CN105098183A - Preparation for carbon anode material of lithium ion battery by using rice hull as raw material - Google Patents
Preparation for carbon anode material of lithium ion battery by using rice hull as raw material Download PDFInfo
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- CN105098183A CN105098183A CN201410218426.4A CN201410218426A CN105098183A CN 105098183 A CN105098183 A CN 105098183A CN 201410218426 A CN201410218426 A CN 201410218426A CN 105098183 A CN105098183 A CN 105098183A
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- ion battery
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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
A preparation method for a micropore carbon anode material of a lithium ion battery comprises the following steps of: cleaning and washing agriculture waste rice hull by using distilled water; calcining for 1 to 5 hours in a nitrogen atmosphere at a temperature of 450 to 650 DEG C to obtain a rice hull dry distillate; carrying out acid cooking of the obtained rice hull dry distillate at 50 to 70 DEG C for 0.5 to 2.5 hours in a hydrochloric acid solution with concentration of 0.1M; washing by using the distilled water to neutral, and drying to obtain the rice hull dry distillate subjected to acid treatment; mixing Na2CO3 and the rice hull dry distillate subjected to acid treatment according to a quality rate of (1-5):1, uniformly grinding, placing in a tube furnace, and calcining for 2 to 5 hours in the nitrogen atmosphere at a temperature of 850 to 1,000 DEG C; and repeatedly washing the obtained product by using the distilled water until to remove Na<+> and SiO3<2->, and drying, thereby obtaining the micropore carbon anode material of the lithium ion battery. According to the method, the micropore carbon anode material is finally obtained by dry distillation, acid dipping treatment and alkali heating treatment of the agriculture waste rice hull, raw material is widely available, the experiment process is safe and is easy to implement, the final product is a porous structure, electron transmission and transfer is facilitated, and the micropore carbon anode material is an ideal material for an anode of the lithium ion battery.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery microporous carbon negative material.
Background technology
Lithium ion battery is a kind of novel high-energy secondary power supply, has that specific capacity is large, discharge voltage is high and steady, the advantage such as cryogenic property is good, environmental friendliness, safety, the life-span is long, self discharge is faint.The above-mentioned advantage of lithium ion battery, causes the favor of various countries scientist, thus facilitates the fast development of lithium rechargeable battery.Since appearance, between the short more than ten years, lithium ion battery is just applied in the portable electronic products such as mobile phone, notebook computer, digital camera, some other key areas as the large-scale lithium ion battery in the fields such as electric vehicle, Aero-Space, military affairs also just under development.
The electrode reaction of lithium ion battery comprises the transmission of electronics and the transmission of ion, so just requires that electrode will have good conductivity, and ensure the unimpeded of electron propagation ducts, the pore structure of some necessity, holds electrolyte, ensures the smooth of ion transfer.Only reach the requirement of these two aspects, can ensure that electrode active material has higher utilance and good cyclical stability.
Lithium ion battery negative material remains graphite material in actual applications and occupies an leading position.Delanium and native graphite respectively have merits and demerits as negative material, and Delanium has the advantage of stable circulation, but generally will lower than native graphite on capacity.Although native graphite has the high advantage of capacity, in cyclic process, capacity attenuation is its deadly defect soon.
The present invention is with agricultural wastes rice husk for raw material, and by destructive distillation, the method such as acid treatment, alkali treatment, obtains the amorphous charcoal of microcellular structure, do not need graphitization, utilizes its microcellular structure to carry out embedding lithium/de-lithium.Wide raw material source of the present invention, technique are simple, can reach the requirements as lithium ion battery negative material simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of lithium ion battery microporous carbon negative material.
The present invention proposes with rice husk is the method that microporous carbon lithium ion battery negative material prepared by raw material.
A preparation method for lithium ion battery microporous carbon negative material, comprises the steps:
Agricultural wastes rice husk distilled water is cleaned up, then in a nitrogen atmosphere with the temperature calcination 1 ~ 5 hour of 450 ~ 650 DEG C, obtains rice husk pyrolysate.
Be boil 0.5 ~ 2.5 hour with 50 DEG C ~ 70 DEG C acid in the hydrochloric acid solution of 0.1M at mass fraction by rice husk pyrolysate.Neutrality is washed to distilled water, dry, obtain the rice husk pyrolysate after acid treatment.
