CN107572517A - Alginic acid alkali three-dimensional network layered activated carbon and one step charing preparation method - Google Patents
Alginic acid alkali three-dimensional network layered activated carbon and one step charing preparation method Download PDFInfo
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- CN107572517A CN107572517A CN201710780799.4A CN201710780799A CN107572517A CN 107572517 A CN107572517 A CN 107572517A CN 201710780799 A CN201710780799 A CN 201710780799A CN 107572517 A CN107572517 A CN 107572517A
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- activated carbon
- alginic acid
- dimensional network
- sodium alginate
- acid alkali
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Abstract
Alginic acid alkali three-dimensional network layered activated carbon and one step charing preparation method, including alginic acid and sodium ion reacted to obtain soluble sodium alginate, then sodium alginate is formulated as solution, add CaCl2It is sufficiently stirred, sodium alginate calcium complexes presoma is made, finally obtained presoma is fully washed, is placed in oven drying；Obtained presoma is placed in quartz boat, is put into tube furnace, is passed through nitrogen, from room temperature to final carbonization temperature；To the end of charring process, temperature is down to room temperature, gained insolubility alginate Quito mesoporous activated carbon is subjected to pickling, wash again and remove metallic compound therein, finally it is placed in 110 DEG C of baking ovens and fully dries, the activated carbon sample of drying is ground through row, is placed in dry environment, you can obtain alginic acid alkali three-dimensional network layered activated carbon.Preparation process cleaning of the present invention, step is simple, and product structure is various controllable, and capacitive property is high, and manufacturing cost is low.
Description
Technical field
The present invention relates to a kind of alginic acid alkali three-dimensional network layered activated carbon and one step charing preparation method, specifically relate to
And the preparation of compounding sea alginate source materials and presoma, a step condition of carbonization.
Background technology
Ultracapacitor has the characteristics that charging rate is fast, power density is high, long lifespan, is to solve power used for electric vehicle
The most effective approach of power supply.The sole power power supply that it can both run as electric vehicle, electric vehicle can also be used as to run
Auxiliary power power supply.Ultracapacitor can be additionally used in photovoltaic cell electric power storage, the stabilization of power grids, radio transmitting constant power device,
And the startup energy of tank, rocket extract；The U.S., Europe, Japan etc. also carry out the research of ultracapacitor.
The alginate that this experiment uses, wide material sources, it is easy to extraction and prepares.But alginate monovalence and divalent metal
There is mutual metathesis between ion, can neatly change the species and content of metal ion in presoma, so as to change
The structure of presoma, finally obtain the carbon material of different pore size distribution.Simultaneously because itself contain substantial amounts of metallic atom, because
This need not additionally add any chemical activation reagent, broken the yoke that conventional chemical methods activation prepares activated carbon, overcome
Conventional chemical methods prepare the shortcomings that absorbent charcoal material.Preparation technology is easy, and production equipment will not be caused to corrode, last metal
It can be easy to reclaim, it is free from environmental pollution.And resulting insolubility alginate Quito mesoporous activated carbon has controllable aperture point
Cloth scope, can be by simply changing the ratio of metallic element species and different metal content in presoma, so that it may regulate and control
The aperture of the activated carbon sample of final product.Obtained activated carbon sample has larger specific surface area and total hole volume, simultaneously
Also there is the bulk density of super large, reach 0.9 cm3/g.Therefore electrode material of such a absorbent charcoal material as ultracapacitor
Material also has the volumetric capacitance of super large, can reduce the volume shared by the electrode material of ultracapacitor significantly, has very big
Application prospect.
Zhongrong Geng et al.（Geng Z, Wang H, Wang R, et al. Facile synthesis of
hierarchical porous carbon for supercapacitor with enhanced electrochemical
Performance [J] Materials Letters, 2016,182:1-5.）Research is found, is now carried out sodium alginate low
Temperature charing, the active carbon electrode material then obtained using NaOH activation methods, is had high specific capacitance, can reach 451 F/g,
There is very long and stable cycle life simultaneously.
