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Method for preparing cyclohexanone oxime by ammoximation of cyclohexanone

A technology of cyclohexanone ammonia oxime and cyclohexanone oxime, which is applied in the field of preparation of cyclohexanone oxime by cyclohexanone ammonia oxime, can solve the problems of difficult control of reaction temperature, high equipment investment cost, large amount of waste water, etc., and achieve effective It is beneficial to large-scale industrial production, solves the separation problem, and increases the effect of filtering area

Inactive Publication Date: 2012-07-18
湖南兴鹏化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most foreign cyclohexanone ammoximation methods use large-particle titanium-silicon molecular sieves as catalysts, and a 5 μm porous plate is set in the reactor to intercept the catalyst. The separation effect is not good, and the broken catalyst is easy to block the orifice plate. Inconvenient, due to the limited volume of the reactor, the filter area of ​​the filter element is limited, it is difficult to carry out large-scale operation, and the reaction temperature is not easy to control
However, the domestic cyclohexanone ammoximation method uses 27.5% (wt) hydrogen peroxide as an oxidant, and the amount of wastewater treated after the large amount of water added is also large. In addition, the original powder of titanium-silicon molecular sieve is used as a catalyst. The dissolution and loss of the catalyst is serious, the separation of the catalyst is difficult, the design process of the reaction system is relatively complicated, the design accuracy of the filter is strict, and the investment cost of the equipment is high

Method used

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  • Method for preparing cyclohexanone oxime by ammoximation of cyclohexanone
  • Method for preparing cyclohexanone oxime by ammoximation of cyclohexanone
  • Method for preparing cyclohexanone oxime by ammoximation of cyclohexanone

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Experimental program
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Effect test

Embodiment 1

[0038] Concrete feed parameters and reaction conditions are as follows:

[0039] Cyclohexanone=100 gram / hour; Tertiary butyl alcohol=470 gram / hour; 27.5% (wt) hydrogen peroxide=140 gram / hour; The amount of ammonia is to maintain the concentration of ammonia in the reaction solution as about 2% (wt) (61 grams / hour); titanium silicon molecular sieve concentration = 2.0% (wt).

[0040] The average residence time of the materials in the reactor is 66 minutes, the reaction temperature is maintained at 85±1°C through jacket heat exchange, and the reaction pressure is maintained at 0.35MPa.

[0041] Its reaction result is as follows:

[0042] The conversion rate of cyclohexanone: 97.6%; the conversion rate of hydrogen peroxide: 100%; the reaction selectivity calculated by cyclohexanone: 99.7%; the effective utilization rate of hydrogen peroxide: 91.4%; the yield of cyclohexanone oxime: 97.3%.

Embodiment 2

[0044] Concrete feed parameters and reaction result are as follows:

[0045] Cyclohexanone=100 grams / hour; Tertiary butyl alcohol=470 grams / hour; 35% (wt) hydrogen peroxide=110 grams / hour; The amount of ammonia gas is to maintain the concentration of ammonia in the reaction solution to be about 2% (wt); Molecular sieve concentration = 2% (wt).

[0046] The average residence time of materials in the reactor is 70 minutes, the reaction temperature is controlled at 85±1°C, and the reaction pressure is maintained at 0.35MPa.

[0047] The result of the reaction is as follows:

[0048] The conversion rate of cyclohexanone: 98.1%; the conversion rate of hydrogen peroxide: 100%; the reaction selectivity in terms of cyclohexanone: 99.7%; the effective utilization rate of hydrogen peroxide: 91.4%; the yield of cyclohexanone oxime: 97.8%.

Embodiment 3

[0050] Concrete feed parameters and reaction result are as follows:

[0051] Cyclohexanone=100 gram / hour; Tertiary butyl alcohol=470 gram / hour; 50% (wt) hydrogen peroxide=76 gram / hour; The amount of ammonia gas is to maintain the concentration of ammonia in the reaction solution to be about 2% (wt); Molecular sieve concentration = 2% (wt).

[0052] The average residence time of materials in the reactor is 72 minutes, the reaction temperature is controlled at 85±1°C, and the reaction pressure is maintained at 0.35MPa.

[0053] The result of the reaction is as follows:

[0054] The conversion rate of cyclohexanone: 98.5%; the conversion rate of hydrogen peroxide: 100%; the reaction selectivity calculated by cyclohexanone: 99.6%; the effective utilization rate of hydrogen peroxide: 89.8%; the yield of cyclohexanone oxime: 98.1%.

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Abstract

The invention provides a method for preparing cyclohexanone oxime by ammoximation of cyclohexanone. According to the method, 5.0-100 mu m of titanium silicalite molecular sieve is used as a catalyst, the reaction temperature is controlled by using an external circulation heating mode, and a reaction product and the titanium silicalite molecular sieve are separated in an external circulating filter. Compared with the prior art, the method has the advantages that the device investment is low, the separation problem between the catalyst and the reaction product can be better solved, the utilization rates of a molecular sieve and a reaction device can be improved, the reaction effect is better under the condition that the concentration of the catalyst is the same, the control is more stable, the overhauling of the device is easier, and the effective utilization rate of hydrogen peroxide can reach 90% or so.

Description

technical field [0001] The invention relates to a method for ammoximation of cyclohexanone, and more particularly relates to a method for preparing cyclohexanone oxime by ammoximation of cyclohexanone using titanium silicon molecular sieve as a catalyst. Background technique [0002] Caprolactam is a monomer for the production of nylon 6, and is also an important chemical raw material, and the preparation step of cyclohexanone oxime by ammoximation of cyclohexanone is a key step in the production of caprolactam. [0003] At present, there are three process routes for industrial production of caprolactam: one is the production route of cyclohexanone-hydroxylamine, including traditional Raschig process, DSM / HPO process, BASF-NO reduction process, Inventa-NO reduction process, Allied cumene / phenol process and Capropol process; the second is the cyclohexane photonitrosation process of Toray Corporation of Japan; the third is the toluene process of SNIA Company of Italy. [0004...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/44C07C249/04
Inventor 刘怡宏邓联平卿光宗
Owner 湖南兴鹏化工科技有限公司
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