CN105024048A - Anode material for lithium-ion battery and preparation method of anode material - Google Patents
Anode material for lithium-ion battery and preparation method of anode material Download PDFInfo
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- CN105024048A CN105024048A CN201410178767.3A CN201410178767A CN105024048A CN 105024048 A CN105024048 A CN 105024048A CN 201410178767 A CN201410178767 A CN 201410178767A CN 105024048 A CN105024048 A CN 105024048A
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- porous charcoal
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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
Abstract
The invention relates to an anode material for a lithium-ion battery. Porous carbon is prepared with pig bones abandoned after meals as raw materials, chromium-contained waste water is adsorbed through the porous carbon, and porous carbon compounds which have adsorbed harmful substances are used for preparing the anode material for the lithium-ion battery. The designed porous carbon purifies the chromium-contained waste water, the porous carbon which adsorbs chromium is used for preparing the anode material for the lithium-ion battery, and therefore the chromium-contained waste water purified through the porous carbon can be fully used, and the green and environment-friendly properties of the process are achieved. The battery has the high specific capacity, and therefore porous carbon adsorbent is effectively utilized, and meanwhile the anode material is expected to become a new material for lithium battery anode development.
Description
Technical field
The invention belongs to energy field, be specifically related to a kind of lithium ion battery negative material utilizing the remaining discarded pig bone of meal to prepare for raw material.
Background technology
The reserves of chromium in the earth's crust ranked tenth position, its content different along with the difference of region (1-2000mg/kg).It is mainly for the manufacture of industrial circle, and the whole world is the annual nearly millions of tons of chromite produced only.Alloy containing chromium can increase the mechanical performance of metal, as increased its tensile strength and hardness, can also improve the wear-resisting of metal and corrosion resistance.Manufacturing in the process containing chromium product, people exacerbate irrational discharge (as air, water and soil) of chromium in environment, cause the severe contamination of human environment.Wherein, one of the most serious is exactly the water pollutions caused.According to statistics, 600,000 tons, the chromium waste material that China discharges every year, the amount of process or comprehensive utilization of passing through is less than 17%(Liu Wan, Li Zeqin. the progress [J] that in water, pollution of chromium is administered. Guangdong trace element science, 2007, 14 (9): 5-9), the chromium waste liquid wherein produced from chromium plating factory pollutes comparatively serious, as needed outwardly to discharge a large amount of chromium sewage in the process changing electroplate liquid, other chemical plant is used for the same chromium containing high level in the recirculated water of cooling effect, the environment that these high concentration chrome wastewater severe contaminations mankind depend on for existence, everybody the common target [Yang Lu paid close attention to has been become with prevention pollution of chromium so remove, Hu Cheng. chromium pollution water recovery technique progress [J]. Guangxi light industry, 2008, 7:96-97].
In environment, the main chromium valence state existed comprises for Cr (VI) and Cr (III).Because Cr (VI) has higher water-soluble and mobility and strong oxidizability relative to Cr (III), make the toxicity ratio Cr (III) of Cr (VI) want high a lot, it is reported its toxicity the chances are 100 times of Cr (III).Research shows, sucks the material containing Cr (VI), can cause asthma, tracheitis, pneumonia, causes throat's inflammation, causes liver inflammation, strengthens the probability suffering from Bronchopneumonia and cancer.1ug/cm is greater than in chromic acid concentration
3environment under, if the staff of Long Term Contact chromic acid (chromic compound), be easy to cause nasal allergy; And often contact chromic acid concentration and be greater than 201ug/cm
3time, then cause nasal perforation.In addition, chromic acid can produce skin to stimulate and induced ulcer, cause formation (the Medeiros M G of " chrome aperture " and scar, Rodrigues A S, Batoreu, M C, et al. Elevated levels of DNA-protein crosslinks and micronuclei in peripheral lymphocytes of tannery workers exposed to trivalent chromium [J]. Mutagenesis, 2003,18:19; Costa M. Toxicity and carcinogenicity of Cr (VI) in animal models and humans [J]. Crit Rev Toxicol., 1,997 27 (5): 431-42; Beyersmann D, Hartwig A. Carcinogenic metal compounds:recent insight into molecular and cellular mechanisms [J]. Arch Toxicol., 2008,82 (8): 493-512).At present, cause the source of Cr (VI) water pollution mainly to comprise chromium plating, chemistry manufactures and wet cooling tower.In addition, the burning of coal and oil also can produce chromium (1700 tonnes/annual), and wherein only have an appointment 2% for Cr (III), all the other major parts are Cr (VI).
