CN106848472A - A kind of method that lithium is reclaimed in waste lithium iron phosphate battery - Google Patents
A kind of method that lithium is reclaimed in waste lithium iron phosphate battery Download PDFInfo
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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Abstract
The invention provides a kind of method of high efficiente callback lithium in waste lithium iron phosphate battery, be calcined for waste lithium iron phosphate battery and sort by the method, obtain positive mix containing lithium, powder containing lithium reacts with calcic alkaline solution under oxidative conditions, iron and phosphate radical are converted into water insoluble compound, lithium is converted to the lithium hydroxide for being dissolved in water, lithium hydroxide solution is obtained after filtering, can be used to further prepare lithium hydroxide or lithium carbonate product；The wet method acid immersion routinely used in old and useless battery removal process has been abandoned in the invention, it is to avoid the use of strong acid, therefore avoids the generation of a large amount of high-salt wastewaters；The process selectivity leaches elemental lithium, iron tramp into the problem of leachate is avoided from source, the final lithium product purity for obtaining is high, and flow is short, chemical agent wide material sources, process conditions are simple, can one-step method obtain high purity lithium product, the organic efficiency of waste lithium iron phosphate battery is greatly improved, with good prospects for commercial application.
Description
Technical field
Recycled the invention belongs to secondary resource and recycling economy technical field, more particularly to a kind of waste lithium iron phosphate
The method that lithium is reclaimed in battery.
Background technology
The energy and environment turn into the problem of people's growing interest.As the exhausted and vehicle exhaust increasingly of petroleum resources is arranged
The harm aggravation of the atmosphere pollution for causing is put, electric motor car and hybrid electric vehicle obtain the attention of national governments and Automobile Enterprises.With
The development of electric automobile, ferric phosphate lithium cell is because with raw material resources is abundant, cheap, environmentally safe, structure
The advantages of stabilization and heat endurance are good, is widely applied.A large amount of with ferric phosphate lithium cell are used, and old and useless battery is returned
Receive using a new task is just become, its recovery can not only mitigate influence of the old and useless battery to environment, moreover it is possible to bring certain
Economic benefit, reduce battery cost.
The recovery technology of waste lithium iron phosphate battery combines hydrometallurgy and pyrometallurgy, by wet-leaching and high temperature
Calcination and regeneration obtains lithium iron phosphate positive material, and such as CN102280673A, CN104362408A and CN102751548A is public respectively
Cloth old and useless battery wet-leaching and in an oxidizing atmosphere calcining prepare the process of LiFePO4 product.High temperature above is forged
Burn the method for directly reclaiming LiFePO4, need to by ball milling, high-temperature calcination, again ball milling, the multiple operations, process conditions such as re-sinter
Harsh, energy consumption is big, flow is complicated, therefore is not used widely.In order to simplify recovery process, cost recovery is reduced, it is domestic
Outer researcher develops various recovery technologies based on hydrometallurgy, and its main flow is that old and useless battery is fired, broken
Batch mixing is obtained, aluminium is then removed using alkaline process, obtain iron, lithium mixing slag, while leaching iron, elemental lithium, selective precipitation is obtained afterwards
To lithium product.As CN102285673A discloses a kind of side that iron and lithium are reclaimed from electric automobile lithium ferric phosphate power cell
Method, iron and lithium are leached using acid and reducing agent simultaneously, then adjust the pH value of leachate to 1.5 ~ 3, and Precipitation iron hydroxide is obtained
To iron oxide articles, then filtrate pH value is adjusted with alkali, lithium carbonate is prepared after removal of impurities.CN101847763A is then molten using organic solvent
Solution and the mode of acidolysis obtain copper, iron, lithium, phosphorus solution, and then auxiliary adds vulcanized sodium and adjusts pH and removes copper removal and ferro element.With
On the wet-leaching that refers to reclaim the method for elemental lithium in leach iron and elemental lithium simultaneously, further separate iron and lithium unit
Element, often consumes substantial amounts of acid solution, and with leachate containing miscellaneous and a large amount of high-salt wastewaters of generation problems.
