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Preparation method for ultrafine impurity-doped ferrous oxalate special for lithium iron phosphate

A technology of lithium ferrous phosphate and ferrous oxalate is applied in the preparation of carboxylate, the preparation of carboxylate, the preparation of organic compounds, etc., which can solve the problem that the doping element is difficult to solidify, and achieves a simple preparation process, The effect of improving electrical conductivity and high-rate discharge performance

Active Publication Date: 2014-02-26
NINGBO SHENGTENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Most of the current doping methods are to dope the lithium iron phosphate material itself, or do solid-phase mixed doping during its preparation process, and it is difficult for the introduced doping elements to enter the crystal uniformly to form a solid solution

Method used

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  • Preparation method for ultrafine impurity-doped ferrous oxalate special for lithium iron phosphate
  • Preparation method for ultrafine impurity-doped ferrous oxalate special for lithium iron phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Dissolve 170g of titanium dioxide by-product ferrous sulfate solid with a Fe content of 16.5% in tap water at a liquid-solid mass ratio of 1.5:1, stir, heat up to 90°C, and add ferrous sulfate with an average particle size of less than 74 μm and an iron content of more than 98%. Reduce the iron powder, keep the reaction pH at 4.5, and the reaction time is 10 hours. After the impurity removal reaction is completed, filter to obtain a pure ferrous sulfate solution.

[0021] 0.01molMgSO 4 .7H 2 O is added in the pure ferrous sulfate solution, then ammoniacal liquor is joined in the ferrous sulfate solution, and the ammoniacal liquor addition is 100% of theoretical amount, and feed time is 50 minutes, and 60 ℃ of reaction temperatures, promptly generate ferrous hydroxide precipitation at this moment, Heat preservation reaction for 0.5 hours. Make 68g of oxalic acid with a content of 99% into 200ml solution with tap water, drop it into the ferrous hydroxide suspension, the...

Embodiment 2

[0023] Dissolve 170g of titanium dioxide by-product ferrous sulfate solid with a Fe content of 16.5% in tap water at a ratio of liquid to solid mass ratio of 2.5:1, stir, heat up to 85°C, and add ferrous sulfate with an average particle size of less than 74 μm and an iron content of more than 98%. Reduce the iron powder, keep the reaction pH at 4.0, and the reaction time is 8 hours. After the impurity removal reaction is completed, filter to obtain a pure ferrous sulfate solution.

[0024] 0.003molCo(NO 3 ) 2 .6H 2 O is added in the pure ferrous sulfate solution, then ammoniacal liquor is joined in the ferrous sulfate solution, the ammoniacal liquor addition is 105% of theoretical amount, 10 minutes of feeding time, 50 ℃ of reaction temperature, promptly generate ferrous hydroxide precipitation at this moment, Heat preservation reaction for 0.5 hours. Make 68g of oxalic acid with a content of 99% into 200ml solution with tap water, drop it into the ferrous hydroxide suspens...

Embodiment 3

[0026] Dissolve 170g of titanium dioxide by-product ferrous sulfate solid with a Fe content of 16.5% in tap water at a liquid-to-solid mass ratio of 3.0:1, stir, heat up to 95°C, and add ferrous sulfate with an average particle size of less than 74 μm and an iron content greater than 98%. Reduce the iron powder, keep the reaction pH at 4.0, and the reaction time is 5 hours. After the impurity removal reaction is completed, filter to obtain a pure ferrous sulfate solution.

[0027] 0.001molCo(NO 3 ) 2 .6H 2 O and 0.007molMgCl 2 .6H 2 O is added in the pure ferrous sulfate solution, then ammoniacal liquor is joined in the ferrous sulfate solution, and the ammoniacal liquor addition is 105% of theoretical amount, and feed time is 30 minutes, and 90 ℃ of reaction temperatures, promptly generate ferrous hydroxide precipitation at this moment, Heat preservation reaction for 0.5 hours. Make 68g of oxalic acid with a content of 99% into 200ml solution with tap water, drop it into...

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Abstract

A disclosed preparation method for ultrafine impurity-doped ferrous oxalate special for lithium iron phosphate comprises: solving titanium dioxide by-product ferrous sulphate solid, stirring, heating, adding reduced iron powder to remove heavy metal impurity and ferric iron, and filtering to obtain a pure ferrous sulphate solution; adding a compound containing to-be doped ions into the pure ferrous sulphate solution with stirring, then adding ammonia ater into the ferrous sulphate solution to generate ferrous hydroxide precipitate; and dropwise adding oxalic acid aqueous solution into the ferrous hydroxide suspension to convert ferrous hydroxide into ferrous oxalate and enable the to-be doped ions to generate corresponding oxalate precipitate and form oxalate mixed crystal, adjusting pH value of the reaction material, after the reaction is finished, and performing solid-liquid separation, water washing and drying to obtain the impurity-doped ferrous oxalate product. The method is simple in technology and is accord with the policy of national circular economy; and the prepared ultrafine impurity-doped ferrous oxalate has a particle size of 3.0 mu m-5.0 mu and purity more than 99%.

Description

technical field [0001] The invention relates to the field of power lithium battery raw materials, in particular, the invention relates to a preparation method of ferrous oxalate special for lithium iron phosphate. Background technique [0002] Lithium-ion battery, as a kind of green battery, is not only widely used in various portable electronic products and communication tools, but also the preferred supporting power source for electric vehicles and space power sources that are vigorously researched by various countries. Its role in power vehicles and energy storage power stations The application will alleviate the crisis of the depletion of global oil resources to a certain extent. Advanced battery materials, especially cathode materials, are one of the key technologies of lithium-ion batteries. Lithium iron phosphate has been widely recognized and focused on research by researchers due to its good safety performance and high-rate discharge performance. However, the lithi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/07C07C51/41
CPCC07C51/412C07C55/07
Inventor 张玉广李博
Owner NINGBO SHENGTENG NEW MATERIALS
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