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A kind of preparation method of β-isophorone

A technology of isophorone and trimethyl, which is applied in the preparation of organic compounds, carbon-based compounds, chemical instruments and methods, etc., can solve the problems of high content of β-IP-2, affecting the quality of downstream VE, and low production efficiency. Advanced problems, to achieve the effect of stable catalytic system, low catalyst consumption and easy operation

Active Publication Date: 2022-07-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] To sum up, most of the current processes have the following deficiencies: 1) The amount of catalyst is too large, and the production efficiency is not high; 2) The content of high boilers and key impurities β-IP-2 is too high, which affects the quality of downstream VE; 3) Inorganic acids or alkalis are used as catalysts, which are prone to salting out and require high material requirements

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0029] Add the α-IP raw material containing 0.05wt% n-hexanoic acid+cyclohexylamine (mol ratio is 1:1) catalyst to the tower reactor tower reactor, at the tower reactor temperature 210 ℃, the number of theoretical plates is 30, and the reflux ratio is 30:1, reactive distillation was carried out under the condition of absolute pressure of 0.9Bar in the tower reactor, α-IP isomerization reaction occurred, and the reaction selectivity was 99.7%, and β-IP (gas phase purity was 97.0wt%) was collected from the top of the tower. ).

Embodiment 2-10 and Embodiment 11

[0030] Example 2-10 and Example 11 (comparative example)

[0031] On the basis of Example 1, the catalyst type and amount, the theoretical plate number of the reactive distillation column reactor, the temperature of the tower kettle, the pressure, the reflux ratio, and the residence time were changed. The results are shown in Table 1.

Embodiment 11

[0032] Example 11 (comparative example)

[0033] catalyst The preparation method:

[0034] Add potassium carbonate to in dichloromethane solution (the molar ratio of the two is 1:2), vigorously stirred at room temperature for 10 hours, and then the precipitated potassium bromide (KBr) was filtered off. The filtrate was evaporated to remove the solvent, washed three times with ether, and finally dried at 90 °C for 10 h to obtain the corresponding ionic liquid.

[0035] Table 1

[0036]

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Abstract

A preparation method of β-isophorone, using 3,5,5-trimethyl-2-cyclohexene-1-ketone (α-IP) as raw material, using acid-base co-catalyst, reacting rectifying technology to carry out isomerization reaction to prepare 3,5,5-trimethyl-3-cyclohexene-1-ketone (β-IP), the purity of the product β-IP can reach 99.9wt%, and the reaction selectivity can reach 99.5%‑99.9%. The process has the advantages of easy availability of catalyst, high reaction efficiency, low content of key impurities and no alkali precipitation, and is an efficient synthesis process.

Description

technical field [0001] The invention relates to a preparation method of β-isophorone, in particular to the preparation of 3,5,5,5,5,5,5 by isomerization of 3,5,5-trimethyl-2-cyclohexen-1-one (α-IP). Method for 5-trimethyl-3-cyclohexen-1-one. Background technique [0002] β-Isophorone, or 3,5,5-trimethyl-3-cyclohexen-1-one, or β-IP for short, is an important intermediate in the production of many nutritional chemicals and fragrances, such as vitamin E, Carotenoids and tea ketones. Among them, the most important application field is the synthesis of vitamin E, which is an innovative route of domestic vitamin E production, breaking the limitation of foreign raw materials. [0003] For the production of β-IP, α-IP is generally used as the raw material, and is prepared by reactive distillation process. Under catalytic conditions, α-IP and β-IP are in isomeric equilibrium. Since β-IP is a relatively unstable structure, its equilibrium concentration is very low, but the differen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/67C07C49/603
CPCC07C45/67C07C2601/16C07C49/603Y02P20/10
Inventor 张涛宋明焱郭劲资程晓波吕英东张旭林龙朱龙龙王延斌黎源
Owner WANHUA CHEM GRP CO LTD
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