CN109336107A - A kind of preparation method of alkali lignin porous carbon electrode material - Google Patents

A kind of preparation method of alkali lignin porous carbon electrode material Download PDF

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CN109336107A
CN109336107A CN201811308120.2A CN201811308120A CN109336107A CN 109336107 A CN109336107 A CN 109336107A CN 201811308120 A CN201811308120 A CN 201811308120A CN 109336107 A CN109336107 A CN 109336107A
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alkali lignin
porous carbon
electrode material
carbon electrode
preparation
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CN109336107B (en
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郭大亮
沙力争
胡志军
张学金
刘蓓
袁康帅
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Zhejiang Lover Health Science and Technology Development Co Ltd
Zhejiang University of Science and Technology ZUST
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Zhejiang Lover Health Science and Technology Development Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/342—Preparation characterised by non-gaseous activating agents
    • C01B32/348—Metallic compounds
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • 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 preparation methods of alkali lignin porous carbon electrode material.The present invention quantitatively adds the alkali lignin of reference state sodium group using lignin dissolution and the preparation of the relationship of acid-base property; then pyrolysis carbonization and the priming reaction of the catalysis of state sodium group are combined under protective gas atmosphere; the alkali lignin porous carbon electrode material based on reference state sodium group activation is obtained, with this porous carbon electrode material group capacitor.The present invention can effectively improve the yield and specific surface area of porous carbon electrode material, optimize the constituent content of porous carbon electrode material simultaneously, can the electrode with excellent chemical property obtained, furthermore the present invention also has the characteristics that manufacturing process is simple, operates and be easy, can reduce environmental pollution.

Description

A kind of preparation method of alkali lignin porous carbon electrode material
Technical field
The present invention relates to a kind of preparation methods of alkali lignin porous carbon electrode material, belong to electrode material preparation field.
Background technique
Carbonaceous material is due to big specific surface area, adjustable aperture, excellent physical and chemical stability, easy processing Property and relatively low cost, thus receive maximax concern.Currently, many researchers be dedicated to developing it is novel carbon-based Electrode material, high performance capacitor, such as porous carbon, onion, carbon nanotube, carbon ball, carbon aerogels and graphene.Wherein, Porous carbon electrode material causes the broad interest of scientific research person as capacitor electrode material because they have it is sustainable before Body, the adjustable form of specific ion, simple preparation process and especially low cost.
Compared with coal, petroleum or its derived product, utilization is sustainable, cheap and environmental sound biomass energy storage It deposits especially noticeable.Nearly 1.5 hundred million tons of waste wood quality can be all generated all over the world every year, and the maximum application of lignin is directly to fire It burns and generates energy, this is there may be many persistence organic pollutants and causes serious environmental problem.In fact, lignin has There are high-carbon content and the molecular structure similar with pitch.Micropore provides site abundant in lignin-base porous carbon electrode material As the position of charge accumulated and mesoporous as the channel for shortening ion diffusion length, and macropore can serve as reservoir to buffer Electrolyte ion, so lignin-base porous carbon electrode material is a kind of good electrode material.Therefore, how lignin to be turned Being converted into excellent chemical property porous carbon electrode material for being simple and efficient is a urgent problem to be solved.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of alkali lignin porous carbon electrode material, the present invention can be with The yield and specific surface area of porous carbon electrode material are effectively improved, while optimizing the constituent content of porous carbon electrode material, can be made The electrode with excellent chemical property obtained；Furthermore also with manufacturing process, simple, operation is easy, can reduce the present invention The characteristics of environmental pollution.
Technical solution of the present invention: a kind of preparation method of alkali lignin porous carbon electrode material carries out in the steps below:
A, alkali lignin is added in deionized water in the ratio of mass parts 1:10-30, adds sodium hydroxide solution, alkali Lignin and sodium hydroxide reaction generate the alkali lignin of reference state sodium group, until alkali lignin fully reacting；
B, solution is centrifuged, supernatant liquor is taken to be freeze-dried；
C, by the powder after freeze-drying under the protection of protective gas, with 3-10 DEG C/min heating rate, by temperature liter Temperature arrives 750-850 DEG C, keeps 1.5-2.5h, finished product.
