Preparation method for diacetylmonoxime

A technology of methyl ethyl ketone oxime and methyl ethyl ketone, which is applied in the field of chemical process, can solve the problems of low utilization rate of hydroxylamine sulfate, low product yield, high content of butanone, etc., and achieves easy operation and control, good mass transfer condition and long residence time short effect

Inactive Publication Date: 2007-10-24
QUZHOU JUHUA POLYAMIDE FIBER +1
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AI Technical Summary

Problems solved by technology

Though this technological method has improved the efficiency of equipment, hydroxylamine sulfate utilization rate is low, and butanone content is high in the butanone oxime product, and the yield of product is low

Method used

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  • Preparation method for diacetylmonoxime

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Experimental program
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Effect test

Embodiment 1

[0017] A butanone oxime plant adopts a two-stage countercurrent oximation process as shown in the attached figure, and its operating parameters are: the feed molar ratio of butanone and hydroxylamine sulfate is 1:1; 1 # The reaction temperature in the oximation reactor is 35°C-40°C, and the pH value is 5-5.5; 2 # The reaction temperature in the oximation reactor is 45°C-50°C, and the pH value is 3.5-4. The obtained butanone oxime product has a content of 99.9%, a water content of 0.02%, and a butanone content of 0.020%; the by-product ammonium sulfate contains hydroxylamine sulfate of 0.03 mg / l.

Embodiment 2

[0019] A butanone oxime plant adopts a two-stage countercurrent oximation process as shown in the attached figure, and its operating parameters are: the feed molar ratio of butanone and hydroxylamine sulfate is 1:1; 1 # The reaction temperature in the oximation reactor is 40°C-45°C, and the pH value is 4-4.5; 2 # The reaction temperature in the oximation reactor is 50°C-55°C, and the pH value is 3-3.5. The obtained butanone oxime product has a content of 99.9%, a water content of 0.02%, and a butanone content of 0.018%; the by-product ammonium sulfate contains hydroxylamine sulfate of 0.025 mg / l.

Embodiment 3

[0021] A butanone oxime plant adopts a two-stage countercurrent oximation process as shown in the attached figure, and its operating parameters are: the feed molar ratio of butanone and hydroxylamine sulfate is 1:1; 1 # The reaction temperature in the oximation reactor is 65°C to 70°C, and the pH value is 5 to 5.5; 2 # The reaction temperature in the oximation reactor is 70°C-75°C, and the pH value is 4-5. The obtained butanone oxime product has a content of 99.8%, a water content of 0.03%, and a butanone content of 0.022%; the by-product ammonium sulfate contains hydroxylamine sulfate of 0.035 mg / l.

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Abstract

The invention discloses a making method of butanone oxime, which comprises the following steps: adopting two-segment reflow oximation technique flow path with oximation reactor, oximation separator and oximation circulating pump; making the quantity of butanone surplus in the 1# oximation reactor; reacting sulfuric hydroxylamine completely; making the sulfuric hydroxylamine excess in the 2# oximation reactor; reacting the butanone completely; setting the molar rate of butanone and sulfuric hydroxylamine at 1: 1 in the whole flow path. The invention improves utilizing rate of raw material and simplifies the equipment, which shortens the staying time of material with good condition of mass transfer.

Description

technical field [0001] The invention relates to a process method for preparing butanone oxime by adopting two-stage countercurrent oximation, and belongs to the technical field of chemical process. Background technique [0002] At present, the domestic industrial production process of butanone oxime mainly adopts the discontinuous method, that is, a certain amount of butanone and hydroxylamine sulfate are added to the reactor, mixed for a certain period of time, neutralized by ammonia, and separated in the same reactor. Obtain butanone oxime. The process method has low equipment production efficiency, frequent operation changes, and large consumption of raw materials, resulting in poor product quality. [0003] Due to the low equipment efficiency of the discontinuous method, which affects the yield, domestic manufacturers also adopt a single-stage continuous oximation method for production. This method is to continuously add butanone and hydroxylammonium sulfate to the firs...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/36C07C249/08
Inventor 刘建青张坚国吕养心张家森罗晟陈幼坚茅志清吕俊英
Owner QUZHOU JUHUA POLYAMIDE FIBER
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