High molecular weight poly(butylene succinate) and preparation method thereof

A technology of polybutylene succinate and double-ended hydroxybutylene succinate, which is applied in the field of high molecular weight polybutylene succinate and its preparation, can solve the problem of limited application range, long production cycle, Limited strength and other issues, to achieve cost reduction, low cost, good heat resistance and mechanical properties

Active Publication Date: 2007-11-28
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The company uses polybutylene succinate with a number-average molecular weight of at least 10,000 as a prepolymer, and diisocyanate as a chain extender to prepare high-molecular-weight polybutylene succinate through melt reaction. Its patent (US5391644, US5348700, US5525409) disclosed specific preparation process is as follows: first 1,4-butanedioic acid and butanediol are esterified at 190~210 DEG C under normal pressure for 3.5 hours, then at 190~210 DEG C, 2~20mmHg After 3.5 hours of polycondensation under vacuum conditions, add a catalyst to the reaction system, raise the temperature to 215-220°C, and continue the reaction for 5.5 hours under vacuum conditions of 15-0.2mmHg to obtain a number-average molecular weight of 16,800 and a weight-average molecular weight of 43,600 Butanediol succinate prepolymer, and then react the prepolymer with diisocyanate for 1 hour at 180-200°C to prepare polybutylene succinate with a number average molecular weight of 35,500 and a weight average molecular weight of 170,000 Ester products, but due to the wide molecular weight distribution of this product (4.8), its strength is limited, and its production cycle is long and its cost is high, which greatly limits its application range

Method used

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  • High molecular weight poly(butylene succinate) and preparation method thereof
  • High molecular weight poly(butylene succinate) and preparation method thereof
  • High molecular weight poly(butylene succinate) and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put 1,4-butanediol and succinic acid with a molar ratio of 1.5:1 in the reaction device, stir and raise the temperature to 180-190°C under the protection of nitrogen, and after esterification to remove water for 3.5 hours, add succinic acid , butanediol with a total weight of 0.01% catalyst tetrabutyl titanate, change the water separation device to a vacuum device, and react for 30 minutes at 190°C and 30Pa vacuum conditions to obtain an intrinsic viscosity of 0.08dL / g double-ended hydroxybutyrate Diacid butanediol prepolymer, its number average molecular weight recorded is 1200.

[0027] Put 87 parts of prepolymer in the reaction device first, stir and heat up to 150°C under the protection of nitrogen, after it is completely melted, add 13 parts of chain extender toluene diisocyanate, and react for 30 minutes to obtain the product. The number average molecular weight of the measured product is 5.67×10 4 , with a weight average molecular weight of 1.02×10 5 , the mole...

Embodiment 2

[0029] Put 1,4-butanediol and succinic acid with a molar ratio of 1.4:1 in the reaction device, stir and raise the temperature to 180-190°C under the protection of nitrogen, after 3.5 hours of esterification to remove water, add succinic acid The total weight of butanediol is 0.5% catalyst tin oxide, the water separation device is changed to a vacuum device, and the reaction is carried out at 200 ° C and 30 Pa for 10 minutes to obtain an intrinsic viscosity of 0.12 dL / g double-ended hydroxybutyric acid The number average molecular weight of the diol prepolymer is 2100.

[0030] Put 92 parts of prepolymer in the reaction device first, stir and heat up to 160°C under the protection of nitrogen, after it is completely melted, add 8 parts of chain extender toluene diisocyanate, and react for 30 minutes to obtain the product. The number average molecular weight of the measured product is 7.63×10 4 , with a weight average molecular weight of 1.35×10 5 , the molecular weight distri...

Embodiment 3

[0032] Put 1,4-butanediol and succinic acid with a molar ratio of 1.35:1 in the reaction device, stir and raise the temperature to 180-190°C under the protection of nitrogen, after 3.5 hours of esterification to remove water, add succinic acid , butanediol with a total weight of 2% catalyst p-toluenesulfonic acid, change the water separation device to a vacuum device, and react for 30 minutes at 210 ° C and 30 Pa vacuum conditions to obtain an intrinsic viscosity of 0.17 dL / g double-ended hydroxybutane Acid butylene glycol prepolymer, its number-average molecular weight recorded is 3100.

[0033] Put 92.5 parts of prepolymer in the reaction device first, stir and heat up to 160°C under the protection of nitrogen, and then add 7.5 parts of chain extender diphenylmethane diisocyanate after it is completely melted, and react for 30 minutes to obtain the product. The number average molecular weight of the measured product is 9.01×10 4 , with a weight average molecular weight of 1.5...

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Abstract

The present invention relates to one kind of high molecular weight polybutanediol succinate and its preparation process, and features that bihydroxy terminated butanediol succinate, especially low molecular weight bihydroxy terminated butanediol succinate, as the pre-polymer and diisocyanate as the chain extender in 0.1-13 % are molten and reacted to prepare polybutanediol succinate with low cost, great molecular weight, narrow molecular weight distribution and excellent mechanical performance. The polybutanediol succinate has number average molecular weight greater than 5.5x10<4>, molecular weight distribution of 1.4-1.8, tensile strength of 39-58 MPa, and elongation at break of 300-700 %.

Description

technical field [0001] The invention belongs to the technical field of aliphatic polyester and its preparation method, and in particular relates to a high molecular weight polybutylene succinate and its preparation method. Background technique [0002] Due to the excellent performance of petroleum-based plastics, they are widely used in various occasions, but because of their non-degradability, they have brought serious pollution to the social and living environment. In order to reduce or avoid this kind of pollution, biodegradable aliphatic polyester has become a research hotspot of domestic and foreign experts and scholars in recent years. However, most aliphatic polyesters are difficult to compete with traditional petroleum-based plastics due to poor thermal stability and poor mechanical properties caused by their structural factors. Even a small number of aliphatic polyesters with better performance, due to high cost factors, also determine that it is temporarily diffic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/16C08G63/78C08G63/85
Inventor 王玉忠曾建兵李以东丁颂东杨科珂汪秀丽周茜陈思翀
Owner SICHUAN UNIV
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