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Preparation method of sodium vanadium phosphate material

A technology of sodium vanadium phosphate and phosphate, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of particle size uniformity and particle size of difficult particles, achieve rapid nucleation and reduce crystal nuclei The effect of growing up and increasing the electronic conductivity

Active Publication Date: 2022-06-03
ANSTEEL BEIJING RES INST
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, so far, there are few reports on the preparation of nano-scale sodium vanadium phosphate, and it is difficult to effectively control the uniformity and particle size of its particle size at the nano-scale.

Method used

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  • Preparation method of sodium vanadium phosphate material
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  • Preparation method of sodium vanadium phosphate material

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preparation example Construction

[0034] The embodiment of the present invention provides a preparation method of a sodium vanadium phosphate material, and the method comprises the following steps:

[0035] 1) Dissolving the vanadium source in deionized water is denoted as solution A;

[0036] 2) Dissolve the alkaline substance in deionized water, denoted as solution B; then add solution B dropwise to solution A, stir to pH=4~8 of the mixed solution at room temperature, and obtain vanadium oxyhydroxide precursor after centrifugal filtration ;

[0037] 3) Dissolve phosphate, or phosphate and fluoride in deionized water, and denote it as solution C; then disperse the vanadium oxyhydroxide precursor obtained in step 2) in solution C, stir at room temperature for 0.5-24 h, filter, After drying, the sodium vanadium phosphate material is obtained.

[0038] In some embodiments, the molecular formula of the sodium vanadium phosphate material prepared by the method of the present invention is NaVOPO 4 , Na 3 (VOPO ...

Embodiment 1

[0052] A preparation method of sodium vanadium phosphate material, comprising the steps:

[0053] 1) Weigh 1.6 g of vanadyl sulfate, dissolve it in 50 mL of deionized water, and prepare solution A.

[0054] 2) Weigh 2.8 g of sodium hydroxide, dissolve it in 50 mL of deionized water, and configure it as solution B; then add solution B dropwise to solution A at a rate of one drop per second, stir continuously to pH=5 at room temperature, and centrifuge. Vanadium oxyhydroxide precursor is obtained after filtration, and its XRD pattern is as follows figure 1 The middle curve 1 is shown.

[0055] 3) Weigh 1.2 g of sodium fluoride and 9.0 g of sodium dihydrogen phosphate, dissolve in 50 ml of deionized water, and configure solution C. The vanadium oxyhydroxide precursor obtained in step 2) is dispersed in solution C, continuously stirred at room temperature for 24 h, filtered and dried to obtain the product.

[0056] XRD test is carried out to the product obtained in the present ...

Embodiment 2

[0060] A preparation method of sodium vanadium phosphate material, comprising the steps:

[0061] 1) Weigh 2.6 g of vanadium chloride, dissolve it in 50 mL of deionized water, and prepare solution A.

[0062] 2) Weigh 2.4 g of sodium hydroxide, dissolve it in 50 mL of deionized water, and configure it as solution B; then add solution B dropwise to solution A at a rate of one drop per second, stir continuously to pH=7 at room temperature, and centrifuge. The vanadium oxyhydroxide precursor is obtained after filtration.

[0063] 3) Weigh 1.2 g of sodium fluoride and 10.6 g of disodium hydrogen phosphate, dissolve them in 50 ml of deionized water, and configure solution C. The vanadium oxyhydroxide precursor obtained in step 2) is dispersed in solution C, continuously stirred at room temperature for 12 h, filtered and dried to obtain the product.

[0064] XRD and SEM tests were carried out on the obtained products, and the test results were as follows Image 6 and Figure 7 s...

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Abstract

The invention discloses a preparation method of a sodium vanadium phosphate material, which comprises the following steps: 1) dissolving a vanadium source in deionized water to obtain a solution A; 2) dissolving an alkaline substance in deionized water to obtain a solution B; dropwise adding the solution B into the solution A, stirring until the pH value of the mixed solution is 4-8, and centrifugally filtering to obtain a hydroxyl vanadium oxide precursor; 3) dissolving phosphate or phosphate and fluoride in deionized water to obtain a solution C; and dispersing hydroxyl vanadium oxide in the solution C, stirring for 0.5-24 hours, filtering, and drying to obtain the sodium vanadium phosphate material. The method comprises the following steps: firstly, quickly precipitating vanadium by using an alkaline solution to form a nanoscale hydroxyl vanadium oxide precursor; according to the preparation method, PO4 < 3->, F <-> and other anions are utilized for in-situ ion exchange with OH <->, the nanoscale sodium vanadium phosphate material is obtained, controllable preparation of nanoscale sodium vanadium phosphate is achieved, and the preparation method is easy to operate, mild in reaction condition and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of electrode materials, and in particular, the invention relates to a preparation method of a sodium vanadium phosphate material. Background technique [0002] As a sodium ion superconductor material, sodium vanadium phosphate has excellent sodium ion migration efficiency, and has become a popular object of research as a cathode material for sodium ion secondary batteries. At this stage, the preparation methods of sodium vanadium phosphate materials mainly focus on high-temperature solid-phase synthesis, sol-gel method and other methods. For example, in 2012, Hao Xiaogang et al. reported the synthesis of Na using a sol-gel method at a heat treatment temperature of 700 °C. 3 (VPO 4 ) 2 F 3 And patent CN103594716A discloses a kind of method that utilizes sol-gel to assist 850 ℃ of high temperature solid phase, successfully prepared sodium vanadium phosphate, but the particle size distribution of the sodium vanadium ...

Claims

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Application Information

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IPC IPC(8): C01B25/455
CPCC01B25/455C01P2004/62C01P2002/72C01P2004/03C01P2006/40Y02E60/10
Inventor 张东彬滕艾均代宇刘天豪彭显著尹翔鹭曾泽华
Owner ANSTEEL BEIJING RES INST