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Method for synthesizing poly (1, 4-butanediol succinate) through ring-opening polymerization

A technology of polysuccinate and butylene glycol ester, which is applied in the field of ring-opening polymerization to synthesize polybutanediol succinate, can solve the problems of intermittent operation, high production cost, and poor environmental protection, and achieve Improve efficiency and production capacity, reduce raw material costs, and improve production efficiency

Active Publication Date: 2022-02-08
SHANGHAI NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In view of this, the object of the present invention is to provide a method for synthesizing polysuccinate-1,4-butanediol by ring-opening polymerization. The method provided by the invention takes cyclic succinic anhydride and cyclic tetrahydrofuran as the main unit Bulk raw materials, low-cost continuous production of high-molecular-weight poly-1,4-butylene succinate (PBS), overcome the existing technology with many by-products of small molecules, low yield, low molecular weight of PBS, poor chromaticity and performance , poor environmental protection, high production cost, intermittent operation, etc.

Method used

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  • Method for synthesizing poly (1, 4-butanediol succinate) through ring-opening polymerization
  • Method for synthesizing poly (1, 4-butanediol succinate) through ring-opening polymerization
  • Method for synthesizing poly (1, 4-butanediol succinate) through ring-opening polymerization

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Experimental program
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Effect test

Embodiment 1～4

[0032] Without adding succinic acid and changing the ratio of tetrahydrofuran and 1,4-butanediol, succinic anhydride, tetrahydrofuran and 1,4-butanediol were synthesized by ring-opening polymerization to synthesize PBS. The specific synthesis process and result analysis are as follows:

[0033] Add the cyclic monomer succinic anhydride, the cyclic monomer tetrahydrofuran and the chain monomer 1,4-butanediol into the raw material mixing tank according to the metering ratio in Table 1, stir well and preheat to 50°C, then Continuously feed into the esterification reactor and mix uniformly with all p-toluenesulfonic acid and 50wt% titanium tetrachloride (see Table 1 for the amount), and carry out the ring-opening esterification reaction at a temperature of 180°C, a pressure of 0.2MPa and a residence time of 60min ; The esterification product is continuously sent into the decompression kettle, and after the small molecules in the esterification product are decompressed at a pressure...

Embodiment 5～7

[0036] In the case of adding succinic acid and fixing the ratio of tetrahydrofuran and 1,4-butanediol, the ring-opening polymerization of succinic anhydride, tetrahydrofuran and 1,4-butanediol is used to synthesize PBS. The specific synthesis process and results are analyzed as follows:

[0037] Add the cyclic monomer succinic anhydride, the chain monomer succinic acid, the cyclic monomer tetrahydrofuran and the chain monomer 1,4-butanediol according to the metering ratio in Table 1, respectively, into the raw material mixing tank, and stir evenly and preheated to 45°C, and then continuously sent to the esterification reactor and mixed with all the p-toluenesulfonic acid and all the titanium tetrachloride (see Table 1 for the amount), and carried out at a temperature of 200°C, a pressure of 0.15MPa and a residence time of 45min. Ring-opening esterification reaction; then the esterification product is continuously sent into the vacuum kettle, and after the small molecules in the...

Embodiment 8～11

[0040] In the case of changing the ratio of four monomer raw materials and the type of polymerization catalyst, succinic anhydride, succinic acid, tetrahydrofuran and 1,4-butanediol were synthesized by ring-opening polymerization. The specific synthesis process and results are analyzed as follows:

[0041] Add the cyclic monomer succinic anhydride, the chain monomer succinic acid, the cyclic monomer tetrahydrofuran and the chain monomer 1,4-butanediol according to the metering ratio in Table 1, respectively, into the raw material mixing tank, and stir evenly And preheated to 60°C, then continuously sent into the esterification reactor and all the p-toluenesulfonic acid, the dosage is shown in Table 1) and mixed evenly, and the ring-opening esterification reaction was carried out at a temperature of 160°C, a pressure of 0.22MPa and a residence time of 90min; Then the esterification product is continuously sent into the decompression kettle, and after the small molecules in the e...

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Abstract

The invention provides a method for synthesizing poly (1, 4-butanediol succinate) through ring-opening polymerization, the method comprises the following steps: taking two cyclic monomers, namely succinic anhydride and tetrahydrofuran, as main raw materials and 1, 4-butanediol and / or succinic acid as auxiliary monomer raw materials, under the action of a composite catalyst, preparing the poly (1, 4-butylene succinate) (PBS) through three reaction steps of ring-opening esterification, pre-polymerization and final polymerization; essentially, transmission of active groups (hydroxyl and carboxyl) is achieved through addition-ring opening, growth of chains (alkyl and ester groups) is achieved through esterification-condensation, and finally high-molecular-weight PBS is obtained through polycondensation. Compared with the prior art, the PBS product synthesized by the method has the advantages of high polymerization degree, good chromaticity, low raw material and energy consumption and high product yield so that the quality of the PBS product can be improved, the production cost can be reduced, and the process is clean and environment-friendly.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis, in particular to a method for synthesizing poly-1,4-butylene succinate through ring-opening polymerization. Background technique [0002] With the rapid development of my country's economy and society and the continuous improvement of people's living standards, more and more attention has been paid to the environmental pollution of traditional plastics. It has become an inevitable trend to replace them with biodegradable plastics. Therefore, the development potential of degradable plastics in my country's market is huge. In particular, fully biodegradable plastic PBS, as one of the best comprehensive properties of degradable plastics, will have a huge demand in my country in the future, so it is urgent to develop high-quality, low-cost and large-scale continuous production of PBS technology. [0003] In the existing methods for synthesizing PBS, succinic acid or succinic acid diester and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/42C08G63/85C08G63/87
CPCC08G63/42C08G63/85C08G63/87Y02P20/584
Inventor 张春雷魏超王相茹张宝孙国梁王瑞旭
Owner SHANGHAI NORMAL UNIVERSITY
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