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Process and device for continuous preparation of lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and preparation process, which is applied in phosphorus compounds, inorganic chemistry, electrochemical generators, etc., can solve problems such as non-continuous production, and achieve the effect of achieving continuity and reducing equipment investment and production costs.

Active Publication Date: 2009-09-30
산산어드밴스드머테리얼스(취저우)컴퍼니리미티드
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] The present invention provides a continuous preparation process and device for lithium hexafluorophosphate in order to solve the technical defect of non-continuous production existing in the existing process of synthesizing lithium hexafluorophosphate by adopting kettle-type batch reaction

Method used

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  • Process and device for continuous preparation of lithium hexafluorophosphate
  • Process and device for continuous preparation of lithium hexafluorophosphate
  • Process and device for continuous preparation of lithium hexafluorophosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Such as figure 1 , shown in 2, the present embodiment is carried out in a multi-stage tubular reactor, and the effective reaction volume is 10L. A compressor is used to send gaseous reactants from the reactor inlet into the reactor, and the reactants have the following composition:

[0047] PF5----98.5%

[0048] Inert gas----1.1%

[0049] The above content is the molar content.

[0050] The total flow rate is 26.5 mol / hr, and the converted flow rate of phosphorus pentafluoride is 26.1 mol / hr, that is, 3290 grams per hour. At the same time, anhydrous hydrogen fluoride solution containing lithium fluoride is pumped into as liquid reactant, and the solution has the following composition:

[0051] LiF ---- 3.0%

[0052] HF----97%

[0053] The above content is the mass content.

[0054] The total flow rate of liquid reactants is 20kg / hr, of which 600g / hr of lithium fluoride is equivalent to 23.1mol / hr. Therefore, the molar ratio of phosphorus pentafluoride to lithiu...

Embodiment 2

[0058] Take the mother liquor after crystallization and filtration in Example 1, and add purified lithium fluoride under stirring to form a solution. The content of lithium fluoride in the solution is 3.06%, and the rest is anhydrous hydrogen fluoride and dissolved lithium hexafluorophosphate. This solution was used as the liquid reactant in the tubular reactor.

[0059] A compressor is used to send the gaseous reactants into the reactor from the reactor inlet, and the composition of the gaseous reactants is exactly the same as in Example 1.

[0060] The total flow rate is 26.5 mol / hr, and the converted flow rate of phosphorus pentafluoride is 26.1 mol / hr, that is, 3290 grams per hour.

[0061] The total flow rate of liquid reactants is 20g / hr, of which 612g / hr of lithium fluoride is equivalent to 23.5mol / hr.

[0062] Therefore, the molar ratio of phosphorus pentafluoride to lithium fluoride is about 1.11.

[0063] The above gas and liquid reactants react in the tubular rea...

Embodiment 3

[0066] Multi-stage synthesis reaction: the mixed gas and solution enter the multi-stage tubular reactor through the gas-liquid mixer with the molar ratio of phosphorus pentafluoride and lithium fluoride at a ratio of 1 to 5:1, and the reaction is carried out at a temperature of -40°C ~ 30°C, reaction pressure -0.5 ~ 1.5MPa, after multi-stage full reaction, synthesize lithium hexafluorophosphate.

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Abstract

The invention discloses a process for the continuous preparation of lithium hexafluorophosphate and a device thereof. The process comprises the following steps that: a fluorine hydride solution A of lithium fluoride and phosphorus pentafluoride or a mixed gas of the phosphorus pentafluoride and other gases are subjected to raw material mixing; the raw material mixture undergoes a multistage synthetic reaction; the product of the multistage synthetic reaction enters a gas-liquid separator to remove unreacted gases; the liquid product of the multistage reaction undergoes a consequent hybrid reaction and the product of the consequent hybrid reaction is reacted with the additionally introduced phosphorus pentafluoride gas B to remove a micro amount of possibly unreacted lithium fluoride in the solution; the product of the reaction is then subjected to evaporation, cooling, crystallization, filtration and drying to form lithium hexafluorophosphate crystal with a purity of 99.9 percent; and a parent solution obtained after separation and crystallization is added with the lithium fluoride to form the raw material solution A for cycle use. The invention adopts a multistage tubular reactor which has excellent mass and heat transfer performance and can realize full gas-liquid contact, continuous material feeding and discharging and the like and consequently realize the continuous operation of a production process.

Description

technical field [0001] The invention relates to the technical field of manufacturing lithium batteries, in particular to a continuous preparation process and device for lithium hexafluorophosphate. Background technique [0002] As an electrolyte salt, lithium hexafluorophosphate has good application and environmental performance, and is currently the only commercial lithium-ion battery electrolyte. [0003] Generally speaking, lithium hexafluorophosphate can be synthesized by direct reaction of lithium fluoride and phosphorus pentafluoride: [0004] LiF+PF 5 =LiPF 6 . [0005] At present, the commonly used preparation of lithium hexafluorophosphate is to prepare lithium fluoride solution in a reaction kettle, slowly pass phosphorus pentafluoride gas into the reaction kettle and mix the reaction until the reaction between lithium fluoride and phosphorus pentafluoride is complete, and then the reaction All the products in the kettle are transferred to the next process, suc...

Claims

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Application Information

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IPC IPC(8): C01B25/445H01M10/36
CPCY02E60/12Y02E60/10
Inventor 韩保国崔武孝阎晓冬
Owner 산산어드밴스드머테리얼스(취저우)컴퍼니리미티드
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