CN106744793B - 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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Abstract
A kind of alkali lignin based super capacitor porous carbon material and its preparation method and application, by the alkali lignin slightly purified in black liquid and triblock polymer Pluronic F127 and Mg (CH3COO)2·4H2O mixing, is added formaldehyde and hydrochloric acid stirs to obtain mixed liquor；Above-mentioned mixed liquor is placed in drying in baking oven, obtains dark brown solid；Then dark brown solid is placed in tube furnace and carries out carbonization reaction, be continually fed into nitrogen after reaction or inert gas is cooled to room temperature；Pickling, washing are finally carried out, obtains the porous carbon material of black powder after dry.Resulting materials can be applied in double electric layers supercapacitor, in carbonization process, without using strong corrosives chemical substances such as strong acid, highly basic, be preferably minimized to the loss of equipment；The raw materials used by-product in pulp and paper industry, realizes maximally utilizing for resource, and lignin is from a wealth of 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, prepares the application of porous carbon material and this material in terms of supercapacitor by double-template method.
Background technique
Lignin is the renewable resource abundant of content second in nature, is only second to cellulose, while being that nature contains
Measure aromatics high molecular polymer the most abundant.However, current by-product of the lignin as pulp and paper industry, does not have always
It can be utilized effectively, also create certain environmental pollution.Contain a large amount of phenylpropyl alcohol alkyl structure, carbon content in lignin molecule
More than 60%, not only rich content, from a wealth of sources but also low in cost, therefore be to prepare the most promising ideal forerunner of Carbon Materials
One of body.Increasingly depleted with the energy and resource, the storing technology of the energy is quickly grown.Carbon Materials are because have compared with Gao Bibiao
Area and micropore abundant and central hole structure and have good charge storage capacity, reversibly adsorbed in double layer capacitor
Ion in electrolyte is widely applied as electrode material.
Active carbon is prepared by raw material of lignin at present, and uses other biological matter raw material (such as coconut husk, shell or sawdust
Deng) preparation method it is identical, mostly with traditional physical activation method, chemical activation method or physical-chemical combination activation method based on, system
Standby absorbent charcoal material has high specific surface area and flourishing pore structure, is a kind of ideal adsorbent material and storage
It can material.But its pore structure is based on micropore, it is poor to the adsorbing separation of macromolecular and other effects.And it is limited by aperture,
Molecule largely conveys slowly, and conductivity is low, and a large amount of functional groups in surface and defect lead to high-temperature process or graphitization Shi Kongjie
Structure is easy to collapse.Mesoporous Carbon Materials, have larger aperture and high specific surface area, and duct rule, pore-size distribution are narrow.Therefore, in
The preparation and research and development of hole Carbon Materials are increasingly becoming the research hotspot and advanced subject of Carbon Materials science in recent years.
It, perhaps can adjustment hole size to a certain extent by adjusting charing and activating process.But complex process, cost
It greatly increases.The structure-directing effect of template is utilized in 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 without using corrosivity such as strong acid, highly basic in carbonization process
Chemical substance, it is smaller to the damage of equipment, it is the preparation process of more convenient close friend a kind of.
Summary of the invention
The technical issues of solution: the present invention provides a kind of alkali lignin based super capacitor porous carbon material and its systems
Preparation Method and application, the material have good chemical property when being applied in double electric layers supercapacitor.And the present invention
Use the by-product alkali lignin in pulp and paper industry for raw material, " turning waste into wealth " realizes maximally utilizing for resource, together
When slow down influence of the papermaking wastewater to environment.
