CN111847430A - Preparation method of high-strength high-resilience graphene aerogel - Google Patents
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Abstract
The invention relates to the technical field of graphene, and discloses a preparation method of a high-strength high-resilience graphene aerogel, which comprises the following steps: a. adding a certain amount of graphite oxide into the alkaline solution, mechanically stirring for 0.5-6 h, and preparing a graphene oxide solution with a concentration of 2-10 mg/ml and good dispersibility; b. b, adjusting the temperature of the graphene oxide solution prepared in the step a to be between the freezing point and the boiling point of water, adding a reducing agent, magnetically stirring for 0.5-2 h, pouring into a reaction kettle, sealing, and then putting into an oven for hydrothermal reaction to obtain graphene hydrogel; c. and c, washing the graphene hydrogel prepared in the step b with 2% -20% ethanol solution for multiple times, and freeze-drying to obtain the high-strength high-resilience graphene aerogel. The graphene aerogel is low in density, high in mechanical strength, uniform in cross-linked pores, high in conductivity, good in rebound resilience and high in application value.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a high-strength high-resilience graphene aerogel and a preparation method thereof.
Background
Aerogel was first proposed by Kistler in 1931 asA nano-porous solid material with ultra-low density, large pore volume and high specific surface area is characterized by a three-dimensional network structure formed by connecting nano-particles, generally speaking, an aerogel is firstly prepared into wet gel through a sol-gel process, then a solvent with larger surface tension in network gaps is removed through a solvent exchange process, and finally a special drying method (such as supercritical CO) is utilized (for example, the solvent exchange process is adopted)2Drying, freeze-drying) to produce an aerogel.
The graphene has excellent physicochemical properties, and the unique structure enables the graphene to resist acid and alkali; the material has unique thermal property and excellent heat conductivity, and the heat conductivity coefficient of the material is more than one time higher than that of other materials; unique electrical and optical properties, high electron mobility, good transparency and excellent mechanical properties, the Young modulus can reach 1TPa, and the theoretical specific surface area can reach 2600m2(ii)/g; the unique and excellent performance ensures that the graphene has wide potential application prospect in many fields; however, graphene is often agglomerated and accumulated due to pi-pi interaction, so that the specific surface area is reduced, the resistance is increased, and the performance is greatly reduced, thereby limiting the application prospect of the graphene.
One of the most effective solutions to this problem is to self-assemble graphene sheets to have a three-dimensional network structure, i.e., Graphene Aerogel (GA); the graphene aerogel inherits the characteristics of high specific surface area, high porosity, high electrical conductivity, good thermal conductivity, good mechanical strength and the like of the graphene and the aerogel; although graphene aerogels have unique properties such as ultra-low density, superelasticity, and versatility, developing a superelasticity and fatigue-resistant graphene aerogel with ultra-low density is a great challenge, as increasing mechanical properties while decreasing aerogel density is often contradictory.
Disclosure of Invention
The invention aims to solve the technical problem that the low density and the mechanical property of the traditional graphene aerogel can not be simultaneously considered, and provides a preparation method of the graphene aerogel, which is simple in process, green and environment-friendly, has high strength and high resilience, and has extremely high conductivity.
The technical scheme of the invention is as follows:
a preparation method of a high-strength high-resilience graphene aerogel comprises the following steps:
a. adding a certain amount of graphite oxide into the alkaline solution, mechanically stirring for 0.5-6 h, and preparing a graphene oxide solution with a concentration of 2-10 mg/ml and good dispersibility;
b. B, adjusting the temperature of the graphene oxide solution prepared in the step a to be between the freezing point and the boiling point of water, adding a reducing agent, magnetically stirring for 0.5-2h, pouring into a reaction kettle, sealing, and then putting into an oven for hydrothermal reaction to obtain graphene hydrogel;
c. and c, washing the graphene hydrogel prepared in the step b with 2% -20% ethanol solution for multiple times, and freeze-drying to obtain the high-strength high-resilience graphene aerogel.
