CN102311113A - Tobacco stalk based porous carbon material for electrodes of super capacitor and preparation method thereof - Google Patents
Tobacco stalk based porous carbon material for electrodes of super capacitor and preparation method thereof Download PDFInfo
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Abstract
The invention provides a tobacco stalk based porous carbon material for electrodes of a super capacitor and a preparation method thereof. The preparation method comprises the following steps: taking tobacco stalk solid waste as a carbon precursor material, and after dehydration and crushing, impregnating the carbon precursor material by a carbonate solution with concentration of alkali mental ion being 2.0 to 3.8mol/L; and then carrying out carbonization-activation treatment, carrying out acid pickling, washing with hot deionized water, drying and carrying out vacuum treatment to obtain the porous carbon material. The preparation method is simple and has low cost, is environmentally friendly, and is suitable for industrial production. According to the invention, the obtained porous carbon material has the specific surface area between 1500 and 2200m<2>/g, the mesoporosity reaches 30-50%, the average pore size is between 2.3 and 2.5nm, the pore size distribution is narrow, and the adsorption performance is excellent. The electrodes of the super capacitor manufactured by the porous carbon material provided by the invention have the characteristics of high capacity, high power, long cycle life and the like.
Description
Technical field
The present invention relates to nonmetal charcoal preparation methods, particularly be used for the preparation method of the porous carbon material of electrode of super capacitor.
Background technology
Porous carbon material is as the ideal electrode material of ultracapacitor, and its performance depends primarily on inner pore structure, comprises pore size, pore size distribution, hole shape and pore volume etc., and the control punch structure is the key point that obtains the high-performance porous charcoal effectively.Electrode of super capacitor adopts chemical activation method preparation with porous carbon material more in the market, and wherein the most frequently used chemical activating agent is KOH, and tracing it to its cause is that this method can obtain height (> 2000m2/g) porous carbon material of specific surface area.
When adopting KOH to be acvator, very high to equipment requirements because its corrodibility is big, therebetween in order to pursue high-specific surface area, KOH add-on often big (consumption is to be activated 3 ~ 4 times of material) makes production cost increase; Simultaneously, the porous carbon material that this method makes belongs to the micropore charcoal more, and < 2 nm when the electrode material for super capacitor, exist under the high current density especially in organic electrolyte capacity attenuation serious, problems such as power characteristic reduction to mean pore size.
CN1872674A discloses a kind of preparation method who is used for ultracapacitor with porous carbon material; Adopting refinery coke is rich carbon source material; After the preparatory charing of process, mix by weight flooding, after overactivation pore-creating, obtain the carbonaceous electrode materials for 1:4 ~ 1:6 with KOH; Gained porous carbon material specific surface area is at 1500 ~ 2000m2/g, and mean pore size is at 2 ~ 3nm.The usage quantity of this method KOH is bigger, and production cost is high, do not provide in this patent simultaneously this porous carbon material in different electrolytes chemical property like size than capacitance.
CN1693189A discloses a kind of preparation method who is rich in the mesopore active carbon with high specific surface area who can be used for fields such as electrode material for super capacitor, lithium ion battery negative material; It is raw material with the petroleum coke powder; Through KOH aqueous solution dipping and adding metal-salt, wherein KOH and refinery coke impregnating effect ratio are to make after 3 ~ 6:1, dehydration and the activation.Having made the BET specific surface area is that 2000～2900 m2/g, mesopore volume are that 0.6～1.5 cm3/g and mean pore size are the active carbon with high specific surface area of 1.3～2.6 nm, and this porous carbon material is suitable for inorganic electrolyte liquid, reaches 270 ~ 300 F/g than electric capacity.But this method KOH consumption is big, seriously polluted equally, and cost is higher.
CN166998A discloses a kind of method of producing active carbon with high specific surface area; With the tobacco rod solid waste is raw material, through pulverizing, after the drying; Flood with potassium hydroxide solution; The mass ratio of potassium hydroxide solution and tobacco rod waste is 1: 1～5: 1, inserts to be heated to 600 ℃ in the microwave radiation device, and insulation for some time comes out of the stove; Use the hydrochloric acid soln pickling again, obtain the active carbon with high specific surface area product with hot wash, oven dry.The porous carbon material specific surface area that makes is at 2000～2500 m2/g.This method KOH activator level is high, and needs to adopt expensive microwave device, has further increased production cost.
Therefore select suitable carbon precursor raw material and acvator, confirm suitable activating process, the pore texture of assurance porous carbon material and specific surface area reduce environmental pollution and production cost when being applicable to electrode of super capacitor, are the keys of dealing with problems.
