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Method for preparing epoxy cyclohexane

A technology of epoxy cyclohexane and cyclohexene, which is applied in the direction of organic chemistry, can solve the problems of catalyst loss, difficult operation, deterioration, etc., and achieve the effects of convenient recycling operation, prolonging the life, and increasing the amount of recycling

Active Publication Date: 2009-01-14
昌德新材科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, adding a reducing aqueous solution, such as Na 2 SO 3 、Na 2 S 2 o 3 , NaHSO 3 Treatment of excess oxygen sources - and these reducing substances are alkaline, which has a significant negative impact on the quantity and quality of catalyst precipitation
That is to say, these two methods have not substantially solved the problems of catalyst loss, deterioration and difficult operation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] In the four-necked flask of 500ml, add the catalyst of 1.0mol cyclohexene, 320mL ethanol and 2.00 grams [(C 2 h 5 ) 3 NCH 2 Ph] 2 HPMo 2 o 10 0.5 mol of 50% hydrogen peroxide aqueous solution (w / w) was added dropwise within 0.5 h. After reacting at 60 DEG C for 2.0 hours, the hydrogen peroxide content was 3.7%, and the catalyzer did not separate out; at this moment, the water phase was removed, and the oil phase continued to react for about 20 minutes. At this time, the catalyzer was separated out from the reaction system, and the catalyzer recovered by filtration (and dry metering). Unreacted raw material cyclohexene, acetonitrile and product epoxycyclohexane in the filtrate are rectified and separated. Repeat the above experiment with the recovered catalyst. In the process of repeating 9 times, the amount of catalyst recovered each time is about 0.94 times that of the last time. After 9 times, 1.08 grams of catalyst was recovered. The catalyst showed good catal...

Embodiment 2

[0015] In a four-necked flask of 500ml, add 0.5mol cyclohexene, 200mL pyrrolidone and 1.5 grams of catalyst [(C 2 h 5 ) 3 NCH 2 Ph] 2 HAs 2 o 10 0.3mol27.5% hydrogen peroxide aqueous solution (w / w) was added dropwise within 0.5h. After reacting at 40 DEG C for 2.5 hours, the hydrogen peroxide content was 5.5%, and the catalyzer did not separate out; at this moment, the water phase was removed, and the oil phase continued to react for about 30 minutes. At this moment, the catalyzer was separated out from the reaction system, and the catalyzer recovered by filtration (and dry metering). Unreacted raw material cyclohexene, acetonitrile and product epoxycyclohexane in the rectification filtrate. Repeat the above experiment with the recovered catalyst. In the process of repeating 9 times, the amount of catalyst recovered each time is about 0.97 times that of the last time. After 9 times, 1.47 grams of catalyst was recovered. The catalyst showed good catalytic activity throug...

Embodiment 3

[0017] at 6.0m 3 In the reactor, add 1.5m 3 Cyclohexene, 3m 3 Chloroform and the catalyst of 60kg [(C 2 h 5 ) 3 NCH 2 Ph] 2 HPMo 2 o 10 , add 0.75m within 2.0 hours 3 35% industrial hydrogen peroxide in water (w / w). Reacted at 45°C for 2.5 hours, the hydrogen peroxide content was 3.3%, and the catalyst did not precipitate; at this time, the water phase was removed from the specially designed overflow port of the reactor, and the oil phase was left in the kettle to continue the reaction for about 45 minutes. At this time, the catalyst It precipitated from the reaction system, and the catalyst was recovered by filtration. Unreacted raw material cyclohexene, acetonitrile and product epoxycyclohexane in the rectification filtrate. Return the recovered catalyst to the above-mentioned reaction kettle and repeat the test. In the process of repeating 9 times, 36.4 kg of catalyst was recovered after 9 times, and the average amount of catalyst recovered each time was about 0....

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PUM

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Abstract

The invention relates to a method for preparing cyclohexene oxide. The method is to take cyclohexene as a raw material, and hydrogen peroxide as an oxidizing agent, in the presence of a solvent and an additive, the cyclohexene oxide is prepared through the catalytic oxidation by a catalyst prepared by CN1204970C, and the method is characterized in that: in the process of oxidation reaction, a water phase is moved out from a reaction system after the oxidizing agent consumption is reduced to a certain extent, but an oil phase continues to react for a period of time until the catalyst is fully separated out. Compared with the CN 1401640A process, the method shortens the reaction time and also obviously increases the recovery rate of catalyst, and is suitable for the industrialized production.

Description

technical field [0001] The invention relates to a method for preparing epoxycyclohexane, in particular to provide a method for preparing epoxycyclohexane by catalytic oxidation of a catalyst prepared in CN1204970C. Background technique [0002] Cyclohexane oxide is an important fine chemical intermediate. It can be directly used as a reactive diluent for epoxy resins, and can be used to synthesize compounds such as cyclohexanediol, aminocyclohexanol, and adipaldehyde; it is also an important intermediate for high-efficiency and low-toxicity pesticides such as clofenac and some medicines. With the continuous development and utilization of epoxycyclohexane, its demand is also increasing rapidly. [0003] At present, there are methods for recovering a small amount of epoxycyclohexane from the by-products of the process of producing cyclohexanone and cyclohexanol from cyclohexane oxidation at home and abroad. Such as JP / 1975 / 95248 adopts alkali method to remove low boiling mat...

Claims

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Application Information

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IPC IPC(8): C07D303/04C07D301/12
Inventor 袁年武何嘉勇屈铠甲郑宏翠姜红军谢正堂蒋卫何建华肖海军高林辉夏立锋何双林
Owner 昌德新材科技股份有限公司
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