Preparation method of fluorine-doped Prussian blue sodium ion battery positive electrode material

A sodium-ion battery, Prussian blue technology, applied in the field of preparation of Prussian blue-type sodium-ion battery cathode materials, can solve problems such as poor cycle performance, poor crystallinity, crystal surface residue, etc., to improve purity, increase gram capacity, inhibit Effect of Precipitation Reaction Rate

Active Publication Date: 2022-03-22
GUANGDONG BRUNP RECYCLING TECH +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For this reason, the present invention proposes a preparation method of a fluorine-doped Prussian blue sodium ion battery positive electrode material, which can solve the problems of poor crystallinity, poor cycle performance, and residual crystal surface of the Prussian blue sodium ion battery positive electrode material

Method used

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  • Preparation method of fluorine-doped Prussian blue sodium ion battery positive electrode material

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Embodiment 1

[0028] In this example, a fluorine-doped Prussian blue-type sodium-ion battery positive electrode material is prepared, and the specific process is as follows:

[0029] (1) Prepare 100 mL of a mixed solution of sodium ferrocyanide and sodium fluoride, and add ascorbic acid as an antioxidant. The concentration of sodium ferrocyanide in the mixed solution is 0.1mol / L, and the concentration of sodium fluoride is 0.6mol / L L, the concentration of antioxidant is 0.01mol / L;

[0030] (2) preparation concentration is respectively 100mL of manganese sulfate solution of 0.1mol / L and concentration of 2mol / L of sodium chloride solution 100mL;

[0031] (3) Add manganese sulfate solution to the mixed solution of sodium ferrocyanide and sodium fluoride at a fixed flow rate of 25mL / h;

[0032] (4) After the feeding is finished, add sodium chloride solution to the mixed solution, and age for 12 hours;

[0033] (5) solid-liquid separation obtains precipitate;

[0034] (6) After washing the pr...

Embodiment 2

[0036] In this example, a fluorine-doped Prussian blue-type sodium-ion battery positive electrode material is prepared, and the specific process is as follows:

[0037] (1) Prepare 100 mL of a mixed solution of sodium ferrocyanide and sodium fluoride, and add ascorbic acid as an antioxidant. The concentration of sodium ferrocyanide in the mixed solution is 0.1mol / L, and the concentration of sodium fluoride is 0.6mol / L L, the concentration of antioxidant is 0.01mol / L;

[0038] (2) Preparation concentration is 100mL of ferrous chloride mixed solution of 0.25mol / L and ferric chloride of 0.05mol / L, preparation concentration is 100mL of sodium chloride solution of 2mol / L;

[0039] (3) Add the iron salt mixed solution to the mixed solution of sodium ferrocyanide and sodium fluoride at a fixed flow rate of 25mL / h;

[0040] (4) After the feeding is finished, add sodium chloride solution to the mixed solution, and age for 48 hours;

[0041] (5) solid-liquid separation obtains precipi...

Embodiment 3

[0045] In this example, a fluorine-doped Prussian blue-type sodium-ion battery positive electrode material is prepared, and the specific process is as follows:

[0046] (1) Prepare 100mL of a mixed solution of sodium ferrocyanide and sodium fluoride, and add butyl hydroxyanisole as an antioxidant. The concentration of sodium ferrocyanide in the mixed solution is 0.01mol / L and the concentration of sodium fluoride is 0.06mol / L, and the concentration of antioxidant is 0.001mol / L;

[0047] (2) preparing respectively concentration is 100mL of cobalt sulfate solution of 0.01mol / L and concentration is 100mL of sodium chloride solution of 4mol / L;

[0048] (3) The cobalt sulfate solution is added to the mixed solution of sodium ferrocyanide and sodium fluoride at a fixed flow rate of 50mL / h;

[0049] (4) After the feeding is finished, add sodium chloride solution to the mixed solution, and age for 24 hours;

[0050] (5) solid-liquid separation obtains precipitate;

[0051] (6) After...

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Abstract

The invention discloses a preparation method of a fluorine-doped Prussian blue sodium-ion battery positive electrode material, which comprises the following steps: preparing a mixed solution of sodium ferrocyanide and sodium fluoride, adding an antioxidant into the mixed solution, adding a transition metal salt solution into the mixed solution at a certain flow rate, and after the charging is finished, carrying out vacuum drying to obtain the fluorine-doped Prussian blue sodium-ion battery positive electrode material. And adding a sodium chloride solution into the mixed solution, aging, carrying out solid-liquid separation on the aged material to obtain a precipitate, and washing and drying the precipitate to obtain the Prussian blue sodium ion battery positive electrode material. The mixed solution contains a large amount of fluorine ions, and the fluorine ions can be complexed with transition metal ions when the transition metal ions are added, so that the precipitation reaction speed is inhibited, crystallization is slowly carried out, particles with better crystallinity are obtained, and fluorine complexed metal sodium salt can generate precipitates along with the reaction, so that the crystallization effect is improved. The fluorine ions and the ferrocyanide are co-precipitated to form co-crystals, and the fluorine ions play a role in supporting a framework of the material.

Description

technical field [0001] The invention belongs to the technical field of sodium-ion batteries, and in particular relates to a preparation method of a fluorine-doped Prussian blue-type sodium-ion battery cathode material. Background technique [0002] Lithium-ion batteries are widely used in portable electronic devices and electric vehicles due to their long life and high specific energy. However, safety concerns and limited lithium resources hinder the application of lithium-ion batteries in large-scale energy storage systems. In this context, low-cost, long-life Na-ion batteries offer an attractive alternative to Li-ion batteries for energy storage systems. Therefore, it is imperative to develop sustainable electrode materials for Na-ion batteries. [0003] Na-ion batteries have the characteristics of low raw material cost, abundant resources, and great electrochemical performance potential, so they are expected to be applied in the field of large-scale energy storage, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01C3/12H01M4/58
CPCC01C3/12H01M4/58C01P2004/03C01P2006/40Y02E60/10H01M10/054H01M4/36
Inventor 余海军谢英豪李爱霞张学梅李长东
Owner GUANGDONG BRUNP RECYCLING TECH
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