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Method of catalytic dehydration by 4-hydroxyl-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: 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, low space velocity and poor catalyst activity in the prior art, and a new method for catalytic dehydration of 4-hydroxyl-3-hexanone is provided

Method used

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  • Method of catalytic dehydration by 4-hydroxyl-3-hexanone

Examples

Experimental program
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Effect test

Embodiment 1

[0014] 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 =145,H 2 O / SiO 2 =32.8, NaCl / SiO 2 =0.6, NaOH / SiO 2 = 0.08, TBABr / SiO 2 = 0.12.

[0015] Get 50 gram grain diameters and be the ZSM-11 molecular sieve (SiO 2 / Al 2 o 3 =145), put into 250 gram concentration and be in the aqueous sodium hydroxide solution of 0.5 mol / liter, stir at 80 ℃ of constant temperature for 0.5 hour under reflux, filter, wash with distilled water, then use the ammonium nitrate aqueous solution of 10% mass concentration at 80 Exchanged three times at ℃, the we...

Embodiment 2

[0018] Get 50 grams of grain diameter and be the ZSM-11 molecular sieve (SiO 2 / Al 2 o 3 =40), put into 100 gram concentration and be in the sodium hydroxide aqueous solution of 1 mol / liter, stir 3 hours at 60 ℃ of constant temperatures under reflux, filter, wash with distilled water, exchange, dry, roast with [Example 1] ammonium , molding, and the obtained sample is marked as B.

[0019] Press each step of [embodiment 1] and condition to evaluate the performance of catalyst, and reaction condition and reaction result are shown in Table 1.

Embodiment 3

[0021] Get 50 grams of ZSM-11 molecular sieves (SiO 2 / Al 2 o 3 =100), put into 500 grams of concentration and be 0.2 mol / liter of potassium hydroxide aqueous solution, stir at 50 ℃ of constant temperature for 3.5 hours under reflux, filter, wash with distilled water, exchange, dry, roast with [Example 1] ammonium , forming, and the obtained sample is marked as C.

[0022] Press each step of [embodiment 1] and condition to evaluate the performance of catalyst, and reaction condition and reaction result are shown in Table 1.

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Abstract

The invention relates to a method of catalytic dehydration by 4-hydroxyl-3-hexanone and mainly solves the problem that catalysts are low in activity, high in reaction temperature and low in space velocity in the prior art. The 4-hydroxyl-3-hexanone is used as material to contact with catalyst at the reaction temperature of 200 DEG C-400 DEG C at the weight hourly space velocity of 0.5-15 hours-1 relative to the 4-hydroxyl-3-hexanone so as to generate 4-hexene-3-one. The catalyst is molecular sieve ZSM-11(zeolite socony mobil-11) not larger than 5 micrometers in grain diameter. The problem is solved well by the application of the technical scheme. The method is applicable to industrial production of 4-hexene-3-one by catalytic dehydration of 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 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, and a hydrogen ion...

Claims

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Application Information

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