Method for preparing cyclohexene oxide through hydrogen peroxide epoxidation

A technology of epoxycyclohexane and epoxidation, which is applied in chemical instruments and methods, organic chemistry, chemical recovery, etc., can solve the problems of insufficient satisfaction and small output, and achieve the effect of improving selectivity and reducing hydrolysis

Inactive Publication Date: 2009-12-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

This method of recovering epoxycyclohexane in the by-product has a small output, which is not enough to meet the increasing demand

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] 3.6g cyclohexene is dissolved in 40mL chloroform, adds 4g mass concentration 35% hydrogen peroxide aqueous solution, the catalyst of 0.3g [(CH 3 ) 3 C 8 h 17 N] 3 (PO 4 ) (WO 3 ) 4 ], 0.06g NaHCO 3 , At 65°C, after reacting for 2 hours, the conversion rate of cyclohexene was 97%, and the selectivity of cyclohexane was 98%.

Embodiment 2

[0013] 2.4g cyclohexene is dissolved in 40mL ethylene dichloride, adds 2g mass concentration 50% hydrogen peroxide aqueous solution, the catalyst of 0.19g [(CH 3 ) 3 C 16 h 33 N] 3 (PO 4 ) (WO 3 ) 4 ], 0.04g Na 2 HPO 3 , At 55°C, after reacting for 4 hours, the conversion rate of cyclohexene was 98%, and the selectivity of cyclohexane was 99%.

Embodiment 3

[0015] 1.2g cyclohexene is dissolved in 30mL methylene chloride, adds 1.6g mass concentration 30% hydrogen peroxide aqueous solution, the catalyst of 0.12g [(CH 3 ) 3 C 16 h 33 N] 3 (PO 4 ) (WO 3 ) 4 ], 0.03gNa 2 HPO 3 , At 45°C, after 7 hours of reaction, the conversion rate of cyclohexene was 97%, and the selectivity of epoxycyclohexane was 97%.

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PUM

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Abstract

The invention relates to a method for preparing cyclohexene oxide by directly taking hydrogen peroxide as an oxygen source and adopting the heteropolyacid salt mixture with reaction-controlled phase transfer catalysis property to catalyze cyclohexene epoxidation. Cyclohexene reacts with hydrogen peroxide under the action of a reaction-controlled phase transfer catalyst; through the regulation of additives, the conversion rate of cyclohexene is greater than 96 percent; the selectivity of hydrogen peroxide to cyclohexene is greater than 98 percent; after reaction ends, the hydrogen peroxide is separated and purified through atmospheric distillation; and the catalyst can be separated and recycled after the reaction ends.

Description

technical field [0001] The invention relates to a method for preparing epoxycyclohexane by catalytic epoxidation. Background technique [0002] Epoxycyclohexane is an important fine chemical raw material and intermediate, such as used in the synthesis of new pesticides Kemoite; unsaturated resins with high hardness, high temperature resistance, acid and alkali resistance; photosensitive materials; polycarbonate; Aldehydes, etc. With the continuous development of the use of epoxy cyclohexane, the demand for it is also increasing. [0003] At present, the method for preparing epoxycyclohexane by cyclohexene epoxidation is mainly divided into separation method and synthesis method: the separation method is mainly produced by recycling cyclohexanone and cyclohexanol in the process of cyclohexanone and cyclohexanol. A small amount of epoxy cyclohexane to obtain. Japan Nakahigashi [JP1975-95245] adopts alkali method to remove low boilers and convert them into high boilers to re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/12C07D303/04B01J31/02
CPCY02P20/584
Inventor 高爽吕迎张恒耘奚祖威
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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