CN107604480A - A kind of lignin-base activated carbon fiber preparation method for electrode of super capacitor - Google Patents
A kind of lignin-base activated carbon fiber preparation method for electrode of super capacitor Download PDFInfo
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- CN107604480A CN107604480A CN201711017105.8A CN201711017105A CN107604480A CN 107604480 A CN107604480 A CN 107604480A CN 201711017105 A CN201711017105 A CN 201711017105A CN 107604480 A CN107604480 A CN 107604480A
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- lignin
- carbon fiber
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- activated carbon
- super capacitor
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- 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
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Abstract
The invention discloses a kind of lignin-base activated carbon fiber preparation method for electrode of super capacitor, nanometer electrode manganese dioxide is added in sodium alginate aqueous solution, graphene oxide is added after ultrasonic agitation, solution ph is then adjusted to 10~11, purifying lignin is added, hybrid material is obtained after vacuum rotary steam；Gained hybrid material is added in melt spinning machine at 200~250 DEG C and carries out spinning, obtains hybridized fiber；Gained hybridized fiber is placed in high temperature furnace, rises to 280~300 DEG C with 0.01~3 DEG C/min heating rate, 1~6h of constant temperature；1000~2000 DEG C are then heated to, is carbonized, the time is 0.5~12h, obtains the carbon fiber for electrode of super capacitor.The beneficial effects of the invention are as follows the lignin-base active carbon fiber electrode of offer to possess the advantages that production cost is low, energy density is high.
Description
Technical field
The invention belongs to the preparing technical field of activated carbon fiber, is related to a kind of lignin for electrode of super capacitor
Based activated carbon fiber preparation method.
Background technology
With the appearance and fast development of intelligent clothing, corresponding flexibility, lightweight, efficient ultracapacitor are developed
It is particularly urgent.Its key problem is fibrous electrodes of the research and development with high-energy-density and power density.Fiber at present
The electrode of shape ultracapacitor is prepared using one-dimensional CNT and two-dimensional graphene more, and production cost is high, while is difficult to advise
Modelling produces.And the production cost of fibrous electrode of super capacitor then can be effectively reduced using activated carbon fiber.As activity
The presoma of carbon fiber, lignin due to have the advantages that resource is renewable, cheap, melt-processable and it is interesting.
The A of patent CN 106744793 disclose a kind of alkali lignin based super capacitor porous carbon materials and preparation method thereof and should
With, but prepared carbon material is three-dimensional bulk material, it is difficult to be woven, strongly limit its answering in intelligent clothing
With.Electrode material obtained by simultaneously stores electric charge due to only relying on specific surface area, causes its energy density relatively low.
The content of the invention
It is an object of the invention to provide a kind of lignin-base activated carbon fiber preparation side for electrode of super capacitor
Method, solve the problems, such as that current lignin-base activated carbon fiber energy density is relatively low.
The technical solution adopted in the present invention is to follow the steps below：
Step 1：Nanometer electrode manganese dioxide is added in sodium alginate aqueous solution, graphene oxide is added after ultrasonic agitation,
Then adjustment solution ph adds purifying lignin, hybrid material is obtained after vacuum rotary steam to 10~11；By gained hydridization material
Material, which is added in melt spinning machine at 200~250 DEG C, carries out spinning, obtains hybridized fiber；
Step 2：Step 1 gained hybridized fiber is placed in high temperature furnace, risen to 0.01~3 DEG C/min heating rate
280~300 DEG C, 1~6h of constant temperature；1000~2000 DEG C are then heated to, is carbonized, the time is 0.5~12h, is used for
The carbon fiber of electrode of super capacitor.
Further, lignin is purified as lignin of the hydroxy radical content more than 6mmol/g in step 1, between its construction unit
Connected mode be β-β and β -1.
Further, the weight average molecular weight of the sodium alginate in step 1 be less than 80,000, addition for gross mass 0.05~
10%.
Further, the addition of the nano-manganese dioxide in step 1 is the 0.1~20% of gross mass.
