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Method for rapidly synthesizing poly (butylene succinate) or copolymer thereof

The technology of polybutylene succinate and copolymer, which is applied in the field of polymer synthesis, can solve the problems of many by-products of small molecules, long reaction time and high investment in the early stage of the device, so as to improve the efficiency of polymerization reaction, High-efficiency catalytic effect and less catalyst dosage

Active Publication Date: 2021-01-29
ANHUI XUELANG BIOTECHNOLOGY CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polybutylene succinate prepared by this invention has a weight-average molecular weight of up to 100,000. It is a thermoplastic resin with good mechanical properties, but the requirements for equipment are relatively high and the cost is relatively high.
The patent application with publication number CN101935391 discloses a preparation method of high molecular weight aliphatic polyester, which uses aliphatic diacid diester and aliphatic diol as raw materials for melt polycondensation to obtain a weight average molecular weight of 5-25 Wan, an aliphatic polyester with a molecular weight distribution coefficient of 1.9-2.2, but the disadvantage of this method is that the reaction time is long and the catalyst activity is low, especially in the transesterification stage, the side reaction of 1,4-butanediol cyclization to THF is serious, This will seriously affect the further increase of the molecular weight of aliphatic polyester and cause a great waste of raw materials, especially the recovery and treatment of by-products, which will indirectly increase production costs
In addition, this method does not involve issues such as product color and luster, which will seriously limit the wider application range of this product
Tsinghua University disclosed in the patent document CN1861660A the synthesis method of dibasic acid and dibasic alcohol to prepare aliphatic polyester. It adopts the two-step method of pre-condensation and vacuum polycondensation, and adds the third monomer dibasic acid to obtain high molecular weight aliphatic polyester. Polyester, this method has the shortcoming that there are many small molecular by-products, and the product yield is low
[0005] The related patents mentioned above all use dibasic acid as raw material. Dibasic acid is highly corrosive and requires high material requirements for production equipment, resulting in high initial investment and high maintenance costs for the device. That is to say, from the other hand Increased product manufacturing costs
Moreover, the reaction time of the above-mentioned schemes is long, the polymerization efficiency is not high, and the industrialized production value of the overall process is not high.

Method used

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  • Method for rapidly synthesizing poly (butylene succinate) or copolymer thereof
  • Method for rapidly synthesizing poly (butylene succinate) or copolymer thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1. Catalyst preparation:

[0032] Add 30g of solid nano-silica and 800ml of 1,2-dichloroethane into a three-necked flask, then slowly add 17.3g of chlorosulfonic acid dropwise at room temperature, and the dropwise addition is completed within half an hour, and then the reaction system Vigorously stir for one hour, and react at room temperature for 36 hours. After almost no hydrogen chloride gas is detected, 1,2-dichloroethane is removed by a rotary evaporator to obtain an off-white solid powder. The mass after drying is 43.5g, which is stored in Standby as catalyst A in the desiccator.

Embodiment 2

[0033] The preparation of embodiment 2.PBS

[0034] In the 1000ml flask, add succinic acid 360g, add butanediol 340g, add the catalyst A0.75g that embodiment 1 prepares. Turn on the power of the microwave reactor to 300w, raise the temperature to 220°C, react for 20 minutes, and the reaction ends. The carboxyl group content at the detection terminal is 210mol / t. After the esterification reaction is completed, the polymerization reaction is started, and the polymerization catalyst tetrabutyl titanate 1.5g, the auxiliary agent B zinc acetate 0.2g, the power of the microwave reactor is 450w, the temperature is raised to 240°C, and the pressure is 100 ~200pa, reaction time 2h, get PBS product, number average molecular weight 10×10 4 , dispersibility 2.2, weight average molecular weight 22×10 4 , the product color is white.

Embodiment 3

[0035] The preparation of embodiment 3.PBS

[0036] In the 1000ml flask, add succinic acid 360g, add butanediol 340g, add the catalyst A1.0g that embodiment 1 prepares. Turn on the power of the microwave reactor to 300w, raise the temperature to 220°C, react for 30 minutes, and the reaction ends. The carboxyl group content at the detection terminal is 110mol / t. The esterification reaction is completed, and the polymerization reaction is started. Add 1.5g of the polymerization catalyst tetrabutyl titanate, 0.3g of the auxiliary agent B zinc acetate, and the power of the microwave reactor is 450w. The temperature is raised to 240°C and the pressure is 100 ~200pa, reaction time 3h, get PBS product, number average molecular weight 12×10 4 , dispersibility 2.2, weight average molecular weight 26.4×10 4 , the product color is white.

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Abstract

The invention provides a method for rapidly synthesizing poly (butylene succinate) or a copolymer thereof, which comprises the following steps: modifying solid nano silicon dioxide by using chlorosulfonic acid to obtain solid nano silicon dioxide grafted with sulfonic acid groups on the surface, and marking as a catalyst A; in the presence of the catalyst A, carrying out microwave treatment on polymerization monomers at 200-240 DEG C to carry out esterification reaction, wherein the polymerization monomers comprise butanediol and a binary acid, and the binary acid at least comprises succinic acid; after the esterification reaction is finished, adding a polymerization catalyst and an assistant B, wherein the assistant B is used for forming sulfonate with the sulfonic acid group of the catalyst A; vacuumizing and carrying out microwave treatment, and carrying out condensation polymerization at 220-260 DEG C to obtain the polybutylene succinate or the copolymer thereof. The method disclosed by the invention overcomes the problems that the molecular weight of the copolymer prepared by the traditional process is lower and the molecular weight is increased by using a toxic chain extender, and remarkably shortens the reaction time, so that the production of the poly (butylene succinate) and the copolymer thereof is more efficient and economic, and is more beneficial to industrialization.

Description

technical field [0001] The invention relates to a synthesis method of a high molecular polymer, in particular to a synthesis method of polybutylene succinate or a copolymer thereof. Background technique [0002] Plastics are widely used in industry and life due to their good performance, low density, and good processing performance. However, a large amount of solid waste plastics has brought serious environmental problems and become a worldwide public hazard. Traditional burial and incineration will cause pollution, and the search for a temporary and permanent solution must start from the source. Vigorously developing degradable materials is an effective way for the greening of polymer materials today. At the same time, the supply of global oil resources is becoming increasingly tense, and the development of a low-carbon economy has also brought new development opportunities for biodegradable plastics, and the market demand for degradable plastics is growing rapidly. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/87C08G63/83C08G63/85C08G63/16C08G63/183
CPCC08G63/87C08G63/83C08G63/85C08G63/16C08G63/183Y02W90/10
Inventor 李云政李福甲万玉青
Owner ANHUI XUELANG BIOTECHNOLOGY CO LTD
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