CN103904328A - Preparation method of biomass lamella carbon material and application - Google Patents
Preparation method of biomass lamella carbon material and application Download PDFInfo
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- H01M4/00—Electrodes
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention discloses a preparation method of a biomass lamella carbon material and application of the biomass lamella carbon material in a lithium ion battery. The biomass lamella carbon material is prepared by processing betel nut shells through an alkaline solution and an acid solution, carbonizing the betel nut shells and ball milling the betel nut shells and can be used as a battery electrode material. The renewable betel nut shells are selected as a carbon source, the raw material is cheap and wide in source, the preparation process is simple, the cycling stability of the prepared battery is good, and the capacity is large.
Description
Technical field
The invention belongs to material with carbon element preparing technical field, relate in particular to a kind of preparation method and application thereof of biomass lamella material with carbon element.
Technical background
In recent years, along with non-renewable energy resources and the more and more serious environmental problem that reduce gradually in the whole world, the novel high-energy chemical power source of green non-pollution has become the focus that countries in the world are competitively developed.Lithium ion battery, owing to having high-energy, long-life, low consumption, nuisanceless, memory-less effect and the advantage such as self discharge is little, internal resistance is little, cost performance is high, pollution is few, is widely used in the fields such as photoelectricity, information, traffic, national defense and military.
Lithium ion battery is mainly made up of positive pole, negative pole and electrolyte solution etc., and negative material is one of key factor determining lithium ion battery combination property quality.Because material with carbon element has that electrode potential is low, cycle efficieny is high, has extended cycle life and the advantage such as security performance is good, and become current lithium ion battery commercialization negative material, and obtain a wide range of applications.Current various material with carbon element mainly makes from the mineral resources such as coal, pitch, petroleum coke and synthetic macromolecular compound, but due to the significant damage in the rare of mineral resources and macromolecular compound building-up process, environment being caused, make the development of material with carbon element and application be subject to certain limitation.
Biomass carbon is by biomass (comprising stalk, branch, leaf etc.) Pintsch process, carbonization and material with carbon element of forming under anoxia condition, there is the advantages such as raw material is easy to get, cheap, technique is simple, meet the requirement of green chemical industry, thereby start to be in recent years subject to the people's attention.The present invention prepares a kind of biomass lamella material with carbon element take PERICARPIUM ARECAE as charcoal source, and use it for the field such as lithium ion battery, ultracapacitor, the green that is beneficial to battery industry is produced, there is important practical value and good application prospect, by promoting the benign cycle of human lives and the Nature, be conducive to the sustainable development of biological environment simultaneously.
Application number is that 200910019348.4 Chinese patents " a kind of preparation method of porous carbon electrode material " disclose one take peanut shell as raw material, makes the preparation method of porous carbon materials.At room temperature, discharge and recharge with 0.2A/g constant current from open circuit voltage between 0.005V, the discharge capacity first of survey is 245 mAh/g, and capacity attenuation is 45 mAh/g for the second time, and the lower and decay of capacity rapidly, is difficult to as lithium ion battery negative material.Paper " High capacity disordered carbons obtained from coconut shells as anode materials for lithium batteries " (Journal of Alloys and Compounds 448 (2008) 141 – 147) has proposed take cocoanut shell as raw material, using KOH or ZnCl2 as pore-foaming agent, in the time that cocoanut shell/pore-foaming agent mass ratio is 1:5, under room temperature, place 5 days.Under nitrogen protection, by sample charing 1 hour at 800 ℃ and 900 ℃, obtain carbon electrode material.But the quality of this preparation method pore-foaming agent used is 5 times of cocoanut shell quality, and standing time is long; On market, the price of potassium hydroxide is about 10,000 yuan/ton, and cost is high; And zinc chloride has excitant and corrosivity, long-term suction will cause Bronchopneumonia, and serious suction can be lethal, has larger potential safety hazard.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides preparation method and the application thereof of a kind of environmental protection, safety, preparation is simple and easy, cost is low biomass lamella material with carbon element.
