CN105439137A - Method for preparing graphene by using anode material of waste aluminum ion secondary battery - Google Patents
Method for preparing graphene by using anode material of waste aluminum ion secondary battery Download PDFInfo
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- CN105439137A CN105439137A CN201610005984.1A CN201610005984A CN105439137A CN 105439137 A CN105439137 A CN 105439137A CN 201610005984 A CN201610005984 A CN 201610005984A CN 105439137 A CN105439137 A CN 105439137A
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- Prior art keywords
- electrolysis
- ion secondary
- aluminum ion
- graphene
- battery
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- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- 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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
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Abstract
The invention relates to a method for preparing graphene by using an anode material of a waste aluminum ion secondary battery, being an efficient method for recycling the anode material graphite of a waste aluminum ion battery, and belonging to the fields of waste battery recycling and advanced material preparation. According to the method, the waste aluminum ion battery taking a graphite structure material as an anode is used, and the graphite anode of the waste battery is directly changed into the graphene to be recycled in an electrolytic way; a principle of the method is that aluminum complex ions in ionic liquid are enabled to be continuously embedded into a carbon layer under high potential, a layered structure of the graphite is further cracked, and the high value-added graphene is produced.
Description
Technical field
The present invention relates to old and useless battery to reclaim and high end materials preparation field, especially relate to a kind of method utilizing waste aluminum ion secondary battery to prepare Graphene.
Background technology
The strong seminar of Jiao Shu has carried out large quantifier elimination to aluminum ion secondary cell, and propose the negative material adopting aluminum metal, alloy aluminum as aluminum ion secondary cell, graphite type material as positive electrode material, and has applied for multinomial patent.As CN201510188866.4 rechargeable aluminium ionization cell and preparation method thereof; CN201510269862.9 non-aqueous solution aluminum ion secondary cell and preparation method thereof etc.This kind of battery has good cycle performance, and positive and negative pole material price is cheap, and this kind of battery can large-scale application, but how to be reclaimed by the old and useless battery after application be the technical problem that urgently will solve.
At present, there are very many preparation methods about Graphene both at home and abroad, mainly contain physical method and chemical process.Physical method prepares single or multiple lift Graphene by the direct stripping method of micromechanics stripping method, liquid phase or gas phase.Chemical process comprises chemical Vapor deposition process (CVD), crystal epitaxy method (SiC high temperature annealing), oxidation-reduction method etc.And oxidation-reduction method is the main method realizing preparing in enormous quantities Graphene, but this method needs the oxygenant such as the vitriol oil, potassium permanganate, and often can at high temperature carry out, aforesaid method exists potential safety hazard, produces a large amount of waste liquid, causes environmental pollution.
As can be seen here, in order to the Sustainable development of aluminum ion secondary cell, the recovery of its battery is technical problem urgently to be resolved hurrily; Secondly, preparation method's cost of existing Graphene is high, environmental pollution is serious, poor stability.Thus, adopting the positive pole graphite material of electrochemical method to waste aluminum ionization cell carry out electrolysis treatment and obtain the Graphene of high added value, because it is easy and simple to handle, additionally do not add the reasons such as other chemical reagent, is very promising a kind of way of recycling.
Summary of the invention
The object of the invention is to: aluminum ion cell positive material is recycled, utilize the positive electrode material of aluminum ion battery to prepare Graphene, turn waste into wealth.Complete battery provides the passage of electrolysis graphite type material, thus make in the continual embedding graphite linings of the aluminum complex ion in electrolytic solution, the embedding of this lasting coordination ion can make to lose Van der Waals force between nano-carbon layer, so peel off, dispersion, formed Graphene.The method processing step is simple, raw materials cost is low.Very large effect is served to the extensive commercial application of aluminum ion battery and recovery.
For solving the problems of the technologies described above, technical scheme of the present invention is: utilize waste aluminum ion secondary battery positive electrode material to prepare the method for Graphene, comprise the following steps:
Step one. choose raw material: adopt content of graphite to be the positive electrode material of more than 40%, the waste aluminum ion secondary battery containing aluminum complex ion in electrolytic solution, for subsequent use;
Step 2. electrolysis: the waste aluminum ion secondary battery chosen step 1 is filled with continuous current or constant voltage carries out electrolysis, the electrolysis regular hour, is then discharged to 0.3V, then charges, circulate more than 5 times, complete electrolysis, for subsequent use;
Step 3: taken out by the cell positive material processed through step 2 and be placed in the beaker that dehydrated alcohol is housed, cleans, dries, obtain Graphene after removing impurity in air dry oven for ultrasonic echography 20-30 minute.