The content of the invention
It is low and the problems such as produced with a large amount of high-salt wastewaters in order to solve to reclaim at present extract technology long flow path, leaching rate,
The present invention is intended to provide a kind of method that lithium is reclaimed in waste lithium iron phosphate battery.Methods described Selectively leaching elemental lithium, from
Iron tramp into the problem of leachate is avoided on source, therefore it is high to reclaim the lithium product purity for obtaining.By waste lithium iron phosphate
Battery roasting sorting, obtains positive mix containing lithium.Powder containing lithium reacts with calcic alkaline solution under oxidative conditions, by iron and phosphorus
Acid group is converted to water insoluble compound, and lithium is converted to the lithium hydroxide for being dissolved in water.Lithium hydroxide solution is obtained after filtering,
Can be used to further prepare lithium hydroxide or lithium carbonate product.The invention is routinely used in having abandoned old and useless battery removal process
Wet method acid immersion, it is to avoid the use of strong acid, therefore avoid the generation of a large amount of high-salt wastewaters.Because flow of the present invention is short, change
Learn medicament wide material sources, process conditions it is simple, can one-step method obtain high purity lithium product, greatly improve waste lithium iron phosphate electricity
The organic efficiency in pond, with good prospects for commercial application.
It is that, up to this purpose, the present invention uses following technical scheme：
A kind of method that lithium is reclaimed in waste lithium iron phosphate battery, comprises the following steps：
（1）Waste lithium iron phosphate battery is calcined and is sorted, obtain positive mix containing lithium；
（2）Step（1）Gained positive mix is added to the calcic alkaline solution in oxidative environment, and iron and phosphate radical are converted to
Water insoluble compound, lithium is converted to the lithium hydroxide for being dissolved in water；
（3）Step（2）The compound and phosphate of the water insoluble iron of resulting solution filtering removal, obtain lithium hydroxide solution；
（4）Step（3）Gained lithium hydroxide solution further prepares lithium hydroxide or lithium carbonate product.
Method according to claim 1, it is characterised in that step（1）LiFePO4 old and useless battery is crushed and is calcined
Sorting, obtains positive mix containing lithium；
Preferably, cell positive material is broken for the fragment of 1 ~ 20mm × 1 ~ 20mm by Mechanical Crushing；
Preferably, sintering temperature is 200 ~ 1200 DEG C；
Preferably, roasting time is 1 ~ 6h.
Step（1）Calcic powder can be sprayed into roasting process to absorb the generation of fluoro-gas；
Preferably, calcic powder is a kind of in calcic inorganic matter, calcic organic matter and calcic biomass or any several combination；
Preferably, the calcic powder is CaC2、CaCl2、CaCO3、Ca(NO3)2、CaO、Ca(OH)2、Ca5(PO4)3(OH)、
C36H70CaO4、C6H10CaO6、C6H10CaO6、Ca(HCO2)2、Ca(CH3COO)2、CaC2O4In one kind or any several combinations；
Preferably, the battery waste and the quality proportioning of calcic powder are 0.1 ~ 3000:1, more preferably 20 ~ 300:1；
Preferably, gravity separation can be used after roasting, eddy flow or screening remove the metals such as aluminium, copper, obtain powder containing lithium.
Step（2）Gained positive mix is added to calcic alkaline solution, is reacted in an oxidizing environment, by iron and phosphate radical
Water insoluble compound is converted to, lithium is converted to the lithium hydroxide for being dissolved in water；
Preferably, the oxidative environment is to add or be passed through oxidant air, H in the solution2O2、MnO2、KMnO4、O2One
Plant or several combinations；
Preferably, calcic aqueous slkali is or the suspension containing calc-alkaline containing calcium ion alkaline solution；
Preferably, it is described containing calcium constituent in calcium solution, suspension（Ion or solid）Mass concentration is 0.1 ~ 100%.