Porous charcoal is widely used, and its function is constantly developed, and particularly pore diameter range has caused the extensive concern of scientific circles at nano level porous carbon material.As having excellent absorption property, be therefore used for the field of Environment Protection such as air, sewage purification by as cleanser; Meanwhile, porous carbon material also plays an important role in energy storage field because it has good electric conductivity, and it is the important materials of the aspects such as ultracapacitor, lithium ion battery and biology sensor.By porous charcoal to purification of waste water process time, harmful ion is adsorbed onto in porous charcoal by it, but purification after porous charcoal desorption recycling also become a key issue.How efficiently to address this problem the attention always attracting a lot of people.
The present invention design porous charcoal purifying chromium-containing wastewater and Adsorption of Chromium after porous charcoal for the preparation of lithium ion battery negative, porous charcoal purifying chromium-containing wastewater afterproduct is fully utilized, achieves the environmental protection of technique.Battery obtains higher specific capacity, and this not only makes porous carbon adsorbent obtain effective utilization, is also expected to the new material for cathode of lithium battery exploitation simultaneously.
Summary of the invention
The invention provides a kind of lithium ion battery negative material, the remaining discarded pig bone of meal is utilized to prepare porous charcoal for raw material, utilize porous charcoal to adsorb the waste water containing chromium, then the porous charcoal compound having adsorbed harmful substance is used for the preparation of the negative material of lithium ion battery.
The preparation method of lithium ion battery negative material provided by the invention comprises the steps:
(1) porous charcoal preparation
Remaining for meal discarded pig bone is cleaned, then pulverizes oven dry, calcining; To be cooled to room temperature, obtain product black powder stand-by; Get activation of potassium hydroxide agent and black powder Homogeneous phase mixing; Then mixture is put into high temperature furnace and keep a period of time, after being then cooled to room temperature, removing the inorganic matter in activator and bone by Diluted Acid Washing, then be washed till neutrality with deionized water, dry, namely obtain product porous charcoal.
(2) preparation of the porous charcoal of adsorption cleaning chromate waste water
Get finite concentration and be placed in reactor containing the waste water of Cr (VI), regulate different pH, add porous charcoal and adsorb, get a certain amount of supernatant liquor, measure chromium content, filter the solid obtained and dry stand-by;
(3) preparation of cathode pole piece
The porous charcoal of Adsorption of Chromium ion, acetylene black are placed in vacuum drying chamber drying, then the porous charcoal of Adsorption of Chromium ion, acetylene black, binder are mixed to form slurry by a certain percentage, on copper foil of affluxion body, obtain cathode pole piece with scraper for coating, dry.
In a preferred embodiment of the invention, the calcining in step (1) is 400-600 under nitrogen protection
oCcalcining 1-3 hour; Be more preferably 450
oCcalcining 1-3 hour; High temperature furnace is electric tube furnace, under nitrogen protection in 600-900
o1-3 hour is kept under C; More preferably pull out is 850
okeep 1 hour under C.
In a preferred embodiment of the invention, the mass ratio of activation of potassium hydroxide agent and black powder is 1:2-2:1; Be more preferably 1.
In a preferred embodiment of the invention, the adsorption time of step (2) is greater than 24h.
In a preferred embodiment of the invention, in step (3), binder adopts gelatin, and gelatin solution is placed in 60 DEG C of waters bath with thermostatic control and first dissolves, and the concentration of preferred gelatin is 2%.
In a preferred embodiment of the invention, in step (3), the mass ratio of porous charcoal, acetylene black, binder is 80:10:10, and its hand mill 2-3h is formed the slurry mixed.
In a preferred embodiment of the invention, in step (3), cathode pole piece is placed in the dry 12-18h of vacuum drying chamber.
The present invention also protects the application of the above-mentioned lithium ion battery negative material prepared in cell manufacturing process.
The invention provides the battery adopting the above-mentioned lithium ion battery negative material prepared to prepare, with lithium sheet for positive pole, barrier film adopts Celgard2400,1M LiPF
6being dissolved in EC/DEC (V:V=1:1) solution is electrolyte, is assembled into battery.
