Preparation method for chlorothalonil

A technology of chlorothalonil and chlorine gas, which is applied in the preparation of organic compounds, carboxylic acid nitrile preparation, chemical instruments and methods, etc., can solve the problems of large amount of catalyst, uneven heat distribution, low conversion rate of chlorothalonil, etc., to achieve The effect of high utilization rate of raw materials, high product purity and low environmental pollution

Inactive Publication Date: 2012-10-10
张苏侠
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to overcome the defects of large amount of catalyst used in a single fluidized bed, low conversion rate of chlorothalonil; low thermal efficiency of a single fixed bed, uneven heat distribution, temperature difference in the bed, and difficult loading and unloading of the catalyst, the present invention adopts a fluidized bed first, Then fixed bed technology, this method can effectively overcome the shortcoming of single fluidized bed and fixed bed, and can produce the product chlorothalonil of good quality, the raw material that the present invention uses has isophthalonitrile, nitrogen, chlorine, special-purpose Ammonia oxidation catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Send a certain amount of isophthalonitrile into the vaporizer for vaporization. After the isophthalonitrile is vaporized, it is taken out of the vaporizer by nitrogen and mixed with chlorine in the mixer and then enters the fluidized bed. The molar ratio of the intake amount is isophthalonitrile Formonitrile: chlorine: nitrogen = 3: 8: 15, add a special ammoxidation catalyst at the same time, the amount is 2% of the total gas in the bed, adjust the temperature in the fluidized bed to 280 ° C, the pressure is 0.05Mpa, and react for 1 hour ; Send the reacted gas into the fixed bed, maintain the same temperature and pressure as the fluidized bed, and add the same catalyst and chlorine as the fluidized bed, so that the first reacted gas and chlorine react again , time 1 hour, after the reaction is over, the mixed gas after the reaction in the fixed bed is sent to the receiver, condensed and then dried to obtain chlorothalonil.

Embodiment 2

[0012] Send a certain amount of isophthalonitrile into the vaporizer for vaporization. After the isophthalonitrile is vaporized, it is taken out of the vaporizer by nitrogen and mixed with chlorine in the mixer and then enters the fluidized bed. The molar ratio of the intake amount is isophthalonitrile Formaldehyde: chlorine: nitrogen=3.5: 9: 16, add special ammoxidation catalyst simultaneously, the quantity is 2%-4% of the gas total amount in the bed, the temperature in the fluidized bed is adjusted to 290 ℃, pressure is 0.065Mpa, React for 1 hour; send the reacted gas into the fixed bed, keep the same temperature and pressure as the fluidized bed, and add the same catalyst and chlorine as the fluidized bed quantity, so that the gas and chlorine after the first reaction are re- One reaction takes place for 1 hour. After the reaction is over, the mixed gas after reaction in the fixed bed is sent to the receiver, condensed and then dried to obtain chlorothalonil.

Embodiment 3

[0014] Send a certain amount of isophthalonitrile into the vaporizer for vaporization. After the isophthalonitrile is vaporized, it is taken out of the vaporizer by nitrogen and mixed with chlorine in the mixer and then enters the fluidized bed. The molar ratio of the intake amount is isophthalonitrile Formonitrile: chlorine: nitrogen = 4: 10: 18, add a special ammoxidation catalyst at the same time, the amount is 4% of the total gas in the bed, adjust the temperature in the fluidized bed to 300 ° C, the pressure is 0.08Mpa, and react for 1 hour ; Send the reacted gas into the fixed bed, maintain the same temperature and pressure as the fluidized bed, and add the same catalyst and chlorine as the fluidized bed, so that the first reacted gas and chlorine react again , time 1 hour, after the reaction is over, the mixed gas after the reaction in the fixed bed is sent to the receiver, condensed and then dried to obtain chlorothalonil.

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Abstract

The invention discloses a preparation method for chlorothalonil, and belongs to the field of agricultural fungicide production. With chlorothalonil uses m-phthalonitrile, nitrogen, chlorine, and a special ammoxidation catalyst as raw materials, the preparation method for chlorothalonil uses fluidized bed and fixed bed technologies to obtain chlorothalonil. The reaction conditions are that the temperature of the fluidized bed and the fixed bed is in the range of 280 DEG C to 300 DEG C, the pressure is in the range of 0.05 to 0.08Mpa, the catalyst is the special ammoxidation catalyst with an amount of 2% to 4% of the total amount of gases in the beds, and the reaction time is one hour. The preparation method for chlorothalonil has the following advantages: the process is simple, utilization ratio of the raw materials is high, product purity is high, environmental pollution is little, and qualified chlorothalonil products can be produced.

Description

Technical field: [0001] The invention belongs to the field of agricultural fungicide manufacture, and in particular relates to a method for preparing chlorothalonil by using isophthalonitrile as a raw material. Background technique: [0002] Chlorothalonil pure product is white odorless powder, molecular formula: C 8 N 2 Cl 4 , the molecular weight is 265.91, the melting point is 250°C-251°C, the boiling point is 350°C, it is slightly yellow when it contains a small amount of impurities, it is stable under normal temperature storage conditions, it is stable to weak alkali or weak acid medium and light, and it is stable in strong alkali medium break down. Chlorothalonil is a high-efficiency and safe broad-spectrum fungicide. Its mechanism of action is: it can interact with glyceraldehyde triphosphate dehydrogenase in fungal cells, combine with the protein containing cysteine ​​in the enzyme, Thereby destroying the enzyme activity, destroying the metabolism of fungal cells...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/51C07C253/30
Inventor 张苏侠
Owner 张苏侠
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