Technical solution: the preparation method of alkali lignin based super capacitor porous carbon material will slightly mention in black liquid
Pure alkali lignin and triblock polymer Pluronic F127 and Mg (CH3COO)2·4H2O mixing, wherein alkali lignin with
The mass ratio of Pluronic F127 is 1:(1 ~ 3), Mg (CH3COO)2·4H2The additional amount of O is the 1 ~ 10 of alkali lignin quality
Times, formaldehyde is added and hydrochloric acid stirs to obtain mixed liquor, formaldehyde additional amount is the 1% ~ 2% of total solution volume, and hydrochloric acid is added
Amount is the 0.5% ~ 1% of total solution volume；Above-mentioned mixed liquor is placed in drying in 40 DEG C ~ 80 DEG C baking ovens, obtains dark brown solid；So
Dark brown solid is placed in tube furnace afterwards and carries out carbonization reaction, carbonization temperature is 800 DEG C ~ 1000 DEG C, and carbonization reaction is with program
The mode of heating, carries out under nitrogen or inert gas shielding, is continually fed into nitrogen after reaction or inert gas is cooled to
Room temperature；Pickling, washing are finally carried out, obtains the alkali lignin based super capacitor porous carbon of black powder after dry
Material.
The thick method of purification of above-mentioned alkali lignin are as follows: after alkali lignin is dissolved in water in black liquid, adjusted with inorganic acid
PH to 7 ~ 9 takes filtrate after filtering；It then proceedes to inorganic acid for adjusting pH to 2 ~ 3, stirring 6h ~ 9h, mistake in 70 DEG C ~ 100 DEG C
Filter, the alkali lignin washed 2 ~ 3 times and slightly purified after drying.
Above-mentioned alkali lignin is dissolved in 200mL ~ 400mL tetra- according to the mass ratio of 1:1,1:2 or 1:3 with Pluronic F127
In hydrogen furans, the Mg (CH of 1 ~ 10 times 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.
Program temperature-rising method is with 1 DEG C/min rate to be heated to 300 DEG C ~ 400 DEG C in above-mentioned carbonization process, 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 of hydrochloric acid, sulfuric acid；It is described
Washing, which refers to, to be washed with deionized 2 ~ 3 times.
Alkali lignin based super capacitor porous carbon material is made to obtain in the above method, which is black powder
Shape solid particle, mesoporous >=81%, aperture integrated distribution are up to 682.3 ~ 853.4m in 6 ~ 10nm, specific surface area2/ g, total hole
Volume is 0.73 ~ 1.02cm3/g。
Above-mentioned porous carbon material is preparing the application in double electric layers supercapacitor electrode.
When concrete application, the electrode material is by porous carbon material: acetylene black: polytetrafluoroethylene (PTFE)=85%:10%:
5% mass ratio is formulated.
The utility model has the advantages that the present 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, without using the strong corrosives such as strong acid, highly basic chemistry
Substance is preferably minimized the loss of equipment.The raw materials used by-product in pulp and paper industry, " turning waste into wealth " realizes
Resource maximally utilizes.And lignin is from a wealth of sources, cheap, reduces production cost, meets the reason of Green Chemistry
It reads.The chemical property of the porous carbon material is good, has the characteristics that electrochemical cycle stability, specific capacitance are high, or even in 1A/g
Current density under, still keep the specific capacitance of 73.1 ~ 141.4F/g.
Detailed description of the invention
Fig. 1 is nitrogen adsorption/desorption isotherm of the product of the preparation of the embodiment of the present invention 2 at 77K: adsorption isothermal curve
In there are hysteresis loop, according to the classification of IUPAC, be IV type adsorption isotherm, show that there are a large amount of central hole structures.
Fig. 2 is the graph of pore diameter distribution that product prepared by the embodiment of the present invention 2 uses DFT method to be calculated: 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
Corresponding sweep speed is followed successively by 10mVs to curve from inside to outside-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 stable, 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 further explained, specific embodiment following is a brief introduction of.These embodiments are only limitted to illustrate the present invention
Rather than it limits the scope of the invention.The change or modification of any pair of equivalent form of the present invention are wanted 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；It then proceedes to
With inorganic acid for adjusting pH to 3, filtering, washing 3 times, the alkali lignin slightly purified after dry.