Raymundo et al. (E. Raymundo-Pi ero, Leroux F, B é guin F. A High-
Performance Carbon for Supercapacitors Obtained by Carbonization of a Seaweed
Biopolymer [J] Advanced Materials, 2006,18 (14):1877-1882.) by simply to marine alga
Sour sodium carries out 600 DEG C of charings of low temperature, obtains three-dimensional porous carbon material.And its chemical property is analyzed, before discovery is this
Carbon material obtained by driving body preparation has at a relatively high oxygen content, and on the premise of bulk density is very high, it surpasses as water system
Level capacitor electrode material has high volumetric capacitance.But researcher has only carried out weight analysis to surface nature, only prepare
A kind of sodium alginate base porous carbon materials.
Ma et al. (Ma G F, Mu J J, Zhang Z G, et al. Preparation of
Polypyrrole/Sodium Alginate Nanospheres and Their Application for High-
Performance Supercapacitors [J] Acta Physico-Chimica Sinica, 2013,29 (11):
2385-2391 (7)) sodium alginate/Pt/Polypyrrole composite material is prepared, the specific capacity with 347 F/g, and 500 circulations
It is functional, but long-term cycle stability is poor, and the composite used is expensive, without actual application value.
(Ma L, Xu L M, Zhou X P, the et al. Biopolymer-assisted such as Ma L
Hydrothermal synthesis of flower-like MoS2, microspheres and their
Supercapacitive properties [J] Materials Letters, 2014,132:291-294.) use sea
Mosanom is as carrier, compound MoS2Metal sulfide is as electrode material for super capacitor, but performance is general, and using high
Expensive metal material, the prospect without application.
In summary, although at present someone carbonized using one kind-sodium alginate in alginate, activation with
Conducting polymer is compound, compound etc. with metallic compound.But all there is certain limitation, and lived using chemical reagent
Change, corrosivity is too strong, and equipment investment is excessive, can not continuous production, and finally produce substantial amounts of toxic gas and liquid can not
Recovery, compound using expensive conducting polymer and metallic compound progress, step is more, and pollution is big, and performance is general, leads
Cause actual application value not high
The content of the invention
The technical problem of solution：Preparation process is seriously polluted existing for prior art in order to solve, and step is more, and product knot
The problem of structure is single, and capacitive property is low, and cost is high, the present invention propose a kind of alginic acid alkali three-dimensional network layered activated carbon and its
One step carbonizes preparation method, and preparation process cleaning, step is simple, and product structure is various controllable, and capacitive property is high, manufacturing cost
It is low.
Technical scheme：The step of alginic acid alkali three-dimensional network layered activated carbon one carbonizes preparation method, and preparation process is：First
Step, the preparation of presoma：Alginic acid and sodium ion are reacted to obtain soluble sodium alginate, then sodium alginate is formulated as molten
Liquid, add CaCl2It is sufficiently stirred, sodium alginate calcium complexes presoma is made, finally obtained presoma is fully washed, put
In oven drying；Second step, charing：Obtained presoma is placed in quartz boat, is put into tube furnace, is passed through nitrogen, with 10
DEG C/min heating rate is from room temperature to final carbonization temperature；3rd step, washing and drying：To the end of charring process, temperature
Room temperature is down to, gained insolubility alginate Quito mesoporous activated carbon is subjected to pickling, then wash and remove metal compound therein
Thing, finally it is placed in 110 DEG C of baking ovens and fully dries, be placed in dry environment, you can obtains alginic acid alkali three-dimensional network stratiform
Activated carbon.
The mass ratio of calcium chloride mass concentration 1%-10% in the above-mentioned first step, sodium alginate and calcium chloride is 1: 0.02.
Charing is the flow velocity under inert gas shielding in above-mentioned second step：1L/min, charing final temperature are 700-1000 DEG C,
Carbonization time 30-120 min.
Above-mentioned pickling is to be washed first by 1+9 hydrochloric acid through row, reuses deionized water and washs 2-4 times.
Alginic acid alkali three-dimensional network layered activated carbon made from the above method.
