IPC분류정보
| 국가/구분 |
United States(US) Patent
등록
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| 국제특허분류(IPC7판) |
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| 출원번호 |
US-0468687
(2012-05-10)
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| 등록번호 |
US-8748559
(2014-06-10)
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발명자
/ 주소 |
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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 :
34 |
초록
▼
Polyester compositions, especially polyethylene terephthalate homopolymer and copolymers, are disclosed containing titanium catalysts and catalyst deactivator added late in the manufacturing processing having reduced acetaldehyde generation rates. The polyester compositions are low in free acetaldeh
Polyester compositions, especially polyethylene terephthalate homopolymer and copolymers, are disclosed containing titanium catalysts and catalyst deactivator added late in the manufacturing processing having reduced acetaldehyde generation rates. The polyester compositions are low in free acetaldehyde, making them suitable for fabrication into beverage containers for relatively tasteless beverages such as bottle water. Furthermore, the polyesters are polymerized to a high inherent viscosity in reduced processing time, without the necessity of further polymerization in the solid state, and in the absence of acetaldehyde scavengers leading to polyester polymers having reduced color.
대표청구항
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1. A method for the production of solid polyester polymer particles comprising: a) polycondensing a molten polyester polymer composition in the presence of a polycondensation catalyst composition comprising titanium species;b) adding a catalyst deactivator compound to the molten polyester polymer co
1. A method for the production of solid polyester polymer particles comprising: a) polycondensing a molten polyester polymer composition in the presence of a polycondensation catalyst composition comprising titanium species;b) adding a catalyst deactivator compound to the molten polyester polymer composition;c) after reaching an It.V. of about 0.69 dL/g or more, solidifying the molten polyester polymer composition into solid polyester polymer particles which do not contain added acetaldehyde scavengers; andd) reducing the amount of residual acetaldehyde in the solid particles to a level of about 10 ppm or less in the solid state without increasing the It.V. of the particles by more than about 0.03 dL/g in the solid state;wherein the catalyst deactivator compound is added to the molten polyester polymer composition in step b) at one or more of the following points: (i) within a final reactor for polycondensing the molten polyester polymer or between said final reactor and before a cutter for cutting the molten polyester polymer composition into said solid particles; or(ii) after the It.V. of the molten polyester polymer composition has risen to at least 0.5 dL/g; or(iii) vacuum applied to the molten polyester polymer melt, if any, is at least partially released; or(iv) following at least 75% of the polycondensation time; or(v) within +/−0.10 dL/g, of the It.V. obtained upon solidification; or(vi) within 30 minutes before solidifying the melt. 2. The method of claim 1, wherein said molten polyester polymer composition comprises: (a) a dicarboxylic acid component comprising at least about 60 mole % residue of terephthalic acid or of a diester derivate of terephthalic acid and(b) a diol component comprising at least about 60 mole % of residues of ethylene glycol,based on 100 mole percent of dicarboxylic acid component residues and 100 mole percent of diol component residues in the molten polyester polymer composition. 3. The method of claim 1, wherein the molten polyester polymer composition comprises: (a) a carboxylic acid component comprising at least 80 mole % residues of terephthalic acid or of a diester derivative of terephthalic acid, and(b) a hydroxyl component comprising at least 80 mole % of the residues of ethylene glycol,based on 100 mole percent of carboxylic acid component residues and 100 mole percent of hydroxyl component residues in the molten polyester polymer composition. 4. The method of claim 2, wherein the molten polyester polymer composition comprises: (a) a dicarboxylic acid component comprising at least 92 mole % residues of terephthalic acid or of a diester derivative of terephthalic acid, and(b) a diol component comprising at least 92 mole % of the residues of ethylene glycol,based on 100 mole percent of carboxylic acid component residues and 100 mole percent of hydroxyl component residues in the molten polyester polymer composition. 5. The method of claim 1, wherein the amount of titanium in the molten polyester polymer composition is present in an amount of from about 3 ppm to about 35 ppm based to the weight of the molten polyester polymer composition. 6. The method of claim 1, wherein the amount of titanium in the polyester polymer particles is present in an amount of from 4 ppm to 20 ppm based to the weight of the molten polyester polymer composition. 7. The method of claim 1, wherein the amount of titanium in the polyester polymer particles is present in an amount of from 5 ppm to 15 ppm based to the weight of the molten polyester polymer composition. 8. The method of claim 1, wherein the titanium catalyst comprises a titanium alkoxide. 9. The method of claim 1, wherein the polycondensation is continued to an It.V. of at least 0.76 dL/g. 10. The method of claim 1 wherein the catalyst deactivator comprises phosphoric acid; phosphorous acid; pyrophosphoric acid; polyphosphoric acid; carboxyphosphonic acids, phosphonic acid derivatives, or each of their salts and esters and derivatives. 11. The method of claim 1, wherein the catalyst deactivator comprises phosphoric acid. 12. The method of claim 1, wherein the catalyst deactivator comprises a phosphorus compound present in a P:Ti mole ratio of at least 1:1. 13. The method of claim 1, wherein the catalyst deactivator compound is added to the molten polyester polymer after the polyester melt obtains an It.V. of at least about 0.74 dL/g. 14. The method of claim 1, wherein the catalyst deactivator compound is added to the molten polyester polymer after bringing the pressure in a final reactor to a level of about 600 mm Hg or greater and before the polyester melt is solidified. 15. The method of claim 1, wherein the catalyst deactivator compound is added to the molten polyester polymer following at least about 95% of the polycondensation time. 16. The method of claim 1, wherein the catalyst deactivator compound is added to the molten polyester polymer when the It.V. of the polyester melt is within about 0.05 dL/g of the polymer It.V. upon solidification. 17. The method of claim 1, wherein the catalyst deactivator compound is added to a final reactor for polycondensing the molten polyester polymer through a pipe inlet, said phosphorus compound contained within a portion of the molten polyester polymer exiting the final reactor and recirculated back to the final reactor. 18. The method of claim 1, wherein the solid particles have an acetaldehyde generation rate of 10 ppm or less. 19. The method of claim 1, wherein an organic colorant is added to the molten polyester polymer to produce the solid polyester polymer particles, which are molded into preforms having a L* color of at least 70 and a b* color no greater than 3. 20. The method of claim 1, wherein the solid polyester polymer particles produced by the process have an acetaldehyde generation rate of 20 ppm or less. 21. The method of claim 1, wherein the catalyst deactivator is a phosphorous compound and the reducing (d) forms solid polyester polymer particles comprising from 12 to 18 ppm phosphorus.
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