CN106693842B - A kind of biomass carbon aeroge and its preparation method and application - Google Patents
A kind of biomass carbon aeroge and its preparation method and application Download PDFInfo
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- CN106693842B CN106693842B CN201611102855.0A CN201611102855A CN106693842B CN 106693842 B CN106693842 B CN 106693842B CN 201611102855 A CN201611102855 A CN 201611102855A CN 106693842 B CN106693842 B CN 106693842B
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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 biomass carbon aeroges and its preparation method and application, which solve existing carbon aerogels preparation method complexity, the technical problem that cost of manufacture is higher, raw material sources are few, it is internal in the presence of multistage pore-size distribution, and the structure to form class duct is serially connected between Kong Yukong, and there is resilience under stress；Based on the biomass carbon aeroge density of bacteria cellulose self assembly up to 1.6mg cm‑3, conductivity reaches 227S m‑1, specific capacity reaches 180F g under the conditions of three electrode tests‑1.Invention also provides preparation methods.It invention can be widely used in the preparation field of carbon aerogels.
Description
Technical field
The present invention relates to electrochemical material field, specifically a kind of biomass carbon aeroge and preparation method thereof and answer
With.
Background technique
Supercapacitor is divided into double electric layers supercapacitor and pseudocapacitors.Double electric layers supercapacitor electrode material is main
It is carbon material, pseudocapacitors electrode material mainly includes metal oxide and conducting polymer.Currently, pseudocapacitors are due to price
Simultaneously commercialization completely is not implemented in the reasons such as valuableness, poor circulation, is commercialized supercapacitor mainly with electric double layer super capacitor
Based on device.Porous carbon materials have the advantages such as large specific surface area, stable structure, long service life, cost performance height, become commercialization
The main electrode material of supercapacitor.
The research of current graphene carbon aeroge and it is prepared into a popular domain.But graphene carbon aeroge is deposited
In cost of manufacture valuableness, the problems such as raw material sources are few, and the preparation process of raw material is complicated.Therefore, the carbon gas of biomass-based self assembly
Gel just obtains the concern of numerous scientific research personnel.There are following advantages for biomass self assembly carbon aerogels: firstly, biomass is from group
The raw material sources for filling carbon aerogels are wide, cheap.Secondly, the aeroge preparation process of biomass self assembly and requirement compare
It is relatively simple, the cost of carbon aerogels can be substantially reduced, so that can be realized large-scale preparation for aeroge provides one kind
It may.
Summary of the invention
The present invention is exactly to solve existing carbon aerogels preparation method complexity, cost of manufacture compared with high, raw material sources are few
Technical problem provides a kind of simple method, low manufacture cost and raw material sources biomass carbon aeroge abundant and its preparation side
Method and application.
For this purpose, the present invention provides a kind of biomass carbon aeroge based on bacteria cellulose self assembly, it is internal in the presence of more
Grade pore-size distribution, and the structure to form class duct is serially connected between Kong Yukong, and there is resilience under stress；Based on thin
The biomass carbon aeroge density of fungin self assembly is up to 1.6mg cm-3, conductivity is up to 227S m-1, three electrode tests
Under the conditions of specific capacity reach 180F g-1。
Present invention simultaneously provides a kind of preparation methods of biomass carbon aeroge, it is characterized in that the following steps are included: (1) powder
Broken and fiber spin-off process: weighing the bacteria cellulose block stored in glacial acetic acid, after being cleaned with deionized water, and be added go from
Sub- water makes its quality and deionized water ratio 1:(5-20), by blocky bacteria cellulose 9000-18000r/min revolving speed,
5-15min is mechanically pulverized into uniform pulpous state suspension；Acetone is added after bacteria cellulose slurries after mechanical crushing are poured out,
And the volume ratio for controlling deionized water and acetone is 1:(1-5), after sealing, stand 1-3 days；(2) self assembling process: by step
(1) the bacteria cellulose pulpous state suspension that obtains takes out, and removes acetone, and additions concentration is 20% ammonium hydroxide, and controls ammonium hydroxide and carefully
The volume ratio of fungin suspension is 1:(5-30), it shakes up, is statically placed under the thermal environment that temperature is 50-150 DEG C, keeps 2-
10h；(3) drying process: the bacteria cellulose aquagel that the self assembly that step (2) obtains is completed is placed at a temperature of -50 DEG C
Quick pre-freeze, and it is freeze-dried 24-48h in the environment of vacuum degree 1Pa, -50 DEG C of temperature, until being completely dried；(4) heat treated
Journey: the biogas gel that step (3) is obtained takes out, and under inert gas shielding atmosphere, carries out at a temperature of 500-900 DEG C
Carbonization, liters temperature rate are 1-10 DEG C/min, and cooling rate is 1-10 DEG C/min, and soaking time 1-4h is to get to bacteria cellulose
The biomass carbon aeroge of self assembly.
