CN111662478A - Preparation method of graphene aerogel with stable structure - Google Patents
Preparation method of graphene aerogel with stable structure Download PDFInfo
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- CN111662478A CN111662478A CN202010464489.3A CN202010464489A CN111662478A CN 111662478 A CN111662478 A CN 111662478A CN 202010464489 A CN202010464489 A CN 202010464489A CN 111662478 A CN111662478 A CN 111662478A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
Abstract
The invention discloses a preparation method of graphene aerogel with a stable structure, which comprises the following steps: step S1, obtaining bacterial cellulose; and step S2, obtaining the graphene/metal salt/bacterial cellulose aerogel composite material. By adopting the technical scheme of the invention, no adhesive is needed to be added, the bacterial cellulose hydrogel provides a support framework of the composite material, compared with the traditional graphene aerogel material, the graphene aerogel material has good structural stability, the filled graphene can provide good electronic conductivity, and the ion conductivity of the composite material can be enhanced by the filled metal salts, such as lithium nitrate, copper nitrate and the like. The technical scheme can provide a preparation method of the novel composite material with better structural stability and excellent electronic/ionic conductivity.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of graphene/metal salt/bacterial cellulose aerogel with a stable structure.
Background
The super capacitor is used as a novel green energy source in the 21 st century, and has the advantages of high charging and discharging speed, high efficiency, good stability and the like, so that the super capacitor has great market potential. The current electrode material for the super capacitor is mainly a carbon material, wherein the activated carbon has low cost and meets the characteristic of high specific surface area required by the electrode material for the super capacitor. However, the conductivity of the activated carbon is general, and the microstructure mainly exists in a micropore form, so that the activated carbon has a large resistance in an electrolyte, and the process of soaking the electrode with the electrolyte is slow, and the process of storing and transmitting charges is also slow.
The bacterial cellulose has the characteristics of high water absorption and water retention, high transmittance to liquid and gas, high wet strength, in-situ processing and forming in a wet state, and the like. The high purity and excellent performance enable the bacterial cellulose fiber to be widely applied in special fields. Although the bacterial cellulose has excellent properties, the bacterial cellulose also has defects of mechanical properties and electrical conductivity, and the development and the application of the bacterial cellulose are influenced.
The graphene material is greatly valued since the coming out, and has the advantages of good electrical conductivity, high specific surface area, small density, special heat-conducting property and optical property, high mechanical property and the like, and can meet the requirements of ideal supercapacitor electrode materials.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of graphene/metal salt/bacterial cellulose aerogel with a stable structure. The preparation process does not need to add an adhesive, and can be applied to the preparation of the electrode material of the super capacitor.
In order to solve the technical problems in the prior art, the invention provides a preparation method of a graphene aerogel with a stable structure, which comprises the following steps:
step S1, obtaining bacterial cellulose;
step S2, obtaining a graphene/metal salt/bacterial cellulose hydrogel composite material;
wherein the step S1 further comprises the steps of:
s10: soaking the bacterial cellulose hydrogel in deionized water for 2 days, replacing the deionized water every day, and removing impurities in the cellulose hydrogel;
s11: covering and pressing the soaked bacterial cellulose hydrogel with a weight for 2 days to remove water in the hydrogel;
the step S2 further includes the steps of:
s20: dispersing graphene in deionized water, adding metal salts such as lithium nitrate, copper nitrate and the like, mixing and stirring for 20-40 minutes;
s21: putting the bacterial cellulose into the mixed solution, stirring in a water bath at 26-50 ℃ for 1-3 hours to enable the bacterial cellulose to fully absorb the solution, and obtaining a finished product of graphene/metal salt/bacterial cellulose hydrogel;
s22: and (3) putting the bacterial cellulose hydrogel into a freeze dryer, freezing for 6-10 hours and drying for 12 hours, and taking out to obtain the finished product graphene/metal salt/bacterial cellulose aerogel composite material.
