Method for preparing 4-hexene-3-ketone by carrying out catalytic dehydration on 4-hydroxy-3-hexanone

A technology of catalytic dehydration and hexanone, applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of high reaction temperature, poor catalyst activity, low space velocity, etc., and achieve good technical effects. Effect

Inactive Publication Date: 2013-04-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is the problem of high reaction temperature, low space velocity and poor catalyst activity in the prior art, and a new catalytic dehydration of 4-hydroxy-3-hexanone is provided to prepare 4-hexen-3-one Methods

Method used

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  • Method for preparing 4-hexene-3-ketone by carrying out catalytic dehydration on 4-hydroxy-3-hexanone
  • Method for preparing 4-hexene-3-ketone by carrying out catalytic dehydration on 4-hydroxy-3-hexanone
  • Method for preparing 4-hexene-3-ketone by carrying out catalytic dehydration on 4-hydroxy-3-hexanone

Examples

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Effect test

Embodiment 1

[0018] Dissolve 30 grams of aluminum nitrate in 25 grams of deionized water, take 20 grams of MCM-41 carrier, impregnate the above solution at 20°C, take it out after 3 hours and dry it at 120°C for 5 hours, then bake it in a muffle furnace at 600°C for 4 hours. After cooling, it is taken out and then impregnated twice, dried and calcined to obtain catalyst A. Al in the catalyst 2 o 3 The parts by weight of the surface coating are 22.5 parts, and the parts by weight of MCM-41 are 77.5 parts. The performance evaluation of the catalyst was carried out on a fixed-bed reaction device at normal pressure. A stainless steel reactor with an inner diameter of 10 mm was used. The loading amount of the catalyst was 10 ml, the reaction temperature was 350 °C, and the liquid space velocity was 1 hour. -1 , reacted under normal pressure. The reaction product was analyzed by HP 6890 gas chromatography, hydrogen flame detector, and HP-6 capillary column (60m×0.25mm×0.25μm). The reaction r...

Embodiment 2

[0020] Dissolve 20 grams of aluminum sulfate in 100 grams of deionized water, take 20 grams of MCM-48 carrier, impregnate the above solution at 50°C, take it out after 4 hours and dry it at 100°C for 6 hours, then bake it in a muffle furnace at 500°C for 5 hours. After cooling, the catalyst B is obtained by taking it out, impregnating it twice, drying it, and roasting it. Al in the catalyst 2 o 3 The parts by weight of the surface coating are 25.2 parts, and the parts by weight of MCM-48 are 74.8 parts. Catalyst performance was evaluated according to the conditions of [Example 1], except that the reaction temperature was 260°C and the liquid space velocity was 3 hours -1 . The reaction results are shown in Table 1.

Embodiment 3

[0022] Dissolve 12 grams of aluminum nitrate in 20 grams of deionized water, take 15 grams of SBA-15 carrier, impregnate the above solution at 70°C, take it out after 2 hours and dry it at 110°C for 4 hours, then bake it in a muffle furnace at 650°C for 4 hours. Catalyst C is obtained. Al in the catalyst 2 o 3 The parts by weight of the surface coating are 13.0 parts by weight, and the parts by weight of SBA-15 are 87.0 parts by weight. Evaluation catalyst performance by the condition of [embodiment 1], just reaction temperature is 270 ℃, and liquid space velocity is 8 hours -1 . The reaction results are shown in Table 1.

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Abstract

The invention relates to a method for preparing 4-hexene-3-ketone by carrying out catalytic dehydration on 4-hydroxy-3-hexanone, mainly aiming at solving the problems of low catalyst activity, high reaction temperature and slow space velocity in the prior art. The method takes the 4-hydroxy-3-hexanone as raw material, and can be used for producing the 4-hexene-3-ketone by enabling the reaction raw material to be contacted with catalyst under the conditions that the reaction temperature is 200-400 DEG C and the space velocity relative to the mass of the 4-hydroxy-3-hexanone liquid is 0.5-15h<-1>, wherein the catalyst comprises the components in parts by weight: a) 1-99 parts of pure silicon molecular sieve which is at least one selected from MCM-41, MCM-48, SBA-15, HMS, Silicate-1 or Silicate-2, and b) 1-99 parts of Al2O3 surface coating. The technical scheme better solves the problems, and can be used in the industrial production of the 4-hexene-3-ketone prepared by the 4-hydroxy-3-hexanone.

Description

technical field [0001] The invention relates to a method for preparing 4-hexen-3-one by catalytic dehydration of 4-hydroxyl-3-hexanone. Background technique [0002] 4-Hexen-3-one (CAS: 2497-21-4) is a unique spice (China GB 2760-2007), which is mainly used to prepare food flavors such as Laomu, butter, and horseradish, and has a wide range of uses. [0003] The dehydration reaction of hydroxyl compounds is a reaction in which the hydroxyl and hydrogen atoms on two adjacent atoms in the reactant molecule are removed in the form of water in the presence of a catalyst. Since the oxygen atom of the hydroxyl group contains a lone pair of electrons, it can interact with the proton (H + ) to form oxonium ions, which become strong electron-withdrawing groups due to the positive charges on the oxygen atoms, making the C-O bond easy to dissociate. The whole dehydration reaction includes: generating protonated oxonium salt (R-OH 2 + ), the oxonium salt slowly dissociates into a ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/203C07C45/66B01J29/03B01J29/035
Inventor 李亚男金照生金萍
Owner CHINA PETROLEUM & CHEM CORP
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