CN109022803A - The recovery method of elemental lithium during a kind of waste phosphoric acid lithium iron battery is positive - Google Patents
The recovery method of elemental lithium during a kind of waste phosphoric acid lithium iron battery is positive Download PDFInfo
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- CN109022803A CN109022803A CN201811032353.4A CN201811032353A CN109022803A CN 109022803 A CN109022803 A CN 109022803A CN 201811032353 A CN201811032353 A CN 201811032353A CN 109022803 A CN109022803 A CN 109022803A
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- phosphoric acid
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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- Manufacturing & Machinery (AREA)
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- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
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- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of recovery methods of elemental lithium in waste phosphoric acid lithium iron battery anode, positive electrode is separated from waste and old ferric phosphate lithium cell first, positive electrode is soaked in N- methyl pyrrole network alkanone, so that the positive active material in positive electrode is kept completely separate with aluminum substrate, it then will impregnate positive electrode taking-up drying, calcining, grinding after reacting and obtain LiFePO4 powder；LiFePO4 powder and oxalic acid solution are put into reactor, then reactor is placed under 40-90 DEG C of bath temperature and carries out Leach reaction, after reaction, after filtering and washing, yellow green liquid and black residue are generated, then black residue is filtered and is dried, obtains waste material.The present invention uses oxalic acid to carry out the recycling of lithium ion as leaching agent, has many advantages, such as that recovery method is simple, at low cost, secondary pollution is few, energy-saving effect is good and high financial profit, by the setting to parameter is leached, obtains higher leaching rate.
Description
Technical field
The present invention relates to battery recycling field, the recycling side of elemental lithium in specifically a kind of waste phosphoric acid lithium iron battery anode
Method.
Background technique
Lithium iron phosphate positive material is abundant, and versus environmental is friendly, and has excellent thermal stability.But due to electricity
The disadvantages of electron conductivity is low, volume energy density is low, poor performance at low temperatures needs to have obtained further hair in following development
It opens up and perfect.On the other hand, the processing for lithium iron phosphate battery of giving up is very important.Improper use and irresponsible disposition is useless
It will lead to environmental problem, since harmful electrolyte and phosphorus are found in LiFePO4.Once these harm enter natural water, just
It will lead to water eutrophication.Therefore, it is necessary to ensure to recycle the harmless treatment of lithium and phosphorus from LiFePO4.Waste and scrap
It carries out main removal process and is based primarily upon three types: hydrometallurgical processes, pyrometallurgical method and deposit impregnating technology.However, pyrogenic process smelting
Gold is not suitable for because energy consumption is high for it.For bioleaching process, the tenor of concentration is considered as toxic cell, in process
In gradually decrease bacterial activity.In fact, a large amount of research concentrates in various Wet-process metallurgy methods, these methods can substantially divide
For inorganic Ore Leaching, organic Acid leaching, chemical precipitation, organic solvent extraction etc..
Summary of the invention
The technical problem to be solved in the present invention is to provide the recovery method of elemental lithium in a kind of waste phosphoric acid lithium iron battery anode,
Using oxalic acid leaching method, have that recovery method is simple, at low cost, secondary pollution is few, energy-saving effect is good and economic benefit height etc.
Advantage.
The technical solution of the present invention is as follows:
The recovery method of elemental lithium during a kind of waste phosphoric acid lithium iron battery is positive, has specifically included following steps:
(1), positive electrode is separated from waste and old ferric phosphate lithium cell, positive electrode is soaked in 100 DEG C of N- methyl
1 h in pyrrole network alkanone, so that the positive active material in positive electrode is kept completely separate with aluminum substrate, after then impregnating reaction
Positive electrode takes out and is dried to obtain the LiFePO4 powder containing impurity, by the LiFePO4 powder containing impurity at 400 DEG C
Calcining 1 hour, is finally ground to obtain LiFePO4 powder；
(2), the oxalic acid solution of LiFePO4 powder and 0.1~1.5 mol/L are matched simultaneously by the solid-to-liquid ratio of 10~90g/L
It is put into reactor, then reactor is placed under 40-90 DEG C of bath temperature and carries out Leach reaction, after Leach reaction,
After filtering and washing, yellow green liquid and black residue are generated, then black residue is filtered and is dried, is obtained
Waste material.
The concentration of the oxalic acid solution is 0.3mol/L.
The bath temperature is 80 DEG C.
The solid-to-liquid ratio of the LiFePO4 powder and oxalic acid solution is 60g/L.
The time of the Leach reaction is -120 minutes 10 minutes.
The time of the Leach reaction is 60 minutes.