Above-mentioned purpose of the present invention is achieved by the following technical programs:
A preparation method for biomass lamella material with carbon element, adopts PERICARPIUM ARECAE as raw materials, comprises the following steps:
S1. preliminary treatment: first with deionized water, PERICARPIUM ARECAE is cleaned and is cut into bulk, put into the aqueous slkali of 1 ~ 2mol/L, at 70 ~ 90 ℃, water-bath is soaked, then the dilute acid soln of putting into 1 ~ 2mol/L boils to PERICARPIUM ARECAE completely bulkly, then washs PERICARPIUM ARECAE final vacuum drying for standby;
S2. prepare biomass lamella material with carbon element: put into tube type resistance furnace through S1 PERICARPIUM ARECAE after treatment; carbonization 1 ~ 2 hour under nitrogen protection; after naturally cooling to room temperature, prepared material with carbon element is added to ball mill ball milling 12 ~ 24 hours, cross 300 mesh sieves, make biomass lamella material with carbon element.
Selecting reproducible PERICARPIUM ARECAE is charcoal source, raw material cheapness, wide material sources.Through alkali, twice PERICARPIUM ARECAE after treatment of acid solution is more bulk, in the time of high-temperature process, contact fully with nitrogen, makes easy formation lamellar structure after carbonization.
Preferably, in described step S1, water-bath is soaked 9 ~ 11 hours; Washing PERICARPIUM ARECAE is with deionized water washing 3 ~ 5 times.
Preferably, the aqueous slkali described in step S1 is NaOH or potassium hydroxide solution.Dilute acid soln described in step S1 is watery hydrochloric acid or dilution heat of sulfuric acid.
Further, in step S1, vacuum drying temperature is 50 ~ 60 ℃.
Further, in step S2, carburizing temperature is 850 ~ 1000 ℃.In step S2, the heating rate of carbonization is 1 ~ 10 ℃/min.
The described biomass lamella material with carbon element making is prepared the preparation method of lithium ion battery, comprises the steps:
S11. prepare electrode slice: by described biomass lamella material with carbon element, acetylene black, bonding agent in mass ratio for 85:(5 ~ 10): (5 ~ 10) film of sizing mixing, make circular electric pole piece, described bonding agent is LA132 type aqueous binder, and described circular electric pole piece is Φ 10 circular electric pole pieces;
S21. prepare lithium ion battery: by prepared circular electric pole piece in step S11 under 60 ℃ of conditions after vacuumize, in the super purification glove box that is full of argon gas, carry out the assembling of button cell, take metal lithium sheet as anodal, the circular electric pole piece that step S11 makes is negative pole, and microporous polypropylene membrane is barrier film; Electrolyte adopts the mixed solution containing 1mol/L lithium hexafluoro phosphate, and ethylene carbonate, diethyl carbonate and methyl ethyl carbonate that described mixed solution is 1: 1: 1 by volume ratio are obtained by mixing.
Electrode prepared by the biomass lamella material with carbon element that is charcoal source by PERICARPIUM ARECAE, its good cycling stability is carried out charge-discharge test under 100mA/g current density, and after circulation in 100 weeks, Capacitance reserve is more than 200 mAh/g.
Compared with prior art, beneficial effect of the present invention is as follows:
(1) selecting reproducible PERICARPIUM ARECAE is charcoal source, raw material cheapness, wide material sources, and meet the requirement of green chemical industry, and form benign cycle with human lives and the Nature, promote the sustainable development of biological environment;
(2) by PERICARPIUM ARECAE with can be used as safe and reliable lithium ion battery negative material after alkali treatment, there is good using value;
(3) through alkali, twice betel nut after treatment of acid solution is more bulk, in the time of high-temperature process, contacts fully with nitrogen, makes carbonization easily form lamellar structure;
(4) good cycling stability of the electrode that prepared by biomass lamella material with carbon element of the present invention, under 100mA/g current density, carry out charge-discharge test, discharge capacity is 570.2 mAh/g first, initial charge capacity is 235.9 mAh/g, second week discharge capacity is 261.1 mAh/g, after circulation in 100 weeks, Capacitance reserve is at 205.9 mAh/g, and since the 2nd week, average capacitance loss rate was weekly less than 0.22%/week.
Accompanying drawing explanation
Fig. 1 is capacity-cycle-index curve chart of the embodiment of the present invention 1;
Fig. 2 is capacity-cycle-index curve chart of comparative example 1 of the present invention;
Fig. 3 is capacity-cycle-index curve chart of comparative example 2 of the present invention;
Fig. 4 is capacity-cycle-index curve chart of the embodiment of the present invention 5;
Fig. 5 is the electronic scanning video picture figure of the embodiment of the present invention 1;
Fig. 6 is the electronic scanning video picture figure of the embodiment of the present invention 5;
Fig. 7 is the electronic scanning video picture figure of the PERICARPIUM ARECAE fiber prepared of the present invention.
