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Process method for producing high-purity chlorothalonil

A process method, the technology of chlorothalonil, is applied in the purification/separation of carboxylic acid nitrile, organic chemistry and other directions, which can solve the problems of complex operation process, unstable product quality, low degree of automation, etc., and achieve the effect of simple operation process.

Active Publication Date: 2018-07-27
TIANJIN SEPTECH SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the main refining methods are washing method and recrystallization method. Both of these two processes introduce a large amount of solvent, and additional solvent recovery is required. The operation process is complicated, the degree of automation is not high, and the product quality is unstable.

Method used

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  • Process method for producing high-purity chlorothalonil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The mass fraction of chlorothalonil in the raw material 7 is 95.2%, and the raw material 7 containing chlorothalonil isophthalonitrile, trichloroisophthalonitrile, pentachlorobenzonitrile, hexachlorobenzene and water first enters the light removal tower 1 , the operating reflux ratio of the tower is 20:1, a light component mixture containing a small amount of chlorothalonil is extracted from the top of the tower, and the bottom of the tower is a material that does not substantially contain light components (the mass content of light components is 0.008%) , this material enters product tower 2, and this tower operating reflux ratio is 2:1, and this tower tower tower top extracts the qualified product chlorothalonil, and tower bottom extracts the heavy component that contains a small amount of product (the chlorothalonil product quality content is 16 %). The mass fraction of the product chlorothalonil is 99.8%, and the yield is 92.2%.

[0034] In this embodiment, both th...

Embodiment 2

[0037] The mass fraction of chlorothalonil in the raw material 7 is 95.5%, and the raw material 7 containing chlorothalonil isophthalonitrile, trichloroisophthalonitrile, pentachlorobenzonitrile, hexachlorobenzene and water first enters the light removal tower 1 , the operating reflux ratio of the tower is 22:1, a light component mixture containing a small amount of chlorothalonil is extracted from the top of the tower, and the bottom of the tower is a material that does not substantially contain light components (the light component mass content is 0.006%) , this material enters product tower 2, and this tower operation reflux ratio is 2.4:1, and this tower tower top extracts the qualified product chlorothalonil, and the heavy component that contains a small amount of product is extracted at the bottom of the tower (the mass content of chlorothalonil product is 15 %). The mass fraction of the product chlorothalonil is 99.7%, and the yield is 93.4%.

[0038] In this embodimen...

Embodiment 3

[0041] The mass fraction of chlorothalonil in the raw material 7 is 94.7%, and the raw material 7 containing chlorothalonil isophthalonitrile, trichloroisophthalonitrile, pentachlorobenzonitrile, hexachlorobenzene and water first enters the light removal tower 1 , the operating reflux ratio of the tower is 16:1, a light component mixture containing a small amount of chlorothalonil is extracted from the top of the tower, and the bottom of the tower is a material that does not substantially contain light components (the light component mass content is 0.008%) , this material enters product tower 2, and this tower operation reflux ratio is 1.7:1, and this tower tower top extracts the qualified product chlorothalonil, and the heavy component that contains a small amount of product is extracted at the bottom of the tower (the mass content of chlorothalonil product is 18 %). The mass fraction of the product chlorothalonil is 99.6%, and the yield is 92.8%.

[0042]In this embodiment...

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Abstract

The invention provides a process method for producing high-purity chlorothalonil. The process method has the characteristics of comprising the steps of: sending raw materials containing chlorothalonilm-phthalodinitrile, trichloro-m-phthalodinitrile, pentachloro benzonitrile, hexachloro benzene and water to a light-component removing tower, collecting a mixture of the chlorothalonil containing light components with a mass fraction of <= 0.01% with heavy components from the tower bottom of the light-component removing tower, sending the mixture to a product tower, and collecting the chlorothalonil product with a mass fraction of >= 99.5% from the tower top of the product tower. According to the process method for producing the high-purity chlorothalonil, a rectification process method is adopted to refine the chlorothalonil, the operation process is simple, and the chlorothalonil product with a mass fraction of 99.5% or above can be obtained.

Description

technical field [0001] The invention belongs to the technical field of chemical separation, and in particular relates to a process for producing high-purity chlorothalonil. Background technique [0002] Chlorothalonil is a non-systemic broad-spectrum fungicide that has preventive effects on a variety of crop fungal diseases. At present, the main refining methods are washing method and recrystallization method. Both of these two processes introduce a large amount of solvent, and additional solvent recovery is required. The operation process is complicated, the degree of automation is not high, and the product quality is unstable. Contents of the invention [0003] In view of this, the present invention aims to propose a process for producing high-purity chlorothalonil, to overcome the defects of the prior art, adopt rectification process to refine chlorothalonil, the operation process is simple, and the mass fraction can be obtained In 99.5% or more chlorothalonil products...

Claims

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Application Information

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IPC IPC(8): C07C253/34C07C255/51
CPCC07C253/34C07C255/51
Inventor 王吉红王成强孙庆
Owner TIANJIN SEPTECH SCI & TECH
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