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Method for producing lithium ferrous phosphate by using lithium mine as lithium source

A technology of lithium iron phosphate and lithium ore, which is applied in the field of preparation of lithium iron phosphate, can solve the problems of high cost of lithium iron phosphate, and achieve the effects of realizing circular economy, reducing production costs, and low energy consumption

Active Publication Date: 2012-01-25
天齐锂业(射洪)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cost of obtaining lithium iron phosphate with a 1C discharge capacity of more than 140mAh / g is obviously very high

Method used

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  • Method for producing lithium ferrous phosphate by using lithium mine as lithium source
  • Method for producing lithium ferrous phosphate by using lithium mine as lithium source
  • Method for producing lithium ferrous phosphate by using lithium mine as lithium source

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0097] Example 1 Preparation of lithium iron phosphate

[0098] (1) Weigh 50kg of spodumene, calcinate at 1100°C for 50 minutes, cool, grind, add 7.1kg of sulfuric acid (acid to material ratio 1:7) for 50 minutes, pour 114kg (liquid-solid ratio 2 : 1) In water, adjust the pH value to 5.7 with NaOH, stir for 35 minutes, let stand, and filter to obtain mother liquor 1;

[0099] (2) Adjust the pH value of mother liquor 1 to 8.5 with NaOH, stir and react for 5 minutes, let stand, filter to obtain mother liquor 2, then adjust the pH value of mother liquor 2 to 10.8 with NaOH, stir and react for 5 minutes, stand still, filter to obtain mother liquor 3; add 236.6 grams of Na 2 CO 3 , stirring and reacting for 30 minutes, standing still, and filtering to obtain mother liquor 4;

[0100] (3) Evaporate and concentrate the mother liquor 4 until its lithium content is 65g / L, leave it still, filter to obtain the mother liquor 5, wherein the condensed water obtained by evaporation and ...

Embodiment 2

[0112] The preparation of embodiment 2 lithium ferrous phosphate

[0113] (1) Weigh 50kg of lithium phosphate aluminum, calcined at 1380°C for 300 minutes, cooled, ground, added 12.5kg of sulfuric acid (according to the ratio of acid to material 1:4) for 200 minutes, poured into 187.5kg of recovery filtrate while stirring Medium (liquid-solid ratio 3:1), adjust the pH value to 6.2 with NaOH, stir for 50 minutes, let stand, and filter to obtain mother liquor 1;

[0114] (2) Adjust the pH value of mother liquor 1 to 9.7 with NaOH, stir and react for 12 minutes, let stand, filter to obtain mother liquor 2, then adjust the pH value of mother liquor 2 to 10 with NaOH, stir and react for 12 minutes, stand still, filter to obtain mother liquor 3; add 240.5 grams of Na 2 CO 3 , stirred and reacted for 10 minutes, allowed to stand, and filtered to obtain mother liquor 4;

[0115] (3) Evaporate and concentrate the mother liquor 4 until its lithium content is 75g / L, leave it still, fi...

Embodiment 3-9

[0124] The preparation of embodiment 3-9 lithium ferrous phosphate

[0125] The preparation process of Examples 3-9 is the same as that of Example 1, and the required preparation materials and process parameters are shown in Table 2.

[0126] Preparation raw materials and process parameters of table 2 embodiment 3-9

[0127]

[0128] As can be seen from Table 2, according to the assay method of the present invention, the purity of Lithium Ferrous Phosphate is not less than 99.97%, and Ca in Lithium Ferrous Phosphate 2+ , Mg 2+ , SO4 2- , Cl - 、Na + 、K + 、Cu 2+ , Pb 2+ The content of any one is not higher than 0.01%, and the 1C specific capacity is more than 140mAh / g. It can be seen that the lithium ferrous phosphate prepared by the process of the present invention has the advantages of high purity, excellent electrochemical performance, good stability and consistency.

[0129] Moreover, the process of the present invention can control the concentration of lithium io...

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Abstract

The invention relates to a method for producing lithium ferrous phosphate by using a lithium mine as a lithium source and belongs to the field of materials of lithium ion batteries. The invention adopts the technical scheme that: the method comprises the following steps of: (1) treating the lithium mine, and thus obtaining a lithium source solution; (2) performing liquid phase reaction on a ferrite solution, a phosphorus source solution and the lithium source solution which is prepared in the step (1), cooling, filtering and then collecting filter cakes; and (3) washing the filter cakes, adding water into the filter cakes to form slurry, adding a sugar raw material, uniformly mixing, drying, then calcining under the protection of inert gas, and thus obtaining carbon-coated lithium ferrousphosphate. By adoption of the method for producing the lithium ferrous phosphate by using the lithium mine as the lithium source, the content of impurities such as calcium ion (Ca<2+>) and magnesium ion (Mg<2+>) in the lithium ferrous phosphate is well reduced and controlled; the prepared lithium ferrous phosphate has the advantages of high purity, high electrochemical performance, high stability, high consistency and the like; 1C discharge capacity can be over 140 mAh / g; and the comprehensive cost of the lithium ferrous phosphate can be saved by over 12,000 yuan per ton.

Description

technical field [0001] The invention belongs to the field of lithium ion battery materials, and in particular relates to a preparation method for producing lithium ferrous phosphate by using lithium ore as a lithium source. Background technique [0002] Since the discovery of metal lithium phosphate by the Goodenough research group in 1994, and the first report by A.K.Padhi in 1997 that olivine-type lithium iron phosphate has the function of delithiation and intercalation of lithium, lithium iron phosphate has high specific capacity, long cycle life, safety, and source of raw materials. The advantages of abundance, cheapness, and environmental friendliness have been widely studied and become ideal cathode materials for the production of lithium-ion batteries. In recent years, with the strong support of the governments of various countries, the commercial application of lithium iron phosphate power batteries has been increasing. [0003] Existing lithium ferrous phosphate pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCY02E60/12H01M4/5825H01M4/58Y02E60/10
Inventor 王平黄春莲金鹏陈欣
Owner 天齐锂业(射洪)有限公司
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