Step（3）Resulting solution is filtered, the compound and phosphate of water insoluble iron is removed, lithium hydroxide is obtained molten
Liquid.
Step（4）By the concentration of gained lithium hydroxide solution, lithium hydroxide is directly prepared after removal of impurities extraction, cleaning obtains high-purity
Lithium hydroxide, or lithium concentration is concentrated into for 200 ~ 500g/L, saturated sodium carbonate solution precipitation lithium carbonate is added, separate and clear
Wash the pure Lithium Carbonate for obtaining, thickening temperature is 40 ~ 100 DEG C, precipitation temperature is 20 ~ 100 DEG C, precipitation mixing speed is 100 ~
2000rpm, the precipitation stirring and adjusting time is 0.5 ~ 72h, and washing water temperature is 10 ~ 100 DEG C；
Preferably, thickening temperature is 70 ~ 100 DEG C；
Preferably, precipitation temperature is 60 ~ 100 DEG C；
Preferably, precipitation mixing speed is 100 ~ 500rpm；
Preferably, the precipitation stirring and adjusting time is 2 ~ 12h；
Preferably, the carbanion that precipitation is added is 1 ~ 3 with the molar ratio of lithium ion in solution:2；
Preferably, the temperature for washing water used is 40 ~ 100 DEG C.
Brief description of the drawings
Fig. 1 is a kind of process chart of the method for high efficiente callback lithium in waste lithium iron phosphate battery.
Specific embodiment
Further illustrate technical scheme below in conjunction with the accompanying drawings and by specific embodiment.The skill of this area
Art personnel it will be clearly understood that described embodiment be only to aid in understand the present invention, be not construed as to concrete restriction of the invention.
Embodiment
A part of embodiment of the invention, rather than whole embodiments, based on the embodiment in the present invention, art technology
The every other embodiment that personnel are obtained under the premise of innovative labor is not made, belongs to protection scope of the present invention.
Embodiment 1
（1）Positive material of waste lithium iron phosphate is broken for the fragment of 1 ~ 20mm × 1 ~ 20mm, is calcined under 800 DEG C of high temperature
2h, CaO can be sprayed into roasting process prevents the generation of fluoro-gas, and battery waste is controlled 300 with the mass ratio of calcic powder:
1.Roasting removes the metals such as aluminium and copper after terminating using screening, obtains powder containing lithium.
The ferric phosphate lithium cell of the table 1 roasting sorting gained composition of powder containing lithium（wt%）
| Fe | P | Li |
| 25.7 | 14.4 | 3.2 |
（2）Gained positive mix is added to containing Ca (OH)2Alkaline suspension, is passed through oxygen in course of reaction（Oxidant/contain positive pole
Powder liquor capacity ratio is 10）, iron and phosphate radical are converted into water insoluble compound, lithium is converted to the hydrogen-oxygen for being dissolved in water
Change lithium.Solution calcium constituent（Ion or solid）Mass concentration is 15%, and positive mix is 2 with calcium constituent mass ratio：1.
（3）Resulting solution filtering removal iron hydroxide, calcium phosphate, the calcium hydroxide not reacted completely, obtain lithium hydroxide
Solution.
（4）Gained lithium hydroxide solution, is concentrated into lithium concentration for 250g/L, adds saturated sodium carbonate solution precipitation carbon
Sour lithium, separates and cleans the pure Lithium Carbonate for obtaining（Purity 99.97%）.Sodium carbonate precipitation temperature is 95 DEG C, precipitates mixing speed
It is 500rpm, the stirring and adjusting time is 2 ~ 12h, and carbanion is 1.5 with the molar ratio of lithium ion in solution:1, wash institute
It it is 90 DEG C with the temperature of water.
