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Novel process for synthesis of dinotefuran

A new process, the technology of dinotefuran, is applied in the new process field of synthesizing dinotefuran, which can solve the problems of increasing sewage treatment load and cost, inability to directly apply it, and increasing solid waste, so as to reduce the cost of production raw materials, reduce output, The effect of reducing labor intensity

Inactive Publication Date: 2020-06-02
江西汇和化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) The input amount of industrial salt (sodium chloride) is 60% of the weight of 3-aminomethyltetrahydrofuran each time. After subsequent treatment, the industrial salt cannot be used mechanically due to impurities, resulting in an increase in solid waste;
[0005] (2) Because of containing a large amount of industrial salts (sodium chloride) in the centrifugal mother liquor, can't directly apply mechanically;
[0006] (3) The leaching mother liquor is directly discharged, which increases the load and cost of sewage treatment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The technique of synthesizing dinotefuran in the prior art:

[0025] Throw 1000L of new process water, 218kg of industrial salt, 10kg of caustic soda, 400kg of 3-aminomethyltetrahydrofuran and 530kg of 1,3-dimethyl-2-nitroisourea into the reactor at room temperature, and raise the temperature to 58°C until The remaining amount of 1,3-dimethyl-2-nitroisourea is equal to 0.3% of its input amount, then cool down to 20°C, adjust the pH to 3-4, then heat up to 50°C to dissolve, and cool down to Centrifuge at 0°C, rinse with 1000L of new process water during centrifugation, and dry the solid after rinsing and centrifugation to obtain 645kg, a quantitative content of 90.32%, and a white solid powder with a yield of 80.7% (based on 3-aminomethyl tetrahydrofuran).

Embodiment 2

[0027] The present invention only adopts the novel process of synthesizing dinotefuran from centrifugal mother liquor:

[0028] Throw 1000L of centrifuged mother liquor and 10kg of caustic soda into the reactor at room temperature, then cool down to -5°C, put in 400kg of 3-aminomethyltetrahydrofuran and 530kg of 1,3-dimethyl-2-nitroisourea, and stir evenly. Raise the temperature to 55°C, and keep it warm while stirring until the remaining amount of 1,3-dimethyl-2-nitroisourea is equal to 0.3% of its input amount, then cool down to 20°C, adjust the pH to 4 to acidify the crystallization, Then heat up to 50°C to dissolve, after the dissolution, cool down to 0°C and centrifuge, and dry the solid after centrifugation to obtain 654kg, with a quantitative content of 98.24%, a white solid powder, and a yield of 99.6% (calculated as 3-aminomethyltetrahydrofuran) , the liquid after centrifugation is the ultimate mother liquor, which is pumped to the concentration tank for concentration...

Embodiment 3

[0031] The present invention simultaneously adopts the new technique of synthesizing dinotefuran of centrifugal mother liquor and leaching mother liquor:

[0032] Throw 1000L of centrifuged mother liquor and 10kg of caustic soda into the reactor at room temperature, then cool down to -5°C, put in 400kg of 3-aminomethyltetrahydrofuran and 530kg of 1,3-dimethyl-2-nitroisourea, and stir evenly. Raise the temperature to 55°C, and keep it warm while stirring until the remaining amount of 1,3-dimethyl-2-nitroisourea is equal to 0.3% of its input amount, then cool down to 20°C, adjust the pH to 4 to acidify the crystallization, Then heat up to 50°C to dissolve, after the dissolution is completed, cool down to 0°C and centrifuge, use new process water to rinse the centrifugal filter cake, collect the rinsing mother liquor, and the number of times the rinsing mother liquor is used for rinsing the centrifugal filter cake is 25 times , the solid drying after centrifugation obtains 667kg,...

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PUM

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Abstract

The invention belongs to the technical field of chemical synthesis, and particularly relates to a novel process for synthesis of dinotefuran. The process comprises the following synthesis procedures of: adding centrifugal mother liquor and caustic soda flakes into a reaction kettle at room temperature, then performing cooling to a temperature ranging from -8DEG C to -3DEG C, adding 3-aminomethyl tetrahydrofuran and 1, 3-dimethyl-2-nitroisourea, stirring the substances uniformly, performing heating to 50-60DEG C, carrying out heat preservation reaction while stirring until the residual amount of 1, 3-dimethyl-2-nitroisourea is less than 0.5% of the input amount thereof, performing cooling to 18-22DEG C, adjusting the pH value to 3-5, conducting acidifying and crystallizing, then performingheating to 45-55DEG C for dissolving, conducting cooling to a temperature ranging from -5DEG C to 0DEG C after complete dissolution, performing centrifuging, and drying the centrifuged solid to obtainthe target dinotefuran, with the centrifuged liquid being ultimate mother liquor. According to the process provided by the invention, industrial salt is not used any more, and meanwhile, the centrifugal mother liquor and leaching mother liquor are applied to the reaction of the synthesis process, so that the solid waste yield is reduced, the wastewater yield is greatly reduced, and the product yield is increased.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a new process for synthesizing dinotefuran. Background technique [0002] Dinotefuran is the third generation neonicotinoid insecticide developed by Mitsui Corporation of Japan. It has excellent control effect on piercing-sucking mouthparts pests, and shows high insecticidal activity at a very low dose. It is mainly used to control aphids, leafhoppers, planthoppers, thrips, whiteflies and their resistant strains on wheat, rice, cotton, vegetables, fruit trees, tobacco leaves and other crops. It is highly effective against pests of the order Pteroptera, Diptera, Beetles and Totaloptera, and has high efficiency against sanitary pests such as cockroaches, termites, houseflies, etc., and has broad development and application prospects. [0003] According to the different key intermediates in the synthesis of dinotefuran, the synthesis methods of dinotefuran c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/14
CPCC07D307/14
Inventor 尹旺华韩井卫曾小明
Owner 江西汇和化工有限公司
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