The reactor of the step (2) selects three neck round bottom reactor, is equipped on three neck round bottom reactor
There is impeller magnetic stirrer to be stirred, while being provided with steam condenser to reduce the moisture of evaporation loss.
Washing is washed using distilled water in the step (2).
Advantages of the present invention:
(1), the present invention uses oxalic acid to carry out the recycling of lithium ion as leaching agent, has recovery method simple, at low cost, secondary
The advantages that pollution is less, energy-saving effect is good and high financial profit.
(2), the present invention passes through the setting to parameter is leached, the i.e. solid-to-liquid ratio of the concentration, Leach reaction of oxalic acid solution, leaching
The time of reaction and the setting of temperature, obtain higher leaching rate.
Detailed description of the invention
Fig. 1 is the linear graph that concentration of oxalic acid of the present invention influences Li ion, Fe ion leaching efficiency;
Fig. 2 is the linear three-dimensional figure influenced on Li ion leaching efficiency in Leach reaction temperature of the present invention and reaction time;
Fig. 3 is the linear three-dimensional figure influenced on Fe ion leaching efficiency in Leach reaction temperature of the present invention and reaction time;
Fig. 4 is the linear graph that solid-to-liquid ratio influences Li ion, Fe ion leaching efficiency in Leach reaction of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The recovery method of elemental lithium during a kind of waste phosphoric acid lithium iron battery is positive, has specifically included following steps:
(1), positive electrode is separated from waste and old ferric phosphate lithium cell, positive electrode is soaked in 100 DEG C of N- methyl
1 h in pyrrole network alkanone, so that the positive active material in positive electrode is kept completely separate with aluminum substrate, after then impregnating reaction
Positive electrode takes out and is dried to obtain the LiFePO4 powder containing impurity, by the LiFePO4 powder containing impurity at 400 DEG C
Calcining 1 hour, is finally ground to obtain LiFePO4 powder；
(2), the oxalic acid solution of LiFePO4 powder and 0.1~1.5 mol/L are matched simultaneously by the solid-to-liquid ratio of 10~90g/L
It is put into three neck round bottom reactor, is stirred on three neck round bottom reactor equipped with impeller magnetic stirrer, together
When be provided with steam condenser to reduce the moisture of evaporation loss, three neck round bottom reactor is then placed in 40-90 DEG C of water
It is carried out Leach reaction 10-120 minutes under bath temperature, after Leach reaction, after filtering and washing, generates yellow green liquid
Then body and black residue are filtered and dry to black residue, obtain waste material；Li ion and Fe ion rubs in waste material
That ratio shows the significant loss for not having metal in LiFePO4 powder close to 1: 1.
For operation conditions optimization, so that a series of experiment has been carried out, the influence of these factors of integrated survey.Wherein survey
The analysis method for determining lithium ion and iron ion total amount is that waste material is dissolved completely in in the solution of dense HNO3 and dense HCl (dense HNO3
With the molar ratio of dense HCl: 1:3), dissolution digest waste material after, with Inductively coupled plasma atomic emission sperctrometry Li
The total amount of ion and Fe ion.
Influence of the concentration of oxalic acid to leaching rate, within the scope of 0.1~1.5 mol/L of concentration of oxalic acid, 80 DEG C of bath temperature, anti-
Between seasonable in the condition of 60min, 60 g/L of solid-to-liquid ratio, influence of the concentration of oxalic acid to leaching rate is had studied.As shown in Figure 1, with
The leaching rate of the increase of concentration of oxalic acid, Li ion dramatically increases, and 98% is reached in 0.3 mol/L, then 0.3mol/L~
Stablize between 1.25mol/L 98%, then 86% is dropped in 1.5mol/L leaching rate, this is because solution middle and high concentration ion
Resistance and cause.Meanwhile most of Fe ion releasing, the leaching rate of Fe ion are lower than Li ion.Oxalic acid can provide proton
Metal is leached with acidic group free radical, with the increase of concentration, more protons can be discharged to promote the dissolution of LiFePO4,
Meanwhile ferrous ion can generate ferrous oxalate by oxalic acid precipitation.In view of from leachate separate Li and Fe it is subsequent from
Reason, needs higher Li and low Fe leaching rate, therefore, the suitable of concentration of oxalic acid is selected as 0.3 mol/L.