The preparation method of above-mentioned alkali lignin porous carbon electrode material carries out in the steps below:
A, alkali lignin is added in deionized water in the ratio of mass parts 1:20, adds the hydrogen that concentration is 0.1mol/L Sodium hydroxide solution, alkali lignin and sodium hydroxide reaction generate the alkali lignin of reference state sodium group, until alkali lignin reacts Completely；
B, solution is centrifuged, supernatant liquor is taken to be freeze-dried；
C, by the powder after freeze-drying under the protection of protective gas, with 5 DEG C/min heating rate, temperature is warming up to 800 DEG C, 2h is kept, is combined pyrolysis carbonization and the priming reaction of state sodium group catalysis alkali lignin, finished product.
The preparation method of alkali lignin porous carbon electrode material above-mentioned, the alkali lignin and sodium hydroxide reaction generate The chemical program of lignin reference state sodium group are as follows:
The preparation method of alkali lignin porous carbon motor material above-mentioned, the alkali lignin are acid precipitating alkali lignins.
The preparation method of alkali lignin porous carbon electrode material above-mentioned in step c, naturally cools to after heat preservation Room temperature washs finished product by dilute hydrochloric acid and deionized water, filtration drying after washing, obtains reference state sodium group activation system Standby alkali lignin base porous carbon electrode material finished product.
The preparation method of alkali lignin porous carbon electrode material above-mentioned, the concentration of the dilute hydrochloric acid are 0.1mol/L.
The preparation method of alkali lignin porous carbon electrode material above-mentioned, in step c, the protective gas is nitrogen.
Compared with the prior art, the present invention is chemically reacted using alkali lignin is molten with sodium hydroxide solution in deionized water Relationship quantitatively adds the alkali lignin of reference state sodium group, and the catalysis of state sodium group is then combined under the protection of protective gas Pyrolysis carbonization and priming reaction, obtain yield rate it is more sodium hydroxide catalyzed pyrolysis carbonization and priming reaction preparation it is porous Carbon electrode material yield rate is improved close to 1.6 times, and specific surface area is improved close to 3 times, while optimizing porous carbon electrodes The constituent content of material, so that the porous carbon electrode material of preparation is by micropore, small mesoporous and macropore composition, with this porous carbon electrodes Material group capacitor, chemical property and cycle performance are excellent.Preparation method of the present invention is simple, and alkali lignin is secondary as industry Product, it is cheap to be easy to obtain, waste resource bring environmental problem can not only be reduced, and huge economic effect can be brought Benefit.In addition, the present invention also passes through dilute hydrochloric acid and deionized water washs finished product, filtration drying after washing removes impurity, So that conveniently obtaining porous carbon electrode material sterling.And it employs nitrogen as protective gas, low in cost, warp with higher Ji interests.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
Embodiment 1: a kind of preparation method of alkali lignin porous carbon electrode material carries out in the steps below:
A, the acid precipitating alkali lignin of 10g absolute dry mass is added in the beaker equipped with 200ml deionized water, it is then slow It is slow that 0.1mol/L sodium hydroxide solution is added, until acid precipitating alkali lignin is completely dissolved, mixed solution is formed, and record addition The volume of sodium hydroxide solution is then analyzed to identify reference state sodium group in alkali lignin using ICP-AES and quantitative 31P-NMR Additive amount, wherein the chemical equation of the adding procedure of alkali lignin reference state sodium group be:
When acid precipitating alkali lignin be add to deionized water, acid precipitating alkali lignin can ionize out hydrogen ion, to its After middle addition sodium hydroxide solution, hydroxide ion in sodium hydroxide solution can be ionized out with acid precipitating alkali lignin hydrogen from Son, which combines, generates water, and sodium ion is integrated to hydrogen ion position in lignin phenol's hydroxyl at this time, realizes lignin reference state sodium group Addition.
