CN108483418A - A kind of LiFePO4 waste material treatment process - Google Patents
A kind of LiFePO4 waste material treatment process Download PDFInfo
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- CN108483418A CN108483418A CN201810276359.XA CN201810276359A CN108483418A CN 108483418 A CN108483418 A CN 108483418A CN 201810276359 A CN201810276359 A CN 201810276359A CN 108483418 A CN108483418 A CN 108483418A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of LiFePO4 waste material treatment process, are following steps：(1) after being 0 by waste lithium cell progress discharge treatment to voltage, in the case where completely cutting off air, the shell of the waste lithium cell is destroyed, electrolyte, shell and lug are isolated, dry core packet is obtained, positive plate is isolated from the dry core packet and is crushed, obtain LiFePO4 waste material, aqueous slkali stirring and dissolving 5 hours at 75 DEG C are added in LiFePO4 waste material, are then filtered, obtain containing aluminum solutions and the first filter residue；(2) the first filter residue is added in sulfuric acid solution, is stirred to react at 88 DEG C 5 hours, while iron powder is added in reaction process continuously and smoothly, it is 2.5 to react to the pH of solution.Present invention process reasonable design, at low cost, technological process is short, and the ferric phosphate of LITHIUM BATTERY and the lithium carbonate of LITHIUM BATTERY can be obtained, the recycling of full constituent is realized, and the added value of product that recycling obtains is high, it is the raw material of LiFePO4, and the rate of recovery of each component is high.
Description
Technical field
The invention belongs to chemical technology fields, and in particular to a kind of LiFePO4 waste material treatment process.
Background technology
With the development of electric vehicle, the LiFePO4 waste material in old and useless battery and production process that LiFePO4 is scrapped
Recycling become everybody focus of attention, the recycling of waste lithium iron phosphate at present is mainly the following：
(1) LiFePO4 for directly arranging in pairs or groups new after screening by waste lithium iron phosphate uses, although the method is simple,
It is the reduced performance of the LiFePO4 obtained later of arranging in pairs or groups, is only used for low side industry；
(2) after dissolving LiFePO4, iron precipitates to obtain iron oxide red, lithium recycling, phosphate recycling, but this technique
Long flow path, and value-added content of product is low.
Invention content
One, technical problems to be solved
The technical problem to be solved in the present invention is to provide a kind of LiFePO4 waste material treatment process, are asked with solving the technology
Topic.
Two, technical solution
To solve the technical problem, the technical solution adopted in the present invention is：A kind of LiFePO4 waste material treatment process,
For following steps：
It (1), will be described waste and old in the case where completely cutting off air after being 0 by waste lithium cell progress discharge treatment to voltage
The shell of lithium battery is destroyed, and electrolyte, shell and lug are isolated, and obtains dry core packet, is isolated from the dry core packet
Positive plate simultaneously crushes, and obtains LiFePO4 waste material, and aqueous slkali stirring and dissolving 5 hours at 75 DEG C are added in LiFePO4 waste material,
Then it filters, obtains containing aluminum solutions and the first filter residue；
(2) the first filter residue is added in sulfuric acid solution, is stirred to react at 88 DEG C 5 hours, while continuously even in reaction process
Iron powder is added in speed, and it is 2.5 to react to the pH of solution, and hydroxylamine hydrochloride is then added and makes a concentration of of hydroxylamine hydrochloride in reaction system
Then 0.02mol/L is filtered, obtain the first filtrate and the second filter residue；
(3) it is 55 DEG C, mixing speed 400r/min in temperature by the first filtrate, hydrogen peroxide is added, hydrogen peroxide is added
Time is 1.5 hours, then heats to 90 DEG C and continues stirring 3 hours, then filters, obtain the second filtrate and third filter residue, will
Third filter residue is according to solid-to-liquid ratio 1:2 add pure water pulp to obtain pulp material, the phosphoric acid solution of 4mol/L are then prepared, then by pulp