Further, the current density of described current electroanalysis is 10-500mAg
-1; The voltage of described potential electrolysis is 1.8V-2.7V.
Further, described electrolysis time is 2-60 hour.
Further, described bake out temperature is 50-200 DEG C.
Further, described aluminum complex ion is: [AlCl
4]
-or [Al
2cl
7]
-or the mixture of the two.
Further, the composition of electrolytic solution contains Al
3+the non-aqueous solution of ion, containing Al
3+the non-aqueous solution of ion comprises aluminum halide and ionic liquid, and the negatively charged ion of described ionic liquid comprises F
-, Cl
-, Br
-, I
-, PF
6-, CN
-, SCN
-, [N (CF
3sO
2)]
-or [N (CN)
2]
-ion; Positively charged ion comprises imidazoles drone ion, pyridinium ion, pyrroles's drone ion, piperidines drone ion, morpholine drone ion, quaternary ammonium salt ion, quaternary alkylphosphonium salt ion or tertiary sulfosalt ion.
The invention has the advantages that: the present invention utilizes the aluminum ion battery of graphitiferous material, by containing aluminum complex ion in electrolytic solution under continued electrolysis effect, making coordination ion constantly embed graphite layers, finally make graphite linings disperse to peel off formation Graphene.Its technique is simple, and cost is lower, can reclaim waste aluminum ion secondary battery, environmental protection.The industrial applications of method to aluminum ion battery of this high efficiente callback aluminum ion secondary cell has very large meaning.
Accompanying drawing explanation
Fig. 1 is the graphic representation of electrolytic process under aluminum ion secondary cell 2.3V in embodiment 4.
Fig. 2 is the shape appearance figure of the transmission electron microscope of the graphene product of preparation in embodiment 4.
Fig. 3 is electrolytic process graphic representation under aluminum ion secondary cell 2.0V in embodiment 7.
Embodiment
The present invention will be described in more detail by specific embodiment, but protection scope of the present invention is not limited to these embodiments.
Embodiment 1
The positive electrode material of the aluminum ion secondary cell that the present invention will reclaim is high purity graphite sheet, containing aluminum complex ion in electrolytic solution, by waste aluminum ionization cell constant current (current density 10mAg
-1) charge to 2.3V, then constant-potential electrolysis graphite flake 2 hours under 2.0V, after be discharged to 0.3V, circulate more than 5 times.When pulling down battery, its state is non-discharge condition.By the battery roll of at least five times that circulates, within 20 minutes, cleaned by cell positive material ultrasonic echography, dry in 70 DEG C of air dry ovens after removing impurity, obtaining Graphene ratio is 20%.
Embodiment 2
The positive electrode material of the aluminum ion secondary cell that the present invention will reclaim is high purity graphite sheet, containing aluminum complex ion in electrolytic solution, by waste aluminum ionization cell constant current (current density 100mAg
-1) charge to 2.3V, then constant-potential electrolysis graphite flake 4 hours under 2.5V, after be discharged to 0.3V, circulate more than 5 times.Pull down battery status for non-discharge condition.By the battery roll of at least five times that circulates, within 40 minutes, cleaned by cell positive material ultrasonic echography, dry in 70 DEG C of air dry ovens after removing impurity, obtaining Graphene ratio is 30%.
Embodiment 3
The positive electrode material of the aluminum ion secondary cell that the present invention will reclaim is high purity graphite sheet, containing aluminum complex ion in electrolytic solution, by waste aluminum ionization cell constant current (current density 500mAg
-1) charge to 2.3V, then constant-potential electrolysis graphite flake 6 hours under 2.7V, after be discharged to 0.3V, circulate more than 5 times.Pull down battery status for non-discharge condition.By the battery roll of at least five times that circulates, within 60 minutes, cleaned by cell positive material ultrasonic echography, dry in 70 DEG C of air dry ovens after removing impurity, obtaining Graphene ratio is 35%.
Embodiment 4
The positive electrode material of the aluminum ion secondary cell that the present invention will reclaim is high purity graphite sheet, containing aluminum complex ion in electrolytic solution, by waste aluminum ionization cell constant current (current density 10mAg
-1) charge to 2.3V, then constant-potential electrolysis graphite flake 10 hours under 2.3V, after be discharged to 0.3V, circulate more than 5 times, its electrolysis cycle curve is as Fig. 1.Pull down battery status for non-discharge condition.By the battery roll of at least five times that circulates, within 20 minutes, cleaned by cell positive material ultrasonic echography, remove impurity and dry in 80 DEG C of air dry ovens, obtaining Graphene ratio is 40%.Shown in Fig. 2, the shape appearance figure of the transmission electron microscope (TEM) of the three layer graphene materials that the present invention obtains.
