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Method of preparing chlorothalonil with hexachlorobenzene content lower than 10ppm

A technology of hexachlorobenzene and chlorothalonil, applied in the field of pesticides, can solve problems such as easy wear, low conversion rate of raw materials, and reduced service life

Active Publication Date: 2015-03-25
JIANGYIN SULI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome a series of problems encountered in the current production of chlorothalonil, such as: excessive accumulation of residues, low conversion rate of raw materials, easy blockage of catalysts, easy wear and tear during use, and reduced service life, etc. The content of chlorobenzene is less than 10ppm, which meets the requirements of exporting to Europe and the United States

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～5

[0030] Embodiment 1~5 (activation of catalyst)

Embodiment 1

[0031] Embodiment 1 (do not add rare earth Lewis acid ytterbium chloride)

[0032] The coconut shell activated carbon (purchased from Jiangxi Tiantian Chemical Co., Ltd.) selected in embodiment 1, the granularity of the coconut shell activated carbon that fluidized bed adopts is 10~14 orders, and pore diameter is in The range of pore volume is 0.6ml / g, where the diameter is The proportion of pores is 70.4%; the particle size of the coconut shell activated carbon used in the fixed bed is preferably 6-8 mesh, and the pore diameter is The range of pore volume is preferably 0.62ml / g, where the diameter is The proportion of pores is preferably 67.5%. The above coconut shell activated carbon was impregnated to Cl - The solubility is 5mol / L in the metal chloride solution (ferric chloride FeCl 3 The concentration is 1mol / L, zinc chloride ZnCl 2 The concentration is 1mol / L), heated to 80°C, soaked for 30h, filtered out activated carbon, and dried to obtain modified activated c...

Embodiment 2

[0033] Embodiment 2 (only adding rare earth Lewis acid ytterbium chloride)

[0034] The coconut shell activated carbon (purchased from Jiangxi Tiantian Chemical Co., Ltd.) selected in embodiment 2, the particle size of the coconut shell activated carbon that fluidized bed adopts is 10~14 orders, and pore diameter is in The range of pore volume is 0.6ml / g, where the diameter is The proportion of pores is 70.4%; the particle size of the coconut shell activated carbon used in the fixed bed is preferably 6-8 mesh, and the pore diameter is The range of pore volume is preferably 0.62ml / g, where the diameter is The proportion of pores is preferably 67.5%. The above coconut shell activated carbon was impregnated to Cl - The solubility is 0.06mol / L in the metal chloride solution (ytterbium chloride YbCl 3 The concentration is 20mmol / L), heated to 80°C, soaked for 30h, filtered out activated carbon, and dried to obtain modified activated carbon (activated carbon used in fluidize...

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Abstract

The invention relates to a method of preparing chlorothalonil with hexachlorobenzene content lower than 10ppm. According to the method, modified coconut shell activated carbon is used as a catalyst, the chlorothalonil is prepared on a large scale by virtue of an improved composite bed process, and the content of hexachlorobenzene in a final product is lower than 10ppm. By adopting the method disclosed by the invention, the content of hexachlorobenzene in the final product is reduced to be lower than 10ppm, the conversation ratio of isophthalonitrile is increased to be not smaller than 96%, the purity of the tetrachloroisophthalonitrile product is increased to be not lower than 99%, the yield is increased to be not lower than 93%, the service life of activated carbon is over 600 hours, and the large-scale production of the chlorothalonil with hexachlorobenzene content lower than 10ppm is realized.

Description

technical field [0001] The invention relates to the field of pesticides, in particular to a method for preparing chlorothalonil with a hexachlorobenzene content lower than 10 ppm. technical background [0002] Chlorothalonil, i.e. tetrachloroisophthalonitrile, is a protective broad-spectrum fungicide, which has the characteristics of high efficiency, low toxicity, and low residue. It can prevent and treat fungal diseases of various crops, and has dual functions of protection and treatment. ; And it can be used as an antifungal agent for coatings, electrical appliances, leather, paper, cloth, etc. in industry. To produce chlorothalonil with isophthalonitrile as raw material, the most commonly used production processes include: fluidized bed, fixed bed and compound bed. Compared with the traditional addition of alumina, silica and other raw materials, adding activated carbon as a catalyst in the production process can increase the conversion rate of isophthalonitrile, reduce ...

Claims

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Application Information

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IPC IPC(8): C07C255/51C07C253/30B01J27/138B01J27/125
Inventor 黄岳兴缪金凤严秋钫王成宇
Owner JIANGYIN SULI CHEM
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