CN109516458A - A kind of biomass-based graded porous carbon and preparation method thereof - Google Patents
A kind of biomass-based graded porous carbon and preparation method thereof Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
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- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of biomass-based graded porous carbons and preparation method thereof.This method comprises the following steps: biomass material shearing being screened to 20-80 mesh, is added in double salt system aqueous solutions, stirring, the pre- carbonization treatment 5-20 h of hydrothermal reaction at low temperature at 180-300 DEG C, washing filtering obtains pre- carbonized product；Then it is warming up to 600-1000 DEG C of carbonization-activation processing 0.5-8 h under an inert atmosphere, products therefrom is washed with water and washs to neutrality through pickling, alkali cleaning or ultrasound, and it is dry, obtain the biomass-based graded porous carbon.The present invention carries out hydrothermal carbonization in pre- carbonization, using double salt systems as salt template and pre- pore creating material, porous carbon is prepared for subsequent carbonization-activation, and advantage is provided, not only specific surface area with higher and loose three-dimensional are coupled cellular structure to resulting porous carbon, conductivity with higher and good capacitive character can be applied in supercapacitor as carbon electrode.
Description
Technical field
The invention belongs to material science and field of energy and chemical technology, and in particular to a kind of biomass-based graded porous carbon and
Preparation method.
Background technique
Supercapacitor is as a kind of novel energy-storing equipment, with power density is high, energy density is big, specific capacitance is high, follows
The advantages that ring service life is good, with good stability has huge in fields such as electronic equipment energy storage, military science and technology, space flight and aviation
Big application prospect.Wherein, porous carbon materials are considered as the electrode material for super capacitor of most prospect.
Porous carbon materials are due to chemical stability height, large specific surface area, porosity height, aperture controllable, good conductivity, mistake
The features such as convenient, cheap, from a wealth of sources and environmental-friendly is regenerated after effect, is widely used in absorption, catalysis, sensing, electricity
The fields such as chemical energy storage.In recent years, with the exhaustion of fossil energy, development and the application of porous carbon materials are restricted.It is raw
Material carbon content rich in, largely exists in nature, belongs to renewable energy, as presoma for making
Standby porous carbon materials have broad prospects.
The prior art mainly prepares biomass-based porous carbon using physically activated, chemical activation, physical-chemical activation.?
In combination with hard template, soft template and double-template method during activation carbonization, porous carbon materials hole is solved while activating pore-creating
The problem of diameter wider distribution.In addition, the fiber skeleton of biological material can be fixed by carrying out pre- carbonization before activation is carbonized, three are constituted
Tie up template.Hydro-thermal method is common pre- carbonization method, can effectively fix biological material in low-temperature carbonization process, improve porous carbon
Yield.However, be easy to causeing the problems such as pre- char-forming material pattern is irregular, carbon particle stacking is agglomerating using hydro-thermal method merely；And
And the prior art is generally focused on the porosity that subsequent activation process improves carbon, it is fresh few in the proposition corrective measure of pre- carbonation stage.
Therefore, hydro-thermal method, which is purely by way of pre- carbonization means, still limitation, acts on more single.Double salt systems are introduced in water-heat process
It can effectively induce carbon material to form regular pattern as salt template and pore creating material, so that carbon particle is uniformly dispersed, in hydro-thermal process rank
The preliminary pore-creating of section provides defect sites as pore site for high-temperature calcination aperture, is conducive to subsequent activation carbonization and prepares high hole
The graded porous carbon of gap rate.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of biomass-based graded porous carbon and its preparations
Method, the material may be used as electrode material for super capacitor.
The present invention is realized especially by following technical scheme.
A kind of preparation method of biomass-based graded porous carbon provided by the invention, includes the following steps:
(1) 20 ~ 80 mesh powdered biomass and double salt templates are added to the water, are sealed, under conditions of 100 ~ 200 r/min stirring
It is placed in high-temperature high-pressure reaction kettle after carrying out the pre- carbonization treatment of low-temperature hydrothermal, is cooled to room temperature, filter to take precipitating, solid product warp
Washing, drying, obtain pre- carbonized product；
(2) take pre- carbonized product made from step (1) and activator, template ground and mixed uniform, then in an inert atmosphere
600-1000 DEG C is warming up in tube furnace, carbonization-activation 0.5-8 h, carbonized product is washed with water and washs into after removing impurity
Property, it is dry, obtain the biomass-based graded porous carbon.
