Process for producing oxime

A production method and technology for products, applied in the field of organic chemical synthesis, can solve the problems of high hydroxylamine salt dosage, inability to obtain conversion rate and the like, and achieve the effects of high conversion rate, high selectivity to oxime formation, and high utilization rate

Active Publication Date: 2007-07-25
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has two main disadvantages: (1) high hydroxylamine salt consumption; (2) generate a large amount of by-product inorganic salts at the same time
In summary, the method of the background technology cannot obtain a sufficiently high conversion rate of ketones and a sufficiently high selectivity for forming oximes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Ketones are cycloaliphatic ketones: cyclohexanone

[0030] The first step ketone: catalyst: the weight ratio of solvent is 1: 0.05: 5, and the mol ratio of ketone: ammonia is 1: 1.15, and catalyst is Ti-ECNU-1 molecular sieve, and ammonia is liquid ammonia, and concentration is 25%, and solvent is water;

[0031] The second step reaction temperature and pressure are 73 DEG C and 1 atm respectively, the mol ratio of ketone: hydrogen peroxide is 1: 1.06, the concentration of hydrogen peroxide is 30%, the time of dropping is 1 hour, continue to react after dropping for 0.5 Hour.

[0032] The analysis results showed that the conversion rate of ketone was 98.5%, and the selectivity of oxime was 99.8%.

Embodiment 2

[0034] Except following difference, all the other are the same with embodiment 1:

[0035] In the first step, the weight ratio of ketone:catalyst:solvent is 1:0.05:10; in the second step, the molar ratio of ketone:hydrogen peroxide is 1:1.

[0036] The analysis results showed that the conversion rate of ketone was 97.3%, and the selectivity of oxime was 99.5%.

Embodiment 3

[0038] Except following difference, all the other are the same with embodiment 1:

[0039] Ketones are cycloaliphatic ketones: cyclooctanone

[0040] In the first step, the weight ratio of ketone:catalyst:solvent is 1:0.1:10, and the molar ratio of ketone:ammonia is 1:1.3; in the second step, the reaction temperature is 80°C, the ketone:hydrogen peroxide The molar ratio was 1:1.3, and the dropwise addition time was 2 hours, and the reaction was continued for 1 hour after the dropwise addition was completed.

[0041] The analysis results showed that the conversion rate of ketone was 97.8%, and the selectivity of ketoxime was 99.3%.

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PUM

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Abstract

The invention relates to a method to produce oxime. Putting ketone, ammonia, hydrogen peroxide into the solvent that contains catalyst Ti-ECNU-1 molecular sieve, whisking and heating to take catalyzing compounding reaction, ketone would be gained. It has good catalyzing effect, no harmful to environment, easy post process, etc.

Description

technical field [0001] The invention relates to a method for producing oxime, in particular to a method for producing oxime by using titanium silicon molecular sieve, ketone, ammonia and hydrogen peroxide as catalyst and reaction system respectively, belonging to the technical field of organic chemical synthesis. Background technique [0002] At present, oximes are mainly synthesized by the reaction of hydroxylamine salts and ketones. This technique has two main disadvantages: (1) high hydroxylamine salt consumption; (2) generate a large amount of by-product inorganic salts simultaneously. This process is an environmentally unfriendly process. [0003] In order to solve the above problems, people have developed an environment-friendly synthesis process of oxime: using titanium-silicon molecular sieve as a catalyst, and using hydrogen peroxide and ammonia to ammoximate ketone to produce oxime. U.S. Patent No. 4,745,221 discloses a method for synthesizing cyclohexanone oxime...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C249/04C07C251/32B01J29/89
Inventor 吴鹏刘月明宋芬吴海虹何鸣元
Owner EAST CHINA NORMAL UNIV
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