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Method used for preparation of sodium hexafluoroferrate through electrolysis

A technology of sodium hexafluoroferrate and sodium fluoride, applied in the electrolysis process, electrolysis components, electrodes and other directions, can solve the problems of slow development of sodium ion batteries, extremely poor electrochemical performance, etc., and achieve good social and economic benefits and small particle size. , the effect of mild reaction conditions

Active Publication Date: 2019-01-22
HUNAN INSTITUTE OF ENGINEERING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the extremely poor electrochemical performance of the electrode materials developed in the early stage, the development of sodium-ion batteries has been very slow

Method used

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  • Method used for preparation of sodium hexafluoroferrate through electrolysis
  • Method used for preparation of sodium hexafluoroferrate through electrolysis

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Embodiment 1

[0023] In a 1.2L electrolytic cell without a diaphragm, add 30mL of hydrofluoric acid solution with a mass fraction of 10% and 800mL of a 0.2mol / L sodium fluoride solution, and use pure iron and stainless steel with a size of 15cm×8cm×1cm as Anode and cathode with a current density of 0.05 A / cm 2 , electrolysis temperature is 30 ℃, direct current electrolysis 3h. After the electrolysis, the reaction solution was taken out, 40 mL of 30% hydrogen peroxide was added to it, the oxidation reaction was 1.5 h, the electrolyte was filtered, and the precipitate was washed 4 times with deionized water. Then, the precipitate was dried in a vacuum oven at 90° C. for 10 h, crushed, and passed through a 300-mesh sieve to obtain sodium hexafluoroferrate.

Embodiment 2

[0025] In a 1.2L electrolytic cell without a diaphragm, add 140mL of hydrofluoric acid solution with a mass fraction of 30% and 800mL of a 0.5mol / L sodium sulfate solution, and use pure iron and graphite with a size of 15cm×8cm×1cm as the anode respectively. and cathode with a current density of 0.1 A / cm 2 , electrolysis temperature is 50 ℃, direct current electrolysis 5h. After the electrolysis, the reaction solution was taken out, and pure oxygen was passed into it, and the oxidation reaction was carried out for 5 hours, the electrolyte solution was filtered, and the precipitate was washed 5 times with deionized water. Then, the precipitate was dried in a vacuum oven at 80° C. for 12 hours, crushed, and passed through a 400-mesh sieve to obtain sodium hexafluoroferrate.

Embodiment 3

[0027] In a 1.2L electrolytic cell without a diaphragm, add 900mL of 0.5mol / L sodium fluoride solution and 20mL of nitric acid solution with a mass fraction of 69%, and use ferrosilicon alloy and nickel with a size of 20cm×10cm×1cm as the anode and nickel respectively. Cathode with a current density of 0.3 A / cm 2 , electrolysis temperature is 70 ℃, direct current electrolysis 8h. After the electrolysis, take out the reaction solution, add 50mL of 2mol / L sodium persulfate to it, perform an oxidation reaction for 3h, filter the electrolyte solution, and wash the precipitate 6 times with deionized water. Then, the precipitate was dried in a vacuum oven at 70° C. for 15 hours, crushed, and passed through a 500-mesh sieve to obtain sodium hexafluoroferrate.

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Abstract

The invention discloses a method used for preparation of sodium hexafluoroferrate through electrolysis. According to the method, a mixed solution of hydrofluoric acid and a soluble sodium salt, or a mixed solution of sodium fluoride and an inorganic acid is taken as an electrolyte, pure iron or iron ally is taken as an anode, graphite, nickel, stainless steel, iron, or iron ally is taken as a cathode, 0.01 to 1A / cm2 electric current density is adopted, electrolysis temperature is controlled to be 25 to 95 DEG C, direct current or alternating current electrolysis is adopted, an oxidizing agentis added for oxidation of an obtained product, and precipitate filtering, washing, and drying are carried out so as to obtain sodium hexafluoroferrate. The reaction conditions are mild; operation is convenient; cost is low; the particle size of the obtained product is small; the sodium hexafluoroferrate can be directly taken as a lithium / sodium ion battery electrode material; industrialized production is convenient to realize; and excellent social benefit and economical benefit are achieved.

Description

technical field [0001] The invention relates to the preparation of an electrode material, in particular to a method for electrolytically preparing sodium hexafluoroferrate. Background technique [0002] Sodium-ion batteries have the same working principle as lithium-ion batteries, and their research began around the 1980s. However, the development of sodium-ion batteries is very slow due to the extremely poor electrochemical performance of the electrode materials developed in the early stage. With the rapid development of electric vehicles and smart grids, the development of lithium-ion batteries has brought great challenges. Therefore, sodium-ion batteries with abundant raw material reserves and low price have attracted people's attention again, and finding suitable sodium-ion electrode materials has become the primary research task of current sodium-ion batteries. [0003] Cryolite-type fluoride sodium hexafluoroferrate (Na 3 FeF 6 ) is beige, has the ability to store ...

Claims

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Application Information

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IPC IPC(8): C25B1/24C25B11/04H01M4/58H01M10/0525H01M10/054
CPCC25B1/245C25B11/04H01M4/582H01M10/0525H01M10/054Y02E60/10
Inventor 刘万民秦牡兰邓继勇
Owner HUNAN INSTITUTE OF ENGINEERING
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