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A technology of rimsulfuron-methyl technical material and purification method, which is applied in the field of pesticide production, can solve the problems of low purity of rimsulfuron-methyl technical material, achieve the effects of reducing the content of impurities, reducing the proportion of main impurities, and reducing the purification cost
Inactive Publication Date: 2018-05-11
绍兴上虞银邦化工有限公司
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Problems solved by technology
[0005] In order to solve the problem that the purity of the rimsulfuron-methyl original drug is not high, the present invention provides a purification method of the rimsulfuron-methyl original drug with low cost and good effect
Method used
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Embodiment 1
[0025] (1) Add 50g of rimsulfuron-methyl crude product into 150mL of toluene with a concentration of 99wt%, heat to 30°C under stirring condition, and maintain for 10h;
[0026] (2) Slowly cool down to -20°C, wait until the product is completely precipitated, filter, and take the filter cake;
[0027] (3) Add the above filter cake into 100mL of chloroform, stir and beat, the beating temperature is -20°C, and the beating time is 8h to obtain a slurry;
[0028] (4) Filtering and drying the above slurry to obtain purified rimsulfuron technical product.
Embodiment 2
[0030] (1) Add 50g of rimsulfuron-methyl crude product into 200mL of xylene, heat to 160°C under stirring condition, and keep for 0.5h;
[0031] (2) Add 50mL of ethylene glycol dimethyl ether, slowly cool down to 30°C, wait until the product is completely precipitated, filter, and take the filter cake;
[0032] (3) Add the above filter cake into 200mL ethanol, stir and beat, the beating temperature is 30°C, and the beating time is 4h, to obtain a slurry;
[0033] (4) Filtering and drying the above slurry to obtain purified rimsulfuron technical product.
Embodiment 3
[0035] (1) Add 50g of rimsulfuron-methyl crude product into 100mL of tetrahydrofuran with a concentration of 99wt%, and heat to 100°C under stirring conditions for 4h;
[0036] (2) Add 25mL of petroleum ether and stir evenly, slowly cool down to 20°C, wait until the product is completely precipitated, filter, and take the filter cake;
[0037] (3) Add the above filter cake into 150mL 1,1-dichloroethane, stir and beat, the beating temperature is 25°C, and the beating time is 5h to obtain a slurry;
[0038] (4) Filtering and drying the above slurry to obtain purified rimsulfuron technical product.
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Abstract
The invention relates to the technical field of pesticide production, in particular to a purifying method of rimsulfuron original medicine. The purifying method comprises the following steps: (1) adding a rimsulfuron original medicine crude product into a solvent, and heating under a stirring condition; (2) adding or not adding a solvent, slowly cooling, filtering after completely separating out aproduct, and taking filter cake; (3) adding the filter cake in the solvent, and stirring and pulping; (4) filtering and drying, thus obtaining a purified rimsulfuron original medicine product. According to the purifying method disclosed by the invention, through selection of a new purifying method, proportions of main purities can be reduced, the purity of original medicine can be increased, thepurity of the rimsulfuron original medicine purified by utilizing the technology of the invention is not lower than 98.5 percent, the content of purities is reduced to a large extent, and the problemof low purity generally existing in the industry is solved; meanwhile, the technical scheme of the invention is very easy to operate, the purification cost is relatively low, and the purifying methodis beneficial for being adopted in industrial production.
Description
technical field [0001] The invention relates to the technical field of pesticide production, in particular to a method for purifying the rimsulfuron original drug with low cost and good effect. Background technique [0002] Rimsulfuron, also known as rimsulfuron, trade name Titus, is a new variety of sulfonylurea herbicides discovered and successfully developed by DuPont in the mid-1980s. It was launched in 1992 It was registered in Europe for corn, in 1995 in the United States for potatoes and corn, and in 1997 in my country as a post-emergence herbicide for corn. It is one of the more prominent varieties among the many new varieties of sulfonylurea herbicides developed in recent years. [0003] Trisulfuron-methyl is a heterocyclic selective pre-emergence and post-emergence herbicide, which causes the action through the contact and absorption of the weed sprouts or seedlings with the agent, and the application of the drug after the emergence, the weeds absorb through the ab...
Claims
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Application Information
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