The present invention also provides a kind of biomass carbon aeroges to prepare the application in electrode, and pole is made as follows
Polarizing electrode: by bacteria cellulose self assembly carbon aerogels and Kynoar adhesive and N-Methyl pyrrolidone solvent according to matter
Amount is mixed than the ratio for being 70:10:20, and is fully ground by mortar to uniform paste, and platinized platinum is evenly coated at
Pole piece is made in surface, and the pole piece made is dried in vacuo 12 hours in 120 DEG C.
Polarizing electrode is made in bacteria cellulose self assembly carbon aerogels obtained in the present invention as follows, is gone forward side by side
Row electrochemical property test: by bacteria cellulose self assembly carbon aerogels and Kynoar adhesive and N-Methyl pyrrolidone
Solvent is mixed according to the ratio that mass ratio is 70:10:20, and is fully ground by mortar to uniform paste, equably by it
Pole piece is made coated in platinized platinum surface, the pole piece made is dried in vacuo 12 hours in 120 DEG C, in 1M H2SO4 electrolytic cell carries out
Electrochemical property test.
The invention has the following advantages that
(1) the mesoporous of uniformly continuous provides a kind of class cellular structure being serially connected, while existing inside carbon aerogels
A kind of multistage pore-size distribution, the presence of this kind of structure can further improve the specific surface area of bacteria cellulose, thus into one
Its specific capacity of the raising of step and stable circulation performance.Bacteria cellulose self assembly aeroge is due to passing through carbon nano-fiber phase interconnection
It connects, in the carbon nanofiber networks for being partially formed a kind of crosslinking, after high temperature cabonization, so that bacteria cellulose carbon aerogels have
There is excellent electric conductivity, conductivity reaches conductance of the 227S/m much higher than the graphene aerogel of existing report when uncompressed
Rate 20-100S/m.
(2) present invention preparation is simple, controllability is strong, low in cost, application easy to spread, and the present invention with
Bacteria cellulose self assembly prepares carbon aerogels, and cost is only one thousandth of graphene aerogel or so, be good for the environment and
Reduce cost.
Detailed description of the invention
Fig. 1 a is the SEM figure (amplification of the biomass carbon aeroge of bacteria cellulose self assembly prepared by the embodiment of the present invention 1
200 times)；
Fig. 1 b is the SEM figure (amplification of the biomass carbon aeroge of bacteria cellulose self assembly prepared by the embodiment of the present invention 1
10000 times)；
Fig. 2 is the charge and discharge cycles curve of inventive embodiments 2；
Fig. 3 is charge and discharge cycles curve comparison of the charge and discharge cycles curve of the present invention with general aeroge.
Specific embodiment
With reference to the accompanying drawing with preparation method of the invention to the biology of bacteria cellulose self assembly prepared by the present invention
Matter carbon aerogels are further described:
Bacteria cellulose block used in following embodiment of the present invention is purchased from Hainan Lai Ze biochemical technology Co., Ltd.
Embodiment 1
(1) it crushes and fiber spin-off process: weighing the bacteria cellulose block stored in glacial acetic acid, cleaned with deionized water
Afterwards, and deionized water is added makes its quality and deionized water ratio 1:5, by blocky bacteria cellulose turning with 9000r/min
5min is mechanically pulverized into uniform pulpous state suspension in speed；After bacteria cellulose slurries after mechanical crushing are poured out, acetone is added
And the volume ratio for controlling deionized water and acetone is 1:1, is placed in fridge freshness retaining cabinet with preservative film sealing, stands about 1 day or so；
(2) self assembling process: the bacteria cellulose pulpous state suspension that step (1) is obtained takes out a little, and concentration is added and is
20% ammonium hydroxide, and the volume ratio for controlling ammonium hydroxide and bacteria cellulose suspension is 1:5, is shaken up, and places in an oven and controls
Oven temperature is 50 DEG C, stands 2h；
(3) bacteria cellulose aquagel that the self assembly that step (2) obtains is completed drying process: is placed on -50 DEG C of temperature
Quick pre-freeze under degree, and be freeze-dried in the environment of vacuum degree 1Pa, -50 DEG C of temperature for 24 hours to being completely dried；
(4) heat treatment process: the biogas gel that step (3) is obtained takes out, under inert gas shielding atmosphere,
It is carbonized at a temperature of 500 DEG C, heating rate is 1 DEG C/min, and cooling rate is 1 DEG C/min, and soaking time 1h is to get to carefully
The biomass carbon aeroge of fungin self assembly.