Embodiment 2
（1）Positive material of waste lithium iron phosphate is broken for the fragment of 1 ~ 20mm × 1 ~ 20mm, is calcined under 1000 DEG C of high temperature
2h, CaO can be sprayed into roasting process prevents the generation of fluoro-gas, and battery waste is controlled 300 with the mass ratio of calcic powder:
1.Roasting removes the metals such as aluminium and copper after terminating using screening, obtains powder containing lithium.
The ferric phosphate lithium cell of the table 2 roasting sorting gained composition of powder containing lithium（wt%）
| Fe | P | Li |
| 19.2 | 8.7 | 1.7 |
（2）Gained positive mix is added to containing Ca (OH)2Alkaline suspension, while adding KMnO2Solution（Positive mix solution/
KMnO2Solution quality compares 20, KMnO2Solution concentration is 10%）, iron and phosphate radical are converted into water insoluble compound, by lithium
Be converted to the lithium hydroxide for being dissolved in water.Solution calcium constituent（Ion or solid）Mass concentration is 15%, positive mix and calcium constituent
Mass ratio is 2：1.
（3）Resulting solution filtering removal iron hydroxide, calcium phosphate, the calcium hydroxide not reacted completely, obtain lithium hydroxide
Solution.
（4）Gained lithium hydroxide solution, concentration directly prepares lithium hydroxide, and 95 DEG C of thickening temperature is obtained after removal of impurities extraction
Lithium hydroxide（Purity reaches 99.95%）, the temperature of washing water used is 90 DEG C.
Embodiment 3
（1）Positive material of waste lithium iron phosphate is broken for the fragment of 1 ~ 20mm × 1 ~ 20mm, is calcined under 1200 DEG C of high temperature
2h, can spray into CaCO in roasting process3The generation of fluoro-gas is prevented, battery waste exists with the mass ratio control of calcic powder
300:1.Roasting removes the metals such as aluminium and copper after terminating using screening, obtains powder containing lithium.
The ferric phosphate lithium cell of the table 3 roasting sorting gained composition of powder containing lithium（wt%）
| Fe | P | Li |
| 23.1 | 10.5 | 2.1 |
（2）Gained positive mix is added to solution containing Ca, and adds H2O2Solution（Positive mix solution/H2O2Solution quality ratio
30, H2O2Solution concentration is 15%）, iron and phosphate radical are converted into water insoluble compound, lithium is converted to the hydrogen for being dissolved in water
Lithia.Solution calcium constituent（Ion or solid）Mass concentration is 15%, and positive mix is 2 with calcium constituent mass ratio：1.
（3）Resulting solution filtering removal iron hydroxide, calcium phosphate, the calcium hydroxide not reacted completely, obtain lithium hydroxide
Solution.
（4）Gained lithium hydroxide solution, is concentrated into lithium concentration for 250g/L, adds saturated sodium carbonate solution precipitation carbon
Sour lithium, separates and cleans the pure Lithium Carbonate for obtaining（Purity 99.98%）.Sodium carbonate precipitation temperature is 95 DEG C, precipitates mixing speed
It is 500rpm, the stirring and adjusting time is 2 ~ 12h, and carbanion is 1.5 with the molar ratio of lithium ion in solution:1, wash institute
It it is 90 DEG C with the temperature of water.
Applicant states that the present invention illustrates process of the invention by above-described embodiment, but the present invention not office
It is limited to above-mentioned processing step, that is, does not mean that the present invention has to rely on above-mentioned processing step and could implement.Art
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to raw material selected by the present invention
Addition, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosing.
