Process for producing polyester resin
View Patent ↗A polyester resin prepared by polycondensing a dicarboxylic acid component containing terephthalic acid or derivative thereof with a diol component containing ethylene glycol through esterification or transesterification, thereby producing a melt polymerization polymer and subjecting the melt polymerization polymer to solid-phase polycondensation, wherein (1) the melt polymerization polymer contains comonomer units other than terephthalic acid units and ethylene glycol units in an amount of 5.5 or less, and whose intrinsic viscosity ranges from 0.08 dL/g to 0.50 dL/g and which has an apparent crystallite size smaller than 9 nm, and wherein (2) the melt polymerization polymer is subjected to solid-phase polycondensation at a temperature which is higher by at least 140° C. than the glass transition temperature of the melt polymerization polymer and is not higher than the melting point of the polymer to thereby obtain a polyester resin having an apparent crystallite size smaller than 9 nm.
1. A process for producing a polyester resin, which comprises:
polycondensing a dicarboxylic acid component containing terephthalic acid or an ester-forming derivative thereof as the main component and a diol component containing ethylene glycol as the main component, wherein the reacting components contain comonomers other than terephthalic acid and ethylene glycol in total amount of 5.5 mol % or less, by esterification or transesterification;
melt polymerizing the polycondensed material obtained, thereby obtaining a polymerized product having an intrinsic viscosity ranging from 0.08 dL/g to 0.50 dL/g and an apparent crystallite size smaller than 9 nm; and
solid-phase polycondensing the melt polymerized product obtained at a temperature which is higher by at least 140° C. than the glass transition temperature of the melt polymerization polymer and is not higher than the melting point of the polymer to thereby obtain a polyester resin having an apparent crystallite size smaller than 9 nm and having an intrinsic viscosity of 0.60 dL/g or higher.
2. The process for producing a polyester resin according to claim 1 , wherein the solid-phase polycondensation reaction is conducted at a temperature which is higher by at least 145° C. than the glass transition temperature of the melt polymerization polymer and is not higher than the melting point of the polymer.
3. The process for producing a polyester resin according to claim 2 , wherein the solid-phase polycondensation reaction is conducted at a temperature which is higher by at least 150° C. than the glass transition temperature of the melt polymerization polymer and is not higher than the melting point of the polymer.
4. The process for producing a polyester resin according to claim 1 , wherein the melt polymerization polymer has an apparent crystallite size of 8 nm or smaller and the polyester resin has an apparent crystallite size of 8 nm or smaller.
5. The process for producing a polyester resin according to claim 1 , wherein the melt polymerization polymer has an intrinsic viscosity ranging from 0.10 dL/g to 0.45 dL/g.
6. The process for producing a polyester resin according to claim 1 , wherein the amount of comonomer units other than terephthalic acid units and ethylene glycol units is 4.5 or less.
7. The process for producing a polyester resin according to claim 1 , wherein the melt polymerization polymer has an average particle diameter ranging from 10 to 1,500 μm.
8. The process for producing a polyester resin according to claim 1 , wherein the polyester resin has an average particle diameter ranging from 10 to 1,500μm.
9. The process for producing a polyester resin according to claim 1 , wherein the melt polymerization polymer is heated to the solid-phase polycondensation temperature at a rate of 100° C./min or less in heating the polymer to 200° C.
10. The process for producing a polyester resin according to claim 1 , wherein the proportion of the diol component to the dicarboxylic acid component (molar ratio) ranges from 1 to 2 times.
11. The process for producing a polyester resin according to claim 1 , wherein melt polymerization is conducted at a temperature of 250 to 290° C.
12. The process for producing a polyester resin according to claim 1 , wherein melt polymerization is conducted at a pressure ranging from 1,333 to 13.3 Pa.
13. The process for producing a polyester resin according to claim 1 , wherein the solid-phase polycondensation is conducted at a pressure ranging from 100 to 150 kPa.
14. The process for producing a polyester resin according to claim 1 , wherein the polycondensation is conducted in the presence of a titanium compound as a catalyst.