Preparation method of battery-grade iron phosphate

An iron phosphate, battery-level technology, applied in chemical instruments and methods, phosphorus compounds, heating water/sewage treatment, etc., can solve the untargeted problems of high ammonia nitrogen wastewater, low value of by-products, low anion content, etc., and achieve reduction Energy consumption, low impurity content and high yield

Inactive Publication Date: 2019-11-22
RUYUAN DONGYANGGUANG MAGNETIC MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is following shortcoming in said method: production mother liquor is in high ammonia nitrogen waste water, as (NH 4 ) 2 SO 4 , NH 4 Cl, NH 4 NO 3 , at the same time to ensure that the anions (such as SO 4 2- , Cl - , NO 3- ) content is low, it is usually necessary to use a large amount of pure water to wash the ferric phosphate filter cake after press filtration, thereby producing a large amount of ammonia nitrogen (such as (NH 4 ) 2 SO 4 , NH 4 Cl, NH 4 NO 3 ) waste water
If this kind of high ammonia n...

Method used

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  • Preparation method of battery-grade iron phosphate

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Embodiment 1

[0030] A preparation method of battery-grade iron phosphate, comprising the steps of:

[0031] S1. Use 99% iron powder as raw material, add 10% dilute sulfuric acid solution, obtain ferrous sulfate solution after fully dissolving, iron mass fraction 5.4%;

[0032] S2. be that 5.4% ferrous sulfate solution 1716kg is added in the reactor with iron massfraction, the stirring speed of reactor is 180rpm, with massfraction be 27.5% hydrogen peroxide 133kg, massfraction is 85% H 3 PO 4 193kg, added into the reactor to form a mixed solution of phosphoric acid and ferric sulfate, wherein the oxidizing agent: H 3 PO 4 : the mol ratio of ferrous sulfate is 0.65:1.01:1;

[0033] S3. Add pure water to the mixed solution of phosphoric acid and ferric sulfate for dilution, adjust the pH value of the mixed solution to 1.7, and the reaction time is 2 hours, and the temperature is controlled at 40 ° C to make Fe 3+ with PO 4 3- combine and settle down;

[0034] S4. After the iron phosph...

Embodiment 2

[0036] A preparation method of battery-grade iron phosphate, comprising the steps of:

[0037] S1. Use 99% iron powder as raw material, add 10% dilute sulfuric acid solution, obtain ferrous sulfate solution after fully dissolving, iron mass fraction 5.4%;

[0038] S2. adding the ferrous sulfate solution that the iron mass fraction is 5.4% in the reactor, the reactor stirring speed is 180rpm, with the hydrogen peroxide that the mass fraction is 27.5%, the H that the mass fraction is 85% 3 PO 4 , added into the reactor to form a mixed solution of phosphoric acid and ferric sulfate, in which the oxidizing agent: H 3 PO 4 : the molar ratio of ferrous sulfate is 0.6:1:1;

[0039]S3. Add pure water to the mixed solution of phosphoric acid and ferric sulfate for dilution, adjust the pH value of the mixed solution to 1.7, and the reaction time is 2 hours, and the temperature is controlled at 40 ° C to make Fe 3+ with PO 4 3- combine and settle down;

[0040] S4. After the iron ...

Embodiment 3

[0042] A preparation method of battery-grade iron phosphate, comprising the steps of:

[0043] S1. Use 99% iron powder as raw material, add 10% dilute sulfuric acid solution, obtain ferrous sulfate solution after fully dissolving, iron mass fraction 5.4%;

[0044] S2. adding the ferrous sulfate solution that the iron mass fraction is 5.4% in the reactor, the reactor stirring speed is 180rpm, with the hydrogen peroxide that the mass fraction is 27.5%, the H that the mass fraction is 85% 3 PO 4 , added into the reactor to form a mixed solution of phosphoric acid and ferric sulfate, in which the oxidizing agent: H 3 PO 4 : the mol ratio of ferrous sulfate is 0.75:1.05:1;

[0045] S3. Add pure water to the mixed solution of phosphoric acid and ferric sulfate for dilution, adjust the pH value of the mixed solution to 1.7, and the reaction time is 2 hours, and the temperature is controlled at 40 ° C to make Fe 3+ with PO 4 3- combine and settle down;

[0046] S4. After the ir...

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Abstract

The invention discloses a preparation method of battery-grade iron phosphate. The preparation method comprises the following steps: preparing a ferrous sulfate solution of which the mass percent of iron is 5.0-10.0%, adding an oxidizing agent and H3PO4 for oxidizing Fe <2+> into Fe <3+> to form a mixed solution of phosphoric acid and ferric sulfate, adding water to adjust the pH value to 1.5-2.5,performing a reaction to obtain iron phosphate precipitate, and washing, filtering, and drying and calcining a filter cake to obtain battery-grade iron phosphate. According to the invention, reactionpH is adjusted through pure water dilution; instead of adjusting the pH by ammonia water in a conventional route the product quality can be ensured and implementation of zero emission of ammonia nitrogen is achieved; no solid by-product is generated, the prepared battery-grade iron phosphate material is low in impurity content, dilute sulfuric acid in wastewater can be recycled through concentration, condensate water generated by heating evaporation can also be recycled for diluting and adjusting the pH value of a phosphoric acid and ferric sulfate mixed solution, zero emission of wastewater is achieved, and energy consumption and production cost are reduced.

Description

technical field [0001] The invention relates to the technical field of iron phosphate production, in particular to a method for preparing battery-grade iron phosphate. Background technique [0002] The synthesis process routes of lithium iron phosphate, the cathode material of lithium ion batteries, include hydrothermal process, ferrous oxalate process, iron red process, and iron phosphate process. The iron phosphate process has gradually become the mainstream route for lithium iron phosphate production due to its good batch stability and excellent electrochemical performance. Battery-grade iron phosphate usually adopts the following two production processes: 1. Using ferric salts such as iron sulfate Fe 2 (SO 4 ) 3 , Fe(NO 3 ) 3 , ferric chloride (FeCl 3 ) is the iron source, and H 3 PO 4 or NH 4 h 2 PO 4 Mix according to a certain ratio, then add ammonia water to adjust temperature and pH value, so that Fe 3+ with PO 4 3- Combined and precipitated, press filt...

Claims

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Application Information

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IPC IPC(8): C01B25/37C01B17/88C02F1/04C02F103/34
CPCC01B17/88C01B25/375C02F1/04C02F2103/34
Inventor 张军钟乔温益凡
Owner RUYUAN DONGYANGGUANG MAGNETIC MATERIAL
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