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Method for oxidizing cyclohexanone

A technology of cyclohexanone and oxidation reaction, applied in the field of cyclohexanone oxidation, can solve the problems of low conversion rate of cyclohexanone and/or low selectivity of hydroxy acid

Active Publication Date: 2019-04-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although the above method simplifies the process, the conversion rate of pimelinketone and / or the selectivity of hydroxyacids are low

Method used

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  • Method for oxidizing cyclohexanone
  • Method for oxidizing cyclohexanone
  • Method for oxidizing cyclohexanone

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Experimental program
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Embodiment approach

[0056] According to a preferred embodiment of the present invention, the alkali source is one or more of ammonia, aliphatic amines, aliphatic alcohol amines and quaternary ammonium bases.

[0057] In the present invention, the quaternary ammonium base can be various organic quaternary ammonium bases, and the aliphatic amine can be various NH 3 A compound formed after at least one hydrogen in is replaced by an aliphatic hydrocarbon group (preferably an alkyl group), and the aliphatic alcohol amine can be various NH 3 A compound formed after at least one hydrogen in is substituted by a hydroxyl-containing aliphatic hydrocarbon group (preferably an alkyl group).

[0058] Specifically, the quaternary ammonium base may be a quaternary ammonium base as shown in formula II, the aliphatic amine may be an aliphatic amine represented by formula III, and the aliphatic alcohol amine may be an aliphatic amine represented by formula IV Alcoholamine:

[0059]

[0060] In formula II, R ...

preparation example 1

[0081] Preparation of titano-silicate-alumina molecular sieve

[0082] (1) Take TS-1 molecular sieve (prepared according to the method described in "Zeolites, 1992, Vol.12: 943-950", TiO 2 The mass percentage composition is 2.1%) is placed in 100mL belt continuous feed and membrane separation device slurry bed reactor, adds the mixture of water and the hydrogen peroxide of 30wt% with the speed of 5.7mL / h under stirring state ( The volume ratio of water to hydrogen peroxide is 10:9), and the mixture of cyclohexanone and tert-butanol is added at a speed of 10.5mL / h (the volume ratio of cyclohexanone and tert-butanol is 1:2.5), and the mixture is added at a rate of 5.7 Add 36wt% ammonia water at a speed of mL / h, the above-mentioned three material streams are added simultaneously, and are continuously discharged at a corresponding speed at the same time, the reaction temperature is maintained at 80 ° C, and the product is sampled every 1 h after the reaction is stable. The compos...

Embodiment 1

[0092] According to the molar ratio of cyclohexanone, hydrogen peroxide and solvent methanol is 1:2:20, wherein the mass of solvent methanol is 30g, the concentration of catalyst (TS-A) in the reaction system is 0.05g / mL, and the temperature is 60°C And pressure is to react under 0.1MPa, and the result of reacting 8 hours is shown in table 1.

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Abstract

The invention relates to the preparation field of hydroxy acid and discloses a method for oxidizing cyclohexanone. The method comprises the step of contacting cyclohexanone, hydrogen peroxide and a catalyst under an oxidation reaction condition, wherein the catalyst is titanium silicon aluminum molecular sieve. The titanium silicon aluminum molecular sieve is prepared by the following steps: (1) mixing a catalyst containing a titanium silicon molecular sieve and first thermal treatment liquid, carrying out primary thermal treatment, and separating to obtain a first solid with a relative crystallization degree of 50%-90%, wherein the first thermal treatment liquid is an acid solution with a concentration more than 0.1mol / L; and (2) mixing the first solid, a silicon source, an aluminum source, an optional titanium source, an alkali source and water, and carrying out secondary thermal treatment, wherein the temperature of the secondary thermal treatment is 100-200 DEG C. According to themethod, the conversion rate and cyclohexanone and the selectivity of hydroxy acid can be effectively increased, and the utilization rate of an oxidizing agent, namely hydrogen peroxide can be increased.

Description

technical field [0001] The invention belongs to the field of preparation of hydroxy acids, and in particular relates to a method for oxidation of cyclohexanone, and furthermore relates to a method for oxidation of cyclohexanone using titanium-silicon-aluminum molecular sieve as a catalyst. Background technique [0002] Hydroxy acid is a kind of important chemical raw material, such as 6-hydroxycaproic acid is an important organic chemical raw material, which has a wide range of applications in the field of organic synthesis and polymer materials, its physical properties: melting point 38-40 ℃, boiling point 113 -116°C, density 0.981g / mL, refractive index 1044, flash point >110°C. Using 6-hydroxycaproic acid, 6-formylcaproic acid, ε-caprolactone, adipic acid, etc. can be prepared. Its derivative 6-hydroxyhexanoic acid ethyl ester etc. are commonly used organic chemical intermediates. [0003] At present, the raw materials for preparing 6-hydroxycaproic acid mainly includ...

Claims

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Application Information

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IPC IPC(8): C07C51/31C07C59/01B01J29/89
CPCC07C51/31B01J29/89C07C59/01
Inventor 史春风林民朱斌
Owner CHINA PETROLEUM & CHEM CORP