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A kind of microwave-assisted depolymerization method of polycaprolactone polyol

A polycaprolactone and microwave-assisted technology, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of waste of resources and achieve the effect of mild conditions and simple separation process

Active Publication Date: 2016-01-20
安徽红太阳新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The PCL synthesis industry is currently in a stage of rapid development, and the consumption is increasing day by day. If it is not recycled reasonably, it will cause huge waste of resources in the future
There is no report on the research on the degradation and recovery of PCL

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Put 20g of polycaprolactone polyol and 20g of diethanolamine into the reactor after mixing, and react under the condition that the reaction temperature is 200°C, the reaction pressure is 2.5Mpa and the power of microwave radiation is 550W. After reacting for 60min, cool In the reactor, the temperature of the reaction product was lowered to 0° C., unreacted PCL polyester and diethanolamine crystallized, and 15.7 g of the liquid was separated. The content of ε-caprolactone monomer in the liquid detected by gas chromatography was 92.1%, the content of ethylene glycol was 3.4%, and the recovery rate of ε-caprolactone was 72.3%.

Embodiment 2

[0020] 20g of polycaprolactone polyol and 30g of diethanolamine are mixed and put into the reactor. The reaction is carried out under the conditions that the reaction temperature is 220°C, the reaction pressure is 2.5Mpa and the power of microwave radiation is 600W. After reacting for 70 minutes, the reactor was cooled, and the temperature of the reaction product was lowered to 0° C., unreacted PCL polyester and diethanolamine crystallized, and 17.8 g of liquid was separated. The content of ε-caprolactone monomer in the liquid detected by gas chromatography was 91.9%, the content of ethylene glycol was 2.7%, and the recovery rate of ε-caprolactone was 81.8%.

Embodiment 3

[0022] 20g of polycaprolactone polyol and 30g of diethanolamine are mixed and put into the reactor. The reaction is carried out under the conditions that the reaction temperature is 240°C, the reaction pressure is 3.0Mpa and the microwave radiation power is 600W. After reacting for 80 minutes, the reactor was cooled, and the temperature of the reaction product was lowered to 0° C., unreacted PCL polyester and diethanolamine crystallized, and 16.7 g of liquid was separated. The content of ε-caprolactone monomer in the liquid detected by gas chromatography was 92.1%, the content of ethylene glycol was 3.6%, and the recovery rate of ε-caprolactone was 76.9%.

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PUM

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Abstract

The invention discloses a microwave-assisted depolymerizing method for polycaprolactone polyhydric alcohol and belongs to the technical field of chemical engineering. The method includes the steps that polycaprolactone polyhydric alcohol and diethanol amine are mixed, and then react on the conditions that the temperature is 150-250 DEG C, the pressure is 1-3 Mpa and microwave irradiation is achieved. Monomers can be separated from a depolymerizing agent through low temperature crystallization after the mixture reacts, and the monomers generated through depolymerization can be recycled as chemical materials. According to the microwave-assisted depolymerizing method, the conditions are mild and the separation process is simple.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a microwave-assisted depolymerization method of polycaprolactone polyol. Background technique [0002] Polyε-caprolactone polyol (PCL) is composed of caprolactone monomer, initiator (diol, diamine and alcohol amines), catalyst (tetrabutyl titanate, tetraisopropyl titanate, octanoic acid Sn, etc.) formed by ring-opening polymerization. PCL is mainly used in elastomers, coatings, adhesives, etc., and can improve the performance of coatings, elastomers, and adhesives in many aspects such as wear resistance and hydrolysis resistance. In addition, it is an ideal biomedical material, and its biodegradability has important value in environmental protection and medical applications. [0003] The synthesis of ε-caprolactone has high technical requirements and great difficulty due to the quality, stability and safety of raw materials. In addition, during the synthe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D313/04C07C31/20C07C29/00
CPCC07C29/00C07D313/04C07C31/202
Inventor 李健周建华孙兰娟黎广郭畅葛九敢陈新春
Owner 安徽红太阳新材料有限公司