PTT preparation method

A dibasic acid and dibasic alcohol technology, applied in the field of polyester, can solve the problems of low activity compounds, deposition, blocked pipes, etc., and achieve the effect of overcoming easy hydrolysis and high catalyst efficiency

Inactive Publication Date: 2016-11-16
SINOPEC YIZHENG CHEM FIBER +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, titanate compounds such as tetrabutyl titanate, isopropyl titanate, etc. have a serious defect, they are easily hydrolyzed to generate compounds with low activity, and the hydrolyzed products block the pipeline and easily deposit on the surface of the heat exchanger of the reactor ,affect production
During the esterification reaction process of PTT preparation, the esterification reaction of terephthalic acid and propylene glycol generates water, and the water generated by the esterification reaction unavoidably causes the side reaction of hydrolyzing the catalyst, which affects the long-term stable operation of the PTT production device.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 360 grams of propylene glycol, 325 grams of terephthalic acid, and 0.4 grams of titanium lactate aqueous solution (Ti content 3.2%) into a 2L reaction kettle, heat up, and control the esterification reaction temperature at 220°C to 250°C, and the gauge pressure is about 0.25MPa. The esterification water is discharged for about 2 hours. After the esterification water reaches the theoretical amount, the esterification is completed, and the temperature is gradually raised and transferred to the low vacuum stage. After the low vacuum time is about 45 minutes, it enters the high vacuum polycondensation stage (vacuum <100Pa), and the polycondensation temperature is 245 ° C ~ 265 ℃, after high vacuum polycondensation for about 98 minutes, when the stirring power reaches the rated value, the material is discharged. The intrinsic viscosity of the synthesized PTT is 0.921dL / g, the terminal carboxyl group is 22mol / t, and the color value (L / a / b) is 87.3 / -1.1 / 3.2.

Embodiment 2

[0021] Add 360 grams of propylene glycol, 325 grams of terephthalic acid, 0.01 grams of cobalt acetate, and 0.6 grams of titanium lactate aqueous solution (Ti content 2.0%) into a 2L reaction kettle, heat up, and control the esterification reaction temperature at 220°C to 250°C. About 0.25MPa, when the esterification effluent is about 2 hours, after the esterification effluent reaches the theoretical amount, the temperature is gradually raised and transferred to the low vacuum stage. After the low vacuum time is about 45min, it enters the high vacuum polycondensation stage (vacuum<100Pa), and the polycondensation temperature is 246°C ~260°C, after high vacuum polycondensation for about 108min, when the stirring power reaches the rated value, the material is discharged. The synthesized PTT has an intrinsic viscosity of 0.925dL / g, a terminal carboxyl group of 26mol / t, and a color value (L / a / b) of 85.4 / -1.1 / 1.3.

Embodiment 3

[0023] Add 360 grams of propylene glycol, 325 grams of terephthalic acid, 0.70 grams of titanium lactate aqueous solution (Ti content 1.8%), 1.2 grams of matting agent titanium dioxide into a 2L reactor, heat up, and the esterification reaction temperature is controlled at 225 ° C ~ 250 ° C, the table The pressure is about 0.25MPa. When the esterification water is discharged for about 2 hours, the esterification is completed after the esterification water reaches the theoretical amount, and the temperature is gradually raised and transferred to the low vacuum stage. After the low vacuum time is about 45min, it enters the high vacuum polycondensation stage (vacuum<100Pa). The polycondensation temperature is 245℃~265℃, after high vacuum polycondensation for about 115min, when the stirring power reaches the rated value, the material is discharged. The intrinsic viscosity of the synthesized PTT is 0.930dL / g, the terminal carboxyl group is 32mol / t, and the color value (L / a / b) is 84.6...

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Abstract

The invention discloses a PTT preparation method. The method comprises the step that dicarboxylic acid, dihydric alcohol and a catalyst lactic acid titanium are used for preparing polyester PTT through a direct esterification method, wherein dicarboxylic acid is terephthalic acid or comprises one or more of isophthalic acid or naphthalic acid or adipic acid, and dihydric alcohol is propanediol or comprises ethylene glycol or butanediol or 2-methyl-1,3-propylene glycol or 2,2-dimethyl-1,3-propanediol. PTT is prepared from terephthalic acid, propanediol and the lactic acid titanium catalyst through the direct esterification method; compared with PTT prepared from a traditional titanate catalyst, conventional performance indexes such as a terminal carboxyl group, intrinsic viscosity and hue of prepared PTT are equivalent to those of PTT synthesized by means of the traditional titanate catalyst, the lactic acid titanium catalyst overcomes the defect that the titanate catalyst is prone to hydrolysis, and the efficiency of the catalyst is higher.

Description

technical field [0001] The invention belongs to the field of polyester, and in particular relates to a preparation method of novel polyester PTT. Background technique [0002] Polytrimethylene terephthalate (PTT) is a new type of semi-crystalline thermoplastic polyester. Compared with polyethylene terephthalate (PET) and butylene terephthalate (PBT), it has It has a unique spiral structure and good elasticity. PTT has the softness of nylon, the bulkiness of acrylic fiber and the stain resistance of polyester. In short, PTT integrates the advantages of various synthetic fibers. Due to the excellent performance of PTT, it is widely used in clothing, industry, decoration and engineering plastics, especially in the carpet field as a strong competitor of PA, and about 55% of PTT fibers are used in carpets. [0003] Catalysts prepared by PTT mainly include antimony series, tin series, rare earth and titanium series, etc. Among them, although antimony series catalysts are cheap, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/85C08G63/183C08G63/181C08G63/189C08G63/16
CPCC08G63/85C08G63/16C08G63/181C08G63/183C08G63/189
Inventor 戴志彬夏峰伟王金堂王余伟朱兴松何胜君
Owner SINOPEC YIZHENG CHEM FIBER
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