Method for catalyzing and dehydrating 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 the problems of low space velocity, poor catalyst activity, high reaction temperature, etc., and achieve reduced deep reaction and stable activity Sexual improvement, sodium content reduction effect

Inactive Publication Date: 2011-01-12
SHANGHAI RES INST OF PETROCHEMICAL TECH SINOPEC
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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 ve...

Method used

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  • Method for catalyzing and dehydrating 4-hydroxy-3-hexanone
  • Method for catalyzing and dehydrating 4-hydroxy-3-hexanone
  • Method for catalyzing and dehydrating 4-hydroxy-3-hexanone

Examples

Experimental program
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Embodiment 1

[0017] 40% silica sol, sodium metaaluminate, tetrapropylammonium bromide (TPABr), sodium chloride, sodium hydroxide and water, SiO in molar ratio 2 :Al 2 o 3 :Cl - :OH - :TPABr:H 2 O=1: 0.013: 0.68: 0.15: 0.4: 51, mixed, stirred for 20 minutes, put into a reaction kettle, and crystallized dynamically at 170° C. (200 rpm) for 3 days. The crystallized product was rapidly cooled, filtered, washed with water until the pH value was 8, and dried at 120°C for 12 hours to obtain NaZSM-5 zeolite raw powder with an average grain diameter of 0.5 microns.

Embodiment 2

[0019] The raw NaZSM-5 zeolite powder synthesized in [Example 1] was treated with 0.3 mol / L hydrochloric acid at 80°C for 4 hours for 3 consecutive times to obtain HZSM-5, which was dried at 120°C for 12 hours and calcined at 550°C for 5 hours.

Embodiment 3

[0021] According to the steps and conditions of [Example 1], only SiO in the synthetic formula 2 : Al 2 o 3 =0.025, the templating agent is 1,6-hexamethylenediamine, the crystallization temperature is 200°C for 5 days, and 1.0 mol / L citric acid is exchanged at 70°C for 5 hours for 4 consecutive times. The average crystal grain diameter of the synthesized HZSM-5 zeolite raw powder is 1 micron.

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Abstract

The invention relates to a method for catalyzing and dehydrating 4-hydroxy-3-hexanone, which mainly solves the problems of low catalyst activity, high reaction temperature and low airspeed in the prior art. In the method, the 4-hydroxy-3-hexanone is adopted as a raw material; the reaction raw material and a catalyst contact to prepare 4-hydroxy-3-ketone under the condition that the reaction temperature is between 200 to 400 DEG C and the quality airspeed is 0.5 to 15 hours corresponding to 4-hydroxy-3-hexanone liquid; the technological scheme that the catalyst is HZSM-5 zeolite, the grain diameter of the zeolite is less than 5 micrometers and the molar ratio of SiO2 to Al2O3 is 1: 0.003 to 0.05 to solve the problem; and the method is suitable for industrial production for preparing the 4-hydroxy-3-ketone by the 4-hydroxy-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 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 combine with a proton (H+) to form an oxonium ion. Since the oxygen atom is positively charged, it becomes a strong electron-withdrawing group, which makes 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 is...

Claims

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Application Information

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IPC IPC(8): C07C49/203C07C45/66B01J29/40A23L1/226A23L27/20
Inventor 李亚男金照生徐菁周海春金萍孙兰萍黄祖娟
Owner SHANGHAI RES INST OF PETROCHEMICAL TECH SINOPEC
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