A kind of sodium vanadium fluorophosphate and its preparation method and application

A technology of vanadium sodium salt of fluorophosphate and organic phosphoric acid, which is applied to structural parts, electrical components, battery electrodes, etc., can solve problems such as difficult operation and high energy consumption, and achieve resource and cost saving, high discharge specific capacity, and electrochemical The effect of excellent performance

Active Publication Date: 2018-11-02
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In view of the above-mentioned prior art for the preparation of sodium vanadium phosphate, high-temperature solid-phase calcination is used, the problems of high energy consumption, difficult operation, etc., and the application of solvent extraction to achieve phase transfer in the preparation of ternary and multi-component inorganic compounds

Method used

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  • A kind of sodium vanadium fluorophosphate and its preparation method and application
  • A kind of sodium vanadium fluorophosphate and its preparation method and application
  • A kind of sodium vanadium fluorophosphate and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0055] P507 and N1923 are mixed in molar ratio 1:1 to obtain mixed extractant PN; 10g mixed extractant is dissolved in 50ml n-heptane, and its mass volume percent concentration is 20%; 25ml above-mentioned PN-n-heptane solution is mixed with 2ml Commercial concentrated phosphoric acid is mixed into a homogeneous phase (the volume ratio of PN-n-heptane solution to commercial concentrated phosphoric acid is 12.5:1), and the concentration of phosphoric acid is 2mol / L to obtain 4 3- Microemulsion phase with a concentration of about 1.06mol / L; 0.180g vanadium acetylacetonate, 1.5mL containing PO4 3- The above-mentioned microemulsion phase, 0.035g sodium fluoride (Na:V:P:F is about 1.6:1:3:1.6) are ultrasonically dispersed in 1.5mL ethanol and 0.5mL acetone to obtain a uniformly mixed reaction material; Transfer the uniformly mixed material 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 f...

Embodiment 2

[0057] Mix Cyanex272 and N1923 at a molar ratio of 1:1 to obtain a mixed extractant; dissolve 10 g of the mixed extractant in 100 ml of n-heptane, and its mass volume percentage concentration is 10%; mix 25 ml of the above PN-n-heptane solution with 4 ml of commercial Concentrated phosphoric acid is mixed into a homogeneous phase, (the volume ratio of PN-n-heptane solution to commercial concentrated phosphoric acid is 6.25:1), and the concentration of phosphoric acid is 3mol / L to obtain 4 3- Microemulsion phase with a concentration of about 2.0mol / L; 0.137g vanadyl acetylacetonate, 0.75mL containing PO 4 3-The above-mentioned microemulsion phase, 0.035g sodium fluoride (Na:V:P:F is about 1.6:1:3:1.6) are ultrasonically dispersed in 1.5mL ethanol and 0.5mL acetone to obtain a uniformly mixed reaction material; Transfer the uniformly mixed material 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 ...

Embodiment 3

[0059] Except that 20g mixed extractant is dissolved in 100ml n-hexane, and its mass volume percent concentration is 20%; the volume ratio of PN-n-heptane solution to commercial concentrated phosphoric acid is 3.85:1, and wherein the phosphoric acid concentration is 1mol / L, to obtain PO-containing 4 3- Microemulsion phase; according to Na:V:P:F about 1:1:1:1, vanadium tribromide, containing PO 4 3- The above microemulsion phase, hydrofluoric acid and sodium dihydrogen phosphate were ultrasonically dispersed in 1.5mL ethanol and 0.5mL acetone; the temperature was raised to 140°C at a heating rate of 4°C per minute, and kept at this temperature for 5h; Dry in the air for 2 hours, and the rest of the steps are the same as in Example 1.

[0060] Product 0.092 is weighed, and productive rate is close to 90%, and XRD shows that product is Na 3 (VPO 4 ) 2 f 3 , has the characteristics of good crystallinity and high purity; the upper organic phase is volatilized to remove the or...

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Abstract

The invention provides a preparation method for vanadium sodium fluorophosphorate. The preparation method comprises the following steps: (1) preparing an acid-base-coupled extraction agent; (2) preparing a microemulsion phase containing PO4<3->; (3) with a sodium source compound, a vanadium source compound, a fluorine source compound and the microemulsion phase prepared in the step (2) as raw materials, dissolving the raw materials or dispersing the raw materials in an organic solvent; and (4) transferring a mixture obtained in the step (3) into a reaction vessel, heating the mixture to 80 to 140 DEG C for a reaction, then carrying out natural cooling to room temperature, then carrying out centrifugation, recovering an organic phase located at an upper layer and obtained after centrifugation so as to obtain the acid-base-coupled extraction agent and subjecting a precipitate to washing and drying so as to obtain vanadium sodium fluorophosphorate powder. The prepared vanadium sodium fluorophosphorate has the characteristics of good crystallinity and high purity; a nano-micro material thereof has excellent electrochemical performance; and more importantly, the acid-base-coupled extraction agent is recoverable and recyclable.

Description

technical field [0001] The invention belongs to the technical field of electrode materials, in particular to a vanadium sodium fluorophosphate salt Na 3 (VO 1-x PO 4 ) 2 f 1+2x (x=0, 1) and its preparation method and use. Background technique [0002] Lithium-ion batteries have attracted widespread attention due to their advantages such as small size, light weight, large specific capacity, long cycle life, and no memory effect, and their market demand is gradually increasing. However, lithium-ion batteries also have disadvantages such as low-temperature lithium precipitation, low conductivity, and easy sintering; in addition, the high raw material cost of lithium-ion batteries has also become a bottleneck restricting its rapid development. The chemical properties of sodium ions and lithium ions, which are also the main group I, have many similarities, and the raw material cost of sodium-ion batteries is low, the half-cell potential is relatively high, and the safety per...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58
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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