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A method for preparing battery-grade iron phosphate with low impurity, high iron-phosphorus ratio and large specific surface area

A large specific surface area, iron phosphate technology, applied in nanotechnology, chemical instruments and methods, phosphorus compounds, etc. for materials and surface science, can solve problems such as unfavorable processing

Active Publication Date: 2019-09-03
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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  • A method for preparing battery-grade iron phosphate with low impurity, high iron-phosphorus ratio and large specific surface area
  • A method for preparing battery-grade iron phosphate with low impurity, high iron-phosphorus ratio and large specific surface area
  • A method for preparing battery-grade iron phosphate with low impurity, high iron-phosphorus ratio and large specific surface area

Examples

Experimental program
Comparison scheme
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 iron powder with 0.5% ferrous mass, raise the temperature to 60°C, keep it warm for 3 hours, and purify and remove Ti, Cu, and Al , Zn and other impurity ions, take the supernatant after standing, and filter to obtain the purified ferrous sulfate solution.

[0046] Inject 1000L pure water into 10m 3 The reaction kettle is used as the bottom liquid, and the temperature is raised to 30°C. Under stirring, the iron ion concentration is 60g / L ferrous sulfate solution, 120g / L diammonium hydrogen phosphate solution and 20% hydrogen peroxide are added into the reaction kettle at the same time for precipitation reaction. The flow rate of ferrous sulfate solution is 2000L / h, the flow rate of 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 re...

Embodiment 2

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

[0053] Inject 1000L pure water into 10m 3 The reaction kettle 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 added to the reaction kettle at the same time to cause precipitation reaction. The flow rate of ferrous sulfate solution is 1000L / h, the flow rate of 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 2 hours of reaction...

Embodiment 3

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

[0060] Inject 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 added to the reaction kettle at the same time for precipitation reaction. The flow rate of iron solution is 1600L / h, the flow rate of diammonium hydrogen phosphate solution is 2800L / h, the flow rate of hydrogen peroxide is 510L / h, the synthetic pH value is 3, and the feeding is stopped after 1.5h of reaction. Stirring was continued for 30 ...

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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 method for preparing ferric phosphate, in particular to a method for preparing ferric phosphate with low impurity, high iron-phosphorus ratio and large specific surface area for lithium iron phosphate power batteries, which removes 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-toxic, non-polluting, and wide source of raw materials. Lithium iron phosphate batteries are used in electric tools: electric drills, chainsaws, 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, and are used in electric buses; another major power source field is energy stora...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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