Method for preparing cyclohexene oxide by using micro flow field reaction technique

A technology of epoxy cyclohexane and microfluidic field, applied in organic chemistry and other directions, can solve the problems of difficult reaction control, high cost, low efficiency, etc., and achieve the effects of high yield and conversion rate, and easy and low-cost raw materials

Active Publication Date: 2015-08-05
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved in the present invention is to provide a method for preparing epoxycyclohexane by microflow field reaction technology, so as to solve the p

Method used

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  • Method for preparing cyclohexene oxide by using micro flow field reaction technique

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Embodiment 1

[0035]Inject the mixed solution of m-chlorobenzoyl chloride, hydrogen peroxide and sodium hydroxide into the first microstructure reactor of the microchannel modular reaction device, the molar ratio of m-chlorobenzoyl chloride and hydrogen peroxide is 1:4, hydrogen peroxide and hydrogen The molar ratio of sodium oxide is 1:1, and stay at 10°C for 0.5min; the output from the first microstructure reactor is mixed with the acidic dichloromethane solution and injected into the oil-water separation device, and the dichloromethane solution in the lower layer is mixed with cyclohexene After mixing, pass through the micro-mixer and the second micro-structure reactor successively, wherein the molar ratio of cyclohexene and m-chloroperoxybenzoic acid is controlled to be 1:1, stay at 20°C for 10 minutes, and the second micro-structure reactor exits The raw material was introduced into a separator, and the organic phase was washed with 5wt% sodium carbonate solution and distilled water to ...

Embodiment 2

[0037] Inject the mixed solution of m-chlorobenzoyl chloride, hydrogen peroxide and sodium hydroxide into the first microstructure reactor of the microchannel modular reaction device, the mol ratio of m-chlorobenzoyl chloride and hydrogen peroxide is 1:8, hydrogen peroxide and hydrogen The molar ratio of sodium oxide is 1:4, and stay at 40°C for 3 minutes; the output from the first microstructure reactor is mixed with acidic dichloromethane solution and injected into the oil-water separation device, and the dichloromethane solution in the lower layer is mixed with cyclohexene After passing through the micro-mixer and the second micro-structure reactor successively, the molar ratio of cyclohexene and m-chloroperoxybenzoic acid is controlled to be 1:6, and it stays at 40° C. for 20 minutes, and the second micro-structure reactor discharges Imported into a separator, the organic phase was washed with 5wt% sodium carbonate solution and distilled water to pH = 7.0, and dried to obta...

Embodiment 3

[0039] Inject the mixed solution of m-chlorobenzoyl chloride, hydrogen peroxide and sodium hydroxide into the first microstructure reactor of the microchannel modular reaction device, the mol ratio of m-chlorobenzoyl chloride and hydrogen peroxide is 1:6, hydrogen peroxide and hydrogen The molar ratio of sodium oxide is 1:2, and stay at 30°C for 2 minutes; the output of the first microstructure reactor is mixed with the acidic dichloromethane solution and injected into the oil-water separation device, and the dichloromethane solution in the lower layer is mixed with cyclohexene After passing through the micro-mixer and the second micro-structure reactor successively, the molar ratio of cyclohexene and m-chloroperoxybenzoic acid is controlled to be 1:4, and it stays at 30° C. for 15 minutes, and the second micro-structure reactor discharges Introduce it into a separator, wash the organic phase with 5wt% sodium carbonate solution and distilled water to pH = 7.0, and dry to obtain...

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Abstract

The invention discloses a method for preparing cyclohexene oxide by using a micro flow field reaction technique. According to the method, cyclohexene oxide is prepared from raw materials such as m-chlorobenzoyl chloride, an aqueous hydrogen peroxide solution and inorganic base in a microchannel modular reaction device. Compared with the prior art, the method is simple and easy to control, adopts easily available and cheap raw materials, is high in yield and percent conversion and can be put into industrial production favorably.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for preparing epoxycyclohexane by adopting a microflow field reaction technology. Background technique [0002] Epoxycyclohexane is a widely used organic intermediate, which has been used in the fields of surfactants, epoxy resins, paints, adhesives, medicines, pesticides and polymer materials. Due to the active epoxy group in the molecular structure of epoxycyclohexane, under the catalysis of acid or base, the epoxy group is prone to ring-opening reaction and reacts with ammonia, amine, alcohol, phenol, carboxylic acid, water and other substances Generate high value-added compounds. [0003] The preparation method of epoxycyclohexane mainly contains now: (1) organic peroxyacid method, but peroxyformic acid or acetic acid etc. are commonly used as oxidizing agent in this process, and peroxyacid is unstable, easy to decompose, difficult for storage, and the ...

Claims

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Application Information

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IPC IPC(8): C07D301/12C07D303/04
CPCC07D301/12C07D303/04
Inventor 郭凯方正何伟欧阳平凯
Owner NANJING UNIV OF TECH
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