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A kind of preparation method of high molecular weight polybutylene succinate

A polybutylene succinate and high molecular weight technology is applied in the field of preparation of high molecular weight polybutylene succinate, and can solve the problems of low molecular weight of products, unstable reaction process, low product conversion rate and the like , to achieve the effect of continuous preparation process, narrow molecular weight distribution and high molecular weight

Active Publication Date: 2018-02-09
陕西延长泾渭新材料科技产业园有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For above-mentioned existing problems, the present invention aims to provide a kind of preparation method of high molecular weight polybutylene succinate, with succinic acid, butanediol as raw material, adopts oligomer formation stage, high polymer formation stage successively stage, extrusion chain extension reaction stage to produce high molecular weight polybutylene succinate, the present invention aims to solve the low product conversion rate, low product molecular weight, reaction Unstable process, easy to produce gel and other problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Oligomer formation stage: add succinic acid and butanediol into the reaction kettle, the molar ratio of succinic acid and butanediol is 1: 1.0, and nitrogen gas is introduced to remove air, and the flow rate of nitrogen gas is 0.10- 0.20m 3 / h, add catalyst n-butyl titanate and butanediol titanium, the weight ratio of n-butyl titanate and butanedioxide titanium is 1:1, the total weight of n-butyl titanate and butanedioxide titanium is butanedioxide 0.5% of the weight of the acid, vacuumize the reactor, keep the pressure below 3Kpa during the reaction, keep the temperature of the reactor at 160°C, collect the water produced in the reaction process through a condensation device, and the reaction time is 1.5 hours to obtain succinic acid and The hydroxyl-terminated oligomer of butanediol, the number average molecular weight is Mn=1.1×10 4 ;

[0022] (2) Polymer formation stage: pass the reaction product of step (1) into another reaction kettle, pass nitrogen gas to e...

Embodiment 2

[0026] (1) Oligomer formation stage: add succinic acid and butanediol to the reaction kettle, the molar ratio of succinic acid and butanediol is 1: 1.2, and nitrogen gas is introduced to remove air, and the flow rate of nitrogen gas is 0.20m 3 / h, add catalyst n-butyl titanate and butanediol titanium, the weight ratio of n-butyl titanate and butanedioxide titanium is 1:1, the total weight of n-butyl titanate and butanedioxide titanium is butanedioxide 1.5% of the weight of the acid, vacuumize the reactor, keep the reaction pressure below 2Kpa, keep the temperature of the reactor at 200°C, collect the water generated during the reaction through a condensation device, and the reaction time is 2.5 hours to obtain succinic acid and butyric acid Hydroxyl-terminated oligomers of diols with a number average molecular weight of Mn=1.8×10 4 ;

[0027] (2) Polymer formation stage: pass the reaction product of step (1) into another reaction kettle, pass nitrogen gas to exclude air, and ...

Embodiment 3

[0031] (1) Oligomer formation stage: add succinic acid and butanediol into the reaction kettle, the molar ratio of succinic acid and butanediol is 1: 1.1, and nitrogen gas is introduced to remove air, and the flow rate of nitrogen gas is 0.15m 3 / h, add catalyst n-butyl titanate and butanediol titanium, the weight ratio of n-butyl titanate and butanedioxide titanium is 1:1, the total weight of n-butyl titanate and butanedioxide titanium is butanedioxide 1.0% of the weight of the acid, vacuumize the reactor, keep the reaction pressure below 1Kpa, keep the temperature of the reactor at 180°C, collect the water generated during the reaction through a condensation device, and the reaction time is 2 hours to obtain succinic acid and butyric acid Hydroxyl-terminated oligomer of diol, number average molecular weight Mn=1.5×104 ;

[0032] (2) Polymer formation stage: pass the reaction product of step (1) into another reaction kettle, pass nitrogen gas to exclude air, and the flow rate...

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Abstract

The invention provides a preparation method of high-molecular-weight poly(butylene succinate).Butanedioic acid and butanediol are adopted as raw materials, the product poly(butylene succinate) is formed through an oligomer forming stage, a polymer forming stage and an extrusion chain extension reaction stage in sequence, the oligomer forming stage is completed under the condition of negative pressure being 3 Kpa, the number-average molecular weight of poly(butylene succinate) finally generated after the reaction is larger than or equal to 1.0*105, and the distribution range of the molecular weight is 1.2-1.6.The preparation method is high in esterification rate, the molecular weight of the generated product is high, the distribution range of the molecular weight is narrow, no gel is generated in the reaction process, and the preparation process is easy to control.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis, and in particular relates to a preparation method of high molecular weight polybutylene succinate. Background technique [0002] Traditional polyolefin plastics are not degradable, and their products have caused serious environmental pollution problems. Degradable plastics have become an effective way to fundamentally solve this problem. Polybutylene succinate (PBS), as an aliphatic polyester plastic, is prone to hydrolysis under the action of enzymes in various microorganisms or animals and plants in nature because its molecular backbone contains ester bonds that are easily hydrolyzed. Decomposition, metabolism, and finally decomposed into carbon dioxide and water. Therefore, polybutylene succinate, as a typical fully biodegradable material, can be used as various plastic products, such as packaging, tableware, cosmetic bottles, medicine bottles, agricultural materials and me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/16C08G63/78
CPCC08G63/16C08G63/78
Inventor 王波黄捷杨金明田小艳汤粤豫刘旭张玉娟郭潜
Owner 陕西延长泾渭新材料科技产业园有限公司
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