CN105140042B - A kind of preparation method and applications of bacteria cellulose/activated carbon fiber/CNT membrane material - Google Patents
A kind of preparation method and applications of bacteria cellulose/activated carbon fiber/CNT membrane material Download PDFInfo
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Abstract
A kind of preparation method and applications of bacteria cellulose/activated carbon fiber/CNT membrane material, the present invention relates to a kind of preparation method and applications of membrane material, the invention aims to solve, existing flexible electrode material preparation technology is complicated, cost is high, do not possess the problem of good stability and mechanical property, method is：Standby bacteria cellulose is prepared, prepares activated carbon fiber dispersion liquid；Prepare bacteria cellulose slurry；Composite dispersion liquid is prepared, bacteria cellulose slurry is filtered by vacuum film forming, composite dispersion liquid is then added and continues to filter drying, bacteria cellulose/activated carbon fiber/CNT membrane material is made, the materials application is in ultracapacitor.The present invention is produced on a large scale, and preparation technology is simple, cost is low, conducting membrane material stability and mechanical property are good, and being prepared into ultracapacitor has good capacitive character.The invention belongs to technical field of nano material.
Description
Technical field
The present invention relates to a kind of preparation method and applications of membrane material.
Background technology
Traditional energy sources is increasingly depleted, stimulates people to look for the alternative energy and effective energy storage
Device, and ultracapacitor has high power density and higher energy density, applied to hybrid electric vehicle, electric car, portable
The important field such as formula electronic equipment, enjoys people to favor always.
For today's society to the rapid growth of flexible, flexible equipment energy storage demand, it is of future generation inexpensive, soft that people are badly in need of research and development
Soft, flexible ultracapacitor, and electrode material is most important part.But existing flexible electrode material preparation technology
Complicated, cost height, does not possess good stability and mechanical property.Therefore, using one it is simple, effectively, environmental protection, suitable for rule
The preparation method of modelling production prepares high performance flexible electrode material and is even more important.
The content of the invention
It is high the invention aims to solve existing flexible electrode material preparation technology complexity, cost, do not possess good
Stability and mechanical property the problem of, there is provided a kind of preparation side of bacteria cellulose/activated carbon fiber/CNT membrane material
Method and its application.
A kind of preparation method of bacteria cellulose/activated carbon fiber/CNT membrane material of the present invention, enters as follows
OK：
First, by bacteria cellulose shear it is blocking be immersed in supersound washing in deionized water, then carried out with after liquid nitrogen frozen
15~30h is freeze-dried, obtains standby bacteria cellulose；
2nd, standby bacteria cellulose is placed in tube furnace and carries out high temperature pyrolysis, produce activated carbon fiber, then to activity
Surfactant is added in carbon fiber, redisperse in deionized water, obtains activated carbon fiber dispersion liquid；
3rd, bacteria cellulose is sheared into blocking rear immersion supersound washing in deionized water, is subsequently placed in deionized water,
Stirring makes it be uniformly dispersed, and is then transferred in refiner and stirs, obtains bacteria cellulose slurry；
4th, surfactant is added into the CNT of acidifying, be then dispersed in deionized water, obtain CNT
Dispersion liquid；Carbon nano tube dispersion liquid is added in activated carbon fiber dispersion liquid, stirring makes CNT and activated carbon fiber point
Dissipate uniformly, obtain composite dispersion liquid；
5th, the bacteria cellulose slurry of step 3 is filtered by vacuum film forming, then adds composite dispersion liquid and continue to take out
Film forming is filtered, places into vacuum drying chamber and is dried, bacteria cellulose/activated carbon fiber/CNT membrane material is made；Its
The quality of bacteria cellulose and the activated carbon fiber of step 2 in middle bacteria cellulose/activated carbon fiber/CNT membrane material
Than for (15~1.5):1；Bacteria cellulose and acid in step 4 in bacteria cellulose/activated carbon fiber/CNT membrane material
The mass ratio of the CNT of change is 1:(0.02~0.2).
