Method for preparing 4-hexene-3-ketone by 4-hydroxy-3-hexanone dehydration

A technology of hexanone and hydroxyl, applied in the field of preparing 4-hexen-3-one, can solve the problems of poor catalyst activity, low space velocity, high reaction temperature, etc., achieve high specific surface area, developed pore structure, and avoid molding steps Effect

Inactive Publication Date: 2013-04-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • 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 po...

Method used

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  • Method for preparing 4-hexene-3-ketone by 4-hydroxy-3-hexanone dehydration
  • Method for preparing 4-hexene-3-ketone by 4-hydroxy-3-hexanone dehydration
  • Method for preparing 4-hexene-3-ketone by 4-hydroxy-3-hexanone dehydration

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 4 grams of 1 mol / liter nitric acid solution and 5 grams of water, add 1 gram of polyoxyethylene-polyoxypropylene-polyoxyethylene (molecular weight 5800, referred to as P123), stir and dissolve at room temperature, and add polyethylene oxide to the mixed solution. Diol (molecular weight 10000) 0.7 grams and 1.26 grams of aluminum nitrate (Al(NO 3 ) 3 9H 2 0), after stirring evenly, transfer to the ice-water mixing bath and continue to stir for 5 minutes. 5.1 g of tetramethyl orthosilicate was added to the mixed solution, and vigorously stirred for 20 minutes. Pour the mixture into a mold to seal it, and place it in an oven at 60°C for 72 hours of aging. After taking it out, it was demoulded, dried at 25°C, and finally fired at 600°C for 8 hours to obtain a monolithic silicon-aluminum oxide material with a silicon-aluminum molar ratio Si / Al=16. The mass ratio of each component is: R1 / SiO 2 =0.35, R2 / SiO 2 =0.5,H 2 O / SiO 2 =4.5,H + / SiO 2 =0.13, Al 2 o 3 ...

Embodiment 2

[0023] Weigh 12 grams of 0.3 mol / liter phosphoric acid solution, add 4.0 grams of polyoxyethylene-polyoxypropylene-polyoxyethylene (molecular weight 1500), stir and dissolve at room temperature, add polyethylene glycol (molecular weight 10000) 0.6 After stirring evenly, the mixed solution was added to the isopropanol solution containing 8.9 grams of tetrapropyl orthosilicate and 0.14 grams of aluminum isopropoxide, and vigorously stirred for 20 minutes. Pour the mixture into a mold and seal it, and place it in an oven at 80°C for 72 hours of aging. After taking it out, it was demolded, dried at room temperature, and finally baked at 550° C. for 5 hours to obtain a monolithic silicon-aluminum oxide material with a silicon-aluminum molar ratio Si / Al=75. The pore structure of the product is similar to the product of [Example 1]. The mass ratio of each component is: R1 / SiO 2 =0.3, R2 / SiO 2 = 2.0, H 2 O / SiO 2 =6,H + / SiO 2 =0.18, Al 2 o 3 / SiO 2 = 0.017. The specific sur...

Embodiment 3～15

[0026] According to the various steps and conditions of [Example 1], the silicon-aluminum oxide material is obtained, but the silicon source (tetramethyl orthosilicate TMOS, tetraethyl orthosilicate TEOS, tetrapropyl orthosilicate TPOS, orthosilicate) is changed. tetrabutyl silicate (TBOS), aluminum source (aluminum nitrate, aluminum sulfate, aluminum chloride, aluminum isopropoxide, aluminum isobutoxide and pseudoboehmite Al 2 o 3 ), the type of phase separation inducer R1 (polyethylene glycol PEG, polyoxyethylene PEO) or structure directing agent R2 (polyoxyethylene-polyoxypropylene-polyoxyethylene (molecular weight 12000, F127), polyoxyethylene-polyoxyethylene Oxypropylene-polyoxyethylene (molecular weight 2900, L64), cetyl trimethyl ammonium bromide CTAB, citric acid CA, lactic acid LA, tartaric acid TA, malic acid MA), raw material ratio, gel aging temperature and other parameters , specifically listed in Table 1. Characterization of the synthesized product shows that i...

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Abstract

The invention relates to a method for preparing 4-hexene-3-ketone by 4-hydroxy-3-hexanone dehydration, which mainly solves the problems of low activity of a catalyst, high reaction temperature, and low space velocity in the prior art. Aiming at well solving the problems, the method adopts the technical scheme that the 4-hydroxy-3-hexanone is used as a raw material, and the reaction raw material comes into contact with the catalyst to generate the 4-hexene-3-ketone when the reaction temperature is 200 to 400 DEG C and the liquid weight hourly space velocity is 0.5 to 15 h<-1> relative to the 4-hydroxy-3-hexanone; and the catalyst is a mesoporous/macroporous silica and alumina oxide material with a composite pore structure The method can be used for 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 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 carbanion, a...

Claims

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Application Information

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IPC IPC(8): C07C49/203C07C45/66B01J21/12B01J35/10
Inventor 李亚男金照生
Owner CHINA PETROLEUM & CHEM CORP
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