Preparation process of high-purity trichloroacetone

A technology of trichloroacetone and preparation process, which is applied in the directions of hydrolysis to prepare carbonyl compounds, separation/purification of carbonyl compounds, organic chemistry, etc., can solve problems such as cost increase, environmental pollution, flammability, etc. Corrosion performance, the effect of improving selectivity

Inactive Publication Date: 2018-11-02
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 increa...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] S1: Mix 580kg of acetone and 600kg of ethylene glycol 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 6 mol / L concentrated sulfuric 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 monoch...

Embodiment 2

[0038] S1: Mix 550kg of acetone and 600kg of ethylene glycol 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 6 mol / L concentrated sulfuric 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 monochlo...

Embodiment 3

[0046] S1: Mix 500kg of acetone and 620kg of ethylene glycol 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 6 mol / L concentrated sulfuric 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 monoc...

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PUM

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Abstract

The invention relates to the technical field of production of chemicals, in particular to a preparation process of high-purity trichloroacetone, which can apparently increase the content of thetrichloroacetone in a crude product obtained in the one-step production of trichloroacetone, and can improve the purity of a product. The preparation process specifically comprises the following steps: S1: mixing acetone and ethylene glycol, adding accelerant, heating, uniformly stirring, and performing addition reaction; S2: introducing chlorine into a mixture prepared in step S1, adding a catalyst, uniformly stirring and mixing, and performing chlorination reaction; S3: adding concentrated sulfuric acid into the mixture prepared in step S2, performing hydrolysis to obtain a trichloroacetone crude product; S4: primarily purifying the trichloroacetone crude product prepared in step S3 by using water; S5: continuously secondary purifying the trichloroacetone crude product by using benzene; S6: performing tertiary purification for trichloroacetone by using alcohol; and S7: re-crystallizing a product processed in step S6 to obtain a trichloroacetone final product.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a process for preparing high-purity trichloroacetone. 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 a...

Claims

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Application Information

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IPC IPC(8): C07C45/78C07C45/81C07C45/42C07C49/16
CPCC07C45/78C07C45/42C07C45/81C07D317/12C07D317/16C07C49/16
Inventor 李仁峰
Owner 枣阳天燕硅普材料有限公司
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