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Complete cycle preparation method of lithium iron phosphate by using lithium ores as lithium source

A technology of lithium iron phosphate, cycle preparation, applied in chemical instruments and methods, phosphorus compounds, lithium compounds, etc., can solve the problem of high production cost

Active Publication Date: 2012-01-11
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

And, all adopt limestone (CaCO 3 ) to adjust the pH value, so that a large amount of Ca is produced in the neutralized slurry 2+ Plasma, and partly generated Li 2 CO 3 Precipitation and loss of part of Li +
In addition, a large amount of condensed water and other by-products are not comprehensively utilized in the process of evaporation and concentration, resulting in high production costs

Method used

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  • Complete cycle preparation method of lithium iron phosphate by using lithium ores as lithium source
  • Complete cycle preparation method of lithium iron phosphate by using lithium ores as lithium source
  • Complete cycle preparation method of lithium iron phosphate by using lithium ores as lithium source

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0131] Example 1 Preparation of lithium iron phosphate

[0132] (1) Weigh 50kg of spodumene, calcinate at 1100°C for 50 minutes, cool, grind finely, add 7.1kg of sulfuric acid (acid to material ratio 1:7) for 50 minutes, and add sulfuric acid to lithium Pour pyroxene powder into 114kg (liquid-solid ratio 2:1) water, adjust the pH value to 5.7 with NaOH, stir for 35 minutes, let stand, and filter to obtain mother liquor 1;

[0133] (2) Adjust the pH value of mother liquor 1 to 8.5 with NaOH, stir and react for 5 minutes, stand still, 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 in the mother liquor 3 2 CO 3 , stirring and reacting for 30 minutes, standing still, and filtering to obtain mother liquor 4;

[0134] (3) Evaporate and concentrate the mother liquor 4 until its lithium content is 65g / L, leave it still, filter to obt...

Embodiment 2

[0147] Example 2 Preparation of lithium iron phosphate

[0148] (1) Weigh 50 kg of lithium phosphate aluminum, calcined at 1380 ° C for 300 minutes, cooled, ground, added 12.5 kg of sulfuric acid (according to the ratio of acid to material 1:4) for 200 minutes, under stirring conditions, will add acid The spodumene powder was poured into 187.5kg of reclaimed filtrate (liquid-solid ratio 3: 1), and the pH value was adjusted to 6.2 with NaOH, stirred for 50 minutes, left standstill, and filtered to obtain mother liquor 1;

[0149] (2) Adjust the pH value of mother liquor 1 to 9.7 with NaOH, stir and react for 12 minutes, stand still, 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 in the mother liquor 3 2 CO 3 , stirred and reacted for 10 minutes, allowed to stand, and filtered to obtain mother liquor 4;

[0150] (3) Evaporate and ...

Embodiment 3-9

[0159] Example 3-9 Preparation of lithium iron phosphate

[0160] 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. Simultaneously, the said lithium ore is first made into corresponding lithium salt according to the sulfuric acid method, then adding deionized water to make a lithium solution with a concentration of 25-27g / L, and the rest of the steps for preparing lithium ferrous phosphate are the same as implementing (6)~(10) of example 1, but do not recycle the preparation method of recovering filtrate and condensed water " as comparative example, and comparative example is compared with the production cost of the lithium ferrous phosphate that embodiment 3-9 prepares , the results are shown in Table 2.

[0161] Preparation raw materials and process parameters of table 2 embodiment 3-9

[0162]

[0163] As can be seen from Table 2, according to the detection met...

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Abstract

The invention relates to a complete cycle preparation method of lithium iron phosphate by using lithium ores as a lithium source, comprising the following steps: carrying out calcining, acidifying, leaching, purifying and separating on the lithium ores to obtain a primary lithium liquid, carrying out conversion and refrigeration, filtering and washing, evaporative concentration on the primary lithium liquid to obtain a lithium liquid for synthesis, letting the lithium liquid for synthesis, a ferrite solution, and a phosphor source solution be subject to liquid phase synthesis, and calcining to obtain the carbon coated lithium iron phosphate. According to the invention, cooling crystallization, separation, drying and other steps in the preparation of lithium iron phosphate with lithium ores are left out, and the byproducts obtained by evaporative concentration, filtering and separating are recycled, so that the utilization rate of resource is increased, and the cost is saved; and the prepared lithium iron phosphate has the characteristics of high purity, excellent electrochemical performance and the like, so that the circular economy is realized.

Description

technical field [0001] The invention belongs to the field of lithium ion battery materials, and in particular relates to a complete cycle 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 ferro...

Claims

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Application Information

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IPC IPC(8): C01B25/45H01M4/58
CPCC01D15/00H01M4/58C22B3/44C01P2006/40H01M4/5825C01G49/009C01B25/45C22B26/12C22B3/22Y02E60/12Y02E60/10Y02P10/20
Inventor 王平黄春莲金鹏高宜宝
Owner 天齐锂业(射洪)有限公司
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