A continuous refining method and device for high-purity ε-caprolactone

A caprolactone, high-purity technology, applied in the direction of sustainable manufacturing/processing, climate sustainability, organic chemistry, etc., can solve the problems of not meeting the requirements of polycaprolactone application, large difference in boiling point, etc.

Active Publication Date: 2021-08-20
安徽卓泰化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The boiling points of benzoic acid and ε-caprolactone are quite different, so this method ignores the difficulty in the separation process of ε-caprolactone
And obtaining ε-caprolactone with a purity of 99% also fails to meet the requirements of polycaprolactone in medical applications

Method used

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  • A continuous refining method and device for high-purity ε-caprolactone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A continuous refining method for high-purity ε-caprolactone comprises a refining system composed of a reactive distillation column and an azeotropic distillation column. The ε-caprolactone from the ε-caprolactone raw material tank is added from the middle of the reactive distillation tower T101, and the polycarbonate alcohol from the polycarbonate alcohol circulation tank V101 is added from the lower part of the tower. After the countercurrent contact between the polycarbonate alcohol and ε-caprolactone A self-catalyzed esterification reaction occurs, unreacted polycarbonate alcohols, low-boiling-point esters produced by the reaction and water in the raw materials are evaporated from the top of the tower and then enter the top condenser E101 of T101. The raw material of boiling distillation column T102, the bottom side line of T101 extracts ε-caprolactone with a purity ≥ 99.95%, and the bottom of the tower extracts high-boiling point esters generated by the reaction and ...

Embodiment 2

[0043] A continuous refining method for high-purity ε-caprolactone comprises a refining system composed of a reactive distillation column and an azeotropic distillation column. The ε-caprolactone from the ε-caprolactone raw material tank is added from the middle of the reactive distillation tower T101, and the polycarbonate alcohol from the polycarbonate alcohol circulation tank V101 is added from the lower part of the tower. After the countercurrent contact between the polycarbonate alcohol and ε-caprolactone A self-catalyzed esterification reaction occurs, unreacted polycarbonate alcohols, low-boiling-point esters produced by the reaction and water in the raw materials are evaporated from the top of the tower and then enter the top condenser E101 of T101. The raw material of boiling distillation column T102, the bottom side line of T101 extracts ε-caprolactone with a purity ≥ 99.95%, and the bottom of the tower extracts high-boiling point esters generated by the reaction and ...

Embodiment 3

[0050] A continuous refining method for high-purity ε-caprolactone comprises a refining system composed of a reactive distillation column and an azeotropic distillation column. The ε-caprolactone from the ε-caprolactone raw material tank is added from the middle of the reactive distillation tower T101, and the polycarbonate alcohol from the polycarbonate alcohol circulation tank V101 is added from the lower part of the tower. After the countercurrent contact between the polycarbonate alcohol and ε-caprolactone A self-catalyzed esterification reaction occurs, unreacted polycarbonate alcohols, low-boiling-point esters produced by the reaction and water in the raw materials are evaporated from the top of the tower and then enter the top condenser E101 of T101. The raw material of boiling distillation column T102, the bottom side line of T101 extracts ε-caprolactone with a purity ≥ 99.95%, and the bottom of the tower extracts high-boiling point esters generated by the reaction and ...

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Abstract

The present invention proposes a continuous refining method and device for high-purity ε-caprolactone. The present invention proposes a continuous refining method for high-purity ε-caprolactone, using refined ε-caprolactone as raw material, Using multi-carbon alcohols as entraining agents, in the reactive distillation column, poly-carbon alcohols, polybasic acids, and hydroxycaproic acid undergo autocatalytic reactions to generate corresponding esters, thereby changing the difficulty of separation from ε-caprolactone, and The azeotropic property of water and polycarbonate alcohols can also effectively separate water and ε‑caprolactone. Effectively remove water, polyacids and hydroxycaproic acid from ε-caprolactone through reactive distillation-azeotropic distillation. This process is simple and easy to implement, and can realize continuous production of high-purity ε-caprolactone. The purity of the obtained ε-caprolactone is ≥99.95%, and the yield is ≥99%. Not only can the polycaprolactone produced by ε-caprolactone be used in the medical field, but also greatly improve the economic and social benefits of the enterprise.

Description

technical field [0001] The invention relates to the field of refining ε-caprolactone, in particular to a continuous refining method and device for high-purity ε-caprolactone. Background technique [0002] ε-caprolactone is a non-toxic organic chemical intermediate, which is mainly used as a monomer to prepare high-performance polymers, while polycaprolactone has shape memory. The phenomenon that the treatment of external conditional stimuli can restore its original shape. On the other hand, polycaprolactone materials are blended with materials such as starch to produce completely biodegradable materials. At present, the characteristics of these two aspects have been applied in many fields, especially in the medical field, such as adhesive tapes, bandages, correctors, sutures, drug release agents, etc. ε-caprolactone can also be used as a good solvent and has good solubility for some polymer materials. As a monomer, ε-caprolactone is mainly used to produce thermoplastic po...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D313/04
CPCC07D313/04Y02P20/10
Inventor 刘杨林鹏增彭宏岳文娣
Owner 安徽卓泰化工科技有限公司
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