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Preparation method of polybutylene terephthalate/adipate butanediol copolyester

A technology of polybutylene terephthalate and butylene diacid copolyester, applied in the field of polyester synthesis, can solve problems such as adverse effects on product quality, and achieve shortened synthesis reaction time, high intrinsic viscosity and catalytic activity high effect

Active Publication Date: 2010-10-20
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] Add 820g terephthalic acid (PTA), 180g adipic acid (AA) and 383g 1,4-butanediol (1,4-BD) into a 5L stainless steel reactor equipped with nitrogen inlet, condensate outlet and stirrer. ), 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). Keep the pressure in the kettle and stir at a constant speed. When the temperature in the reactor rises to 150℃, the water will be removed. Continue to increase the temperature and control the temperature in the reactor to not higher than 220℃. Wait until the amount of by-product water distilled from the reactor reaches the theoretical level. When the water output is reached, the esterification reaction ends. Continue to add 0.05g of trimethyl phosphate (equivalent to 50ppm of the total weight of PTA and AA) into the kettle, vacuum, reduce the pressure in the polymerization kettle to below 150Pa within 60 minutes, and react at ...

Embodiment 2

[0033] Add 630g terephthalic acid (PTA), 370g adipic acid (AA) and 686g 1,4-butanediol (1,4-BD) to a 5L stainless steel reactor equipped with nitrogen inlet, condensate outlet and stirrer. ), 0.2g of tetrapropyl titanate (equivalent to 200ppm of the total weight of PTA and AA) and 0.3g of antimony trioxide (equivalent to 300ppm of the total weight of PTA and AA). Keep the pressure in the kettle and stir at a constant speed. When the temperature in the reactor rises to 150℃, the water will be removed. Continue to increase the temperature and control the temperature in the reactor to not higher than 220℃. Wait until the amount of by-product water distilled from the reactor reaches the theoretical level. When the water output is reached, the esterification reaction ends. Continue to add 0.3g of tetrapropyl titanate (equivalent to 300ppm of the total weight of PTA and AA), 0.1g of antimony trioxide (equivalent to 100ppm of the total weight of PTA and AA) and 0.15g of trimethyl phos...

Embodiment 3

[0035] Add 532g terephthalic acid (PTA), 468g adipic acid (AA) and 806g 1,4-butanediol (1,4-BD) into a 5L stainless steel reactor equipped with nitrogen inlet, condensate outlet and stirrer. ), 0.3g tetramethyl titanate (equivalent to 300ppm of the total weight of PTA and AA) and 0.3g ethylene glycol antimony (equivalent to 300ppm of the total weight of PTA and AA). Keep the pressure in the kettle and stir at a constant speed. When the temperature in the reactor rises to 150℃, the water will be removed. Continue to increase the temperature and control the temperature in the reactor to not higher than 220℃. Wait until the amount of by-product water distilled from the reactor reaches the theoretical level. When the water output is reached, the esterification reaction ends. Continue to add 0.5 g of tetramethyl titanate (equivalent to 500 ppm of the total weight of PTA and AA) and 0.2 g of triphenyl phosphate (equivalent to 200 ppm of the total weight of PTA and AA) into the kettle...

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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 at normal 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 the fields of various soft package plastic products.

Description

Technical field: [0001] The present invention relates to polyester synthesis, and more specifically to the production of aliphatic-aromatic copolyesters prepared by direct esterification and copolycondensation of aromatic dicarboxylic acids, aliphatic dicarboxylic acids and aliphatic diols . Background technique: [0002] Polyester prepared by condensation polymerization method has been widely used in various fields of people's daily life as engineering materials. They can be made into materials such as fibers, beverage bottles, and films. The preparation of these polymers goes through two processes: the esterification or transesterification of terephthalic acid / aliphatic esters or their esterified products with aliphatic diols. Usually the esterification process takes place under high pressure conditions. The process is carried out under normal pressure; vacuum polycondensation of esterification or transesterification products. [0003] Polybutylene terephthalate / butylene adipat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/85C08G63/86C08G63/87C08G63/183
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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