By Na
2cO
3with the rice husk pyrolysate after acid treatment according to mass ratio (1 ~ 5): the ratio of 1 mixes, grinding evenly, is placed in tube furnace, calcines 2 ~ 5 hours in a nitrogen atmosphere at 850 ~ 1000 DEG C.With distilled water by gains cyclic washing to removing Na
+ion and SiO
3 2-till, pH value is 7-7.5, dry, obtains lithium ion battery microporous carbon negative material.
Wherein in an embodiment, the described raw material preparing micro-pore carbon material are rice husk.
Wherein in an embodiment, alkali activator is sodium carbonate.
Wherein in an embodiment, pyrolysis temperature is 450 ~ 650 DEG C, and the time is 1 ~ 5 hour.
Wherein in an embodiment, acid treatment temperature is 50 DEG C ~ 70 DEG C, and the time is 0.5 ~ 2.5 hour.
Wherein in an embodiment, activation temperature is 850 ~ 1000 DEG C, and the time is 2 ~ 5 hours.
Said method utilizes the destructive distillation of agricultural wastes rice husk, and through peracid treatment, alkali treatment finally obtains microporous carbon negative material, raw material sources is extensive, and experimentation safety is easily implemented, and end product is loose structure, being easy to conveying and the transfer of electronics, is the ideal material as lithium ion battery negative.
Accompanying drawing illustrates:
Fig. 1 is the preparation flow figure of lithium ion battery microporous carbon negative material
Fig. 2 is the electron scanning micrograph of the micro-pore carbon material of embodiment 1;
Fig. 3 is the transmission electron microscope photo of the micro-pore carbon material of embodiment 1;
Fig. 4 is X-ray diffraction (XRD) collection of illustrative plates of the micro-pore carbon material of embodiment 1;
Fig. 5 is the first charge-discharge curve of the micro-pore carbon material of embodiment 1, and in figure, red colouring agent for food, also used as a Chinese medicine line is specific discharge capacity curve, and black curve is charge specific capacity curve;
Fig. 6 is the cycle performance collection of illustrative plates that the micro-pore carbon material of embodiment 1 makes after button cell under constant current 0.1C condition, and in figure, red colouring agent for food, also used as a Chinese medicine line is discharge cycles specific capacity curve, and black curve is charging cycle specific capacity curve.
Embodiment:
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public concrete enforcement.
Refer to Fig. 1, the preparation method of the lithium ion battery microporous carbon negative material of an execution mode, comprises the steps:
Step S1, cleans up agricultural wastes rice husk distilled water, then in a nitrogen atmosphere with the temperature calcination 1 ~ 5 hour of 450 ~ 650 DEG C, obtains rice husk pyrolysate.
Rice husk pyrolysate is boil 0.5 ~ 2.5 hour with 50 DEG C ~ 70 DEG C acid in the hydrochloric acid solution of 10% ~ 20% at mass fraction by step S2.Neutrality is washed to distilled water, dry, obtain the rice husk pyrolysate after acid treatment.
Step S3, by Na
2cO
3with the rice husk pyrolysate after acid treatment according to mass ratio (1 ~ 5): the ratio of 1 mixes, grinding evenly, is placed in tube furnace, calcines 2 ~ 5 hours in a nitrogen atmosphere at 850 ~ 1000 DEG C.With distilled water by gains cyclic washing to removing Na
+ion and SiO
3 2-till, pH value is 7-7.5, dry, obtains lithium ion battery Microporous Carbon negative material.
Such as, by Na
2cO
3with the rice husk pyrolysate after acid treatment in mass ratio (1 ~ 5): 1 Homogeneous phase mixing, after grinding, put into tube furnace, under an argon atmosphere at 850 ~ 1000 DEG C calcine 2 ~ 5 hours, discharging through distilled water cyclic washing to going out Na
+ion and SiO
3 2-ion, dry, obtain lithium ion battery microporous carbon negative material.Chemical equation is as follows: Na
2cO
3+ C/SiO
2→ Na
2siO
3+ CO
2+ C.