Material volume 1/4 is added in phosphoric acid solution, and it is 98 DEG C to be warming up to temperature, and 850r/min high-speed stirreds 2 hours to solution become
Clarification, is then added thereto the 3/4 of remaining pulp material volume again, then in temperature is 95 DEG C, under 850r/min high-speed stirreds
The reaction was continued 2 hours, until the color of material stops reaction after becoming white slightly powder, then filters, obtained phosphoric acid mother liquor is independent
It collects, until then the pH of pure water to washings is 6.2, then passes through drying, except iron, screening obtain LITHIUM BATTERY phosphoric acid
Iron；
(4) it is 83 DEG C in temperature by the second filtrate, it is 5 that magnesia, which is added, and adjusts the pH of solution, is then stirred to react 3 hours
After filter, obtain iron-containing filter residue and third filtrate, by third filtrate be added urea, temperature be 95 DEG C at react, maintain eventually
The pH of point is 9, and filtering obtains crude carbonic acid crystalline lithium and the 4th filtrate；
(5) the crude lithium carbonate that step (4) obtains is added into water slurry, vacuumized in sealing reaction kettle and maintains the pressure to be
8000Pa is then heated to water and boils completely, is then reacted 4 hours under the conditions of boiling, then filters, obtain magnesium carbonate filter residue
And the mixed solution of lithium hydroxide and lithia, it is passed through at being 95 DEG C in temperature by the mixed solution of lithium hydroxide and lithia
CO2, pH is 9 to terminal for reaction, obtains precipitation lithium carbonate, detaches and clean to obtain battery-level lithium carbonate, washing water temperature is
80℃。
What the step (1) obtained is added neopelex and polyethylene glycol containing aluminum solutions so that in solution
A concentration of 0.01mol/L of neopelex, a concentration of 0.01mol/L of polyethylene glycol, it is then molten with aluminium chloride ammonium
Liquid, acid-base modifier cocurrent are added in the liquid of bottom, and reaction temperature is 30 DEG C, and bottom liquid is the mixing of ammonium carbonate and ammonium hydroxide that pH is 9.5
Solution, it is 9.5 to maintain dropwise addition process pH, and it is 2 hours that the time, which is added, is added dropwise that the reaction was continued 1 hour, is then filtered, filter residue
It is dried at 85 DEG C after washing, after air-flow is broken, is calcined at 1000 DEG C and obtain nano aluminium oxide.
Molar ratio hydroxy is 1 in aluminium and aqueous slkali in the step (1) in LiFePO4 waste material:1.1, aqueous slkali
A concentration of 1mol/L.
The molar ratio of phosphate radical is 0.1 in the iron powder and the first filter residue that are added in the step (2):1, sulfuric acid solution it is dense
Degree is 4mol/L, and the second filter residue obtained by the reaction returns to be continued to dissolve in the first filter residue.
The molar ratio of step (3) hydrogen peroxide and the first filtrate ferrous ions is 1.1:2, the mass fraction of hydrogen peroxide
It is 30%, the molar ratio of the phosphoric acid in the phosphoric acid solution of addition and iron ion in third filter residue is 0.3:1.
The phosphoric acid mother liquor obtained in the step (3) returns after being concentrated into a concentration of 5mol/L to be continuing with.
The molar ratio of urea and lithium ion in third filtrate is 5 in the step (4):1, the 4th filtrate is filtered with third
The reaction was continued after liquid mixing, until the lithium ion content in the 4th filtrate is less than outer row after 100ppm.
Magnesium carbonate filter residue return in the step (5) is mixed with the first filter residue to continue to dissolve, the lithium in magnesium carbonate filter residue
Content is arranged less than outside 100ppm.
The present invention is prepared into nano aluminium oxide first by the way of alkali soluble solution to dissolve aluminium, then by aluminium, then is dissolved using acid,
Iron powder is added simultaneously, maintains whole process and carries out under reducing atmosphere, avoid the oxidation of ferrous ion, while ferrous ion
It is slightly excessive, the utilization rate of phosphate radical can also be improved.
