Continuous crystallization process for preparing nitroguanidine through nitric acid method
A nitroguanidine, nitric acid method technology, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry and other directions, can solve the problems of reducing product yield, energy waste, complicated process routes, etc., to reduce waste water discharge, The effect of improving product yield and reducing reaction conditions
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Embodiment 1
[0024] The present embodiment carries out as follows:
[0025] (1) Turn on the constant temperature water tank 3 and the refrigeration device 9, and set the temperature to 43°C and -3°C respectively;
[0026] (2) close emptying valve 8, be that the dilute nitric acid 200ml of 40% is joined in the continuous crystallizer 6 with mass concentration, open agitator 5, rotating speed is controlled at 800r / min;
[0027] (3) will dissolve 90g guanidine nitrate, 240ml of nitric acid solution of mass concentration 70%, squeeze in the microtube reactor 2 through metering pump 1, the flow rate of regulating and controlling metering pump is 20ml / min, the stop of liquid in the microtube reactor The time is 150s, drips in the continuous crystallizer 6 afterwards, crystallizes out white nitroguanidine crystal;
[0028] (4) Open the overflow valve 10 and the water inlet valve 4. Control tap water to flow into the continuous crystallizer 6 at a flow rate of 10ml / min, and the mixed suspension ...
Embodiment 2
[0032] The present embodiment carries out as follows:
[0033] (1) Turn on the constant temperature water tank 3 and the refrigeration device 9, and set the temperature to 45°C and -3°C respectively;
[0034] (2) close emptying valve 8, be that 30% dilute nitric acid 200ml joins in the continuous crystallizer 6 with mass concentration, open agitator 5, and the rotating speed is controlled at 800r / min;
[0035] (3) will dissolve 90g guanidine nitrate, 240ml of nitric acid solution of mass concentration 68%, squeeze in the microtube reactor 2 through metering pump 1, the flow velocity of regulating and controlling metering pump is 20ml / min, the stay of liquid in the microtube reactor The time is 150s, drips in the continuous crystallizer 6 afterwards, crystallizes out white nitroguanidine crystal;
[0036] (4) Open the overflow valve 10 and the water inlet valve 4. Control tap water to flow into the continuous crystallizer 6 at a flow rate of 10ml / min, and the mixed suspension...
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