Embodiment 5
The positive electrode material of the aluminum ion secondary cell that the present invention will reclaim is high purity graphite sheet, containing aluminum complex ion in electrolytic solution, by waste aluminum ionization cell constant current (current density 100mAg
-1) charge to 2.3V, then constant-potential electrolysis graphite flake 20 hours under 2.3V, after be discharged to 0.3V, circulate more than 5 times.Pull down battery status for non-discharge condition.By the battery roll of at least five times that circulates, within 40 minutes, cleaned by cell positive material ultrasonic echography, remove impurity and dry in 80 DEG C of air dry ovens, obtaining Graphene ratio is 45%.
Embodiment 6
The positive electrode material of the aluminum ion secondary cell that the present invention will reclaim is high purity graphite sheet, containing aluminum complex ion in electrolytic solution, by waste aluminum ionization cell constant current (current density 200mAg
-1) charge to 2.3V, then constant-potential electrolysis graphite flake 40 hours under 2.3V, after be discharged to 0.3V, circulate more than 5 times.Pull down battery status for non-discharge condition.By the battery roll of at least five times that circulates, within 60 minutes, cleaned by cell positive material ultrasonic echography, remove impurity and dry in 80 DEG C of air dry ovens, obtaining Graphene ratio is 50%.
Embodiment 7
The positive electrode material of the aluminum ion secondary cell that the present invention will reclaim is high purity graphite sheet, containing aluminum complex ion in electrolytic solution, by waste aluminum ionization cell constant current (current density 10mAg
-1) charge to 2.3V, then constant-potential electrolysis graphite flake 10 hours under 2.0V, after be discharged to 0.3V, circulate more than 5 times, its test loop curve is as Fig. 3.Pull down battery status for non-discharge condition.By the battery roll of at least five times that circulates, within 60 minutes, cleaned by cell positive material ultrasonic echography, remove impurity and dry in 120 DEG C of air dry ovens, obtaining Graphene ratio is 40%.
Embodiment 8
The positive electrode material of the aluminum ion secondary cell that the present invention will reclaim is high purity graphite sheet, containing aluminum complex ion in electrolytic solution, by waste aluminum ionization cell constant current (current density 300mAg
-1) charge to 2.3V, then constant-potential electrolysis graphite carbon paper 40 hours under 2.0V, after be discharged to 0.3V.Circulate more than 5 times.Pull down battery status for non-discharge condition.By the battery roll of at least five times that circulates, within 60 minutes, cleaned by cell positive material ultrasonic echography, remove impurity and dry in 120 DEG C of air dry ovens, obtaining Graphene ratio is 50%.
Embodiment 9
The positive electrode material of the aluminum ion secondary cell that the present invention will reclaim is high purity graphite sheet, containing aluminum complex ion in electrolytic solution, by waste aluminum ionization cell constant current (current density 400mAg
-1) charge to 2.3V, then constant-potential electrolysis graphite carbon paper 10 hours under 1.8V, after be discharged to 0.3V.Circulate more than 5 times, its test loop curve is as Fig. 3.Pull down battery status for non-discharge condition.By the battery roll of at least five times that circulates, within 60 minutes, cleaned by cell positive material ultrasonic echography, remove impurity and dry in 120 DEG C of air dry ovens, obtaining Graphene ratio is 35%.
Embodiment 10
The positive electrode material of the aluminum ion secondary cell that the present invention will reclaim is high purity graphite sheet, by waste aluminum ionization cell constant current (current density 500mAg
-1) charge to 2.3V, then constant-potential electrolysis graphite carbon paper 40 hours under 1.8V, after be discharged to 0.3V.Circulate more than 5 times, pull down battery status for non-discharge condition.By the battery roll of at least five times that circulates, within 60 minutes, cleaned by cell positive material ultrasonic echography, remove impurity and dry in 120 DEG C of air dry ovens, obtaining Graphene ratio is 45%.
These are only preferred embodiment of the present invention, limiting technical scope of the invention process when not being able to this, therefore all with reference to description of the present invention do simple equivalence change with modify, all still should belong to protection scope of the present invention.
