CN109859953A - A kind of preparation method of bamboo matrix activated carbon/manganese aerogel composite - Google Patents
A kind of preparation method of bamboo matrix activated carbon/manganese aerogel composite Download PDFInfo
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- CN109859953A CN109859953A CN201711239396.5A CN201711239396A CN109859953A CN 109859953 A CN109859953 A CN 109859953A CN 201711239396 A CN201711239396 A CN 201711239396A CN 109859953 A CN109859953 A CN 109859953A
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- manganese
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- activated carbon
- matrix activated
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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
Abstract
The present invention relates to a kind of method for preparing composite material with biomass material, aeroge, especially a kind of method for preparing composite material with bamboo matrix activated carbon, manganese aeroge belongs to capacitor material field.Utilize the electric double layer effect of bamboo matrix activated carbon and the fake capacitance effect of manganese aeroge, by on bamboo matrix activated carbon surface and inner void load there is the manganese aeroge of nanoscale three-dimensional network structure to obtain the composite material with special appearance, its chemical property is better than raw material, and cyclical stability is good, it solves the problems, such as that fake capacitance capacitor cycle stability is low low with specific capacity of double-layer capacitor, is applied in supercapacitor field.
Description
Technical field
The present invention relates to a kind of methods for preparing composite material with biomass material, aeroge, especially a kind of to use bamboo base
The method that active carbon, aeroge prepare composite material belongs to capacitor material field.
Background technique
From since the 21th century, the fossil energies such as coal, petroleum and industrial chemicals are increasingly rare, and environmental protection problem is got over
More it is taken seriously, finding new energy becomes the topic that people discuss warmly, and as the continuous of environmental pollution aggravates and energy resources
Increasingly reduction, exploitation by the novel charcoal material of raw material of plant biomass causes extensive attention, recently to bioenergy
Material focuses primarily upon on timber, rice husk, coconut husk, stalk and wood-base materials, therefore sight is placed on bamboo matrix activated carbon, has
Certain novelty and environment protection significance, bamboo is as a kind of traditional biological material, fertility short with growth cycle
By force, growth conditions requires low, resourceful and primary the features such as afforesting successfully, from the point of view of " environmentally conscious materials " to its into
Row develops and utilizes, and can not only extend bamboo wood applies chain, but also can widen its application field, and carbonizes to bamboo wood
Bamboo matrix activated carbon can be obtained with after activating process processing, it is with good performance and economical to be applied to supercapacitor field
Environment-friendly advantage.
Supercapacitor can be divided into carbon electrode capacitor, metal oxide capacitor, conducting polymer according to electrode material
Object capacitor, composite electrode capacitor can be divided into symmetry type capacitance device, asymmetric according to the reaction in structure and electrode
Type capacitor can be divided into double layer capacitor, Faraday pseudo-capacitance capacitor, hybrid capacitor according to energy storage mechnism,
Receiving and losing electrons reaction is occurring between electrode surface in charge and discharge process simply by electrolyte ion for double layer capacitor, no
Electrode material is consumed, has capacity big, small in size, charge/discharge speed is fast, and use temperature range is wide, the advantages that having extended cycle life,
Faraday hawk capacity capacitor is then that redox reaction occurs with electrolyte ion using electrode material and produces electricl energy, and is being followed
Electrode material can be consumed during ring, because charge and discharge process can all occur on electrode interior and surface, therefore is also had good
Specific energy and capacitance, double layer capacitor and the respective advantage of Faraday pseudo-capacitance capacitor play it in new energy field
Increasing effect, and create considerable economic benefits.
Bamboo matrix activated carbon has porous structure and good electric conductivity, and porous structure can produce biggish specific surface
Product, greatly increases the contact area of electrolyte and electrode material, and manganese aeroge has three-dimensional network skeleton structure, this structure
It can promote the performance of its fake capacitance characteristic, and manganese source is cheap and easy to get, be the good substitute of noble metal oxide electrodes material, therefore
Electrode material of the present invention using bamboo matrix activated carbon/manganese aerogel composite as supercapacitor, can make bamboo base therein
Active carbon plays its electric double layer effect, and manganese aeroge is made to play its fake capacitance effect, gives full play to the respective advantage of the two, realizes
The reasonable balance of material property and cost, maximizes favourable factors and minimizes unfavourable ones, and has excellent performance not available for unitary electrode material, application prospect
It is wide, thus be also one of the emphasis for being from now on supercapacitor research direction.
Summary of the invention
Bamboo matrix activated carbon is evenly dispersed in manganese colloidal sol, by colloidal sol-gel process, in conjunction with supercritical drying work
Skill prepares the aerogel carried composite material in bamboo matrix activated carbon surface and inner void of manganese.
To achieve the above object of the invention, the technical solution adopted by the present invention is that: a kind of bamboo matrix activated carbon/manganese aeroge is compound
The preparation method of material, is made in the steps below.
