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Method for preparing iron phosphate by recycling mother liquor

A technology of iron phosphate and mother liquor, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of incapable of comprehensive utilization of resources, high cost of wastewater treatment, unfavorable energy saving and cost reduction, etc. The effect of utilization, good appearance, and cost reduction of wastewater treatment

Active Publication Date: 2021-09-03
河南佰利新能源材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the production of wet-process iron phosphate will produce a large amount of high-salt wastewater, not only the cost of wastewater treatment is high, but also the consumption of a large amount of water resources, which is not conducive to energy saving and cost reduction, and does not reflect the value of comprehensive utilization of resources

Method used

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  • Method for preparing iron phosphate by recycling mother liquor
  • Method for preparing iron phosphate by recycling mother liquor
  • Method for preparing iron phosphate by recycling mother liquor

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Such as figure 1 Shown, a kind of mother liquor reuses the method for preparing ferric phosphate, and this method may further comprise the steps:

[0033] 1. Mix calcium hydrogen phosphate, sulfuric acid, and sodium sulfate mother liquor, stir at 45°C for 60 minutes, and filter to obtain sodium dihydrogen phosphate solution; the molar ratio of calcium hydrogen phosphate, sulfuric acid, and sodium sulfate added is 2: 1.05: 1.

[0034] 2. Add sodium hydroxide to the sodium dihydrogen phosphate solution until the solution pH=2.0, and then filter to obtain filtrate B;

[0035] 3, the filtrate B is mixed with hydrogen peroxide, the consumption of hydrogen peroxide is 0.4: 1 with the mol ratio of ferrous sulfate in the ferrous sulfate solution, after mixing, add the reaction kettle together with the ferrous sulfate solution (80g / L) after the purification, To synthesize and prepare ferric phosphate, slowly add the two solutions according to the molar ratio of sodium dihydrog...

Embodiment 2

[0041] Such as figure 1 Shown, a kind of mother liquor reuses the method for preparing ferric phosphate, and this method may further comprise the steps:

[0042] 1. Mix calcium hydrogen phosphate, sulfuric acid, and sodium sulfate mother liquor, stir at 98°C for 30 minutes, and filter to obtain sodium dihydrogen phosphate solution; the molar ratio of calcium hydrogen phosphate, sulfuric acid, and sodium sulfate added is 2.05: 1:1.

[0043] 2. Add sodium hydroxide to the sodium dihydrogen phosphate solution until the solution pH=7.0, and then filter to obtain filtrate B;

[0044] 3. The filtrate B is mixed with hydrogen peroxide, the molar ratio of the amount of hydrogen peroxide to ferrous sulfate in the ferrous sulfate solution is 0.5:1, after mixing, add the purified ferrous sulfate solution (120g / L) to the reactor, and synthesize To prepare ferric phosphate, slowly add the two solutions according to the molar ratio of sodium dihydrogen phosphate and ferrous sulfate at a r...

Embodiment 3

[0050] Such as figure 1 Shown, a kind of mother liquor reuses the method for preparing ferric phosphate, and this method may further comprise the steps:

[0051] 1. Mix calcium hydrogen phosphate, sulfuric acid, and sodium sulfate mother liquor, stir at 60°C for 50 minutes, and filter to obtain sodium dihydrogen phosphate solution; the molar ratio of calcium hydrogen phosphate, sulfuric acid, and sodium sulfate added is 2: 1:1.

[0052] 2. Add sodium hydroxide to the sodium dihydrogen phosphate solution until the solution pH=4.0, and then filter to obtain filtrate B;

[0053]3. The filtrate B is mixed with hydrogen peroxide, the mol ratio of the consumption of hydrogen peroxide and ferrous sulfate in the ferrous sulfate solution is 0.5: 1, after mixing, add the reactor together with the purified ferrous sulfate solution (80g / L), To synthesize and prepare ferric phosphate, slowly add the two solutions according to the molar ratio of sodium dihydrogen phosphate and ferrous sul...

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Abstract

The invention belongs to the technical field of lithium ion battery positive electrode materials, and particularly discloses a method for preparing iron phosphate by recycling mother liquor. The method comprises the steps of mixing calcium hydrophosphate, sulfuric acid and sodium sulfate mother liquor, stirring for reaction, and filtering to obtain a sodium dihydrogen phosphate solution; adding sodium hydroxide into the sodium dihydrogen phosphate solution, and stirring to obtain filtrate B; mixing the filtrate B with hydrogen peroxide to obtain a solution C; adding the solution C and a ferrous sulfate solution into a reaction kettle, stirring for reaction, and heating for aging after reaction; filtering the slurry obtained in the previous step to obtain mother liquor D and a filter cake E; washing the filter cake E to obtain a filter cake F and filtrate G; performing membrane concentration on the filtrate G to obtain pure water and high-concentration wastewater H, recycling the pure water as washing water, and recycling the high-concentration wastewater H and the mother liquor D as sodium sulfate mother liquor; and enabling the filter cake F to be subjected to crushing drying, rotary drying, sieving and iron removal, and obtaining anhydrous iron phosphate. The raw materials of the method are cheap and easy to obtain, the mother liquor can be recycled, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of cathode materials for lithium ion batteries, and in particular relates to a method for preparing ferric phosphate by reusing mother liquor. Background technique [0002] Iron phosphate is the precursor of lithium iron phosphate, the cathode material of energy storage and power lithium ion batteries. With the rapid development of new energy vehicles, industrial and civil energy storage fields, the market demand for energy storage and power batteries is gradually increasing. Large, lithium iron phosphate battery has obvious market advantages such as its own safety, environmental protection, and low price, and the demand for iron phosphate is also increasing year by year. However, the production of wet-process ferric phosphate will produce a large amount of high-salt wastewater, which not only has high wastewater treatment costs, but also consumes a large amount of water resources, which is not conducive to ...

Claims

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Application Information

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IPC IPC(8): C01B25/37
CPCC01B25/375C01P2004/03C01P2004/32C01P2004/62C01P2004/61Y02E60/10
Inventor 周大桥张悦李紫金杨德威
Owner 河南佰利新能源材料有限公司
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