Method for preparing nitroguanidine by adopting micro-channel reactor
A micro-channel reactor, nitroguanidine technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of large reactor volume, occupying large workshops, and high temperature control requirements, avoiding the need for Severely corroded equipment, reduced waste acid production, and excellent corrosion resistance
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Embodiment 1
[0042] (1) Device used: Corning high-throughput microchannel reactor (Corning straight channel module + Corning heart-shaped channel module), refer to image 3 Determine the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.
[0043] (2) Raw material tanks 1 and 2 are equipped with guanidine sulfate with a mass concentration of sulfuric acid solution of 10% and a mass concentration of nitric acid of 30%. Set the flow control of each metering pump 3, pump 4 to change the sulfuric acid solution of guanidine sulfate: nitric acid mol ratio=1:0.9, control the sulfuric acid solution flow rate of guanidine sulfate: 0.25mL / min, control the nitric acid flow rate: 0.2mL / min, and The materials are respectively injected into the preheating modules of each straight channel, and the reaction temperature is controlled to be 40°C; the sulfuric...
Embodiment 2
[0046] (1) Device used: Corning high-throughput microchannel reactor (Corning straight channel module + Corning heart-shaped channel module), refer to image 3 Determine the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.
[0047] (2) Raw material tanks 1 and 2 are configured with a mass concentration of sulfuric acid solution of guanidine sulfate to be 15%; and a mass concentration of nitric acid to be 35%. Set the flow control of each metering pump 3 and pump 4 to change the sulfuric acid solution of guanidine sulfate: nitric acid molar ratio=1:1, control the sulfuric acid solution flow rate of guanidine sulfate: 0.2mL / min, control the nitric acid flow rate: 0.2mL / min, and The materials are respectively injected into the preheating modules of each straight channel, and the reaction temperature is controlled to be 50°C; the...
Embodiment 3
[0050] (1) Device used: Corning high-throughput microchannel reactor (Corning straight channel module + Corning heart-shaped channel module), refer to image 3 Determine the connection mode of the microchannel reactor, the number of mixed reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.
[0051] (2) Raw material tanks 1 and 2 are configured with a mass concentration of sulfuric acid solution of guanidine sulfate to be 20%; and a mass concentration of nitric acid to be 35%. Set the flow control of each metering pump 3 and pump 4 to change the sulfuric acid solution of guanidine sulfate: nitric acid molar ratio=1:2, control the sulfuric acid solution flow rate of guanidine sulfate: 0.2mL / min, control the nitric acid flow rate: 0.8mL / min, and The materials are poured into the preheating modules of each straight channel respectively, and the reaction temperature is controlled to be 80°C; the s...
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