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A kind of synthetic method of polyether ester block copolymer

A technology of block copolymers and synthesis methods, which is applied in the field of synthesis of polyether ester block copolymers, can solve the problems of unstable production products, many side reactions, large dosage, etc., achieve stable production products, and improve the efficiency of esterification. Reaction rate, effect of increasing product yield

Active Publication Date: 2018-05-04
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0019] The object of the present invention is to provide a kind of synthetic method of polyether ester block copolymer, to solve the instability of batch polymerization production product existing in the prior art, and in chain exchange method polymerization, the consumption of 1,4-butanediol is large, side effects Questions with many responses

Method used

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  • A kind of synthetic method of polyether ester block copolymer
  • A kind of synthetic method of polyether ester block copolymer
  • A kind of synthetic method of polyether ester block copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Add PTA: 996g, BD: 972ml, tetrahydrofuran polyether (PTMG, molecular weight: 1000) 664g, antimony acetate 0.35g, magnesium acetate 0.2g, sodium acetate 0.2g into the reaction kettle, then open the reaction kettle to stir and heat, PTA and BD The molar ratio is 1:1.8, and the mass ratio of PTA to PTMG is 60:40. When the temperature in the kettle (that is, the internal temperature) reaches 130°C, add 0.55ml of tetrabutyl titanate and continue to heat up to 210°C to start the esterification reaction and The esterification starts to effluent, the esterification reaction is normal pressure reaction, the internal temperature is controlled between 210-250°C, the water temperature at the top of the fractionation column is about 100°C, and the esterification reaction is ended when the temperature at the top of the fractionation column naturally drops to 85°C ( At this time, the reaction water is relatively slow, which proves that the esterification reaction is close to the end), ...

Embodiment 2

[0060] Add PTA: 996g, BD: 810ml, tetrahydrofuran polyether (PTMG, molecular weight: 1000) 664g, antimony acetate 0.35g, magnesium acetate 0.2g, sodium acetate 0.2g into the reaction kettle, then start the reaction kettle to stir and heat, the PTA and BD The molar ratio is 1:1.5, and the mass ratio of PTA to PTMG is 60:40. When the temperature in the kettle reaches 130°C, add 0.55ml of tetrabutyl titanate and continue to raise the temperature to 210°C to start the esterification reaction and start esterification to effluent. The esterification reaction is a normal pressure reaction, the internal temperature is controlled between 210 and 250°C, and the temperature of the outlet water at the top of the fractionation column is about 100°C. Slowly proves that the esterification reaction is close to the end), the esterification time is 75 minutes, and the esterification effluent is 220ml. After adding 0.55ml of tetrabutyl titanate into the obtained esterification reactant, it starts ...

Embodiment 3

[0062] Add PTA: 996g, BD: 918ml, tetrahydrofuran polyether (PTMG, molecular weight: 1000) 815g, antimony acetate 0.35g, magnesium acetate 0.2g, sodium acetate 0.2g in the reaction kettle, then open the reaction kettle to stir and heat, the PTA and BD The molar ratio is 1:1.7, and the mass ratio of PTA to PTMG is 55:45. When the temperature in the kettle reaches 130°C, add 0.55ml of tetrabutyl titanate and continue to raise the temperature to 210°C to start the esterification reaction and start esterification to effluent. The esterification reaction is a normal pressure reaction, the internal temperature is controlled between 210 and 250°C, and the temperature of the outlet water at the top of the fractionation column is about 100°C. Slowly proves that the esterification reaction is close to the end), the esterification time is 1.5 hours, and the esterification effluent is 260ml. After adding 0.55ml of tetrabutyl titanate into the obtained esterification reactant, it begins to e...

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Abstract

The present invention relates to a kind of synthesis method of polyether ester block copolymer, comprises the following steps: (1) adding raw material terephthalic acid, 1,4-butanediol and polyether diol into the reactor, simultaneously adding Co-catalyst and auxiliary agent, start stirring, when the internal temperature rises to 100-170 °C, then add the main catalyst, continue to heat up to 210-250 °C for esterification reaction, and obtain the esterification reaction product; (2) in the obtained ester After adding the main catalyst to the chemical reaction product, it starts to enter the vacuum polycondensation stage. After the low vacuum polycondensation reaction and high vacuum polycondensation reaction, the composition including the hard segment is polybutylene terephthalate and the soft segment is polyether. The polyether ester block copolymer, the copolymer is an elastomer material; the present invention is continuous polymerization, the production product is stable, and the occurrence of side reactions of 1,4-butanediol is suppressed, and the positive reaction rate of esterification is improved , which increases the product yield and is suitable for large-scale industrialized continuous production.

Description

technical field [0001] The invention relates to the field of chemically synthesized polymer materials, in particular to a method for synthesizing polyether ester block copolymers. Background technique [0002] Polyether ester (TPEE) is a thermoplastic elastomer with excellent performance and wide application. It is based on crystalline high melting point aromatic polyester hard segment (such as PBT) or aliphatic polyester (such as polylactide PLLA, Polyglycolide PGA, polycaprolactone PCL, etc.) and polyether soft segments with a lower glass transition temperature (such as polyethylene glycol ether PEG, polypropylene glycol ether PPG, polytetramethylene glycol ether PTMG, etc.) block copolymers. [0003] At the use temperature, the hard segment of the polyetherester elastomer partially crystallizes to form a crystalline microdomain, and the soft segment and the uncrystallized hard segment of the polyetherester elastomer form an amorphous phase, and the crystalline microdomai...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/672C08G63/85
Inventor 吴佩华张元礼陈颖石艳曹鼎李振忠邹妍李彦钧孙一峰赵晶林妍妍王文娟
Owner PETROCHINA CO LTD
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