A kind of method that prepares manganese iron phosphate lithium by lithium iron phosphate

A technology of lithium iron manganese phosphate and lithium iron phosphate, applied in chemical instruments and methods, phosphorus compounds, structural parts, etc., can solve the problems of complex recovery process, large equipment investment, long process, etc., and achieve simple process flow and high purity. , the effect of low cost

Active Publication Date: 2020-09-08
GUANGDONG GUANGHUA SCI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The recovery process mentioned above is complicated, the process is long, and the investment in equipment is large. The use of different acid systems in the recovery process will inevitably introduce impurities and bring new by-products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Remove the residual power of the waste lithium iron phosphate battery, take out the positive electrode sheet of the battery, freeze it with liquid nitrogen, then shower the positive electrode sheet with 95°C hot water, and obtain lithium iron phosphate with the electrolyte and polyvinylidene fluoride removed after sieving solid;

[0032] (2) Take 2.9 kg of the lithium iron phosphate solid obtained in step (1), add 30 g of agar, 2.9 kg of manganese carbonate, and 0.7 kg of lithium carbonate, transfer the material into a ball mill, and grind it by ball milling at a speed of 400 rpm 3 hours, obtain 6.4 kilograms of mixed powders;

[0033] (3) Transfer the mixed powder into the feeding tank of the sand mill, add 18.5 kg of phosphoric acid solution with a mass concentration of 10%, so that the solid-liquid mass ratio is 1:2.9, and sand the material at a speed of 750 rpm , and the sanding time was 6 hours to obtain the slurry;

[0034] (4) Transfer the slurry to a spray...

Embodiment 2

[0038] (1) Remove the residual power of the waste lithium iron phosphate battery, take out the positive electrode sheet of the battery, freeze it with liquid nitrogen, then shower the positive electrode sheet with 95°C hot water, and obtain lithium iron phosphate with the electrolyte and polyvinylidene fluoride removed after sieving solid;

[0039] (2) Take 2.88 kg of lithium iron phosphate solid obtained in step (1), add 40 g of lignin, 2.9 kg of manganese carbonate, and 0.7 kg of lithium carbonate, transfer the material into a ball mill, and ball mill at a speed of 500 rpm Pulverized for 1 hour to obtain 6.4 kg of mixed powder;

[0040] (3) Transfer the mixed powder into the feeding tank of the sand mill, add 16 kg of phosphoric acid solution with a mass concentration of 12%, so that the solid-liquid weight ratio of the material is 1:2.5, and sand the material at a speed of 1500 rpm Grinding, sanding time 10 hours, obtain slurry;

[0041] (4) Transfer the slurry to a spray...

Embodiment 3

[0045] (1) Remove the residual power of the waste lithium iron phosphate battery, take out the positive electrode sheet of the battery, freeze it with liquid nitrogen, then shower the positive electrode sheet with 95°C hot water, and obtain the lithium iron phosphate solid with polyvinylidene fluoride removed after sieving;

[0046] (2) Take 2.93 kg of lithium iron phosphate solid obtained in step (1), add 30 g of sorbitol, 1.8 kg of manganese carbonate, and 0.7 kg of lithium carbonate, transfer the material into a ball mill, and ball mill at a speed of 800 rpm Pulverized for 5 hours to obtain 5.2 kg of mixed powder;

[0047] (3) Transfer the mixed powder into the feed tank of the sand mill, add 20.6 kg of phosphoric acid solution with a mass concentration of 8.5%, so that the solid-liquid weight ratio of the material is 1:4, and process the material at a speed of 2000 rpm Sanding, sanding time 10 hours, obtain slurry;

[0048] (4) Transfer the slurry to a spray dryer for dry...

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PUM

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Abstract

The invention provides a method for preparing lithium manganese iron phosphate from lithium iron phosphate. The method comprises the steps of utilizing lithium iron phosphate solid as a raw material;adding a reducing agent of 1 to 5% of the weight of the lithium iron phosphate solid at first; then adding a manganese source according to the weight ratio of lithium iron phosphate solid to the manganese source as (0.9 to 11) to 1; adding a lithium source according to the weight ratio of the lithium iron phosphate solid to the lithium source as (3 to 30) to 1; ball milling and smashing to obtainmixed powder; adding a phosphoric acid solution that is 1 to 4 times the weight of the mixed powder, wherein the mass concentration of the phosphoric acid solution is 7.5 to 17%; sanding at the certain rotation speed after solid-liquid mixing; transferring the sanded materials into a spray dryer; roasting at 450 to 800 DEG C for 5 to 10 hours after drying. According to the preparation method disclosed by the invention, a technology is simple, the manganese to iron proportion in a product of lithium manganese iron phosphate can be conveniently and accurately regulated by adjusting the adding amount of the manganese source; the prepared lithium manganese iron phosphate is of an orthogonal olivine structure; furthermore, the impurity content is lower than 0.005%, and the D95 granularity is 90to 160 nanometers; thus, the lithium manganese iron phosphate is especially suitable for serving as a lithium battery positive electrode material to be used.

Description

technical field [0001] The present invention relates to a method for preparing an inorganic compound, in particular to a method for preparing lithium iron manganese phosphate, and more particularly to a method for preparing lithium iron manganese phosphate from lithium iron phosphate. Background technique [0002] Lithium manganese iron phosphate is an important cathode material for lithium batteries. It has a variety of structures. Among them, the orthorhombic olivine structure is similar to the structure of lithium ion battery cathode materials such as lithium iron phosphate and lithium manganese phosphate. Lithium ions can move and intercalate in the crystal. , has electrochemical activity, and within a certain voltage range, the olivine structure of lithium manganese iron phosphate is stable, and it is not easy to transform into a spinel structure. Compared with lithium iron phosphate, lithium manganese iron phosphate with olivine structure has a theoretical capacity of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/45H01M4/58H01M10/0525
CPCC01B25/45C01P2004/62H01M4/5825H01M10/0525Y02E60/10
Inventor 谭泽黄司平陈旭波李煜乾
Owner GUANGDONG GUANGHUA SCI TECH
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