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Preparation method of battery grade iron phosphate with low impurity, high iron-phosphorus ratio and large specific surface

A ferric phosphate, low impurity technology, applied in chemical instruments and methods, nanotechnology for materials and surface science, phosphorus compounds, etc., can solve problems such as unfavorable processing

Active Publication Date: 2018-08-28
취저우화여우코발트뉴머터리얼컴퍼니리미티드 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The specific surface area of ​​anhydrous iron phosphate on the market is mostly 7-10m 2 / g, not conducive to subsequent processing

Method used

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  • Preparation method of battery grade iron phosphate with low impurity, high iron-phosphorus ratio and large specific surface
  • Preparation method of battery grade iron phosphate with low impurity, high iron-phosphorus ratio and large specific surface
  • Preparation method of battery grade iron phosphate with low impurity, high iron-phosphorus ratio and large specific surface

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Dissolve ferrous sulfate in pure water to prepare a ferrous sulfate solution with an iron ion concentration of 60g / L, add 0.5% ferrous iron powder, heat up to 60℃, keep it for 3h, and purify and remove Ti, Cu, Al Zn, Zn and other impurity ions, extract the supernatant after standing, and filter to obtain purified ferrous sulfate solution.

[0046] Pour 1000L pure water into 10m 3 The reactor is used as the bottom liquid, and the temperature is raised to 30°C. Under stirring, the iron ion concentration of 60g / L ferrous sulfate solution, 120g / L diammonium hydrogen phosphate solution and 20% hydrogen peroxide are simultaneously added to the reactor to cause precipitation reaction. The flow rate of the ferrous sulfate solution is 2000L / h, the flow rate of the diammonium hydrogen phosphate solution is 3200L / h, the flow rate of hydrogen peroxide is 400L / h, the synthetic pH value is 2, and the feeding is stopped after 1 hour of reaction. Stirring is continued for 30 minutes, and ...

Embodiment 2

[0052] Dissolve ferrous sulfate in pure water to prepare a ferrous sulfate solution with a ferrous ion concentration of 100g / L, add 1.2% ferrous iron powder, heat up to 80℃, keep it for 2h, and purify and remove Ti, Cu, Al Zn, Zn and other impurity ions, extract the supernatant after standing, and filter to obtain purified ferrous sulfate solution.

[0053] Pour 1000L pure water into 10m 3 The reactor is used as the bottom liquid, and the temperature is raised to 40°C. Under stirring, the iron ion concentration of 100g / L ferrous sulfate solution, 160g / L ammonium dihydrogen phosphate solution and 20% hydrogen peroxide are simultaneously added to the reactor to cause precipitation reaction. The flow rate of the ferrous sulfate solution is 1000L / h, the flow rate of the ammonium dihydrogen phosphate solution is 1400L / h, the flow rate of hydrogen peroxide is 430L / h, the synthetic pH value is 2.5, and the feeding is stopped after 2h of reaction. Stirring is continued for 30 minutes, an...

Embodiment 3

[0059] Dissolve ferrous sulfate in pure water to prepare a ferrous sulfate solution with an iron ion concentration of 120g / L, add 2% iron powder of ferrous mass, heat up to 99℃, keep for 1h, and purify and remove Ti, Cu, Al Zn, Zn and other impurity ions, extract the supernatant after standing, and filter to obtain purified ferrous sulfate solution.

[0060] Pour 1000L pure water into 10m 3 The reaction kettle is used as the bottom liquid, and the temperature is raised to 50°C. Under stirring, the concentration of 120g / L ferrous sulfate solution, 200g / L diammonium hydrogen phosphate solution and 20% hydrogen peroxide are simultaneously added to the reaction kettle to cause precipitation reaction. The iron solution flow rate is 1600L / h, the diammonium hydrogen phosphate solution flow rate is 2800L / h, the hydrogen peroxide flow rate is 510L / h, the synthetic pH value is 3, and the feeding is stopped after 1.5h of reaction. Stirring is continued for 30 minutes, and the crude iron pho...

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Abstract

The invention discloses a preparation method of a battery grade iron phosphate with low impurity, high iron-phosphorus ratio and large specific surface. The iron-phosphorus ratio in the current iron phosphate is 0.97 to 1.00, however a small amount of iron hydroxide is contained in the iron phosphate and absorbs a large amount of impurity ions, so that the contents of S, Mn and Mg impurity ions are high, and the requirement of battery grade iron phosphate is difficult to meet. The method comprises the following steps: firstly, preliminarily purification and impurity removal: removing titanium,copper and aluminum impurity metal ions at high temperature; secondly, deep purification and impurity removal: removing manganese and magnesium metal ion impurities at low temperature; thirdly, performing ageing to remove sulfate radical in crude iron phosphate, adding alkali to control the endpoint pH value to be 5.5 to 6.5, and removing acidic salt; fourthly, washing and drying; fifthly, performing low-temperature calcinations to remove crystal water. Iron phosphate obtained through the method has the advantages that the iron-phosphorus ratio reaches greater than 0.975, the contents of mainimpurity elements Mn, Mg and S are smaller than 30ppm, the contents of other elements are smaller than 10ppm, the specific surface is adjustable between 8 to 12m2 / g, and the total water content is smaller than 0.3 percent.

Description

Technical field [0001] The invention relates to a preparation method of iron phosphate, in particular to a preparation method of low-impurity, high-iron-phosphorus ratio and large surface iron phosphate for lithium iron phosphate power batteries for removing manganese and magnesium metal ion impurities in ferrous sulfate at low temperature. Background technique [0002] Lithium iron phosphate is a kind of cathode material for lithium-ion batteries. It is characterized by large discharge capacity, good safety, long life, low price, non-toxicity, non-polluting, and extensive sources of raw materials. Lithium iron phosphate batteries are used in power tools: electric drills, electric saws, lawn mowers, etc.; UPS and emergency lights, warning lights and miner's lamps. Lithium iron phosphate batteries are also an important development direction of power batteries for new energy vehicles, which are used in electric buses; the other main power source field is energy storage. The PO bon...

Claims

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Application Information

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IPC IPC(8): C01B25/37B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B25/375C01P2002/72C01P2004/03C01P2004/61C01P2004/64C01P2006/12C01P2006/80
Inventor 刘人生田礼平胡招文詹礼良殷建强吴建明
Owner 취저우화여우코발트뉴머터리얼컴퍼니리미티드
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