CN109921121A - A kind of method that waste and old saggar recycles anode material of lithium battery automatically - Google Patents
A kind of method that waste and old saggar recycles anode material of lithium battery automatically Download PDFInfo
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- CN109921121A CN109921121A CN201910120316.7A CN201910120316A CN109921121A CN 109921121 A CN109921121 A CN 109921121A CN 201910120316 A CN201910120316 A CN 201910120316A CN 109921121 A CN109921121 A CN 109921121A
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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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Abstract
The invention discloses a kind of methods that waste and old saggar recycles anode material of lithium battery automatically, which comprises the following steps: S1 crushes waste lithium cell, obtains positive plate；Positive plate is put into waste and old saggar, is calcined by S2；S3 grinds the material in waste and old saggar with grinder；Positive electrode after grinding is placed on forging oar furnace by S4 together with waste and old saggar；S5 is put into NaOH solution；S6 is filtered the solution after reaction to obtain filter residue；Filter residue is put into the mixed solution of H2SO4 solution, H2O2, Ni, Co, Mn by S7；Mixed liquor is filtered by S8；NH3H2O, NaOH is added in S9；S10 is filtered after reaction sufficiently；Na2CO3 is added in S11 in filtrate, and positive electrode is obtained by filtration.The present invention takes the technique to carry out the metal in Jiong receipts battery, and the rate of recovery is not less than 95%, and the big fourth 90% of the rate of recovery of positive electrode in waste lithium iron phosphate, feasibility with higher, it is easy to accomplish industrialization.
Description
Technical field
The present invention relates to lithium battery recovery technology fields more particularly to a kind of waste and old saggar to recycle lithium battery anode material automatically
The method of material.
Background technique
It by lithium metal or lithium alloy is negative electrode material, using the battery of non-aqueous electrolytic solution that " lithium battery ", which is a kind of,.
Lithium metal battery is proposed and is studied by Gilbert N.Lewis earliest within 1912.When the 1970s,
M.S.Whittingham is proposed and the lithium ion battery that begins one's study.Since the chemical characteristic of lithium metal is very active, so that lithium is golden
Processing, preservation, the use of category, it is very high to environmental requirement.So lithium battery is not applied for a long time.With science and technology
Development, present lithium battery has become mainstream.
According to statistics, the consumption figure of whole world lithium ion battery in 2000 is 500,000,000, has reached 7,000,000,000 within 2015.Due to
The service life of lithium ion battery be it is limited, a large amount of waste and old lithium ion battery also generates therewith, brings environmental pollution therewith.
Cell positive material cost occupies 1/3 or more single battery cost, and since cathode uses the carbon materials such as graphite at present
Expect it is more, lithium titanate Li4Ti5O12 and silicon-carbon cathode S i/C using less, so the recovery technology of current battery mainly for
Be cell positive material recycling.
The prior art, cell positive material recovery difficult is big, rate of recovery bottom, at high cost, and removal process is complicated, operation difficulty
Greatly, and it be easy to cause environmental pollution.
Summary of the invention
The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of waste and old saggar proposed returns automatically
The method for receiving anode material of lithium battery.
To achieve the goals above, present invention employs following technical solutions:
A kind of method that waste and old saggar recycles anode material of lithium battery automatically, which comprises the following steps:
S1 crushes waste lithium cell, obtain positive plate and prepare chemical material NaOH solution, H2SO4 solution,
H2O2,Ni,Co,Mn；
Positive plate is put into waste and old saggar by S2, is then put into the seal box filled with H2 and is calcined through waste and old saggar；
S3 takes out waste and old saggar, is ground with grinder to the material in waste and old saggar；
Positive electrode after grinding is placed on forging oar furnace by S4 together with waste and old saggar；
S5 takes out calcined material, is put into NaOH solution, is stirred；
Solution after reaction is filtered to obtain filter residue by S6, and by H2O2, Ni, Co, Mn be put into H2SO4 solution into
Row stirring；
Filter residue is put into the mixed solution of H2SO4 solution, H2O2, Ni, Co, Mn, is stirred by S7；
Mixed liquor is filtered by S8, obtains filter residue and filtrate；
S9 is added NH3H2O, NaOH, is stirred in obtained filtrate；
S10 is filtered after reaction sufficiently, obtains filter residue and filtrate；
Na2CO3 is added in S11 in filtrate, and after reacting sufficiently, positive electrode is obtained by filtration.
