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
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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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