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A method of continuously preparing 3,5,5-trimethyl-3-cyclohexene-1-one

The technology of a trimethylcyclohexyl and reactive distillation column is applied in the field of continuous preparation of 3,5,5-trimethylcyclohex-3-en-1-one, and can solve the problems of low extraction rate, difficulty in industrial production, The problems of low space-time yield and other problems have achieved the effects of easy recovery, less equipment corrosion, and less generation of three wastes.

Active Publication Date: 2015-07-08
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its space-time yield is low, and the extraction rate is also low. When the product is formed, it will be accompanied by the accumulation of a large amount of by-products, which makes it difficult for this method to realize industrial production.

Method used

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  • A method of continuously preparing 3,5,5-trimethyl-3-cyclohexene-1-one

Examples

Experimental program
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Effect test

Embodiment 1

[0036] 10gLa(NO 3 ) 3 Dissolve in 200ml deionized water to form a salt solution, and La(NO 3 ) 3 : NiFe 2 o 4 (Zibo Innaite Nano Technology Co., Ltd.) = 15:1 (mass ratio), with an appropriate amount of NiFe 2 o 4Add it to the salt solution, stir well, and soak for 8 hours. After filtering, dry at 60°C for 8h; then bake at 600°C for 3h in a muffle furnace to obtain the magnetic nano-solid alkali catalyst La 2 o 3 / NiFe 2 o 4 .

[0037] Add 10g La in advance at the bottom of 1m rectification tower 2 o 3 / NiFe 2 o 4 and 200g alpha-isophorone. The reaction system was replaced by nitrogen for 3 times. Under the conditions of 206°C and 0.1MPa, the number of plates was 20, and the reflux ratio was 3. After 1 hour of stable total reflux, the top and bottom of the tower began to be withdrawn, and the bottom of the tower began to feed α - Isophorone, the flow rate is 100g / h for continuous reactive distillation. After 48 hours, the selectivity of β-isophorone measured by...

Embodiment 8

[0041] With reference to the technical process of Example 1, only the continuous reaction rectification time is extended at 500h, the reaction selectivity is maintained at 99.5%, and the total yield is 98.1%. After 1000 hours of continuous reaction and rectification, the activity of the catalyst decreased. The catalyst was recovered by applying an external magnetic field, and the activity recovered after being calcined again in a muffle furnace at 600°C for 3 hours.

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Abstract

The invention relates to a method of continuously preparing 3,5,5-trimethyl-3-cyclohexene-1-one (beta-isophorone) by utilization of a heterogeneous catalyst. 3,5,5-trimethyl-2-cyclohexene-1-one is adopted as a raw material, and is subjected to an isomerization reaction by adoption of a reactive distillation column under conditions of a solid alkali catalyst without adding other organic alkalis to obtain the 3,5,5-trimethyl-3-cyclohexene-1-one. The method has advantages of high conversion ratio, good selectivity, less heavy components, easy catalyst recovery, and the like and is a green synthetic process.

Description

technical field [0001] The invention relates to a method for continuously preparing 3,5,5-trimethylcyclohex-3-en-1-one (β-isophorone). Background technique [0002] β-isophorone is an important intermediate for the preparation of carotenoids, vitamins (such as vitamin E) and spices. It also deals directly with synthetic fragrances and natural products such as astaxanthin, abscisic acid and some derivatives. Especially the main raw material for the artificial synthesis of oxidized isophorone (2,6,6-trimethyl-2-cyclohexene-1,4-dione, KIP). [0003] At present, the preparation methods of β-isophorone reported at home and abroad basically all synthesize 3,5,5-trimethylcyclohex-2-en-1-one (α-isophorone) from basic organic raw materials at first. ketone), and then under certain conditions, α-isophorone is subjected to isomerization reaction to generate β-isophorone. Since the isomerization of α-isophorone to β-isophorone is an equilibrium reaction in which the double bond decon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/603C07C45/67C07C45/82
CPCY02P20/10
Inventor 董岩峰张涛何光文郭劲资崔乾王鹏丛鑫赵晶陈海波黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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