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Preparation of high-purity chlorothalonil

A chlorothalonil, high-purity technology, applied in the preparation of protective bactericide chlorothalonil, and the field of preparation of high-purity chlorothalonil, can solve the problem of large processing workload, many control points for chlorine flow, and excessive chlorine flow and other problems, to achieve the effect of simple steps, reduction of chlorine control points, and strong process and operation practicability

Inactive Publication Date: 2017-08-18
JIANGSU WEUNITE FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The scheme proposed by CN201410740625.1 is to use modified coconut shell activated carbon as a catalyst, and the same two-step chlorine flow method is adopted for production. The disadvantages are that there are many control points for chlorine flow, the amount of chlorine flow is too large, and the workload of tail gas post-treatment is large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Put the measured amount of isophthalonitrile into the vaporizer for vaporization. After the isophthalonitrile is vaporized, it is taken out of the vaporizer by nitrogen gas and mixed with chlorine gas, and then enters the fluidized bed and fixed bed equipped with a special chlorination catalyst in turn. react. The molar ratio of the intake air is isophthalonitrile: nitrogen: chlorine = 1:2.5:4.2. The reaction temperature of the fluidized bed and the fixed bed are respectively controlled at 342°C and the pressure is 0.003MP. After the reaction is completed, the reaction mixture is sent to into the receiver, after condensing and drying to obtain chlorothalonil, the yield is 97.2%, the content is 99.5%, and HCB is 9.5ppm.

Embodiment 2

[0016] Put the measured amount of isophthalonitrile into the vaporizer for vaporization. After the isophthalonitrile is vaporized, it is taken out of the vaporizer by nitrogen gas and mixed with chlorine gas, and then enters the fluidized bed and fixed bed equipped with a special chlorination catalyst. react. The molar ratio of the intake air is isophthalonitrile: nitrogen: chlorine = 1:3:4.5. The reaction temperature of the fluidized bed and the fixed bed are respectively controlled at 345°C and the pressure is 0.003MP. After the reaction is completed, the reaction mixture is sent to into the receiver, after condensing and drying to obtain chlorothalonil, the yield is 97.3%, the content is 99.6%, and HCB is 9ppm.

Embodiment 3

[0018] Put the measured amount of isophthalonitrile into the vaporizer for vaporization. After the isophthalonitrile is vaporized, it is taken out of the vaporizer by nitrogen gas and mixed with chlorine gas, and then enters the fluidized bed and fixed bed equipped with a special chlorination catalyst. react. The molar ratio of the intake air is isophthalonitrile: nitrogen: chlorine = 1:4:5, the reaction temperature of the fluidized bed and the fixed bed are respectively controlled at 345°C, and the pressure is 0.004MP. After the reaction, the reaction mixture is sent to into the receiver, after condensing and drying to obtain chlorothalonil, the yield is 97.2%, the content is 99.7%, and HCB is 8ppm.

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Abstract

The invention discloses a preparation method of high-purity chlorothalonil. The preparation method is characterized in that metered isophthalonitrile is thrown into a vaporizer to be vaporized, vaporized isophthalonitrile is taken out of the vaporizer through nitrogen and mixed with chlorine, the mixture sequentially enters a fluidized bed and a fixed bed both containing a special chlorination catalyst, the molar ratio of the air inflow is as follows: isophthalonitrile:nitrogen:chlorine=1:(2-5):(4-5), the reaction temperatures of the fluidized bed and the fixed bed are controlled to be 340-350 DEG C, the pressure is 0.002-0.005 MP, and reaction mixed gas is fed into a collector after finish of reaction and condensed and dried to obtain chlorothalonil.

Description

technical field [0001] The invention belongs to the technical field of chemical production, and relates to a preparation method of protective fungicide chlorothalonil, in particular to the preparation of high-purity chlorothalonil. Background technique [0002] The chemical name of chlorothalonil is tetrachloroisophthalonitrile (2,4,5,6-tetrachloro-1,3-benzenedicyanonitrile). The pure product is a white odorless powder with a boiling point of 350°C and a melting point of 250-251°C. Slightly soluble in water, soluble in organic solvents such as xylene and acetone. The original powder contains 96% active ingredients, the appearance is light yellow powder, slightly irritating odor, stable to acid, alkali and ultraviolet rays. Low toxicity, it has obvious stimulating effect on rabbit eyes and cornea, and can cause corneal turbidity, which is irreversible, but has no such effect on human eyes. Stimulates the skin of a few people. Chlorothalonil is a non-systemic broad-spectrum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/51
CPCC07C253/30C07C255/51
Inventor 蒙健张松林
Owner JIANGSU WEUNITE FINE CHEM CO LTD
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