B, after mixed solution being centrifuged, supernatant liquor is freeze-dried, sample is made；
C, it takes 2g sample to be put into porcelain boat, under nitrogen protection using mini type high temperature tube furnace, is heated up with 5 DEG C/min fast Temperature is warming up to 800 DEG C, keeps 2h by rate, is combined pyrolysis carbonization and the priming reaction of state sodium group catalysis alkali lignin, Alkali lignin base porous carbon electrode material is made；
D, room temperature is naturally cooled to after heat preservation, then by 0.1mol/L dilute hydrochloric acid and deionized water to alkali lignin Porous carbon electrode material is washed to pH value to 7, and filtration drying after washing obtains the alkali wood of reference state sodium group activation preparation Quality porous carbon electrode material sterling, and calculate the porous carbon electrode material of reference state sodium group activation alkali lignin preparation Yield rate is 46.5%.
Embodiment 2: a kind of preparation method of alkali lignin porous carbon electrode material carries out in the steps below:
A, the acid precipitating alkali lignin of 10g absolute dry mass is added in the beaker equipped with 150ml deionized water, it is then slow It is slow that 0.1mol/L sodium hydroxide solution is added, until acid precipitating alkali lignin is completely dissolved, mixed solution is formed, and record addition The volume of sodium hydroxide solution is then analyzed to identify reference state sodium group in alkali lignin using ICP-AES and quantitative 31P-NMR Additive amount, wherein the chemical equation of the adding procedure of alkali lignin reference state sodium group be:
When acid precipitating alkali lignin be add to deionized water, acid precipitating alkali lignin can ionize out hydrogen ion, to its After middle addition sodium hydroxide solution, hydroxide ion in sodium hydroxide solution can be ionized out with acid precipitating alkali lignin hydrogen from Son, which combines, generates water, and sodium ion is integrated to hydrogen ion position in lignin phenol's hydroxyl at this time, realizes lignin reference state sodium group Addition.
B, after mixed solution being centrifuged, supernatant liquor is freeze-dried, sample is made；
C, it takes 2g sample to be put into porcelain boat, under nitrogen protection using mini type high temperature tube furnace, is heated up with 4 DEG C/min fast Temperature is warming up to 760 DEG C, keeps 1.8h by rate, and pyrolysis carbonization and the activation for being combined state sodium group catalysis alkali lignin are anti- It answers, alkali lignin base porous carbon electrode material is made；
D, room temperature is naturally cooled to after heat preservation, then by 0.1mol/L dilute hydrochloric acid and deionized water to alkali lignin Porous carbon electrode material is washed to pH value to 7, and filtration drying after washing obtains the alkali wood of reference state sodium group activation preparation Quality porous carbon electrode material sterling, and calculate the porous carbon electrode material of reference state sodium group activation alkali lignin preparation Yield rate is 44.3%.
Embodiment 3: a kind of preparation method of alkali lignin porous carbon electrode material carries out in the steps below:
A, the acid precipitating alkali lignin of 10g absolute dry mass is added in the beaker equipped with 250ml deionized water, it is then slow It is slow that 0.1mol/L sodium hydroxide solution is added, until acid precipitating alkali lignin is completely dissolved, mixed solution is formed, and record addition The volume of sodium hydroxide solution is then analyzed to identify reference state sodium group in alkali lignin using ICP-AES and quantitative 31P-NMR Additive amount, wherein the chemical equation of the adding procedure of alkali lignin reference state sodium group be:
When acid precipitating alkali lignin be add to deionized water, acid precipitating alkali lignin can ionize out hydrogen ion, to its After middle addition sodium hydroxide solution, hydroxide ion in sodium hydroxide solution can be ionized out with acid precipitating alkali lignin hydrogen from Son, which combines, generates water, and sodium ion is integrated to hydrogen ion position in lignin phenol's hydroxyl at this time, realizes lignin reference state sodium group Addition.