1 gained bacteria cellulose biomass carbon aeroge density of embodiment is 3mg/cm, conductivity 100S/m, three electrodes
Measure specific capacity 98F/g.
Embodiment 2
(1) it crushes and fiber spin-off process: weighing the bacteria cellulose block stored in glacial acetic acid, cleaned with deionized water
Afterwards, and deionized water is added makes its quality and deionized water ratio 1:8, by blocky bacteria cellulose turning with 12000r/min
10min is mechanically pulverized into uniform pulpous state suspension in speed；Acetone is added after bacteria cellulose slurries after mechanical crushing are poured out
And the volume ratio for controlling deionized water and acetone is 1:2, is placed in fridge freshness retaining cabinet with preservative film sealing, stands about 2 days or so；
(2) self assembling process: the bacteria cellulose pulpous state suspension that step (1) is obtained takes out a little, removes acetone, adds
Enter concentration and be 20% ammonium hydroxide, and the volume ratio for controlling ammonium hydroxide and bacteria cellulose suspension is 1:15, shakes up, is placed on baking oven
In and control oven temperature be 90 DEG C, stand 5h；
(3) bacteria cellulose aquagel that the self assembly that step (2) obtains is completed drying process: is placed on -50 DEG C of temperature
Quick pre-freeze under degree, and 36h is freeze-dried to being completely dried in the environment of vacuum degree 1Pa, -50 DEG C of temperature；
(4) heat treatment process: the biogas gel that step (3) is obtained takes out, under inert gas shielding atmosphere,
It is carbonized at a temperature of 750 DEG C, liter temperature rate is 5 DEG C/min, and cooling rate is 5 DEG C/min, and soaking time 2h is to get to carefully
The biomass carbon aeroge of fungin self assembly.
2 gained bacteria cellulose biomass carbon aeroge density of embodiment is 2mg/cm, conductivity 226S/m, three electrodes
Measure specific capacity 180F/g.
Embodiment 3
(1) it crushes and fiber spin-off process: weighing the bacteria cellulose block stored in glacial acetic acid, cleaned with deionized water
Afterwards, and deionized water is added makes its quality and deionized water ratio 1:20, by blocky bacteria cellulose with 18000r/min's
15min is mechanically pulverized into uniform pulpous state suspension in revolving speed；Third is added after bacteria cellulose slurries after mechanical crushing are poured out
Ketone simultaneously controls the volume ratio of deionized water and acetone as 1:5, is placed in fridge freshness retaining cabinet with preservative film sealing, stands about 3 days left sides
It is right；
(2) self assembling process: the bacteria cellulose pulpous state suspension that step (1) is obtained takes out a little, removes acetone, adds
Enter the ammonium hydroxide that concentration is 20% and the volume ratio for controlling ammonium hydroxide and bacteria cellulose suspension is 1:30, shakes up, be placed on baking oven
In and control oven temperature be 150 DEG C, stand 10h；
(3) bacteria cellulose aquagel that the self assembly that step (2) obtains is completed drying process: is placed on -50 DEG C of temperature
Quick pre-freeze under degree, and 48h is freeze-dried to being completely dried in the environment of vacuum degree 1Pa, -50 DEG C of temperature；
(4) heat treatment process: the biogas gel that step (3) is obtained takes out, under inert gas shielding atmosphere,
It is carbonized at a temperature of 900 DEG C, liter temperature rate is 10 DEG C/min, and cooling rate is 10 DEG C/min, and soaking time 4h is to get arriving
The biomass carbon aeroge of bacteria cellulose self assembly.