The influence of Leach reaction temperature and reaction time to leaching rate, Fig. 2 and Fig. 3 show Leach reaction temperature and reactions
Time is 0.3 mol/L to concentration of oxalic acid, the influence that solid-to-liquid ratio is leaching efficiency under the conditions of 60 g/L.See Fig. 2, Li ion
Leaching rate increases with the increase in temperature and reaction time, obviously increases when starting, and then keeps stablizing, the reaction time gets over
Long, oxalic acid solution can more be mixed with LiFePO4 powder, promote solid-liquid reaction.See Fig. 3, the reaction time is to Fe ion leaching rate
Influence very little, be maintained at 8.3% or so, do not fluctuate significantly, when reaction after sixty minutes, when temperature is increased to 70 DEG C from 40 DEG C
When, the leaching rate of Li ion is increased to 98.7% by 93%, and when temperature is more than 70 DEG C, leaching rate keeps stablizing, on the contrary, Fe ion
Leaching rate decline.Higher temperature successfully activating reaction object, to accelerate to react, this is mainly due to the endothermic reaction.This
Outside, since the degree of ionization of oxalic acid increases, influence ratio Li ion of the temperature to Fe ion is big, at a higher temperature, release
More oxalate ions are to form precipitating with Fe ionic reaction.Additionally, due to extraction temperature improve 10 DEG C (from 80 DEG C to
90 DEG C), 1% leaching rate is improved only, considers that leaching efficiency and energy consumption, the suitable of Leach reaction temperature are selected as 80 DEG C,
The suitable selection in reaction time 60 minutes.
Influence of the solid-to-liquid ratio to leaching rate, in 0.3 mol/L of concentration of oxalic acid, 80 DEG C of bath temperature, reaction time 60min
In condition, the influence that leaching rate is compared from the different solid of 10~90g/L is studied.As shown in figure 4, with the increase of solid-to-liquid ratio,
The leaching rate of Li ion and Fe ion reduces.In fact, when solid-to-liquid ratio increases to 60 g/L from 10 g/L, the leaching of Li ion
Rate remains unchanged, and about 97%, decline between 60 g/L and 90 g/L.The photon amount of reaction is bigger, and leaching rate is got over
High solid-to-liquid ratio is bigger.When solid-to-liquid ratio is increased to 50 g/L from 10 g/L, the leaching rate of Fe ion is reduced；In conclusion solid
Influence of the liquor ratio to Fe ion in useless LiFePO4 and Li ion leaching rate rests on 8% left side when solid-to-liquid ratio is greater than 50 g/L
The right side, under the conditions of low solid-to-liquid ratio, the high reason of Fe ion leaching rate is molten due to excessive oxalic acid solution mesoxalic acid ferrous precipitation
Solution.Obviously, the suitable of solid-to-liquid ratio is selected as 60 g/L, and the yield to Li ion and Fe ion is best.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. the recovery method of elemental lithium in a kind of waste phosphoric acid lithium iron battery anode, it is characterised in that: specifically included following steps:
(1), positive electrode is separated from waste and old ferric phosphate lithium cell, positive electrode is soaked in 100 DEG C of N- methyl
1 h in pyrrole network alkanone, so that the positive active material in positive electrode is kept completely separate with aluminum substrate, after then impregnating reaction
Positive electrode takes out and is dried to obtain the LiFePO4 powder containing impurity, by the LiFePO4 powder containing impurity at 400 DEG C
Calcining 1 hour, is finally ground to obtain LiFePO4 powder；
(2), the oxalic acid solution of LiFePO4 powder and 0.1~1.5 mol/L are matched simultaneously by the solid-to-liquid ratio of 10~90g/L
It is put into reactor, then reactor is placed under 40-90 DEG C of bath temperature and carries out Leach reaction, after Leach reaction,
After filtering and washing, yellow green liquid and black residue are generated, then black residue is filtered and is dried, is obtained
Waste material.
2. the recovery method of elemental lithium in a kind of waste phosphoric acid lithium iron battery anode according to claim 1, it is characterised in that:
The concentration of the oxalic acid solution is 0.3mol/L.
3. the recovery method of elemental lithium in a kind of waste phosphoric acid lithium iron battery anode according to claim 1, it is characterised in that:
The bath temperature is 80 DEG C.
4. the recovery method of elemental lithium in a kind of waste phosphoric acid lithium iron battery anode according to claim 1, it is characterised in that:
The solid-to-liquid ratio of the LiFePO4 powder and oxalic acid solution is 60g/L.
5. the recovery method of elemental lithium in a kind of waste phosphoric acid lithium iron battery anode according to claim 1, it is characterised in that:
The time of the Leach reaction is -120 minutes 10 minutes.
6. the recovery method of elemental lithium in a kind of waste phosphoric acid lithium iron battery anode according to claim 5, it is characterised in that:
The time of the Leach reaction is 60 minutes.
7. the recovery method of elemental lithium in a kind of waste phosphoric acid lithium iron battery anode according to claim 1, it is characterised in that:
The reactor of the step (2) selects three neck round bottom reactor, equipped with impeller magnetic on three neck round bottom reactor
Blender is stirred, while being provided with steam condenser to reduce the moisture of evaporation loss.