Beneficial effect of the present invention is:
(1) the remaining pig bone of dining can prepare the porous charcoal of high absorption property, the remaining discarded pig bone of meal is fully utilized, and the preparation technology of porous charcoal is simplified, energy-conserving and environment-protective;
(2) porous charcoal prepared to containing chromic waste water absorption property higher than current commercially available active carbon, be expected to the cleanser of the high concentration chrome wastewater becoming excellent performance;
(3) utilize porous charcoal to adsorb the waste water containing chromium, not only make industrial chromium-containing waste water be purified, the porous charcoal compound having adsorbed harmful substance is used for the positive electrode of lithium ion battery simultaneously, save the cost of porous charcoal regeneration and reprocessing;
(4) porous charcoal of adsorbing chromium is demonstrated its feasibility as the research of lithium ion battery negative material, battery obtains higher specific capacity, this not only makes porous carbon adsorbent obtain effective utilization, also be expected to for cathode of lithium battery exploitation new material, for Environmental Protection in China electric automobile provides effectively power simultaneously.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further described:
Fig. 1 is the SEM test result of the porous charcoal that the present invention prepares;
Lithium ion battery voltage-the capacity curve of Fig. 2 to be the porous charcoal of having adsorbed chromium be negative electrode active material.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
The battery performance of this experiment by constant current charge-discharge tester (Land CT2001A) measure and draw.In this experiment, the specific capacity of sample all calculates with the quality of active material in material (namely deducting the quality of C in material).Method of testing: adopt two electrode systems, probe temperature is room temperature, and test voltage scope is 0.005-3 V, and charge and discharge process constant current all uses 50mA/g.The Characterization of The Products of this experiment adopts the microscopic appearance of the porous charcoal of HIT HITACHI S-4700 type Scanning Electron microscope (SEM) observation experiment gained, adopt the content of spectrophotometric determination Cr (VI), and calculate adsorbance.
Embodiment
(1) porous charcoal preparation
Remaining discarded for meal pig bone is cleaned, then pulverizes oven dry, under nitrogen protection 450
oCcalcine 1 hour; To be cooled to room temperature, obtain product black powder stand-by; Get a certain amount of activation of potassium hydroxide agent and black powder Homogeneous phase mixing, both mass ratioes are 1:1; Then mixture is put into high temperature furnace, in 850 under nitrogen protection
okeep 1 hour under C, after being cooled to room temperature, with dust technology wash-out except the inorganic matter in activator and bone, then being washed till neutrality with deionized water, drying, namely obtain product porous charcoal.
For observing the structure in its hole, carry out the test result of SEM as shown in Figure 1.The porous charcoal of preparation contains abundant nano-pore,
(2) preparation of the porous charcoal of adsorption cleaning chromate waste water
Get finite concentration and be placed in bottle containing the waste water of Cr (VI), add porous charcoal and adsorb, get a certain amount of supernatant liquor, measure chromium content, filter the solid obtained and dry stand-by.
When absorption after 24 hours chromium concn be that the chromate waste water bottle of 100 mg/L becomes colourless, and the color of another bottle (chromium concn is 300mg/L) has also shoaled, and illustrates that porous charcoal has good adsorption capacity to chromium in waste water.After absorption in 48 hours, concentration is that the bottle of 300mg/L also becomes colourless, illustrates that chromium ion wherein adsorbed clean substantially through 48 hours.This illustrates that also not adsorbing of this porous charcoal is saturated, can increase adsorbance further.Comparative study result is carried out as table 1 by producing porous charcoal from the porous charcoal prepared and commercially available Japan.
The result of table 1 shows, under the same conditions, the adsorption capacity of porous charcoal prepared by this experimental design is slightly stronger to chromic adsorption capacity than commercially available active carbon.And in this scope of experiment, along with the increase of chromium solution initial concentration, the amount of absorption increases.
To using initial concentration solution 500mg/L, porous charcoal consumption is 50mg, 27 DEG C of absorption after 48 hours the porous charcoal of having adsorbed chromium that the obtain product after 500 DEG C of calcinings as negative electrode active material to prepare pole piece.
(3) preparation of cathode pole piece
The porous charcoal of Adsorption of Chromium ion, acetylene black are placed in vacuum drying chamber drying, binder adopts gelatin, and the gelatin solution of 2% is placed in 60 DEG C of waters bath with thermostatic control and first dissolves, by the porous charcoal of Adsorption of Chromium ion, acetylene black, binder in mass ratio for 80:10:10 is mixed to form slurry, its hand mill 2-3h is formed the slurry mixed, on copper foil of affluxion body, obtain cathode pole piece with scraper for coating, cathode pole piece is placed in the dry 12h of vacuum drying chamber.
(4) assembling of battery
Using above-mentioned obtained material as negative pole, with lithium sheet for positive pole, barrier film adopts Celgard2400, it is electrolyte that 1M LiPF6 is dissolved in EC/DEC (V:V=1:1) solution, is assembled into battery, tests its charge status, result as shown in Figure 2, visible this porous charcoal can as the active material of lithium ion battery negative, and specific discharge capacity of first three circulation is higher, is about 800 mAh/g.
Electrochemical Properties finds, the porous charcoal of Adsorption of Chromium has good stability as negative material, remaining for meal discarded pig bone is used for the preparation of lithium ion battery to the porous charcoal obtained after chromate waste water purification, the porous charcoal also for adsorbing chromium has opened up new application direction.
Above embodiment display and describe general principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification just illustrates principle of the present invention; instead of limit the scope of the invention by any way; without departing from the scope of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in claimed scope.