Summary of the invention
The present invention aims to provide that a kind of environmental protection is good, production cost is lower and the preparation method of the material specific surface area height of preparation, even aperture distribution, and the porous carbon material that be used for electrode of super capacitor that electrical property good more higher than capacitance,
Implementation of the present invention is following:
The preparation method of porous carbon material may further comprise the steps.
The step 1 raw materials pretreatment: raw material tobacco rod waste is carried out drying treatment through the mode of chemical dehydration, and abrasive dust makes the tobacco rod powder then; Generally speaking, need chemical dehydration 0.5 ~ 2 h under 250 ~ 400 ℃ temperature, then dried raw material tobacco rod waste is crushed to below 5 mm.Preferred metallic salt and the quality sum of mineral substance wherein of raw materials used tobacco rod waste accounts for total mass 8 ~ 13%.
Charing-the activation treatment of step 2 tobacco rod powder: place activator solution to soak 8 ~ 12 h in the prepared exsiccant tobacco rod of step 1 powder, after dehydrating, carry out charing-activation treatment, make the porous carbon material that contains impurity after the cooling; Wherein said acvator is selected from one or more among Na2CO3, K2CO3, NaHCO3 or the KHCO3; And the total concn of alkalimetal ion is 2.0～3.8 mol/L in the activator solution, and activator solution is (0.5～2) with the quality of tobacco rod powder-like than scope: 1.
When said acvator adopted the cationic carbonate of different metal, it mixes ratio was 0.5 ~ 2.
Charing-activation treatment can adopt prior art; Promptly put into activation furnace at 120 ℃ after dehydrating, under protective atmosphere, carry out charing-activation treatment, temperature rise rate is 5 ~ 10 ℃/min; Top temperature is 950 ~ 1050 ℃, and charing-soak time is 0.5 ~ 2 h.
The purification processes of step 3 impurity porous carbon material: with the prepared porous carbon material that contains impurity of step 2 earlier with hot-water soak 4 ~ 8 h; Using volumetric concentration again is that 10 ~ 20 % hydrochloric acid solns soak; The pH value of control solution is 2 ~ 3; Reusable heat water washing then, the pH value of control washing back material is 6.5 ~ 7, obtains porous carbon material after the oven dry; The water temperature of hot water generally is controlled at 80～90 ℃, and institute's water is generally deionized water, and bake out temperature is about 120 ℃.
The functional group that goes of step 4 porous carbon material handles: the porous carbon material of step 3 gained is carried out ball milling and screening; Selecting particle diameter is the powder of 5～20 μ m, under following condition, carries out vacuum high-temperature thermal treatment, and pressure is 0.01 MPa ~ 0.02 MPa; Temperature rise rate is 3 ~ 5 ℃/min; Thermal treatment temp is 550 ~ 700 ℃, and soaking time is 1 ~ 3 h, makes the finished product.
Adopt aforesaid method can make the porous carbon material that electrode of super capacitor is used; And be each item performance when guaranteeing that material is used, preferred specific surface area is that 1500～2200 m2/g, total pore volume are that 1.02～2.0 cm3/g, aperture are concentrated and be distributed between 1.5～3 nm and middle porosity reaches 30%～50% porous carbon material.
Compare with existing porous carbon material technology of preparing, advantage applies of the present invention exists:
1. the present invention selects the tobacco rod waste as carbon precursor; Be to consider that cigarette tobacco can apply more fertilizer for its growth people of promotion in process of growth; Therefore contain a certain amount of metallic salt and mineral substance in its tobacco rod waste; And these will be 850 ℃ of follow-up high temperature (>) can play certain pore-creating effect in the reactivation process, can reduce the consumption that adds acvator; Simultaneously, tobacco rod owing to himself structure, can more easily obtain being rich in the porous carbon material of mesopore high-specific surface area as biomass waste through simple activation treatment process.Experiment shows that the tobacco rod waste is a kind of good carbon precursor, not only can make the porous carbon material of excellent property, and realize being recycled of resource.
The present invention select for use single or compound carbonate as acvator, its alkalescence a little less than, corrodibility is little; And the acvator adding proportion is less in the present invention; Its consumption only is equivalent to 10 ~ 75% of tobacco rod base processed sample, and than traditional KOH activation method, consumption significantly reduces; Therefore equipment requirements is reduced, the pollution of environment is reduced.And utilize again as the carbonate of acvator is recyclable in the preparation process.
3. technical process of the present invention is simple than other method, control and realization more easily in the operation, and cost is lower.