Claims (6)
1. a kind of method that lithium is reclaimed in waste lithium iron phosphate battery, it is characterised in that comprise the following steps：
（1）Waste lithium iron phosphate battery is calcined and is sorted, obtain positive mix containing lithium；
（2）Step（1）Gained positive mix is added to the calcic alkaline solution in oxidative environment, and iron and phosphate radical are converted to
Water insoluble compound, lithium is converted to the lithium hydroxide for being dissolved in water；
（3）Step（2）The compound and phosphate of the water insoluble iron of resulting solution filtering removal, obtain lithium hydroxide solution；
（4）Step（3）Gained lithium hydroxide solution further prepares lithium hydroxide or lithium carbonate product.
2. method according to claim 1, it is characterised in that step（1）LiFePO4 old and useless battery is crushed and roasting point
Choosing, obtains positive mix containing lithium；
Preferably, cell positive material is broken for the fragment of 1 ~ 20mm × 1 ~ 20mm by Mechanical Crushing；
Preferably, sintering temperature is 200 ~ 1200 DEG C；
Preferably, roasting time is 1 ~ 6h.
3. method according to claim 1, it is characterised in that calcic powder can be sprayed into roasting process to absorb fluoro-gas
Generation；
Preferably, calcic powder is a kind of in calcic inorganic matter, calcic organic matter and calcic biomass or any several combination；
Preferably, the calcic powder is CaC2、CaCl2、CaCO3、Ca(NO3)2、CaO、Ca(OH)2、Ca5(PO4)3(OH)、
C36H70CaO4、C6H10CaO6、C6H10CaO6、Ca(HCO2)2、Ca(CH3COO)2、CaC2O4In one kind or any several combinations；
Preferably, the battery waste and the quality proportioning of calcic powder are 0.1 ~ 3000:1, more preferably 20 ~ 300:1；
Preferably, the metals such as aluminium, copper can be removed using gravity separation, eddy flow or screening after roasting, obtains powder containing lithium.
4. method according to claim 1, it is characterised in that step（2）Gained positive mix is added to molten containing calc-alkaline
Liquid, is reacted in an oxidizing environment, and iron and phosphate radical are converted into water insoluble compound, and lithium is converted to the hydrogen-oxygen for being dissolved in water
Change lithium；
Preferably, the oxidative environment is to add or be passed through oxidant air, H in the solution2O2、MnO2、KMnO4、O2One
Plant or several combinations；
Preferably, calcic aqueous slkali is or the suspension containing calc-alkaline containing calcium ion alkaline solution；
Preferably, it is described containing calcium constituent in calcium solution, suspension（Ion or solid）Mass concentration is 0.1 ~ 100%.
5. method according to claim 1, it is characterised in that step（3）Resulting solution is filtered, water insoluble iron is removed
Compound and phosphate, obtain lithium hydroxide solution.
6. method according to claim 1, it is characterised in that step（4）By the concentration of gained lithium hydroxide solution, removal of impurities extraction
Lithium hydroxide is directly prepared afterwards, and cleaning obtains Lithium hydroxide, or is concentrated into lithium concentration for 200 ~ 500g/L, adds full
Lithium carbonate is precipitated with sodium carbonate liquor, the pure Lithium Carbonate for obtaining is separated and clean, thickening temperature is 40 ~ 100 DEG C, precipitation temperature
It it is 20 ~ 100 DEG C, precipitation mixing speed is 100 ~ 2000rpm, the precipitation stirring and adjusting time is 0.5 ~ 72h, and washing water temperature is
10~100℃；
Preferably, thickening temperature is 70 ~ 100 DEG C；
Preferably, precipitation temperature is 60 ~ 100 DEG C；
Preferably, precipitation mixing speed is 100 ~ 500rpm；
Preferably, the precipitation stirring and adjusting time is 2 ~ 12h；
Preferably, the carbanion that precipitation is added is 1 ~ 3 with the molar ratio of lithium ion in solution:2；
Preferably, the temperature for washing water used is 40 ~ 100 DEG C.