Step 1: weighing potassium hydroxide and bamboo charcoal with certain alkali charcoal mass ratio (2:1~5:1), and mixing is dissolved in a small amount of water,
Water is evaporated under 80 DEG C of magnetic agitation, is uniformly mixed potassium hydroxide and bamboo charcoal；
Step 2: the mixture of potassium hydroxide and bamboo charcoal is put into nickel crucible, is heated up under tube type resistance furnace nitrogen atmosphere, right
Bamboo charcoal is activated；
Step 3: obtained bamboo matrix activated carbon is subjected to pickling and washing, impurity is washed away, is put into baking oven in 80 DEG C of dryings；
Step 4: by manganese nitrate aqueous solution (ml of 0 ml~3), dehydrated alcohol (ml of 10 ml~25) and template (5 ml~20
Ml it) is added in beaker, stirs 15 min under magnetic stirring；
Step 5: the g bamboo matrix activated carbon of 0 g~1 is slowly added in step 4 acquired solution, is ultrasonically treated 0 min~30
min；
Step 6: gelling agent is dropped evenly into mixed liquor, stirs duration 5 min~15 min, is stood, gel；
Step 7: it after wet gel ethanol replacement aging obtained by step 6, is put into overcritical kettle and carries out supercritical drying；
Step 8: obtained bamboo matrix activated carbon/manganese aeroge is placed in Muffle furnace and carries out oxidizing roasting；
500 DEG C preferably are warming up to the rate of 2 K/min in tube type resistance furnace heating activation described in step 2, then with 5
The rate of K/min is warming up to 700 DEG C~1000 DEG C；
Template described in step 4 is preferably the citric acid of the g of 1 g~3；
Gelling agent described in step 6 is preferably the propylene oxide of the ml of 5 ml~20；
Oxidizing roasting is preferably warming up to 350 DEG C~550 DEG C with 5 K/min in Muffle furnace described in step 8, heat preservation
The h of 4 h~7.
Detailed description of the invention
Fig. 1 is bamboo matrix activated carbon/manganese aerogel composite scanning electron microscope (SEM) photograph prepared by embodiment 1.
Fig. 2 is BET nitrogen adsorption-desorption curve of bamboo matrix activated carbon prepared by embodiment 2.
Fig. 3 is bamboo matrix activated carbon/manganese aerogel composite XRD curve prepared by embodiment 3.
Fig. 4 is charging and discharging curve of the bamboo matrix activated carbon of the preparation of embodiment 4 under different current densities.
Fig. 5 is bamboo matrix activated carbon/charge and discharge of the manganese aerogel composite under different current densities prepared by embodiment 5
Curve.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
Potassium hydroxide and bamboo charcoal are weighed with alkali charcoal mass ratio 4:1, mixing is dissolved in a small amount of water, will under 80 DEG C of magnetic agitation
Water is evaporated, and is uniformly mixed potassium hydroxide and bamboo charcoal, the mixture of potassium hydroxide and bamboo charcoal is put into nickel crucible, in tubular type electricity
500 DEG C are warming up to 2 K/min under resistance furnace nitrogen atmosphere, then is warming up to 800 DEG C with 5 K/min, bamboo charcoal is activated, it will
Obtained bamboo matrix activated carbon with the equimolar dilute hydrochloric acid of potassium hydroxide in beaker 12 h of agitator treating, then washed with deionization
It washs to neutrality, is put into baking oven after suction filtration in 80 DEG C of dryings, by the 50 wt% manganese nitrate aqueous solutions of 0.01 mol, 25 ml ethyl alcohol
It is added in beaker with 2.10 mg citric acids, stirs 15min under magnetic stirring, uniformly mixed solution is obtained, into mixed liquor
It is added 17.86 mg bamboo matrix activated carbons, i.e. bamboo matrix activated carbon 1 wt% that accounts for manganese source quality, is ultrasonically treated 10 after stirring 10 min
9 ml propylene oxide are added dropwise into the mixed liquor after ultrasound by min, stand after stirring 10 min, gel after about 5 min, will be wet solidifying
Glue is put into overcritical kettle with after ethanol replacement aging 7 days and carries out ethanol supercritical drying, obtained bamboo matrix activated carbon/manganese airsetting
Glue composite material places it in Muffle furnace and is warming up to 550 DEG C with 5 K/min, keeps the temperature 6 h.
As seen from Figure 1, there is nanoscale three-dimensional porous web in bamboo matrix activated carbon/manganese aerogel composite of synthesis
The manganese aeroge of network structure is largely covered on the inner void and surface of bamboo based activated carbon particles.
Embodiment 2
Operating method is with embodiment 1, the difference is that being warming up to 500 under tube type resistance furnace nitrogen atmosphere with 2 K/min
DEG C, then 700 DEG C are warming up to 5 K/min, bamboo charcoal is activated.