Preferably, in the S2, calcination time 1-1.5h, 500-750 DEG C of temperature.
Preferably, in the S3, calcination time 30-55min, 300-500 DEG C of temperature.
Preferably, in the S1, chemical material NaOH solution: H2SO4 solution: H2O2:Ni:Co:Mn proportion is 2:5:3:
0.3:0.3:0.3。
Preferably, in the S5, stirring is stirred with high speed peeler, revolving speed 1500r min-2000r min, when
Between 20-30min.
Preferably, in the S6, positive electrode is dissolved in solution in the form of NaALO2, and filter residue product is obtained after filtering and is
Lithium-iron phosphate active material.
Preferably, in the S7, stirring is stirred with high speed peeler, revolving speed 800r min-1200r min, the time
25-35min。
Preferably, in the S7, product Fe2 (SO4) 3 and Li2SO4 solution are obtained.
Preferably, in the S9, filtrate: the proportion of NH3H2O:NaOH is 3:1:3.
Preferably, in the S10, filter residue is Fe (OH) 3, and in the S11, filtrate and Na2CO3 proportion are 3:1, anode
Material product is Li2CO3 solid.
Compared with prior art, the beneficial effects of the present invention are:
1. the present invention passes through, after being dissolved waste positive with strong acid, NaOH solution is added in solution, in solution
Fe, Li, P04 can be precipitated with precipitation form.The present invention carries out ball milling, drying and calcining, and whole process is placed in inert atmosphere and carries out
Calcining, finally obtains new LiFePO 4 material.
2. the present invention takes the technique to carry out the metal in Jiong receipts battery, the rate of recovery is not less than 95%, and waste and old phosphoric acid
The big fourth 90% of the rate of recovery of positive electrode, feasibility with higher, it is easy to accomplish industrialization in iron lithium.
3. whole process of the present invention it is easy to operate and, and secondary pollution will not be generated.
Detailed description of the invention
Fig. 1 is reaction mechanism figure 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.
A kind of embodiment 1: method that waste and old saggar recycles anode material of lithium battery automatically, which is characterized in that including following
Step: S1 crushes waste lithium cell, obtain positive plate and prepare chemical material NaOH solution, H2SO4 solution, H2O2,
Ni,Co,Mn；Positive plate is put into waste and old saggar by S2, is then put into the seal box filled with H2 and is forged through waste and old saggar
It burns；S3 takes out waste and old saggar, is ground with grinder to the material in waste and old saggar；S4, by the positive electrode after grinding
It is placed on forging oar furnace together with waste and old saggar；S5 takes out calcined material, is put into NaOH solution, is stirred；S6, will be anti-
Solution after answering is filtered to obtain filter residue, and H2O2, Ni, Co, Mn are put into H2SO4 solution and are stirred；S7 will be filtered
Slag is put into the mixed solution of H2SO4 solution, H2O2, Ni, Co, Mn, is stirred；Mixed liquor is filtered by S8, is filtered
Slag and filtrate；S9 is added NH3H2O, NaOH, is stirred in obtained filtrate；S10 is filtered after reaction sufficiently, obtains
To filter residue and filtrate；Na2CO3 is added in S11 in filtrate, and after reacting sufficiently, positive electrode is obtained by filtration.