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|---|---|---|---|---|
| CN107381604A (en) * | 2017-07-12 | 2017-11-24 | 深圳佳彬科技有限公司 | A kind of method that lithium carbonate is reclaimed from ferric phosphate lithium cell |
| CN107959080A (en) * | 2018-01-05 | 2018-04-24 | 广东省稀有金属研究所 | A kind of preprocess method of waste and old lithium ion battery material recovery valuable element |
| CN107959076A (en) * | 2017-11-13 | 2018-04-24 | 中国恩菲工程技术有限公司 | The processing method of waste and old lithium ion battery |
| CN108390120A (en) * | 2017-12-11 | 2018-08-10 | 中国科学院过程工程研究所 | A kind of method of lithium in selective recovery waste lithium ion cell anode material |
| CN108642304A (en) * | 2018-05-15 | 2018-10-12 | 湖南邦普循环科技有限公司 | A kind of comprehensive recovering process of LiFePO4 waste material |
| CN108977665A (en) * | 2018-08-17 | 2018-12-11 | 湖南金凯循环科技有限公司 | A method of recycling waste and old lithium manganese phosphate |
| CN109652654A (en) * | 2018-12-30 | 2019-04-19 | 沈阳化工研究院有限公司 | A kind of method of waste and old ternary dynamic lithium battery resource utilization metallic element |
| CN110013822A (en) * | 2018-01-07 | 2019-07-16 | 中南大学 | A kind of method of waste and old lithium ion battery recycling co-production lithium adsorbent |
| CN110510664A (en) * | 2018-05-22 | 2019-11-29 | 银隆新能源股份有限公司 | A kind of preparation method and application of lithium titanate anode material |
| CN111960396A (en) * | 2020-08-26 | 2020-11-20 | 界首市南都华宇电源有限公司 | Method for preparing soluble phosphate from iron phosphate slag |
| CN113061723A (en) * | 2021-03-04 | 2021-07-02 | 长沙友合金属材料有限公司 | Method for recovering lithium from waste lithium iron phosphate batteries and preparing iron phosphate |
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| CN107381604A (en) * | 2017-07-12 | 2017-11-24 | 深圳佳彬科技有限公司 | A kind of method that lithium carbonate is reclaimed from ferric phosphate lithium cell |
| CN107381604B (en) * | 2017-07-12 | 2019-04-26 | 深圳佳彬科技有限公司 | A method of recycling lithium carbonate from ferric phosphate lithium cell |
| CN107959076A (en) * | 2017-11-13 | 2018-04-24 | 中国恩菲工程技术有限公司 | The processing method of waste and old lithium ion battery |
| CN108390120A (en) * | 2017-12-11 | 2018-08-10 | 中国科学院过程工程研究所 | A kind of method of lithium in selective recovery waste lithium ion cell anode material |
| CN107959080A (en) * | 2018-01-05 | 2018-04-24 | 广东省稀有金属研究所 | A kind of preprocess method of waste and old lithium ion battery material recovery valuable element |
| CN110013822B (en) * | 2018-01-07 | 2020-02-14 | 中南大学 | Method for recycling waste lithium ion batteries and co-producing lithium adsorbent |
| CN110013822A (en) * | 2018-01-07 | 2019-07-16 | 中南大学 | A kind of method of waste and old lithium ion battery recycling co-production lithium adsorbent |
| CN108642304A (en) * | 2018-05-15 | 2018-10-12 | 湖南邦普循环科技有限公司 | A kind of comprehensive recovering process of LiFePO4 waste material |
| CN108642304B (en) * | 2018-05-15 | 2020-08-07 | 湖南邦普循环科技有限公司 | Comprehensive recovery method of lithium iron phosphate waste |
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| CN110510664B (en) * | 2018-05-22 | 2021-08-10 | 银隆新能源股份有限公司 | Preparation method and application of lithium titanate negative electrode material |
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| CN116837216B (en) * | 2023-09-01 | 2023-11-21 | 北京怀柔北珂新能源科技有限公司 | Impurity removal method for recycling positive electrode powder of lithium ion battery |
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