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

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

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

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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 method for catalytic dehydration of 4-hydroxy-3-hexanone to produce 4-hexen-3-one is provided. method

Method used

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

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Effect test

Embodiment 1

[0019] Dissolve 30 grams of aluminum nitrate in 25 grams of deionized water, take 20 grams of silica gel carrier, impregnate the above solution at 20 ° C, take it out after 3 hours and dry it at 120 ° C for 5 hours, put it in a muffle furnace and bake it at 600 ° C for 4 hours, after cooling The catalyst A is obtained by taking out and impregnating for the second time, drying and roasting. Al in the catalyst 2 o 3 The parts by weight of the surface coating is 23 parts, SiO 2 The parts by weight of the inner core are 77 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 ...

Embodiment 2

[0021] Dissolve 20 grams of aluminum sulfate in 100 grams of deionized water, take 20 grams of silica carrier, impregnate the above solution at 50°C, take it out after 4 hours, dry it at 100°C for 6 hours, and 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 is 25 parts, SiO 2 The parts by weight of the inner core are 75 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

[0023] Dissolve 12 grams of aluminum nitrate in 20 grams of deionized water, take 15 grams of white carbon black carrier, impregnate the above solution at 70 ° C, take it out after 2 hours and dry it at 110 ° C for 4 hours, put it in a muffle furnace and bake it 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 is 14 parts, SiO 2 The parts by weight of the kernel are 86 parts. 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 producing 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 SiO2 inner core, 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 producing 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): C07C49/203C07C45/66B01J21/12
Inventor 金照生李亚男孙兰萍
Owner CHINA PETROLEUM & CHEM CORP
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