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Preparation method of lithium monofluorophosphate

A monofluorolithium phosphate, monofluorophosphoric acid technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc. Good and other problems, to achieve the effect of less by-products, simple process method and easy reaction

Pending Publication Date: 2020-11-20
湖北九宁化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] With the rapid development of lithium-ion batteries, lithium-ion batteries have been rapidly applied to many fields such as electrical appliances, automobiles, and aerospace. High-temperature storage and other properties have a bad impact, and cannot meet the increasingly high requirements for high-low temperature performance, battery capacity, and cycle performance of lithium-ion batteries in the current market. Therefore, it is imminent to develop various electrolyte additives with excellent performance.

Method used

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  • Preparation method of lithium monofluorophosphate

Examples

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Effect test

preparation example Construction

[0022] Technical solution of the present invention: a preparation method of lithium monofluorophosphate, comprising the following steps:

[0023] S1. Preparation of monofluorophosphoric acid: react phosphorus pentoxide and hydrofluoric acid in a closed reaction vessel made of fluorine-resistant material to obtain monofluorophosphoric acid;

[0024] Among them, the preparation of hydrofluoric acid: first prepare hydrofluoric acid with a mass fraction of 65% to 75% for later use, according to the concentration ratio, first take pure water in a polytetrafluoroplastic bucket, then slowly add the corresponding amount of hydrofluoric acid, stir and mix well Can;

[0025] Wherein, with phosphorus pentoxide and hydrofluoric acid as raw materials, the reaction molar ratio is n(P 2 o 5 ):n(HF)=1:2~1:2.05, first put a certain amount of phosphorus pentoxide into the airtight monel alloy reaction vessel, and then pump 69% of the corresponding amount of hydrofluoric acid into the reaction...

Embodiment 1

[0038] First take 710g of phosphorus pentoxide in a closed monel alloy reaction vessel, take 310g of prepared hydrofluoric acid, and pump it into the reaction vessel through a peristaltic pump at a constant speed. React for 2 hours, the reaction is over, raise the temperature to 110°C~120°C, adjust the vacuum to 0-0.05MPa, and the distillation time is 30min, connect the tail gas absorber of the reaction vessel to the end of the reaction vessel, and weigh the obtained monofluorophosphoric acid after the reaction is over 968g;

[0039]In example 1, different concentrations of hydrofluoric acid were used for experiments, and compared by calculating the yield and purity of monofluorophosphoric acid, the experimental data are as follows:

[0040]

[0041] .

Embodiment 2

[0043] Choose LiOH as the lithium source, put 432g of lithium hydroxide into the reaction vessel, take 900g of monofluorophosphoric acid in step S1 and pass it into the reaction vessel, heat while stirring, keep the reaction temperature at 50°C-100°C, and the reaction time is 2h, until the reaction is completely completed , raise the temperature to 100°C-150°C until the water is evaporated to dryness, and dry the crystallized product in a vacuum drying oven at a set temperature of 180°C-220°C for 3 hours to obtain 930 g of lithium monofluorophosphate with a yield of 92.3%.

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Abstract

The invention discloses a preparation method of lithium monofluorophosphate. The preparation method comprises the following steps: S1, preparation of monofluorophosphoric acid: reacting phosphorus pentoxide with hydrofluoric acid in a closed reactor made of a fluorine-resistant material to obtain monofluorophosphoric acid; S2, separating and purifying the product obtained in the step S1 through vacuum distillation; and S3, searching a lithium source, reacting the lithium source with the product obtained in the step S2, after the reaction, evaporating, concentrating and crystallizing the solution to obtain crystals, namely lithium monofluorophosphate, and drying the crystals in vacuum to obtain a lithium monofluorophosphate product; wherein the mass fraction of hydrofluoric acid is 65%-75%;the fluorine-resistant material of the closed reactor can be selected from one of titanium-nickel alloy, hastelloy, monel alloy and Inconel alloy; wherein the closed reactor made of the fluorine-resistant material in the step S1 is provided with a solid and liquid feeding device; the preparation method is simple in process and few in by-products, the reactions are easy to trigger, and the productpurity is high.

Description

technical field [0001] The invention relates to the technical field of preparation of lithium monofluorophosphate, in particular to a preparation method of lithium monofluorophosphate. Background technique [0002] With the rapid development of lithium-ion batteries, lithium-ion batteries have been rapidly applied to many fields such as electrical appliances, automobiles, and aerospace. Performance such as high temperature storage has a negative impact, and cannot meet the increasingly high requirements for high and low temperature performance, battery capacity, and cycle performance of lithium-ion batteries in the current market. Therefore, it is imminent to develop various electrolyte additives with excellent performance. Lithium monofluorophosphate, as an additive for lithium-ion batteries, can significantly improve the low-temperature characteristics and cycle stability of lithium-ion secondary batteries. Therefore, in the context of the continuous expansion of the mark...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455H01M10/0567
CPCC01B25/455H01M10/0567C01P2006/80Y02E60/10
Inventor 刘松高月姜灿刘东洋
Owner 湖北九宁化学科技有限公司
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