Dissolving obtains being dissolving that ferrous ion, phosphate radical and lithium ion coexist, and oxidant is added and makes ferrous ion
It is oxidized to ferric ion, then is combined with phosphate radical to obtain ferric phosphate, in this way, the recycling of phosphate radical, iron ion can be thus achieved,
The separation for also achieving phosphate radical, iron ion and lithium ion simultaneously in turn avoids lithium ion caused by generating ferric hydroxide colloid
Loss the problem of, obtained battery-grade iron phosphate compares iron oxide red etc., and added value improves, current battery grade ferric phosphate
Price about per ton 2.7 ten thousand or so, and the price of iron oxide red it is per ton be only 5000 yuan or so.
Remaining iron ion adjusts pH using magnesia, can to avoid the generation of ferric hydroxide colloid, so as to avoid
The loss of lithium ion, then using urea come precipitation from homogeneous solution lithium ion, compare carbonate deposition, of obtained crude lithium carbonate
Grain bigger, crystallinity is more preferable, facilitates washing, avoids the entrainment of other ions, purity higher.
Lithium carbonate is boiled using boiling under vacuum again again, while under vacuum condition so that lithium carbonate decomposes faster generates oxygen
Change lithium and carbon dioxide, carbon dioxide are pumped immediately, to accelerate the decomposition of lithium carbonate, obtained lithia can dissolve
Into water, simultaneous oxidation lithium is obtained by the reaction lithium hydroxide with water and can also be dissolved into water, and magnesium carbonate cannot then be decomposed, then will
The mixed solution of pure lithium hydroxide and lithia, then it is passed through carbon dioxide under high temperature, lithium carbonate can be obtained with a step, obtained
Lithium carbonate narrow particle size distribution, purity is high.
Three, advantageous effect
The present invention is compared to the prior art, has the advantages that：
Present invention process reasonable design, at low cost, technological process is short, and can obtain the ferric phosphate and LITHIUM BATTERY of LITHIUM BATTERY
Lithium carbonate, realize the recycling of full constituent, and the added value of product that recycling obtains is high, is the raw material of LiFePO4, and
The rate of recovery of each component is high.
Specific implementation mode
With reference to embodiment, the specific implementation mode of the present invention is described in detail.
A kind of LiFePO4 waste material treatment process is following steps：
It (1), will be described waste and old in the case where completely cutting off air after being 0 by waste lithium cell progress discharge treatment to voltage
The shell of lithium battery is destroyed, and electrolyte, shell and lug are isolated, and obtains dry core packet, is isolated from the dry core packet
Positive plate simultaneously crushes, and obtains LiFePO4 waste material, and aqueous slkali stirring and dissolving 5 hours at 75 DEG C are added in LiFePO4 waste material,
Then it filters, obtains containing aluminum solutions and the first filter residue；
(2) the first filter residue is added in sulfuric acid solution, is stirred to react at 88 DEG C 5 hours, while continuously even in reaction process
Iron powder is added in speed, and it is 2.5 to react to the pH of solution, and hydroxylamine hydrochloride is then added and makes a concentration of of hydroxylamine hydrochloride in reaction system
Then 0.02mol/L is filtered, obtain the first filtrate and the second filter residue；
(3) it is 55 DEG C, mixing speed 400r/min in temperature by the first filtrate, hydrogen peroxide is added, hydrogen peroxide is added
Time is 1.5 hours, then heats to 90 DEG C and continues stirring 3 hours, then filters, obtain the second filtrate and third filter residue, will
Third filter residue is according to solid-to-liquid ratio 1:2 add pure water pulp to obtain pulp material, the phosphoric acid solution of 4mol/L are then prepared, then by pulp