The application of bacteria cellulose/activated carbon fiber/CNT membrane material of the present invention refers to as application of electrode in super
In level capacitor.
Activated carbon fiber has good chemical stability, electric conductivity and fake capacitance energy storage characteristic, it is considered to be Yi Zhongji
Potential electrode material for super capacitor.Bacteria cellulose, its film have hyperfine network structure, thin after cracking
Fungin can make carbon nano-fiber, gained activated carbon fiber function admirable.
Bacteria cellulose is obtained by the fermentation of microorganism, its function admirable, aboundresources, environment-friendly, film
With hyperfine network structure, high-crystallinity, high-purity, high mechanical properties, as a kind of emerging environmentally friendly material into
For the focus of domestic and international Material Field research, bacteria cellulose contains substantial amounts of hydroxyl, has good hydrophily, with other water
Hydrogenbond easily occurs for the macromolecule of dissolubility, thus bacteria cellulose has natural advantage as composite.
CNT is wide concerned due to its unique structure, chemical property, hot property and electrical property.Its application is
It is related to the many-sides such as nano electron device, catalyst carrier, hydrogen storage material and composite.When it is compound with other carbon materials
Had broad prospects applied to ultracapacitor aspect.
The present invention using it is a kind of it is inexpensive, it is environmentally friendly and can scale preparation method, pass through vacuum filtration, prepare
Go out membrane material and capacitor is assembled into this.Structure shows membrane material good mechanical performance, has good capacitive properties and excellent
Good recycling.Therefore, application of this membrane material in ultracapacitor has wide commercial promise.
Beneficial effects of the present invention：(1) spies such as the hyperfine network structure of bacteria cellulose and excellent mechanical property are utilized
Property, as base load nano active material, ultracapacitor self-supporting self-supporting flexible electrode can be prepared into；(2) it is sharp
Activated carbon fiber is prepared with the direct Pintsch process of the hyperfine network structure of bacteria cellulose；(3) it is produced on a large scale, preparation technology
Simply, energy-conservation, reaction condition be gentle, small toxicity, and raw material cost cheap and easy to get is low, membrane material stability and mechanical property are good；(4)
Directly being used as electrode of super capacitor has good capacitive character.
Brief description of the drawings
Fig. 1 is the photo of bacteria cellulose/activated carbon fiber/CNT membrane material prepared by embodiment 1；
The work prepared with bacteria cellulose/activated carbon fiber/CNT membrane material that Fig. 2 is obtained by embodiment 1
Cyclic voltammetry curve under different scanning speed of the electrode in 6M potassium hydroxide electrolytes；Wherein a is 10mV/s, b 20mV/
S, c 50mV/s；
The work prepared with bacteria cellulose/activated carbon fiber/CNT membrane material that Fig. 3 is obtained by embodiment 1
Constant current charge-discharge curve of the electrode in 6M potassium hydroxide electrolytes；Wherein a is 1mA/cm2, b 2mA/cm2, c 5mA/
cm2, d 10mA/cm2, e 15mA/cm2；
Fig. 4 is the work prepared with bacteria cellulose/activated carbon fiber/CNT membrane material obtained in embodiment 1
Make the AC impedance spectroscopy of electrode；
The work prepared with bacteria cellulose/activated carbon fiber/CNT membrane material that Fig. 5 is obtained by embodiment 2
Cyclic voltammetry curve under different scanning speed of the electrode in 6M potassium hydroxide electrolytes；Wherein a is 10mV/s, b 30mV/
S, c 50mV/s；
The work prepared with bacteria cellulose/activated carbon fiber/CNT membrane material that Fig. 6 is obtained by embodiment 2
Constant current charge-discharge curve of the electrode in 6M potassium hydroxide electrolytes；Wherein a is 1mA/cm2, b 2mA/cm2, c 5mA/
cm2, d 10mA/cm2, e 15mA/cm2；
Fig. 7 is the work prepared with bacteria cellulose/activated carbon fiber/CNT membrane material obtained in embodiment 2
Make the AC impedance spectroscopy of electrode；
The work prepared with bacteria cellulose/activated carbon fiber/CNT membrane material that Fig. 8 is obtained by embodiment 1~2
Make specific capacitance curve of the electrode in 6M potassium hydroxide electrolytes obtained by the calculating of foundation constant current charge-discharge curve, wherein a is BC-
ACF-CNT-1, b BC-ACF-CNT-2.
