Separation method for epichlorohydrin

A technology of epichlorohydrin and separation method, which is applied in the field of epichlorohydrin separation, can solve the problems of difficult phase separation, high energy consumption of distillation separation, etc., achieve short phase separation time, reduce requirements and difficulty and ease of extraction operation Achieved effect

Active Publication Date: 2013-12-04
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0008] The purpose of the present invention is to overcome the problems of difficult phase separation in the extraction and separation process and relatively high energy consumption of distillation separation in the existing separation method of epichlorohydrin, and provide a method that is easy to phase separation in the extraction process and easy to use in the distillation process. Separation method of epichlorohydrin with low energy consumption, so as to facilitate the application in large-scale continuous production process

Method used

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  • Separation method for epichlorohydrin
  • Separation method for epichlorohydrin
  • Separation method for epichlorohydrin

Examples

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Effect test

Embodiment 1

[0069] This embodiment is used to illustrate the separation method of epichlorohydrin provided by the present invention.

[0070] At 28°C, 100 parts by mass of the known solution S1 containing epichlorohydrin, methanol, 3-chloropropene and water was mixed with 49.9 parts by mass of water (the density at 20°C was 998.2 kg / m3, The boiling point is 100°C) contacting and mixing, after standing to separate layers, collect the heavy phase of the lower layer, and then use 70.0 parts by mass of ethyl trichloroacetate (TCH (Shanghai) Chemical Industry Development Co., Ltd., the density at 20°C is 1383.6 kg / m3, the boiling point is 168°C) and 34.8 parts by mass of 3-chloropropene (industrial chloropropene, Baling Petrochemical Co., Ltd., the content of 3-chloropropene is 98 mass%, and the density at 20°C is 939.2 kg / m3, with a boiling point of 45°C), the mixed organic solvent is divided into five parts of equal mass and extracted five times to extract the upper light phase, and all the ...

Embodiment 2

[0084] This embodiment is used to illustrate the separation method of epichlorohydrin provided by the present invention.

[0085] At 15°C, 100 parts by mass of the known solution S2 containing epichlorohydrin, methanol, 3-chloropropene and water is first mixed with 50.1 parts by mass of water (the density at 20°C is 998.2 kg / m3, The boiling point is 100°C), contact and mix, after standing to separate layers, collect the heavy phase of the lower layer, and then use 40.0 parts by mass of ethyl trichloroacetate (TSI (Shanghai) Chemical Industry Development Co., Ltd., the density at 20°C is 1383.6 kg / m3, the boiling point is 168°C) and 49.9 parts by mass of 3-chloropropene (industrial chloropropene, Baling Petrochemical Co., Ltd., the content of 3-chloropropene is 98 mass%, and the density at 20°C is 939.2 kg / m3, with a boiling point of 45°C), the mixed organic solvent is divided into five parts of equal mass and extracted five times to extract the upper light phase, and all the h...

Embodiment 3

[0097] This embodiment is used to illustrate the separation method of epichlorohydrin provided by the present invention.

[0098] At 28°C, 100 parts by mass of the known solution S3 containing epichlorohydrin, methanol, 3-chloropropene and water was first mixed with 60.2 parts by mass of water (the density at 20°C was 998.2 kg / m3, The boiling point is 100°C) contacting and mixing, after standing to separate layers, collect the heavy phase of the lower layer, and then use 50.0 parts by mass of p-chloroanisole (TSI (Shanghai) Chemical Industry Development Co., Ltd., the density at 20°C is 1160 kg / m3, the boiling point is 200°C) and 49.9 parts by mass of 3-chloropropene (industrial 3-chloropropene, Baling Petrochemical Co., Ltd., the content of 3-chloropropene is 98% by mass, at 20°C Density is 939.2 kg / m3, boiling point is 45 ℃) the mixed organic solvent is divided into five parts of equal mass and extracted five times to extract the upper light phase, and combine all the heavy ...

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Abstract

A separation method for epichlorohydrin comprises: mixing a solution containing epichlorohydrin, methanol, 3-chloropropene and water and an extraction agent, separating to obtain a liquid phase rich in epichlorohydrin and a liquid phase rich in methanol, distilling the obtained the liquid phase rich in epichlorohydrin to obtain epichlorohydrin, wherein the extraction agent comprises water and an organic solvent immiscible with water, and the density difference between the organic solvent and water is at least 10 Kg/m<3>, the organic solvent is lower in methanol extraction capability and higher in epichlorohydrin extraction capability than water, and the organic solvent has a boiling point different with that of epichlorohydrin. The method has short separation time (less than 3 min) during extraction, so that the requirement on extractive separation equipment and the difficulty in extraction operation are reduced; also during distillation, only part of the extraction agent needs evaporative recovery, so that energy consumption is effectively reduced; and therefore, the method is quite suitable for large-scale continuous production.

Description

technical field [0001] The invention relates to a method for separating epichlorohydrin. Background technique [0002] Epichlorohydrin is an important basic organic chemical raw material and intermediate, widely used in the synthesis of epoxy resin, glycerin, chlorohydrin rubber, pharmaceuticals, pesticides, surfactants, plasticizers and other products. [0003] Epichlorohydrin can be prepared by epoxidizing hydrogen peroxide and 3-chloropropene by using titanium silicon molecular sieve as a catalyst. Since 3-chloropropene and hydrogen peroxide are immiscible, the reaction rate is slow, therefore, a large amount of solvent such as methanol needs to be added to make 3-chloropropene and hydrogen peroxide undergo epoxidation reaction in the solvent. The epoxidation reaction product obtained after solid-liquid separation with titanium-silicon molecular sieve usually contains excess reactant 3-chloropropene, solvent methanol, target product epichlorohydrin, hydrogen peroxide fee...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/32
CPCY02P20/50
Inventor 张永强刘易杜泽学
Owner CHINA PETROLEUM & CHEM CORP
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