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Preparation method of 2',2',4'-trichloroacetophenon

A technology of trichloroacetophenone and its production method, which is applied in the 2,2' field, can solve the problems of difficult separation and purification of hydrogen chloride gas, large environmental impact, and low product quality, and achieve simple and convenient separation and purification, high product quality, and reaction The effect of high speed and conversion rate

Inactive Publication Date: 2014-03-05
TAIZHOU KEYAN FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the production method of domestic production of 2,2',4'-trichloroacetophenone has a series of defects such as low product quality, difficult separation and purification of hydrogen chloride gas obtained from the reaction, and great impact on the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 2,2 ', the production method of 4'-trichloroacetophenone, comprises the steps:

[0017] a, first add 450 parts by weight of m-dichlorobenzene and aluminum trichloride of 600 parts by weight in the acylation kettle, after throwing in, raise the temperature of the material to 58°C;

[0018] b. Add 380 parts by weight of chloroacetyl chloride dropwise to the acylation kettle in step a within 2 hours, and keep the temperature at 58° C. during the dropwise addition;

[0019] c. After the dropwise addition of chloroacetyl chloride is completed, raise the temperature of the material to 80° C., and keep it warm for 3 hours;

[0020] d. Put the feed liquid after step c heat preservation reaction is completed into a hydrolysis kettle filled with 1800 parts by mass of dilute hydrochloric acid in advance, control the hydrolysis temperature to ≤90°C, and stand still for 30 minutes after hydrolysis;

[0021] e. The oil layer of the feed liquid reacted...

Embodiment 2

[0023] 2,2 ', the production method of 4'-trichloroacetophenone, comprises the steps:

[0024] a. First, add 500 parts by weight of m-dichlorobenzene and 680 parts by weight of aluminum trichloride in the acylation kettle, after finishing the feeding, raise the temperature of the material to 60°C;

[0025] b. Add 400 parts by weight of chloroacetyl chloride dropwise into the acylation kettle in step a within 3 hours, and keep the temperature at 60° C. during the dropwise addition;

[0026] c. After the dropwise addition of chloroacetyl chloride is completed, raise the temperature of the material to 90° C., and keep the temperature for 2.5 hours;

[0027] d. Put the feed liquid after step c heat preservation reaction is completed into a hydrolysis kettle filled with 2000 parts by mass of dilute hydrochloric acid in advance, control the hydrolysis temperature to ≤90°C, and stand still for 35 minutes after hydrolysis;

[0028] e. The oil layer of the feed li...

Embodiment 3

[0030] 2,2 ', the production method of 4'-trichloroacetophenone, comprises the steps:

[0031] a. First, add 550 parts by weight of m-dichlorobenzene and 750 parts by weight of aluminum trichloride in the acylation kettle, after finishing the feeding, raise the temperature of the material to 62°C;

[0032] b. Add 420 parts by weight of chloroacetyl chloride dropwise into the acylation kettle in step a within 2-4 hours, and keep the temperature at 62° C. during the dropwise addition;

[0033] c. After the dropwise addition of chloroacetyl chloride is completed, raise the temperature of the material to 100° C., and keep it warm for 2 hours;

[0034] d. Put the feed liquid after step c heat preservation reaction is completed into a hydrolysis kettle filled with 2200 parts by mass of dilute hydrochloric acid in advance, control the hydrolysis temperature to ≤90°C, and stand still for 40 minutes after hydrolysis;

[0035] e. The oil layer of the feed liquid rea...

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PUM

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Abstract

The invention discloses a preparation method of 2',2',4'-trichloroacetophenon and belongs to the field of organic synthesis. The technical scheme adopted by the invention is as follows: the preparation method of 2',2',4'-trichloroacetophenon comprises the following steps: adding 450-550 parts by weight of m-dichlorobenzene and 600-750 parts by weight of aluminum chloride into an acylation reactor, then raising the temperature of materials to 58-62 DEG C; dropwise adding 380-420 parts by weight of chloroacetyl chloride into the acylation reactor in 2-4 hours, and keeping the temperature at 58-62 DEG C; after dropwise adding, raising the temperature of the materials to 80-100 DEG C, and thermally reacting for 2-3 hours; putting the feed liquid after the thermal reaction into a hydrolysis reactor for hydrolyzing at a temperature not higher than 90 DEG C, and standing for 30-40 minutes after the hydrolysis, wherein 1800-2200 parts by weight of dilute hydrochloric acid is held in the hydrolysis reactor in advance; extracting an oil layer in the feed liquid after the reaction into a rinsing reactor for rinsing till the PH value of the feed liquid is 4-6, extracting an oil phase into a distiller, distilling a course product through negative pressure, dissolving by using a solvent, crystallizing, centrifuging and drying to acquire a finished product. The preparation method of 2',2',4'-trichloroacetophenon has the advantages that raw materials are easily available, the product yield is high, the product quality is good, resource conservation is facilitated, the environment friendliness is achieved.

Description

technical field [0001] The invention relates to a production method of 2,2',4'-trichloroacetophenone, which belongs to the field of organic synthesis. Background technique [0002] 2,2',4'-Trichloroacetophenone is a kind of off-white or light yellow crystalline powder. It is an important intermediate in the preparation of pesticides and medicines, mainly used in the production of miconazole nitrate, econazole nitrate and other drugs. [0003] At present, the production method of domestic production of 2,2',4'-trichloroacetophenone has a series of defects such as low product quality, difficulty in separation and purification of hydrogen chloride gas obtained from the reaction, and great impact on the environment. Therefore, be badly in need of providing a kind of new technical scheme to solve. Contents of the invention [0004] The purpose of the present invention is to address above-mentioned deficiencies, and a kind of raw material is easy to get, product quality i...

Claims

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Application Information

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IPC IPC(8): C07C49/80C07C45/46
CPCC07C45/46C07C49/80
Inventor 游培成
Owner TAIZHOU KEYAN FINE CHEM CO LTD
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