Alkali lignin 35g after weighing thick purification is dissolved in 870mL water, with dilute sulfuric acid tune pH to neutrality, is filtered.It takes
Filtrate is continued with dilute sulfuric acid tune pH value of solution to 2.5, and flow back 8h in 80 DEG C of oil bath pans.Filtering, washing 3 times extremely neutral and dryings
For use.Weigh 10g alkali lignin, 10g polyethers F127 and 32g Mg (CH3COO)2·4H2O is dissolved in the four of 550mL volume ratio 1:1
In hydrogen furans and water mixed solution, 2mL formaldehyde and 1.5mL hydrochloric acid is added, and stir.Above-mentioned mixing liquid is placed in
It is dry in 75 DEG C, obtain dark brown blocks of solid.Then 400 DEG C are heated to 1 DEG C/min rate under nitrogen protection, then with
5 DEG C/min is heated to 1000 DEG C from 400 DEG C and is carbonized, and 15min is kept at 1000 DEG C, nitrogen is then continually fed into and is cooled to
Room temperature obtains black bulk Carbon Materials.Finally use the dilute sulfuric acid dip of 2mol/L to neutrality, deionization is washed 2 times, is placed in 105 DEG C
Dry 12h obtains final porous carbon material for supercapacitor in baking oven.The porous carbon material that above-mentioned steps are obtained is abundant
Partial size is ground to less than 10 μm, according to porous carbon material: acetylene black: the mass ratio of PTFE=85%:10%:5% prepares electrode material,
With 1mol/L H2SO4Its chemical property is measured under three-electrode system for electrolyte.
The porous carbon material BET specific surface area is up to 679.4m2/ g, total hole volume 0.83cm3/g.In the electric current of 1A/g
Under density, specific capacitance can reach 101.4F/g.
Embodiment 2
It takes black liquid 500mL to be diluted in 1000mL water, with dilute hydrochloric acid tune pH to neutrality, is filtered.Filtrate is taken, after
Continuous to adjust pH value of solution to 2, flow back 8h in 90 DEG C of oil bath pans.Filtering, washing 2 times are to neutral and dry that alkali lignin is stand-by.It takes
10g alkali lignin, 15g polyethers F127 and 42.6g Mg (CH3COO)2·4H2O is dissolved in the tetrahydrofuran of 600mL volume ratio 1:1
In water mixed solution, 2mL formaldehyde and 1.3mL hydrochloric acid is added, and stir.Above-mentioned mixing liquid is placed in 70 DEG C
It is dry, obtain dark brown blocks of solid.Then 70 DEG C are heated to by room temperature with 10 DEG C/min rate under nitrogen protection, with 2 DEG C/
Min rate is heated to 400 DEG C, is then heated to 1000 DEG C from 400 DEG C with 2 DEG C/min and is carbonized, is kept at 1000 DEG C
Then 30min is continually fed into nitrogen and is cooled to room temperature to obtain black bulk Carbon Materials.It finally is washed till neutrality with dilute hydrochloric acid, is spent
Ion is washed 2 times, is placed in 105 DEG C of baking ovens dry 12h and is obtained final porous carbon material for supercapacitor.By above-mentioned steps
Obtained porous carbon material is fully ground to partial size less than 10 μm, according to porous carbon material: acetylene black: PTFE=85%:10%:5%
Mass ratio prepare active electrode material, with 1mol/L H2SO4Its chemical property is measured under three-electrode system for electrolyte.
The porous carbon material BET specific surface area is up to 711.9m2/ g, total hole volume 0.90cm3/ g, mesopore volume product are 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；It then proceedes to
With inorganic acid for adjusting pH to 3, filtering, washing 3 times, the alkali lignin slightly purified after dry.
Alkali lignin 30g after weighing thick purification is dissolved in 800mL water, with dilute sulfuric acid tune pH to neutrality, is filtered.It takes
Filtrate continues to adjust pH value of solution to 2, and flow back 9h in 80 DEG C of oil bath pans.Filtering, washing 3 times extremely neutral and dried for standby.It weighs
10g alkali lignin, 32g polyethers F127 and 21.3g Mg (CH3COO)2·4H2O is dissolved in the tetrahydrofuran of 400mL volume ratio 4:6
In the mixed solution of water, 2mL formaldehyde and 1.34mL hydrochloric acid is added, and stir.Above-mentioned mixing liquid is placed in 70
It is dry 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 from 300 DEG C and is carbonized, and 30min is kept at 900 DEG C, nitrogen is then continually fed into and is cooled to room temperature
To black bulk Carbon Materials.It finally is washed till neutrality with the dilute hydrochloric acid of 1mol/L, is then washed with deionized water 2 times, 105 DEG C of bakings are placed in
Dry 12h obtains final porous carbon material for supercapacitor in case.The porous carbon material that above-mentioned steps obtain sufficiently is ground
Partial size is milled to less than 10 μm, according to porous carbon material: acetylene black: the mass ratio of PTFE=85%:10%:5% prepares active electrode material
Material, with 1mol/L H2SO4Its chemical property is measured under three-electrode system for electrolyte.