Claims (10)
1. a lithium ion battery negative material, it is characterized in that, utilize the remaining discarded pig bone of meal to prepare porous charcoal for raw material, utilize porous charcoal to adsorb waste water containing chromium, then the porous charcoal compound having adsorbed harmful substance is used for the preparation of the negative material of lithium ion battery.
2. the preparation method of material according to claim 1, is characterized in that, comprises the steps:
(1) porous charcoal preparation
Remaining for meal discarded pig bone is cleaned, then pulverizes oven dry, calcining; To be cooled to room temperature, obtain product black powder stand-by; Get activation of potassium hydroxide agent and black powder Homogeneous phase mixing; Then mixture is put into high temperature furnace and keep a period of time, after being then cooled to room temperature, removing the inorganic matter in activator and bone by Diluted Acid Washing, then be washed till neutrality with deionized water, dry, namely obtain product porous charcoal;
(2) preparation of the porous charcoal of adsorption cleaning chromate waste water
Get finite concentration and be placed in reactor containing the waste water of Cr (VI), regulate different pH, add porous charcoal and adsorb, get a certain amount of supernatant liquor, measure chromium content, filter the solid obtained and dry stand-by;
(3) preparation of cathode pole piece
The porous charcoal of Adsorption of Chromium ion, acetylene black are placed in vacuum drying chamber drying, then the porous charcoal of Adsorption of Chromium ion, acetylene black, binder are mixed to form slurry by a certain percentage, on copper foil of affluxion body, obtain cathode pole piece with scraper for coating, dry.
3. the preparation method of material according to claim 2, is characterized in that, the calcining in step (1) is 400-600 under nitrogen protection
oCcalcining 1-3 hour; High temperature furnace is electric tube furnace, under nitrogen protection in 600-900
o1-3 hour is kept under C.
4. the preparation method of material according to claim 2, is characterized in that, the mass ratio of activation of potassium hydroxide agent and black powder is 1:2-2:1.
5. the preparation method of material according to claim 2, is characterized in that, the adsorption time of step (2) is greater than 24h.
6. the preparation method of material according to claim 2, is characterized in that, in step (3), binder adopts gelatin, and gelatin solution is placed in 60 DEG C of waters bath with thermostatic control and first dissolves, and wherein the concentration of gelatin is 2%.
7. the preparation method of material according to claim 2, is characterized in that, in step (3), the mass ratio of porous charcoal, acetylene black, binder is 80:10:10, and its hand mill 2-3h is formed the slurry mixed.
8. the preparation method of material according to claim 2, is characterized in that, in step (3), cathode pole piece is placed in the dry 12-18h of vacuum drying chamber.
9. according to the application of lithium ion battery negative material in cell manufacturing process that the preparation method of any one of claim 2-8 prepares.
10. a lithium ion battery, is characterized in that, adopt lithium ion battery negative material that the preparation method of any one of claim 2-8 prepares as negative pole, with lithium sheet for positive pole, barrier film adopts Celgard2400,1M LiPF
6being dissolved in EC/DEC (V:V=1:1) solution is electrolyte, is assembled into battery.
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Cited By (3)
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| CN107134566A (en) * | 2017-04-20 | 2017-09-05 | 浙江工业大学 | The method for preparing lithium ion battery negative material using iron content solid waste obtained by electric flocculation dyeing waste water |
| CN107959010A (en) * | 2017-11-14 | 2018-04-24 | 中航锂电（洛阳）有限公司 | A kind of graphite composite material and preparation method thereof |
| WO2018227535A1 (en) * | 2017-06-12 | 2018-12-20 | 黎烈武 | Energy storage material prepared by using active sludge and method therefor and applications thereof |
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| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| CN101993068A (en) * | 2010-10-27 | 2011-03-30 | 北京化工大学 | Preparation method of porous structured active carbon |
| CN103420353A (en) * | 2012-05-15 | 2013-12-04 | 北京化工大学 | Porous carbon material and preparation method and application thereof |
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2014
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| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| CN101993068A (en) * | 2010-10-27 | 2011-03-30 | 北京化工大学 | Preparation method of porous structured active carbon |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107134566A (en) * | 2017-04-20 | 2017-09-05 | 浙江工业大学 | The method for preparing lithium ion battery negative material using iron content solid waste obtained by electric flocculation dyeing waste water |
| WO2018227535A1 (en) * | 2017-06-12 | 2018-12-20 | 黎烈武 | Energy storage material prepared by using active sludge and method therefor and applications thereof |
| CN107959010A (en) * | 2017-11-14 | 2018-04-24 | 中航锂电（洛阳）有限公司 | A kind of graphite composite material and preparation method thereof |
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Application publication date: 20151104 |