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Method for preparing 3,5,5-trimethyl-3-cyclohexene-1-one

A technology of cyclohexene and trimethyl, which is applied in the field of preparation of 3,5,5-trimethyl-3-cyclohexen-1-one, can solve the problem of excessive catalyst consumption, low space-time yield, Avoid problems such as strong corrosion of equipment, achieve high isomerization selectivity, reduce the generation of by-products, and reduce the effects of three wastes

Active Publication Date: 2017-09-29
WANHUA CHEM GRP CO LTD
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  • 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

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  • Method for preparing 3,5,5-trimethyl-3-cyclohexene-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, at a temperature of 210°C in the tower reactor, 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 (purity in gas phase 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 obtains the product β-IP with a purity of 99.5wt%, and the tower top temperature 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 still, pressure, reflux ratio, residence time, the results are shown in Table 1.

[0054] Table 1

[0055]

[0056]

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Abstract

The invention discloses a method for preparing 3,5,5-trimethyl-3-cyclohexene-1-one. The method comprises the following steps: taking 3,5,5-trimethyl-2-cyclohexene-1-one (alpha-IP) as a raw material, taking preazophosphorine as a catalyst, and carrying out an isomerization reaction by adopting a reactive distillation technique, thereby obtaining the 3,5,5-trimethyl-3-cyclohexene-1-one (beta-IP). The purity of the product beta-IP can reach 99.5-99.8wt%, and the reaction selectivity can reach 99.2-99.9%. The process has the advantages of small catalyst usage amount, high selectivity, avoidance of alkaline separation, less high-boiling residues and the like and a high-efficiency synthetic 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

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Application Information

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Patent Type & Authority Applications(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
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