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

Inactive Publication Date: 2020-07-24
福建省龙德新能源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the mixed acid generated from the recovery of lithium hexafluorophosphate tail gas, the subsequent industrial reuse is greatly limited due to the phosphorus content
Phosphorus pentafluoride enters the exhaust system and reacts with water to produce phosphoric acid, fluorophosphoric acid, etc., which belong to protonic acids like hydrogen chloride and hydrogen fluoride, have similar properties, and are difficult to separate, which has become a difficult problem restricting subsequent development and utilization
However, there is no effective method for the separation and recycling of phosphorus pentafluoride in the tail gas of lithium hexafluorophosphate synthesis in the prior art

Method used

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  • Method for recycling phosphorus pentafluoride in lithium hexafluorophosphate synthesis tail gas by utilizing amine and derivatives thereof
  • Method for recycling phosphorus pentafluoride in lithium hexafluorophosphate synthesis tail gas by utilizing amine and derivatives thereof

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Effect test

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).

...

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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Abstract

The invention provides a method for recycling phosphorus pentafluoride in lithium hexafluorophosphate synthesis tail gas by utilizing amine and derivatives thereof. The method comprises the followingsteps: reacting amine and derivatives thereof with phosphorus pentafluoride in lithium hexafluorophosphate synthesis tail gas to form a solid or liquid complex, separating the solid or liquid complex,heating the solid or liquid complex to release phosphorus pentafluoride, purifying the released phosphorus pentafluoride, and introducing the purified phosphorus pentafluoride into a lithium hexafluorophosphate synthesis system for the second time. The method is high in raw material utilization rate and reduces pollution.

Description

technical field [0001] The invention relates to a method for reusing lithium hexafluorophosphate to synthesize phosphorus pentafluoride in tail gas by using amine and its derivatives, and belongs to the technical field of lithium hexafluorophosphate synthesis. Background technique [0002] Since the second half of the 20th century, with the advancement of science and technology, human society has entered a stage of rapid development, and the demand for energy is also increasing. As a primary energy source, fossil fuels have played an infinite role in human development so far. However, human beings are also facing the problems of energy depletion and environmental pollution. Finding alternative new clean energy has become a common challenge for human beings. In the 21st century, the development and utilization of new energy sources have made remarkable progress, especially lithium-ion batteries have been successfully used in traditional 3C (computers, cameras, mobile phones, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/10C01D15/00
CPCC01B25/10C01D15/005
Inventor 杨瑞甫赖育河周利彬陈东林肖文绪肖丰贤
Owner 福建省龙德新能源有限公司
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