Said method tool has the following advantages: 1. prepare the raw material of use for rice husk, hydrochloric acid, sodium carbonate, distilled water, and raw material easily obtains and subsequent products easily processes.2. gained lithium ion battery Microporous Carbon negative material is loose structure, and Stability Analysis of Structures is homogeneous, is conducive to electro transfer and transmission, is suitable for ion cathode material lithium.3. the method utilizes the destructive distillation of agricultural wastes rice husk, and through peracid treatment, alkali treatment finally obtains Microporous Carbon negative material, and raw material sources is extensive, and experimentation safety is easily implemented.4. the charging and discharging capacity of the lithium ion battery microporous carbon negative material of gained is high, and good cycle.
Further illustrate below in conjunction with specific embodiment.
Embodiment one
By the distilled water cleaning, drying of agricultural wastes rice husk, under tube furnace nitrogen atmosphere, destructive distillation 2 hours at 500 DEG C.Obtain rice husk pyrolysate.Gained rice husk pyrolysate is put into the hydrochloric acid solution of 0.1M, place 120 minutes, then repeatedly clean with distilled water at 70 DEG C, suction filtration to filtrate pH value is 7 ~ 7.5.Drying, obtains the rice husk pyrolysate after acid treatment.According to the ratio of mass ratio 1.75:1, sodium carbonate is mixed with the rice husk pyrolysate after acid treatment, fully after grinding, put into tube furnace, in a nitrogen atmosphere, calcine 3 hours for 900 DEG C.Discharging is fully washed through distilled water, the Na gone out wherein
+ion and SiO
3 2-ion, suction filtration, drying obtains lithium ion battery microporous carbon negative material.
The transmission electron microscope picture of this lithium ion battery microporous carbon negative material, scanning electron microscopic picture and X ray diffracting spectrum respectively as shown in Figure 2, Figure 3 and Figure 4 shown in, have figure known, this lithium ion battery negative material is microporous carbon structure.
In order to measure the chemical property of this negative material, by above-mentioned lithium ion battery negative material, acetylene black and PVDF(Kynoar, mass fraction is 8%) be mixed to form slurry at normal temperatures according to the ratio of mass ratio 70:20:10, slurry was evenly coated on Copper Foil substrate after 6 hours by mechanical agitation, after put it in vacuum drying chamber, at 120 DEG C, drying 12 hours, then becomes area to be 1cm by Copper Foil punching
2thin rounded flakes and pour lithium slice be electrode, with the LiPF of 1mol/L
6/ EC:DC+DMC(volume ratio 1:1:1) as electrolyte, with PP/PE hybrid films for barrier film, in the glove box being full of argon gas, be assembled into LIR2025 type experimental cell.
Experimental cell carries out charge and discharge cycles test by by computer-controlled auto charge and discharge instrument.Charging and discharging currents is 50mA/g, and charge cutoff voltage is 1.5V, and discharge cut-off voltage is 0V.Cycle efficieny is 108.1% first, and first discharge specific capacity is 604.0mAh/g, and 100 capability retentions that circulate are 57.5%, and as shown in Figure 5, as seen from the figure, this cell positive material has wider charge and discharge platform to first charge-discharge curve, 2.6 ~ 4.0V.At the cycle performance curves of 25 DEG C as shown in Figure 6, as seen from the figure, the battery capacity conservation rate after 100 times that circulates is 57.5%, reaches 347.2mAh/g.
Embodiment two
By the distilled water cleaning, drying of agricultural wastes rice husk, under tube furnace nitrogen atmosphere, destructive distillation 2 hours at 500 DEG C.Obtain rice husk pyrolysate.Gained rice husk pyrolysate is put into the hydrochloric acid solution of 0.1M, place 120 minutes, then repeatedly clean with distilled water at 70 DEG C, suction filtration to filtrate pH value is 7 ~ 7.5.Drying, obtains the rice husk pyrolysate after acid treatment.According to the ratio of mass ratio 1.75:1, sodium carbonate is mixed with the rice husk pyrolysate after acid treatment, fully after grinding, put into tube furnace, in a nitrogen atmosphere, calcine 3 hours for 900 DEG C.Discharging is fully washed through distilled water, the Na gone out wherein
+ion and SiO
3 2-ion, suction filtration, drying obtains lithium ion battery microporous carbon negative material.