Embodiment
Technical solution of the present invention is not limited to the embodiment of act set forth below, in addition to each embodiment it
Between any combination.
Embodiment one：A kind of system of bacteria cellulose/activated carbon fiber/CNT membrane material of present embodiment
Preparation Method, carry out as follows：
First, by bacteria cellulose shear it is blocking be immersed in supersound washing in deionized water, then carried out with after liquid nitrogen frozen
15~30h is freeze-dried, obtains standby bacteria cellulose；
2nd, standby bacteria cellulose is placed in tube furnace and carries out high temperature pyrolysis, produce activated carbon fiber, then to activity
Surfactant is added in carbon fiber, redisperse in deionized water, obtains activated carbon fiber dispersion liquid；
3rd, bacteria cellulose is sheared into blocking rear immersion supersound washing in deionized water, is subsequently placed in deionized water,
Stirring makes it be uniformly dispersed, and is then transferred in refiner and stirs, obtains bacteria cellulose slurry；
4th, surfactant is added into the CNT of acidifying, be then dispersed in deionized water, obtain CNT
Dispersion liquid；Carbon nano tube dispersion liquid is added in activated carbon fiber dispersion liquid, stirring makes CNT and activated carbon fiber point
Dissipate uniformly, obtain composite dispersion liquid；
5th, the bacteria cellulose slurry of step 3 is filtered by vacuum film forming, then adds composite dispersion liquid and continue to take out
Film forming is filtered, places into vacuum drying chamber and is dried, bacteria cellulose/activated carbon fiber/CNT membrane material is made；Its
The quality of bacteria cellulose and the activated carbon fiber of step 2 in middle bacteria cellulose/activated carbon fiber/CNT membrane material
Than for (15~1.5):1；Bacteria cellulose and acid in step 4 in bacteria cellulose/activated carbon fiber/CNT membrane material
The mass ratio of the CNT of change is 1:(0.02~0.2).
Activated carbon fiber has good chemical stability, electric conductivity and fake capacitance energy storage characteristic, it is considered to be Yi Zhongji
Potential electrode material for super capacitor.Bacteria cellulose, its film have hyperfine network structure, thin after cracking
Fungin can make carbon nano-fiber, gained activated carbon fiber function admirable.
Bacteria cellulose is obtained by the fermentation of microorganism, its function admirable, aboundresources, environment-friendly, film
With hyperfine network structure, high-crystallinity, high-purity, high mechanical properties, as a kind of emerging environmentally friendly material into
For the focus of domestic and international Material Field research, bacteria cellulose contains substantial amounts of hydroxyl, has good hydrophily, with other water
Hydrogenbond easily occurs for the macromolecule of dissolubility, thus bacteria cellulose has natural advantage as composite.
CNT is wide concerned due to its unique structure, chemical property, hot property and electrical property.Its application is
It is related to the many-sides such as nano electron device, catalyst carrier, hydrogen storage material and composite.When it is compound with other carbon materials
Had broad prospects applied to ultracapacitor aspect.
Present embodiment using it is a kind of it is inexpensive, it is environmentally friendly and can scale preparation method, by vacuum filtration,
Prepare membrane material and capacitor is assembled into this.Structure shows membrane material good mechanical performance, has good capacitive properties
With excellent recycling.Therefore, application of this membrane material in ultracapacitor has wide commercial promise.
