Method for preparing weedicide diuron

A technology of diuron and herbicide, applied in the field of herbicide preparation, can solve the problems of unreasonable catalyst, high cost of preparation method, low synthesis yield, etc., and achieve the effect of low cost, environment-friendly and reasonable synthesis process

Inactive Publication Date: 2012-08-01
LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The catalyst used in the preparation method of diuron in the prior art is unreasonable, so that the synthesis yield is low and the cost of the preparation method is high

Method used

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  • Method for preparing weedicide diuron

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1, a kind of method for preparing herbicide Diuron, its specific steps are as follows:

[0015] (1) Add an appropriate amount of aromatic compound solvent into a reaction kettle equipped with an exhaust gas treatment system, stirring, a condenser, a vent pipe, and a thermometer, cool to -15°C, and pass in phosgene for 0.5 hours; stop cooling, and add an appropriate amount The catalyst dimethylformamide; at the same time, continue to pass phosgene, and slowly drop into the solution composed of 3,4-dichloroaniline and aromatic compound solvent, as the reaction progresses, the temperature slowly rises to 20 ° C, and ~50°C, 0.5~2.0 hours to complete the dropwise addition; after dropping, keep stirring below 20°C for 0.4 hours, stop passing phosgene; then add an appropriate amount of co-catalyst triethylenediamine and the same aromatic compound as above to form a solution; slowly Heat to 90°C and keep it warm for 4 hours. After the heat preservation is over, nitro...

Embodiment 2

[0017] Embodiment 2, a kind of method for preparing herbicide Diuron, its specific steps are as follows:

[0018] (1) Add an appropriate amount of aromatic compound solvent into a reaction kettle equipped with an exhaust gas treatment system, stirring, a condenser tube, a vent tube, and a thermometer, cool to -30°C, and pass in phosgene for 2.0 hours; stop cooling and add an appropriate amount The catalyst dimethylformamide; at the same time, continue to pass through phosgene, and slowly drop into the solution composed of 3,4-dichloroaniline and the same aromatic compound solvent as above. As the reaction progresses, the temperature slowly rises to 20°C , and drop it at 20-50°C within 0.5-2.0 hours; after dropping, keep stirring below 50°C for 1.0 hour, stop passing through phosgene; then add an appropriate amount of cocatalyst triethylenediamine and the same aromatic compound as above Form a solution; slowly heat to 100°C and keep it warm for 4.0 hours; pass through nitrogen,...

Embodiment 3

[0020] Example 3, in the method for preparing the herbicide Diuron described in Example 1 or 2: the mass ratio of the raw material 3,4-dichloroaniline to dimethylamine is 1:1.00.

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Abstract

The invention provides a method for preparing weedicide diuron. The method is characterized in that aromatic compound solvents are added in a reaction kettle, cooling and phosgene introduction are carried out, less dimethylformamide is added, 3, 4-dichloro phenylamine solution is dripped, and cocatalyst triethylene-diamine is added after the dripping completion; the temperature is raised to 80 to 100 DEG C, and the stirring is carried out under the heat insulation condition; solution consisting of 3, 4-dichloro phenyl isocyanate and the aromatic compound solvents is obtained through the reaction; and partial solvents are removed through evaporation, then, 40-percent dimethylamine is dripped, and dinitramine is prepared. Because the catalyst dimethylformamide and the cocatalyst triethylene-diamine are used in the reaction in the method provided by the invention, so the total yield of the synthesized dinitramine is higher than 91 percent, and the purity of the dinitramine raw medicine is higher than 99 percent. The synthesis process provided by the invention is more reasonable, the cost is low, the quality is high, a better environment-friendly effect is realized, the safety is higher, the international standard is reached, and the method is more suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for preparing a herbicide, in particular to a method for preparing the herbicide diuron. Background technique [0002] Diuron’s English common name is Diuron, its chemical name is N-(3,4-dichlorophenyl)-N’,N’-dimethylurea, and its CAS number is 330-54-1. The pure product is a white crystalline solid. m.p. 158~159℃, vapor pressure 4.13×10 -4 Pa (50°C). Easily soluble in hot alcohol; at 27°C, the solubility in acetone is 5.3%; slightly soluble in dioxane, ethyl acetate, ethanol and hot benzene; at 25°C, the solubility in water is 42mg / L. It is stable in the air, decomposes when heated to 180-190°C, easily decomposes in case of strong acid and strong alkali, non-corrosive and non-flammable. Industrial product m.p.>150℃. [0003] Diuron is a substitute for urea herbicides, used to prevent common weeds in non-cultivated land, and also used for selective weeding in cotton fields. It has a systemic conduction effect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C275/30C07C273/18
Inventor 季政石卫兵王耀良刘旭冉
Owner LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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