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Refined monochloroacetic acid crystalline product complexometric extraction method

A technology of crystallization of chloroacetic acid, which is applied in the field of complex extraction and purification of monochloroacetic acid crystalline products, can solve the problems of low product purity and long separation time, and achieve the effect of high selectivity and low energy consumption

Inactive Publication Date: 2014-09-03
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has simple process, low investment, and is easy for industrial application, but the separation time is long and the product purity is low. Generally, the purity of monochloroacetic acid is about 99.0 wt%, and the content of dichloroacetic acid is about 0.3 wt%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1. Dissolve monochloroacetic acid crystals (the purity of monochloroacetic acid is about 99.0 wt%, and the purity of dichloroacetic acid is about 0.3 wt%) in deionized water to prepare an aqueous solution with a mass concentration of 120 g / L;

[0029] 2. Dissolve tri-n-octylamine and di-n-octylamine at a mass ratio of 100:1 in n-hexane to prepare an organic solution with a mass concentration of about 20 g / L;

[0030] 3. Add the organic solution prepared in step 2 to the aqueous solution prepared in step 1. The volume ratio of the organic solution to the aqueous solution is 1:1. Stir at the bottom for 0.5 h, stand and separate, the upper phase is the organic phase, and the lower phase is the water phase;

[0031] 4, in the water phase that obtains in step 3, add the normal hexane of 1 times water phase volume, at 25 Stir at the bottom for 0.5 h, let stand and separate, the upper phase is the organic phase, the lower phase is the water phase, and the water phase is tak...

Embodiment 2

[0037] 1. Dissolve monochloroacetic acid crystals (the purity of monochloroacetic acid is about 99.0 wt%, and the purity of dichloroacetic acid is about 0.3 wt%) in deionized water to prepare an aqueous solution with a mass concentration of 50 g / L;

[0038] 2. Dissolve tri-n-octylamine and di-n-octylamine with a mass ratio of 100:10 in n-hexane to prepare an organic solution with a mass concentration of about 300 g / L;

[0039] 3. Add the organic solution prepared in step 2 to the aqueous solution prepared in step 1. The volume ratio of the organic solution to the aqueous solution is 1:3. Stir at the bottom for 1 h, let stand and separate into layers, the upper phase is an organic phase, and the lower phase is an aqueous phase;

[0040] 4, in the aqueous phase that obtains in step 3, add the normal hexane of 3 times of aqueous phase volumes, at 25 Stir for 1 h at the bottom, let stand and separate, the upper phase is the organic phase, the lower phase is the water phase, and...

Embodiment 3

[0046] 1. Dissolve monochloroacetic acid crystals (the purity of monochloroacetic acid is about 99.0 wt%, and the purity of dichloroacetic acid is about 0.3 wt%) in deionized water to prepare an aqueous solution with a mass concentration of 90 g / L;

[0047] 2. Dissolve tri-n-octylamine and di-n-octylamine with a mass ratio of 100:5 in n-hexane to prepare an organic solution with a mass concentration of about 100 g / L;

[0048] 3. Add the organic solution prepared in step 2 to the aqueous solution prepared in step 1. The volume ratio of the organic solution to the aqueous solution is 1:2. Stir at the bottom for 1 h, let stand and separate into layers, the upper phase is an organic phase, and the lower phase is an aqueous phase;

[0049] 4, in the aqueous phase that obtains in step 3, add the normal hexane of 2 times of aqueous phase volumes, at 25 Stir for 1 h at the bottom, let stand and separate, the upper phase is the organic phase, the lower phase is the water phase, and th...

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PUM

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Abstract

The invention discloses a refined monochloroacetic acid crystalline product complexometric extraction method. The method comprises: first using the normal hexane solution of aliphatic amine to carry out complexometric extraction to obtain the water solution of the monochloroacetic acid crystalline product (quality purity about 99.0%), standing for layering with the upper phase being an organic phase and the lower phase being a water phase, then using the normal hexane to extract the water phase, and vaporizing the water phase to obtain a solid which is the refined monochloroacetic acid (quality purity above 99.9%). The key in the technology is the employed aliphatic amine is a mixture of tri-n-octylamine and di-n-octylamine. As a complexometric extraction agent, the mixture can effectively remove the main impurity of dichloroacetic acid in the monochloroacetic acid crystalline product.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation, and in particular relates to a method for refining monochloroacetic acid crystals through complex extraction. Background technique [0002] Monochloroacetic acid is an important intermediate in organic synthesis, and its application scope involves various sectors of the national economy such as medicine, dyes, pesticides, textile auxiliaries, and surfactants. Monochloroacetic acid is mainly synthesized by acetic acid catalyzed chlorination method, which has the advantages of simple production process and sufficient supply of raw material acetic acid. It is the most widely used and most common synthesis method in the world. Its disadvantage is that the reaction product cannot be completely controlled, and the product is a mixture of acetic acid, monochloroacetic acid and dichloroacetic acid, which needs further purification. The purification method used more abroad is hydrodehal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/16C07C51/48
Inventor 沈剑陈颍颍何潮洪陈冬璇陈新志钱超
Owner ZHEJIANG UNIV
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