Embodiment
Below in conjunction with Figure of description and specific embodiment, the present invention is made further and being elaborated, but embodiment does not limit in any form the present invention.
A preparation method for biomass lamella material with carbon element, adopts PERICARPIUM ARECAE as raw materials, comprises the following steps:
S1. preliminary treatment: first water is by the dry PERICARPIUM ARECAE clean dry of buying on market, again dried PERICARPIUM ARECAE is cut into bulk, put into the sodium hydroxide solution of concentration 2mol/L, at 80 ℃, water-bath is soaked 10 hours, put into again in the watery hydrochloric acid of 2mol/L, boil to PERICARPIUM ARECAE completely bulk, then with for subsequent use in 60 ℃ of vacuumizes after deionized water washing 5 times;
S2. prepare biomass lamella material with carbon element: put into tube type resistance furnace through S1 PERICARPIUM ARECAE after treatment, in 950 ℃ of carbonizations 1 hour, heating rate was 5 ℃/min, naturally cools to room temperature under nitrogen protection.Again prepared material with carbon element is added to ball mill ball milling 12 hours, cross 300 mesh sieves, make biomass lamella material with carbon element, be labeled as C1.
The described biomass lamella material with carbon element making is prepared the preparation method of lithium ion battery, comprises the steps:
S11. prepare electrode slice: described biomass lamella material with carbon element, acetylene black, bonding agent, in mass ratio for the 85:7:8 film of sizing mixing, are made to circular electric pole piece; Described bonding agent is LA132 type aqueous binder, and described circular electric pole piece is Φ 10 circular electric pole pieces;
S21. prepare lithium ion battery: by prepared circular electric pole piece in step S11 under 60 ℃ of conditions after vacuumize, be full of the super purification glove box (Mikrouna of argon gas, Sukei1220/750) in, carry out the assembling of button cell, take metal lithium sheet as anodal, the circular electric pole piece that step S11 makes is negative pole, and microporous polypropylene membrane Celgard2400 is barrier film assembling CR2016 type button cell; Electrolyte adopts the mixed solution containing 1mol/L lithium hexafluoro phosphate, and ethylene carbonate, diethyl carbonate and methyl ethyl carbonate that described mixed solution is 1: 1: 1 by volume ratio are obtained by mixing.
Embodiment 2
In step S1, the concentration of sodium hydroxide solution is 1mol/L, and other conditions are with embodiment 1;
Embodiment 3
In step S1, the concentration of watery hydrochloric acid is 1 mol/L, and other conditions are with embodiment 1;
Embodiment 4
In step S2, Ball-milling Time is 18h, and other conditions are with embodiment 1;
Embodiment 5
In step S2, Ball-milling Time is 24h, and other conditions are with embodiment 1;
Comparative example 1
In step S1, the concentration of sodium hydroxide solution is 0mol/L, and other conditions are with embodiment 1;
Comparative example 2
In step S1, the concentration of sodium hydroxide solution is 3mol/L, and other conditions are with embodiment 1;
Comparative example 3
In step S1, the concentration of watery hydrochloric acid is 0mol/L, and other conditions are with embodiment 1;
Comparative example 4
In step S1, the concentration of watery hydrochloric acid is 3mol/L, and other conditions are with embodiment 1;
Comparative example 5
In step S2, Ball-milling Time is 11h, and other conditions are with embodiment 1;
Comparative example 6
In step S2, Ball-milling Time is 25h, and other conditions are with embodiment 1.
