CN106744793A - A kind of alkali lignin based super capacitor porous carbon material and its preparation method and application - Google Patents
A kind of alkali lignin based super capacitor porous carbon material and its preparation method and application Download PDFInfo
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- CN106744793A CN106744793A CN201611094497.3A CN201611094497A CN106744793A CN 106744793 A CN106744793 A CN 106744793A CN 201611094497 A CN201611094497 A CN 201611094497A CN 106744793 A CN106744793 A CN 106744793A
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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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- 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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
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- C01P2006/14—Pore volume
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/40—Electric properties
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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
A kind of alkali lignin based super capacitor porous carbon material and its preparation method and application, by the alkali lignin and triblock polymer Pluronic F127 and Mg (CH of thick purification in black liquid3COO)2·4H2O mixes, and adds formaldehyde to stir to obtain mixed liquor with hydrochloric acid；Above-mentioned mixed liquor is placed in baking oven and is dried, obtain dark brown solid；Then dark brown solid is placed in carries out carbonization reaction in tube furnace, reaction is continually fed into nitrogen after terminating or inert gas is cooled to room temperature；Pickling, washing are finally carried out, the porous carbon material of black powder is obtained after drying.Resulting materials can be applied in double electric layers supercapacitor, in carbonization process, the severe corrosive chemical substance such as strong acid, highly basic not used, and the loss to equipment is preferably minimized；The raw materials used accessory substance in pulp and paper industry, realizes maximally utilizing for resource, and lignin wide material sources, cheap, reduces production cost.
Description
Technical field
It is specifically a kind of to utilize the renewable money of biomass the present invention relates to a kind of preparation method and application of porous carbon material
Source lignin is raw material, and porous carbon material, and application of this material in terms of ultracapacitor are prepared by double-template method.
Background technology
Lignin is the abundant renewable resource of content second in nature, cellulose is only second to, while being that nature contains
Amount aromatics high molecular polymer the abundantest.However, lignin does not have always as the accessory substance of pulp and paper industry at present
Can be utilized effectively, also create certain environmental pollution.Contain substantial amounts of phenylpropyl alcohol alkyl structure, carbon content in lignin molecule
More than 60%, not only rich content, wide material sources, and also it is with low cost, therefore be to prepare the most promising preferable forerunner of Carbon Materials
One of body.With the energy and the increasingly depleted of resource, the storing technology of the energy quickly grows.Carbon Materials are because have compared with Gao Bibiao
Area and abundant micropore and central hole structure and possess good charge storage capacity, reversibly adsorbed in double layer capacitor
Ion in electrolyte, extensive use is electrode material.
Activated carbon is prepared by raw material of lignin at present, with use other biological matter raw material（Such as coconut husk, shell or wood chip
Deng）Preparation method it is identical, more with traditional physical activation method, chemical activation method or physical-chemical combination activation method based on, system
Standby absorbent charcoal material has the pore structure of high specific surface area and prosperity, is a kind of ideal sorbing material and storage
Can material.It is poor to the adsorbing separation of macromolecular and other effects but its pore structure is based on micropore.And limited by aperture,
Largely conveying is slow for molecule, and conductivity is low, and a large amount of functional groups in surface and defect are tied in hole when causing high-temperature process or graphitization
Structure easily caves in.Mesoporous Carbon Materials, with larger aperture and high specific surface area, duct rule, pore-size distribution are narrow.Therefore, in
The preparation of hole Carbon Materials is increasingly becoming the study hotspot and advanced subject of Carbon Materials science in recent years with research and development.
By adjusting charing and activating process, perhaps can adjustment hole size to a certain extent.But complex process, cost
Greatly increase.Template make use of the structure-directing effect of template, by change templating nanoparticles space size and shape, with
And its order of structure, it is restricted organic matter carbonizing process therein, and then control the structure of Carbon Materials.Template
Appearance makes it possible that the aperture of porous carbon material accurately regulates and controls.And the corrosivity such as strong acid, highly basic are not used in carbonization process
Chemical substance, the damage to equipment is smaller, is a kind of more convenient friendly preparation technology.
The content of the invention
The technical problem of solution：The invention provides a kind of alkali lignin based super capacitor porous carbon material and its system
Preparation Method and application, possess good chemical property when the materials application is in double electric layers supercapacitor.And the present invention
It is raw material to use the accessory substance alkali lignin in pulp and paper industry, " turning waste into wealth ", realizes maximally utilizing for resource, together
When slow down influence of the papermaking wastewater to environment.
