Preparation method of polycaprolactone

A technology of polycaprolactone and hydroxycaproate, which is applied in the field of preparation of polycaprolactone, can solve the problems of raw material pollution, high production cost, unfavorable environmental protection and construction safety, and achieve environmental friendliness, low cost, Conducive to the effect of environmental protection and circular economy

Active Publication Date: 2022-02-15
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the invention is to provide a preparation method of polycaprolactone to solve the problem that the current preparation method for polycaprolactone is a high temperature and high pressure environment, high temperature operation is not conducive to environmental protection and construction safety, high production cost, and the use of The technical problem that the raw material has the risk of polluting the environment

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0020] The application provides a preparation method of polycaprolactone, comprising the steps of: adding a solvent to the raw material, hydrolyzing it under acidic conditions to form a 6-hydroxycaproate solution, and dissolving the 6-hydroxycaproate solution under vacuum pressure Remove water and solvent at one temperature in the environment, and polycondensation of 6-hydroxycaproic acid salt occurs at the same time, and adjust according to different molecular weights to obtain polycaprolactone with a molecular weight greater than 60,000 and preferably less than 100,000,000. After the polymerization reaction material is cooled Add acid to make it neutral, separate the lower layer of water after static layering and remove it, wash the oil phase with water, heat up after passing the test, vacuum dehydrate and dry to obtain the finished product of polycaprolactone.

[0021] In the examples of the present application, the raw materials include recycled polycaprolactone, polycaprol...

Embodiment 1

[0041] Weigh 300g of recovered polycaprolactone, add 100g of ethylene glycol, 50g of 30% sodium hydroxide aqueous solution, reflux at 100°C for 5h, then turn on the vacuum, heat to 110°C for dehydration and ethylene glycol solvent for 5h, then heat up to 180°C ℃, react for 10 hours, and polycaprolactone with a molecular weight greater than 60,000 can be obtained. After the polymerization reaction material is cooled down, acid is added to make it neutral. A finished product of polycaprolactone is obtained.

Embodiment 2

[0043] Weigh 300g of recovered polycaprolactone polyol, add 100g of ethylene glycol, 50g of 30% sodium hydroxide aqueous solution, reflux at 100°C for 3h, then turn on the vacuum, heat to 110°C for dehydration and ethylene glycol solvent for 5h, then raise the temperature Reaction at 190°C for 10 hours to obtain polycaprolactone with a molecular weight greater than 65,000. After the polymerization reaction material is cooled down, acid is added to make it neutral. After static layering, the lower layer of water is separated to remove sewage. Dehydration and drying to obtain the finished polycaprolactone.

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PUM

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Abstract

The invention discloses a preparation method of polycaprolactone. The preparation method comprises the following steps: adding a solvent into a raw material, hydrolyzing under an acidic or alkaline condition to form a 6-hydroxy hexanoate solution, removing water and the solvent from the 6-hydroxy hexanoate solution in a vacuum pressure environment at a temperature, carrying out 6-hydroxy hexanoate polycondensation at the same time, adjusting according to different molecular weights to obtain polycaprolactone with a molecular weight greater than 60,000, cooling the polymerization reaction materials, adding an acid to adjust the materials to be neutral, standing for layering, separating out and removing lower-layer water, washing an oil phase with water, heating after the oil phase is qualified, and performing vacuum dehydration and drying to obtain a polycaprolactone finished product. According to the method, waste generated in the production and use process of numerous caprolactone downstream products can be converted into degradable polycaprolactone products, the cost is low, recycling of the caprolactone downstream waste is achieved, environmental protection and circular economy are facilitated, and the yield of polycaprolactone is increased.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a preparation method of polycaprolactone. Background technique [0002] Polycaprolactone (Polycaprolactone, PCL), also known as polyε-caprolactone, is a high molecular organic polymer formed by ring-opening polymerization of ε-caprolactone monomer under the catalysis of a metal anion complex catalyst. conditions, different molecular weights can be obtained. Its appearance is white solid powder, non-toxic, insoluble in water, soluble in many polar organic solvents. PCL has good biocompatibility, good organic polymer compatibility, and good biodegradability. It can be used as a cell growth support material and is compatible with a variety of conventional plastics. 6-12 in the natural environment Months can be completely degraded. In addition, PCL also has good shape memory temperature control properties, and is widely used in the production and processing of drug car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/78C08G63/08
CPCC08G63/78C08G63/08Y02W30/62
Inventor 谢传欣谢玉玲谢博
Owner QINGDAO UNIV OF SCI & TECH
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