3 gained bacteria cellulose biomass carbon aeroge density of embodiment is 4.8mg/cm, conductivity 198S/m, three electricity
Pole measures specific capacity 120F/g.
Embodiment 4
(1) it crushes and fiber spin-off process: weighing the bacteria cellulose block stored in glacial acetic acid, cleaned with deionized water
Afterwards, and deionized water is added makes its quality and deionized water ratio 1:15, by blocky bacteria cellulose with 18000r/min's
15min is mechanically pulverized into uniform pulpous state suspension in revolving speed；Third is added after bacteria cellulose slurries after mechanical crushing are poured out
Ketone simultaneously controls the volume ratio of deionized water and acetone as 1:2, is placed in fridge freshness retaining cabinet with preservative film sealing, stands about 2 days left sides
It is right；
(2) self assembling process: the bacteria cellulose pulpous state suspension that step (1) is obtained takes out a little, removes acetone, adds
Enter the ammonium hydroxide that concentration is 20% and the volume ratio for controlling ammonium hydroxide and bacteria cellulose suspension is 1:15, shakes up, be placed on baking oven
In and control oven temperature be 80 DEG C, stand 10h；
(3) bacteria cellulose aquagel that the self assembly that step (2) obtains is completed drying process: is placed on -50 DEG C of temperature
Quick pre-freeze under degree, and 48h is freeze-dried to being completely dried in the environment of vacuum degree 1Pa, -50 DEG C of temperature；
(4) heat treatment process: the biogas gel that step (3) is obtained takes out, under inert gas shielding atmosphere,
It is carbonized at a temperature of 800 DEG C, liter temperature rate is 3 DEG C/min, and cooling rate is 10 DEG C/min, and soaking time 1h is to get arriving
The biomass carbon aeroge of bacteria cellulose self assembly.
4 gained bacteria cellulose biomass carbon aeroge density of embodiment is 1.6mg/cm, conductivity 226S/m, three electricity
Pole measures specific capacity 180F/g.
Claims (1)
1. a kind of preparation method of biomass carbon aeroge, it is characterized in that the following steps are included:
(1) it crushes and fiber spin-off process: weighing the bacteria cellulose block stored in glacial acetic acid, after being cleaned with deionized water simultaneously
Deionized water, which is added, makes its quality and deionized water ratio 1:(5-20), by blocky bacteria cellulose in 9000-18000r/
5-15min is mechanically pulverized into uniform pulpous state suspension in the revolving speed of min；Bacteria cellulose slurries after mechanical crushing are poured out
After acetone is added, and controls deionized water and acetone volume ratio be 1:(1-5), after sealing, stand 1-3 days；
(2) self assembling process: the bacteria cellulose pulpous state suspension that step (1) is obtained takes out, and removes acetone, and concentration is added and is
20% ammonium hydroxide, and the volume ratio for controlling ammonium hydroxide and bacteria cellulose suspension is 1:(5-30), it shakes up, being statically placed in temperature is 50-
Under 150 DEG C of thermal environment, 2-10h is kept；
(3) drying process: the bacteria cellulose aquagel that the self assembly that step (2) obtains is completed is placed at a temperature of -50 DEG C
Quick pre-freeze, and it is freeze-dried 24-48h in the environment of vacuum degree 1Pa, -50 DEG C of temperature, until being completely dried；
(4) heat treatment process: the biogas gel that step (3) is obtained takes out, under inert gas shielding atmosphere, 500-
Be carbonized at a temperature of 900 DEG C, liter temperature rate be 1-10 DEG C/min, cooling rate be 1-10 DEG C/min, soaking time 1-4h,
Obtain the biomass carbon aeroge of bacteria cellulose self assembly.
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| CN109317063B (en) * | 2018-12-13 | 2021-01-29 | 黑龙江科技大学 | Carbon aerogel and preparation method thereof |
| CN110127653B (en) * | 2019-05-22 | 2021-06-04 | 中国林业科学研究院木材工业研究所 | Method for preparing flexible block carbon by carbonizing small wood blocks |
| CN111933457A (en) * | 2020-08-13 | 2020-11-13 | 武汉理工大学 | Preparation method of novel staggered communicated nanowire supercapacitor electrode |
| CN112103090B (en) * | 2020-08-24 | 2021-11-30 | 宁波工程学院 | Self-supporting flexible supercapacitor |
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