The beneficial effect of present embodiment：(1) the hyperfine network structure of bacteria cellulose and excellent mechanical property are utilized
Etc. characteristic, as base load nano active material, ultracapacitor self-supporting self-supporting flexible electrode can be prepared into；
(2) activated carbon fiber is prepared using the direct Pintsch process of the hyperfine network structure of bacteria cellulose；(3) it is produced on a large scale, makes
Standby technique is simple, energy-conservation, reaction condition are gentle, small toxicity, and raw material cost cheap and easy to get is low, membrane material stability and mechanical property
It is good；(4) being directly used as electrode of super capacitor has good capacitive character.
Freeze-drying is carried out in freeze drier in present embodiment, and bacteria cellulose is commercially available prod.
Embodiment two：Present embodiment is unlike embodiment one：Described bacteria cellulose is
Bacteria cellulose leftover pieces.It is other identical with embodiment one.
Embodiment three：Present embodiment is unlike embodiment one or two：It is super described in step 1
The condition of sound washing is ultrasonic time 10h, and each hour changes deionized water.Other and embodiment one or two-phase
Together.
Embodiment four：Unlike one of present embodiment and embodiment one to three：Described in step 2
The method of high temperature degradation be：Standby bacteria cellulose is placed in porcelain boat, is then placed in tube furnace；Argon is passed through into tube furnace
3~8h of gas or nitrogen, and using argon gas or nitrogen as protection gas；Tube furnace is warming up to 270 with 2~4 DEG C/min speed again
DEG C, then be warming up to 390 DEG C with 0.3~0.5 DEG C/min speed, then with 2~4 DEG C/min speed be warming up to 700 DEG C~
1100 DEG C, 2~4h is kept, then 400 DEG C are cooled to 3~5 DEG C/min speed, room temperature is finally naturally cooled to again, that is, completes.
It is other identical with one of embodiment one to three.
Embodiment five：Unlike one of present embodiment and embodiment one to four：Described in step 2
The method of high temperature degradation be：Standby bacteria cellulose is placed in porcelain boat, is then placed in tube furnace；Argon is passed through into tube furnace
Gas or nitrogen 6h, and using argon gas or nitrogen as protection gas, then tube furnace is warming up to 270 DEG C with 4 DEG C/min speed, then with
0.3 DEG C/min speed is warming up to 390 DEG C, is then warming up to 900 DEG C with 4 DEG C/min speed, keeps 2h, then with 5 DEG C/min
Speed be cooled to 400 DEG C, finally naturally cool to room temperature again, that is, complete other phases one of with embodiment one to four
Together.
Embodiment six：Unlike one of present embodiment and embodiment one to five：Described in step 2
Activated carbon fiber and surfactant mass ratio be 1:(0.3~3).Other phases one of with embodiment one to five
Together.
Embodiment seven：Unlike one of present embodiment and embodiment one to six：Described in step 3
Refiner in stir and refer under conditions of stir speed (S.S.) 10000rpm~15000rpm, 5min is stirred in refiner.Its
It is identical with one of embodiment one to six.
Embodiment eight：Unlike one of present embodiment and embodiment one to seven：Described in step 4
The CNT of acidifying and the mass ratio of surfactant be (0.5~0.8):1.It is other with embodiment one to seven it
One is identical.
Embodiment nine：Unlike one of present embodiment and embodiment one to eight：Described surface
Activating agent is neopelex.It is other identical with one of embodiment one to eight.
Embodiment ten：Unlike one of present embodiment and embodiment one to nine：Described in step 4
The preparation method of CNT of acidifying be that CNT is ultrasonically treated 24h in the nitric acid that concentration is 64%, spend from
Sub- water washing, filter drying.It is other identical with one of embodiment one to nine.
Embodiment 11：The application of present embodiment bacteria cellulose/activated carbon fiber/CNT membrane material
Refer to as application of electrode in ultracapacitor.