The porous carbon material specific surface area is up to 682.3m2/ g, total hole volume 0.88cm3/g.In the current density of 1A/g
Under, specific capacitance can reach 107.9F/g.
Claims (8)
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 mixing, the alkali lignin it is thick
Method of purification are as follows: after alkali lignin is dissolved in water in black liquid, with inorganic acid for adjusting pH to 7 ~ 9, take filtrate after filtering；Then
Continue with inorganic acid for adjusting pH to 2 ~ 3, stirring 6h ~ 9h in 70 DEG C ~ 100 DEG C, filtering is washed 2 ~ 3 times and obtained after drying thick
The alkali lignin of purification；The alkali lignin and Pluronic F127 according to the mass ratio of 1:1,1:2 or 1:3 be dissolved in 200mL ~
In 400mL tetrahydrofuran, the Mg (CH of 1 ~ 10 times of alkali lignin quality is then weighed3COO)2·4H2O is dissolved in 200mL ~ 400mL
In water, finally two kinds of solution are mixed, formaldehyde is added and hydrochloric acid stirs to obtain mixed liquor, formaldehyde additional amount is total solution
The 1% ~ 2% of volume, hydrochloric acid additional amount are 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 done
It is dry, obtain dark brown solid；Then dark brown solid is placed in tube furnace and carries out carbonization reaction, carbonization temperature be 800 DEG C ~
1000 DEG C, carbonization reaction is carried out under nitrogen or inert gas shielding, is continually fed into after reaction in a manner of temperature programming
Nitrogen or inert gas are cooled to room temperature；Pickling, washing are finally carried out, the alkali lignin base that black powder is obtained after dry is super
Grade capacitor porous carbon material.
2. the preparation method of alkali lignin based super capacitor porous carbon material according to claim 1, feature exist
It is 2mL in the optimum amount of the formaldehyde, the concentration of hydrochloric acid is 6mol/L.
3. the preparation method of alkali lignin based super capacitor porous carbon material according to claim 1, feature exist
It is that argon gas or any of nitrogen argon compare gaseous mixture in the inert gas.
4. the preparation method of alkali lignin based super capacitor porous carbon material according to claim 1, feature exist
Program temperature-rising method is with 1 DEG C/min rate to be heated to 300 DEG C ~ 400 DEG C in the carbonization process, 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.
5. the preparation method of alkali lignin based super capacitor porous carbon material according to claim 1, feature exist
Refer in the pickling with inorganic acid elution to neutrality, the inorganic acid is at least one of hydrochloric acid, sulfuric acid；The washing is
Finger is washed with deionized 2 ~ 3 times.
6. alkali lignin based super capacitor porous carbon material, feature made from any the method for claim 1 ~ 5 exist
In: the porous carbon material is black powder solid particle, and mesoporous >=81%, aperture integrated distribution is in 6 ~ 10nm, specific surface area
Up to 682.3 ~ 853.4m2/ g, total hole volume are 0.73 ~ 1.02cm3/g。
7. porous carbon material described in claim 6 is preparing the application in double electric layers supercapacitor electrode.
8. application according to claim 7, it is characterised in that the electrode material is by porous carbon material: acetylene black: poly- four
Vinyl fluoride (PTFE)=85%:10%:5% mass ratio is formulated.
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Families Citing this family (5)
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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 |
| CN109485029B (en) | 2018-11-19 | 2020-07-28 | 华南理工大学 | Lignin porous carbon nanosheet, preparation method thereof and application thereof in supercapacitor electrode material |
| 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 |
| 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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