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

Method for synthesizing ε-caprolactone

A technology of caprolactone and cyclohexanone, which is applied in the continuous process field of synthesizing ε-caprolactone, can solve the problems of difficulty in large-scale production, high separation cost, and long process flow, so as to avoid the decline of product yield and high Conversion rate, high selectivity effect

Active Publication Date: 2021-12-28
CHINA PETROLEUM & CHEM CORP +1
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese patent CN 103539770 A discloses a microchannel reaction technology for preparing ε-caprolactone based on the oxidation of cyclohexanone with peracetic acid, and Chinese patent CN 106279093 A discloses a method for preparing ε-caprolactone based on the oxidation of cyclohexanone with m-chloroperoxybenzoic acid. For the microchannel reaction technology of ε-caprolactone, the above two processes need to prepare peroxyacid first and then use peroxyacid to oxidize cyclohexanone. The process is relatively long, and the organic acid after the reaction must be separated and recovered. For the re-preparation of peroxyacid, the separation cost is relatively high, and it is difficult in large-scale production

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 synthesizing ε-caprolactone
  • Method for synthesizing ε-caprolactone
  • Method for synthesizing ε-caprolactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Use a metering pump to transport the aqueous phase raw material containing oxidant and catalyst, wherein the mass fraction of hydrogen peroxide is 40%, the mass fraction of catalyst is 1.5%, and the molar ratio of oxalic acid and sodium tungstate in the catalyst is 1.0; The oil phase raw material, wherein the water-carrying agent toluene mass fraction is 50%. The molar ratio of the oxidant in the water phase raw material to the cyclohexanone in the oil phase raw material is 3.5, and the two streams of materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50°C. The liquid at the outlet of the micro-mixer enters the micro-reactor as a liquid-phase raw material through the connecting pipeline, enters the micro-reactor through the liquid-phase raw material inlet, and contacts with the air entering from the lower gas-phase inlet in countercurrent to carry out the cyclohexanone oxidation reaction. The heating medium in the tube wall provides ...

Embodiment 2

[0016] Use a metering pump to transport the aqueous phase raw material containing oxidant and catalyst, wherein the mass fraction of hydrogen peroxide is 30%, the mass fraction of catalyst is 1.5%, and the molar ratio of oxalic acid to sodium tungstate in the catalyst is 1.0; The oil phase raw material, wherein the water-carrying agent toluene mass fraction is 50%. The molar ratio of the oxidizing agent in the water phase raw material to the cyclohexanone in the oil phase raw material is 3.5, and the two streams of materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50°C. The liquid at the outlet of the micro-mixer enters the micro-reactor as a liquid-phase raw material through the connecting pipeline, enters the micro-reactor through the liquid-phase raw material inlet, and contacts with the air entering from the lower gas-phase inlet in countercurrent to carry out the cyclohexanone oxidation reaction. The heating medium in the tube wall pr...

Embodiment 3

[0018]Use a metering pump to transport the aqueous phase raw material containing oxidant and catalyst, wherein the mass fraction of peracetic acid is 15%, the mass fraction of catalyst is 1.5%, and the molar ratio of oxalic acid and sodium tungstate in the catalyst is 1.0; The oil phase raw material of the water agent, wherein the toluene mass fraction of the water agent is 50%. The molar ratio of the oxidizing agent in the water phase raw material to the cyclohexanone in the oil phase raw material is 3.5, and the two streams of materials are respectively preheated by a preheater and fully mixed in a micro mixer at 50°C. The liquid at the outlet of the micro-mixer enters the micro-reactor as a liquid-phase raw material through the connecting pipeline, enters the micro-reactor through the liquid-phase raw material inlet, and contacts with the air entering from the lower gas-phase inlet in countercurrent to carry out the cyclohexanone oxidation reaction. The heating medium in th...

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

PropertyMeasurementUnit
porosityaaaaaaaaaa
porosityaaaaaaaaaa
porosityaaaaaaaaaa
Login to View More

Abstract

The invention discloses a method for synthesizing ε-caprolactone, which comprises making the water-phase raw material containing a homogeneous catalyst of sodium tungstate and an oxidant and the oil-phase raw material containing cyclohexanone and a water-carrying agent, in a micro-mixer In the mixing process, the obtained liquid-phase raw materials and gas-phase raw materials continue to undergo the reaction separation coupling process in the microreactor to obtain the step of ε-caprolactone, and use a low-concentration oxidant to oxidize cyclohexanone in one step, without the technical scheme of preparing peroxyacid , which better solves the problem of the safety of the reaction process in the prior art, and can be used in the field of strengthening the coupling process of mixed reactions by microchannel technology.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and in particular relates to a continuous process for synthesizing ε-caprolactone in a micro-reaction device using cyclohexanone and hydrogen peroxide as raw materials. Background technique [0002] ε-caprolactone is an environmentally friendly polyester monomer, mainly used for the synthesis of polycaprolactone, a polymer material with unique biocompatibility, biodegradability and good permeability, and can also be used as a modified material Copolymerization with other polymer monomers or blending with polymer materials to improve its gloss, transparency, biodegradability and anti-adhesive properties, etc., is a fine chemical with a very broad market application prospect in recent years. [0003] At present, the production method of ε-caprolactone in the world is mainly peroxyacid oxidation method, that is, using peroxyacid as an oxidant to oxidize cyclohexanone to synthesi...

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 Patents(China)
IPC IPC(8): C07D313/04B01J19/00
CPCC07D313/04B01J19/0093B01J2219/00873
Inventor 储博钊钟思青何乐路马俊
Owner CHINA PETROLEUM & CHEM CORP
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