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Method for extracting epoxy chloropropane

An epichlorohydrin and extraction technology, applied in organic chemistry and other directions, can solve the problems of difficult separation, small density difference between oil and water phases, etc., to shorten the extraction time, ensure clarity without entrainment, and solve the problem of material separation.

Active Publication Date: 2020-12-11
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the problem that the oil-water phase density difference is small and the separation is difficult when 3-chloropropene is used as the extraction agent

Method used

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  • Method for extracting epoxy chloropropane
  • Method for extracting epoxy chloropropane
  • Method for extracting epoxy chloropropane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) Use two metering pumps to respectively mix the first extractant # and the phase to be extracted (3.57% of epichlorohydrin, 19.64% of methanol, 0.68% of 3-chloro-1,2-propanediol, 1-chloro-3-methyl Oxygen-2-propanol 0.47%, etc.) is pumped into the light phase and heavy phase inlets of the CTL-350 centrifugal extractor, the weight ratio of the feed oil phase to the water phase is 1 / 4, the speed is adjusted to 3000rpm, and the residence time is 60s The light phase I# and the heavy phase I# obtained from the outlet of the light phase and heavy phase at a jacket temperature of 30°C are clear and transparent without entrainment. Heavy phase I# composition: epichlorohydrin 0.67%, methanol 20.63%, 3-chloro-1,2-propanediol 0.68%, 1-chloro-3-methoxy-2-propanol 0.42%, centrifugal extraction efficiency 81%.

[0044] (2) Use an extraction tower (built-in structured packing) to perform tower extraction on the heavy phase I#, the extraction temperature is 30°C, the residence time ...

Embodiment 2

[0046] (1) The first extractant # and the phase to be extracted (6.57% of epichlorohydrin, 29.21% of methanol, 1.28% of 3-chloro-1,2-propanediol, 1-chloro-3-methyl Oxygen-2-propanol 0.23%, etc.) is pumped into the light phase and heavy phase inlets of the CTL-350 centrifugal extractor, the weight ratio of the feed oil phase to the water phase is 1 / 3, the speed is adjusted to 3200rpm, and the residence time is 30s , The light phase I# and heavy phase I# obtained from the outlet of the light phase and heavy phase at a jacket temperature of 40°C are clear and transparent without entrainment. Heavy phase I# composition: epichlorohydrin 0.87%, methanol 30.63%, 3-chloro-1,2-propanediol 1.37%, 1-chloro-3-methoxy-2-propanol 0.21%, centrifugal extraction efficiency 84.2%.

[0047] (2) Use an extraction tower (built-in structured packing) to perform column extraction on the heavy phase I#, the extraction temperature is 40 ° C, the residence time is 30 minutes, the heavy phase I#: 3-chl...

Embodiment 3

[0049] (1) The first extractant # and the phase to be extracted (epichlorohydrin 1.52%, methanol 10.29%, 3-chloro-1,2-propanediol 0.54%, 1-chloro-3-methyl Oxygen-2-propanol 0.38%, etc.) is pumped into the light phase and heavy phase inlets of the CTL-350 centrifugal extractor, the weight ratio of the feed oil phase to the water phase is 1 / 6, the speed is adjusted to 3500rpm, and the residence time is 120s The light phase I# and the heavy phase I# obtained from the outlet of the light phase and heavy phase at a jacket temperature of 25°C are clear and transparent without entrainment. Heavy phase I# composition: epichlorohydrin 0.33%, methanol 10.62%, 3-chloro-1,2-propanediol 0.49%, 1-chloro-3-methoxy-2-propanol 0.32%, centrifugal extraction efficiency 78.3%.

[0050] (2) Use an extraction tower (built-in structured packing) to perform tower extraction on the heavy phase I#, the extraction temperature is 25°C, the residence time is 120min, the heavy phase I#: 3-chloropropene=6:...

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Abstract

The invention discloses a method for extracting epoxy chloropropane, wherein the method is characterized in that centrifugal extraction and tower-type extraction are connected in series, and an extraction oil layer separated after tower-type extraction enters centrifugal extraction. The method greatly shortens the extraction time, ensures that the oil-water phase is clear and free of entrainment,and solves the problem of separation of two materials with approximate density difference; the tower-type extraction oil layer (light phase II) can be recycled to the centrifugal extraction process, and the dosage of the extractant 3-chloropropene is reduced by 50% or more.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and relates to an extraction method of epichlorohydrin in water phase, more specifically, relates to a method for recovering epichlorohydrin in water phase by a composite extraction method combining centrifugal extraction and tower extraction , the method has fast separation speed and high extraction efficiency. Background technique [0002] Epichlorohydrin is an important basic chemical raw material, which is mainly used in the production of epoxy resin, chlorohydrin rubber, glycerin, surfactant and other products. At present, there are two main industrial production methods of epichlorohydrin: chlorohydrin method and glycerin method. The main reaction process of the chlorohydrin method consists of three steps: high-temperature chlorination of propylene to obtain chloropropene, hypochlorous acidification of chloropropene to obtain dichloropropanol, and saponification of dichlo...

Claims

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Application Information

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IPC IPC(8): C07D303/08C07D301/32
CPCC07D303/08C07D301/32Y02P20/10
Inventor 孙诚徐林丁克鸿李明李幸霏吕丽胡钦邓小伟
Owner JIANGSU YANGNONG CHEM GROUP