In the S2, calcination time 1h, 600 DEG C of temperature, in the S3, calcination time 35min, 380 DEG C of temperature, institute
State in S1, chemical material NaOH solution: H2SO4 solution: H2O2:Ni:Co:Mn proportion is 2:5:3:0.3:0.3:0.3, the S5
In, stirring is stirred with high speed peeler, revolving speed 1600r min, in time 20-30min, the S6, positive electrode with
The form of NaALO2 is dissolved in solution, filter residue product is obtained after filtering as lithium-iron phosphate active material, in the S7, stirring is used high
Fast peeler is stirred, revolving speed 900r min, in time 25min, the S7, obtain product Fe2 (SO4) 3 and Li2SO4 be molten
Liquid, in the S9, filtrate: the proportion of NH3H2O:NaOH is 3:1:3, and in the S10, filter residue is Fe (OH) 3, in the S11,
Filtrate and Na2CO3 proportion are 3:1, and positive electrode product is Li2CO3 solid.
The filter residue in S8 is taken, and prepares H2SO4 solution, H2O2 mixed solution, filter residue is put into H2SO4 solution, H2O2 is mixed
Close solution in, be stirred with high speed peeler, revolving speed be 600r min, time 25min, obtain 3 He of Fe2 (SO4)
Li2SO4 solution, is filtered, and after insoluble filter residue is filtered, then adds NaOH solution as in filtrate, the iron in filtrate from
Son is reacted with NaOH generates the precipitating of Fe (OH) 3, is measured to the iron of acquisition, and the precipitation capacity of iron reaches 98.7%, in separation iron
Later, lithium carbonate is precipitated with the hot sodium carbonate liquor of saturation, be measured, the primary depositing rate of lithium metal can reach 86.7%.
The present embodiment rate of recovery is high, feasibility with higher, it is easy to accomplish industrialization.
A kind of embodiment 2: method that waste and old saggar recycles anode material of lithium battery automatically, which is characterized in that including following
Step: S1 crushes waste lithium cell, obtain positive plate and prepare chemical material NaOH solution, H2SO4 solution, H2O2,
Ni,Co,Mn；Positive plate is put into waste and old saggar by S2, is then put into the seal box filled with H2 and is forged through waste and old saggar
It burns；S3 takes out waste and old saggar, is ground with grinder to the material in waste and old saggar；S4, by the positive electrode after grinding
It is placed on forging oar furnace together with waste and old saggar；S5 takes out calcined material, is put into NaOH solution, is stirred；S6, will be anti-
Solution after answering is filtered to obtain filter residue, and H2O2, Ni, Co, Mn are put into H2SO4 solution and are stirred；S7 will be filtered
Slag is put into the mixed solution of H2SO4 solution, H2O2, Ni, Co, Mn, is stirred；Mixed liquor is filtered by S8, is filtered
Slag and filtrate；S9 is added NH3H2O, NaOH, is stirred in obtained filtrate；S10 is filtered after reaction sufficiently, obtains
To filter residue and filtrate；Na2CO3 is added in S11 in filtrate, and after reacting sufficiently, positive electrode is obtained by filtration.
In the S2, calcination time 1-1.5h, 550 DEG C of temperature, in the S3, calcination time 40min, temperature 600
DEG C, in the S1, chemical material NaOH solution: H2SO4 solution: H2O2:Ni:Co:Mn proportion is 2:5:3:0.3:0.3:0.3,
In the S5, stirring is stirred with high speed peeler, revolving speed 1600r min, in time 26min, the S6, positive electrode
It is dissolved in solution in the form of NaALO2, filter residue product is obtained after filtering as lithium-iron phosphate active material, in the S7, stirring is used
High speed peeler is stirred, revolving speed 900r min, in time 30min, the S7, obtain product Fe2 (SO4) 3 and Li2SO4
Solution, in the S9, filtrate: the proportion of NH3H2O:NaOH is 3:1:3, and in the S10, filter residue is Fe (OH) 3, the S11
In, filtrate and Na2CO3 proportion are 3:1, and positive electrode product is Li2CO3 solid.
The present embodiment whole process it is easy to operate and, and secondary pollution will not be generated, low energy consumption in removal process.