B, after mixed solution being centrifuged, supernatant liquor is freeze-dried, sample is made；
C, it takes 2g sample to be put into porcelain boat, under nitrogen protection using mini type high temperature tube furnace, is heated up with 7 DEG C/min fast Temperature is warming up to 840 DEG C, keeps 2.2h by rate, and pyrolysis carbonization and the activation for being combined state sodium group catalysis alkali lignin are anti- It answers, alkali lignin base porous carbon electrode material is made；
D, room temperature is naturally cooled to after heat preservation, then by 0.1mol/L dilute hydrochloric acid and deionized water to alkali lignin Porous carbon electrode material is washed to pH value to 7, and filtration drying after washing obtains the alkali wood of reference state sodium group activation preparation Quality porous carbon electrode material sterling, and calculate the porous carbon electrode material of reference state sodium group activation alkali lignin preparation Yield rate is 45.3%.
Embodiment 4: a kind of preparation method of alkali lignin porous carbon electrode material carries out in the steps below:
A, the acid precipitating alkali lignin of 10g absolute dry mass is added in the beaker equipped with 300ml deionized water, it is then slow It is slow that 0.1mol/L sodium hydroxide solution is added, until acid precipitating alkali lignin is completely dissolved, mixed solution is formed, and record addition The volume of sodium hydroxide solution is then analyzed to identify reference state sodium group in alkali lignin using ICP-AES and quantitative 31P-NMR Additive amount, wherein the chemical equation of the adding procedure of alkali lignin reference state sodium group be:
When acid precipitating alkali lignin be add to deionized water, acid precipitating alkali lignin can ionize out hydrogen ion, to its After middle addition sodium hydroxide solution, hydroxide ion in sodium hydroxide solution can be ionized out with acid precipitating alkali lignin hydrogen from Son, which combines, generates water, and sodium ion is integrated to hydrogen ion position in lignin phenol's hydroxyl at this time, realizes lignin reference state sodium group Addition.
B, after mixed solution being centrifuged, supernatant liquor is freeze-dried, sample is made；
C, it takes 2g sample to be put into porcelain boat, under nitrogen protection using mini type high temperature tube furnace, is heated up with 7 DEG C/min fast Temperature is warming up to 810 DEG C, keeps 2.5h by rate, and pyrolysis carbonization and the activation for being combined state sodium group catalysis alkali lignin are anti- It answers, alkali lignin base porous carbon electrode material is made；
D, room temperature is naturally cooled to after heat preservation, then by 0.1mol/L dilute hydrochloric acid and deionized water to alkali lignin Porous carbon electrode material is washed to pH value to 7, and filtration drying after washing obtains the alkali wood of reference state sodium group activation preparation Quality porous carbon electrode material sterling, and calculate the porous carbon electrode material of reference state sodium group activation alkali lignin preparation Yield rate is 44.8%.
Embodiment 5: a kind of preparation method of alkali lignin porous carbon electrode material carries out in the steps below:
A, 10g alkali lignin is added in the beaker equipped with 200ml deionized water, is then slowly added to 0.1mol/L hydrogen Sodium hydroxide solution forms mixed solution until alkali lignin is completely dissolved, and records the volume that sodium hydroxide solution is added, with The additive amount of reference state sodium group in alkali lignin is analyzed to identify using ICP-AES and quantitative 31P-NMR afterwards, wherein alkali lignin The chemical equation of the adding procedure of reference state sodium group is:
When acid precipitating alkali lignin be add to deionized water, acid precipitating alkali lignin can ionize out hydrogen ion, to its After middle addition sodium hydroxide solution, hydroxide ion in sodium hydroxide solution can be ionized out with acid precipitating alkali lignin hydrogen from Son, which combines, generates water, and sodium ion is integrated to hydrogen ion position in lignin phenol's hydroxyl at this time, realizes lignin reference state sodium group Addition.
B, after mixed solution being centrifuged, supernatant liquor is freeze-dried, sample is made；
C, it takes 2g sample to be put into porcelain boat, under nitrogen protection using mini type high temperature tube furnace, is heated up with 5 DEG C/min fast Temperature is warming up to 800 DEG C, keeps 2h by rate, is combined pyrolysis carbonization and the priming reaction of state sodium group catalysis alkali lignin, Alkali lignin base porous carbon electrode material is made；
D, room temperature is naturally cooled to after heat preservation, then by 0.1mol/L dilute hydrochloric acid and deionized water to alkali lignin Porous carbon electrode material is washed to pH value to 7, and filtration drying after washing obtains the alkali wood of reference state sodium group activation preparation Quality porous carbon electrode material sterling, and calculate the porous carbon electrode material of reference state sodium group activation alkali lignin preparation Yield rate is 43.5%.
