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A kind of technique for continuous synthesis of β-isophorone

A technology of isophorone and process, which is applied in the field of chemical intermediate preparation, can solve the problems of low catalytic efficiency of acidic ceramic materials, non-recyclable catalyst, large amount of acidic ceramic materials, etc., achieves convenient recovery and activation, and improves contact Area and residence time, recycling and regenerating convenient effects

Active Publication Date: 2017-01-04
ZHEJIANG NHU PHARMA +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Many patents have reported the method for synthesizing β-isophorone by isomerization of α-isophorone, but there are many shortcomings: mainly, the catalyst cannot be regenerated, the space-time yield is not high, and by-products accumulate a lot
The disadvantage of this method is: there are many reaction by-products, which are isophorone self-condensation products; the conversion rate is not high, and the catalyst is not easy to recycle.
This synthetic method promotes the reaction to the β-isophorone by constantly steaming out the β-isophorone, and the conversion rate of the reaction is high. However, the consumption of acidic ceramic materials in this synthetic method is too large, and the unit dosage The catalytic efficiency of the acidic ceramic material is not high, and the acidic ceramic material is fixed to the packing section of the reactor. When the catalyst needs to be regenerated, the entire reactor needs to be disassembled, and the operation is very inconvenient.
At the same time, when this method is used for rectification, because the acidic ceramics are solidly loaded in the packing section, there will be a certain air resistance, which restricts the rectification efficiency.

Method used

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  • A kind of technique for continuous synthesis of β-isophorone
  • A kind of technique for continuous synthesis of β-isophorone
  • A kind of technique for continuous synthesis of β-isophorone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In the tower reactor, add 600g of α-isophorone and 5g (mass ratio 0.83%) of 3A molecular sieve catalyst, and carry out isomerization reaction at 210-240°C, with a reaction pressure of 0.05MPa. β-isophorone was collected at the top for subsequent vacuum distillation treatment, and finally β-isophorone with a content of 95.5% was obtained, and the proportion of heavy components in the entire isomerization reaction was 3.87%. The results are listed in Table 1.

Embodiment 2

[0035] The 3A molecular sieves obtained by filtering and separating the liquid in the tower still obtained in Example 1 carried a small amount of heavy components and added it to the tower again as a catalyst. At the same time, 600 g of new α-isophorone was added. According to the conditions of Example 1, Continue to catalyze the reaction, the final selectivity of β-isophorone is 94.6%, and the proportion of heavy components is 5.12%. The results are listed in Table 1.

Embodiment 3～4

[0037]Continue to repeat the operation steps of the second experiment, and carry out two more reactions, and the proportions of heavy components are 5.23% and 6.04% respectively.

[0038] The β-isophorone obtained in Examples 1 to 4 was combined for subsequent oxidation reaction to finally obtain oxoisophorone with a yield of 91.64%. The results are listed in Table 1.

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Abstract

The invention discloses a continuous synthesis technology of beta-isophorone. The technology comprises the following steps: by using alpha-isophorone as a starting raw material and using molecular sieve as a catalyst, an isomerization reaction is carried out in a column reactor by a reaction-distillation technology, and beta-isophorone is collected at the top of the column reactor; and heavy components are discharged out of the column reactor, and recovery is carried out to obtain alpha-isophorone for recycling. Conditions of the isomerization reaction are as follows: reaction temperature is 180-290 DEG C; reaction pressure is 0.05-0.30 MPa; and the molecular sieve accounts for 0.3-5.0% of mass of alpha-isophorone. In the technology, the molecular sieve and alpha-isophorone are together added into the column reactor to be fully contacted and react, and the obtained beta-isophorone is continuously distilled off. According to the invention, selectivity of products is high; dosage of the molecular sieve catalyst is low; and the catalyst and the heavy components can be conveniently recovered and separated.

Description

technical field [0001] The invention belongs to the field of preparation of chemical intermediates, in particular to a process for continuously synthesizing β-isophorone. Background technique [0002] 3,5,5-Trimethylcyclohex-3-en-1-one, also known as β-isophorone (β-IP), is the same fraction of α-isophorone (α-IP) Isomers, formed by α-isophorone through high-temperature catalytic isomerization, are important intermediates for the synthesis of vitamin series (such as vitamin E), carotenoids, astaxanthin and various flavors and fragrances, especially The main raw material for the synthesis of 3,5,5-trimethylcyclohex-2-ene-1,4-dione (KIP, tea aroma ketone), and the precursor for the preparation of trimethylhydroquinone. [0003] Many patents have reported the method of synthesizing β-isophorone by isomerization of α-isophorone, but there are many disadvantages: mainly, the catalyst cannot be regenerated, the space-time yield is not high, and by-products accumulate a lot. Exis...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/603C07C45/67
CPCC07C45/67C07C2601/16C07C49/603Y02P20/10Y02P20/584
Inventor 张琴潘洪韦良张亚飞赵江
Owner ZHEJIANG NHU PHARMA