Material volume 1/4 is added in phosphoric acid solution, and it is 98 DEG C to be warming up to temperature, and 850r/min high-speed stirreds 2 hours to solution become
Clarification, is then added thereto the 3/4 of remaining pulp material volume again, then in temperature is 95 DEG C, under 850r/min high-speed stirreds
The reaction was continued 2 hours, until the color of material stops reaction after becoming white slightly powder, then filters, obtained phosphoric acid mother liquor is independent
It collects, until then the pH of pure water to washings is 6.2, then passes through drying, except iron, screening obtain LITHIUM BATTERY phosphoric acid
Iron；
(4) it is 83 DEG C in temperature by the second filtrate, it is 5 that magnesia, which is added, and adjusts the pH of solution, is then stirred to react 3 hours
After filter, obtain iron-containing filter residue and third filtrate, by third filtrate be added urea, temperature be 95 DEG C at react, maintain eventually
The pH of point is 9, and filtering obtains crude carbonic acid crystalline lithium and the 4th filtrate；
(5) the crude lithium carbonate that step (4) obtains is added into water slurry, vacuumized in sealing reaction kettle and maintains the pressure to be
8000Pa is then heated to water and boils completely, is then reacted 4 hours under the conditions of boiling, then filters, obtain magnesium carbonate filter residue
And the mixed solution of lithium hydroxide and lithia, it is passed through at being 95 DEG C in temperature by the mixed solution of lithium hydroxide and lithia
CO2, pH is 9 to terminal for reaction, obtains precipitation lithium carbonate, detaches and clean to obtain battery-level lithium carbonate, washing water temperature is
80℃。
What the step (1) obtained is added neopelex and polyethylene glycol containing aluminum solutions so that in solution
A concentration of 0.01mol/L of neopelex, a concentration of 0.01mol/L of polyethylene glycol, it is then molten with aluminium chloride ammonium
Liquid, acid-base modifier cocurrent are added in the liquid of bottom, and reaction temperature is 30 DEG C, and bottom liquid is the mixing of ammonium carbonate and ammonium hydroxide that pH is 9.5
Solution, it is 9.5 to maintain dropwise addition process pH, and it is 2 hours that the time, which is added, is added dropwise that the reaction was continued 1 hour, is then filtered, filter residue
It is dried at 85 DEG C after washing, after air-flow is broken, is calcined at 1000 DEG C and obtain nano aluminium oxide.
Molar ratio hydroxy is 1 in aluminium and aqueous slkali in the step (1) in LiFePO4 waste material:1.1, aqueous slkali
A concentration of 1mol/L.
The molar ratio of phosphate radical is 0.1 in the iron powder and the first filter residue that are added in the step (2):1, sulfuric acid solution it is dense
Degree is 4mol/L, and the second filter residue obtained by the reaction returns to be continued to dissolve in the first filter residue.
The molar ratio of step (3) hydrogen peroxide and the first filtrate ferrous ions is 1.1:2, the mass fraction of hydrogen peroxide
It is 30%, the molar ratio of the phosphoric acid in the phosphoric acid solution of addition and iron ion in third filter residue is 0.3:1.
The phosphoric acid mother liquor obtained in the step (3) returns after being concentrated into a concentration of 5mol/L to be continuing with.
The molar ratio of urea and lithium ion in third filtrate is 5 in the step (4):1, the 4th filtrate is filtered with third
The reaction was continued after liquid mixing, until the lithium ion content in the 4th filtrate is less than outer row after 100ppm.
Magnesium carbonate filter residue return in the step (5) is mixed with the first filter residue to continue to dissolve, the lithium in magnesium carbonate filter residue
Content is arranged less than outside 100ppm.
The index of obtained battery-grade iron phosphate is as follows：
The rate of recovery of final products is as follows：
The rate of recovery 98.9% of ferric phosphate, the rate of recovery 98.2% of lithium, the rate of recovery 99.1% of aluminium.
