Preparation method of polybutylene terephthalate/adipate butanediol copolyester

A technology of polybutylene terephthalate and butylene diacid copolyester, which is applied in the field of polyester synthesis, can solve problems such as adverse effects on product quality, and achieve shortened synthesis reaction time, improved reaction speed, and high performance characteristics. The effect of viscosity

Active Publication Date: 2012-03-07
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This is mainly because the direct esterification process is generally carried out under high pressure and high temperature conditions, which makes part of 1,4-BD easy to dehydrate and cyclize to generate tetrahydrofuran (THF) by-products, which adversely affects product quality.

Method used

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  • Preparation method of polybutylene terephthalate/adipate butanediol copolyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Into a 5 L stainless steel reaction kettle equipped with nitrogen inlet, condensate outlet and stirrer, 820 g of terephthalic acid (PTA), 180 g of adipic acid (AA) and 383 g of 1,4-butanediol (1,4-BD ), 0.2g tetrabutyl titanate (equivalent to 200ppm of the total weight of PTA and AA), 0.6g antimony acetate (equivalent to 600ppm of the total weight of PTA and AA). Maintain normal pressure in the kettle and stir at a constant speed. When the temperature in the reaction kettle rises to 150°C, water will start to come out. Continue to raise the temperature and control the inner temperature of the reaction kettle to not exceed 220°C. When the amount of water is produced, the esterification reaction ends. Continue to add 0.05g trimethyl phosphate (50ppm equivalent to the total weight of PTA and AA) in the kettle, vacuumize, make the pressure in the polymerization kettle be reduced to below 150Pa in 60 minutes, react under this pressure for 85 minutes, react The final tempera...

Embodiment 2

[0033]Into a 5 L stainless steel reaction kettle equipped with nitrogen inlet, condensate outlet and stirrer, 630 g of terephthalic acid (PTA), 370 g of adipic acid (AA) and 686 g of 1,4-butanediol (1,4-BD ), 0.2g tetrapropyl titanate (equivalent to 200ppm of the total weight of PTA and AA) and 0.3g antimony trioxide (equivalent to 300ppm of the total weight of PTA and AA). Maintain normal pressure in the kettle and stir at a constant speed. When the temperature in the reaction kettle rises to 150°C, water will start to come out. Continue to raise the temperature and control the inner temperature of the reaction kettle to not exceed 220°C. When the amount of water is produced, the esterification reaction ends. Continue to add 0.3g tetrapropyl titanate (equivalent to 300ppm of the total weight of PTA and AA), 0.1g antimony trioxide (equivalent to 100ppm of the total weight of PTA and AA) and 0.15g trimethyl phosphate (equivalent to 100ppm of the total weight of PTA and AA) in t...

Embodiment 3

[0035] Into a 5 L stainless steel reaction kettle equipped with nitrogen inlet, condensate outlet and stirrer, 532 g of terephthalic acid (PTA), 468 g of adipic acid (AA) and 806 g of 1,4-butanediol (1,4-BD ), 0.3g tetramethyl titanate (equivalent to 300ppm of the total weight of PTA and AA) and 0.3g antimony ethylene glycol (equivalent to 300ppm of the total weight of PTA and AA). Maintain normal pressure in the kettle and stir at a constant speed. When the temperature in the reaction kettle rises to 150°C, water will start to come out. Continue to raise the temperature and control the inner temperature of the reaction kettle to not exceed 220°C. When the amount of water is produced, the esterification reaction ends. Continue to add 0.5g tetramethyl titanate (equivalent to 500ppm of the total weight of PTA and AA) and 0.2g triphenyl phosphate (equivalent to 200ppm of the total weight of PTA and AA) in the kettle, and vacuumize to make the polymerization kettle The pressure i...

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Abstract

The invention relates to a preparation method of polybutylene terephthalate / adipate butanediol copolyester, which utilizes a titanium compound and an antimony compound as the composite catalyst, the mole ratio of terephthalic acid to adipate is 3:7-8:2, the ratio of the total mole of the terephthalic acid and the adipate to the mole of 1,4-butanediol is 1:1.0-1.8, esterification is carried out atnormal pressure and the temperature of 150-220 DEG C, the pressure is reduced to high vacuum 10-150 Pa for the reaction, the final temperature for the reaction is 265-280 DEG C, and inert gas is utilized to recover the pressure to be normal to obtain the copolyester. The reaction time is shortened, the production amount of tetrahydrofuran is small, the intrinsic viscosity of copolyester chips is 0.90-1.32 dL / g, the hue b value of the product is between 0 and 8, the L value is between 68 and 85, and the product of the polybutylene terephthalate / adipate butanediol copolyester can be used in thefields of various soft package plastic products.

Description

Technical field: [0001] The present invention relates to the synthesis of polyester, in particular to the production of aromatic dicarboxylic acids, aliphatic dicarboxylic acids and aliphatic dihydric alcohols through direct esterification and co-condensation reactions to prepare aliphatic-aromatic copolyesters . Background technique: [0002] Polyester prepared by condensation polymerization has been widely used in various fields of people's daily life as an engineering material. They can be made into fibers, beverage bottles, films and other materials. These polymers are prepared through two processes: esterification or transesterification of terephthalic acid / aliphatic esters or their esterification products with aliphatic diols, usually under high pressure conditions, transesterification The process is carried out under normal pressure; vacuum polycondensation of esterification or transesterification products. [0003] Polybutylene terephthalate / butylene adipate copoly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/85C08G63/86C08G63/183C08G63/87
Inventor 陈颖王晓慧史君朱景利付志峰李连斌邹妍石艳温国防王子镐黄一平段微微
Owner PETROCHINA CO LTD
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