Reference examples: the acid precipitating alkali lignin of 10g absolute dry mass in 1 step a of embodiment is added and is combined in embodiment It receives in the sodium hydroxide solution of 0.1mol/L identical in quality, is freeze-dried after mixing, sample is made, remaining step is by real The operation for applying step b, c in example 1 carries out, and obtains the alkali lignin base porous carbon electrode material of sodium hydroxide activation preparation.Control Acid precipitating alkali lignin can be added directly into sodium hydroxide solution in example, at this time due to the effect of no deionized water, acid precipitating Alkali lignin will not ionize out hydrogen ion so that sodium ion will not in conjunction with hydrogen ion position in lignin phenol's hydroxyl, thus Carry out sodium hydroxide activation preparation obtains alkali lignin base porous carbon electrode material, calculates sodium hydroxide activation alkali lignin The yield of the porous carbon electrode material of preparation is 29.7%.
Above-described embodiment and reference examples are subjected to yield rate, constituent content and specific surface area statistics, obtained as shown in Table 1 As a result.
It sees from table 1 and clearly finds out, the finished product of the porous carbon electrode material of reference state sodium group activation alkali lignin preparation Rate is greater than 44%, and the yield that sodium hydroxide activates the porous carbon electrode material of alkali lignin preparation is 29.7%, in embodiment Finished rate is much greater than the pyrolysis carbonization and the yield rate of priming reaction of pressing common mode in reference examples and carry out alkali lignin, and make The preparation of porous carbon electrode material is carried out with acid precipitating alkali lignin, yield rate, constituent content better than use alkali lignin The porous carbon electrode material of preparation.This is because dealkalize can be carried out to alkali lignin using acid precipitating, so that acid precipitating alkali wood Quality reference state receives group, and a little inorganic states sodium is had also combined, so that sour in addition to reference state receives group in alkali lignin The result for precipitating the porous carbon motor material of alkali lignin preparation is preferable.Come from the constituent content of porous carbon electrode material obtained It sees, the content accounting of carbon significantly improves in the porous carbon electrode material of reference state sodium group activation alkali lignin preparation, hydrogen The content accounting of element, nitrogen and element sulphur declines, therefore the porous carbon electrode material prepared has micropore, small mesoporous and big Hole, so that specific surface area is much larger than the specific surface area in reference examples in embodiment.From above-mentioned data as can be seen that based on combining State receive group activation can obtain compared with high finished product rate and with high-specific surface area porous carbon electrode material.
The alkali lignin porous carbon electrode material and acetylene black, polytetrafluoroethyl-ne that above-described embodiment and reference examples are prepared Alkene according to mass ratio be 8:1:1 after mixing, be applied in nickel foam, be dried in vacuo 5h, electrode slice is made；Then with poly- third Alkene film is that diaphragm prepares capacitor in the pressure lower sheeting encapsulation of 10Mpa, measure it using the KOH solution of 6mol/L as electrolyte Cyclic voltamogram, the results are shown in Table 2:
Table 2
Experiments have shown that the capacitance that reference state sodium group activation alkali lignin prepares capacitor reaches 66F/g to 71F/g.Electricity When stream increases to 1A/g from 0.1A/g, the specific capacitance down ratio of porous carbon electrode material is little；It discharges in 1A/g super-large current In the case where recycle 500 times, whole specific capacitance still remains stable, and cycle performance is good.And in reference examples, sodium hydroxide activation The capacitance that alkali lignin prepares capacitor reaches 37F/g, as electric current increases to 1A/g, porous carbon electrode material from 0.1A/g Specific capacitance drop to 21F/g；Specific capacitance stability and cycle performance are not so good as reference state sodium group catalytic activation alkali lignin Porous carbon electrode material.
