Method for preparing Na4Fe3 (PO4) 2 (P2O7) by homogeneous phase method and application

A homogeneous method and sand grinding technology, applied in chemical instruments and methods, inorganic chemistry, positive electrodes, etc., to achieve the effect of improving purity, wide distribution and high sphericity

Inactive Publication Date: 2021-07-02
HUBEI WANRUN NEW ENERGY TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Wet homogeneous sand milling combined with spray drying is an effective method to achieve batch preparation of spherical powders with uniform particle size, but the synthesis of Na 4 Fe 3 (PO 4 ) 2 (P 2 o 7 ) There are almost no reports on the promotion of powder industrialization

Method used

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  • Method for preparing Na4Fe3 (PO4) 2 (P2O7) by homogeneous phase method and application
  • Method for preparing Na4Fe3 (PO4) 2 (P2O7) by homogeneous phase method and application
  • Method for preparing Na4Fe3 (PO4) 2 (P2O7) by homogeneous phase method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0034] A positive electrode active material whose chemical formula is Na 4 Fe 3 (PO 4 ) 2 (P 2 o 7 ), the preparation method of the positive electrode active material is:

[0035] Sodium pyrophosphate Na 4 P 2 o 7 、FePO 4 、CH 3 COONa and citric acid are raw materials, and ethanol is a solvent. Among them, sodium pyrophosphate Na 4 P 2 o 7 Both sodium and phosphorus source, FePO 4 For iron source, sodium acetate CH 3 COONa is a supplementary sodium source, and citric acid is a carbon source;

[0036] 4.4605 g Na 4 P 2 o 7 10 hours 2 O, 9.06 g FePO4, 3.2808 g sodium acetate, and 8.4056 g citric acid monohydrate were added to 500 mL of 95% ethanol, ball milled at 20 rpm for 3 h, then sand milled at 2000 rpm for 3 h, and then 80% of the air inlet rate, 130 ° C Inlet air temperature, 0.5% feed rate feeding is spray-dried to obtain the precursor;

[0037] Then the precursor was placed in an argon atmosphere and calcined at 400 °C for 15 h to obtain Na 4 Fe 3 (...

Embodiment 2

[0040] A positive electrode active material whose chemical formula is Na 3 Fe 2 (PO 4 ) 2 (P 2 o 7 ), the preparation method of the positive electrode active material is:

[0041] as NaH 2 PO 4 , Fe 2 o 3 , Citric acid as raw material, acetone as solvent. Among them, NaH 2 PO 4 Both a source of sodium and phosphorus, Fe 2 o 3 as iron source, glucose as carbon source;

[0042] 18.7212 g NaH 2 PO 4 , 7.185g Fe 2 o 3 12.6084 g of glucose was dispersed in 400mL of 95% acetone, ball milled at 20rpm for 3h, then sand milled at 2000rpm for 3h, and then fed at 80% air inlet rate, 130°C inlet air temperature, and 0.5% feed rate. Spray drying to obtain the precursor;

[0043] Then the precursor was placed in a nitrogen atmosphere and calcined at 500 °C for 10 h to obtain Na 4 Fe 3 (PO 4 ) 2 (P 2 o 7 ). And assemble the button battery in a glove box with water and oxygen lower than 0.01ppm.

[0044] From Figure 4 It can be seen that the Na prepared in this ex...

Embodiment 3

[0046] A positive electrode active material whose chemical formula is Na 4 Fe 3 (PO 4 ) 2 (P 2 o 7 ), the preparation method of the positive electrode active material is:

[0047] Sodium pyrophosphate Na 4 P 2 o 7 、FePO 4 , sodium acetate CH 3 COONa and sucrose are used as raw materials, and ether is used as a solvent. Among them, sodium pyrophosphate Na 4 P 2 o 7 Both sodium and phosphorus source, FePO 4 For iron source, sodium acetate CH 3 COONa is a supplementary sodium source, and citric acid is a carbon source;

[0048] 8.921 g Na 4 P 2 o 7 10 hours 2 O, 18.12 g FePO4, 6.5616 g sodium acetate, and 16.8112 citric acid monohydrate were added to 500 mL of anhydrous diethyl ether, ball milled at 20 rpm for 3 hours, then sand milled at 2000 rpm for 3 hours, and then 80% of the air inlet rate, 130 ° C Air temperature, 0.5% feed rate feeding is spray-dried to obtain the precursor;

[0049] Then the precursor was placed in a mixed atmosphere of argon and hydr...

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Abstract

The invention discloses a method for preparing Na4Fe3 (PO4) 2 (P2O7) by a homogeneous method and an application, and the preparation method comprises the following steps: mixing a carbon source, an iron source, a sodium source and a phosphorus source according to a certain stoichiometric ratio, adding an organic solvent, and sanding to form a homogeneous dispersion system; and carrying out spray drying to obtain a precursor, and sintering the precursor in an inert atmosphere to obtain Na4Fe3 (PO4)2(P2O7) powder. According to the method, the agglomeration phenomenon of the Na4Fe3 (PO4) 2 (P2O7) micro-nano powder can be remarkably improved, the morphology and the electrical performance of the powder are improved, the used organic solvent can be recycled through a cooling system for secondary utilization, the latent heat of vaporization of the organic solvent is far lower than that of water, and the heating power consumption is reduced. Compared with the existing transition metal oxide, Prussian blue and vanadium-based polyanionic compound positive electrode materials, the Na4Fe3 (PO4) 2 (P2O7) positive electrode material prepared by the invention is lower in cost, better in cycling stability, green and pollution-free, and can provide an ideal positive electrode for a commercial sodium ion battery.

Description

technical field [0001] The invention belongs to the technical field of battery electrode material powder preparation, in particular to a homogeneous method for preparing Na 4 Fe 3 (PO 4 ) 2 (P 2 o 7 ) method and application. Background technique [0002] In order to cope with the energy and environmental problems caused by the excessive consumption of fossil fuels, countries around the world have incorporated renewable energy such as solar energy and wind energy into the construction of smart grids. However, the intermittency and instability of renewable energy make it unfavorable to be connected to the grid, so electrochemical energy storage has become the key to efficiently utilize renewable energy. The large installed capacity of the energy storage system puts forward higher requirements on the efficiency, safety and economy of the electrochemical energy storage technology. The working principle of sodium-ion batteries is similar to that of lithium-ion batteries, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/58H01M10/054
CPCC01B25/45H01M4/5825H01M10/054H01M2004/028H01M2004/021C01P2002/72C01P2004/32C01P2006/40Y02E60/10
Inventor 曹余良陈重学付承龙赵阿龙熊健王勤陈世涛
Owner HUBEI WANRUN NEW ENERGY TECH DEV
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