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Method for preparing high-molecular weight aliphatic polycarbonate

A technology of polycarbonate and high molecular weight, which is applied in the field of high-efficiency synthesis of high molecular weight aliphatic polycarbonic acid, which can solve the problems of reduced yield of target polymers, accelerated side reactions, etc., and facilitates large-scale application, suppresses side reactions, and has no loss of raw materials Effect

Inactive Publication Date: 2016-12-28
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the shortcomings that the acidity in the traditional Lewis acid zinc salt catalyst system is too strong, and the progress of side reactions will be accelerated and the yield of the target polymer will be reduced.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add diphenyl carbonate, 1,4-butanediol and zinc fluoride catalyst in a molar ratio of 1:1 into the reactor, wherein the molar ratio of Zn to diphenyl carbonate is 0.3%, and the N 2 After dissolving at 120°C in the atmosphere, stir rapidly for 1 h. Then react at 220°C for 2.0h, reduce the pressure to 600Pa, and react until no distillate comes out. Then continue to reduce the pressure below 300Pa, react at the same temperature for 2 hours, and the obtained polymer is the aliphatic polycarbonate material. The molecular weight M of the polymer was tested by gel chromatography w =168 000, Y=92%. .

Embodiment 2

[0020] Diphenyl carbonate and 1,4-butanediol and zinc glutarate catalyst that the ratio of substance amount is 1:1 join in the reactor, wherein the mol ratio of Zn and diphenyl carbonate is 0.4%, in N 2 Rapid stirring was carried out at 120° C. for 1 h in the atmosphere. Then react at 220°C for 2.0h, reduce the pressure to 600Pa, and react until no distillate comes out. Then continue to reduce the pressure below 300Pa, and continue to react at the same temperature for 2 hours, and the obtained polymer is an aliphatic polycarbonate material. The molecular weight M of the polymer was tested by gel chromatography w =177000, Y=86%. .

Embodiment 3

[0022] Diphenyl carbonate and 1,4-butanediol and the zinc oxide catalyst that the ratio of substance amount is 1:1 join in the reactor, wherein the mol ratio of Zn and diphenyl carbonate is 0.4%, in N 2 Rapid stirring was carried out at 120° C. for 1 h in the atmosphere. Then react at 220°C for 2.0h, reduce the pressure to 600Pa, and react until no distillate comes out. Then continue to reduce the pressure below 300Pa, and continue to react at the same temperature for 2 hours, and the obtained polymer is an aliphatic polycarbonate material. The molecular weight M of the polymer was tested by gel chromatography w =91 300, Y=90%.

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Abstract

The invention relates to a method for preparing high-molecular weight aliphatic polycarbonate. The method is characterized in that diphenyl carbonate and aliphatic diol are taken as raw materials, and then subjected to two-step reaction of melting ester exchange and polycondensation in a zinc-based catalysis system to obtain the high-molecular weight aliphatic polycarbonate. The zinc-based catalyst takes zinc halide, zinc glutarate and zinc acetate as active components, the active components are loaded on the surface of an inorganic mesoporous material and an organic polymer material to obtain the catalyst, and the carrier mass accounts for 0-95 wt% of that of the catalyst mass. The method has the characteristics of fast reaction rate and high yield, in the invention, diphenyl carbonate and aliphatic diol are rapidly subjected to ester exchange and polycondensation to obtain the high-molecular weight aliphatic polycarbonate. A synthesis polymer is a white solid, the color is good, the number-average molecular weight is more than 100000, the polymer can be used as plastic, and the polymer yield can reach as high as 95%. The method has the advantages of simple process, large synthesis polymer molecular weight, and high yield, and has good industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and relates to a method for efficiently synthesizing high-molecular-weight aliphatic polycarbonic acid by using diphenyl carbonate and aliphatic dihydric alcohol as raw materials through two-step melt transesterification and polycondensation reactions. Background technique [0002] In order to deal with the "white pollution" caused by waste plastics and industrial CO 2 The two major environmental problems of the "greenhouse effect" caused by emissions, the synthesis of CO under the action of a catalyst 2 Base polymers have become an important research direction in the chemical industry, and some processes have been industrialized. Take industrial waste gas CO 2 Synthesizing biodegradable plastics as raw materials not only solves the problem of greenhouse gas CO 2 In addition, it has found an inexhaustible source of raw materials for the manufacture of new biodegradable polymer materi...

Claims

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Application Information

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IPC IPC(8): C08G64/30C08G64/02
Inventor 王公应王自庆杨先贵刘绍英姚洁张华
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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