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Preparation method of sodium salt for sodium battery

A sodium battery and sodium salt technology, applied in the field of sodium batteries, can solve the problems of difficulty in meeting actual needs, low yield of sodium hexafluorophosphate, etc., and achieve the effects of increasing yield, mild conditions, and improving utilization rate

Active Publication Date: 2022-07-15
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current yield of sodium hexafluorophosphate is low, and it is difficult to meet the actual demand

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0016] A preparation method of sodium salt for sodium battery, comprising the following steps:

[0017] Mixing polyvinyl alcohol, sodium fluoride and water uniformly to prepare a mixed slurry, then drying the slurry and calcining to obtain porous sodium fluoride;

[0018] Pour phosphorus pentafluoride gas into the mixture of porous sodium fluoride and hydrogen fluoride liquid, and react to obtain sodium hexafluorophosphate solution;

[0019] The sodium hexafluorophosphate solution is crystallized, filtered and dried to obtain sodium hexafluorophosphate.

[0020] After the mixed slurry of polyvinyl alcohol and sodium fluoride is dried, it is calcined at high temperature, and the polyvinyl alcohol generates gas, thereby preparing porous sodium fluoride.

[0021] In some embodiments, the mass ratio of polyvinyl alcohol and sodium fluoride is 1:1-15.

[0022] In some embodiments, the calcination temperature is 600-900° C., and the calcination time is 0.5-5 h.

[0023] In some e...

Embodiment 1

[0029] A preparation method of high-yield sodium hexafluorophosphate, comprising the steps:

[0030] Synthesis of porous sodium fluoride: Take 1 g of sodium fluoride and 1 g of polyvinyl alcohol, add deionized water, mix well, and then put it in an oven to dry. The dried product was calcined at 600 °C for 2 h, and the porous sodium fluoride was obtained after cooling down.

[0031] Add 1 g of sodium fluoride and 10 g of hydrogen fluoride to the reaction kettle, stir evenly, and control the temperature at 0 °C.

[0032] Add excess phosphorus pentachloride to another reaction kettle, then slowly add hydrogen fluoride, pass the generated gas into the above reaction kettle, and control the temperature at 15°C.

[0033] After the reaction was completed, it was cooled to 0 °C, stirred and crystallized for 5 hours to obtain a solid through a filter, which was put into an air-evaporating drying oven and dried to obtain the desired sodium hexafluorophosphate product. The yield of sodi...

Embodiment 2

[0035] A preparation method of high-yield sodium hexafluorophosphate, comprising the steps:

[0036] Synthesis of porous sodium fluoride: Take 5g of sodium fluoride and 1g of polyvinyl alcohol, add deionized water, mix well, and then put it in an oven to dry. The dried product was calcined at 800 °C for 1 h, and the porous sodium fluoride was obtained after cooling down.

[0037] Add 1 g of sodium fluoride and 12 g of hydrogen fluoride to the reaction kettle, stir evenly, and control the temperature at 2°C.

[0038] Add excess phosphorus pentachloride to another reaction kettle, then slowly add hydrogen fluoride, pass the generated gas into the above reaction kettle, and control the temperature at 12°C.

[0039] After the reaction was completed, it was cooled to 0°C, stirred and crystallized for 5 hours to obtain a solid through a filter, which was put into an air-evaporating drying oven and dried to obtain the desired sodium hexafluorophosphate product. The yield of sodium h...

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PUM

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Abstract

The invention discloses a preparation method of a sodium salt for a sodium battery, which comprises the following steps: uniformly mixing polyvinyl alcohol and sodium fluoride, adding deionized water, drying, and calcining to obtain porous sodium fluoride; the method comprises the following steps: introducing phosphorus pentafluoride gas into a mixture of porous sodium fluoride and hydrogen fluoride liquid, and reacting to prepare a sodium hexafluorophosphate solution; and crystallizing, filtering and drying the sodium hexafluorophosphate solution to obtain the sodium hexafluorophosphate. Porous sodium fluoride is adopted as a sodium source to prepare sodium hexafluorophosphate, the utilization rate of a precursor can be increased, and the yield is effectively increased; in addition, the yield of the product can be further improved through stirring and crystallization.

Description

technical field [0001] The invention belongs to the technical field of sodium batteries, and relates to a preparation method of a sodium salt for a sodium battery. Background technique [0002] The statements herein merely provide background related to the present invention and do not necessarily constitute prior art. [0003] Sodium has the advantages of abundant resources and low cost, and sodium-ion batteries have received extensive attention. Sodium batteries have the following advantages: First, the reserves of sodium are abundant on the earth, with a content of about 3% in the earth's crust, while lithium is only 0.065% in comparison; second, the distribution of sodium is better than that of lithium. Third, the safety of sodium batteries is higher, and the standard voltage range is wider. [0004] As an important sodium salt in the electrolyte of sodium batteries, sodium hexafluorophosphate has the advantages of high electrical conductivity and stable solid-state ele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D13/00H01M4/58
CPCC01D13/00H01M4/5825C01P2006/80Y02E60/10
Inventor 冯金奎安永灵
Owner SHANDONG UNIV
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