As a preferable technical solution, in step S10, the thickness of the selected bacterial cellulose hydrogel is 0.5 cm, and the deionized water is replaced every 12 hours.
Preferably, in step S20, lithium nitrate is used as the metal salt at room temperature, and the ratio of graphene, lithium nitrate and water is 3:4: 160.
Preferably, in step S21, the water bath heating and stirring temperature is 35 deg.C, the rotation speed is 250r/min, and the stirring time is 2 hours.
Preferably, in step S22, the temperature is maintained at-55 ℃ to-60 ℃ during freeze-drying.
The invention also discloses a super capacitor, and the electrode material of the super capacitor adopts the graphene/metal salt/bacterial cellulose aerogel composite material as claimed in the invention.
Compared with the prior art, the invention has the following beneficial effects:
(1) the graphene aerogel prepared by the traditional method is easy to collapse and collapse, and the scheme adopts the bacterial cellulose as the skeleton support of the graphene aerogel, so that good structural stability can be provided for the material without adding an adhesive.
(2) The bacterial cellulose has a fine nano-scale net structure, the graphene sheet-shaped particles and the metal salt are uniformly filled in the bacterial cellulose hydrogel, wherein the graphene provides excellent electronic conductivity, and the filled metal salt can enhance the ion transmission capability of the composite material.
(3) The invention provides a preparation method of a composite material with good electronic/ionic conductivity, and the preparation method does not need to add an adhesive in the preparation process and can be applied to the preparation of an electrode material of a super capacitor.
Drawings
Fig. 1 is a flow chart illustrating steps of a graphene/metal salt/bacterial cellulose aerogel preparation method according to the present invention;
fig. 2 is an SEM image of the graphene/metal salt/bacterial cellulose aerogel composite material of instantiation 1 of the present invention, as observed under a scanning electron microscope;
the following specific embodiments will further illustrate the invention in conjunction with the above-described figures.
Detailed Description
In order to better explain the process and scheme of the present invention, the following invention is further described with reference to the accompanying drawings and examples. The specific embodiments described herein are merely illustrative of the invention and do not delimit the invention.
Aiming at the problem that the traditional prepared graphene aerogel is easy to collapse, the invention provides an improved scheme, the graphene aerogel is structurally supported by bacterial cellulose, so that good structural stability is obtained, and meanwhile, the material has excellent electronic/ionic conductivity.
Referring to fig. 1, the invention provides a preparation method of graphene aerogel with stable structure, which is based on bacterial cellulose hydrogel to prepare a composite material, wherein the bacterial cellulose is a porous meshed nano-scale biopolymer synthesized by microbial fermentation, and the graphene aerogel has a hyperfine meshed structure, higher water absorption and retention performance, higher biocompatibility, adaptability and good biodegradability.
Step S1, obtaining bacterial cellulose;
step S2, obtaining a graphene/metal salt/bacterial cellulose hydrogel composite material;
wherein the step S1 further comprises the steps of:
s10: soaking the bacterial cellulose hydrogel in deionized water for 2 days, replacing the deionized water every day, and removing impurities in the cellulose hydrogel;
s11: covering and pressing the soaked bacterial cellulose hydrogel with a weight for 2 days to remove water in the hydrogel;
the step S2 further includes the steps of:
s20: dispersing graphene in deionized water, adding metal salts such as lithium nitrate, copper nitrate and the like, mixing and stirring for 20-40 minutes;
s21: putting the bacterial cellulose into the mixed solution, stirring in a water bath at 26-50 ℃ for 1-3 hours to enable the bacterial cellulose to fully absorb the solution, and obtaining a finished product of graphene/metal salt/bacterial cellulose hydrogel;
s22: and (3) putting the bacterial cellulose hydrogel into a freeze dryer, freezing for 6-10 hours and drying for 12 hours at the temperature of-55 ℃ to-60 ℃, and taking out to obtain the finished product graphene/metal salt/bacterial cellulose aerogel composite material.