Further, the addition of the graphene oxide in step 1 is the 0.1~10% of gross mass.
Further, the spinning speed of spinning-drawing machine is 100~6000m/min in step 1.
Further, a diameter of 5~200 μm of the porous carbon fiber in step 2, is continuous multi-stage pore structure, aperture be 1nm~
3μm。
Possess that production cost is low, energy density the beneficial effects of the invention are as follows the lignin-base active carbon fiber electrode of offer
It is high.
Embodiment
With reference to embodiment, the present invention is described in detail.
Lignin used is the sulphur purchased from (Suzano Papel e Celulose S.A.) company in following examples
Hydrochlorate lignin, purified using ceramic membrane filter equipment, purifying precision is 5kDa.
Embodiment 1：0.5g nano-manganese dioxides are added to the sodium alginate for filling that 200ml mass fractions are 0.5wt.%
In the aqueous solution, ultrasonic disperse 30min (ultrasonic power 120W, supersonic frequency 40KHz) adds 1g graphene oxides afterwards, and stirring is equal
It is even.Then adjustment solution ph adds 97g purifying lignin to 11.Obtained after Rotary Evaporators rotary evaporation is used at 80 DEG C
To lignin/graphene oxide/sodium alginate/manganese dioxide hybrid material；Gained hybrid material is added to melt spinning machine
In melt spinning is carried out at 200~230 DEG C, obtain lignin/graphene oxide/sodium alginate/manganese dioxide hybridized fiber,
Wherein spinneret specification is 0.18mm × 12f, spinning speed 100m/min.Gained hybridized fiber is placed in high temperature furnace, with
0.01 DEG C/min heating rate rises to 280 DEG C, constant temperature 1h；1000 DEG C are then heated to, is carbonized, time 0.5h.Drop
Low temperature is activated, soak time 30min to 900 DEG C using vapor (50RH%).By gained activated carbon fiber in hydrogen
Lignin-base activated carbon fiber is obtained after 24h is soaked in fluoric acid.Gained activated carbon fiber has a hierarchical porous structure, and a diameter of 60
μm, tensile strength 120MPa, specific surface area 1300m2/ g, mesoporous pore volume are 0.18cm3/g。
Embodiment 2：1g nano-manganese dioxides are added to fill 200ml mass fractions be 1wt.% sodium alginate it is water-soluble
In liquid, ultrasonic disperse 30min (ultrasonic power 120W, supersonic frequency 40KHz) adds 2g graphene oxides afterwards, stirs.With
Solution ph is adjusted afterwards to 12, adds 96g purifying lignin.It is wooden using being obtained after Rotary Evaporators rotary evaporation at 80 DEG C
Element/graphene oxide/sodium alginate/manganese dioxide hybrid material；Gained hybrid material is added in melt spinning machine 200
Melt spinning is carried out at~240 DEG C, lignin/graphene oxide/sodium alginate/manganese dioxide hybridized fiber is obtained, wherein spraying
Filament plate specification is 0.18mm × 12f, spinning speed 500m/min.Gained hybridized fiber is placed in high temperature furnace, with 0.03 DEG C/
Min heating rate rises to 280 DEG C, constant temperature 2h；1200 DEG C are then heated to, is carbonized, time 1h.Reduce temperature extremely
800 DEG C, activated using vapor (50RH%), soak time 1h.Gained activated carbon fiber is soaked in hydrofluoric acid
Lignin-base activated carbon fiber is obtained after 24h.Gained activated carbon fiber has hierarchical porous structure, and a diameter of 52 μm, stretching is strong
Spend for 110MPa, specific surface area 1400m2/ g, mesoporous pore volume are 0.21cm3/g。
Embodiment 3：2g nano-manganese dioxides are added to fill 200ml mass fractions be 2wt.% sodium alginate it is water-soluble
In liquid, ultrasonic disperse 30min (ultrasonic power 120W, supersonic frequency 40KHz) adds 4g graphene oxides afterwards, stirs.With
Solution ph is adjusted afterwards to 11, adds 90g purifying lignin.It is wooden using being obtained after Rotary Evaporators rotary evaporation at 80 DEG C
Element/graphene oxide/sodium alginate/manganese dioxide hybrid material；Gained hybrid material is added in melt spinning machine 210
Melt spinning is carried out at~250 DEG C, lignin/graphene oxide/sodium alginate/manganese dioxide hybridized fiber is obtained, wherein spraying
