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Method for synthesizing iron phosphate by using titanium dioxide by-product ferrous sulfate

A technology of ferrous sulfate and ferrous sulfate solution, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problem of large amount of wastewater generation, and achieve the effect of reducing the amount of wastewater generated and the number of washings

Active Publication Date: 2022-01-25
ZIJIN MINING GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Battery Grade Iron Phosphate to Na + Ion content has strict requirements, while Na + , NH 4 + Ions will also affect the appearance quality of ferric phosphate, so the existing ferric phosphate synthesis process involves multiple washings, a large amount of washing water is required for product desalination, and a large amount of waste water is generated

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  • Method for synthesizing iron phosphate by using titanium dioxide by-product ferrous sulfate

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Experimental program
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Embodiment 1

[0020] This embodiment provides a method for utilizing titanium dioxide by-product ferrous sulfate to synthesize ferric phosphate, such as figure 1 As shown, the specific steps include:

[0021] (1) Prepare a 300 g / L ferrous sulfate solution with titanium dioxide by-product ferrous sulfate, add iron powder to reduce ferric iron, and stir for 0.5 h. Then heat the solution to 30°C, add ferrous hydroxide to adjust the pH to 3.0, and perform hydrolysis to remove titanium. After the reaction, the solid-liquid separation is obtained to obtain the titanium-removed liquid;

[0022] (2) Add phosphoric acid and hydrogen peroxide to the titanium-removing solution obtained in step (1) to oxidize and synthesize ferric phosphate, and use ferrous hydroxide to control the reaction pH to 1.4. After the reaction, the slurry undergoes solid-liquid separation, washing, drying and dehydration to obtain the iron phosphate product;

[0023] Further, the ferrous hydroxide used is prepared by react...

Embodiment 2

[0025] This embodiment provides a method for utilizing titanium dioxide by-product ferrous sulfate to synthesize ferric phosphate, such as figure 1 As shown, the specific steps include:

[0026] (1) Prepare a 500 g / L ferrous sulfate solution with titanium dioxide by-product ferrous sulfate, add iron powder to reduce ferric iron, and stir for 1 hour. Then heat the solution to 60°C, add ferrous hydroxide to adjust the pH to 4.5, and perform hydrolysis to remove titanium. After the reaction, the solid-liquid separation is obtained to obtain the titanium-removed liquid;

[0027] (2) Add phosphoric acid and hydrogen peroxide to the titanium-removing solution obtained in step (1) to oxidize and synthesize ferric phosphate, and use ferrous hydroxide to control the reaction pH to 1.6. After the reaction, the slurry undergoes solid-liquid separation, washing, drying and dehydration to obtain the iron phosphate product;

[0028] It should be noted that the ferrous hydroxide used is p...

Embodiment 3

[0030] This embodiment provides a method for utilizing titanium dioxide by-product ferrous sulfate to synthesize ferric phosphate, such as figure 1 As shown, the specific steps include:

[0031] (1) Prepare a 700 g / L ferrous sulfate solution with titanium dioxide by-product ferrous sulfate, add iron powder to reduce ferric iron, and stir for 2 hours. Then heat the solution to 70°C, add ferrous hydroxide to adjust the pH to 5.5, and perform hydrolysis to remove titanium. After the reaction, the solid-liquid separation is obtained to obtain the titanium-removed liquid;

[0032] (2) Add phosphoric acid and hydrogen peroxide to the obtained titanium removal solution in step (1) to oxidize and synthesize ferric phosphate, and use ferrous hydroxide to control the reaction pH to 2.0. After the reaction, the slurry undergoes solid-liquid separation, washing, drying and dehydration to obtain the iron phosphate product;

[0033] It should be noted that the ferrous hydroxide used is o...

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Abstract

The invention discloses a method for synthesizing iron phosphate by using titanium dioxide by-product ferrous sulfate, which comprises the following specific steps of: S1, prepare a ferrous sulfate solution from titanium dioxide by-product ferrous sulfate, adding iron powder to reduce ferric iron, and stirring to react; heating the solution, adding ferrous hydroxide to adjust the pH value, and hydrolyzing to remove titanium; and after the reaction is finished, carrying out solid-liquid separation to obtain titanium-removed liquid; and S2, adding phosphoric acid and hydrogen peroxide into the titanium-removed liquid obtained in the step S1 for oxidation synthesis of iron phosphate, and controlling the reaction pH to 1.4-2.0 through ferrous hydroxide; and after the reaction is finished, carrying out solid-liquid separation, washing, drying and dehydration on slurry to to obtain an iron phosphate product. According to the method, Na < + > or NH4 < + > ions can be prevented from being introduced into an iron phosphate synthesis system, the washing frequency of the iron phosphate product can be reduced, and less wastewater is generated.

Description

technical field [0001] The invention relates to the technical field of positive electrode materials for lithium ion batteries, in particular to a method for synthesizing ferric phosphate by using ferrous sulfate, a by-product of titanium dioxide. Background technique [0002] Lithium iron phosphate (LiFePO 4 ) batteries have the core advantages of good safety performance, long cycle life, and low raw material prices. At the same time, after the CTP technology of Ningde era and BYD blade battery technology solved the problem of low energy density, lithium iron phosphate batteries have been used as power batteries in many vehicles. enterprise's favor. In addition to being used as a power battery, lithium iron phosphate batteries also have bright and broad application prospects in the field of energy storage. [0003] The industrial production technologies of lithium iron phosphate cathode materials mainly include solid-phase method and liquid-phase method, among which the so...

Claims

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Application Information

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IPC IPC(8): C01B25/37
CPCC01B25/375Y02E60/10
Inventor 唐定季常青朱莞烨沈青峰庄荣传王乾坤池荷婷廖祥辉
Owner ZIJIN MINING GROUP