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Liquid-phase fixed bed preparation method of cyclohexanone oxime

A cyclohexanone oxime, fixed bed technology, applied in oxime preparation, organic chemistry and other directions, can solve the problems of complex reaction process, unfriendly environment, difficult separation, etc., and achieve the effects of good selectivity, environmental friendliness and simple process

Inactive Publication Date: 2013-06-26
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of these production processes are: the reaction process is complicated, the flow process is long, and there are many by-products, especially involving SO 2 and NO and other substances harmful to the environment, and its production is an environmentally unfriendly process
[0006] So far, the ammoximation reaction of cyclohexanone catalyzed by different titanium-silicon molecular sieves has been reported using nano-sized titanium-silicon molecular sieve powder or micron-sized spray-formed titanium-silicon molecular sieve catalyst, which has disadvantages such as difficult separation during actual operation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] a. Preparation of catalyst

[0019] Mix Ti-MOR titanium silicon molecular sieve and activated carbon evenly, add water glass and appropriate amount of water, knead and shape, dry at 120°C for 10 hours, and then bake at 6000°C for 10 hours to form a granular catalyst. The mass ratio of Ti-MOR titanium silicon molecular sieve to activated carbon and water glass is 100:6:20.

[0020] b, the synthetic reaction of cyclohexanone oxime

[0021] A fixed-bed reactor is used, which is filled with the titanium-silicon molecular sieve granular catalyst prepared above, and when the temperature is raised to 70°C, cyclohexanone, hydrogen peroxide, ammonia and tert-butanol aqueous solution are continuously added to the fixed-bed reactor respectively, Carry out cyclohexanone oxime compound reaction under normal pressure, the cyclohexanone oxime that reaction generates is the reaction liquid of continuous discharge, wherein the mass concentration of hydrogen peroxide is 28%; The mass c...

Embodiment 2

[0026] a. Preparation of catalyst

[0027] Mix Ti-MWW titanium silicon molecular sieve and polyethylene glycol evenly, add silica sol and appropriate amount of water, knead and shape, dry at 120°C for 10 hours, and then bake at 6000°C for 10 hours to form a granular catalyst , the mass ratio of the Ti-MWW titanium silicate molecular sieve to polyethylene glycol and silica sol is 100:5:15.

[0028] b, the synthetic reaction of cyclohexanone oxime

[0029] A fixed-bed reactor is used, which is filled with the titanium-silicon molecular sieve granular catalyst prepared above, and when the temperature is raised to 60°C, cyclohexanone, hydrogen peroxide, ammonia and tert-butanol aqueous solution are continuously added to the fixed-bed reactor respectively, Carry out cyclohexanone oxime compound reaction under normal pressure, the cyclohexanone oxime that reaction generates is the reaction solution of continuous discharge, wherein the mass concentration of hydrogen peroxide is 35%...

Embodiment 3

[0034] a. Preparation of catalyst

[0035] Mix TS-1 titanium silicon molecular sieve and methyl cellulose evenly, add fuming silica gel and appropriate amount of water, knead and shape, dry at 120°C for 10 hours, and then bake at 6000°C for 10 hours to form granules For the catalyst, the mass ratio of the Ti-MOR titanium silicate molecular sieve to methylcellulose and fuming silica gel is 100:10:30.

[0036] b, the synthetic reaction of cyclohexanone oxime

[0037] A fixed-bed reactor is used, which is filled with the titanium-silicon molecular sieve granular catalyst prepared above, and when the temperature is raised to 75°C, cyclohexanone, hydrogen peroxide, ammonia and tert-butanol aqueous solution are continuously added to the fixed-bed reactor respectively, Carry out cyclohexanone oxime compound reaction under normal pressure, the cyclohexanone oxime that reaction generates is the reaction solution of continuous discharge, wherein the mass concentration of hydrogen pero...

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Abstract

The invention discloses a liquid-phase fixed bed preparation method of cyclohexanone oxime. The liquid-phase fixed bed preparation method has the characteristic that high-selectivity cyclohexanone oxime combination reaction is carried out on cyclohexanone, hydrogen peroxide, ammonia gas and a tertiary butanol aqueous solution in a fixed-bed reactor under the catalytic action of titanium silicalite molecular sieve, wherein the mass concentration of the hydrogen peroxide is 5%-50%; the mass concentration of the tertiary butanol aqueous solution is 30%-90%; the weight ratio of the cyclohexanone to the hydrogen peroxide to the ammonia gas to the tertiary butanol aqueous solution is 1:(0.35-1.74):(0.19-0.70):3. Compared with the prior art, the liquid-phase fixed bed preparation method of the cyclohexanone oxime is good in selectivity, high in conversion rate, capable of separating reaction liquid without catalyst, simple in process, capable of continuously charging and discharging, environment-friendly and easy for industrial implementation.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a liquid-phase fixed-bed preparation method of cyclohexanone oxime. Background technique [0002] Cyclohexanone oxime is an important intermediate in the synthesis of caprolactam. Caprolactam can be polymerized to produce nylon-6, and nylon-6 can be further processed into nylon fibers, plastic films and other engineering plastics. In addition, caprolactam is also a raw material for antiplatelet drugs such as 6-aminocaproic acid and lauryl amphetrol. 90% of caprolactam in the world is synthesized by reacting cyclohexanone and hydroxylamine salt to prepare cyclohexanone oxime, and then through Beckmann rearrangement reaction. Catalyzing the ammoximation reaction of cyclohexanone and the reaction process of catalyzing the Beckmann rearrangement of cyclohexanone oxime are the key processes for the production of caprolactam, and there have been major breakthroughs...

Claims

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Application Information

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IPC IPC(8): C07C251/44C07C249/04
Inventor 吴鹏吴静徐乐丁姜宏黄仕杰杨玉林吴海虹
Owner EAST CHINA NORMAL UNIV
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