Continuous process for producing poly(trimethylene terephthalate) containing low levels of by-products

Patent metadata

Field	Value
Publication number	US-10280257-B2
Application number	US-201515519614-A
Country	US
Kind code	B2
Filing date	Oct 5, 2015
Priority date	Oct 22, 2014
Publication date	May 7, 2019
Grant date	May 7, 2019

Abstract

The present invention relates to a continuous process for producing poly(trimethylene terephthalate). According to the process of the present invention, it is possible to continuously produce poly(trimethylene terephthalate) containing low levels of toxic by-products such as acrolein and ally alcohol without additional additives.

First claim

What is claimed is:

1. A continuous process for producing poly(trimethylene terephthalate), comprising the steps of:
forming a first esterification product by providing a raw material mixture including 1,3-propanediol and terephthalic acid or dimethyl terephthalate to a first esterification reactor, and then pressurizing and heating under a non-catalytic condition;
forming a second esterification product by providing the first esterification product to a second esterification reactor and heating under non-catalytic and normal pressure conditions;
forming a prepolymer of poly(trimethylene terephthalate) by providing the second esterification product to a first polymerization reactor and carrying out polycondensation; and
forming a high molecular weight poly(trimethylene terephthalate) by providing the prepolymer together with a catalyst to a second polymerization reactor and carrying out polycondensation.

2. The continuous process for producing poly(trimethylene terephthalate) according to claim 1 , wherein the raw material mixture contains 1.0 to 1.5 mol of 1,3-propanediol with respect to 1 mol of terephthalic acid or dimethyl terephthalate.

3. The continuous process for producing poly(trimethylene terephthalate) according to claim 1 , wherein the formation of the first esterification product is carried out under a pressure of 1 to 4 kgf/cm 2 and a temperature of 230 to 250° C.

4. The continuous process for producing poly(trimethylene terephthalate) according to claim 1 , wherein the formation of the second esterification product is carried out under normal pressure and a temperature of 240 to 260° C.

5. The continuous process for producing poly(trimethylene terephthalate) according to claim 1 , wherein the first and second esterification products each includes bis(3-hydroxypropyl)terephthalate, low molecular weight polyesters of 1,3-propanediol and terephthalic acid or dimethyl terephthalate, or a mixture thereof.

6. The continuous process for producing poly(trimethylene terephthalate) according to claim 1 , wherein the first polymerization reactor is maintained at a temperature of 230 to 270° C. and a pressure of 100 to 300 mmHg.

7. The continuous process for producing poly(trimethylene terephthalate) according to claim 1 , wherein the second polymerization reactor is maintained at a temperature of 230 to 270° C. and a pressure of 10 to 200 mmHg.

8. The continuous process for producing poly(trimethylene terephthalate) according to claim 1 , wherein the polycondensation reaction is further carried out by providing a stream discharged from the second polymerization reactor to the third polymerization reactor.

9. The continuous process for producing poly(trimethylene terephthalate) according to claim 1 , wherein the catalyst provided to the second polymerization reactor is an organic or inorganic compound including one or more active metals selected from the group consisting of titanium and tin.

10. The continuous process for producing poly(trimethylene terephthalate) according to claim 1 , wherein the catalyst provided to the second polymerization reactor is one or more compounds selected from the group consisting of tetraisopropyl titanate, tetrabutyl titanate, and dibutyltin oxide.

11. The continuous process for producing poly(trimethylene terephthalate) according to claim 1 , wherein the catalyst provided to the second polymerization reactor is added so that 20 to 250 ppm of the active metals are included based on the weight of the final polymer.

12. The continuous process for producing poly(trimethylene terephthalate) according to claim 1 , wherein the high molecular weight poly(trimethylene terephthalate) has an intrinsic viscosity of 0.8 to 1.2 dl/g or a weight average molecular weight of 70,000 to 130,000.

Assignees

• Sk Chemicals Co Ltd

Inventors

• Moon Jung-Me
• Kim Tae-Young

Classifications

• C08G63/85 Primary

  Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof {(C08G63/823 takes precedence)} · CPC title

• C08G63/183 Primary

  Terephthalic acids · CPC title

• C08G63/82

  characterised by the catalyst used · CPC title

• C08G63/78

  Preparation processes · CPC title

• C08G65/34 Primary

  from hydroxy compounds or their metallic derivatives {(C08G65/26 takes precedence)} · CPC title