Technical scheme：The preparation method of alkali lignin based super capacitor porous carbon material, will slightly carry in black liquid
Pure alkali lignin and triblock polymer Pluronic F127 and Mg (CH3COO)2·4H2O mix, wherein alkali lignin with
The mass ratio of Pluronic F127 is 1：（1~3）, Mg (CH3COO)2·4H2The addition of O is the 1 ~ 10 of alkali lignin quality
Times, add formaldehyde to stir to obtain mixed liquor with hydrochloric acid, formaldehyde addition is the 1% ~ 2% of total solution volume, and hydrochloric acid is added
Measure is the 0.5% ~ 1% of total solution volume；Above-mentioned mixed liquor is placed in 40 DEG C ~ 80 DEG C baking ovens and is dried, obtain dark brown solid；So
Dark brown solid is placed in afterwards carry out carbonization reaction in tube furnace, carbonization temperature is 800 DEG C ~ 1000 DEG C, and carbonization reaction is with program
The mode of intensification, is carried out under nitrogen or inert gas shielding, and reaction is continually fed into nitrogen after terminating or inert gas is cooled to
Room temperature；Pickling, washing are finally carried out, the alkali lignin based super capacitor porous carbon of black powder is obtained after drying
Material.
The thick method of purification of above-mentioned alkali lignin is：After alkali lignin is dissolved in water in black liquid, adjusted with inorganic acid
PH to 7 ~ 9, takes filtrate after filtering；Then proceed to, with inorganic acid for adjusting pH to 2 ~ 3,6h ~ 9h, mistake be stirred in 70 DEG C ~ 100 DEG C
Filter, wash 2 ~ 3 times and the alkali lignin for slightly purifying is obtained after drying.
Above-mentioned alkali lignin is with Pluronic F127 according to 1:1、1:2 or 1:3 mass ratio is dissolved in 200mL ~ 400mL tetra-
In hydrogen furans, 1 ~ 10 times of Mg (CH of alkali lignin quality is then weighed3COO)2·4H2O is dissolved in 200mL ~ 400mL water, most
Two kinds of solution are mixed afterwards.
Preferably, the optimum amount of above-mentioned formaldehyde is 2mL, and the concentration of hydrochloric acid is 6mol/L.
Above-mentioned inert gas is that argon gas or any of nitrogen argon compare gaseous mixture.
Above-mentioned carbonization process Program temperature-rising method is to be heated to 300 DEG C ~ 400 DEG C with 1 DEG C/min speed, then proceed to
2 ~ 5 DEG C/min is heated to 800 DEG C ~ 1000 DEG C and is carbonized, and 15min ~ 60min is kept under target temperature.
Above-mentioned pickling refers to that with inorganic acid elution to neutrality, the inorganic acid is at least one in hydrochloric acid, sulfuric acid；It is described
Washing refers to be washed with deionized 2 ~ 3 times.
The above method is obtained to obtain alkali lignin based super capacitor porous carbon material, and the porous carbon material is black powder
Shape solid particle, mesoporous >=81%, aperture integrated distribution is up to 682.3 ~ 853.4m in 6 ~ 10nm, specific surface area2/ g, total hole
Volume is 0.73 ~ 1.02cm3/g。
Application of the above-mentioned porous carbon material in double electric layers supercapacitor electrode is prepared.
During concrete application, the electrode material is by porous carbon material:Acetylene black:Polytetrafluoroethylene (PTFE)（PTFE）=85%:10%:
5% mass ratio is formulated.
Beneficial effect：The invention provides a kind of black liquid alkali lignin by double-template prepare porous carbon material and its
Preparation method, and be applied in double electric layers supercapacitor.In carbonization process, the severe corrosives such as strong acid, highly basic chemistry is not used
Material, the loss to equipment is preferably minimized.The raw materials used accessory substance in pulp and paper industry, " turning waste into wealth ", realizes
Resource is maximally utilized.And it is lignin wide material sources, cheap, production cost is reduced, meet the reason of Green Chemistry
Read.The chemical property of the porous carbon material is good, with electrochemical cycle stability, specific capacitance is high the characteristics of, or even in 1A/g
Current density under, still keep the specific capacitance of 73.1 ~ 141.4F/g.
