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Preparation method of 4-hexene-3-ketone by virtue of dehydration of 4-hydroxy-3-hexanone

A technology of hexanone and hydroxyl, which is applied in the field of producing 4-hexen-3-one, can solve the problems of poor catalyst activity, high reaction temperature, and low space velocity, and achieve improved activity stability, large specific surface area, and reduced Effects of Depth Response

Active Publication Date: 2013-04-24
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 that there are problems of high reaction temperature, low space velocity and poor catalyst activity in the prior art, and a new method for producing 4-hexen-3-one by dehydration of 4-hydroxyl-3-hexanone is provided. Methods

Method used

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  • Preparation method of 4-hexene-3-ketone by virtue of dehydration of 4-hydroxy-3-hexanone
  • Preparation method of 4-hexene-3-ketone by virtue of dehydration of 4-hydroxy-3-hexanone
  • Preparation method of 4-hexene-3-ketone by virtue of dehydration of 4-hydroxy-3-hexanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Mix 40% silica sol, sodium metaaluminate, tetrabutylammonium bromide, sodium chloride, sodium hydroxide and water, stir for 20 minutes, put into a reaction kettle, and crystallize at 170°C for 1 day. The crystallized product was quenched, filtered, washed with water until the pH value was 8, and dried at 120°C for 12 hours to obtain the original powder of ZSM-11 molecular sieve. The XRD spectrum is shown in figure 1 , SEM photo see figure 2 , the grain diameter is 0.5 microns. The molar ratio of each raw material in the reaction mixture is: SiO 2 / Al 2 o 3 =149.3,H 2 O / SiO 2 =32.8, NaCl / SiO 2 =0.6, NaOH / SiO 2 = 0.08, TBABr / SiO 2 = 0.12.

[0022] The synthesized ZSM-11 molecular sieve raw powder was treated with 0.3 mol / L nitric acid at 80°C for 4 hours for 3 consecutive times to obtain HZSM-11.

[0023] Mix HZSM-11 with boehmite, Tianqing powder, and 0.3 mol / liter nitric acid, and the weight ratio of each raw material is ZSM-11 / Al 2 o 3 / Tian Qing powder =...

Embodiment 2

[0026]Mix 40% silica sol, sodium metaaluminate, tetrabutylammonium bromide, sodium chloride, sodium hydroxide and water, stir for 20 minutes, put into a reaction kettle, and crystallize at 170°C for 1 day. The crystallized product was quenched, filtered, washed with water until the pH value was 8, and dried at 120°C for 12 hours to obtain ZSM-11 molecular sieve raw powder with a grain diameter of 0.5 microns. The molar ratio of each raw material in the reaction mixture is: SiO 2 / Al 2 o 3 =149.3,H 2 O / SiO 2 =32.8, NaCl / SiO 2 =0.6, NaOH / SiO 2 = 0.08, TBABr / SiO 2 = 0.12.

[0027] The synthesized ZSM-11 molecular sieve raw powder was treated with 0.3 mol / L hydrochloric acid at 80°C for 4 hours for 3 consecutive times to obtain HZSM-11.

[0028] Mix HZSM-11 with boehmite, Tianqing powder, and 0.3 mol / liter nitric acid, and the weight ratio of each raw material is HZSM-11 / Al 2 o 3 / Tian Qing powder = 1:1:0.1, extruded into strips, dried at 120°C for 12 hours, roasted at ...

Embodiment 3

[0031] According to the steps and conditions of [Example 2], only SiO in the synthetic formula 2 / Al 2 o 3 =52, tetrabutylammonium hydroxide was used as template agent, crystallized at 120° C. for 8 days, and the crystal grain diameter of the synthesized ZSM-11 molecular sieve raw powder was 1 micron. Exchange with 1.0 mol / L citric acid at 80°C for 10 hours. Get a catalyst.

[0032] The performance of the catalyst was evaluated according to the steps of [Example 1]. The reaction conditions and the results are shown in Table 1.

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Abstract

The invention relates to a preparation method of 4-hexene-3-ketone by virtue of dehydration of 4-hydroxy-3-hexanone, and the method is mainly used for solving the problems in the prior art that the catalyst activity is low, the reaction temperature is high and the space velocity is low. The technical scheme adopted by the invention is as follows: according to the preparation method, 4-hydroxy-3-hexanone which is used as a raw material, is contacted with a catalyst so as to generate 4-hexene-3-ketone under the condition that the reaction temperature is 200-400 DEG C, and the space velocity relative to the liquid weight of 4-hexene-3-ketone is 0.5-15h<-1>, wherein the catalyst comprises the following components in parts by weight: a), 40-95 parts of ZSM-11 molecular sieve with the silicon aluminum mole ratio (SiO2 / Al2O3) of 20-300 and the crystal particle diameter of equal to or less than 5 microns and b), 5-6 parts of binding agent, and the ZSM-11 molecular sieve is at least subjected to once acid pickling, so that the problems in the prior art are better solved, and the method can be used in the industrial production of 4-hexene-3-ketone prepared by utilizing 4-hydroxy-3-hexanone.

Description

technical field [0001] The invention relates to a method for producing 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 Laomu, butter, horseradish and other food flavors, 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, and...

Claims

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Application Information

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IPC IPC(8): C07C49/203C07C45/66B01J29/40
Inventor 李亚男金照生黄祖娟
Owner CHINA PETROLEUM & CHEM CORP
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