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Method of 4-hydroxy-3-hexanone catalysis and dehydration

A technology for catalytic dehydration and hexanone, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc. Effects of reaction temperature, acid-enhancing amount and acid strength

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 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-hydroxy-3-hexanone is provided

Method used

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  • Method of 4-hydroxy-3-hexanone catalysis and dehydration

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] H 3 Mo 12 o 40 P·nH 2 O is mixed with boehmite, Tianqing powder, and 0.3 mol / liter nitric acid, and the weight ratio of each raw material is H 3 Mo 12 o 40 P / Al 2 o 3 / Tianqing powder=0.13:1:0.1, molded, dried at 120°C for 12 hours, and roasted at 550°C for 10 hours. Al in the catalyst 2 o 3 The parts by weight of is 88 parts, and the parts by weight of heteropolyacid is 12 parts. The performance evaluation of the catalyst was carried out on a fixed-bed reaction device at normal pressure. A stainless steel reactor with an inner diameter of 10 mm was used, the loading amount of the catalyst was 10 ml, the reaction temperature was 290 °C, and the liquid space velocity was 1 hour. -1 , reacted under normal pressure. The reaction product was analyzed by HP 6890 gas chromatography, hydrogen flame detector, and HP-6 capillary column (60m×0.25mm×0.25μm). The reaction results are shown in Table 1.

Embodiment 2

[0019] Press each step and condition of [embodiment 1], only H 4 o 40 SiW 12 / Al 2 o 3 / Tianqing powder=0.20:1:0.1. Al in the catalyst 2 o 3 The parts by weight of is 83 parts, and the parts by weight of heteropolyacid is 17 parts. Catalyst performance was evaluated according to the conditions of [Example 1], except that the reaction temperature was 270°C and the liquid space velocity was 3 hours -1 . The reaction results are shown in Table 1.

Embodiment 3

[0021] Press each step and condition of [embodiment 1], only H 3 o 40 PW 12 / Al 2 o 3 / Tianqing powder=0.20:1:0.1. Al in the catalyst 2 o 3 The parts by weight of is 83 parts, and the parts by weight of heteropolyacid is 17 parts. The catalyst performance was evaluated according to the conditions of [Example 1], except that the reaction temperature was 340°C and the liquid space velocity was 8 hours -1 . The reaction results are shown in Table 1.

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Abstract

The invention relates to a method of 4-hydroxy-3-hexanone catalysis and dehydration, which mainly solves the problems of low activity of a catalyst, high reaction temperature, and low space velocity in the prior art. Aiming at well solving the problems, the method adopts the technical scheme that the 4-hydroxy-3-hexanone is used as a raw material, and the reaction raw material comes into contact with the catalyst to generate 4-hexene-3-ketone when the reaction temperature is 200 to 400 DEG C and the liquid weight hourly space velocity is 0.5 to 15 h<-1> relative to the 4-hydroxy-3-hexanone; and the catalyst is prepared by the following components in parts by weight: (a) 0.5 to 30 parts of heteropoly acid, and (b) 70 to 99.5 parts of alumina, wherein at least one of H3PMo12O40.nH2O, H4SiW12O40.nH2O or H3PW12O40.nH2O is adopted as the heteropoly acid, and n is 0 to 10. The method can be used for the industrial production of the 4-hexene-3-ketone prepared by the 4-hydroxy-3-hexanone.

Description

technical field [0001] The present invention relates to a process for the 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 carbanion, and a ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/203C07C45/66B01J31/26
Inventor 李亚男金照生李玉宁
Owner CHINA PETROLEUM & CHEM CORP
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