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Preparation method of cyclohexanone oxime

A technology of cyclohexanone oxime and cyclohexanone, which is applied in oxime preparation, organic chemistry and other directions, can solve the problems of incomplete oximation reaction, poisoning of catalytic catalyst, and reduction of reaction efficiency.

Active Publication Date: 2010-07-07
CHINA PETROCHEM DEVMENT
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0004] However, there are disadvantages in this preparation method. When the design of the original oximation tower remains unchanged, when the operating conditions exceed the original design load range of the oximation tower, such as increasing the flow rate of hydroxylamine phosphate and cyclohexanone entering the oximation tower , or increase the concentration of hydroxylamine phosphate and cyclohexanone to increase the output of cyclohexanone oxime to increase its production per unit time, the problems it causes include: reducing the reaction efficiency, and the output cannot be improved
However, when the concentration of hydroxylamine phosphate entering the oximation tower is significantly increased or its flow rate is greatly increased, changing the feed position can lead to incomplete oximation reaction and increase the phosphate discharged from the bottom under the condition that the original equipment cannot be changed. The total carbonyl content of the inorganic treatment liquid poisons the catalytic catalyst in the hydroxylamine reactor

Method used

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  • Preparation method of cyclohexanone oxime
  • Preparation method of cyclohexanone oxime
  • Preparation method of cyclohexanone oxime

Examples

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preparation example Construction

[0013] The preparation method of the invention can be applied in the circulation process of hydroxylamine-oximation. In this cycle process, the phosphate inorganic treatment solution is used as the aqueous reaction medium of the entire cycle. In the hydroxylamine reactor, hydrogen is used to reduce nitrate ions to form hydroxylamine phosphate, and then pre-mixed with part of cyclohexanone in the pre-mixing reactor to reduce The concentration of phosphohydroxylamine is then entered into the oximation reactor for oximation reaction with cyclohexanone to produce cyclohexanone oxime; after removing organic impurities and supplementing the content of nitrate ions, the phosphate inorganic treatment solution is recycled back to hydroxylamine reactor for the next cycle of reaction. Such as figure 2 Shown, in this concrete example, use the hydroxylamine-oximation circulation process of the inventive method to comprise hydroxylamine reactor (10), premix tank (20), oximation tower (30)...

Embodiment 1

[0022] Repeat Comparative Example 1, but the inorganic treatment solution of hydroxylamine phosphate and part of the toluene solution of cyclohexanone are first fed into the premixing reactor in the same direction, and premixed at a temperature of 37 ° C and atmospheric pressure. In the mixed reaction liquid discharged from the premixed reactor, the concentration ratio of hydroxylamine phosphate is reduced to 45% of the original concentration.

[0023] The pre-mixed mixed reaction solution is fed from the top of the oximation tower, and another part of the toluene solution of cyclohexanone is fed from the bottom of the oximation tower. At a temperature of 51 ° C, the oximation reaction is carried out by countercurrent contact. The molar ratio of ketones (total of both parts) was 0.90. From the organic phase of the overflow discharge from the top of the oximation tower per unit time, 1.434 moles (162.0 grams) of cyclohexanone oxime are contained; The concentration is less than...

Embodiment 2

[0028] Repeat Comparative Example 2, but the inorganic treatment solution of hydroxylamine phosphate and part of the toluene solution of cyclohexanone are first fed into the premixing reactor in the same direction, and premixed at a temperature of 37°C and at atmospheric pressure. In the mixed reaction liquid discharged from the premixed reactor, the concentration ratio of hydroxylamine phosphate was reduced to 63% of the original concentration.

[0029] The pre-mixed mixed reaction solution is fed from the top of the oximation tower, and another part of the toluene solution of cyclohexanone is fed from the bottom of the oximation tower. At a temperature of 51°C, the oximation reaction is carried out by countercurrent contact. Hydroxylamine and cyclohexyl The molar ratio of ketones (total of both parts) was 0.90. In the organic phase of the overflow discharge from the top of this oximation tower per unit time, contain 1.614 (182.4 grams) cyclohexanone oxime, in the phosphate i...

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Abstract

The invention provides a cyclohexanone-oxime preparation method, which comprises the following steps: adding the cyclohexanone in the first part into the inorganic processing fluid with highly concentrated phosphoric acid oxyammonia in the non-reversion mode for premixing to reduce the density of the phosphoric acid oxyammonia below the 80 percent of the original density; then conducting oximation reaction between he the premixed inorganic processing fluid and the cyclohexanone in the second part. The cyclohexanone preparation method reduces the density of the phosphoric acid oxyammonia through the premixing of the inorganic processing fluid with highly concentrated phosphoric acid oxyammonia with the cyclohexanone, and then to conduct oximation reaction. Through the method, not only the density of the prepared cyclohexanone-oxime can be effectively increased, but the efficiency of the oximation reaction can be improved. The organic contents in the inorganic processing fluid can be reduced simultaneously.

Description

technical field [0001] The invention relates to a preparation method of cyclohexanone oxime. More specifically, the present invention relates to a method for preparing cyclohexanone oxime by using high-concentration hydroxylamine phosphate and cyclohexanone. Background technique [0002] Industrially, cyclohexanone oxime is an indispensable intermediate in the step of preparing caprolactam. In the current technical field, reacting cyclohexanone with hydroxylamine phosphate to obtain the corresponding oxime is the main method for preparing cyclohexanone oxime. Therefore, the preparation method of cyclohexanone oxime has a direct impact on the production cost and output of caprolactam. [0003] figure 1 It is a schematic diagram for illustrating the general hydroxylamine-oximation cycle, which includes the following equipment: hydroxylamine reactor (10), oximation tower (30), extraction tower (50), stripping tower (70), and nitric acid absorption tower ( 90). Inorganic tr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C249/08C07C251/42
Inventor 黄志达黄凯弘郑秀丽罗守礼
Owner CHINA PETROCHEM DEVMENT
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