Production method of 4-hexene-3-one by catalyzed dehydration of 4-hydroxy-3-hexanone

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

Inactive Publication Date: 2013-04-10
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 method for preparing 4-hexen-3-one by catalytic dehydration of 4-hydroxy-3-hexanone is provided method

Method used

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  • Production method of 4-hexene-3-one by catalyzed dehydration of 4-hydroxy-3-hexanone
  • Production method of 4-hexene-3-one by catalyzed dehydration of 4-hydroxy-3-hexanone
  • Production method of 4-hexene-3-one by catalyzed dehydration of 4-hydroxy-3-hexanone

Examples

Experimental program
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Effect test

Embodiment 1

[0022] 6.2 g of Zr (NO 3 ) 4 ·5H 2 O was dissolved in 208 grams of deionized water. After the dissolution was complete, 16 grams of cetyltrimethylammonium bromide (CTAB) was added, and it was fully stirred to dissolve it. After the solution was clarified, 80 grams of ethyl orthosilicate was added. Zr: Si: CTAB (mol) = 1: 24.5: 3, under stirring, add concentrated ammonia water dropwise to pH = 10, continue to stir for 2 hours, age for 12 hours, the sample is filtered and washed with deionized water until there are no impurity ions Dry at 100 °C to obtain mesoporous ZrO 2 -SiO 2 vector.

[0023] The carrier was ground to ≤100 mesh, and then impregnated with an equal volume of 0.5 mol / L ammonium tungstate solution for 12 hours, dried in a water bath, and calcined at 700 °C for 5 hours to obtain the catalyst sample WO 3 / ZrO 2 -SiO 2 , so that W:Zr:Si (mol)=0.16:1:24.5. The XRD pattern of the catalyst is shown in figure 1 , see TEM pictures image 3 . Its specific surfa...

Embodiment 2

[0026] According to the steps and conditions of [Example 1], only using tungstic acid, W:Zr:Si (mol)=0.21:1:24.5, calcination at 650°C for 10 hours. The pore size is 4.5 nanometers.

[0027] The performance evaluation of the catalyst was performed according to the steps and conditions of [Example 1], except that the reaction temperature was 270°C and the liquid space velocity was 3 hours. -1 , and the reaction results are shown in Table 1.

Embodiment 3

[0029] According to the steps and conditions of [Example 1], only use ZrOCl 2 , silica sol, polyoxypropylene polyoxyethylene copolymer (P123), Zr:Si:P123 (mol)=1:11.3:0.5, aging for 24 hours. Only molybdic acid was used, Mo:Zr:Si (mol)=0.18:1:11.3, excess impregnation for 12 hours, and calcination at 650°C for 10 hours. The XRD pattern of the catalyst is shown in figure 2 , see TEM pictures Figure 4 . Its specific surface area is 1015.09 meters 2 / g, the hole volume is 0.85 cm 3 / g, with a pore size of 3.4 nm.

[0030]The performance evaluation of the catalyst was carried out according to the steps and conditions of [Example 1], except that the reaction temperature was 340°C and the liquid space velocity was 8 hours. -1 , and the reaction results are shown in Table 1.

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Abstract

The present invention relates to a production method of 4-hexene-3-one by catalyzed dehydration of 4-hydroxy-3-hexanone, and mainly solves the problem of low catalyst activity, high reaction temperature and low space velocity in the prior art. According to the invention, 4-hydroxy-3-hexanone is used as a raw material, and the reaction raw material is in contact with a catalyst to produce 4-hexen-3-one at the conditions of a reaction temperature of 200-450 DEG C and the airspeed of 0.5-15 hr-1 with respect to the mass of 4-hydroxy-3-hexanone liquid, wherein the catalyst is WO3 / ZrO2-SiO2 or MoO3 / ZrO2-SiO2, and the molar ratio of W or Mo:Zr:Si is (0.05-0 .3):1:(5-50). The technical solution solves the problem preferably. The method can be used in the industrial production of 4-hexen-3-one from 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 in the preparation of food flavors such as Laomu, butter, horseradish, etc., 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 the 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 + ) combine to form an oxonium ion, which becomes a strong electron withdrawing group due to the positive charge on the oxygen atom, which makes the C-O bond easy to dissociate. The entire dehydration reaction involves the formation of protonated oxonium salts (R-OH 2 + ), the oxo...

Claims

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Application Information

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IPC IPC(8): C07C49/203C07C45/66
Inventor 李亚男金照生周海春
Owner CHINA PETROLEUM & CHEM CORP
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