Claims (5)
1. utilize waste aluminum ion secondary battery positive electrode material to prepare a method for Graphene, it is characterized in that comprising the following steps:
Step one. choose raw material: adopt content of graphite to be the positive electrode material of more than 40%, the waste aluminum ion secondary battery containing aluminum complex ion in electrolytic solution, for subsequent use;
Step 2. electrolysis: the waste aluminum ion secondary battery chosen step 1 is filled with continuous current or constant voltage carries out electrolysis, the electrolysis regular hour, is then discharged to 0.3V, then charges, circulate more than 5 times, complete electrolysis, for subsequent use;
Step 3: taken out by the cell positive material processed through step 2 and be placed in the beaker that dehydrated alcohol is housed, cleans, dries, obtain Graphene after removing impurity in air dry oven for ultrasonic echography 20-30 minute.
2. method according to claim 1, is characterized in that: in described step 2, and the current density of described current electroanalysis is 10-500mAg
-1; The voltage of described potential electrolysis is 1.8V-2.7V.
3. method according to claim 1, is characterized in that: in described step 2, and described electrolysis time is 2-60 hour.
4. method according to claim 1, is characterized in that: in described step 3, and described bake out temperature is 50-200 DEG C.
5. method according to claim 1, is characterized in that: described step is a kind of, and described aluminum complex ion is: [AlCl
4]
-or [Al
2cl
7]
-or the mixture of the two.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610005984.1A CN105439137B (en) | 2016-01-05 | 2016-01-05 | The method that graphene is prepared using the positive electrode of waste aluminum ion secondary battery |
| PCT/CN2016/072875 WO2017117839A1 (en) | 2016-01-05 | 2016-01-29 | Method for preparing graphene by using anode material of waste aluminum-ion secondary battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610005984.1A CN105439137B (en) | 2016-01-05 | 2016-01-05 | The method that graphene is prepared using the positive electrode of waste aluminum ion secondary battery |
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|---|---|
| CN105439137A true CN105439137A (en) | 2016-03-30 |
| CN105439137B CN105439137B (en) | 2018-07-03 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109792095A (en) * | 2016-07-22 | 2019-05-21 | 魁北克电力公司 | The method of graphene is recycled from electrode material |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111403839B (en) * | 2019-12-23 | 2023-04-25 | 余姚市鑫和电池材料有限公司 | Method for recycling electrolyte of retired power lithium battery |
| CN116161651A (en) * | 2023-03-14 | 2023-05-26 | 昆明理工大学 | Preparation method of doped perforated graphene based on waste battery negative electrode graphite |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534643A (en) * | 2012-01-16 | 2012-07-04 | 清华大学深圳研究生院 | Method for regenerating waste battery carbon rods into graphene |
| JP2014001126A (en) * | 2012-05-25 | 2014-01-09 | National Institute For Materials Science | Method for manufacturing separated graphene film |
| CN103693638A (en) * | 2013-12-09 | 2014-04-02 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene by electrochemical swelling of graphite |
| CN104894594A (en) * | 2015-05-26 | 2015-09-09 | 广东烛光新能源科技有限公司 | Graphene preparation method |
| CN104993130A (en) * | 2015-05-25 | 2015-10-21 | 石嘴山市天和创润新材料科技有限公司 | Non-aqueous solution aluminum ion secondary battery and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466603B (en) * | 2013-08-09 | 2016-01-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | The preparation method of graphene dispersing solution and graphene film |
-
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- 2016-01-05 CN CN201610005984.1A patent/CN105439137B/en active Active
- 2016-01-29 WO PCT/CN2016/072875 patent/WO2017117839A1/en active Application Filing
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534643A (en) * | 2012-01-16 | 2012-07-04 | 清华大学深圳研究生院 | Method for regenerating waste battery carbon rods into graphene |
| JP2014001126A (en) * | 2012-05-25 | 2014-01-09 | National Institute For Materials Science | Method for manufacturing separated graphene film |
| CN103693638A (en) * | 2013-12-09 | 2014-04-02 | 中国科学院山西煤炭化学研究所 | Method for preparing graphene by electrochemical swelling of graphite |
| CN104993130A (en) * | 2015-05-25 | 2015-10-21 | 石嘴山市天和创润新材料科技有限公司 | Non-aqueous solution aluminum ion secondary battery and preparation method thereof |
| CN104894594A (en) * | 2015-05-26 | 2015-09-09 | 广东烛光新能源科技有限公司 | Graphene preparation method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109792095A (en) * | 2016-07-22 | 2019-05-21 | 魁北克电力公司 | The method of graphene is recycled from electrode material |
| CN109792095B (en) * | 2016-07-22 | 2022-05-27 | 魁北克电力公司 | Method for recovering graphene from electrode material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105439137B (en) | 2018-07-03 |
| WO2017117839A1 (en) | 2017-07-13 |
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