A green preparation process of 3,5,5-trimethyl-3-cyclohexen-1-one

A preparation process, the technology of cyclohexene, which is applied in the field of preparation process of alkaline ionic liquid to catalyze the synthesis of β-IP, can solve the problems that the catalyst cannot be recycled, the space-time yield is not high, and the environmental pollution is large, so as to achieve high isomerization selectivity , solve the separation problem and reduce the effect of three wastes

Active Publication Date: 2016-07-06
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process uses alkaline ionic liquid as a catalyst, which has the advantages of high product yield, easy recovery of catalyst, environmental protection, and easy realization of industrial production. Many by-products, serious equipment corrosion, serious environmental pollution and other problems

Method used

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  • A green preparation process of 3,5,5-trimethyl-3-cyclohexen-1-one

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Embodiment 1

[0033] Preparation method of alkaline ionic liquid used in the present invention

[0034] The anion potassium salt (K + B — , Purchased from Bailingwei Technology), added to ionic liquid bromide (A + Br — , Purchased from Shanghai Chengjie Chemical Co., Ltd.) in methylene chloride solution, stirred vigorously at room temperature for 10 hours, and then the precipitate potassium bromide (KBr) was filtered off. The filtrate was subjected to rotary evaporation to remove the solvent, and then washed with ether for 3 times, and finally dried at 90°C for 10 hours to obtain the corresponding ionic liquid (A + B — ).

Embodiment 2

[0036] The α-IP raw material containing 0.05wt% alkaline ionic liquid catalyst IL-A is added to the tower reactor of the tower, and the rectification reaction is carried out under the conditions of 210°C and 0.9 Bar, and the α-IP isomerization reaction occurs and stays The reaction time is 24 hours, the reaction selectivity is 99.7%, and the crude product β-IP (purity: 94 wt%) is collected at the top of the tower. The crude product β-IP is subjected to a pressure of 1.5KPa, 30 plates, and a reflux ratio of 3:1, and further vacuum distillation to obtain a product β-IP with a purity of 99.5% by weight. The gas analysis spectrum is shown in Figure 1. .

Embodiment 3-10

[0038] On the basis of Example 2, the type and amount of catalyst, temperature, pressure, and reaction time were changed. The results are shown in Table 1.

[0039] Among them, the structural formulas of the catalysts IL-F, IL-G and IL-H are respectively

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Abstract

The invention discloses a synthetic process of 3,5,5-trimethyl-3- cyclohexene-1-ketone. The synthetic process is characterized by comprising the following steps: by taking 3,5,5-trimethyl-2- cyclohexene-1-ketone (alpha-IP) as a raw material and taking a basic ionic liquid as a catalyst and adopting a reactive distillation technology, performing isomerization reaction to prepare 3,5,5-trimethyl-3-cyclohexene-1-ketone (alpha-IP), wherein the reaction absolute pressure is 0.2-2Bar, the reaction temperature is 150-230 DEG C, the purity of the product beta-IP can reach 99.5wt%-99.8wt%, and the reaction selectivity can reach 99.2%-99.9%. The process has the advantages of high selectivity, no alkali separation, easy catalyst recycling, and the like, and is an environment-friendly synthetic process.

Description

Technical field [0001] The present invention relates to a green preparation process of 3,5,5-trimethyl-3-cyclohexen-1-one (β-IP), in particular to a preparation process for the catalytic synthesis of β-IP by an alkaline ionic liquid. Background technique [0002] 3,5,5-Trimethyl-3-cyclohexen-1-one (β-IP) is an important intermediate for the synthesis of natural products such as vitamin E, carotenoids, astaxanthin 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 preparation of trimethyl hydroquinone (VE main ring ) Of the precursor. [0003] β-IP and 3,5,5-trimethyl-2-cyclohexen-1-one (α-IP) are a pair of isomers. There is an isomeric equilibrium under the catalysis of acid or base, β- IP can be prepared by the isomerization reaction of α-IP. But because β-IP is an unstable structure, its equilibrium concentration is very low, and it needs continuous extraction to brea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/603C07C45/67
CPCC07B2200/09C07C45/67C07C45/82C07C2601/16C07C49/603Y02P20/10Y02P20/584
Inventor 张涛郭劲资董岩峰崔乾王鹏丛鑫何光文陈海波黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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