Preparation method of sodium hexafluorophosphate
A technology of sodium hexafluorophosphate and hexafluorophosphoric acid, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of high toxicity, achieve the effects of less three wastes, ease dependence, and easy control of the reaction process
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Embodiment 1
[0029] The preparation method of the sodium hexafluorophosphate of the present embodiment comprises the following steps:
[0030] (1) in the reaction kettle, add 71g of phosphorus pentoxide, slowly add anhydrous hydrogen fluoride 120g by automatic feeding device, fully stir, control the reaction temperature to be -3 ℃, and the reaction times is 2 hours;
[0031] (2) slowly add 42g sodium fluoride to the solution of step (1) by automatic feeder, react 3 hours at -10 ℃;
[0032] (3) After the reaction, the solution was heated to 65°C for 4 hours, and the water and unreacted hydrogen fluoride were removed by nitrogen purging, and the exhaust gas discharged at the same time was connected to the condensing device for recycling;
[0033] (4) The mother liquor obtained in step (3) was heated and concentrated at 120°C for 6 hours, the obtained crude product of sodium hexafluorophosphate was dissolved in dimethyl carbonate, and the obtained solid was continuously stirred at 50°C for 2 ...
Embodiment 2
[0035] The preparation method of the sodium hexafluorophosphate of the present embodiment comprises the following steps:
[0036] (1) in the reaction kettle, add 213g of phosphorus pentoxide, slowly add anhydrous hydrogen fluoride 300g by automatic feeding device, fully stir, control the reaction temperature to be -3 ℃, and the reaction times is 2 hours;
[0037] (2) slowly add 126g sodium fluoride to the solution of step (1) by automatic feeder, react 3 hours at -10 ℃;
[0038] (3) After the reaction, the solution was heated to 65°C for 4 hours, and the water and unreacted hydrogen fluoride were removed by nitrogen purging, and the exhaust gas discharged at the same time was connected to the condensing device for recycling;
[0039] (4) The mother liquor obtained in step (3) was heated and concentrated at 120°C for 6 hours, the obtained crude product of sodium hexafluorophosphate was dissolved in dimethyl carbonate, and the obtained solid was continuously stirred at 50°C for ...
Embodiment 3
[0041] The preparation method of the sodium hexafluorophosphate of the present embodiment comprises the following steps:
[0042] (1) in the reaction kettle, add 355g of phosphorus pentoxide, slowly add anhydrous hydrogen fluoride 550g by automatic feeding device, fully stir, control the reaction temperature to be-3 ℃, and the reaction times is 2 hours;
[0043] (2) slowly add 210g of sodium fluoride to the solution of step (1) by automatic feeder, react at -10 ℃ for 3 hours;
[0044] (3) After the reaction, the solution was heated to 65°C for 4 hours, and the water and unreacted hydrogen fluoride were removed by nitrogen purging, and the exhaust gas discharged at the same time was connected to the condensing device for recycling;
[0045] (4) The mother liquor obtained in step (3) was heated and concentrated at 120°C for 6 hours, the obtained crude product of sodium hexafluorophosphate was dissolved in dimethyl carbonate, and the obtained solid was continuously stirred at 50°...
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