Further, in step (1), the powdered biomass is to obtain biomass material shearing sieving, biomass
Powder diameter size is 20-80 mesh；
Further, the biomass material is one or more of rice straw, corn stover, straw, bagasse, peanut shell.
Further, the mass ratio of powdered biomass described in step (1), double salt templates and water is 1:(1 ~ 5): (1 ~
10)。
Further, double salt described in step (1) are KCl, LiCl, NaCl, ZnCl2、AlCl3、K2SO4In two kinds；It is double
Molar ratio between salt is (25 ~ 60): (25 ~ 75).
Further, the temperature of the pre- carbonization treatment of low-temperature hydrothermal described in step (1) is 180 ~ 300 DEG C, and the time is 5 ~ 20
h。
Further, activator described in step (2) is KOH, K2CO3、KHCO3、K2C2O4、Na2CO3One of with
On；The mass ratio of activator and pre- carbonized product is (0.5 ~ 5): 1；The template is SiO2、CaCO3、Al2O3、MgCO3In
More than one；The mass ratio of template and pre- carbonized product is (0.25 ~ 5): 1.
Further, the inert atmosphere is nitrogen or argon gas, and the heating rate for being warming up to the heat treatment temperature is 3
~10 ℃/min。
Further, removal impurity described in step (2) be the HCl solution pickling of the M of 0.5 M ~ 3, mass fraction be 10% ~
One or more of 30% NaOH solution alkali cleaning, 50 ~ 80 W ultrasound lift-off processing, 2 ~ 8 h.
Further, under preparation condition of the invention, the specific surface area of prepared biomass-based porous carbon is 1000 ~
2000 m2/g；In three-electrode system, with 1 M H2SO4Electrolyte carries out electro-chemical test, when sweep speed is 20 mV/s,
Specific capacitance is 294 ~ 347 F/g.
A kind of biomass-based graded porous carbon as made from above-mentioned preparation method.The biomass-based porous carbon can be used for
The electrode material of supercapacitor.
Preparation method of the invention and obtained product have the following advantages that and the utility model has the advantages that
(1) preparation method of the present invention uses abundant, cheap biomass castoff for carbon precursor, is with biomass castoff
The method that raw material is pre-processed by low-temperature hydrothermal and activates carbonization prepares graded porous carbon, can not only overcome fossil energy crisis
Limitation to porous carbon development, and it is able to achieve the higher value application of biomass resource.
(2) present invention is carbonized in advance by low-temperature hydrothermal, and biomass material can be made to be changed into loose pre- carbonized product, be
Subsequent carbonization-activation prepares porous carbon and provides favourable conditions.
(3) present invention introduced in low-temperature hydrothermal carbonisation double salt systems as salt template and and pore creating material, can be effective
Induction carbon material forms regular pattern, and carbon particle is made to be uniformly dispersed, and is high-temperature calcination aperture in the preliminary pore-creating of hydro-thermal process stage
Defect sites are provided, the graded porous carbon that subsequent activation carbonization prepares high porosity is conducive to.
(4) present invention is in activation carbonisation in combination with activator and template, and wherein template can be anti-with activator
Gas should be generated and carry out pore-creating, improve the porosity of porous carbon.
(5) carbonized product in the present invention further increases the porosity of porous carbon through pickling, alkali cleaning or ultrasonic treatment.
(6) specific surface area of the biomass-based classifying porous carbon material prepared by the present invention is high, and range is 1000 ~ 2000
m2/ g, cellular structure is loose, has micropore/mesopore/macropore hierarchical structure；In three-electrode system, with 1 M H2SO4Electrolyte
Electro-chemical test is carried out, when sweep speed is 20 mV/s, specific capacitance is 294 ~ 347 F/g, has excellent supercapacitor
Can, and cyclical stability is high.
Detailed description of the invention
Fig. 1 is the SEM figure of biomass-based graded porous carbon prepared by embodiment 1 (amplification factor is 10000 times)；
Fig. 2 is the BET result figure of biomass-based graded porous carbon prepared by embodiment 1；
Fig. 3 is the SEM figure of biomass-based graded porous carbon prepared by embodiment 2 (amplification factor is 3000 times)；
Fig. 4 is the BET result figure of biomass-based graded porous carbon prepared by embodiment 2；
Fig. 5 is cyclic voltammetry curve figure of the biomass-based graded porous carbon of the preparation of embodiment 1 under 20 mV/s sweep speeds.
Fig. 6 is the specific capacitance histogram of biomass-based graded porous carbon prepared by embodiment 1 ~ 5.
Specific embodiment
Combined with specific embodiments below and attached drawing the invention will be further described, but embodiments of the present invention are not limited to
This.