Above-mentioned alginic acid alkali three-dimensional network layered activated carbon, specific surface area 400-1400 m2/ g, quality specific capacitance 100-
300 F/g, volumetric capacitance 100-300 F/cm3。
Beneficial effect：Corresponding compound alginate Quito mesoporous activated carbon material, step letter are prepared using one-step method charing
Single, operation is simple, and only by changing the species and content of metal ion in presoma, it becomes possible to the activity obtained by artificial adjustment
The pore size distribution range of charcoal sample, its electrode material as ultracapacitor, there can be high specific capacitance respectively, it is well forthright again
Can, excellent cycling performance etc., so as to be applied in different demands.Whole technique need not add any chemical activation examination
Agent, it is only necessary to simple step heating charing, you can obtain activated carbon sample to the end.
Brief description of the drawings
Fig. 1 is sodium alginate calcium composite matrix activated carbon N prepared by embodiment2Adsorption-desorption isothermal.
Fig. 2 is sodium alginate calcium composite material base activated carbon pore size distribution prepared by embodiment.
The composite matrix activated carbon constant current charge-discharge curves of Fig. 3 Alg-Na-Ca 900.
The composite matrix activated carbon cyclic voltammetric Tequ lines of Fig. 4 Alg-Na-Ca 900.
Fig. 5 Alg-Na-Ca 900 sodium alginate calcium composite matrix activated carbon high rate performance.
Fig. 6 Alg-Na-Ca 900 sodium alginate calcium composite matrix activated carbon impedance behavior.
Embodiment
The present invention to a kind of method of testing of alginic acid alkali three-dimensional network layered activated carbon material property it is as follows：
（1）Specific surface area, the measure of pore volume：Measure using activated carbon under the conditions of liquid nitrogen to nitrogen adsorption isotherm, according to
BET formula calculates specific surface area.
（2）Surface topography uses FDAC（Hitachi）The S-4800 type cold field emission electron microscope observations of company.
（3）The measure of specific capacitance：Determined using electrochemical workstation under constant current.
A kind of alginic acid alkali three-dimensional network layered activated carbon and one step charing preparation method, comprise the following steps：
The first step, the preparation of presoma：Alginic acid and sodium hydroxide are reacted to obtain sodium alginate.Sodium alginate is configured to again
Solution, add certain density CaCl2It is sufficiently stirred through row, sodium alginate calcium complexes presoma is made.It will finally obtain
Sample fully washs, and is placed in oven drying.
Second step, charing：Obtained presoma is placed in quartz boat, is put into tube furnace, is passed through nitrogen.With 10 DEG C/
Min heating rate is from room temperature to final carbonization temperature；
3rd step, washing and drying：To the end of a step charring process, temperature is down to room temperature, by gained insolubility alginic acid alkali
Porous activated carbon carries out pickling, and repeatedly washing removes metallic compound therein, is finally placed in 110 DEG C of baking ovens and fully dries
12 h, the activated carbon sample of drying is fully ground through row, is placed in dry environment, you can obtain one kind alginic acid alkali three
Tie up network layered activated carbon material.
Use calcium chloride mass concentration 1-10% in the method for the present invention, the mass ratio of sodium alginate/potassium and calcium chloride is 1:
0.0.2.Charing is the flow velocity under inert gas shielding：1L/min, charing final temperature are 700-1000 DEG C, carbonization time 30-120
Min, inert atmosphere are nitrogen or argon gas.Obtained activated carbon sample first by 1+9 hydrochloric acid through row wash, reuse from
Sub- water washing 2-4 times, finally it is placed in baking oven and dries, cool down, milling, obtains ultracapacitor insolubility alginic acid alkali
Absorbent charcoal material.
The activity that a kind of described alginic acid alkali three-dimensional network layered activated carbon and one step charing preparation method obtain
Carbon Materials, it is characterised in that specific surface area 400-1400 m2/ g, quality specific capacitance 100-300 F/g, volumetric capacitance are reachable
To 100-300 F/cm3, the absorbent charcoal material that different presomas are prepared has different pore size distribution ranges, can be divided
Not Wei big mesopore, the absorbent charcoal material based on macropore.