As seen from Figure 2, adsorption desorption isothermal curve type is I type.And BET data is shown, is activated at 700 DEG C
Bamboo matrix activated carbon specific surface area is 1890.48 m2/ g, average pore size are 2.41 nm, mostly micropore.
Embodiment 3
Operating method is with embodiment 1, the difference is that being warming up to 350 DEG C under Muffle furnace air atmosphere with 5 K/min, protects
6 h of temperature.
As seen from Figure 3 after Muffle furnace roasts, there is Mn in bamboo matrix activated carbon/manganese aerogel composite3O4It is brilliant
Type after illustrating high-temperature process, there is Mn3O4It generates.
Embodiment 4
Operating method with embodiment 1, the difference is that into mixed liquor be added quality be 89.32 mg bamboo matrix activated carbons,
That is bamboo matrix activated carbon 5 wt% that account for manganese source quality.
Charging and discharging curve of the bamboo matrix activated carbon under different current densities is more symmetrical triangle as seen from Figure 4
Shape belongs to double layer capacitor type, and specific capacitance can achieve 304 F/g under the current density of 0.1 A/g.
Embodiment 5
Operating method is with embodiment 1, the difference is that it is 178.64 mg bamboo matrix activated carbons that quality is added into mixed liquor, i.e.,
Bamboo matrix activated carbon accounts for 10 wt% of manganese source quality.
It can be seen that bamboo matrix activated carbon/manganese aerogel composite under different current densities by the charging and discharging curve of Fig. 5
Curve distort, present asymmetrically shape.Illustrate composite material there are fake capacitance effect, this phenomenon has with manganese source
Fake capacitance characteristic is consistent.And composite material specific capacitance under the current density of 0.1A/g can achieve 342F/g.
Presently preferred embodiments of the present invention is illustrated above, but the present invention is not limited to the embodiment,
Those skilled in the art can also make various equivalent variation or replacement on the premise of without prejudice to spirit of the invention,
These equivalent variation or replacement are all included in the scope defined by the claims of the present application.
Claims (6)
1. one kind, using biomass bamboo wood and inorganic manganese salt as raw material, bamboo wood is activated rear and manganese sol in situ is compound prepares bamboo base
Active carbon/manganese aerogel composite method, it is characterized in that: bamboo matrix activated carbon hole and area load have manganese aeroge three-dimensional
The special appearance of network structure.
2. being prepared in the steps below:
Step 1: potassium hydroxide and bamboo charcoal are weighed with alkali charcoal ratio 2:1~5:1, mixing is dissolved in a small amount of water, in 80 DEG C of magnetic force
Water is evaporated under stirring, is uniformly mixed potassium hydroxide and bamboo charcoal；
Step 2: the mixture of potassium hydroxide and bamboo charcoal is put into nickel crucible, is heated up under tube type resistance furnace nitrogen atmosphere, right
Bamboo charcoal is activated；
Step 3: obtained bamboo matrix activated carbon is subjected to pickling and washing, impurity is washed away, is put into baking oven in 80 DEG C of dryings；
Step 4: the ml of 0 ml~3 manganese nitrate, the ml of 10 ml~25 ethyl alcohol and template are added in beaker, under magnetic stirring
Stir 15 min；
Step 5: the g bamboo matrix activated carbon of 0 g~1 is slowly added in above-mentioned solution, is ultrasonically treated the min of 0 min~30；
Step 6: gelling agent is dropped evenly into mixed liquor, stirs the min of 5 min~15, until gel；
Step 7: it after obtained bamboo matrix activated carbon/manganese airsetting glue gel ethanol replacement aging, is put into overcritical kettle and carries out
Supercritical drying；
Step 8: obtained bamboo matrix activated carbon/manganese aeroge is placed in Muffle furnace and carries out oxidizing roasting.
3. described preparation bamboo matrix activated carbon/manganese aerogel composite method according to claim 1, it is characterized in that: described
In tube type resistance furnace heating activation with the rate of 2 K/min to be warming up to 500 DEG C, then be warming up to the rate of 5 K/min
700 DEG C~1000 DEG C.
4. described preparation bamboo matrix activated carbon/manganese aerogel composite method according to claim 1, it is characterized in that: described
Template be the g of 1 g~3 citric acid.
5. described preparation bamboo matrix activated carbon/manganese aerogel composite method according to claim 1, it is characterized in that: described
Gelling agent be the ml of 5 ml~20 propylene oxide.
6. bamboo matrix activated carbon/manganese aerogel composite method is prepared according to described in claim 3, it is characterized in that: described
The oxidizing roasting in Muffle furnace be to be warming up to 350 DEG C~550 DEG C with 5 K/min, keep the temperature the h of 4 h~7.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113086967A (en) * | 2021-04-12 | 2021-07-09 | 北京化工大学 | Preparation method of uniform carbon-manganese oxide composite aerogel electrode material |
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Application publication date: 20190607 |