Beneficial effects of the present invention are verified by following examples：
The preparation method of embodiment 1, the present embodiment bacteria cellulose/activated carbon fiber/CNT membrane material, by as follows
Step is carried out：
First, by bacteria cellulose shear it is blocking be immersed in supersound washing 10h in deionized water, and change within each hour go from
Sub- water, freeze drier is transferred to after liquid nitrogen frozen and dries 20h, obtains standby bacteria cellulose；
2nd, standby bacteria cellulose is placed in porcelain boat, is then placed in tube furnace；Nitrogen is passed through into tube furnace and removes oxygen
6h, and as protection gas, tube furnace is warming up to 270 DEG C with 4 DEG C/min speed first, afterwards 0.3 DEG C/min speed liter
Then temperature is warming up to 900 DEG C to 390 DEG C with 4 DEG C/min speed, keep 2h；400 DEG C are cooled to 5 DEG C/min speed again,
Finally it is down to room temperature naturally again, produces activated carbon fiber, 7.5mg detergent alkylate sulphurs is then added into 25mg activated carbon fibers
Sour sodium, redisperse in deionized water, obtain activated carbon fiber dispersion liquid；
3rd, by the blocking rear immersion supersound washing 10h, and each hour is more in deionized water of 10g bacteria celluloses shearing
Deionized water is changed, is subsequently placed in deionized water, stirring makes it be uniformly dispersed, and is then transferred in refiner with per minute 12000
The speed turned, 5min is stirred, obtains bacteria cellulose slurry；
4th, 0.01g neopelexes are added in the CNT being acidified to 0.008g, is then dispersed in deionization
In water, carbon nano tube dispersion liquid is obtained；Carbon nano tube dispersion liquid is added in activated carbon fiber dispersion liquid, stirring makes carbon nanometer
Pipe and activated carbon fiber are uniformly dispersed, and obtain composite dispersion liquid；
5th, the bacteria cellulose slurry of step 3 is filtered by vacuum film forming, then adds composite dispersion liquid and continue to take out
Film forming is filtered, places into vacuum drying chamber and is dried, bacteria cellulose/activated carbon fiber/CNT membrane material is made.
Bacterium is fine in bacteria cellulose/activated carbon fiber/CNT membrane material after vacuum filtration and vacuum drying
The quality of dimension element is 0.3g.
The photo of bacteria cellulose/activated carbon fiber/CNT membrane material manufactured in the present embodiment is as shown in Figure 1.
By bacteria cellulose/activated carbon fiber/carbon nano-tube film material cutting of acquisition into 1.5cm × 2cm rectangles, directly
Connect and be used as ultracapacitor working electrode, platinized platinum is used as to electrode, using mercury/mercuric oxide electrode as reference electrode, tests self-supporting
The capacitance characteristic of flexible membrane material electrode material.Test sample is labeled as BC-ACF-CNT-1.
Electrode prepared by the bacteria cellulose/activated carbon fiber obtained to the present embodiment/CNT membrane material is in 6M
The cyclic voltammetric performance test without sweep speed is carried out in potassium hydroxide electrolyte, as a result referring to Fig. 2.Difference is shown in figure
The activated carbon fiber of speed is swept in scanning potential region -0.9~0.2V, all the CV curves with quasi- rectangle.
Electrode prepared by the bacteria cellulose/activated carbon fiber obtained to the present embodiment/CNT membrane material is in 6M
Constant current charge-discharge performance test is carried out in potassium hydroxide electrolyte, as a result referring to Fig. 3.From the figure 3, it may be seen that curve is shown very well
Triangle, different multiplying lower curve is respectively provided with preferable symmetry.Maximum area specific capacitance reaches 0.59F/cm2.Such as Fig. 5,
The ac impedance spectroscopy of electrode is by the semicircle of high frequency region, the transitional region institute group between the straight line and semicircle and straight line of low frequency range
Into.
