Method for preparing sodium iron phosphate electrode by using industrial byproduct ferrous sulfate

A technology of ferrous sulfate and sodium ferric phosphate, which is applied in battery electrodes, chemical instruments and methods, circuits, etc., can solve the problem that the thermodynamically stable phase does not have the activity of sodium ion insertion and extraction, and there is no ideal post-treatment recycling route. Sodium iron phosphate cathode material and other problems, to achieve excellent capacity and cycle stability, alleviate disposal problems, and achieve the effect of high electrochemical activity

Inactive Publication Date: 2019-05-21
CENT SOUTH UNIV
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Problems solved by technology

[0003] At present, among the positive electrode materials of sodium ion batteries, sodium iron phosphate has become an excellent candidate for the positive electrode of sodium ion batteries due to its stable performance and low raw material cost. However, although the chemical formulas of sodium iron phosphate and lithium iron phosphate are similar, the preparation of sodium iron phosphate Compared with lithium iron phosphate, it is still immature. Because of the crystal structure of sodium iron phosphate, its thermodynamically stable phase theoretically does not have the activity of intercalation and extraction of sodium ions. Therefore, the traditional crystallization scheme and crystal growth scheme are used in the preparation of iron phosphate The field of sodium is not applicable, but to prepare sodium iron phosphate materials with sodium ion intercalation and detachment activity, the laboratory often adopts experimental schemes with harsh conditions or raw materials such as ion replacement method or electrostatic spray method, which greatly improves Therefore, it is of great significance and value to find a simple and feasible preparation scheme of sodium iron phosphate cathode material
[0004] In the current very mature titanium dioxide industry, the by-product ferrous sulfate has a large output and there is no ideal post-treatment recycling method

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  • Method for preparing sodium iron phosphate electrode by using industrial byproduct ferrous sulfate
  • Method for preparing sodium iron phosphate electrode by using industrial byproduct ferrous sulfate
  • Method for preparing sodium iron phosphate electrode by using industrial byproduct ferrous sulfate

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Embodiment 1

[0037] 3g ferrous sulfate (FeSO 4 ·7H 2 O) dissolved in 50mL phosphoric acid (H 3 PO 4 ), then add 15mL hydrogen peroxide (H 2 o 2 ), then add ammonia water drop by drop while pH monitoring, control the target pH value to 1.5, white precipitate is produced in the solution, collect the precipitate by suction filtration and then use 100mL deionized water and 100mL absolute ethanol to repeatedly suction filter the precipitate three times Finally, the precipitate was dried in an oven at 60°C for 12 hours, and then the dried sample was placed in a tube furnace, and heat-treated at 600°C for 12 hours under a nitrogen atmosphere to remove crystal water and obtain a sample of iron phosphate powder.

[0038] Prepare ferric phosphate powder, PVDF, and conductive carbon black into a mixed powder according to the mass ratio of 8:1:1, add NMP liquid of the same quality as PVDF, and continue stirring for 3 hours to obtain iron phosphate slurry. Use a film coating machine to press 0.3mm ...

Embodiment 2

[0042] 3g ferrous sulfate (FeSO 4 ·7H 2 O) dissolved in 50mL phosphoric acid (H 3 PO 4 ), then add 30mL hydrogen peroxide (H 2 o 2 ), then add saturated sodium hydroxide solution drop by drop while pH monitoring, control the target pH value to 1.5, produce white precipitate in the solution, use 100mL deionized water and 100mL absolute ethanol to repeatedly remove the precipitate after collecting the precipitate by suction filtration After three times of suction filtration, the precipitate was dried in an oven at 60°C for 12 hours, and then the dried sample was placed in a tube furnace, and heat-treated at 700°C for 12 hours under a nitrogen atmosphere to remove crystal water and obtain iron phosphate powder sample.

[0043] Prepare ferric phosphate powder, PVDF, and conductive carbon black into a mixed powder according to the mass ratio of 7:2:1, add NMP liquid of the same quality as PVDF, and continue stirring for 3 hours to obtain iron phosphate slurry. Use a film coati...

Embodiment 3

[0047] 3g ferrous sulfate (FeSO 4 ·7H 2 O) dissolved in 50mL phosphoric acid (H 3 PO 4 ), then add 10mL hydrogen peroxide (H 2 o 2 ), then add concentrated ammonia water drop by drop while pH monitoring, and control the target pH value to 1.5, a white precipitate is produced in the solution, collect the precipitate by suction filtration, and then use 100mL deionized water and 100mL absolute ethanol to repeatedly suction-filter the precipitate After three times, the precipitate was dried in an oven at 60°C for 12 hours, and then the dried sample was placed in a tube furnace and heat-treated at 700°C for 12 hours under a nitrogen atmosphere to remove crystal water and obtain a sample of iron phosphate powder.

[0048] Mix iron phosphate powder, PTFE, and acetylene black in a mass ratio of 8:1:1 to make a mixed powder, add isopropanol equal in quality to PTFE, and continue stirring for 3 hours to obtain iron phosphate slurry. Use a coating machine to press 0.3mm The thicknes...

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Abstract

The invention discloses a method for preparing a sodium iron phosphate electrode by using industrial byproduct ferrous sulfate. The method comprises the steps of dissolving the ferrous sulfate in a phosphoric acid solution, then adding hydrogen peroxide, adjusting the pH of the phosphoric acid solution to 1.5-2 for carrying out a reaction, and separating out iron phosphate precipitates; and carrying out thermal dehydration treatment on the iron phosphate precipitates to obtain iron phosphate powder; coating a current collector with the iron phosphate powder, a conductive agent and a binder through a coating method to prepare an iron phosphate electrode plate; and by taking the iron phosphate electrode plate as a positive electrode, metallic sodium as a counter electrode and a sodium perchlorate solution as an electrolyte solution, performing electrochemical sodium embedding to obtain the sodium iron phosphate electrode. According to the method, the cyclic utilization problem of the ferrous sulfate byproduct is effectively relieved, and the sodium iron phosphate positive electrode with high electrochemical activity can be obtained, so that a sodium ion battery with high capacity andhigh cycling stability is obtained.

Description

technical field [0001] The invention relates to a method for preparing a sodium iron phosphate electrode, in particular to a method for preparing a high-activity sodium iron phosphate positive electrode by using ferrous sulfate by-products in the titanium dioxide industry, and belongs to the field of electrode material preparation for sodium ion batteries. Background technique [0002] With the increasingly serious energy crisis and environmental pollution, new rechargeable battery components play an important role in the development and application of new energy, among which lithium-ion batteries have been intensively researched and developed in the past three decades, and have formed A battery component that has established a well-established industry. However, as the requirements for the number and performance of energy storage elements are further improved, and limited by the limited reserves of lithium elements, finding other types of high-performance advanced energy st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M10/054C01B25/45
CPCY02E60/10
Inventor 纪效波田野侯红帅邹国强
Owner CENT SOUTH UNIV
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