Specific surface area, pore-size distribution, the pore volume of the compound alginate matrix activated carbon material of ultracapacitor of the present invention
Can be by changing the species and content of metal ion in presoma, to carry out quantitative regulation and control.Identical presoma obtains simultaneously
The temperature and time that activated carbon sample structure is carbonized by a step is come through row control.The present invention has simply selected sodium alginate calcium to make
For example, such a method is used in the porous carbon that any step charing of insolubility alginate one prepares different pore size distribution
Material.The alginic acid for extracting to obtain from marine alga is purified through row, the removal of impurity is gone in washing, is dried；By obtained alginic acid and phase
The alkali answered reacts to obtain soluble sodium alginate.Solution is configured as again, adds certain density CaCl2Fully stirred through row
Mix, sodium alginate calcium complexes presoma is made.Finally obtained sample is fully washed, is placed in oven drying.By what is obtained
Presoma is placed in quartz boat, is put into tube furnace, is passed through nitrogen.With 10 DEG C/min heating rate from room temperature to most
Whole carbonization temperature；To the end of a step charring process, temperature is down to room temperature, by gained insolubility alginate base porous active
Charcoal carries out pickling, and repeatedly washing removes metallic compound therein, is finally placed in 110 DEG C of baking ovens fully 12 h of drying, will dry
Dry activated carbon sample is fully ground through row, is placed in dry environment, you can the ultracapacitor for obtaining different pore size distribution is used
Insolubility alginate matrix activated carbon material.
Embodiment 1
（1）It is prepared by presoma：First sodium alginate is prepared with NaOH immersions in alginic acid, then by sodium alginate and 1wt.%
Calcium chloride carries out immersion treatment, washs, and dries, obtains sodium alginate calcium presoma.
（2）Charing：Sodium alginate calcium is placed in quartz boat and is put into tube furnace, nitrogen is passed through with 1L/min flows, with 10
DEG C/min heating rate from room temperature to 700 DEG C, keep 60min, be naturally cooling to room temperature.
（3）After the completion of the charing of one step, the activated carbon sample of cooling is washed using 1+9 hydrochloric acid through row, reuses deionization
Water washing 2-4 times, finally it is placed in baking oven and dries, cool down, milling, obtains ultracapacitor sodium alginate calcium matrix activated carbon material
Material.Its specific surface area is 456 m2/ g, total pore volume are 0.54 cm3/ g, the F/g of specific capacitance 86 under 0.5 A/g current density.
Embodiment 2
（1）It is prepared by presoma：First sodium alginate is prepared with NaOH immersions in alginic acid, then by sodium alginate and 5 wt.%
Calcium chloride carry out immersion treatment, wash, dry, obtain sodium alginate calcium presoma.
（2）Charing：Sodium alginate calcium is placed in quartz boat and is put into tube furnace, nitrogen is passed through with 1L/min flows, with 10
DEG C/min heating rate from room temperature to 800 DEG C, keep 60min, be naturally cooling to room temperature.
（3）After the completion of the charing of one step, the activated carbon sample of cooling is washed using 1+9 hydrochloric acid through row, reuses deionization
Water washing 2-4 times, finally it is placed in baking oven and dries, cool down, milling, obtains ultracapacitor sodium alginate calcium matrix activated carbon material
Material.Its specific surface area is 899 m2/ g, total pore volume are 0.92 cm3/ g, the F/ of specific capacitance 158 under 0.5 A/g current density
g。
Embodiment 3
（1）It is prepared by presoma：First sodium alginate is prepared with NaOH immersions in alginic acid, then by sodium alginate and 5 wt.%
Calcium chloride carry out immersion treatment, wash, dry, obtain sodium alginate calcium presoma.
（2）Charing：Sodium alginate calcium is placed in quartz boat and is put into tube furnace, nitrogen is passed through with 1L/min flows, with 10
DEG C/min heating rate from room temperature to 900 DEG C, keep 60min, be naturally cooling to room temperature.
