Catalytic dehydration method of 4-hydroxy-3-hexanone

A technology for catalytic dehydration and hexanone, applied in chemical instruments and methods, molecular sieve catalysts, carbon-based compound preparation, etc., can solve problems such as low space velocity, poor catalyst activity, and high reaction temperature

Active Publication Date: 2016-01-13
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 method of 4-hydroxy-3-hexanone is provided

Method used

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  • Catalytic dehydration method of 4-hydroxy-3-hexanone
  • Catalytic dehydration method of 4-hydroxy-3-hexanone
  • Catalytic dehydration method of 4-hydroxy-3-hexanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Mix 40% silica sol, sodium metaaluminate, tetrapropylammonium bromide TPABr, sodium chloride, sodium hydroxide and water, stir for 20 minutes, then add polyethylene glycol (molecular weight is 6000), stir for 20 minutes, Put it into a reaction kettle, and conduct dynamic crystallization (200 rpm) at 170°C for 3 days. 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-5 zeolite raw powder. The molar ratio of each raw material in the reaction mixture is: SiO 2 / Al 2 o 3 =80.0,H 2 O / SiO 2 =50.8, NaCl / SiO 2 =0.68, NaOH / SiO 2 =0.15, TPABr / SiO 2 =0.40, polyethylene glycol mass / SiO 2 Mass = 0.1.

[0022] figure 1 It is the XRD pattern of the zeolite, showing typical ZSM-5 crystal phase characteristics. figure 2 This is the SEM photo of the zeolite, the crystal grain diameter is 0.2 micron. The micropore volume of the zeolite is 0.12 cm 3 / g, the mesopore volume is 0.37 cm 3 / ...

Embodiment 2

[0026] According to the steps and conditions of [Example 1], only SiO in the synthetic formula 2 / Al 2 o 3 =40.0, 1,6-hexanediamine is used as template agent, starch is used as mesoporous pore-forming agent, starch mass / SiO 2 Mass = 1, crystallization temperature 200°C for 5 days. The parameters of the synthesized zeolite are shown in Table 1. Same as [Example 1] ammonium exchange, drying, roasting, molding to obtain the catalyst.

[0027] The catalyst performance was evaluated according to the conditions of [Example 1]. The specific reaction conditions and results are shown in Table 2.

Embodiment 3

[0029]According to the steps and conditions of [Example 1], only the raw materials and the proportioning ratio of ingredients are different in the synthetic formula. The aluminum source is aluminum sulfate, the silicon source is water glass, and the template agent is tetrapropylammonium hydroxide. The molar ratio of each raw material in the reaction mixture is: SiO 2 / Al 2 o 3 =176.9,H 2 O / SiO 2 =28.15, NaCl / SiO 2 =0.80, NaOH / SiO 2 = 0.39, TPAOH / SiO 2 =0.19, the crystallization temperature was 150°C for 5 days. Mesoporous pore former is dextrin, dextrin mass / SiO 2 quality=5. The parameters of the synthesized zeolite are shown in Table 1. Same as [Example 1] ammonium exchange, drying, roasting, molding to obtain the catalyst.

[0030] The catalyst performance was evaluated according to the conditions of [Example 1]. The specific reaction conditions and results are shown in Table 2.

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Abstract

The invention relates to a 4-hydroxyl-3-hexanone catalytic dehydration method and mainly aims to solve the problems of a catalyst in the prior art, such as low activity, high reaction temperature and low space velocity. According to the technical scheme, 4-hydroxyl-3-hexanone serving as a raw material comes into contact with a catalyst to generate 4-hexylene-3-hexanone under the conditions that the reaction temperature ranges from 200 DEG C to 400 DEG C and the liquid mass space velocity relative to the 4-hydroxyl-3-hexanone is equal to 0.5-15h<-1>, wherein the used catalyst has the crystal grain diameter being at most 5mm, and has ZSM-5 zeolite with mesopores and micropores, and the ratio of the volume of the mesopores to the volume of the micropores in the ZSM-5 zeolite is equal to 1.5-10. The problems in the prior art can be well solved by adoption of the technical scheme. The 4-hydroxyl-3-hexanone catalytic dehydration method can be used for industrial production of 4-hexylene-3-hexanone prepared by using the 4-hydroxyl-3-hexanone.

Description

technical field [0001] The invention relates to a method for catalytic dehydration of 4-hydroxyl-3-hexanone. Background technique [0002] 4-Hexen-3-one (CAS: 2497-21-4) is a unique spice (China GB2760-2007), 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, and a hydrogen ion ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/203C07C45/66B01J29/40B01J35/10
Inventor 李亚男金照生李玉宁
Owner CHINA PETROLEUM & CHEM CORP
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