Battery assembling and performance test are with embodiment one, and wherein lithium ion battery negative material, acetylene black and PVDF(Kynoar, mass fraction is 8%) be mixed to form slurry at normal temperatures according to the ratio of mass ratio 85:5:10.Cycle efficieny is 108.1% first, and first discharge specific capacity is 548.0mAh/g, and 100 capability retentions that circulate are 58.8%.
Embodiment three
By the distilled water cleaning, drying of agricultural wastes rice husk, under tube furnace nitrogen atmosphere, destructive distillation 2 hours at 500 DEG C.Obtain rice husk pyrolysate.Gained rice husk pyrolysate is put into the hydrochloric acid solution of 0.1M, place 120 minutes, then repeatedly clean with distilled water at 70 DEG C, suction filtration to filtrate pH value is 7 ~ 7.5.Drying, obtains the rice husk pyrolysate after acid treatment.According to the ratio of mass ratio 1:1, sodium carbonate is mixed with the rice husk pyrolysate after acid treatment, fully after grinding, put into tube furnace, in a nitrogen atmosphere, calcine 3 hours for 900 DEG C.Discharging is fully washed through distilled water, the Na gone out wherein
+ion and SiO
3 2-ion, suction filtration, drying obtains lithium ion battery microporous carbon negative material.
Battery assembling and performance test are with embodiment two.Cycle efficieny is 106.6% first, and first discharge specific capacity is 439.3mAh/g, and 100 capability retentions that circulate are 56.9%.
Embodiment four
By the distilled water cleaning, drying of agricultural wastes rice husk, under tube furnace nitrogen atmosphere, destructive distillation 2 hours at 500 DEG C.Obtain rice husk pyrolysate.Gained rice husk pyrolysate is put into the hydrochloric acid solution of 0.1M, place 120 minutes, then repeatedly clean with distilled water at 70 DEG C, suction filtration to filtrate pH value is 7 ~ 7.5.Drying, obtains the rice husk pyrolysate after acid treatment.According to the ratio of mass ratio 2:1, sodium carbonate is mixed with the rice husk pyrolysate after acid treatment, fully after grinding, put into tube furnace, in a nitrogen atmosphere, calcine 3 hours for 900 DEG C.Discharging is fully washed through distilled water, the Na gone out wherein
+ion and SiO
3 2-ion, suction filtration, drying obtains lithium ion battery microporous carbon negative material.
Battery assembling and performance test are with embodiment two.Cycle efficieny is 107.0% first, and first discharge specific capacity is 526.0mAh/g, and 100 capability retentions that circulate are 57.3%.
Embodiment five
By the distilled water cleaning, drying of agricultural wastes rice husk, under tube furnace nitrogen atmosphere, destructive distillation 2 hours at 500 DEG C.Obtain rice husk pyrolysate.Gained rice husk pyrolysate is put into the hydrochloric acid solution of 0.1M, place 120 minutes, then repeatedly clean with distilled water at 70 DEG C, suction filtration to filtrate pH value is 7 ~ 7.5.Drying, obtains the rice husk pyrolysate after acid treatment.According to the ratio of mass ratio 3:1, sodium carbonate is mixed with the rice husk pyrolysate after acid treatment, fully after grinding, put into tube furnace, in a nitrogen atmosphere, calcine 3 hours for 900 DEG C.Discharging is fully washed through distilled water, the Na gone out wherein
+ion and SiO
3 2-ion, suction filtration, drying obtains lithium ion battery microporous carbon negative material.
Battery assembling and performance test are with embodiment two.Cycle efficieny is 105.9% first, and first discharge specific capacity is 423.7mAh/g, and 100 capability retentions that circulate are 56.1%.
The performance comparison of embodiment 1 ~ 5 is as shown in table 1.
Table 1
| Cycle efficieny first | First discharge specific capacity (mAh/g) | Circulate 100 capability retentions | |
| Embodiment one | 108.1% | 604.0 | 57.5% |
| Embodiment two | 108.1% | 548.0 | 58.8% |
| Embodiment three | 106.6% | 439.3 | 56.9% |
| Embodiment four | 107.0% | 526.0 | 57.3% |
| Embodiment five | 105.9% | 423.7 | 56.1% |
Can be learnt by table 1, in the charging and discharging capacity of the lithium ion battery obtained by the lithium ion battery negative material of embodiment one to five, the charging and discharging capacity of embodiment one is the highest, and cycle performance is better.
