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Butenediol-based polyester elastomer and preparation method thereof

A technology of butenediol-based polyester and butenediol is applied in the field of butenediol-based polyester elastomer and preparation, and can solve the problem of wide distribution of sample molecular mass, poor controllability of crosslinking degree, and crosslinking. The problem of low dosage of joint agent can achieve the effect of large-scale preparation, simple and feasible preparation method and high molecular weight.

Active Publication Date: 2021-07-20
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the activity of the double bond in itaconic acid is very high, there is a risk of gelation in the polycondensation stage, and the relative molecular mass distribution of the sample is wide; in addition, when using peroxide crosslinking, the crosslinking speed is too fast and the crosslinking The amount of linking agent is too low, and the degree of cross-linking is not well controllable

Method used

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  • Butenediol-based polyester elastomer and preparation method thereof
  • Butenediol-based polyester elastomer and preparation method thereof
  • Butenediol-based polyester elastomer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Add 565g (7.43mol) 1,3-propanediol, 669g (7.43mol) 1,4-butanediol, 145g (1.65 mol) 1,4-butenediol, 1050g (8.89mol) succinic acid, 770g (3.81mol) sebacic acid, 0.32g phosphorous acid and 1.28g hydroquinone; then under a nitrogen atmosphere, the temperature was raised to 180 ℃, normal pressure esterification for 2 hours; then add tetrabutyl titanate with 0.1% of the total mass of the monomers as a catalyst, and raise the temperature to 220 ℃ and 3kPa, and pre-condense for 1 hour; finally, at 220 ℃, evacuate to below 500Pa, After 9 hours of final polycondensation, a butylene glycol-based polyester elastomer was obtained.

[0053] The structure of prepared butylene glycol based polyester elastomer is as follows:

[0054]

[0055] Among them, m1=3, m2=4; n1=2, n2=8;

[0056] In addition, (a+c+e):(k+m+o)≈9.52:4.08.

Embodiment 2

[0058] Add 598g (6.63mol) 1,4-butanediol, 212g (2.41mol) 1,4-butenediol, 931g (10.33mol) lactic acid, 153g (1.29mol) succinic acid, 1306g (6.46mol) sebacic acid, 3.2g tris-(2,4-di-tert-butylphenyl)-phosphite and 12.8g p-hydroxy Anisole; then, under a nitrogen atmosphere, heat up to 130°C, perform esterification at normal pressure for 2 hours, then raise the temperature to 190°C, and continue esterifying at normal pressure for 2 hours; then add tetraisopropyl titanate with a total mass of 0.05% of the monomer It is used as a catalyst, and the temperature is raised to 190°C and 10kPa, and the pre-condensation is carried out for 4 hours; finally, the vacuum is evacuated to below 500Pa at 210°C, and the final polycondensation is carried out for 6 hours to obtain a butylene glycol-based polyester elastomer.

[0059] The structure of prepared butylene glycol based polyester elastomer is as follows:

[0060]

[0061] Among them, m1=4, m2=0 (equivalent to m1=m2=4); n1=2, n2=8;

...

Embodiment 3

[0064] Add 709g (7.86mol) 1,4-butanediol, 277g (3.15mol) 1,4-butenediol, 501g (4.72mol) diethylene glycol, 851g (7.21mol) succinic acid, 862g (5.90mol) adipic acid, 1.6g triphenyl phosphite, 8g p-phenylenediamine; then under nitrogen atmosphere, be warming up to 185 ℃, normal pressure esterification for 3 hours; then add p-toluenesulfonic acid with 0.40% of the total mass of the monomers as a catalyst, and raise the temperature to 210 ℃, 5kPa, pre-condensation for 2 hours; finally vacuumize at 230 ℃ to below 500Pa, final polycondensation 7h to obtain butylene glycol-based polyester elastomer.

[0065] The structure of prepared butylene glycol based polyester elastomer is as follows:

[0066]

[0067] Among them, m1=4, m2=0 (equivalent to m1=m2=4); n1=2, n2=4; x=y=1;

[0068] In addition, (a+e+g):(i+k+o)≈7.21:5.90.

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Abstract

The invention discloses a butylene glycol-based polyester elastomer and a preparation method thereof. The structure of the butenediol-based polyester elastomer is shown as follows: 1, 4-butenediol containing high-stability double bonds is selected to replace itaconic acid, a series of high-molecular-weight narrow-distribution butenediol-based polyester elastomers are synthesized, and the high-molecular-weight narrow-distribution butenediol-based polyester elastomers have high relative molecular mass and narrow relative molecular mass distribution; and the crosslinking in the subsequent processing process is more controllable, and the dosage of the vulcanizing agent is equivalent to that of the traditional rubber.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a butylene glycol-based polyester elastomer and a preparation method thereof. Background technique [0002] Polyester, as a class of degradable polymers, has been extensively studied and concerned in the field of polymer materials. At present, the annual output of the polyester industry has reached tens of millions of tons, but its application is still mainly limited to plastics and fibers, and is rarely involved in the rubber field. In view of this, since the concept of "bio-based engineering elastomer" was proposed in 2008, Beijing University of Chemical Technology proposed and prepared a variety of bio-based polyester elastomer materials for the first time, thereby broadening the application field of polyester. [0003] The design strategy of polyester elastomers is to destroy the crystallization behavior of polyester molecular chains through multi-component copolym...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/52C08G63/676C08G63/78
CPCC08G63/52C08G63/676C08G63/78C08G63/60C08G63/672C08G63/85C08G63/87
Inventor 王朝张奇男张立群王文才张宁赵燕超
Owner BEIJING UNIV OF CHEM TECH
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