Method for recycling phosphorus pentafluoride in lithium hexafluorophosphate synthesis tail gas by utilizing amine and derivatives thereof
A technology of lithium hexafluorophosphate and phosphorus pentafluoride, which is applied in lithium hexafluorophosphate, chemical instruments and methods, phosphorus halides/oxyhalides, etc., can solve the problems of restricting industrial reuse and difficulty in separation, so as to improve the utilization rate of raw materials, reduce losses, cost reduction effect
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Embodiment 1
[0027] The tail gas of lithium hexafluorophosphate synthesis is a mixed gas of hydrogen fluoride, hydrogen chloride and phosphorus pentafluoride. Take a certain volume of mixed gas to measure the content of hydrogen fluoride, hydrogen chloride and phosphorus pentafluoride. The test method is as follows: absorb with three-stage sodium hydroxide lye, the size of the absorption tower is 40mm*300mm (inner diameter*height), and the packing of the absorption tower is uniform It is made of PTFE, Pall ring packing 5mm*φ5mm, the concentration of sodium hydroxide is 2% (w / w), and the alkali absorption solution is combined to determine F by ion chromatography - , Cl - and PO 4 3- The contents were 8.664μg / ml, 11.465μg / ml, 0.931μg / ml ( figure 1 ), according to a molecule of PF 5 After the lye is absorbed, a molecule of PO is produced 4 3- And the quantitative relationship of 5 molecules HF is converted into mass ratio, HF, HCl and PF 5 The mass ratio is 0.552 / 0.384 / 0.064 (w / w).
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Embodiment 2
[0030] The ratio of hydrogen chloride, hydrogen fluoride and phosphorus pentafluoride in the tail gas of lithium hexafluorophosphate synthesis HCl: HF: PF 5=0.552:0.384:0.064 (w / w) (the measurement method is the same as that in Example 1). The mixed gas passes through the scrubber made of PTFE at a flow rate of 10mL / min. The internal size of the scrubber is 40mm*300mm (inner diameter*height), filled with 10*10 Pall ring packing, and the absorbent is benzylamine. The operating temperature is 40°C. The gas that comes out from scrubber passes through three-stage sodium hydroxide alkali absorption tower, and the size of absorption tower is the same as aforementioned scrubber, and the concentration of sodium hydroxide is 2% (w / w), and ion chromatography after alkali washing solution merges Determination of Cl - , F - and PO 4 3- The content is converted into HCl / HF / PF according to the mass ratio 5 = 0.575 / 0.40 / 0.025, PF 5 The absorption efficiency is 60.9%. Control the temp...
Embodiment 3
[0032] In a 500ml stainless steel container, add 250g of absorbent ethylamine, and then pass through PF with a concentration of 99.5% (V / V) 5 Stir while feeding the gas, maintain the pressure in the container at 0.1MPa, and the temperature at 0°C. After the pressure does not change any more, take out the contents of the container after maintaining for another hour. It is a red liquid, weighing 335g, according to the weight before and after The calculated absorption of change is 85g. Heating the vessel, when the temperature rises to 15°C, PF 5 Gas is released. It shows that ethylamine has a good absorption capacity for phosphorus pentafluoride, and can be used for the absorption and reuse of phosphorus pentafluoride in the tail gas of lithium hexafluorophosphate synthesis.
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