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Iron phosphate dihydrate with flexibly adjustable crystal structure and preparation method thereof

A technology of ferric phosphate dihydrate and crystal structure, applied in structural parts, chemical instruments and methods, secondary batteries, etc., can solve the problem of unimproved ionic conductivity, achieve uniform size, improve ion mobility, and rate performance Good results

Active Publication Date: 2021-11-19
HUBEI HONGRUN HIGH-TECH NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Regardless of carbon coating technology or metal ion doping technology, only the electronic conductivity of lithium iron phosphate material is improved, and the equally important ionic conductivity has not been improved.

Method used

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  • Iron phosphate dihydrate with flexibly adjustable crystal structure and preparation method thereof
  • Iron phosphate dihydrate with flexibly adjustable crystal structure and preparation method thereof
  • Iron phosphate dihydrate with flexibly adjustable crystal structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Configure 1.2mol / L ferrous sulfate solution and phosphate solution.

[0033] Weigh the ferrous solution and the phosphate solution according to the molar ratio Fe:P=1:1 for later use, and weigh the excess hydrogen peroxide by 30% for later use.

[0034] Add the weighed phosphate and hydrogen peroxide dropwise to the ferrous solution at the same time, add ammonia water to adjust the pH of the synthetic slurry to 2.2, and react for 1 hour to prepare an amorphous ferric phosphate slurry.

[0035] The amorphous ferric phosphate slurry is pumped into the filter press for filter press rinsing, using pure water with a conductivity lower than 10µs / cm for rinsing, and the conductivity is washed to 5ms / cm to obtain a clean filter cake.

[0036] The filter cake is transported to the paddle tank, and added according to the weight ratio of filter cake and water of 1:5 to obtain a slurry with a solid content of 20%.

[0037] Phosphoric acid and ammonia water are added to the slurry ...

Embodiment 2

[0043] Configure 1.2mol / L ferrous sulfate solution and phosphate solution.

[0044] Weigh the ferrous solution and phosphate solution according to Fe:P=1:1.01 for later use, and weigh 30% excess hydrogen peroxide for later use.

[0045] Add the weighed phosphate and hydrogen peroxide dropwise to the ferrous solution at the same time, add ammonia water to adjust the pH of the synthetic slurry to 3.0, and react for 1 hour to prepare an amorphous ferric phosphate slurry.

[0046] The amorphous ferric phosphate slurry is pumped into the filter press for filter press rinsing, using pure water with a conductivity lower than 10 µs / cm for rinsing, and the conductivity is washed to 5 ms / cm to obtain a clean filter cake.

[0047] Transport the filter cake to the paddle tank, and add it according to the weight ratio of filter cake and water of 1:10 to obtain a slurry with a solid content of 10%;

[0048] Phosphoric acid and ammonia water are added to the slurry to adjust the pH value of...

Embodiment 3

[0054] Configure 1.2mol / L ferrous sulfate solution and phosphate solution.

[0055] Weigh the ferrous solution and phosphate solution according to Fe:P=1:1.05 for later use, and weigh 30% excess hydrogen peroxide for later use.

[0056] Add the weighed phosphate and hydrogen peroxide dropwise into the ferrous solution at the same time, add ammonia water to adjust the pH of the synthetic slurry to 3.5, and react for 1 hour to prepare an amorphous ferric phosphate slurry.

[0057] The amorphous ferric phosphate slurry is pumped into the filter press for filter press rinsing, using pure water with a conductivity lower than 10µs / cm for rinsing, and the conductivity is washed to 5ms / cm to obtain a clean filter cake.

[0058] The filter cake is transported to the paddle tank, and added according to the weight ratio of filter cake and water of 1:2.5 to obtain a slurry with a solid content of 30%.

[0059] Phosphoric acid and ammonia water are added to the slurry to adjust the pH val...

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Abstract

The invention discloses iron phosphate dihydrate with flexibly adjustable crystal structure and a preparation method thereof. The method comprises the following steps: dissolving ferrous sulfate, and removing impurities to prepare a ferrous sulfate reaction solution A; preparing a phosphorus salt solution B from monoammonium phosphate NH4H2PO4 or diammonium phosphate (NH4)2HPO4 according to a certain proportion; reacting the solution A, the solution B and an oxidizing agent to prepare amorphous iron phosphate, and carrying out filter pressing and rinsing by using a filter press to remove impurity elements in an ionic state so as to obtain a clean filter cake; and adding water to disperse the filter cake, adding a certain amount of phosphoric acid to adjust the acidity, and adding non-quantitative ammonia water, wherein the prepared iron phosphate has two phases, namely Fe(PO4).2H2O and NH4Fe2(OH)(PO4)2.2 H2O. According to the invention, the two-phase proportion can be flexibly adjusted according to different adding amounts of ammonia water, iron phosphate particles prepared by the method are uniform in size, compact, spheroidic, high in purity and low in impurity element content, the morphology of the lithium iron phosphate positive electrode material can be regulated and controlled by adjusting the crystal structure of the iron phosphate, and the rate capability of the material is improved.

Description

technical field [0001] The invention relates to the technical field of synthesis process control, in particular to ferric phosphate dihydrate which can flexibly adjust the crystal structure and a preparation method thereof. Background technique [0002] Lithium-ion batteries have attracted widespread attention due to their high energy density, long life, and environmental friendliness. Among them, the positive electrode material is the core material that affects the key performance of lithium-ion batteries. At present, the commonly used stable materials mainly include lithium cobaltate, lithium manganate, nickel-cobalt-manganese ternary, and lithium iron phosphate. Lithium iron phosphate is a battery material with an olivine structure. It has a stable and reliable structure, small deformation during cycling, and long life. It has gradually become the first choice for energy storage power stations and new energy electric vehicles. However, the intrinsic conductivity of lithi...

Claims

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Application Information

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IPC IPC(8): C01B25/37H01M4/58H01M10/0525
CPCC01B25/375H01M4/5825H01M10/0525C01P2002/72C01P2004/03C01P2006/40C01P2006/80Y02E60/10
Inventor 郭米艳李仲君张伟
Owner HUBEI HONGRUN HIGH-TECH NEW MATERIALS CO LTD
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