Embodiment 1
A kind of preparation method of biomass-based graded porous carbon of the present embodiment, specific preparation process is as follows:
(1) the rice straw powder that 5 g shearing is screened to 20 mesh is weighed, rice straw powder, double salt systems and water are pressed 1:
The mass ratio of 5:10 mixes；Wherein, double salt systems select the system of potassium chloride (KCl) and sodium chloride (NaCl), mole of the two
Than for 25:75.By the above mixture be added high temperature and pressure hydro-thermal reaction kettle, heated sealed to 180 DEG C, and 100 r/min perseverance
Temperature stirring is lower to react 20 h；It is cooled to room temperature after reaction, solid product in reaction kettle is washed with deionized to neutrality,
By 80 DEG C of 24 h of drying of product after washing, pre- carbonized product is obtained；
(2) the pre- carbonized product of 1 g is weighed, by pre- carbonized product and potassium hydroxide (KOH) and silica (SiO2) press 1:0.5:
0.25 mass ratio is ground；Said mixture is placed in nitrogen atmosphere pipe type furnace and carries out carbonization-activation, from room temperature,
The heating rate of 10 DEG C/min is warming up to 600 DEG C of target temperature, keeps the temperature 8 h；It is cooled to room temperature after reaction, takes out carbonization
Activation products are simultaneously washed with 0.5 M HCl solution, then are washed with deionized to neutrality, by 80 DEG C of dryings of product after washing
24 h obtain biomass-based graded porous carbon made from embodiment 1.Fig. 1 is porous carbon obtained by the present embodiment at 10000 times
A large amount of fine and closely woven holes are distributed in SEM figure, the rice straw base porous carbon as can be seen from the figure prepared by this method.Fig. 2 is
The nitrogen adsorption desorption curve of sample, it is 1419 m that its specific surface area, which is calculated, by BET2/g.In three-electrode system, with 1
M H2SO4Electrolyte carries out electro-chemical test, and when sweep speed is 20 mV/s, specific capacitance is 328.13 F/g.The present embodiment institute
The cyclic voltammogram of porous carbon is obtained as shown in figure 5, specific capacitance size is as shown in Figure 6.
Embodiment 2
A kind of preparation method of biomass-based graded porous carbon of the present embodiment, specific preparation process is as follows:
(1) maize straw powder that 20 g shearing is screened to 30 mesh is weighed, maize straw powder, double salt systems and water are pressed 1:
The mass ratio of 1:1 mixes；Wherein, double salt systems select potassium chloride (KCl) and zinc chloride (ZnCl2) system, the molar ratio of the two
For 40:60.High temperature and pressure hydro-thermal reaction kettle is added in the above mixture, heated sealed is to 300 DEG C, and in 200 r/min constant temperature
Stirring is lower to react 5 h；It is cooled to room temperature after reaction, the solid product in reaction kettle is washed with deionized to neutrality, incites somebody to action
80 DEG C of 24 h of drying of product after washing, obtain pre- carbonized product；
(2) the pre- carbonized product of 10 g is weighed, by pre- carbonized product and potassium oxalate (K2C2O4) and calcium carbonate (CaCO3) press 1:5:5
Mass ratio be ground；Said mixture is placed in argon atmosphere pipe type furnace and carries out carbonization-activation, from room temperature, 10
DEG C/heating rate of min is warming up to 1000 DEG C of target temperature, keep the temperature 0.5 h；It is cooled to room temperature after reaction, takes out carbonization
Activation products are simultaneously washed with the NaOH solution of 10% mass fraction, then are washed with deionized to neutrality, by the product after washing
80 DEG C of 24 h of drying, obtain biomass-based graded porous carbon made from embodiment 2.Fig. 3 is that porous carbon obtained by the present embodiment exists
A large amount of fine and closely woven holes are distributed in 3000 times of SEM figure, the corn stover base porous carbon as can be seen from the figure prepared by this method
Gap.Fig. 4 is the nitrogen adsorption desorption curve of sample, and it is 1044 m that its specific surface area, which is calculated, by BET2/g.In three electrode bodies
In system, with 1 M H2SO4Electrolyte carries out electro-chemical test, and when sweep speed is 20 mV/s, specific capacitance is 322.76 F/g.This
The specific capacitance size of porous carbon obtained by embodiment is as shown in Figure 6.