According to the technical scheme, water in the bacterial cellulose hydrogel is removed to obtain bacterial cellulose, then graphene dispersion liquid is obtained through stirring, metal salt is added and stirred to obtain mixed solution, the prepared graphene/metal salt mixed solution is uniformly filled into the bacterial cellulose through water bath heating and stirring, and finally the bacterial cellulose hydrogel is subjected to moisture removal through a freeze drying technology to obtain the graphene/metal salt/bacterial cellulose aerogel composite material.
EXAMPLE 1
And (3) soaking the bacterial cellulose hydrogel in deionized water for 2 days, and replacing the deionized water every 12 hours to remove impurities in the cellulose hydrogel. And covering and pressing the soaked bacterial cellulose hydrogel for 2 days by using a weight, and removing water in the hydrogel to obtain pure bacterial cellulose. Taking graphene, lithium nitrate and water in a mass ratio of 3:4:160 at room temperature, mixing and stirring the graphene and the water to obtain a graphene dispersion liquid, adding the lithium nitrate, mixing and stirring for 30 minutes. And (2) putting the bacterial cellulose into the mixed solution, stirring for 2 hours at a speed of 250 revolutions per minute under the condition of heating in a water bath at 35 ℃ to enable the bacterial cellulose to fully absorb the solution, putting the obtained bacterial cellulose hydrogel into a freeze dryer, freezing for 6 hours and drying for 12 hours at-55 ℃, and taking out to obtain the finished product graphene/metal salt/bacterial cellulose aerogel composite material.
Instantiation 2
And (3) soaking the bacterial cellulose hydrogel in deionized water for 2 days, and replacing the deionized water every 12 hours to remove impurities in the cellulose hydrogel. And covering and pressing the soaked bacterial cellulose hydrogel for 2 days by using a weight, and removing water in the hydrogel to obtain pure bacterial cellulose. Taking graphene, lithium nitrate and water in a mass ratio of 1:2:80 at room temperature, mixing and stirring the graphene and the water to obtain a graphene dispersion liquid, adding the lithium nitrate, mixing and stirring for 20 minutes. And (2) putting the bacterial cellulose into the mixed solution, stirring for 2 hours at a speed of 250 revolutions per minute under the condition of heating in a water bath at 35 ℃ to enable the bacterial cellulose to fully absorb the solution, putting the obtained bacterial cellulose hydrogel into a freeze dryer, freezing for 8 hours and drying for 12 hours at-55 ℃, and taking out to obtain the finished product graphene/metal salt/bacterial cellulose aerogel composite material.
Instantiation 3
And (3) soaking the bacterial cellulose hydrogel in deionized water for 2 days, replacing the deionized water every day, and removing impurities in the cellulose hydrogel. And covering and pressing the soaked bacterial cellulose hydrogel for 2 days by using a weight, and removing water in the hydrogel to obtain pure bacterial cellulose. Taking graphene, copper nitrate and water in a mass ratio of 3:6.6:160 at room temperature, mixing and stirring the graphene and the water to obtain a graphene dispersion solution, adding the copper nitrate, mixing and stirring for 30 minutes. And (2) putting the bacterial cellulose into the mixed solution, stirring for 1 hour at the speed of 200 revolutions per minute under the heating of water bath at 26 ℃ to enable the bacterial cellulose to fully absorb the solution, putting the obtained bacterial cellulose hydrogel into a freeze dryer, freezing for 8 hours and drying for 12 hours at the temperature of minus 60 ℃, and taking out to obtain the finished product graphene/metal salt/bacterial cellulose aerogel composite material.