Brief description of the drawings
Fig. 1 is nitrogen adsorption/desorption isotherm of the product of the preparation of the embodiment of the present invention 2 under 77K：Adsorption isothermal curve
In there is hysteresis loop, be IV type adsorption isotherm according to the classification of IUPAC, show there is substantial amounts of central hole structure.
Fig. 2 is the graph of pore diameter distribution that product prepared by the embodiment of the present invention 2 is calculated using DFT methods：The hole of 6 ~ 10nm
Structure is most abundant.
Fig. 3 is the product of the preparation of the embodiment of the present invention 2 using the cyclic voltammetry curve under CV method different scanning rates：4
Curve sweep speed corresponding from inside to outside is followed successively by 10mVs-1、20mV·s-1、50mV·s-1、100mV·s-1。
Fig. 4 is charging and discharging curve of the product of the preparation of the embodiment of the present invention 2 under the current density of 1A/g：By repeatedly following
After ring, specific capacitance still keeps stabilization, substantially undamped.
Fig. 5 is the product specific capacitance of the preparation of the embodiment of the present invention 2 with current density change curve.
Specific embodiment
For the present invention is expanded on further, specific embodiment is following is a brief introduction of.These embodiments are only limitted to the explanation present invention
Rather than limitation the scope of the present invention.Any change or modification to the equivalent form of value of the present invention will with the right for falling within the application
Seek book limited range.
Embodiment 1
After alkali lignin is dissolved in water in black liquid, with inorganic acid for adjusting pH to 9, filtrate is taken after filtering；Then proceed to use nothing
To 3, filtering, washing 3 times obtain the alkali lignin for slightly purifying to machine acid for adjusting pH after drying.
Weigh the alkali lignin 35g after thick purification to be dissolved in 870mL water, adjust pH to neutrality with dilute sulfuric acid, carry out suction filtration.Take
Filtrate, continuation dilute sulfuric acid adjusts pH value of solution to 2.5, and flow back 8h in 80 DEG C of oil bath pans.Filter, wash 3 times to neutrality and dry
It is stand-by.Weigh 10g alkali lignins, 10g polyethers F127 and 32g Mg (CH3COO)2·4H2O, is dissolved in 550mL volume ratios 1:The four of 1
In hydrogen furans and water mixed solution, 2mL formaldehyde and 1.5mL hydrochloric acid are added, and stir.Above-mentioned mixing liquid is placed in
Dried in 75 DEG C, obtain dark brown blocks of solid.Then 400 DEG C are heated to 1 DEG C/min speed under nitrogen protection, then with
5 DEG C/min is heated to 1000 DEG C and is carbonized from 400 DEG C, and 15min is kept at 1000 DEG C, is then continually fed into nitrogen and is cooled to
Room temperature, obtains black bulk Carbon Materials.Finally with the dilute sulfuric acid dip of 2mol/L to neutrality, deionization is washed 2 times, is placed in 105 DEG C
12h is dried in baking oven and obtains final porous carbon material for supercapacitor.The porous carbon material that above-mentioned steps are obtained is abundant
Particle diameter is ground to less than 10 μm, according to porous carbon material:Acetylene black:PTFE=85%:10%:5% mass ratio prepares electrode material,
With 1mol/L H2SO4For electrolyte determines its chemical property under three-electrode system.
The porous carbon material BET specific surface area is up to 679.4m2/ g, total hole volume is 0.83cm3/g.In the electric current of 1A/g
Under density, specific capacitance can reach 101.4F/g.
Embodiment 2
Take black liquid 500mL to be diluted in 1000mL water, adjust pH to neutrality with watery hydrochloric acid, carry out suction filtration.Filtrate is taken, continues to adjust
To 2, flow back pH value of solution 8h in 90 DEG C of oil bath pans.Filtering, washing 2 times are to neutral and dry that alkali lignin is stand-by.Take 10g alkali
Lignin, 15g polyethers F127 and 42.6g Mg (CH3COO)2·4H2O, is dissolved in 600mL volume ratios 1:1 tetrahydrofuran is mixed with water
Close in solution, add 2mL formaldehyde and 1.3mL hydrochloric acid, and stir.Above-mentioned mixing liquid is placed in 70 DEG C and is dried,
Obtain dark brown blocks of solid.Then 70 DEG C are heated to by room temperature with 10 DEG C/min speed under nitrogen protection, with 2 DEG C/min speed
Rate is heated to 400 DEG C, and being then heated to 1000 DEG C from 400 DEG C with 2 DEG C/min is carbonized, and 30min is kept at 1000 DEG C, so
After be continually fed into nitrogen be cooled to room temperature obtain black bulk Carbon Materials.Neutrality finally is washed till with watery hydrochloric acid, 2 are washed with deionized water
It is secondary, it is placed in and dries 12h in 105 DEG C of baking ovens and obtain final porous carbon material for supercapacitor.By above-mentioned steps obtain it is many
Hole Carbon Materials are fully ground to particle diameter less than 10 μm, according to porous carbon material:Acetylene black:PTFE=85%:10%:5% mass ratio
Active electrode material is prepared, with 1mol/L H2SO4For electrolyte determines its chemical property under three-electrode system.
