Eureka AIR delivers breakthrough ideas for toughest innovation challenges, trusted by R&D personnel around the world.

A method for preparing 3,5,5-trimethyl-3-cyclohexen-1-one

A cyclohexene and trimethyl technology, which is applied in the field of preparation of 3,5,5-trimethyl-3-cyclohexene-1-one, can solve the problem of excessive catalyst dosage, low space-time yield, Strong corrosion of equipment, etc., to achieve high isomeric selectivity, reduce the generation of by-products, and reduce the effects of three wastes

Active Publication Date: 2020-07-28
WANHUA CHEM GRP CO LTD
View PDF11 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process uses pre-nitrogen phosphatine as a catalyst, which has the advantages of less catalyst consumption, high yield, green environmental protection, and easy realization of industrial production, and solves the problems of low space-time yield and excessive catalyst consumption in the prior art. , many by-products, strong corrosion of equipment and other problems

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
  • A method for preparing 3,5,5-trimethyl-3-cyclohexen-1-one
  • A method for preparing 3,5,5-trimethyl-3-cyclohexen-1-one
  • A method for preparing 3,5,5-trimethyl-3-cyclohexen-1-one

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Add the α-IP raw material containing 0.05wt% pre-nitrogen phosphatrane catalyst IL-A to the tower reactor of the tower reactor, and the temperature of the tower reactor is 210 ° C, the number of theoretical plates is 30, and the reflux ratio is 3:1. Reactive distillation was carried out under the condition of 0.9 Bar absolute pressure in the reactor, α-IP isomerization reaction occurred, the reaction selectivity was 99.7%, and the crude product β-IP was collected at the top of the tower (the gas phase purity was 70wt%). The crude product β-IP is 1.5kPa in absolute pressure, the number of theoretical plates is 30, and the reflux ratio is 3:1, further vacuum distillation to obtain the product β-IP with a purity of 99.5wt%, and the temperature at the top of the column is 100 ℃.

Embodiment 2-10 and Embodiment 11

[0052] Embodiment 2-10 and embodiment 11 (comparative example)

[0053] On the basis of Example 1, change the catalyst type and consumption, the number of theoretical plates of the reactive distillation column reactor, the temperature of the tower bottom, pressure, reflux ratio, residence time, the results are shown in Table 1.

[0054] Table 1

[0055]

[0056]

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

A kind of preparation method of 3,5,5-trimethyl-3-cyclohexene-1-ketone: with 3,5,5-trimethyl-2-cyclohexene-1-ketone (α-IP) As a raw material, the former nitrogen phosphatrane base is used as a catalyst, and reactive distillation technology is used to carry out isomerization reaction to prepare 3,5,5-trimethyl-3-cyclohexene-1-ketone (β-IP), product β The purity of ‑IP can reach 99.5wt%‑99.8wt%, and the reaction selectivity can reach 99.2%‑99.9%. The process has the advantages of less catalyst consumption, high selectivity, no alkali precipitation, less high boiling matter, etc., and is an efficient synthesis process.

Description

technical field [0001] The present invention relates to a preparation method of 3,5,5-trimethyl-3-cyclohexen-1-one (β-IP), in particular to the 3,5,5-trimethyl-3,5,5-trimethacrylate catalyzed by pro-nitrophosphatrane base A method for preparing 3,5,5-trimethyl-3-cyclohexen-1-one through isomerization of base-2-cyclohexen-1-one (α-IP). Background technique [0002] 3,5,5-Trimethyl-3-cyclohexen-1-one (β-IP) is an important intermediate for the synthesis of vitamin E, carotenoids, astaxanthin and other natural products and spices, especially The main raw material for the preparation of tea aroma ketone (2,6,6-trimethyl-2-cyclohexene-1,4-dione, KIP), tea aroma ketone is also the main raw material for the preparation of trimethylhydroquinone (VE main ring ) precursor. [0003] β-IP and α-IP are a pair of isomers, there is isomerism equilibrium under acid or base catalysis, β-IP can be prepared by isomerization reaction of α-IP. However, since β-IP is an unstable structure, its...

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): C07C45/67C07C49/647B01J31/02
CPCB01J31/0264B01J2231/52C07C45/67C07C49/647Y02P20/10
Inventor 张涛郭劲资程晓波吕英东张旭林龙朱龙龙王延斌黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
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