In conclusion the present invention quantitatively adds reference state sodium group using lignin dissolution and the preparation of the relationship of acid-base property Alkali lignin, be then combined under protective gas atmosphere state sodium group catalysis pyrolysis carbonization and priming reaction, obtain The porous carbon electrode material yield rate of the more sodium hydroxide catalyzed pyrolysis carbonization of yield rate and priming reaction preparation, which improves, to be connect Nearly 1.6 times, and specific surface area is improved close to 3 times, while optimizing the constituent content of porous carbon electrode material, so that preparation is more Hole carbon electrode material is by micropore, small mesoporous and macropore composition, with this porous carbon electrode material group capacitor, chemical property and Cycle performance is excellent.Preparation method of the present invention is simple, and for alkali lignin as industrial by-products, cheap easy acquisition can not only Waste resource bring environmental problem is reduced, and huge economic benefit can be brought.

Claims (7)

1. a kind of preparation method of alkali lignin porous carbon electrode material, it is characterised in that: carry out in the steps below:
A, alkali lignin is added in deionized water in the ratio of mass parts 1:10-30, adds sodium hydroxide solution, alkali is wooden Element and sodium hydroxide reaction generate the alkali lignin of reference state sodium group, until alkali lignin fully reacting；
B, solution is centrifuged, supernatant liquor is taken to be freeze-dried；
C, by the powder after freeze-drying under the protection of protective gas, with 3-10 DEG C/min heating rate, temperature is warming up to 750-850 DEG C, keep 1.5-2.5h, finished product.
2. the preparation method of alkali lignin porous carbon electrode material according to claim 1, it is characterised in that: press following steps It is rapid to carry out:
A, alkali lignin is added in deionized water in the ratio of mass parts 1:20, adds the hydroxide that concentration is 0.1mol/L Sodium solution, alkali lignin and sodium hydroxide reaction generate the alkali lignin of reference state sodium group, until alkali lignin fully reacting；
B, solution is centrifuged, supernatant liquor is taken to be freeze-dried；
C, by the powder after freeze-drying under the protection of protective gas, with 5 DEG C/min heating rate, temperature is warming up to 800 DEG C, 2h is kept, pyrolysis carbonization and the priming reaction of state sodium group catalysis alkali lignin, finished product are combined.
3. the preparation method of alkali lignin porous carbon electrode material according to claim 1 or 2, it is characterised in that: described Alkali lignin and sodium hydroxide reaction generate the chemical program of lignin reference state sodium group are as follows:
4. the preparation method of alkali lignin porous carbon motor material according to claim 1 or 2, it is characterised in that: described Alkali lignin is acid precipitating alkali lignin.
5. the preparation method of alkali lignin porous carbon electrode material according to claim 1 or 2, it is characterised in that: step c In, room temperature is naturally cooled to after heat preservation, finished product is washed by dilute hydrochloric acid and deionized water, crosses and is filtered dry after washing It is dry, obtain the alkali lignin base porous carbon electrode material finished product of reference state sodium group activation preparation.
6. the preparation method of alkali lignin porous carbon electrode material according to claim 5, it is characterised in that: dilute salt The concentration of acid is 0.1mol/L.
7. the preparation method of alkali lignin porous carbon electrode material according to claim 1 or 2, it is characterised in that: step c In, the protective gas is nitrogen.
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CN111634904A (en) * 2020-06-01 2020-09-08 南京博岭节能环保研究院有限公司 Method for preparing carbon nano onion by lignin blending catalytic pyrolysis
CN115346801A (en) * 2022-08-15 2022-11-15 广东工业大学 Lignin-derived porous carbon for supercapacitor and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN111634904A (en) * 2020-06-01 2020-09-08 南京博岭节能环保研究院有限公司 Method for preparing carbon nano onion by lignin blending catalytic pyrolysis
CN115346801A (en) * 2022-08-15 2022-11-15 广东工业大学 Lignin-derived porous carbon for supercapacitor and preparation method and application thereof

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