4. the porous carbon material of the present invention's preparation all has higher quality and volumetric capacitance in water-based and organic system, and specific energy and specific power are high, have the favorable charge-discharge cycle performance simultaneously.
5, the porous carbon material that makes of the present invention shows excellent electrochemical properties in organic electrolyte system, behind 5000 cycle charge-discharges, still reaches 150 ~ 170 F/g than electric capacity, and current density increases 50 times, and capability retention reaches 80 ~ 90 %.
Description of drawings
The charging and discharging curve figure of the hole charcoal of Fig. 1 embodiment of the invention 1 in organic electrolyte;
The porous charcoal of Fig. 2 embodiment of the invention 1 in organic electrolyte than the graphic representation of electric capacity with current density change;
The graph of pore diameter distribution of the porous charcoal of Fig. 3 embodiment of the invention 2.
Embodiment
100 g raw material tobacco rod wastes at 300 ℃ of chemical dehydration 2 h, are crushed to below 5 mm, and the concentration of using the basic metal potassium ion again is K2CO3 solution impregnation 8 h of 3.8 mol/L; The mass ratio of K2CO3 solution and tobacco rod powder is 1:1,120 ℃ dehydrate after, put into activation furnace; Under the protection of nitrogen gas atmospheric condition, carry out carbonization-activation and handle, temperature rise rate is that 5 ℃/min is warming up to 950 ℃, carbonization time 0.5 h; Sample after the charing is first with 80 ℃ of hot-water soak 8 h; Using volumetric concentration again is that 20% hydrochloric acid soln soaks, and the pH value of control solution is washed with 80 ℃ of hot deionized waters 2 ~ 3 again; The pH value of control washing back material is 6.5 ~ 7, obtains porous carbon material after the oven dry down in 120 ℃ again;
Using ball mill to be finely ground to particle diameter above-mentioned porous carbon material is 5 ~ 10 μ m; Under the 0.01MPa vacuum condition, be warming up to 500 ℃ and carry out vacuum heat treatment with 2 ℃/min speed; Treatment time is 1h, obtains the finished product---be used for the porous carbon material of electrode of super capacitor.
Through test; The above-mentioned specific surface area that is used for the porous carbon material of electrode of super capacitor is 1808 m2/g; Pore volume is 1.04 cm3/g; Mean pore size is 2.33 nm, and this porous carbon electrode is 252 F/g than electric capacity when current density is 1 mA/cm2 in 30% KOH electrolytic solution after 5000 charge and discharge cycles; Be 160F/g than electric capacity when current density is 1 mA/cm2 in 1 mol/L Et4NBF4/PC organic electrolyte, current density increases 50 times, still reaches 130F/g than electric capacity.As shown in Figure 1, this porous carbon electrode shows the favorable charge-discharge performance, and charging and discharging curve has good symmetry, and efficiency for charge-discharge is near 100%; As shown in Figure 2, current density increases 50 times, is 130 F/g than electric capacity, and capability retention reaches 81.3%, shows good high rate during charging-discharging.
Embodiment 2
With 100g raw material tobacco rod waste, at 350 ℃ of chemical dehydration 1.5h, be crushed to below the 5mm, the concentration of using the basic metal potassium ion again is that 2.2 mol/L K2CO3 flood 8 h; The mass ratio of K2CO3 solution and tobacco rod powder is 0.5:1,120 ℃ dehydrate after, put into activation furnace; Under the protective atmosphere condition, carry out carbonization-activation and handle, temperature rise rate is that 5 ℃/min is warming up to 950 ℃, carbonization time 0.5h; Earlier with 80 ℃ of hot-water soak 8h, using volumetric concentration again is that 10% hydrochloric acid soln soaks with charing appearance, and control pH value is 2 ~ 3; 80 ℃ of hot deionized water washings, the pH value of control washing back material is about 6.5 ~ 7,120 ℃ obtain porous carbon material after the oven dry down;
Using ball mill to be finely ground to particle diameter above-mentioned porous carbon material is 5 ~ 10 μ m; Under the 0.01MPa vacuum condition, be warming up to 600 ℃ again and carry out vacuum heat treatment with 5 ℃/min speed; Treatment time is 0.5h, obtains the finished product---be used for the porous carbon material of electrode of super capacitor.