The preparation method of embodiment 2, the present embodiment bacteria cellulose/activated carbon fiber/CNT membrane material, by as follows
Step is carried out：
First, by bacteria cellulose shear it is blocking be immersed in supersound washing 10h in deionized water, and change within each hour go from
Sub- water, freeze drier is transferred to after liquid nitrogen frozen and dries 20h, obtains standby bacteria cellulose；
2nd, standby bacteria cellulose is placed in porcelain boat, is then placed in tube furnace；Nitrogen is passed through into tube furnace and removes oxygen
6h, and as protection gas, tube furnace is warming up to 270 DEG C with 4 DEG C/min speed first, afterwards 0.3 DEG C/min speed liter
Then temperature is warming up to 800 DEG C to 390 DEG C with 4 DEG C/min speed, keep 2h；400 DEG C are cooled to 5 DEG C/min speed again,
Finally it is down to room temperature naturally again, produces activated carbon fiber, 15mg detergent alkylate sulphurs is then added into 50mg activated carbon fibers
Sour sodium, redisperse in deionized water, obtain activated carbon fiber dispersion liquid；
3rd, by the blocking rear immersion supersound washing 10h, and each hour is more in deionized water of 10g bacteria celluloses shearing
Deionized water is changed, is subsequently placed in deionized water, stirring makes it be uniformly dispersed, and is then transferred in refiner with per minute 12000
The speed turned, 5min is stirred, obtains bacteria cellulose slurry；
4th, 0.03g neopelexes are added in the CNT being acidified to 0.015g, is then dispersed in deionization
In water, carbon nano tube dispersion liquid is obtained；Carbon nano tube dispersion liquid is added in activated carbon fiber dispersion liquid, stirring makes carbon nanometer
Pipe and activated carbon fiber are uniformly dispersed, and obtain composite dispersion liquid；
5th, the bacteria cellulose slurry of step 3 is filtered by vacuum film forming, then adds composite dispersion liquid and continue to take out
Film forming is filtered, places into vacuum drying chamber and is dried, bacteria cellulose/activated carbon fiber/CNT membrane material is made.
Bacterium is fine in bacteria cellulose/activated carbon fiber/CNT membrane material after vacuum filtration and vacuum drying
The quality of dimension element is 0.3g.
By bacteria cellulose/activated carbon fiber/carbon nano-tube film material cutting of acquisition into 1.5cm × 2cm rectangles, directly
Connect and be used as ultracapacitor working electrode, platinized platinum is used as to electrode, using mercury/mercuric oxide electrode as reference electrode, tests self-supporting
The capacitance characteristic of flexible membrane material electrode material.Test sample is labeled as BC-ACF-CNT-2.
Electrode prepared by the bacteria cellulose/activated carbon fiber obtained to the present embodiment/CNT membrane material is in hydrogen
The cyclic voltammetric performance test without sweep speed is carried out in potassium oxide electrolyte, as a result referring to Fig. 5.Show that difference is swept in figure
The activated carbon fiber of speed is in scanning potential region -0.9~0.2V, all the CV curves with quasi- rectangle.
Electrode prepared by the bacteria cellulose/activated carbon fiber obtained to the present embodiment/CNT membrane material is in hydrogen
Constant current charge-discharge performance test is carried out in potassium oxide electrolyte, as a result referring to Fig. 6.It will be appreciated from fig. 6 that curve is shown well
Triangle, different multiplying lower curve are respectively provided with preferable symmetry.Maximum area specific capacitance reaches 1.33F/cm2.Such as Fig. 7, electricity
The ac impedance spectroscopy of pole is by the semicircle of high frequency region, the transitional region institute group between the straight line and semicircle and straight line of low frequency range
Into.The working electrode prepared with bacteria cellulose/activated carbon fiber/CNT membrane material that embodiment 1~2 is obtained is in 6M
The specific capacitance curve of gained is calculated as shown in figure 8, as shown in Figure 8 according to constant current charge-discharge curve in potassium hydroxide electrolyte,
BC-ACF-CNT-1 specific capacitance difference 0.59F/cm2,0.54F/cm2, 0.51F/cm2, 0.50F/cm2, 0.48F/cm2；BC-
ACF-CNT-2 specific capacitance difference 1.33F/cm2,1.32F/cm2, 1.22F/cm2, 1.19F/cm2, 1.09F/cm2。
The bacteria cellulose of embodiment 1~2 is commercially available prod.Embodiment 1~2 utilizes bacteria cellulose superfinishing refined net knot
The characteristic such as structure and excellent mechanical property, as base load nano active material, ultracapacitor can be prepared into and used from branch
Support self-supporting flexible electrode；Activated carbon fiber is prepared using the direct Pintsch process of the hyperfine network structure of bacteria cellulose；It can advise
Modelling produces, and preparation technology is simple, save, reaction condition is gentle, small toxicity, and raw material cost cheap and easy to get is low, membrane material is stable
Property and mechanical property are good；Directly being used as electrode of super capacitor has good capacitive character.