The porous carbon material BET specific surface area is up to 711.9m2/ g, total hole volume is 0.90cm3/ g, mesopore volume product is high
Up to 0.75 cm3/g.Under the current density of 1A/g, specific capacitance can reach 111.6F/g.
Embodiment 3
After alkali lignin is dissolved in water in black liquid, with inorganic acid for adjusting pH to 9, filtrate is taken after filtering；Then proceed to use nothing
To 3, filtering, washing 3 times obtain the alkali lignin for slightly purifying to machine acid for adjusting pH after drying.
Weigh the alkali lignin 30g after thick purification to be dissolved in 800mL water, adjust pH to neutrality with dilute sulfuric acid, carry out suction filtration.Take
Filtrate, continues to adjust pH value of solution to 2, and flow back 9h in 80 DEG C of oil bath pans.Filtering, 3 extremely neutral simultaneously dried for standby of washing.Weigh
10g alkali lignins, 32g polyethers F127 and 21.3g Mg (CH3COO)2·4H2O, is dissolved in 400mL volume ratios 4:6 tetrahydrofuran
In the mixed solution of water, 2mL formaldehyde and 1.34mL hydrochloric acid are added, and stir.Above-mentioned mixing liquid is placed in 70
Dried in DEG C, obtain dark brown blocks of solid.Then 300 DEG C are heated to 1 DEG C/min under nitrogen protection, then with 5 DEG C/
Min is heated to 900 DEG C and is carbonized from 300 DEG C, and 30min is kept at 900 DEG C, is then continually fed into nitrogen and is cooled to room temperature and obtains
To black bulk Carbon Materials.Neutrality finally is washed till with the watery hydrochloric acid of 1mol/L, is then washed with deionized water 2 times, be placed in 105 DEG C of bakings
12h is dried in case and obtains final porous carbon material for supercapacitor.The porous carbon material that above-mentioned steps are obtained fully is ground
Particle diameter is milled to less than 10 μm, according to porous carbon material:Acetylene black:PTFE=85%:10%:5% mass ratio prepares active electrode material
Material, with 1mol/L H2SO4For electrolyte determines its chemical property under three-electrode system.
The porous carbon material specific surface area is up to 682.3m2/ g, total hole volume is 0.88cm3/g.In the current density of 1A/g
Under, specific capacitance can reach 107.9F/g.
Claims (10)
1. the preparation method of alkali lignin based super capacitor porous carbon material, it is characterised in that will slightly be purified in black liquid
Alkali lignin and triblock polymer Pluronic F127 and Mg (CH3COO)2·4H2O mix, wherein alkali lignin with
The mass ratio of Pluronic F127 is 1：（1~3）, Mg (CH3COO)2·4H2The addition of O is the 1 ~ 10 of alkali lignin quality
Times, add formaldehyde to stir to obtain mixed liquor with hydrochloric acid, formaldehyde addition is the 1% ~ 2% of total solution volume, and hydrochloric acid is added
Measure is the 0.5% ~ 1% of total solution volume；Above-mentioned mixed liquor is placed in 40 DEG C ~ 80 DEG C baking ovens and is dried, obtain dark brown solid；So
Dark brown solid is placed in afterwards carry out carbonization reaction in tube furnace, carbonization temperature is 800 DEG C ~ 1000 DEG C, and carbonization reaction is with program
The mode of intensification, is carried out under nitrogen or inert gas shielding, and reaction is continually fed into nitrogen after terminating or inert gas is cooled to
Room temperature；Pickling, washing are finally carried out, the alkali lignin based super capacitor porous carbon of black powder is obtained after drying
Material.