（3）After the completion of the charing of one step, the activated carbon sample of cooling is washed using 1+9 hydrochloric acid through row, reuses deionization
Water washing 2-4 times, finally it is placed in baking oven and dries, cool down, milling, obtains ultracapacitor sodium alginate calcium matrix activated carbon material
Material.Its specific surface area is 1295 m2/ g, total pore volume are 1.79 cm3/ g, the F/ of specific capacitance 170 under 0.5 A/g current density
g。
Embodiment 4
（1）It is prepared by presoma：First sodium alginate is prepared with NaOH immersions in alginic acid, then by sodium alginate and 10 wt.%
Calcium chloride carry out immersion treatment, wash, dry, obtain sodium alginate calcium presoma.
（2）Charing：Sodium alginate calcium is placed in quartz boat and is put into tube furnace, nitrogen is passed through with 1L/min flows, with 10
DEG C/min heating rate from room temperature to 1000 DEG C, keep 60min, be naturally cooling to room temperature.
（3）After the completion of the charing of one step, the activated carbon sample of cooling is washed using 1+9 hydrochloric acid through row, reuses deionization
Water washing 2-4 times, finally it is placed in baking oven and dries, cool down, milling, obtains ultracapacitor sodium alginate calcium matrix activated carbon material
Material.Its specific surface area is 479 m2/ g, total pore volume are 0.57 cm3/ g, the F/g of specific capacitance 79 under 0.5 A/g current density.
Claims (6)
1. the step of alginic acid alkali three-dimensional network layered activated carbon one carbonizes preparation method, it is characterised in that preparation process is：
The first step, the preparation of presoma：Alginic acid and sodium ion are reacted to obtain soluble sodium alginate, then sodium alginate is matched somebody with somebody
Solution is made as, adds CaCl2It is sufficiently stirred, sodium alginate calcium complexes presoma is made, it is finally that obtained presoma is abundant
Washing, is placed in oven drying；
Second step, charing：Obtained presoma is placed in quartz boat, is put into tube furnace, is passed through nitrogen, with 10 DEG C/min
Heating rate from room temperature to final carbonization temperature；
3rd step, washing and drying：To the end of charring process, temperature is down to room temperature, by gained insolubility alginate Quito hole
Activated carbon carries out pickling, then washes and remove metallic compound therein, is finally placed in 110 DEG C of baking ovens and fully dries, is placed in dry
In dry environment, you can obtain alginic acid alkali three-dimensional network layered activated carbon.
2. the step of alginic acid alkali three-dimensional network layered activated carbon one charing preparation method, its feature exist according to claim 1
In, calcium chloride mass concentration 1%-10% in the first step, the mass ratio of sodium alginate and calcium chloride is 1: 0.02.
3. the step of alginic acid alkali three-dimensional network layered activated carbon one charing preparation method, its feature exist according to claim 1
In charing is the flow velocity under inert gas shielding in second step：1L/min, charing final temperature are 700-1000 DEG C, carbonization time
30-120 min。
4. the step of alginic acid alkali three-dimensional network layered activated carbon one charing preparation method, its feature exist according to claim 1
It is to be washed first by 1+9 hydrochloric acid through row in pickling, reuses deionized water and wash 2-4 times.
5. alginic acid alkali three-dimensional network layered activated carbon made from any methods describeds of claim 1-4.
6. alginic acid alkali three-dimensional network layered activated carbon according to claim 5, it is characterised in that specific surface area 400-
1400 m2/ g, quality specific capacitance 100-300 F/g, volumetric capacitance 100-300 F/cm3。
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| CN110627060A (en) * | 2019-10-17 | 2019-12-31 | 中国林业科学研究院林产化学工业研究所 | Method for preparing porous activated carbon by utilizing bio-based and product thereof |
| CN114653338A (en) * | 2022-03-21 | 2022-06-24 | 青岛理工大学 | Simultaneously removing CS in natural gas2Hg-blended nitrogen-doped metal ion loaded adsorbent and preparation method thereof |
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| CN108950736A (en) * | 2018-08-22 | 2018-12-07 | 贵州森环活性炭有限公司 | Nanoporous carbon fiber and preparation method thereof |
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| CN115448993A (en) * | 2022-09-15 | 2022-12-09 | 中盐金坛盐化有限责任公司 | Coated salt product and preparation method and application thereof |
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Application publication date: 20180112 |