Claims (9)
1. a kind of preparation method of bacteria cellulose/activated carbon fiber/CNT membrane material, it is characterised in that this method is by such as
Lower step is carried out：
First, by bacteria cellulose shear it is blocking be immersed in supersound washing in deionized water, then with being freezed after liquid nitrogen frozen
15~30h is dried, obtains standby bacteria cellulose；
2nd, standby bacteria cellulose is placed in tube furnace and carries out high temperature pyrolysis, produce activated carbon fiber, it is then fine to activated carbon
Surfactant is added in dimension, redisperse in deionized water, obtains activated carbon fiber dispersion liquid；
3rd, it is another to take the blocking rear immersion supersound washing in deionized water of bacteria cellulose shearing, it is subsequently placed in deionized water, stirs
Mixing makes it be uniformly dispersed, and is then transferred in refiner and stirs, and obtains bacteria cellulose slurry；
4th, surfactant is added into the CNT of acidifying, be then dispersed in deionized water, obtained CNT and disperse
Liquid；Carbon nano tube dispersion liquid is added in activated carbon fiber dispersion liquid, stirring makes CNT and activated carbon fiber scattered equal
It is even, obtain composite dispersion liquid；
5th, the bacteria cellulose slurry of step 3 is filtered by vacuum film forming, then add composite dispersion liquid continue to filter into
Film, place into vacuum drying chamber and be dried, bacteria cellulose/activated carbon fiber/CNT membrane material is made；It is wherein thin
The mass ratio of bacteria cellulose and the activated carbon fiber of step 2 is in fungin/activated carbon fiber/CNT membrane material
(15~1.5):1；It is acidified in bacteria cellulose/activated carbon fiber/CNT membrane material in bacteria cellulose and step 4
The mass ratio of CNT is 1:(0.02~0.2)；The method of wherein high temperature pyrolysis is：Standby bacteria cellulose is placed in porcelain boat
In, it is then placed in tube furnace；3~8h of argon gas or nitrogen is passed through into tube furnace, and using argon gas or nitrogen as protection gas；Again will
Tube furnace is warming up to 270 DEG C with 2~4 DEG C/min speed, then is warming up to 390 DEG C with 0.3~0.5 DEG C/min speed, then
700 DEG C~1100 DEG C are warming up to 2~4 DEG C/min speed, keeps 2~4h, then 400 are cooled to 3~5 DEG C/min speed
DEG C, room temperature is finally naturally cooled to again, that is, is completed.
2. a kind of preparation method of bacteria cellulose/activated carbon fiber/CNT membrane material according to claim 1,
It is characterized in that described bacteria cellulose is bacteria cellulose leftover pieces.
3. a kind of preparation method of bacteria cellulose/activated carbon fiber/CNT membrane material according to claim 1,
It is characterized in that the condition of the supersound washing described in step 1 and step 3 is ultrasonic time 10h, and changes within each hour and go
Ionized water.
4. a kind of preparation method of bacteria cellulose/activated carbon fiber/CNT membrane material according to claim 1,
It is characterized in that the mass ratio of the activated carbon fiber and surfactant described in step 2 is 1:(0.3~3).
5. a kind of preparation method of bacteria cellulose/activated carbon fiber/CNT membrane material according to claim 1,
Refer to it is characterized in that being stirred in refiner described in step 3 under conditions of stir speed (S.S.) 10000rpm~15000rpm,
5min is stirred in refiner.
6. a kind of preparation method of bacteria cellulose/activated carbon fiber/CNT membrane material according to claim 1,
It is characterized in that the CNT of acidifying and the mass ratio of surfactant described in step 4 are (0.5~0.8):1.