Instantiation 4
And (3) soaking the bacterial cellulose hydrogel in deionized water for 2 days, replacing the deionized water every day, and removing impurities in the cellulose hydrogel. And covering and pressing the soaked bacterial cellulose hydrogel for 2 days by using a weight, and removing water in the hydrogel to obtain pure bacterial cellulose. Taking graphene, lithium nitrate and water in a mass ratio of 3:4:160 at room temperature, mixing and stirring the graphene and the water to obtain a graphene dispersion liquid, adding the lithium nitrate, mixing and stirring for 40 minutes. And (2) putting the bacterial cellulose into the mixed solution, stirring for 3 hours at the speed of 350 revolutions per minute under the heating of a water bath at 50 ℃ to enable the bacterial cellulose to fully absorb the solution, putting the obtained bacterial cellulose hydrogel into a freeze dryer, freezing for 8 hours and drying for 12 hours at the temperature of-55 ℃, and taking out to obtain the finished product graphene/metal salt/bacterial cellulose aerogel composite material.
Fig. 2 is an SEM image observed under a scanning electron microscope after the graphene/metal salt/bacterial cellulose aerogel composite material in instantiation 1 of the present invention is carbonized at a high temperature, and it can be seen from the figure that the bacterial cellulose stably supports the graphene, increases the electronic and ionic conductivity, and effectively inhibits the aggregation of the graphene.
Further, the aerogel is put into a tube furnace, the temperature is raised to 800 ℃ at the speed of 2 ℃/min under the protection of argon atmosphere, the aerogel is calcined for 2 hours, then the temperature is naturally reduced, and the graphene/metal salt/carbon nanofiber composite material after being cooled is cut into circular electrode plates with the diameter of 16 mm.
The specific assembly process is as follows: the supercapacitor was assembled using CR2016 coin cells. The two electrodes are prepared graphene/metal salt/carbon nanofiber composite electrodes, the TF4030 cellulose diaphragm is used as a diaphragm, and 6mol/L KOH solution is used as electrolyte.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (5)
1. The preparation method of the graphene aerogel with the stable structure is characterized by comprising the following steps:
step S1, preparing bacterial cellulose;
step S2, preparing the graphene/metal salt/bacterial cellulose hydrogel composite material on the basis of the step S1;
wherein the step S1 further comprises the steps of:
s10: soaking the bacterial cellulose hydrogel in deionized water for 2 days, replacing the deionized water every day, and removing impurities in the cellulose hydrogel;
s11: covering and pressing the soaked bacterial cellulose hydrogel with a weight for 2 days to remove water in the hydrogel;
the step S2 further includes the steps of:
s20: dispersing graphene in deionized water, adding metal salts, mixing and stirring for 20-40 minutes;
s21: putting the bacterial cellulose into the mixed solution, stirring in a water bath at 26-50 ℃ for 1-3 hours to enable the bacterial cellulose to fully absorb the solution, and obtaining a finished product of graphene/metal salt/bacterial cellulose hydrogel;
s22: and (3) putting the bacterial cellulose hydrogel into a freeze dryer, freezing for 6-10 hours and drying for 12 hours, and taking out to obtain the finished product graphene/metal salt/bacterial cellulose aerogel composite material.
2. The method for preparing the graphene aerogel with stable structure according to claim 1, wherein in step S20, the metal salt is lithium nitrate or copper nitrate.
3. The method for preparing a graphene aerogel with a stable structure according to claim 1 or 2, wherein in step S10, the thickness of the selected bacterial cellulose hydrogel is 0.5 cm, and the deionized water is replaced every 12 hours.
4. The method for preparing the graphene aerogel with stable structure according to claim 1 or 2, wherein in step S20, lithium nitrate is used as the metal salt at room temperature, and the ratio of graphene, lithium nitrate and water is 3:4: 160.
5. The method for preparing the graphene aerogel with stable structure according to claim 1 or 2, wherein in step S21, the temperature of water bath heating and stirring is 35 ℃, the rotation speed is 250r/min, and the stirring time is 2 hours.
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Citations (5)
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| CN110473711A (en) * | 2019-07-12 | 2019-11-19 | 杭州电子科技大学 | A kind of preparation method of electrode material for super capacitor |
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2020
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