Waste and old LiFePO4 waste material per ton is calculated, the profit that can be generated with LiFePO4 content 70%, aluminium content 20%
Profit is 7.5 ten thousand yuan, higher than other treatment process.
The specific application example that the above is only the present invention, is not limited in any way protection scope of the present invention.
Claims (8)
1. a kind of LiFePO4 waste material treatment process, which is characterized in that be following steps：
(1) after being 0 by waste lithium cell progress discharge treatment to voltage, in the case where completely cutting off air, by the useless old lithium
The shell in pond is destroyed, and electrolyte, shell and lug are isolated, and obtains dry core packet, and anode is isolated from the dry core packet
Piece simultaneously crushes, and obtains LiFePO4 waste material, aqueous slkali stirring and dissolving 5 hours at 75 DEG C is added in LiFePO4 waste material, then
Filtering obtains containing aluminum solutions and the first filter residue；
(2) the first filter residue is added in sulfuric acid solution, is stirred to react at 88 DEG C 5 hours, while adding in reaction process continuously and smoothly
Enter iron powder, it is 2.5 to react to the pH of solution, and hydroxylamine hydrochloride is then added and makes a concentration of of hydroxylamine hydrochloride in reaction system
Then 0.02mol/L is filtered, obtain the first filtrate and the second filter residue；
(3) it is 55 DEG C, mixing speed 400r/min in temperature by the first filtrate, hydrogen peroxide is added, the time of hydrogen peroxide is added
It is 1.5 hours, then heats to 90 DEG C and continue stirring 3 hours, then filter, obtain the second filtrate and third filter residue, by third
Filter residue is according to solid-to-liquid ratio 1:2 add pure water pulp to obtain pulp material, the phosphoric acid solution of 4mol/L are then prepared, then by pulp material body
Long-pending 1/4 is added in phosphoric acid solution, and it is 98 DEG C to be warming up to temperature, and 850r/min high-speed stirreds become clarifying for 2 hours to solution,
Then the 3/4 of remaining pulp material volume is added thereto again, then in temperature is 95 DEG C, continued under 850r/min high-speed stirreds anti-
It answers 2 hours, until the color of material stops reaction after becoming white slightly powder, then filters, obtained phosphoric acid mother liquor is collected separately, so
Afterwards then pure water passes through drying, except iron, screening obtain battery-grade iron phosphate until the pH of washings is 6.2；
(4) it is 83 DEG C in temperature by the second filtrate, it is 5 that magnesia, which is added, and adjusts the pH of solution, is then stirred to react mistake after 3 hours
Filter, obtains iron-containing filter residue and third filtrate, and urea is added in third filtrate, is reacted at being 95 DEG C in temperature, maintains terminal
PH is 9, and filtering obtains crude carbonic acid crystalline lithium and the 4th filtrate；
(5) the crude lithium carbonate that step (4) obtains is added into water slurry, vacuumized in sealing reaction kettle and maintains the pressure to be
8000Pa is then heated to water and boils completely, is then reacted 4 hours under the conditions of boiling, then filters, obtain magnesium carbonate filter residue
And the mixed solution of lithium hydroxide and lithia, it is passed through at being 95 DEG C in temperature by the mixed solution of lithium hydroxide and lithia
CO2, pH is 9 to terminal for reaction, obtains precipitation lithium carbonate, detaches and clean to obtain battery-level lithium carbonate, washing water temperature is
80℃。
2. a kind of LiFePO4 waste material treatment process according to claim 1, it is characterised in that：The step (1) obtains
Neopelex and polyethylene glycol is added containing aluminum solutions so that neopelex in solution it is a concentration of
Then bottom liquid is added with aluminium chloride ammonium salt solution, acid-base modifier cocurrent in 0.01mol/L, a concentration of 0.01mol/L of polyethylene glycol
In, reaction temperature is 30 DEG C, and bottom liquid is the mixed solution of the ammonium carbonate that pH is 9.5 and ammonium hydroxide, and it is 9.5 to maintain dropwise addition process pH,
It is 2 hours that the time, which is added, is added dropwise that the reaction was continued 1 hour, is then filtered, and filter residue is dried after washing at 85 DEG C, air-flow
After broken, calcined at 1000 DEG C and obtain nano aluminium oxide.