Test condition is: under room temperature, carry out charge-discharge test under 100mA/g current density, voltage range is: 0.05 ~ 1.5V.Measurement result is as table 1:
Table 1
| Project | Discharge capacity/mAh/g first | Initial charge amount/mAh/g | Discharge capacity/mAh/g for the second time | Charge volume/mAh/g for the second time | Capacity/mAh/g after circulation in 100 |
| Embodiment | |||||
| 1 | 505.8 | 200.5 | 218.9 | 198.2 | 206.8 |
| Embodiment 2 | 469.8 | 189.4 | 216.8 | 189.1 | 206.1 |
| Embodiment 3 | 483.9 | 186.2 | 211.6 | 190.8 | 204.2 |
| Embodiment 4 | 525.4 | 221.8 | 248.9 | 218.0 | 207.6 |
| Embodiment 5 | 570.2 | 235.9 | 261.1 | 230.6 | 205.9 |
| Comparative example 1 | 396.9 | 190.8 | 186.0 | 196.9 | 200.2 |
| Comparative example 2 | 426.6 | 186.0 | 205.5 | 194.0 | 200.4 |
| Comparative example 3 | 414.5 | 187.6 | 216.3 | 189.2 | 200.2 |
| Comparative example 4 | 422.7 | 195.8 | 202.9 | 194.4 | 201.7 |
| Comparative example 5 | 448.5 | 182.8 | 214.9 | 186.6 | 200.1 |
| Comparative example 6 | 510.2 | 210.2 | 209.6 | 196.8 | 200.6 |
Capacity-cycle-index curve chart of embodiment 1 as shown in Figure 1, as can be seen from the figure, under 100mA/g current density, carry out charge-discharge test, discharge capacity is 505.8mAh/g first, and discharge capacity is 218.9 mAh/g for the second time, and after circulation in 100 weeks, Capacitance reserve is at 206.8 mAh/g, the good cycling stability of lamella carbon electrode material is described, and capacity is higher, but initial stage irreversible capacity loss is larger, and to be electrolyte occur due to a series of side reactions at electrode surface possible cause.
Capacity-cycle-index curve chart of comparative example 1 as shown in Figure 2, as can be seen from the figure, carry out charge-discharge test under 100mA/g current density, discharge capacity is 396.9 mAh/g first, discharge capacity is 186.0 mAh/g for the second time, and after circulation in 100 weeks, Capacitance reserve is at 200.2 mAh/g.Contrast with comparative example 1 by embodiment 1, can find out that alkali treatment has a certain impact to lithium battery capacity, obviously lower without the material capacity of alkali treatment.
Capacity-cycle-index curve chart of comparative example 2 as shown in Figure 3, as can be seen from the figure, carry out charge-discharge test under 100mA/g current density, discharge capacity is 426.6 mAh/g first, discharge capacity is 205.5 mAh/g for the second time, and after circulation in 100 weeks, Capacitance reserve is at 200.4 mAh/g.By the contrast of comparative example 1,2 and embodiment 1,2, the concentration that can find out NaOH has certain effect to raising capacity, when concentration is during at 0 ~ 2mol/L, along with the rising of naoh concentration, the discharge capacity first of electrode material is also along with increase, thereby the increase of explanation alkaline concentration is conducive to improve the chemical property of material.When concentration is during at 2 ~ 3mol/L, along with the increase of naoh concentration, the volume lowering of electrode material, illustrates the too high chemical property variation that makes material of alkali concn.Visible, the present invention gets alkali concn scope for optimum.
Can be obtained by table 1, comparative example 1 is known with comparative example 3, and the indices of comparative example 3 is all lower than embodiment 1, and visible acid treatment can improve the capacity of lithium battery.By embodiment 1,3 and comparative example 3,4 contrasts, can find when acid concentration is during at 0 ~ 2mol/L, along with the rising of watery hydrochloric acid concentration, the discharge capacity first of electrode material is also along with increase, thereby the increase of explanation watery hydrochloric acid concentration is conducive to improve the chemical property of material.When acid concentration is during at 2 ~ 3mol/L, along with the increase of watery hydrochloric acid concentration, the volume lowering of electrode material, illustrates the too high chemical property variation that can make equally material of acid concentration.Visible, the present invention gets acid concentration scope for optimum.
Capacity-cycle-index curve chart of embodiment 5 as shown in Figure 4, as can be seen from the figure, under 100mA/g current density, carry out charge-discharge test, discharge capacity is 570.2 mAh/g first, discharge capacity is 261.1 mAh/g for the second time, and after circulation in 100 weeks, Capacitance reserve, at 205.9 mAh/g, is compared the lamella material with carbon element making in embodiment 1, the discharge capacity first of this material is higher, therefore extends Ball-milling Time the structure and the cycle performance that improve material are had to good contribution.
As shown in Figure 5, as can be seen from the figure, there are some strips in the material with carbon element of ball milling after 12 hours, illustrates that PERICARPIUM ARECAE material is after alkali, twice processing of acid solution, then high-temperature process contacts abundant carbonization, formation lamellar structure with nitrogen.This little lamellar structure is conducive to the embedding of lithium ion in charge and discharge process and deviates from, but still has the existence of a bulk of lamellar structure, and size is unfavorable for more greatly the diffusion of lithium ion in electrode, thereby affects the charge-discharge performance of material.