Through test, the above-mentioned specific surface area that is used for the porous carbon material of electrode of super capacitor is 1508 m2/g, and pore volume is 0.84 cm3/g; Mean pore size is 2.23 nm, and is as shown in Figure 3, and the micropore size of this porous carbon material is bigger; The aperture mainly is distributed in about 2nm, and pore size distribution is concentrated, and is suitable as very much electrode of super capacitor and uses material; This porous carbon electrode is 230 F/g than electric capacity when current density is 1 mA/cm2 in 30% KOH electrolytic solution after 5000 charge and discharge cycles; Be 150F/g than electric capacity when current density is 1 mA/cm2 in 1 mol/L Et4NBF4/PC organic electrolyte, current density increases 50 times, still reaches 125F/g than electric capacity.
Embodiment 3
With 100g raw material tobacco rod waste,, be crushed to below the 5mm at 350 ℃ of chemical dehydration 1.5h; The concentration of using alkalimetal ion again is that 3.8 mol/L KHCO3 flood 6 h, and the mass ratio of KHCO3 solution and tobacco rod powder is 2.5 ︰ 1,120 ℃ dehydrate after; Put into activation furnace, under the protective atmosphere condition, carry out carbonization-activation and handle, temperature rise rate is that 5 ℃/min is warming up to 1050 ℃; Carbonization time 0.5h, earlier with 90 ℃ of hot-water soak 8h (salt in the soak solution can concentrate recycling), using volumetric concentration again is that 20% hydrochloric acid soln soaks with charing appearance; Control pH value is 2 ~ 3; 80 ℃ of hot deionized water washings, the pH value of control washing back material is about 6.5 ~ 7,120 ℃ obtain porous carbon material after the oven dry down;
Using ball mill to be finely ground to particle diameter above-mentioned porous carbon material is 5 ~ 10 μ m; Under the 0.02MPa vacuum condition, be warming up to 500 ℃ again and carry out vacuum heat treatment with 2 ℃/min speed; Treatment time is 1h, obtains the finished product---be used for the porous carbon material of electrode of super capacitor.
Through test; The above-mentioned specific surface area that is used for the porous carbon material of electrode of super capacitor is 2050 m2/g; Pore volume is 1.02 cm3/g; Mean pore size is 2.4 nm, and this porous carbon electrode is 270 F/g than electric capacity when current density is 1 mA/cm2 in 30% KOH electrolytic solution after 5000 charge and discharge cycles; Be 165F/g than electric capacity when current density is 1 mA/cm2 in 1 mol/L Et4NBF4/PC organic electrolyte, current density increases 50 times, still reaches 140F/g than electric capacity.
Embodiment 4
With 100g raw material tobacco rod waste,, be crushed to below the 5mm at 300 ℃ of chemical dehydration 2 h; The total concn of using alkalimetal ion again is 2.8 mol/L K2CO3/Na2CO3 compound activator solution dipping, and K2CO3/Na2CO3 mass ratio is 1:1, and time of immersion is 6 h; The mass ratio of compound activator solution and tobacco rod powder is 2.5 ︰ 1,120 ℃ dehydrate after, put into activation furnace; Under the protective atmosphere condition, carry out carbonization-activation and handle, temperature rise rate is that 10 ℃/min is warming up to 1050 ℃, carbonization time 1 h; Charing appearance is first with 80 ℃ of hot-water soak 8 h (salt in the soak solution can concentrate recycling); Using volumetric concentration again is that 20 % hydrochloric acid solns soak, and control pH value is 2 ~ 3, and 90 ℃ of hot deionized waters wash; The pH value of control washing back material is about 6.5 ~ 7, and 120 ℃ obtain porous carbon material after the oven dry down;
Using ball mill to be finely ground to particle diameter above-mentioned porous carbon material is 10 ~ 20 μ m; Under 0.03 MPa vacuum condition, be warming up to 600 ℃ again and carry out vacuum heat treatment with 2 ℃/min speed; Treatment time is 0.5 h, obtains the finished product---be used for the porous carbon material of electrode of super capacitor.
Through test; The above-mentioned specific surface area that is used for the porous carbon material of electrode of super capacitor is 2110 m2/g; Pore volume is 1.05 cm3/g; Mean pore size is 2.6 nm, and this porous carbon electrode is 260 F/g than electric capacity when current density is 1 mA/cm2 in 30% KOH electrolytic solution after 5000 charge and discharge cycles; Be 165 F/g than electric capacity when current density is 1 mA/cm2 in 1 mol/L Et4NBF4/PC organic electrolyte, current density increases 50 times, still reaches 142 F/g than electric capacity.
