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Preparation method for cyclohexanone oxime

A technology of cyclohexanone oxime and cyclohexanone peroxide, applied in oxime preparation, organic chemistry, etc., can solve the problems of product separation and purification interference, complicated process, complicated reaction, etc., and achieve easy recycling and reuse, and mild reaction conditions , The effect of simple reaction system

Active Publication Date: 2017-10-10
HUNAN INSTITUTE OF ENGINEERING +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But these several methods all have some shortcomings: hydroxylamine sulfate method, reaction generates a large amount of ammonium sulfate impurity, has caused very big interference to the separation and purification of product; Nitric oxide reduction method, equipment scale is high, and investment is too large; Phosphoric acid The hydroxylamine method consumes a lot of raw materials, takes a long time, the process is complicated, and the operation is cumbersome; the ammoximation method has complicated reactions and difficult separation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In the mixed solution of cyclohexanone peroxide, ammonia water and catalyst used in this embodiment, the molar ratio of cyclohexanone peroxide to ammonia is 1:3, and the mass concentration of titanium silicon molecular sieve is 2.5%.

[0022] Add 5.0 g cyclohexanone peroxide, 15.20 g ammonia water, and 0.5 g titanium-silicon molecular sieve into a stirred glass reactor, then stir, and react at 70°C for 3 h. Separation and purification yielded the target product cyclohexanone oxime.

[0023] After analysis and calculation, the conversion rate of cyclohexanone peroxide is 67.46%, and the selectivity of cyclohexanone oxime is 89.64%.

Embodiment 2

[0025] In the mixed solution of cyclohexanone peroxide, ammonia water and tert-butanol used in this embodiment, the molar ratio of cyclohexanone peroxide to ammonia is 1:3, the volume ratio of tert-butanol and water is 1:2, titanium silicon The mass concentration of molecular sieve is 2.5%.

[0026] Add 15.20 g of ammonia water, 5 g of cyclohexanone peroxide, 21.28 mL of tert-butanol, and 0.93 g of titanium-silicon molecular sieve into a stirred glass reactor, stir, heat to 70°C, and react for 12 hours. The obtained liquid is homogeneous, and the target product cyclohexanone oxime is obtained after separation and purification.

[0027] After analysis and calculation, the conversion rate of cyclohexanone peroxide was 87.26%, and the selectivity of cyclohexanone oxime was 90.98%.

Embodiment 3

[0029] In the mixed solution of cyclohexanone peroxide, ammonia water and tert-butanol used in this embodiment, the molar ratio of cyclohexanone peroxide to ammonia is 1:3, the volume ratio of tert-butanol and water is 1:2, titanium silicon The mass concentration of molecular sieve is 2.5%.

[0030] Add 15.20 g of ammonia water, 5 g of cyclohexanone peroxide, 21.28 mL of tert-butanol, and 0.93 g of titanium-silicon molecular sieve into a stirred glass reactor, stir, heat to 70°C, and react for 10 h. The obtained liquid is homogeneous, and the target product cyclohexanone oxime is obtained after separation and purification.

[0031] After analysis and calculation, the conversion rate of cyclohexanone peroxide is 89.25%, and the selectivity of cyclohexanone oxime is 91.25%.

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Abstract

The invention discloses a preparation method for cyclohexanone oxime. A titanium silicalite molecular sieve is taken as catalyst, cyclohexanone peroxide and ammonium hydroxide react under a moderate condition, and organic solvents including tertiary butanol, cyclohexane and the like can be added. The reaction of the preparation method is finished in one step, a reaction system is very simple, and the conversion rate of the cyclohexanone peroxide and the selectivity and the yield of the cyclohexanone oxime are relatively high. The preparation method has the advantages of moderate reaction condition, easiness in control and simple subsequent processing. The related catalyst is the titanium silicalite molecular sieve which is easy in recovery and reuse, in addition, few by-products are generated in reaction, and therefore, the preparation method has a good industrial application prospect.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of cyclohexanone oxime. Background technique [0002] Cyclohexanone oxime appears as a white prismatic crystal at room temperature, and its molecular formula is: C 6 h 11 NO, with a relative molar molecular mass of 113.16 g / mol, melts when heated to 89~90°C, boils at 206~210°C, and has a relative density of 1.1 g / cm 3 , larger than water, generally stored in airtight containers, and keep the surrounding environment cool, dry and ventilated. [0003] As an intermediate in the synthesis of caprolactam, cyclohexanone oxime is an important chemical raw material for the production of nylon-6 chips, nylon fibers, engineering plastics and plastic films. It is widely used in scientific research, medical care and even daily life. . [0004] There are four main methods for preparing cyclohexanone oxime at home and abroad: hydroxylamine sulfate method (HSO method), ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/04C07C251/44
CPCC07C249/04C07C251/44
Inventor 刘华杰刘平乐罗和安符雅芬张帆王聪
Owner HUNAN INSTITUTE OF ENGINEERING
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