As shown in Figure 6, as can be seen from the figure, the material with carbon element of ball milling after 24 hours forms many irregular strips, compare the lamella material with carbon element making in embodiment 1, the material Ball-milling Time that embodiment 5 makes is longer, and material with carbon element more easily forms strip, and structure is more even.
Can be obtained by table 1, the indices of comparative example 5 is all than embodiment Isosorbide-5-Nitrae, 5 low, visible Ball-milling Time crosses that I haven't seen you for ages affects the capacity of lithium battery, the discharge capacity first of comparative example 6 is lower than embodiment 4,5, therefore selection Ball-milling Time is 12 ~ 24h.
Material with carbon element after charing in embodiment 1 is carried out to electronic scanning again with agate mortar grind into powder, and its electronic scanning video picture figure as shown in Figure 7.
As shown in Figure 7, as can be seen from the figure, the diameter of the PERICARPIUM ARECAE fiber after grinding is about 14 μ m, there is obvious layer structure on the surface of fiber, illustrate that PERICARPIUM ARECAE material is after alkali, twice processing of acid solution, fiber surface is corroded, then contacts abundant carbonization with nitrogen through high-temperature process, easily forms lamella material with carbon element.
Claims (10)
1. a preparation method for biomass lamella material with carbon element, is characterized in that, adopts PERICARPIUM ARECAE as raw materials, comprises the following steps:
S1. preliminary treatment: first with deionized water, PERICARPIUM ARECAE is cleaned and is cut into bulk, put into the aqueous slkali of 1 ~ 2mol/L, at 70 ~ 90 ℃, water-bath is soaked, then the dilute acid soln of putting into 1 ~ 2mol/L boils to PERICARPIUM ARECAE completely bulkly, then washs PERICARPIUM ARECAE final vacuum drying for standby;
S2. prepare biomass lamella material with carbon element: put into tube type resistance furnace through S1 PERICARPIUM ARECAE after treatment; carbonization 1 ~ 2 hour under nitrogen protection; after naturally cooling to room temperature, prepared material with carbon element is added to ball mill ball milling 12 ~ 24 hours, cross 300 mesh sieves, make biomass lamella material with carbon element.
2. the preparation method of biomass lamella material with carbon element according to claim 1, is characterized in that, in described step S1, water-bath is soaked 9 ~ 11 hours.
3. the preparation method of biomass lamella material with carbon element according to claim 1, is characterized in that, in described step S1, washing PERICARPIUM ARECAE is with deionized water washing 3 ~ 5 times.
4. the preparation method of biomass lamella material with carbon element according to claim 1, is characterized in that, the aqueous slkali described in step S1 is NaOH or potassium hydroxide solution.
5. the preparation method of biomass lamella material with carbon element according to claim 1, is characterized in that, the dilute acid soln described in step S1 is watery hydrochloric acid or dilution heat of sulfuric acid.
6. the preparation method of biomass lamella material with carbon element according to claim 1, is characterized in that, in step S1, vacuum drying temperature is 50 ~ 60 ℃.
7. the preparation method of biomass lamella material with carbon element according to claim 1, is characterized in that, in step S2, carburizing temperature is 850 ~ 1000 ℃.
8. the preparation method of biomass lamella material with carbon element according to claim 1, is characterized in that, in step S2, the heating rate of carbonization is 1 ~ 10 ℃/min.
9. the biomass lamella material with carbon element being made by claim 1 ~ 8 Arbitrary Term is prepared the preparation method of lithium ion battery, it is characterized in that, comprises the steps:
S11. prepare electrode slice: by described biomass lamella material with carbon element, acetylene black, bonding agent in mass ratio for 85:(5 ~ 10): (5 ~ 10) film of sizing mixing, make circular electric pole piece, described bonding agent is LA132 type aqueous binder;
S21. prepare lithium ion battery: by prepared circular electric pole piece in step S11 under 60 ℃ of conditions after vacuumize, in the super purification glove box that is full of argon gas, carry out the assembling of button cell, take metal lithium sheet as anodal, the circular electric pole piece that step S11 makes is negative pole, and microporous polypropylene membrane is barrier film; Electrolyte adopts the mixed solution containing 1mol/L lithium hexafluoro phosphate, and ethylene carbonate, diethyl carbonate and methyl ethyl carbonate that described mixed solution is 1: 1: 1 by volume ratio are obtained by mixing.
10. the lithium ion battery of being prepared gained by claim 9, is characterized in that, after circulation in 100 weeks, Capacitance reserve is more than 200 mAh/g.
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