Embodiment 3
A kind of preparation method of biomass-based graded porous carbon of the present embodiment, specific preparation process is as follows:
(1) the peanut shell powder that 12 g shearing is screened to 50 mesh is weighed, by peanut shell powder, double salt systems and water by 1:5:1's
Mass ratio mixing；Wherein, double salt systems select aluminium chloride (AlCl3) and sodium chloride (NaCl) system, the molar ratio of the two is 25:
75.High temperature and pressure hydro-thermal reaction kettle is added in the above mixture, heated sealed is stirred to 180 DEG C, and in 100 r/min constant temperature
20 h of lower reaction；It is cooled to room temperature after reaction, the solid product in reaction kettle is washed with deionized to neutrality, will wash
80 DEG C of 24 h of drying of product afterwards, obtain pre- carbonized product；
(2) the pre- carbonized product of 8 g is weighed, by pre- carbonized product and saleratus (KHCO3) and aluminium oxide (Al2O3) press 1:0.5:
0.25 mass ratio is ground；Said mixture is placed in nitrogen atmosphere pipe type furnace and carries out carbonization-activation, from room temperature,
The heating rate of 10 DEG C/min is warming up to 600 DEG C of target temperature, keeps the temperature 8 h；It is cooled to room temperature after reaction, takes out carbonization
Activation products are simultaneously successively washed with the NaOH solution of 1 M HCl and 30 % mass fractions, then are washed with deionized to neutrality, will
80 DEG C of 24 h of drying of product after washing, obtain biomass-based graded porous carbon made from embodiment 3.The present embodiment institute is much
Hole carbon is in three-electrode system, with 1 M H2SO4Electrolyte carries out electro-chemical test, when sweep speed is 20 mV/s, specific capacitance
For 294.27 F/g.The specific capacitance size of porous carbon obtained by the present embodiment is as shown in Figure 6.
Embodiment 4
A kind of preparation method of biomass-based graded porous carbon of the present embodiment, specific preparation process is as follows:
(1) the straw powder that 10 g shearing is screened to 60 mesh is weighed, straw powder, double salt systems and water are pressed to the quality of 1:5:10
Than mixing；Wherein, double salt systems select lithium chloride (LiCl) and zinc chloride (ZnCl2) system, the molar ratio of the two is 40:60.
High temperature and pressure hydro-thermal reaction kettle is added in the above mixture, for heated sealed to 300 DEG C, constant temperature is stirred to react 5 h；Reaction terminates
After be cooled to room temperature, the solid product in reaction kettle is washed with deionized to neutrality, by 80 DEG C of dryings 24 of product after washing
H obtains pre- carbonized product；
(2) the pre- carbonized product of 4 g is weighed, by pre- carbonized product and potassium carbonate (K2CO3) and magnesium carbonate (MgCO3) press 1:5:0.25
Mass ratio be ground；Said mixture is placed in argon atmosphere pipe type furnace and carries out carbonization-activation, from room temperature, 3
DEG C/heating rate of min is warming up to 1000 DEG C of target temperature, keep the temperature 0.5 h；It is cooled to room temperature after reaction, takes out carbonization
Activation products are simultaneously washed with 3 M HCl solutions, then are washed with deionized to neutrality, 50 W, 2 h of ultrasound, by the product after ultrasound
It is dry, obtain biomass-based graded porous carbon.Porous carbon obtained by the present embodiment is in three-electrode system, with 1 M H2SO4Electrolyte
Electro-chemical test is carried out, when sweep speed is 20 mV/s, specific capacitance is 316.08 F/g.The ratio of porous carbon obtained by the present embodiment
Capacitance size is as shown in Figure 6.
Embodiment 5
A kind of preparation method of biomass-based graded porous carbon of the present embodiment, specific preparation process is as follows:
(1) bagasse powder that 15 g shearing is screened to 80 mesh is weighed, bagasse powder, double salt systems and water are pressed to the quality of 1:1:1
Than mixing；Wherein, double salt systems select aluminium chloride (AlCl3) and potassium sulfate (K2SO4) system, the molar ratio of the two is 40:60.