Filament plate specification is 0.18mm × 12f, spinning speed 800m/min.Gained hybridized fiber is placed in high temperature furnace, with 0.03 DEG C/
Min heating rate rises to 280 DEG C, constant temperature 3h；1000 DEG C are then heated to, is carbonized, time 3h.Reduce temperature extremely
900 DEG C, activated using vapor (50RH%), soak time 2h.Gained activated carbon fiber is soaked in hydrofluoric acid
Lignin-base activated carbon fiber is obtained after 24h.Gained activated carbon fiber has hierarchical porous structure, and a diameter of 46 μm, stretching is strong
Spend for 115MPa, specific surface area 1600m2/ g, mesoporous pore volume are 0.28cm3/g。
Embodiment 4：5g nano-manganese dioxides are added to fill 200ml mass fractions be 3wt.% sodium alginate it is water-soluble
In liquid, ultrasonic disperse 50min (ultrasonic power 120W, supersonic frequency 40KHz) adds 5g graphene oxides afterwards, stirs.With
Solution ph is adjusted afterwards to 10, adds 84g purifying lignin.It is wooden using being obtained after Rotary Evaporators rotary evaporation at 80 DEG C
Element/graphene oxide/sodium alginate/manganese dioxide hybrid material；Gained hybrid material is added in melt spinning machine 190
Melt spinning is carried out at~250 DEG C, lignin/graphene oxide/sodium alginate/manganese dioxide hybridized fiber is obtained, wherein spraying
Filament plate specification is 0.18mm × 12f, spinning speed 1000m/min.Gained hybridized fiber is placed in high temperature furnace, with 0.02
DEG C/min heating rate rises to 280 DEG C, constant temperature 3h；1200 DEG C are then heated to, is carbonized, time 3h.Reduce temperature
To 700 DEG C, activated using vapor (50RH%), soak time 3h.Gained activated carbon fiber is soaked in hydrofluoric acid
Lignin-base activated carbon fiber is obtained after bubble 24h.Gained activated carbon fiber has hierarchical porous structure, a diameter of 41 μm, stretches
Intensity is 105MPa, specific surface area 1700m2/ g, mesoporous pore volume are 0.32cm3/g。
It is also an advantage of the present invention that：
(1) the lignin-base activated carbon fiber for electrode of super capacitor provided in the present invention possesses production cost
It is low, energy density is high, pore space structure is controllable, is easy to the advantages that industrialized production.
(2) the lignin-base activated carbon fiber for electrode of super capacitor provided in the present invention is using melting
Spinning process, good spinnability, fiber quality is excellent, and production cost is greatly reduced, and can carry out continuous production.
(3) the lignin-base activated carbon fiber for electrode of super capacitor provided in the present invention possesses multi-stage porous knot
Structure, channel diameter is big, is expected to be widely applied to the fields such as intelligent clothing, wide market.
Described above is only the better embodiment to the present invention, not makees any formal limit to the present invention
System, any simple modification that every technical spirit according to the present invention is made to embodiment of above, equivalent variations and modification,
Belong in the range of technical solution of the present invention.
Claims (7)
1. a kind of lignin-base activated carbon fiber preparation method for electrode of super capacitor, it is characterised in that according to following step
It is rapid to carry out：
Step 1：Nanometer electrode manganese dioxide is added in sodium alginate aqueous solution, adds graphene oxide after ultrasonic agitation, then
Solution ph is adjusted to 10~11, purifying lignin is added, hybrid material is obtained after vacuum rotary steam；Gained hybrid material is added
Enter into melt spinning machine and spinning is carried out at 200~250 DEG C, obtain hybridized fiber；
Step 2：Step 1 gained hybridized fiber is placed in high temperature furnace, 280 are risen to 0.01~3 DEG C/min heating rate~
300 DEG C, 1~6h of constant temperature；1000~2000 DEG C are then heated to, is carbonized, the time is 0.5~12h, obtains being used for super electricity
The carbon fiber of container electrode.
