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High-purity trichloroacetone production technology

A trichloroacetone and production process technology, applied in the field of high-purity trichloroacetone production process, can solve the problems of environmental pollution, cost increase, flammability, etc., achieve high corrosion resistance, increase service life, and improve selectivity.

Inactive Publication Date: 2018-12-14
枣阳天燕硅普材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of these organic solvents for recrystallization not only increases the cost, but also is flammable, explosive, and pollutes the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] S1: Mix 580kg of acetone and 600kg of glycerol in a tower reaction equipment, add 30kg of accelerator nickel into it, heat to 30°C, stir evenly, keep warm for 20min, and carry out addition reaction.

[0031] S2: Stop temperature control, keep the temperature at room temperature, then pass chlorine gas into the mixture prepared in S1 through the air pump and delivery pipeline, and add 25 kg of catalyst diethylamine, stir and mix, carry out chlorination reaction, and maintain the reaction for 1 hour.

[0032] S3: Add 5 L of 3 mol / L dilute nitric acid to the mixture after the chlorination reaction in S2 for hydrolysis to prepare crude trichloroacetone.

[0033] S4: Add water to the crude trichloroacetone prepared in S3, wherein the volume ratio of water to the crude trichloroacetone is 3:1, mix and stir evenly, and then let stand for 30 minutes for initial purification.

[0034] S5: Filtrate the mixture after S4 treatment, the filter residue is mainly monochloroacetone and...

Embodiment 2

[0038] S1: Mix 550kg of acetone and 600kg of glycerol in a tower reaction equipment, add 30kg of accelerator nickel into it, heat to 30°C, stir evenly, keep warm for 20min, and carry out addition reaction.

[0039] S2: Stop temperature control, keep the temperature at room temperature, then pass chlorine gas into the mixture prepared in S1 through the air pump and delivery pipeline, and add 20 kg of catalyst diethylamine, stir and mix, carry out chlorination reaction, and maintain the reaction for 1 hour.

[0040] S3: Add 5 L of 3 mol / L dilute nitric acid to the mixture after the chlorination reaction in S2 for hydrolysis to prepare crude trichloroacetone.

[0041] S4: Add water to the crude trichloroacetone prepared in S3, wherein the volume ratio of water to the crude trichloroacetone is 4:1, mix and stir evenly, and then let stand for 30 minutes for initial purification.

[0042] S5: Filter the mixture after S4 treatment, the filter residue is mainly monochloroacetone and d...

Embodiment 3

[0046] S1: Mix 500kg of acetone and 620kg of glycerol in a tower reaction equipment, add 30kg of accelerator nickel into it, heat to 30°C, stir evenly, keep warm for 20min, and carry out addition reaction.

[0047] S2: Stop temperature control, keep the temperature at room temperature, then pass chlorine gas into the mixture prepared in S1 through the air pump and delivery pipeline, and add 20 kg of catalyst diethylamine, stir and mix, carry out chlorination reaction, and maintain the reaction for 1 hour.

[0048] S3: Add 5 L of 3 mol / L dilute nitric acid to the mixture after the chlorination reaction in S2 for hydrolysis to prepare crude trichloroacetone.

[0049] S4: Add water to the crude trichloroacetone prepared in S3, wherein the volume ratio of water to the crude trichloroacetone is 3.5:1, mix and stir evenly, and then let stand for 30 minutes for initial purification.

[0050]S5: Filtrate the mixture after S4 treatment, the filter residue is mainly monochloroacetone an...

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PUM

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Abstract

The invention relates to the technical field of chemical production, in particular to a high-purity trichloroacetone production technology which can significantly increase the content of trichloroacetone in a crude product obtained by one-step production of trichloroacetone and improve the product purity. The technology specifically comprises the following steps: S1: mixing acetone with glycerin,adding a promoter thereto, heating, stirring uniformly, and performing an addition reaction; S2: introducing chlorine into a mixture prepared in the S1, adding a catalyst, stirring, mixing uniformly,and performing a chlorination reaction; S3: adding acid into the mixture prepared in the S2 for hydrolysis to prepare crude trichloroacetone; S4: performing initial purification on the crude trichloroacetone prepared in the S3 with water; S5: continuously performing secondary purification on the crude trichloroacetone with benzene; S6: performing third-time purification on the crude trichloroacetone with alcohol; and S7: recrystallizing a product treated in the S6 to obtain a final product of trichloroacetone.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a high-purity trichloroacetone production process. Background technique [0002] Trichloroacetone is the main raw material of folic acid crude product, and its stable quality is the guarantee of folic acid quality. However, the content of trichloroacetone on the domestic market is mostly about 50%, and the price of higher-quality trichloroacetone is more than twice that of common trichloroacetone. In actual production, trichloroacetone is extracted with water to remove high chlorine and low chlorine in trichloroacetone, which not only consumes a lot of water, but also contains a part of low chlorine in the trichloroacetone aqueous extract, which affects the reaction of crude products . [0003] Related literature, Journal of Jiangsu Broadcasting University, 2002, 13 (6): 57-58 reported the preparation method of high-purity trichloroacetone, but only stated that addi...

Claims

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Application Information

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IPC IPC(8): C07C45/29C07C49/16C07C45/80C07C45/81C07C45/78
CPCC07C29/143C07C29/62C07C45/29C07C45/78C07C45/80C07C45/81C07C31/10C07C31/34C07C49/16
Inventor 李仁峰
Owner 枣阳天燕硅普材料有限公司
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