2. the preparation method of alkali lignin based super capacitor porous carbon material according to claim 1, its feature exists
It is in the thick method of purification of the alkali lignin：After alkali lignin is dissolved in water in black liquid, with inorganic acid for adjusting pH to 7 ~
9, filtrate is taken after filtering；Then proceed to, with inorganic acid for adjusting pH to 2 ~ 3,6h ~ 9h, filtering, washing 2 be stirred in 70 DEG C ~ 100 DEG C
~ 3 times and the slightly alkali lignin that purifies is obtained after drying.
3. the preparation method of alkali lignin based super capacitor porous carbon material according to claim 1, its feature exists
In the alkali lignin and Pluronic F127 according to 1:1、1:2 or 1:3 mass ratio is dissolved in 200mL ~ 400mL tetrahydrofurans
In, then weigh 1 ~ 10 times of Mg (CH of alkali lignin quality3COO)2·4H2O is dissolved in 200mL ~ 400mL water, finally by two
Plant solution mixing.
4. the preparation method of alkali lignin based super capacitor porous carbon material according to claim 1, its feature exists
It is 2mL in the optimum amount of the formaldehyde, the concentration of hydrochloric acid is 6mol/L.
5. the preparation method of alkali lignin based super capacitor porous carbon material according to claim 1, its feature exists
It is that argon gas or any of nitrogen argon compare gaseous mixture in the inert gas.
6. the preparation method of alkali lignin based super capacitor porous carbon material according to claim 1, its feature exists
Be to be heated to 300 DEG C ~ 400 DEG C with 1 DEG C/min speed in the carbonization process Program temperature-rising method, then proceed to 2 ~ 5 DEG C/
Min is heated to 800 DEG C ~ 1000 DEG C and is carbonized, and 15min ~ 60min is kept under target temperature.
7. the preparation method of alkali lignin based super capacitor porous carbon material according to claim 1, its feature exists
Refer to that with inorganic acid elution to neutrality, the inorganic acid is at least one in hydrochloric acid, sulfuric acid in the pickling；The washing is
Finger is washed with deionized 2 ~ 3 times.
8. alkali lignin based super capacitor porous carbon material obtained in any methods described of claim 1 ~ 7, its feature exists
In：The porous carbon material be black powder solid particle, mesoporous >=81%, aperture integrated distribution is in 6 ~ 10nm, specific surface area
Up to 682.3 ~ 853.4m2/ g, total hole volume is 0.73 ~ 1.02cm3/g。
9. application of the porous carbon material described in claim 9 in double electric layers supercapacitor electrode is prepared.
10. application according to claim 9, it is characterised in that the electrode material is by porous carbon material:Acetylene black:Poly- four
PVF（PTFE）=85%:10%:5% mass ratio is formulated.
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| CN112216526A (en) * | 2020-09-25 | 2021-01-12 | 贵港益乐科技发展有限公司 | Biomass-based porous carbon aerogel supercapacitor electrode material and preparation method thereof |
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| US11952278B2 (en) | 2018-11-19 | 2024-04-09 | South China University Of Technology | Lignin porous carbon nanosheet, preparation method therefor, and application thereof in supercapacitor electrode materials |
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| CN107555413B (en) * | 2017-09-12 | 2020-02-18 | 中国林业科学研究院林业新技术研究所 | Preparation method of nitrogen-doped ordered mesoporous carbon with adjustable nitrogen content |
| CN107934959A (en) * | 2017-12-05 | 2018-04-20 | 中国林业科学研究院林产化学工业研究所 | A kind of lignin-base grading-hole Carbon Materials and its preparation method and application |
| US11952278B2 (en) | 2018-11-19 | 2024-04-09 | South China University Of Technology | Lignin porous carbon nanosheet, preparation method therefor, and application thereof in supercapacitor electrode materials |
| CN112216526A (en) * | 2020-09-25 | 2021-01-12 | 贵港益乐科技发展有限公司 | Biomass-based porous carbon aerogel supercapacitor electrode material and preparation method thereof |
| CN113658806A (en) * | 2021-06-29 | 2021-11-16 | 广西大学 | Gel electrode doped with polyaniline in situ and preparation method and application thereof |
| CN113658806B (en) * | 2021-06-29 | 2022-09-06 | 广西大学 | Gel electrode doped with polyaniline in situ and preparation method and application thereof |
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