Sodium vanadium fluorophosphate as well as low-temperature environment-friendly preparation method and use thereof

A technology of vanadium sodium fluorophosphate and vanadium sodium phosphate, which is applied in the field of low-temperature green preparation of vanadium sodium fluorophosphate, and can solve the problems of restricting large-scale industrial production, high energy consumption, and complex synthesis processes, etc.

Inactive Publication Date: 2017-03-15
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the problems of large-scale industrial production caused by high-temperature preparation of crystalline vanadium sodium fluorophosphate at high temperature and complex synthesis process, as well as the high temperature of hydrothermal preparation in the low-temperature preparation method and pollution caused by the use of solvents One of the objectives of the present invention is to provide a low-temperature green preparation method of sodium vanadium phosphate

Method used

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  • Sodium vanadium fluorophosphate as well as low-temperature environment-friendly preparation method and use thereof
  • Sodium vanadium fluorophosphate as well as low-temperature environment-friendly preparation method and use thereof
  • Sodium vanadium fluorophosphate as well as low-temperature environment-friendly preparation method and use thereof

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Embodiment 1

[0072] 0.359g of vanadium acetylacetonate, 208 μL of concentrated phosphoric acid (85wt%) and 0.072g of sodium fluoride were ultrasonically dispersed in 4mL of deionized water to obtain a uniformly mixed aqueous solution. In the resulting mixed aqueous solution, the molar ratio of Na:V:P:F was about The ratio is 1.7:1:3:1.7, the above mixed aqueous solution is transferred to a hydrothermal reaction kettle, the temperature is raised to 80°C at a rate of 5°C per minute, and the temperature is kept at this temperature for 6h, and the product is passed through a certain amount of deionized water Alternately washed with ethanol for 6 times, dried in air at 60° C. for 3 h, and weighed to obtain 0.150 g of the product, with a yield of 71.6%. XRD shows that the product is Na 3 (VPO 4 ) 2 f 3 , has the characteristics of good crystallinity and high purity; the SEM image shows that the shape of the obtained product is irregular, and it is a sheet-like structure with a thickness of ab...

Embodiment 2

[0074] 0.274g vanadyl acetylacetonate, 104 μL concentrated phosphoric acid (85wt%) and 0.072g sodium fluoride were ultrasonically dispersed in 2mL deionized water to obtain a uniformly mixed mixed aqueous solution. The molar ratio of Na:V:P:F in the resulting mixed aqueous solution About 1.7:1:1.5:1.7, transfer the above mixed aqueous solution into a hydrothermal reaction kettle, raise the temperature to 120°C at a rate of 5°C per minute, and keep the temperature at this temperature for 10h, and the product will undergo a certain amount of deionization Washed alternately with water and acetone for 8 times, dried in air at 65° C. for 2 hours, and weighed to obtain 0.162 g of the product, with a yield of 77.3%. XRD shows that the product is Na 3 (VOPO 4 ) 2 F, has the characteristics of good crystallinity and high purity; the SEM image shows that the obtained product has an irregular shape and is a sheet-like structure with a thickness of about 1 μm; its XRD and SEM are respec...

Embodiment 3

[0076] 0.318g of vanadium trichloride, 0.944g of sodium dihydrogen phosphate dihydrate and 0.286g of sodium fluoride were ultrasonically dispersed in 3mL of deionized water to obtain a uniformly mixed aqueous solution. The molar ratio of Na:V:P:F in the obtained mixed aqueous solution The ratio is about 6.4:1:3:3.3. Transfer the above mixed aqueous solution into a hydrothermal reaction kettle, raise the temperature to 120°C at a rate of 4°C per minute, and keep the temperature at this temperature for 8 hours. The deionized water and ethanol were alternately washed 6 times, dried in the air at 70° C. for 5 h, and 0.324 g of the product was obtained by weighing, with a yield of 77.4%. XRD shows that the product is Na 3 (VPO 4 ) 2 f 3 , has the characteristics of good crystallinity and high purity. The SEM image shows that the obtained product is a flower-like micron structure with uniform particle size distribution and less agglomeration, with a diameter of about 5-10 μm and...

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Abstract

The invention belongs to the technical field of electrode materials and relates to sodium vanadium fluorophosphate as well as a low-temperature environment-friendly preparation method and use thereof. The preparation method comprises the steps of preparing a mixed water solution of a sodium source, a vanadium source, a phosphorus source and a fluorine source, reacting by virtue of the mixed water solution at 20-180 DEG C to obtain sodium vanadium fluorophosphate, wherein the vanadium source is a trivalent vanadium source and/or a tetravalent vanadium source; the chemical constitution of sodium vanadium fluorophosphate is Na3(VOxPO4)2F3-2x, and x is more than or equal to 0 and less than or equal to 1. According to the low-temperature environment-friendly preparation method, the mixed water solution of the sodium source, thephosphorus source, the fluorine source and the trivalent vanadium source and/or a tetravalent vanadium source can generate spontaneous reaction at 20-35 DEG C, the reaction can be accelerated at a temperature high than 35 DEG C and lower than 180 DEG C, and well-crystallized sodium vanadium fluorophosphate can be obtained. Sodium vanadium fluorophosphate can be used as an anode to be assembled into a battery, the specific discharge capacity is not lower than 100mAh/g, and the cycling stability is good.

Description

technical field [0001] The invention belongs to the technical field of electrode materials, in particular to a 3 (VO x PO 4 ) 2 f 3-2x , 0≤x≤1 vanadium sodium phosphate salt, low-temperature green preparation method and use thereof. Background technique [0002] Sodium and lithium in the same main group have similar chemical properties, and sodium is abundant and widely distributed on the earth, so sodium-ion batteries, like lithium-ion batteries, have gradually received widespread attention. Like lithium-ion batteries, sodium-ion batteries are still composed of positive and negative electrode materials, electrolytes and separators, among which the positive electrode material is the key factor restricting the large-scale development of sodium-ion batteries. Suitable cathode materials for sodium-ion batteries must have high redox potential and specific capacity, sufficient ion diffusion channels, small changes in structure with the amount of sodium intercalated, high ele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455H01M4/58
CPCY02E60/10
Inventor 赵君梅戚钰若刘会洲
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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