Catalytic dehydrating preparation method of 4-hexen-3-ketone by 4- hydroxy-3-hexanone

A technology for catalytic dehydration and hexanone, which is applied in the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, and can solve problems such as high reaction temperature, poor catalyst activity, and low space velocity

Active Publication Date: 2013-05-29
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,

Method used

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  • Catalytic dehydrating preparation method of 4-hexen-3-ketone by 4- hydroxy-3-hexanone
  • Catalytic dehydrating preparation method of 4-hexen-3-ketone by 4- hydroxy-3-hexanone
  • Catalytic dehydrating preparation method of 4-hexen-3-ketone by 4- hydroxy-3-hexanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Mix 40% silica sol, sodium metaaluminate, tetrabutylammonium bromide, potassium chloride, sodium hydroxide and water, stir for 20 minutes, then add polyethylene glycol (molecular weight is 6000), stir for 20 minutes, load Put it 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 ZSM-11 molecular sieve powder. 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, KCl / SiO 2 =0.6, NaOH / SiO 2 = 0.08, TBABr / SiO 2 =0.12, polyethylene glycol mass / SiO 2 Mass = 0.1.

[0022] figure 1 It is the XRD pattern of the zeolite, showing typical ZSM-11 crystal phase characteristics. figure 2 This is the SEM photograph of the zeolite, with an average grain size of 0.3 microns. The micropore volume of the zeolite is 0.12 cm 3 / g, the mesopore volume is 0.38 cm 3 / g, th...

Embodiment 2

[0026] Mix 40% silica sol, sodium metaaluminate, tetrabutylammonium bromide, sodium chloride, sodium hydroxide and water, stir for 20 minutes, then add starch, stir for 20 minutes, put it into a reaction kettle, crystallize at 170°C 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 an average 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, starch / SiO 2 mass=1. The parameters of the synthesized zeolite are shown in Table 1.

[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] The catalyst performance was evaluated according to the conditions of [Example 1]. The specific reacti...

Embodiment 3

[0030] According to the steps and conditions of [Example 2], only the mesoporous pore-forming agent is dextrin, dextrin / SiO 2 Quality = 5, SiO in the synthesis formula 2 / Al 2 o 3 =52.3, tetrabutylammonium hydroxide was used as template agent, and the crystallization temperature was 120°C for 8 days. The parameters of the synthesized zeolite are shown in Table 1. With [Example 1] ammonium exchange, drying, roasting.

[0031] 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 catalytic dehydrating preparation method of 4-hexen-3-ketone by 4- hydroxy-3-hexanone and solves problems of low catalytic activity, high reaction temperature and low airspeed in the prior art. The 4- hydroxy-3-hexanone is adopted as a raw material, on conditions that reaction temperature ranges from 200 DEG C to 400 DEG C and the airspeed of 4- hydroxy-3-hexanone liquid quality is 0.5-15 hour -1, the raw material is contacted with a catalyst to form the 4-hexen-3-ketone. The grain diameter of the catalyst is </= 5 micron, the catalyst is provided with zeolite ZSM-11 with mesopores and micropores, and the values of pore volumes of the mesopores and micropores of the zeolite ZSM-11 are 1.5-10. According to the technical scheme, the catalytic dehydrating preparation method solves the problems effectively and can be used in industrial production of 4-hexen-3-ketone by 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-hydroxy-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 car...

Claims

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Application Information

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