterifying a monomer mixture comprising at least one diol and at least one alkylene terephthalate to form a polyesterified melt;polycondensing the polyesterified melt in the absence of titanium catalysts and in the presence of aluminum atoms and at least one of an alkaline earth metal atom, an alkaline earth metal compound, an alkali metal atom, and an alkali metal compound, to form the polyester polymer; andbefore, during, or after the polycondensing, adding particles to the polyesterified melt, the polyester polymer or its reaction precursors, to obtain a composition,wherein the particles comprise titanium, zirconium, vanadium, niobium, hafnium, tantalum, chromium, tungsten, molybdenum, iron, or nickel atoms or combinations thereof, and adding phosphorous atoms to the polyesterified melt after satisfaction of at least one condition selected from the group consisting of:a) the polyester melt reaches an It.V. of at least 0.50 dL/g;b) releasing vacuum during polycondensation if vacuum is applied;c) at a location near or at an end of a final reactor or between the final reactor and before a cutter;d) following at least 75% of a polycondensation time;e) the It.V. of the polyester melt is within 0.03 dl/g of the final It.V. exiting a melt phase process; andf) at a point within 10 minutes of less of solidifying the polyester melt. 2. The process of claim 1, wherein the median size of the particles ranges from about 1 nm to about 500 nm. 3. The process of claim 1, wherein the It.V. of the polyester polymer obtained from the polycondensing is at least 0.72 dL/g. 4. The process of claim 1, wherein aluminum is added during or before the polycondensing and before the It.V. of the polyester polymer or the polyesterified melt has reached 0.3 dL/g. 5. The process of claim 1, wherein the particles are added to the polyesterified melt after the It.V. of the polyesterified melt has reached 0.45 dL/g. 6. The process of claim 1, wherein the particles are added to a melt phase process at a point proximate to an outlet of a final polycondensation reactor and any point thereafter up to a die for solidifying the polyester melt, or at any point after solidification of the polyester polymer made in the melt phase process. 7. The process of claim 1, wherein the aluminum atoms are added to a melt phase process as a separate stream from a stream comprising alkaline earth metal or alkali metal or alkali compounds. 8. The process of claim 1, wherein aluminum is added to a melt phase process as a liquid solution or dispersion, wherein the aluminum atoms are obtained from an aluminum compound comprising at least one carboxylic acid salt of aluminum, aluminum alcoholate, aluminum hydroxide, aluminum halide, or aluminum hydroxyhalide. 9. The process of claim 1, wherein the alkali and alkaline earth metals comprise atoms of lithium added as a liquid stream to a melt phase process, wherein the lithium is obtained from at least one lithium salt or complex having a counterion of at least one hydroxide, amine, amine derivative, carbonate, or halide. 10. The process of claim 1, wherein the polycondensing is carried out in the absence of added antimony-comprising catalysts. 11. The process of claim 1, wherein the polycondensing is carried out in the absence of cobalt-comprising catalysts, and antimony-comprising catalysts to increase the It.V. of the polyester polymer in a melt phase by more than 0.1 dL/g. 12. The process of claim 1, wherein the polycondensing is carried out without adding any metal-comprising catalyst during the polycondensing other than at least one aluminum-comprising catalyst and at least one alkaline earth or alkali catalyst. 13. The process of claim 1, further comprising adding a catalyst deactivator/stabilizer. 14. The process of claim 1, wherein the phosphorus atoms are obtained from compounds comprising at least one selected from the group consisting of phosphoric acid, phosphorous acid, polyphosphoric acid, a carboxyphosphonic acid, a phosphonic acid derivative, an acidic salt thereof, an acidic ester thereof, and a derivative thereof. 15. The process of claim 1, wherein an amount of phosphorus atoms ranges from 75 ppm up to 300 ppm. 16. The process of claim 1, wherein a molar ratio of phosphorus to a cumulative total of alkaline earth metal, alkali metal, and alkali compounds is at least 0.3:1 to 5:1. 