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Method for preparing iron phosphate by recycling mother liquor

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

Active Publication Date: 2021-08-27
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
Comparison scheme
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 ammonium sulfate mother liquor, stir at 45°C for 60 minutes, and filter to obtain ammonium dihydrogen phosphate solution; the molar ratio of calcium hydrogen phosphate, sulfuric acid, and ammonium sulfate added is 2: 1.05: 1.

[0034] 2. Add hydrogen peroxide to the ammonium dihydrogen phosphate solution, the mol ratio of the consumption of hydrogen peroxide to ferrous sulfate in ferrous sulfate is 0.3:1, mix to obtain filtrate B;

[0035] 3. The filtrate B is mixed with ammonia water to obtain a solution C of pH=2.0, and the solution C is added to the reactor together with the purified ferrous sulfate solution (80g / L) to synthesize and prepare ferric phosphate, according to the method of ammonium dihydrogen phosphate and The molar ratio of ferrous sulfate is 1:1...

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

[0043] 2. Add hydrogen peroxide in the ammonium dihydrogen phosphate solution, the mol ratio of the consumption of hydrogen peroxide and the ferrous iron in ferrous sulfate is 0.5: 1, mix to obtain filtrate B;

[0044] 3. The filtrate B is mixed with ammonia water to obtain a solution C of pH=7.0, and the solution C is added to the reaction kettle together with the purified ferrous sulfate solution (120g / L), and ferric phosphate is synthesized according to ammonium dihydrogen phosphate and ammonium dihydrogen phosphate. The molar ratio of f...

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 ammonium sulfate mother liquor, stir at 65°C for 45 minutes, and filter to obtain ammonium dihydrogen phosphate solution; the molar ratio of calcium hydrogen phosphate, sulfuric acid, and ammonium sulfate added is 2: 1:1.

[0052] 2. Add hydrogen peroxide in the ammonium dihydrogen phosphate solution, the mol ratio of the consumption of hydrogen peroxide and the ferrous iron in ferrous sulfate is 0.4: 1, mix to obtain filtrate B;

[0053]3. The filtrate B is mixed with ammonia water to obtain a solution C of pH=5.0, and the solution C is added to the reaction kettle together with the purified ferrous sulfate solution (100g / L), and ferric phosphate is synthesized according to ammonium dihydrogen phosphate and ammonium dihydrogen phosphate The molar ratio of ferrou...

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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, which comprises the following steps: mixing calcium hydrophosphate, sulfuric acid and ammonium sulfate mother liquor, stirring for reaction, and filtering to obtain an ammonium dihydrogen phosphate solution; adding hydrogen peroxide into the ammonium dihydrogen phosphate solution, and mixing to obtain filtrate B; mixing the filtrate B with ammonia water 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 ammonium sulfate mother liquor; and crushing and drying the filter cake F, carrying out rotary drying, sieving and demagnetizing to obtain the anhydrous iron phosphate. The raw materials of the method are cheap and easy to obtain, 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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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
CPCC01B25/375C01P2004/03Y02E60/10
Inventor 周大桥李紫金张悦杨德威
Owner 河南佰利新能源材料有限公司
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