With 100 g raw material tobacco rod wastes,, be crushed to below 5 mm at 400 ℃ of chemical dehydration 1.0 h; The total concn of using alkalimetal ion again is 3.8 mol/L K2CO3/NaHCO3 compound activator solution dipping, and K2CO3/NaHCO3 mass ratio is 3:2, and time of immersion is 8 h; The mass ratio of compound activator solution and tobacco rod powder is 2:1,120 ℃ dehydrate after, put into activation furnace; Under the protective atmosphere condition, carry out carbonization-activation and handle, temperature rise rate is that 5 ℃/min is warming up to 1000 ℃, carbonization time 0.5 h; Charing appearance is first with 80 ℃ of hot-water soak 8 h (salt in the soak solution can concentrate recycling); Using volumetric concentration again is that 20 % hydrochloric acid solns soak, and control pH value is 2 ~ 3, and 90 ℃ of hot deionized waters wash; The pH value of control washing back material is about 6.5 ~ 7, and 120 ℃ obtain porous carbon material after the oven dry down;
Using ball mill to be finely ground to particle diameter above-mentioned porous carbon material is 5 ~ 10 μ m; Under 0.02 MPa vacuum condition, be warming up to 500 ℃ again and carry out vacuum heat treatment with 5 ℃/min speed; Treatment time is 1 h, obtains the finished product---be used for the porous carbon material of electrode of super capacitor.
Through test; The above-mentioned specific surface area that is used for the porous carbon material of electrode of super capacitor is 2210 m2/g; Pore volume is 1.35 cm3/g; Mean pore size is 2.4 nm, and this porous carbon electrode is 280 F/g than electric capacity when current density is 1 mA/cm2 in 30% KOH electrolytic solution after 5000 charge and discharge cycles; Be 170 F/g than electric capacity when current density is 1 mA/cm2 in 1 mol/L Et4NBF4/PC organic electrolyte, current density increases 50 times, still reaches 140 F/g than electric capacity.
Claims (6)
1. a preparation method who is used for the porous carbon material of electrode of super capacitor is characterized in that, comprises the steps:
The step 1 raw materials pretreatment: raw material tobacco rod waste is carried out drying treatment through the mode of chemical dehydration, and abrasive dust makes the tobacco rod powder then;
Charing-the activation treatment of step 2 tobacco rod powder: place activator solution to soak 8 ~ 12 h in the prepared exsiccant tobacco rod of step 1 powder, after dehydrating, carry out charing-activation treatment, make the porous carbon material that contains impurity after the cooling; Wherein said acvator is selected from one or more among Na2CO3, K2CO3, NaHCO3 or the KHCO3; And the total concn of alkalimetal ion is 2.0～3.8 mol/L in the activator solution, and activator solution is (0.5～2.5) with the quality of tobacco rod powder-like than scope: 1;
The purification processes of step 3 impurity porous carbon material: with the prepared porous carbon material that contains impurity of step 2 earlier with hot-water soak 4 ~ 8 h; Using volumetric concentration again is that 10 ~ 20 % hydrochloric acid solns soak; Control pH value of solution value is 2 ~ 3; Reusable heat water washing then, the pH value of control washing back material is 6.5 ~ 7, obtains porous carbon material after the oven dry;
The functional group that goes of step 4 porous carbon material handles: with prepared porous carbon material ball milling of step 3 and screening; Selecting particle diameter is the powder of 5 ~ 20 μ m; Pressure be 0.01 ~ 0.02 MPa, temperature rise rate be 3 ~ 5 ℃/min, thermal treatment temp to be 550 ~ 700 ℃ be to carry out vacuum high-temperature thermal treatment under the condition of 1 ~ 3 h with soaking time, make the finished product.
2. be used for the preparation method of the porous carbon material of electrode of super capacitor according to claim 1, it is characterized in that: need chemical dehydration 0.5 ~ 2 h under 250 ~ 400 ℃ temperature, then dried raw material tobacco rod waste is crushed to below 5 mm.
3. be used for the preparation method of the porous carbon material of electrode of super capacitor according to claim 1, it is characterized in that: when said acvator adopted the cationic carbonate of different metal, the mixing ratio of two kinds of cationic solution volumetric molar concentrations was 0.5 ~ 2.
4. be used for the preparation method of the porous carbon material of electrode of super capacitor according to claim 1, it is characterized in that: the metallic salt in the said raw material tobacco rod waste and the quality sum of mineral substance account for 8 ~ 13% of total mass.
5. a porous carbon material that is used for electrode of super capacitor is characterized in that: adopt to prepare like the described method of one of claim 1～4.
6. the porous carbon material that is used for electrode of super capacitor as claimed in claim 4 is characterized in that: preferred specific surface area is that 1500～2200 m2/g, total pore volume are that 1.02～2.0 cm3/g, aperture are concentrated and be distributed between 1.5～3 nm and middle porosity reaches 30%～50% porous carbon material.
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