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A preparation method of manganese vanadium molybdenum phosphopolyacid and its application in lithium battery

A technology of heteropoly acid and molybdenum phosphorus, applied in battery electrodes, secondary batteries, circuits, etc., can solve the problems of restricting the application of heteropoly acid and poor electrical conductivity, and achieve the effect of good electrochemical performance and high thermal stability.

Active Publication Date: 2022-02-25
BAOJI KEDIPU NON FERROUS METALS GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, while heteropoly acid has high lithium storage capacity, it also has some defects, such as poor electrical conductivity and easy dissolution in LiPF. 6 Electrolyte, these shortcomings restrict the application of heteropolyacids in lithium-ion battery materials

Method used

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  • A preparation method of manganese vanadium molybdenum phosphopolyacid and its application in lithium battery
  • A preparation method of manganese vanadium molybdenum phosphopolyacid and its application in lithium battery
  • A preparation method of manganese vanadium molybdenum phosphopolyacid and its application in lithium battery

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A preparation method of manganese vanadium molybdenum phosphopolyacid, comprising the following steps:

[0020] Weigh the ammonium metavanadate (NH 4 VO 3 ), 0.4 mmol (0.0624g) sodium dihydrogen phosphate (NaH 2 PO 4 2H 2 O), 2.0 mmol (0.68 g) ammonium dimolybdate ((NH 4 ) 2 Mo 2 o 7 ) and 2.0 mmol (0.49 g) manganese acetate ((CH 3 COO) 2 Mn 4H 2 O) Dissolve in 25 mL of distilled water, stir to dissolve evenly, and use ammonia water NH 3 ·H 2 O adjusted the pH=13 of the solution to obtain an orange mixture turbid solution; the obtained orange mixture turbid solution was transferred to a 50 mL reaction kettle, and continued to react at 160° C. for 72 hours, naturally cooled to room temperature, and centrifuged to obtain Orange solid sample; the sample was washed three times alternately with distilled water and absolute ethanol, and dried in an oven at 75 °C for 15 hours to obtain a solid powder; the solid powder was sintered in a muffle furnace at a high temp...

Embodiment 2

[0023] Weigh 1.0 mmol (0.117 g) of ammonium metavanadate (NH 4 VO 3 ), 2.0 mmol (0.212 g) sodium dihydrogen phosphate (NaH 2 PO 4 2H 2 O), 10 mmol (3.40 g) ammonium dimolybdate ((NH 4 ) 2 Mo 2 o 7 ) and 1.0 mmol (0.245 g) manganese acetate ((CH 3 COO) 2 Mn 4H 2 O) Dissolve in 30 mL of distilled water, stir to dissolve evenly, and use ammonia water NH 3 ·H 2 O adjusted the pH=10 of the solution to obtain an orange mixture turbid solution; the obtained orange mixture turbid solution was transferred to a 50 mL reaction kettle, and continued to react at 190° C. for 36 hours, naturally cooled to room temperature, and centrifuged to obtain Orange solid sample; the sample was washed three times alternately with distilled water and absolute ethanol, and dried in an oven at 85°C for 10 hours to obtain a solid powder; the solid powder was sintered in a muffle furnace at a high temperature of 800°C for 3 hours to obtain a brown solid, Mn 7 [VP 2 Mo 17 o 62 ] 2 .

[0024...

Embodiment 3

[0026] Weigh 1.0 mmol (0.117 g) of ammonium metavanadate (NH 4 VO 3 ), 2.0 mmol (0.212 g) sodium dihydrogen phosphate (NaH 2 PO 4 2H 2 O), 10 mmol (3.40 g) ammonium dimolybdate ((NH 4 ) 2 Mo 2 o 7 ) and 1.0 mmol (0.245 g) manganese acetate ((CH 3 COO) 2 Mn 4H 2 O) Dissolve in 30 mL of distilled water, stir to dissolve evenly, and use ammonia water NH 3 ·H 2 O adjusted the pH=12 of the solution to obtain an orange mixture turbid solution; the resulting orange mixture turbid solution was transferred to a 50 mL reaction kettle, and continued to react at 170° C. for 48 hours, naturally cooled to room temperature, and centrifuged to obtain Orange solid sample; the sample was alternately washed three times with distilled water and absolute ethanol, and dried in an oven at 80 °C for 12 h to obtain a solid powder; the solid powder was sintered in a muffle furnace at a high temperature of 700 °C for 4 hours to obtain a brown solid , that is, manganese vanadium molybdenum ph...

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Abstract

The invention discloses a manganese vanadium molybdenum phosphorus heteropolyacid Mn 7 [P 2 Mo 17 VO 62 ] 2 method of preparation. The present invention uses ammonium metavanadate, sodium dihydrogen phosphate, ammonium molybdate, and manganese acetate as the main raw materials, adding an appropriate amount of distilled water to dissolve, adjusting the pH value, carrying out hydrothermal reaction to obtain precipitation, drying the precipitated product and performing high-temperature sintering. Obtain the manganese vanadium molybdenum phosphoheteropolyacid. Electrochemical tests show that the prepared manganese vanadium molybdenum phosphopolyacid has good electrochemical performance and broad application prospects as the negative electrode material of lithium ion battery. In the whole preparation process, the operation is simple, the cost of raw materials is low, the investment in equipment is small, and it is suitable for mass production.

Description

technical field [0001] The invention relates to the technical field of lithium battery materials, in particular to a preparation method of manganese vanadium molybdenum phosphate heteropolyacid and its use as a lithium battery negative electrode material. Background technique [0002] Heteropoly acid compound (HPC), also known as polyoxometalate (POM), is a kind of inorganic metal composed of counter cations and transition metal atoms according to a certain spatial structure, through the coordination bridge of oxygen atoms clusters. Among them, heteropolyanions are usually central atoms (P, Si, Co, Ge, Al, Fe, etc.) and coordination atoms (V, Mo, W, Nb, Ta, etc.), and counter cations include H + 、Na + , NH 4 + Etc., the space structure includes four types such as tetrahedron, coplanar, common edge and common point. The current research involves more molybdenum-based and tungsten-based two categories. [0003] Vanadium molybdenum phosphopolyacid is a dual-functional cat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/485H01M4/505H01M10/0525
CPCH01M4/485H01M4/505H01M10/0525H01M2004/027Y02E60/10
Inventor 夏雨李星
Owner BAOJI KEDIPU NON FERROUS METALS GROUP
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