Sodium vanadium fluorophosphate, preparation method and uses thereof

A technology for vanadium fluorophosphate sodium salt and vanadium phosphate sodium salt is applied in the field of rapid preparation at room temperature, vanadium fluorophosphate sodium salt Na32F3-2x, and can solve the problems of long time consumption, high requirements for raw material solubility, long ball milling time and the like, To achieve the effect of reducing costs

Active Publication Date: 2017-09-12
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2010, Jiangqing zhao and others proposed the sol-gel method to prepare sodium vanadium phosphate. Although the process is simple, the heat treatment temperature is as high as 800°C
CN103594716A discloses the preparation of NaVPO by sol-gel assisted two-stage high-temperature solid-phase method 4 F, but its process is complex, requires two calcinations, the calcination temperature is as high as 850 ° C, and has high requirements for the solubility of raw materials, so it is difficult to achieve large-scale production
CN 102509789A discloses the synthesis of Na 3 (VOxPO 4 ) 2 f 3-2x (0≤x≤1), although only one-step synthesis is required, the

Method used

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  • Sodium vanadium fluorophosphate, preparation method and uses thereof
  • Sodium vanadium fluorophosphate, preparation method and uses thereof
  • Sodium vanadium fluorophosphate, preparation method and uses thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0076] A preparation method of vanadium sodium salt of fluorophosphate, said method comprising the steps of:

[0077] (1) Dissolving 3.260g of vanadyl sulfate in 40mL of deionized water to obtain a vanadium source solution;

[0078] (2) Add 4.716g sodium dihydrogen phosphate dihydrate and 1.285g sodium fluoride (V:P:F:Na about 1:3:3:6) to the vanadium source solution, stir to dissolve, and heat at 90°C Insulated in an oven for 3h, filtered to obtain a reaction mixture;

[0079] (3) The obtained reaction mixture was washed 7 times with deionized water and 1 time with ethanol, and then dried in air at 60° C. for 5 h to obtain 1.785 g of the product.

[0080] Gained product is carried out XRD test, test result is as follows figure 1 As shown, the test results show that the obtained product is Na 3 (VOPO 4 ) 2 F, and it has good crystallinity and high purity.

[0081] The resulting product was analyzed by a scanning electron microscope (SEM), and the characterization results...

Embodiment 2

[0084] A preparation method of vanadium sodium salt of fluorophosphate, said method comprising the steps of:

[0085] (1) 0.326g vanadyl sulfate and 0.158g vanadium trichloride were dissolved in 8mL deionized water to obtain a vanadium source solution;

[0086] (2) Add 416uL phosphoric acid and 0.143g sodium fluoride (V:P:F:Na about 1:3:1.7:1.7) to the vanadium source solution, stir and adjust the pH to 3.3 with solid sodium hydroxide, and the obtained The suspension containing the precipitate was heated in a water bath at 80°C for 1 hour, and then filtered to obtain a reaction mixture;

[0087] (3) The reaction mixture was washed 6 times with deionized water and 1 time with ethanol, and dried in air at 70° C. for 5 hours to obtain 0.295 g of the product.

[0088] Carry out XRD and SEM test to gained product, test result is as follows Figure 4 with Figure 5 shown. The XRD test result shows that the obtained product is Na 3 (VO 0.5 PO 4 ) 2 f 2 , The SEM image shows ...

Embodiment 3

[0090] A preparation method of vanadium sodium salt of fluorophosphate, said method comprising the steps of:

[0091] (1) 1.630g of vanadyl sulfate was dissolved in 20mL of deionized water to obtain a vanadium source solution;

[0092] (2) Add 7.242g disodium hydrogen phosphate dodecahydrate and 1.071g sodium fluoride (V:P:F:Na about 1:4:5:13) to the vanadium source solution, filter to obtain the reaction mixture;

[0093] (3) The reaction mixture was washed 6 times with deionized water, and then dried in air at 100° C. for 5 h to obtain 1.483 g of the product.

[0094] Carry out XRD and SEM test to gained product, test result is as follows Image 6 with Figure 7 shown. XRD showed that the obtained product was Na 3 (VOPO 4 ) 2 F, and the product has good crystallinity and high purity; the SEM figure shows that the morphology of the product obtained is a micron-scale aggregate.

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Abstract

The present invention provides a sodium vanadium fluorophosphate, a preparation method and uses thereof, wherein the molecular formula of the sodium vanadium fluorophosphate is Na3(VOxPO4)2F3-2x, x is more than or equal to 0 and is less than or equal to 1, the morphology is a spherical wool ball, loose hollow ball or nanoparticle aggregate, and the size is from nanometer to micron. The preparation method comprises: (1) dissolving a vanadium source in water to obtain a vanadium source solution; (2) adding a phosphorus source, a fluorine source and a sodium source to the vanadium source solution to obtain a reaction mixture; and (3) post-treating the obtained reaction mixture to obtain the sodium vanadium fluorophosphate. According to the present invention, the water is directly used as the solvent so as to provide the advantage of no pollution; the sodium vanadium fluorophosphates can be directly synthesized at the room temperature of 10-35 DEG C, such that the temperature is low, the reaction kinetics is rapid, and the large-scale preparation of the sodium vanadium fluorophosphates can be achieved; the morphology and the crystallinity of the sodium vanadium fluorophosphate can be adjusted; the pentavalent vanadium industrial product can be used as the vanadium source so as to substantially reduce the cost of the vanadium source; and the prepared material has good electrochemical properties, and is suitable for the sodium ion battery positive electrode material.

Description

technical field [0001] The invention belongs to the technical field of electrode materials, and relates to a vanadium sodium fluorophosphate salt Na 3 (VO x PO 4 ) 2 f 3-2x (0≤x≤1) and its preparation method and application, especially a kind of vanadium sodium salt of fluorophosphate Na 3 (VO x PO 4 ) 2 f 3-2x (0≤x≤1), its rapid preparation method at room temperature and its use. Background technique [0002] At present, the global power energy is still dominated by thermal power, supplemented by nuclear power and hydropower. In recent years, in order to cope with the energy crisis and alleviate the increasingly severe environmental pressure, renewable energy has been developed and utilized. Research and development of efficient and cheap large-scale energy storage technology has become a key link in the sustainable development of electric energy and an important part of the country's future energy strategy. An electrochemical energy storage system with an energy...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M10/0525
CPCH01M4/582H01M4/5825H01M10/0525Y02E60/10
Inventor 赵君梅戚钰若潘峰刘会洲穆林沁胡勇胜
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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