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Preparation method of copolyether ester

A technology of copolyetherester and transesterification, which is applied in the field of thermoplastic block copolyetherester elastomers, can solve the problems of difficult processing, high processing temperature, and the melting point of copolyetherester higher than 220°C, and achieve physical property changes and processability Excellent, melting point and crystallization rate lowering effects

Inactive Publication Date: 2010-06-16
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the processing temperature of this polyether ester is relatively high, about 260°C, which brings certain difficulties to the processing.
Japanese patent JP2175719 reported polycondensation of phthalic acid and its derivatives with ethylene glycol, 1,4-cyclohexanedimethanol, and polyalkylene ether glycol to form polyether esters, and found that cyclohexanedimethanol introduced The elasticity and heat resistance of the post polyether ester are excellent, but the melting point of the obtained copolyether ester is higher than 220°C

Method used

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  • Preparation method of copolyether ester
  • Preparation method of copolyether ester
  • Preparation method of copolyether ester

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Weigh 970 grams of dimethyl terephthalate (DMT), 720 grams of 1,4-butanediol (BG), 1000 grams of polytetramethylene ether glycol (PTMG, molecular weight 1000), 144 grams of 1 , 4-cyclohexanedimethanol (CHDM, 10% total glycol mole fraction), 50ppm tetrabutyl titanate, 3065ppm antioxidant. Add part of dimethyl terephthalate (DMT) powder into the 5L reactor equipped with inlet and outlet, nitrogen inlet, condenser, agitator and fractionation column, turn on the heating, and then add the remaining materials into slurry . Gradually rise from room temperature to the range of 180-220°C, keep the temperature at the top of the fractionation column at 63-65°C, and when the amount of by-product methanol distilled out of the reaction kettle reaches more than 90% of the theoretical amount, start to reduce the pressure and heat up, and reduce the temperature in about 40 minutes. The pressure is reduced below 150Pa, while the temperature rises to 280-290°C. Keep this temperature and...

Embodiment 2

[0034] First weigh 776 grams of dimethyl terephthalate (DMT), 500 grams of 1,4-butanediol (BG), 185 grams of polytetramethylene ether glycol (PTMG, molecular weight 500, 5% total binary Alcohol mole fraction), 200 g 1,4-cyclohexanedimethanol (CHDM, 19% total glycol mole fraction), 32 ppm tetrabutyl titanate, 2625 ppm antioxidant. Add dimethyl terephthalate (DMT) powder into a 3L reaction kettle equipped with inlet and outlet, nitrogen inlet, condenser, stirrer and fractionation column, turn on the heating, and then add the slurry made of the remaining materials into . Gradually rise from room temperature to the range of 200-220°C, keep the temperature at the top of the fractionation column at 63-65°C, and when the amount of by-product methanol distilled out of the reactor reaches more than 90% of the theoretical amount, start to reduce the pressure and heat up, and reduce the temperature in about 40 minutes. The pressure is reduced below 130 Pa, while the temperature rises to...

Embodiment 3

[0036]Will weigh 776 grams of dimethyl terephthalate (DMT), 578 grams of 1,4-butanediol (BG), 264 grams of polytetramethylene ether glycol (PTMG, molecular weight 1500, 2% total di Alcohol mole fraction), 317 grams of 1,4-cyclohexanedimethanol (CHDM, 25% total glycol mole fraction), tetrabutyl titanate of 35ppm titanium, magnesium acetate of 25ppm, 2976ppm antioxidant The slurry is added into a 3L reactor equipped with inlet and outlet, nitrogen inlet, condenser, stirrer and fractionation column. Gradually raise the temperature of the reactor from room temperature to the range of 210-220°C, keep the top temperature of the fractionation column at 64-65°C, and when the amount of by-product methanol distilled out of the reactor reaches more than 90% of the theoretical amount, start to reduce the pressure and increase the temperature. Reduce the pressure to below 120Pa in about 40 minutes, and at the same time, raise the temperature to 280-290°C, continue the polycondensation reac...

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Abstract

The invention relates to a preparation method of copolyether ester, belonging to the field of thermoplastic block copolyether ester elastomers. The copolyether ester contains a short-chain polyester hard segment and a long-chain polyether ester soft segment, wherein the short-chain polyester hard segment comprises repeating units of a dicarboxylic acid component and a dihydric alcohol component, and the long-chain polyether ester soft segment comprises repeating units of a dicarboxylic acid component and a poly alkylene ether glycol component. The polyester hard segment comprises a polyester segment (A) and a polyester segment (B), wherein the polyester segment (A) comprises repeating units of an aromatic dicarboxylic acid component and a 1,4-butanediol component, and the polyester segment (B) comprises repeating units of an aromatic dicarboxylic acid component and a 1,4-cyclohexanedimethanol component; and the polyether ester soft segment is a polyether ester segment (C) which comprises repeating units of an aromatic dicarboxylic acid component and a poly alkylene ether glycol component. The product has excellent comprehensive performance, the melting point is 160-220 DEG C, the elongation at break is 500-1400%, and the thermal decomposition temperature is 360-450 DEG C.

Description

technical field [0001] The invention belongs to the field of thermoplastic block copolyetherester elastomers, in particular to a preparation method of copolyetherester elastomers containing 1,4-cyclohexanedimethanol (CHDM) as one of its glycol components. Background technique [0002] As a kind of engineering grade elastomer, linear thermoplastic polyether ester elastomer has excellent physical and mechanical properties, such as toughness, fatigue resistance, high strength, abrasion resistance, oil resistance and chlorine resistance, and its elasticity and strength are between Between plastic and rubber, it is widely used in many fields such as automobile industry, electronic appliances, electrical instruments, industrial products, communications, sporting goods, and shoemaking. [0003] At present, most industrialized polyether ester elastomers use polytetramethylene ether (PTMG) as the soft segment and polybutylene terephthalate (PBT) as the hard segment. However, the the...

Claims

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Application Information

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IPC IPC(8): C08G63/672C08G63/78
Inventor 田英良孙诗兵张继光张港汤清琼
Owner BEIJING UNIV OF TECH
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