3. a kind of LiFePO4 waste material treatment process according to claim 1, it is characterised in that：Phosphorus in the step (1)
Molar ratio hydroxy is 1 in aluminium and aqueous slkali in sour iron lithium waste material:1.1, a concentration of 1mol/L of aqueous slkali.
4. a kind of LiFePO4 waste material treatment process according to claim 1, it is characterised in that：Add in the step (2)
The molar ratio of phosphate radical is 0.1 in the iron powder and the first filter residue that enter:1, a concentration of 4mol/L of sulfuric acid solution, obtained by the reaction
Two filter residues return to be continued to dissolve in the first filter residue.
5. a kind of LiFePO4 waste material treatment process according to claim 1, it is characterised in that：Step (3) dioxygen
The molar ratio of water and the first filtrate ferrous ions is 1.1:2, the mass fraction of hydrogen peroxide is 30%, in the phosphoric acid solution of addition
Phosphoric acid and third filter residue in the molar ratio of iron ion be 0.3:1.
6. a kind of LiFePO4 waste material treatment process according to claim 1, it is characterised in that：In the step (3)
To phosphoric acid mother liquor return and be continuing with after being concentrated into a concentration of 5mol/L.
7. a kind of LiFePO4 waste material treatment process according to claim 1, it is characterised in that：Urine in the step (4)
The molar ratio of element and lithium ion in third filtrate is 5:1, the reaction was continued after the 4th filtrate mixes with third filtrate, until the 4th
Lithium ion content in filtrate is less than outer row after 100ppm.
8. a kind of LiFePO4 waste material treatment process according to claim 1, it is characterised in that：In the step (5)
The return of magnesium carbonate filter residue is mixed with the first filter residue to continue to dissolve, and the lithium content in magnesium carbonate filter residue is arranged less than outside 100ppm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109179358A (en) * | 2018-11-08 | 2019-01-11 | 广东省稀有金属研究所 | A method of preparing battery-grade iron phosphate from waste lithium iron phosphate battery |
| CN109554545A (en) * | 2018-09-29 | 2019-04-02 | 广东邦普循环科技有限公司 | A method of lithium is selectively mentioned from LiFePO4 waste material |
| CN113912035A (en) * | 2021-11-29 | 2022-01-11 | 材料科学姑苏实验室 | Method for recovering battery-grade iron phosphate material from phosphorus-iron slag |
| CN113955753A (en) * | 2021-08-24 | 2022-01-21 | 安徽南都华铂新材料科技有限公司 | Method for recovering waste lithium iron phosphate battery powder |
-
2018
- 2018-03-30 CN CN201810276359.XA patent/CN108483418A/en not_active Withdrawn
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109554545A (en) * | 2018-09-29 | 2019-04-02 | 广东邦普循环科技有限公司 | A method of lithium is selectively mentioned from LiFePO4 waste material |
| CN109554545B (en) * | 2018-09-29 | 2020-12-11 | 广东邦普循环科技有限公司 | Method for selectively extracting lithium from lithium iron phosphate waste |
| CN109179358A (en) * | 2018-11-08 | 2019-01-11 | 广东省稀有金属研究所 | A method of preparing battery-grade iron phosphate from waste lithium iron phosphate battery |
| CN113955753A (en) * | 2021-08-24 | 2022-01-21 | 安徽南都华铂新材料科技有限公司 | Method for recovering waste lithium iron phosphate battery powder |
| CN113912035A (en) * | 2021-11-29 | 2022-01-11 | 材料科学姑苏实验室 | Method for recovering battery-grade iron phosphate material from phosphorus-iron slag |
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