The present invention passes through, and after being dissolved waste positive with strong acid, NaOH solution is added in solution, in solution
Fe, Li, P04 can be precipitated with precipitation form.The present invention carries out ball milling, drying and calcining, and whole process is placed in inert atmosphere and carries out
Calcining, finally obtains new LiFePO 4 material.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of method that waste and old saggar recycles anode material of lithium battery automatically, which comprises the following steps:
S1 crushes waste lithium cell, obtain positive plate and prepare chemical material NaOH solution, H2SO4 solution, H2O2, Ni,
Co,Mn；
Positive plate is put into waste and old saggar by S2, is then put into the seal box filled with H2 and is calcined through waste and old saggar；
S3 takes out waste and old saggar, is ground with grinder to the material in waste and old saggar；
Positive electrode after grinding is placed on forging oar furnace by S4 together with waste and old saggar；
S5 takes out calcined material, is put into NaOH solution, is stirred；
Solution after reaction is filtered to obtain filter residue, and H2O2, Ni, Co, Mn is put into H2SO4 solution and stirred by S6
It mixes；
Filter residue is put into the mixed solution of H2SO4 solution, H2O2, Ni, Co, Mn, is stirred by S7；
Mixed liquor is filtered by S8, obtains filter residue and filtrate；
S9 is added NH3H2O, NaOH, is stirred in obtained filtrate；
S10 is filtered after reaction sufficiently, obtains filter residue and filtrate；
Na2CO3 is added in S11 in filtrate, and after reacting sufficiently, positive electrode is obtained by filtration.
2. the method that a kind of waste and old saggar according to claim 1 recycles anode material of lithium battery automatically, which is characterized in that
In the S2, calcination time 1-1.5h, 500-750 DEG C of temperature.
3. the method that a kind of waste and old saggar according to claim 1 recycles anode material of lithium battery automatically, which is characterized in that
In the S3, calcination time 30-55min, 300-500 DEG C of temperature.
4. the method that a kind of waste and old saggar according to claim 1 recycles anode material of lithium battery automatically, which is characterized in that
In the S1, chemical material NaOH solution: H2SO4 solution: H2O2:Ni:Co:Mn proportion is 2:5:3:0.3:0.3:0.3.
5. the method that a kind of waste and old saggar according to claim 1 recycles anode material of lithium battery automatically, which is characterized in that
In the S5, stirring is stirred with high speed peeler, revolving speed 1500r min-2000r min, time 20-30min.
6. the method that a kind of waste and old saggar according to claim 1 recycles anode material of lithium battery automatically, which is characterized in that
In the S6, positive electrode is dissolved in solution in the form of NaALO2, and it is LiFePO4 active matter that filter residue product is obtained after filtering
Matter.
7. the method that a kind of waste and old saggar according to claim 1 recycles anode material of lithium battery automatically, which is characterized in that
In the S7, stirring is stirred with high speed peeler, revolving speed 800r min-1200r min, time 25-35min.
8. the method that a kind of waste and old saggar according to claim 1 recycles anode material of lithium battery automatically, which is characterized in that
In the S7, product Fe2 (SO4) 3 and Li2SO4 solution are obtained.
9. the method that a kind of waste and old saggar according to claim 1 recycles anode material of lithium battery automatically, which is characterized in that
In the S9, filtrate: the proportion of NH3H2O:NaOH is 3:1:3.
10. the method that a kind of waste and old saggar according to claim 1 recycles anode material of lithium battery automatically, feature exist
In in the S10, filter residue is Fe (OH) 3；In the S11, filtrate and Na2CO3 proportion are 3:1, and positive electrode product is
Li2CO3 solid.
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Cited By (2)
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| CN110422832A (en) * | 2019-07-19 | 2019-11-08 | 南安市淇凯工业设计有限公司 | A kind of lithium iron phosphate battery positive material waste and old baking sagger smashing and grinding equipment |
| WO2021174348A1 (en) * | 2020-03-02 | 2021-09-10 | Li-Cycle Corp. | A method for processing lithium iron phosphate batteries |
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| CN108923090A (en) * | 2018-05-29 | 2018-11-30 | 深圳市德方纳米科技股份有限公司 | A method of carbon-coated lithium iron manganese phosphate anode material is prepared from waste lithium iron phosphate battery recycling |
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Application publication date: 20190621 |