Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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 large dosage, many side reactions, and unstable production products, so as to achieve stable production products and improve the efficiency of esterification. Reaction rate, effect of increasing product yield

Active Publication Date: 2016-12-07
PETROCHINA CO LTD
View PDF11 Cites 11 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Synthetic method of polyether ester block copolymer
  • Synthetic method of polyether ester block copolymer
  • 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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Intrinsic viscosityaaaaaaaaaa
Tensile strengthaaaaaaaaaa
Intrinsic viscosityaaaaaaaaaa
Login to View More

Abstract

The invention relates to a synthetic method of a polyether ester block copolymer. The synthetic method includes the steps of: 1) adding raw materials comprising terephthalic acid, 1,4-butanediol and polyether glycol into a reaction kettle, and adding a co-catalyst and an additive, starting stirring, and when the internal temperature is increased to 100-170 DEG C, adding a main catalyst, and continuously increasing the temperature to 210-250 DEG C to perform an esterification reaction to obtain an esterification reaction product; 2) supplying the main catalyst to the esterification reaction product, performing a vacuum poly-condensation process including a low-vacuum poly-condensation and a high-vacuum poly-condensation steps to obtain the polyether ester block copolymer which includes a hard chain segment being polybutylene terephthalate and a soft chain segment being polyether. The copolymer is an elastomer material. The method belongs to continuous polymerization and is stable in the product, inhibits generation of side reactions of the 1,4-butanediol, is increased in esterification positive reaction rate and product yield, and is suitable for large-scale industrial 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com