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Cyclohexanone oxime synthesis method

A technology of cyclohexanone oxime and cyclohexanone, applied in oxime preparation, organic chemistry, etc., can solve the problems of low concentration of hydroxylamine sulfate solution, high sulfate water content, organic dissolution loss, etc., to reduce the amount of evaporated water and improve diffusion Performance, the effect of reducing consumption

Active Publication Date: 2016-03-09
SINOPEC NANJING ENG & CONSTR +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually, the SO in the flue gas discharged from the factory 2 Low content, usually less than 5000ppm, when SO in the flue gas 2 When the concentration is low, the concentration of hydroxylamine sulfate solution, which is a by-product of ammonia flue gas desulfurization, is low, resulting in high water content of sulfate in the inorganic phase of the oximation process, high heat consumption and organic dissolution loss in the crystallization process.

Method used

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  • Cyclohexanone oxime synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Embodiment 1 (two-stage four anti-countercurrent oximation)

[0068] Such as figure 2 , the 95-110°C hydroxylamine sulfate solution produced by ammonia flue gas desulfurization is flashed at 82kPa (absolute pressure) to remove part of the water so that the concentration of the hydroxylamine solution is 1.76mol / L.

[0069] Add cyclohexanone and ammonium sulfate solution containing hydroxylamine sulfate to the first oximation reactor, the feed rate of cyclohexanone is 5.28mol / min, and the molar ratio of cyclohexanone: hydroxylamine sulfate in the first oximation reactor is 1.4 : 1, the hydroxylammonium sulfate amount in the solution is 3.77mol / min, and feeds a small amount of ammonia simultaneously, makes solution overflow to the second oximation reactor, continues to feed ammonia, temperature is maintained at 60 ℃, and pH value remains at about 4. The reaction liquid flows from the bottom of the second oximation reactor to the ammonium sulfate extraction separator, and ...

Embodiment 2

[0072] Example 2 (two-stage two reverse countercurrent oximation)

[0073] Such as image 3 , the 95-110°C hydroxylamine sulfate solution produced by ammonia flue gas desulfurization is flashed at 82kPa (absolute pressure) to remove part of the water so that the concentration of the hydroxylamine solution is 1.76mol / L.

[0074] Add cyclohexanone and ammonium sulfate solution containing hydroxylamine sulfate to the first oximation reactor, the feed rate of cyclohexanone is 5.28mol / min, and the molar ratio of cyclohexanone: hydroxylamine sulfate in the first oximation reactor is 1.4 : 1, the hydroxylammonium sulfate amount in the solution is 3.77mol / min, and feeds a small amount of ammonia simultaneously, makes solution overflow to the second oximation reactor, continues logical ammonia, by primary circulation pump reaction solution is extracted out, through primary The external circulation heat exchanger is cooled, the temperature is maintained at 60°C, and the pH value is mai...

Embodiment 3

[0090] The oximation method of Example 2 was adopted, except that the concentration of the hydroxylamine sulfate solution was 0.8 mol / L.

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Abstract

The invention discloses a cyclohexanone oxime synthesis method. In the process of preparing a flue gas desulfurization byproduct cyclohexanone oxime, sulfur dioxide in flue gas is absorbed by utilizing ammonia or ammonia water as an absorbent to prepare ammonium bisulfite, and the ammonium bisulfite serving as a raw material reacts with cyclohexanone by means of counter-current oximation to prepare cyclohexanone oxime. According to the method, by increasing the concentration of hydroxylamine sulfate and adding the organic solvent, the diffusion performance of a reaction system is improved and consumption of cyclohexanone is reduced; furthermore, due to the extraction effect of the organic solvent, the total content of cyclohexanone-oxime and cyclohexanone in the inorganic phase which leaves a cyclohexanone oxime synthesis system can be reduced to lower than 0.30wt%, and the yield of the cyclohexanone oxime synthesis reaction is increased.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a method for oximating cyclohexanone, in particular to a method for oximating cyclohexanone with hydroxylamine sulfate, a by-product of ammonia flue gas desulfurization. Background technique [0002] Cyclohexanone oxime is the key raw material of caprolactam, and caprolactam is an important monomer for the production of nylon 6 fiber (cotton) and nylon 6 engineering plastics, which are widely used in the fields of automobiles, ships, medical products, daily necessities, electronics and electronic components. Regardless of the currently widely used cyclohexanone ammoximation technology or HPO technology, the intermediate product in the production of caprolactam is cyclohexanone oxime, and the key technology is also the production of cyclohexanone oxime. Cyclohexanone oxime is transformed into caprolactam after rearrangement reaction. At present, the production of cyclohexa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/08C07C251/44
CPCC07C249/08C07C251/44
Inventor 杨春和李贤张鹏
Owner SINOPEC NANJING ENG & CONSTR
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