A kind of 7. preparation of bacteria cellulose/activated carbon fiber/CNT membrane material according to claim 1,4 or 6
Method, it is characterised in that described surfactant is neopelex.
8. a kind of preparation method of bacteria cellulose/activated carbon fiber/CNT membrane material according to claim 1,
It is characterized in that the nitric acid that it is 64% in concentration by CNT that the preparation method of the CNT of acidifying described in step 4, which is,
Middle supersound process 24h, is washed with deionized, and filters drying.
9. bacteria cellulose/activated carbon fiber/CNT membrane material that preparation method as claimed in claim 1 obtains is answered
With, it is characterised in that the bacteria cellulose/activated carbon fiber/CNT membrane material is as application of electrode in ultracapacitor
In.
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| JP2017139435A (en) * | 2016-01-29 | 2017-08-10 | 日本ケミコン株式会社 | Electrode, capacitor using the same, and electrode manufacturing method |
| CN105957729B (en) * | 2016-05-18 | 2019-01-18 | 哈尔滨万鑫石墨谷科技有限公司 | A kind of supercapacitor flexible electrode, preparation method and supercapacitor |
| CN105977046A (en) * | 2016-07-28 | 2016-09-28 | 北京化工大学 | Integrated supercapacitor and manufacturing method thereof |
| CN106905562A (en) * | 2017-03-20 | 2017-06-30 | 江南大学 | A kind of bacteria cellulose in situ/functionalized multi-wall carbonnanotubes membrane material and preparation method thereof |
| CN108390012A (en) * | 2018-01-23 | 2018-08-10 | 柔电（武汉）科技有限公司 | A kind of preparation method of flexibility pole piece |
| CN108912375A (en) * | 2018-05-31 | 2018-11-30 | 江南大学 | The oriented growth nanogold bacteria cellulose/compound film method of carbon pipe |
| CN113788965A (en) * | 2021-09-14 | 2021-12-14 | 大连理工大学 | Bacterial cellulose modified bucky paper and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100652065B1 (en) * | 2005-12-19 | 2006-12-01 | 인하대학교 산학협력단 | A method for producing a conductive cellulose film and the same manufactured by the same |
| CN102634870A (en) * | 2012-04-18 | 2012-08-15 | 江南大学 | Carbon-nanotube-reinforced cellulose-base carbon nanofiber and preparation method thereof |
| CN103184586A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacterial-cellulose-fiber-based nano-grade carbon fiber |
| CN103806130A (en) * | 2014-02-24 | 2014-05-21 | 钟春燕 | Preparation method for bacterial cellulose-based nano active carbon fibers |
| CN103886932A (en) * | 2014-03-25 | 2014-06-25 | 深圳市纳米港有限公司 | Carbon nano tube electric conduction slurry and preparation method and application thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100652065B1 (en) * | 2005-12-19 | 2006-12-01 | 인하대학교 산학협력단 | A method for producing a conductive cellulose film and the same manufactured by the same |
| CN103184586A (en) * | 2011-12-31 | 2013-07-03 | 中原工学院 | Preparation method of bacterial-cellulose-fiber-based nano-grade carbon fiber |
| CN102634870A (en) * | 2012-04-18 | 2012-08-15 | 江南大学 | Carbon-nanotube-reinforced cellulose-base carbon nanofiber and preparation method thereof |
| CN103806130A (en) * | 2014-02-24 | 2014-05-21 | 钟春燕 | Preparation method for bacterial cellulose-based nano active carbon fibers |
| CN103886932A (en) * | 2014-03-25 | 2014-06-25 | 深圳市纳米港有限公司 | Carbon nano tube electric conduction slurry and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| Freestanding bacterial cellulose-polypyrrole nanofibres paper electrodes for advanced energy storage devices;Shaohui Li et al;《Nano Energy》;20140819(第9期);第309页摘要、第311页左栏Experimental Section部分，图1 * |
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