Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for preparing epsilon-caprolactone by using micro-reaction device

A technology of micro-reaction device and caprolactone, which is applied in the direction of organic chemistry, can solve the problems of low yield, difficult to control the reaction, and high cost, and achieve the effects of reducing production cost, improving quality, and reducing content

Inactive Publication Date: 2017-01-04
NANJING UNIV OF TECH
View PDF8 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved in the present invention is to provide a method for preparing ε-caprolactone by means of a micro-reaction device, so as to solve the problems in the prior art that the reaction is difficult to control, the cost is too high and the yield is low.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing epsilon-caprolactone by using micro-reaction device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Dissolve m-chloroperoxybenzoic acid and cyclohexanone in ethyl acetate respectively, the molar ratio of m-chloroperoxybenzoic acid and cyclohexanone is 1.2:1; And cyclohexanone are pumped into the micro-mixer in the micro-reaction device at the same time, the flow rate is 0.5ml / min and 0.5ml / min respectively; after thorough mixing, the mixed system is passed into the micro-structure reactor for reaction, and the reaction temperature is 30°C , the reaction residence time is 10min; after the reaction is completed, collect the product (reaction solution), wash the organic phase to pH=7.0 with 5wt% sodium carbonate solution and distilled water respectively, collect the organic phase, and then use an organic solvent to carry out the above-mentioned aqueous phase Extraction, the organic extract is combined with the organic phase, the solvent is removed by rotary evaporation, and the target product ε-caprolactone is obtained; a certain amount of acid is added to the aqueous pha...

Embodiment 2

[0033]Dissolve m-chloroperoxybenzoic acid and cyclohexanone in ethyl acetate respectively, the molar ratio of m-chloroperoxybenzoic acid and cyclohexanone is 1.7:1; and cyclohexanone are pumped into the micro-mixer in the micro-reaction device at the same time, the flow rates are 1.172ml / min and 0.828ml / min respectively; after thorough mixing, the mixed system is passed into the micro-structure reactor for reaction, and the reaction temperature is 80°C , the reaction residence time is 5min; after the reaction is completed, collect the product (reaction solution), wash the organic phase to pH=7.0 with 5wt% sodium carbonate solution and distilled water respectively, collect the organic phase, and then use an organic solvent to carry out the above-mentioned water phase Extraction, the organic extract is combined with the organic phase, the solvent is removed by rotary evaporation, and the target product ε-caprolactone is obtained; a certain amount of acid is added to the water pha...

Embodiment 3

[0035] Dissolve m-chloroperoxybenzoic acid and cyclohexanone in dichloromethane respectively, and the molar ratio of m-chloroperoxybenzoic acid and cyclohexanone is 2:1; dissolve m-chloroperoxybenzoic acid in ethyl acetate and cyclohexanone are pumped into the micro-mixer in the micro-reaction device at the same time, the flow rates are 1.25ml / min and 0.75ml / min respectively; after thorough mixing, the mixed system is passed into the micro-structure reactor for reaction, and the reaction temperature is 100°C , the reaction residence time is 5min; after the reaction is completed, collect the product (reaction solution), wash the organic phase to pH=7.0 with 5wt% sodium carbonate solution and distilled water respectively, collect the organic phase, and then use an organic solvent to carry out the above-mentioned water phase Extraction, the organic extract is combined with the organic phase, the solvent is removed by rotary evaporation, and the target product ε-caprolactone is obt...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for preparing epsilon-caprolactone by using a micro-reaction device. The epsilon-caprolactone is prepared from meta-chloroperbenzoic acid and ethyl acetate as raw materials by using a micro-channel reaction technique. Compared with the prior art, the method adopts the micro-reaction device for synthesizing the epsilon-caprolactone, so that problems of conventional production can be overcome, the raw material conversion rate can be increased, the reaction time can be shortened, the content of byproducts can be reduced, the process procedures are simplified, circulation of an oxidant can be achieved, the production cost can be lowered, the production process security of the epsilon-caprolactone can be greatly improved, the product quality can be improved, and the industrial production can be facilitated.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for preparing ε-caprolactone by utilizing a micro-reaction device. Background technique [0002] ε-caprolactone is an important organic synthesis intermediate, mainly used for the synthesis of polycaprolactone and copolymerization or blending modification with other esters; ε-caprolactone can also be used as a strong solvent to dissolve many Polymer resin, which has good solubility for some insoluble resins, such as it can dissolve chlorinated polyolefin resin and "ESTANE" polyurethane resin. Among them, polycaprolactone (PCL) is a linear aliphatic polyester obtained by ring-opening polymerization of ε-caprolactone (ε-CL). Due to its superior biodegradability and memory, polycaprolactone has been used in many fields, especially in medical treatment, such as adhesive tapes, bandages, correctors, sutures, drug release agents, etc. Therefore, ε-caprolactone h...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07D313/04
CPCC07D313/04
Inventor 郭凯田启涛方正朱宁李昕万力张锴欧阳平凯
Owner NANJING UNIV OF TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com