High temperature and pressure hydro-thermal reaction kettle is added in the above mixture, heated sealed is stirred to react to 300 DEG C, and in 150 r/min constant temperature
5 h；It is cooled to room temperature after reaction, the solid product in reaction kettle is washed with deionized to neutrality, by the production after washing
80 DEG C of 24 h of drying of object, obtain pre- carbonized product；
(2) the pre- carbonized product of 6 g is weighed, by pre- carbonized product and sodium carbonate (Na2CO3) and silica (SiO2) press 1:0.5:5
Mass ratio be ground；Said mixture is placed in nitrogen atmosphere pipe type furnace and carries out carbonization-activation, from room temperature, 3 DEG C/
The heating rate of min is warming up to 600 DEG C of target temperature, keeps the temperature 8 h；It is cooled to room temperature after reaction, takes out carbonization-activation and produce
Object is simultaneously successively washed with the NaOH solution of 3 M HCl solutions and 20 % mass fractions, then is washed with deionized to neutrality, 80 W
80 DEG C of 24 h of drying of product after ultrasound are obtained biomass-based graded porous carbon by lower ultrasonic 8 h.It is porous obtained by the present embodiment
Carbon is in three-electrode system, with 1 M H2SO4Electrolyte carries out electro-chemical test, and when sweep speed is 20 mV/s, specific capacitance is
347.16 F/g.The specific capacitance size of porous carbon obtained by the present embodiment is as shown in Figure 6.
The specific surface area of biomass-based classifying porous carbon material prepared by the present invention is high, and range is 1000 ~ 2000
m2/ g, cellular structure is loose, has micropore/mesopore/macropore hierarchical structure；In three-electrode system, with 1 M H2SO4Electrolyte
Electro-chemical test is carried out, when sweep speed is 20 mV/s, specific capacitance is 294 ~ 347 F/g, has excellent supercapacitor
Can, and cyclical stability is high.
Above embodiments are only preferrred embodiment of the present invention, for explaining only the invention, are not intended to limit the present invention, this
Field technical staff should belong to guarantor of the invention without departing from change made under spirit of the invention, replacement, modification etc.
Protect range.
Claims (10)
1. a kind of preparation method of biomass-based graded porous carbon, which comprises the steps of:
(1) double salt templates and powdered biomass are successively added to the water, are sealed, it is low under conditions of 100 ~ 200 r/min stirring
The pre- carbonization of warm water heat, is cooled to room temperature, filters to take precipitating, and washing, drying obtain pre- carbonized product；
(2) take pre- carbonized product made from step (1) and activator, template ground and mixed uniform, then in an inert atmosphere
It is warming up to 600-1000 DEG C, carbonization-activation 0.5-8 h, carbonized product is washed with water and washs to neutrality after removing impurity, and it is dry,
Obtain the biomass-based graded porous carbon.
2. preparation method according to claim 1, which is characterized in that in step (1), the powdered biomass is will be biological
The shearing sieving of matter raw material obtains, and powdered biomass particle size is 20-80 mesh；The biomass material is rice straw, jade
One or more of rice stalk, straw, bagasse, peanut shell.
3. preparation method according to claim 1, which is characterized in that powdered biomass described in step (1), double salt templates
Mass ratio with water is 1:(1 ~ 5): (1 ~ 10).
4. preparation method according to claim 1, which is characterized in that double salt templates described in step (1) be KCl, LiCl,
NaCl、ZnCl2、AlCl3、K2SO4In two kinds；Molar ratio between double salt templates is (25 ~ 60): (25 ~ 75).
5. preparation method according to claim 1, which is characterized in that low-temperature hydrothermal described in step (1) is in advance at carbonization
The temperature of reason is 180 ~ 300 DEG C, and the time is 5 ~ 20 h.
6. preparation method according to claim 1, which is characterized in that activator described in step (2) is KOH, K2CO3、
KHCO3、K2C2O4、Na2CO3One or more of；The mass ratio of activator and pre- carbonized product is (0.5 ~ 5): 1；The template
Agent is SiO2、CaCO3、Al2O3、MgCO3One or more of；The mass ratio of template and pre- carbonized product is (0.25 ~ 5): 1.
7. preparation method according to claim 1, which is characterized in that the inert atmosphere is nitrogen or argon gas, is warming up to
The heating rate of the heat treatment temperature is 3 ~ 10 DEG C/min.
8. preparation method according to claim 1, which is characterized in that removal impurity described in step (2) is the M of 0.5 M ~ 3
HCl solution pickling, the NaOH solution alkali cleaning that mass fraction is 10% ~ 30%, 50 ~ 80 W be ultrasonically treated one of 2 ~ 8 h with
On.
9. a kind of biomass-based graded porous carbon as made from any one of the claim 1-8 preparation method.
10. a kind of biomass-based graded porous carbon according to claim 9, it is characterised in that: described biomass-based porous
The specific surface area of carbon is 1000 ~ 2000 m2/g；In three-electrode system, with 1 M H2SO4Electrolyte carries out electro-chemical test, sweeps
Retouch rate be 20 mV/s when, specific capacitance be 294 ~ 347 F/g.
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