The above embodiment only have expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.
Claims (9)
1. be the method that lithium ion battery microporous carbon negative material prepared by raw material with rice husk, it is characterized in that, comprise the steps:
1), by agricultural wastes rice husk water clean up, then in a nitrogen atmosphere with the temperature calcination 1 ~ 5 hour of 450 ~ 650 DEG C, obtain rice husk pyrolysate;
2), by rice husk pyrolysate in concentration be 0.1mol/L hydrochloric acid solution in boil 0.5 ~ 2.5 hour with 50 DEG C ~ 70 DEG C acid.
2. be washed to neutrality with distilled water, dry, obtain the rice husk pyrolysate after acid treatment;
3), by Na
2cO
3with the rice husk pyrolysate after acid treatment according to mass ratio (1 ~ 5): the ratio of 1 mixes, grinding evenly, is placed in tube furnace, calcines 2 ~ 5 hours in a nitrogen atmosphere at 850 ~ 1000 DEG C.
3. with distilled water by gains cyclic washing to removing Na
+ion and SiO
3 2-till, Ph value is 7-7.5, dry, obtains lithium ion battery microporous carbon negative material.
4. the preparation method of lithium ion battery microporous carbon negative material according to claim 1, is characterized in that, the described raw material preparing micro-pore carbon material are rice husk.
5. the preparation method of lithium ion battery microporous carbon negative material according to claim 1, is characterized in that, the diameter of described micro-pore carbon material is 20-30 μm, and aperture is less than 1nm.
6. the preparation method of lithium ion battery microporous carbon negative material according to claim 1, is characterized in that, alkali activator is sodium carbonate.
7. the preparation method of lithium ion battery microporous carbon negative material according to claim 1, is characterized in that, pyrolysis temperature is 450 ~ 650 DEG C, and the time is 1 ~ 5 hour.
8. the preparation method of lithium ion battery microporous carbon negative material according to claim 1, is characterized in that, acid treatment temperature is 50 DEG C ~ 70 DEG C, and the time is 0.5 ~ 2.5 hour.
9. the preparation method of lithium ion battery microporous carbon negative material according to claim 1, is characterized in that, activation temperature is 850 ~ 1000 DEG C, and the time is 2 ~ 5 hours.
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Cited By (6)
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| CN106505218A (en) * | 2016-11-14 | 2017-03-15 | 绥化学院 | A kind of waste mushroom leftover prepares mesoporous carbon and FeS2The method of combination electrode material |
| CN106684336A (en) * | 2016-12-25 | 2017-05-17 | 常州亚环环保科技有限公司 | Preparation method for high-combination degree lithium battery carbon silicon anode material |
| CN107623105A (en) * | 2017-10-09 | 2018-01-23 | 江西理工大学 | A kind of preparation method of lithium ion battery GND and conductive agent material |
| CN108987720A (en) * | 2018-08-01 | 2018-12-11 | 吉林大学 | Carbon/zinc oxide composite and its preparation method and application |
| CN109037677A (en) * | 2017-06-12 | 2018-12-18 | 四川大学 | A kind of porous carbon negative pole material of lithium ion battery and preparation method thereof |
| CN114635201A (en) * | 2022-01-29 | 2022-06-17 | 商丘师范学院 | Periostracum cicadae pyrolytic carbon fiber and preparation method and application thereof |
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| CN106505218A (en) * | 2016-11-14 | 2017-03-15 | 绥化学院 | A kind of waste mushroom leftover prepares mesoporous carbon and FeS2The method of combination electrode material |
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| CN106684336A (en) * | 2016-12-25 | 2017-05-17 | 常州亚环环保科技有限公司 | Preparation method for high-combination degree lithium battery carbon silicon anode material |
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| CN107623105A (en) * | 2017-10-09 | 2018-01-23 | 江西理工大学 | A kind of preparation method of lithium ion battery GND and conductive agent material |
| CN108987720A (en) * | 2018-08-01 | 2018-12-11 | 吉林大学 | Carbon/zinc oxide composite and its preparation method and application |
| CN114635201A (en) * | 2022-01-29 | 2022-06-17 | 商丘师范学院 | Periostracum cicadae pyrolytic carbon fiber and preparation method and application thereof |
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Application publication date: 20151125 |