Preparation method of sodium hexafluorophosphate

A technology of sodium hexafluorophosphate and phosphorus pentafluoride, applied in chemical instruments and methods, sodium/potassium compounds, alkali metal compounds, etc., can solve the problems of high price, limited reserves of lithium carbonate, high cost of lithium batteries, etc., to achieve The effect of high product yield, high yield and mild reaction conditions

Inactive Publication Date: 2018-12-07
MORITA NEW ENERGY MATERIALS ZHANGJIAGANG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reserves of lithium carbonate, the main upstream raw material of lithium hexafluorophosphate, are limited and the price remains high. The cost of lithium batteries is high

Method used

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  • Preparation method of sodium hexafluorophosphate

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preparation example Construction

[0020] (1) Preparation of high-purity raw materials: Control the water content in anhydrous hydrogen fluoride to be less than or equal to 10ppm through conductivity detection to protect against nitrogen gas during synthesis to avoid water entry;

[0021] (2), solution preparation: dissolve the dried sodium fluoride into anhydrous hydrogen fluoride, control the temperature at 0-10°C, and the weight ratio of sodium fluoride to anhydrous hydrogen fluoride is 1:10;

[0022] (3), preparation and purification of phosphorus pentafluoride: add hydrogen fluoride liquid into the reaction kettle that has added phosphorus pentachloride, wherein excess phosphorus pentachloride is 20% relative to anhydrous hydrogen fluoride liquid, anhydrous hydrogen fluoride and pentafluoride Phosphorus chloride reacts to produce phosphorus pentafluoride gas;

[0023] (4) Preparation of sodium hexafluorophosphate: Pass the phosphorus pentafluoride gas obtained in step (3) into the reaction kettle that has ...

Embodiment 1

[0029] A method for rapidly preparing sodium hexafluorophosphate, specifically comprising the following steps:

[0030] (1) Detect the moisture content of anhydrous hydrogen fluoride ≤ 10ppm;

[0031] (2) Introduce nitrogen gas for 5 hours to purge the air in the equipment pipeline (10L fluorine-lined phosphorus pentafluoride generating kettle, 20L sodium hexafluorophosphate reaction kettle, filter);

[0032] (3) Carefully add 10 kg of anhydrous hydrogen fluoride into a 20L sodium hexafluorophosphate reactor, slowly add 1 kg of dried sodium fluoride, stir to dissolve, and keep the temperature at 0-10°C;

[0033] (4) Add excess phosphorus pentachloride to the 10L phosphorus pentafluoride generation kettle, slowly add anhydrous hydrogen fluoride, pass the generated gas into the 20L reaction kettle, and control the temperature at about 10°C

[0034] (5) After the reaction is completed, cool to 0°C, stir and crystallize for 5 hours, filter to obtain a solid, put it into a vacuum ...

Embodiment 2

[0037] A method for preparing sodium hexafluorophosphate with special specifications, specifically comprising the following steps:

[0038] (1) reutilize the remaining mother liquor of example one;

[0039] (2) Introduce nitrogen gas for 5 hours to purge the air in the equipment pipeline (10L fluorine-lined phosphorus pentafluoride generating kettle, 20L sodium hexafluorophosphate reaction kettle, filter);

[0040] (3) Carefully add 10 kg of anhydrous hydrogen fluoride mother liquor into a 20L sodium hexafluorophosphate reactor, slowly add 0.5 kg of dried sodium fluoride, stir to dissolve, and keep the temperature at 0-10°C;

[0041] (4) Add excess phosphorus pentachloride to a 10L phosphorus pentafluoride generating kettle, slowly add anhydrous hydrogen fluoride, pass the generated gas into a 20L reaction kettle, and control the temperature at about 10°C;

[0042] (5) After the reaction is finished, cool to 0°C, stir and crystallize for 5 hours, filter to obtain a solid, put...

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Abstract

The invention discloses a preparation method of sodium hexafluorophosphate. The preparation method comprises the following steps: (1) introducing phosphorus pentafluoride gas into a reaction kettle containing lithium fluoride and hydrogen fluoride liquid for reaction, so as to obtain a sodium hexafluorophosphate solution; (2) carrying out crystallization under a stirring condition; and (3) drying.The preparation method has the advantages that the reaction conditions are mild, the yield is high, the process equipment is simple, and a high-purity sodium hexafluorophosphate target product can beprepared. Sodium hexafluorophosphate can be used as sodium salt for sodium-ion battery electrolyte.

Description

technical field [0001] The present application relates to the technical field of lithium ion batteries, in particular to a method for preparing sodium hexafluorophosphate. Background technique [0002] Lithium hexafluorophosphate has been used commercially as an electrolyte for lithium-ion batteries for more than two decades. The main reason is that lithium hexafluorophosphate has excellent chemical properties as an electrolyte and the synthesis method is mature. However, the reserves of lithium carbonate, which is the main upstream raw material of lithium hexafluorophosphate, are limited, and the price remains high, and the cost of lithium batteries is high. With the advent of the era of electric vehicles and smart grids, the shortage of lithium resources will become an important factor restricting its development. In order to meet the large-scale market demand, it is far from enough to measure battery materials only by energy density, charge-discharge rate and other prop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D13/00
CPCC01D13/00C01P2006/80C01P2006/82
Inventor 堀尾博英
Owner MORITA NEW ENERGY MATERIALS ZHANGJIAGANG CO LTD
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