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Separation method for epichlorohydrin

A technology of epichlorohydrin and separation method, which is applied in the field of separation of epichlorohydrin, can solve the problem of high energy consumption, and achieve the effect of reducing energy consumption and good phase separation

Active Publication Date: 2013-12-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a low-energy-consumption separation method for epichlorohydrin in order to overcome the relatively high energy consumption problem in the existing separation method of epichlorohydrin, so that it can be applied 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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Embodiment 1

[0053] This embodiment is used to illustrate the separation method of epichlorohydrin provided by the present invention.

[0054] At 24°C, 100 parts by mass of the known solution S1 containing epichlorohydrin, methanol, 3-chloropropene and water was first mixed with 50 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 for stratification, collect the heavy phase of the lower layer, and then use 150 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) divided into five parts of equal mass and extracted the upper light phase five times, combined all the heavy phases to obtain the p-chloroanisole phase, epichlorohydrin, methanol in the p-chloroanisole phase , 3-chloropropene and water content are respectively 6.97 mass %, 1.24 mass %, 11.36 mass % and 0.21 mass %, the light phase obtained at last is the wat...

Embodiment 2

[0068] This embodiment is used to illustrate the separation method of epichlorohydrin provided by the present invention.

[0069] At 12°C, 100 parts by mass of the known solution S2 containing epichlorohydrin, methanol, 3-chloropropene and water was first mixed with 60 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 lower heavy phase, and then use 120 parts by mass of butyl chloroacetate (Ticier (Shanghai) Chemical Industry Development Co., Ltd., the density at 20°C is 1070.4 kg / cubic meter, the boiling point is 183 ℃) divided into five parts of equal mass and extracted the upper light phase five times, combined all the heavy phases to obtain the butyl chloroacetate phase, in the butyl chloroacetate phase, epichlorohydrin, methanol, 3- The contents of allyl chloride and water are respectively 5.96 mass %, 2.14 mass %, 20.68 mass % and 0.46 mass %, and the light phas...

Embodiment 3

[0081] This embodiment is used to illustrate the separation method of epichlorohydrin provided by the present invention.

[0082] At 13°C, 100 parts by mass of the known solution S3 containing epichlorohydrin, methanol, 3-chloropropene and water was first mixed with 60 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 for stratification, collect the heavy phase of the lower layer, and then use 100 parts by mass of p-chloroanisole (TSI (Shanghai) Chemical Industry Development Co., Ltd., the density at 20°C is 1160 kilogram / cubic meter, boiling point is 200 ℃) is divided into five parts of equal mass and extracts the light phase of the upper layer five times, and combines all the heavy phases to obtain the p-chloroanisole phase (that is, the organic solvent phase described in the present invention, and the same below ), the contents of epichlorohydrin, methanol, 3-chloropropene and water in the p-chloro...

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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 oxygen-containing no-halogen-containing organic solvent immiscible with water, 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. Good separation is easy to realize by using the separation method of the invention; the epichlorohydrin product can be obtained at the top of a distillation column by simple distillation, and the organic solvent is recovered from the bottom of the distillation column without evaporation; and compared with methods in which an extraction agent with a boiling point lower than that of epichlorohydrin is employed, the separation method of the invention helps to effectively reduce energy consumption.

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
Inventor 张永强刘易杜泽学
Owner CHINA PETROLEUM & CHEM CORP
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