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Synthesizing method for oxime

A synthesis method and technology of the combination are applied in the directions of chemical instruments and methods, oxime preparation, molecular sieve catalyst, etc., can solve the problems of high hydroxylamine salt dosage, increased cost and difficulty of separation, etc., and achieve high conversion rate, high utilization rate, high Simple processing effect

Inactive Publication Date: 2008-03-19
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
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Problems solved by technology

This process has two disadvantages: (1) high hydroxylamine salt consumption; (2) generate a large amount of by-product inorganic salts at the same time
US 6,462,235 discloses a method for producing oxime in a liquid phase method using aldehydes or ketones, ammonia and hydrogen peroxide as raw materials, using titanium-silicon molecular sieve TS-1 as a catalyst, under the coexistence of ammonium salts or substituted ammonium salts. The method is very effective for macromolecular cyclic ketones, but it is necessary to add co-catalyst ammonium salts or substituted ammonium salts in the reaction to obtain high conversion and selectivity, which increases the cost of the reaction and the difficulty of separation

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0029] The catalyst is Ti-MWW-F molecular sieve.

[0030] The first step ketone: catalyst: the weight ratio of solvent is 1: 0.2: 4, ketone: the molar ratio of ammonia is 1: 1.5, ketone is methyl ethyl ketone, solvent is water, ammonia is ammonia water, and concentration is 25%;

[0031] The second step reaction temperature is 62 DEG C, the ketone: the molar ratio of hydrogen peroxide is 1: 1.2, the concentration of hydrogen peroxide solution is 30%, and the time for dropping is 1 hour, and the reaction is continued for 0.5 hours after the dropping is completed, the reaction system The pressure is 1atm.

[0032] The analysis results showed that the ketone conversion rate was 99.0%.

Embodiment 2

[0034] Implementation process is except following difference, and all the other are all the same with embodiment 1:

[0035] In the first step, the weight ratio of ketone:catalyst:solvent is 1:0.1:10; in the second step, the molar ratio of ketone:hydrogen peroxide is 1:1.

[0036] Analysis results showed that the ketone conversion rate was 93.3%.

Embodiment 3

[0038] Implementation process is except following difference, and all the other are all the same with embodiment 1:

[0039] In the first step, the weight ratio of ketone:catalyst:solvent is 1:0.15:10, the molar ratio of ketone:ammonia is 1:1.3, and the ketone is acetone; in the second step, the reaction temperature is 50°C, ketone:peroxidation The molar ratio of hydrogen was 1:1.5, and the dropwise addition time was 2 hours, and the reaction was continued for 1 hour after the dropwise addition was completed.

[0040] The analysis results showed that the ketone conversion rate was 91.5%.

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Abstract

The invention relates to a synthesis method of oxime, which belongs to the technical field of organic synthesis. At present, the oxime is synthesized mainly by utilizing the reaction between hydroxylamine salt and ketone and aldehyde, and defects are the high dosage of hydroxylamine salt and the production of a large amount of byproduct (inorganic salt). The technique is an environment-friendly process. In the technical scheme of the invention, reactant (ketone or aldehyde), ammonia and hydrogen peroxide are ordinally added into the reaction system of catalyst containing Ti-MWW-F molecular sieve and solvent, and after stiring, temperature raising and reaction are finished, an oxime product is produced by filtering, distillation, liquor filtering and separation. The invention has the advantages of high conversion rate of ketone or aldehyde, high utilization rate of hydrogen peroxide, usage of water as resolvent, simple post-processing procedure and environment-friendly reaction procedure.

Description

technical field [0001] The invention relates to a synthesis method of oxime, in particular to a method for producing oxime using titanium silicon molecular sieve as a catalyst and ketone or aldehyde, ammonia and hydrogen peroxide as a reaction system, belonging to the technical field of organic chemical synthesis. Background technique [0002] Oxime is a very versatile fine chemical. Especially small molecule oxime, such as butanone oxime, is used as a good antioxidant in polyurethane sealant, as an anti-skinning agent in coatings, paints, and inks; acetone oxime, as an oxygen scavenger, is used in thermal boiler water deoxidation; Acetaldehyde oxime is an intermediate of medicine and pesticide. [0003] Currently, oximes are mainly synthesized by the reaction of hydroxylamine salts with ketones or aldehydes. This technique has two disadvantages: (1) high hydroxylamine salt consumption; (2) generate a large amount of by-product inorganic salts simultaneously. This process...

Claims

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Application Information

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IPC IPC(8): C07C249/08B01J29/89
Inventor 吴鹏刘月明宋芬吴海虹何鸣元
Owner EAST CHINA NORMAL UNIV
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