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Method for purifying tetrachloroisophthalonitrile crystal

A technology of tetrachloroisophthalonitrile and tetrachloroisophthalonitrile is applied in the field of tetrachloroisophthalonitrile crystallization and purification, and achieves the effects of simple operation, high purification rate and high biological activity

Active Publication Date: 2014-07-16
JIANGSU XINHE AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the international market has significantly improved the internal quality requirements of chlorothalonil. In addition to the content and appearance, it is particularly emphasized that the content of the harmful substance hexachlorobenzene should be less than 10 mg / kg. There is no report that such a product can be produced during the reaction process. products, so only refined and purified methods can be used

Method used

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  • Method for purifying tetrachloroisophthalonitrile crystal
  • Method for purifying tetrachloroisophthalonitrile crystal

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Embodiment 1

[0013] A method for tetrachloroisophthalonitrile crystallization purification, the flow chart of the method is as figure 1 Shown, comprise the following steps: the raw material tetrachloroisophthalonitrile that contains harmful substance hexachlorobenzene is placed in the dissolving kettle that toluene is housed, the weight percent concentration of tetrachloroisophthalonitrile is 90%, harmful substance The content of hexachlorobenzene is 40mg / kg, and the stirring device is turned on to stir and mix, then the temperature in the dissolution tank is raised to 85°C, and the heat preservation reaction is carried out for 1h, then the temperature of the dissolution tank is lowered to 20°C with cooling water, and finally separated by a centrifuge to obtain After the wet material is dried, the finished product tetrachloroisophthalonitrile is obtained. The centrifuged residual liquid is collected through precipitation, and the remaining part is condensed in a condenser, and then placed i...

Embodiment 2

[0026] A method for crystallization and purification of tetrachloroisophthalonitrile, the method comprises the following steps: placing the raw material tetrachloroisophthalonitrile containing the harmful substance hexachlorobenzene in a dissolution tank equipped with toluene, and tetrachloroisophthalonitrile The weight percent concentration of dinitrile is 95%, the harmful substance hexachlorobenzene content is 200mg / kg, and the stirring device is turned on to stir and mix, then the temperature in the dissolving tank is raised to 90°C, and the heat preservation reaction is carried out for 1.5h, and then cooled with cooling water. The temperature of the dissolution kettle is lowered to 30°C, and finally separated by a centrifuge, and the obtained wet material is dried to obtain the finished tetrachloroisophthalonitrile.

Embodiment 3

[0028] A method for crystallization and purification of tetrachloroisophthalonitrile, the method comprises the following steps: placing the raw material tetrachloroisophthalonitrile containing the harmful substance hexachlorobenzene in a dissolution tank equipped with toluene, and tetrachloroisophthalonitrile The weight percent concentration of dinitrile is 92%, and the content of harmful substance hexachlorobenzene is 150 mg / kg. Turn on the stirring device to stir and mix, then raise the temperature in the dissolution tank to 88 ° C, keep the temperature for 1.5 hours, and then use cooling water to dissolve The temperature of the dissolution kettle was lowered to 25°C, and finally separated by a centrifuge, and the obtained wet material was dried to obtain the finished tetrachloroisophthalonitrile.

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Abstract

The invention relates to a method for purifying tetrachloroisophthalonitrile crystal, which comprises the following steps of: putting a harmful substance-containing raw material tetrachloroisophthalonitrile into a dissolving kettle filled with an organic solvent, and starting a stirring device for stirring and mixing; raising the temperature in the dissolving kettle to between 85 and 90 DEG C, keeping the temperature and reacting for 1 to 1.5 hours, and reducing the temperature of the dissolving kettle to between 20 and 30 DEG C by using cooling water; and finally, separating by using a centrifugal machine, drying the obtained wet material to prepare finished tetrachloroisophthalonitrile. Compared with the prior art, the method has the advantages of simple operation, higher purification rate, high bioactivity of the obtained product, purity of more than or equal to 99 percent, yield of more than or equal to 95 percent, main impurity hexachlorobenzene content of less than or equal to 10mg / kg and dimethylbenzene undissolved substance content of less than 0.3 percent.

Description

technical field [0001] The invention relates to a method for crystallization and purification, in particular to a method for crystallization and purification of tetrachloroisophthalonitrile. Background technique [0002] Tetrachloroisophthalonitrile is obtained by chlorination of isophthalonitrile in a fluidized bed. Tetrachloroisophthalonitrile, the English name is chlorothalonil, and the common name is chlorothalonil. It is a broad-spectrum fungicide with high efficiency and low toxicity. Its main function is to prevent crops from being infected by fungi; Agents, fruit preservatives, fungicides, protective agents for coatings and adhesives. At present, the international market has significantly improved the internal quality requirements of chlorothalonil. In addition to the content and appearance, it is particularly emphasized that the content of the harmful substance hexachlorobenzene should be less than 10 mg / kg. There is no report that such a product can be produced du...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/51C07C253/34A01N37/34A01P3/00
Inventor 陆正松胡清
Owner JIANGSU XINHE AGROCHEM
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