8. the recovery method of elemental lithium in a kind of waste phosphoric acid lithium iron battery anode according to claim 1, it is characterised in that:
Washing is washed using distilled water in the step (2).
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Cited By (9)
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|---|---|---|---|---|
| CN109687051A (en) * | 2018-12-25 | 2019-04-26 | 云南能投汇龙科技股份有限公司 | A kind of method for recycling anode material of waste and old lithium ion battery |
| CN110459828A (en) * | 2019-08-23 | 2019-11-15 | 贵州红星电子材料有限公司 | Positive material of waste lithium iron phosphate comprehensive recovering process |
| CN111270072A (en) * | 2020-01-19 | 2020-06-12 | 广西师范大学 | Recycling method of waste lithium iron phosphate battery positive electrode material |
| CN111822140A (en) * | 2020-06-16 | 2020-10-27 | 合肥国轩电池材料有限公司 | Recovery method of waste soft package lithium battery |
| CN113264821A (en) * | 2021-04-29 | 2021-08-17 | 广东邦普循环科技有限公司 | Recovery method and application of lithium iron phosphate waste |
| CN113353909A (en) * | 2021-05-31 | 2021-09-07 | 蜂巢能源科技有限公司 | Method for preparing lithium iron phosphate cathode material by utilizing recovered lithium |
| CN113913615A (en) * | 2021-09-23 | 2022-01-11 | 北京理工大学前沿技术研究院 | Method for selectively recovering valuable metals of waste lithium iron phosphate batteries |
| CN113991204A (en) * | 2021-10-22 | 2022-01-28 | 国网黑龙江省电力有限公司电力科学研究院 | Short-process recovery method of waste lithium iron phosphate anode material |
| CN114196821A (en) * | 2021-12-01 | 2022-03-18 | 国网黑龙江省电力有限公司电力科学研究院 | Efficient leaching method of waste lithium iron phosphate cathode material |
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| CN108218690A (en) * | 2018-01-20 | 2018-06-29 | 湖南省正源储能材料与器件研究所 | A kind of method that waste lithium iron phosphate anode material prepares the oxalates of lithium |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109687051A (en) * | 2018-12-25 | 2019-04-26 | 云南能投汇龙科技股份有限公司 | A kind of method for recycling anode material of waste and old lithium ion battery |
| CN110459828A (en) * | 2019-08-23 | 2019-11-15 | 贵州红星电子材料有限公司 | Positive material of waste lithium iron phosphate comprehensive recovering process |
| CN110459828B (en) * | 2019-08-23 | 2022-08-30 | 贵州红星电子材料有限公司 | Comprehensive recovery method of waste lithium iron phosphate battery positive electrode material |
| CN111270072A (en) * | 2020-01-19 | 2020-06-12 | 广西师范大学 | Recycling method of waste lithium iron phosphate battery positive electrode material |
| CN111822140B (en) * | 2020-06-16 | 2021-12-17 | 合肥国轩电池材料有限公司 | Recovery method of waste soft package lithium battery |
| CN111822140A (en) * | 2020-06-16 | 2020-10-27 | 合肥国轩电池材料有限公司 | Recovery method of waste soft package lithium battery |
| CN113264821A (en) * | 2021-04-29 | 2021-08-17 | 广东邦普循环科技有限公司 | Recovery method and application of lithium iron phosphate waste |
| CN113264821B (en) * | 2021-04-29 | 2023-05-05 | 广东邦普循环科技有限公司 | Recovery method and application of lithium iron phosphate waste |
| CN113353909A (en) * | 2021-05-31 | 2021-09-07 | 蜂巢能源科技有限公司 | Method for preparing lithium iron phosphate cathode material by utilizing recovered lithium |
| CN113353909B (en) * | 2021-05-31 | 2024-03-26 | 蜂巢能源科技有限公司 | Method for preparing lithium iron phosphate positive electrode material by utilizing recovered lithium |
| CN113913615A (en) * | 2021-09-23 | 2022-01-11 | 北京理工大学前沿技术研究院 | Method for selectively recovering valuable metals of waste lithium iron phosphate batteries |
| CN113991204A (en) * | 2021-10-22 | 2022-01-28 | 国网黑龙江省电力有限公司电力科学研究院 | Short-process recovery method of waste lithium iron phosphate anode material |
| CN114196821A (en) * | 2021-12-01 | 2022-03-18 | 国网黑龙江省电力有限公司电力科学研究院 | Efficient leaching method of waste lithium iron phosphate cathode material |
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Application publication date: 20181218 |
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