17. The process of claim 1, wherein the polyester polymer is made in a continuous manufacturing process where a throughput of a melt phase process is at least 50 tons/day. 18. The process of claim 1, wherein a reaction time of the polyesterified melt from an It.V. of 0.40 dL/g through and up to a final It.V. obtained in a melt phase process is 80 minutes or less. 19. The process of claim 1, wherein the composition comprises phosphorus atoms, and the polyester polymer has an It.V. of at least 0.72 dL/g obtained in a melt phase process. 20. The process of claim 1, wherein the polyester polymer has an L* of at least 73. 21. The process of claim 1, wherein an organic acetaldehyde scavenger is not added to a melt phase process for making the polyester polymer. 22. The process of claim 1, wherein the particles comprise atoms of tungsten or molybdenum. 23. The process of claim 1, wherein the polyester polymer has an acetaldehyde generation rate, when measured at 295° C. for 5 minutes, of 11 ppm or less. 24. The process of claim 1, wherein the polycondensing is carried out in the presence of catalyst consisting of aluminum atoms and at least one of an alkaline earth metal atom and an alkali metal atom. 25. The process of claim 1, wherein the polycondensing is carried out in the presence of catalyst metals consisting of aluminum atoms lithium atoms. 26. The process of claim 1, wherein the particles are added to the polyesterified melt before the polycondensing. 27. The process of claim 1, wherein the particles are added to the polyester polymer during the polycondensing. 28. The process of claim 1, wherein the particles are added to the polyesterified melt after the polycondensing. 29. The process of claim 1, wherein the polyester polymer comprises repeating units of alkylene terephthalate or alkylene naphthalate. 30. The process of claim 29, wherein the polyester polymer comprises repeating units of ethylene terephthalate. 31. The process of claim 1, wherein the polycondensing comprises polycondensing the polyesterified melt in the presence of aluminum atoms and lithium atoms. 32. The process of claim 31, wherein the particles comprise titanium atoms. 33. The process of claim 1, wherein the particles comprise titanium nitride, titanium carbide, titanium boride, or combinations thereof, the alkaline earth metal or alkali metal or alkali compounds comprise lithium, and wherein the composition further comprises phosphorus atoms. 34. The process of claim 33, wherein an amount of particles present ranges from 1 ppm to about 50 ppm and have a median particle size ranging from 0.001 μm to 5 μm, the aluminum atoms are present in an amount ranging from 4 ppm to about 100 ppm, and an amount of phosphorus atoms ranges from 30 ppm to 400 ppm. 35. The process of claim 1, wherein the polyester polymer is esterified in the presence of lithium atoms. 36. The process of claim 35, wherein the lithium atoms are added to a diol feed to an esterification reactor. 37. The process of claim 1, wherein the composition comprises 10 to 50 ppm lithium,10 to 50 ppm aluminum,a plurality of reheat particles of a size ranging from 15 to 60 nm in amount of about 2 to 30 ppm,based on polymer weight. 38. The process of claim 37, wherein an amount of phosphorus atoms ranges from 75 to 170 ppm, based on weight of final polymer. 39. The process of claim 37, wherein the phosphorus atoms are added at completion of the polycondensing or thereafter. 40. The process of claim 1, wherein phosphorus atoms are added to the polyesterified melt after the polyesterified melt obtains an It.V. of at least 0.72 dL/g. 41. The process of claim 40, wherein phosphorus atoms are added to the polyesterified melt immediately before or after bringing a pressure within a final polycondensation reactor to a level of 0.01 mmHg or greater. 42. The process of claim 40, wherein phosphorus atoms are added at a location near or at an end of a final polycondensation reactor or between a final polycondensation reactor and before a cutter. 43. The process of claim 40, wherein phosphorus atoms are added to the polyesterified melt following at least 90% of a polycondensation time. 44. The process of claim 40, wherein phosphorus atoms are added to the polyesterified melt when the It.V. of the polyesterified melt is within 0.015 dl/g of the final It.V. exiting a melt phase process. 45. The process of claim 40, wherein phosphorus atoms are added to the polyester polymer at a point within 5 minutes or less of solidifying the polyester polymer.
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