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Method for preparing diepoxide by one-pot method

A technology of diepoxide and epoxidation reaction, which is applied in the direction of organic chemistry, can solve the problems of poor process safety and low conversion rate of raw materials, and achieve the effects of reducing the difficulty of process operation, saving solvents and reducing costs

Active Publication Date: 2020-04-10
INST OF CHEM ENG GUANGDONG ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved in the present invention is to overcome the defects and deficiencies of the existing epoxide preparation method, such as low conversion rate of raw materials and poor process safety, and provide a method for preparing diepoxide by a one-pot method. Diepoxide avoids the solvent distilled out by high vacuum in the traditional process, and does not need to separate the solid raw material of m-chloroperoxybenzoic acid, which reduces the difficulty of process operation, improves product yield and purity, increases process safety, and has Conducive to large-scale industrial production

Method used

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  • Method for preparing diepoxide by one-pot method

Examples

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Effect test

Embodiment 1

[0078] A kind of one-pot method prepares the method for diepoxide, comprises the steps:

[0079] S1. Epoxidation reaction: Add 10.04g of 1,5-hexadiene into the reactor at low temperature, slowly add m-chloroperoxybenzoic acid solution dropwise, control the rate of addition to keep the system temperature at about 10°C, and maintain React at low temperature for 4 hours, then raise the temperature to 20°C, react for 15 hours, and the reaction is completed to obtain a crude solution of diepoxide, wherein the molar ratio of diene to m-chlorobenzoyl chloride is 1:2.45;

[0080] S2. Separation and purification: add 125 g of 20% sodium sulfite aqueous solution to the crude diepoxide solution, keep the system temperature at 20° C., perform a reduction reaction for 2 hours, extract and separate the organic phase. Add 165g of 20% sodium bicarbonate solution by mass fraction to the organic phase, maintain the system at 20°C, neutralize for 3 hours, and extract the organic phase. Wash the...

Embodiment 2

[0086] A kind of one-pot method prepares the method for diepoxide, comprises the steps:

[0087] S1. Epoxidation reaction: Add 12.69g of 1,7-octadiene into the reactor at low temperature, slowly add m-chloroperoxybenzoic acid solution dropwise, control the rate of addition to keep the system temperature at about 10°C, and maintain React at low temperature for 4 hours, then raise the temperature to 23°C, react for 12 hours, and the reaction is completed to obtain a crude product solution of diepoxyoctane, wherein the molar ratio of diene to m-chlorobenzoyl chloride is 1:2.6;

[0088] S2. Separation and purification: Add 220 g of a 20% mass fraction of sodium bisulfite aqueous solution to the crude diepoxyoctane solution, keep the system temperature at 23° C., perform a reduction reaction for 2 hours, and extract and separate the organic phase. Add 220 g of 20% sodium carbonate solution in mass fraction to the organic phase, maintain the system at 23° C., neutralize for 2 h, ext...

Embodiment 3

[0094] A kind of one-pot method prepares the method for diepoxide, comprises the steps:

[0095] S1. Epoxidation reaction: Add 14.88g of 1,8-nonadiene into the reactor at low temperature, slowly add m-chloroperoxybenzoic acid solution dropwise, control the rate of addition to keep the system temperature at about 5°C, and maintain React at low temperature for 4 hours, then raise the temperature to 25°C, react for 12 hours, and the reaction is completed to obtain a crude solution of diepoxynonane, wherein the molar ratio of diene to m-chlorobenzoyl chloride is 1:2.5;

[0096] S2. Separation and purification: Add 235 g of 20% potassium bisulfite aqueous solution to the crude diepoxynonane solution, keep the system temperature at 22° C., perform a reduction reaction for 1 hour, and extract and separate the organic phase. Add 240 g of 22% potassium bicarbonate solution in mass fraction to the organic phase, maintain the system at 25° C., neutralize for 2 h, extract and separate the...

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Abstract

The invention discloses a method for preparing diepoxide by a one-pot method. The method comprises the following steps: S1, epoxidation reaction: adding dialkene into a reactor at a low temperature, slowly dropwise adding an m-chloroperoxybenzoic acid solution, and reacting to obtain a diepoxide crude product solution; and S2, separation and purification: adding a reducing agent aqueous solution into the diepoxide crude product solution, carrying out a reduction reaction, extracting to separate out an organic phase, carrying out a neutralization reaction, extracting to separate out an organicphase, washing with water, removing water, filtering, and carrying out reduced pressure distillation on filtrate to obtain the diepoxide. According to the invention, the traditional process of preparing a solvent through high vacuum distillation is prevented, an m-chloroperoxybenzoic acid solid raw material does not need to be separated, the diepoxide is obtained through the one-pot reaction of the dialkene and the m-chloroperoxybenzoic acid solution, the process operation difficulty is reduced, the safety is improved, the purity of the prepared diepoxide is 91% or above, the yield is 95% or above, and the large-scale industrial production is facilitated.

Description

technical field [0001] The invention relates to the technical field of preparation of epoxides, and more specifically, to a method for preparing diepoxides in one pot. Background technique [0002] Epoxy can be polymerized to form a cured product with excellent electrochemical, heat and humidity resistance. Among them, the polymer formed by polymerization of diepoxide as a key intermediate can be widely used in resists, coating agents, inks, adhesives, sealants, encapsulants, composite materials, optical materials, electronic materials, etc. multiple fields. At present, there are many methods for synthesizing diepoxides at home and abroad, and they are basically obtained by epoxidizing oxidants and dienes. Commonly used oxidants are hydrogen peroxide, peracetic acid, peroxyformic acid, peroxybenzoic acid, m-chloroperoxybenzoic acid, etc. When hydrogen peroxide is used as the oxidant, expensive catalysts such as phosphotungstate, titanium-containing silicon oxide, etc. are...

Claims

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Application Information

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IPC IPC(8): C07D301/14C07D303/04
CPCC07D301/14C07D303/04
Inventor 赵鹏张小春翁行尚吴正旭李宗沅陈伟健黄淋佳
Owner INST OF CHEM ENG GUANGDONG ACAD OF SCI
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