2. according to a kind of lignin-base activated carbon fiber preparation method for electrode of super capacitor described in claim 1, its
It is characterised by：Lignin is purified as lignin of the hydroxy radical content more than 6mmol/g in the step 1, between its construction unit
Connected mode is β-β and β -1.
3. according to a kind of lignin-base activated carbon fiber preparation method for electrode of super capacitor described in claim 1, its
It is characterised by：The weight average molecular weight of sodium alginate in the step 1 is less than 80,000, and addition is the 0.05~10% of gross mass.
4. according to a kind of lignin-base activated carbon fiber preparation method for electrode of super capacitor described in claim 1, its
It is characterised by：The addition of nano-manganese dioxide in the step 1 is the 0.1~20% of gross mass.
5. according to a kind of lignin-base activated carbon fiber preparation method for electrode of super capacitor described in claim 1, its
It is characterised by：The addition of graphene oxide in the step 1 is the 0.1~10% of gross mass.
6. according to a kind of lignin-base activated carbon fiber preparation method for electrode of super capacitor described in claim 1, its
It is characterised by：The spinning speed of spinning-drawing machine is 100~6000m/min in the step 1.
7. according to a kind of lignin-base activated carbon fiber preparation method for electrode of super capacitor described in claim 1, its
It is characterised by：A diameter of 5~200 μm of porous carbon fiber in described step 2, is continuous multi-stage pore structure, aperture be 1nm~
3μm。
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| CN201711017105.8A CN107604480A (en) | 2017-10-26 | 2017-10-26 | A kind of lignin-base activated carbon fiber preparation method for electrode of super capacitor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE1850127A1 (en) * | 2018-02-05 | 2019-08-06 | Rise Innventia Ab | Method of wet spinning precursor fibers comprising lignin and gelling hydrocolloid, and precursor fibers therefrom |
| CN112870845A (en) * | 2020-12-30 | 2021-06-01 | 湖南翰坤实业有限公司 | Active carbon-based air purification material and preparation method thereof |
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| CN102181961A (en) * | 2011-03-07 | 2011-09-14 | 青岛大学 | Method for preparing graphene functionalized alginate fibers |
| CN104178845A (en) * | 2014-08-14 | 2014-12-03 | 青岛大学 | Multifunctional high-performance carbon-based nanoparticle/sodium alginate composite fibers and preparation method thereof |
| US20160258082A1 (en) * | 2015-03-06 | 2016-09-08 | Ut-Battelle, Llc | Low temperature stabilization process for production of carbon fiber having structural order |
| CN106149083A (en) * | 2015-04-02 | 2016-11-23 | 恒天海龙股份有限公司 | Functional graphene cellulose fiber prepared by melting method and preparation method thereof |
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| CN102181961A (en) * | 2011-03-07 | 2011-09-14 | 青岛大学 | Method for preparing graphene functionalized alginate fibers |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE1850127A1 (en) * | 2018-02-05 | 2019-08-06 | Rise Innventia Ab | Method of wet spinning precursor fibers comprising lignin and gelling hydrocolloid, and precursor fibers therefrom |
| WO2019151937A1 (en) * | 2018-02-05 | 2019-08-08 | Rise Innventia Ab | Method of wet spinning precursor fibers comprising lignin and gelling hydrocolloid, and precursor fibers therefrom |
| SE541449C2 (en) * | 2018-02-05 | 2019-10-08 | Rise Innventia Ab | Method of wet spinning precursor fibers comprising lignin and gelling hydrocolloid, and precursor fibers therefrom |
| CN112870845A (en) * | 2020-12-30 | 2021-06-01 | 湖南翰坤实业有限公司 | Active carbon-based air purification material and preparation method thereof |
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