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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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 consu

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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Example Embodiment

[0031] Example 1

[0032] like figure 1 As shown, a method of preparing a phosphate was prepared by a mother liquor rewind, the method comprising the steps of:

[0033] 1. Mix the hydrogen phosphate, sulfate, sodium sulfate, stirred at 45 ° C, stirred for 60 min, filtered to obtain a sodium hydrogen phosphate solution; wherein the ratio of hydrogen phosphate, sulfate, sulfate, sodium sulfate is 2: 2: 1.05.1.

[0034] 2, sodium hydroxide is added to the sodium phosphate solution until the solution pH = 2.0, then filtered to give the filtrate B;

[0035] 3, mixing the filtrate B and the hydrogen peroxide, the amount of the hydrogen peroxide and the ferrous sulfate solution of ferrous sulfate is 0.4: 1, and after mixing, add the reactor with the purified sulfate solution (80 g / L). The synthesis was prepared, and the two solutions were slowly added, and the two solutions were slowly added in accordance with the molar ratio of ferric sodium dihydrogen phosphate and ferrous sulfate, a...

Example Embodiment

[0040] Example 2

[0041] like figure 1 As shown, a method of preparing a phosphate was prepared by a mother liquor rewind, the method comprising the steps of:

[0042] 1, mixed with hydrogen phosphate, sulfuric acid, sulfate, stirred at 98 ° C, stirred for 30 min, filtered to give a sodium hydrogen phosphate solution; wherein the ratio of hydrogen phosphate, sulfate, sulfate, sulfate is 2.05.05. 1: 1.

[0043] 2, sodium hydroxide is added to the dihydrogenate solution of the phosphate until the solution pH = 7.0, and then filtered to give the filtrate B;

[0044] 3, mixing the filtrate B and the hydrogen peroxide, the amount of the hydrogen peroxide is 0.5.5.5.5.5.5.5.5.5.5.5.5. After mixing, add the ferrous sulfate solution (120 g / L) after purification, synthesis Iron iron was prepared, and the two solutions were slowly added according to the molar ratio of sodium dihydrogen phosphate and ferrous sulfate, and the reaction kettle temperature was 60 ° C and stirred. After the re...

Example Embodiment

[0049] Example 3

[0050] like figure 1 As shown, a method of preparing a phosphate was prepared by a mother liquor rewind, the method comprising the steps of:

[0051] 1. Mix the hydrogen phosphate, sulfate, sodium sulfate, at 60 ° C, stirred for 50 min, filtered to obtain a sodium phosphate solution; wherein the ratio of hydrogen phosphate, sulfate, sodium sulfate is 1 is 2: 2: 1: 1.

[0052] 2. Sodium hydroxide is added to the sodium hydrogen sodium phosphate solution until the solution pH = 4.0, then filtered to give the filtrate B;

[0053]3, mixing the filtrate B and the hydrogen peroxide, the amount of the hydrogen peroxide is 0.5.5% of the ferrous sulfate solution, and after mixing, add the reactor with a ferrous sulfate solution (80 g / L) after purification. The synthesis was prepared, and the two solutions were slowly added in accordance with the molar ratio of sodium dihydrogen sodium dihydrogen phosphate and ferrous sulfate, and the reaction kettle temperature was sti...

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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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