Preferably, the drying method in step c adopts supercritical drying, and specifically comprises the following steps: and (2) carrying out solvent replacement on solvent water, soluble reactants and reaction products existing in the graphene hydrogel by adopting ethanol or ammonia water, freezing, and drying by adopting a supercritical ethanol or supercritical ammonia water mode.
Preferably, the freezing is directional freezing or non-directional freezing, the freezing temperature is-10 ℃ to the liquid nitrogen temperature, the drying time is 20-60 h, and the drying vacuum degree is 0.1-50000 Pa.
Preferably, the reducing agent in step b is one of L-ascorbic acid, saccharides, ammonia water, sodium citrate, sodium borohydride, hydroiodic acid, sodium bisulfate and ethylenediamine.
Preferably, the mass ratio of the reducing agent to the graphene oxide in the step b is 1: 1-50: 1.
Preferably, the hydrothermal reaction in step b is carried out at 85-180 ℃ for 1.5-24 h.
The high-strength high-resilience graphene aerogel is an inorganic conductive aerogel with a three-dimensional network structure formed by mutually crosslinking two-dimensional graphene; the aperture of the graphene aerogel is 1 nm-200 mu m, the porosity is 75-95%, the density is 2-50mg/cm3, the compression rate is 0-90%, the conductivity is 1-1000S/m, the specific surface area is 100-800 m2/g, and the stress is 0-60 KPa.
The invention has the beneficial effects that: the invention provides a high-strength high-resilience graphene aerogel and a preparation method thereof, the method adopts alkali-dispersed graphene oxide to prepare the graphene aerogel, not only can realize low density and high mechanical property, but also can have a highly ordered network structure and high conductivity, and overcomes the technical problem that the low density and the mechanical property of the traditional graphene aerogel can not be simultaneously considered, so that the high-strength high-resilience graphene aerogel prepared by the method can be widely applied to the fields of solvent adsorption, gas-sensitive sensing and the like.
Drawings
Fig. 1 is an SEM image of the graphene aerogel prepared in example 2.
FIG. 2 is a graph of different stress-strain curves for aerogels prepared in example 3.
FIG. 3 is a stress-strain plot of 50% strain for 500 cycles of the aerogel prepared in example 4.
Detailed Description
Example 1:
preparing graphene oxide by using an improved Hummers method: mixing 2g of flake graphite with 50ml of concentrated sulfuric acid, and stirring in an ice water bath for 30min to form a suspension; transferring the beaker to a water bath kettle at 40 ℃, adding 1g of potassium permanganate each time, adding 4g of potassium permanganate in total, adding 1 time every 15min, and continuing to react at the medium temperature of 40 ℃ for 24 hours after the potassium permanganate is added; after the medium-temperature reaction is finished, transferring the beaker to a water bath kettle at the temperature of 98 ℃, continuously stirring, and keeping the temperature of the solution at 98 ℃; then adding hydrogen peroxide until no gas is generated (namely bubbles are not released), then washing for 2 times by using 5% hydrochloric acid, washing by using deionized water until the pH value is =7, and freeze-drying to obtain graphite oxide powder.
Mixing 200mg of graphene oxide powder with 100ml of deionized water, mechanically stirring for 0.5 h, preparing a graphene oxide solution with the concentration of 2mg/ml, and adjusting the pH to 12; adding 600mg of L-ascorbic acid into the solution, stirring for 1h, pouring the solution into a reaction kettle, reacting for 6h at 85 ℃, performing solvent replacement for 3 days by using 10% ethanol, replacing the ethanol solution twice a day, freezing at-20 ℃ after the solvent replacement is finished, and drying for 20h under the condition of drying vacuum degree of 1000 Pa to obtain the high-strength high-resilience graphene aerogel.
Example 2:
preparing graphene oxide by using an improved Hummers method: mixing 2g of flake graphite with 50ml of concentrated sulfuric acid, and stirring in an ice water bath for 30min to form a suspension; transferring the beaker to a water bath kettle at 40 ℃, adding 1g of potassium permanganate each time, adding 4g of potassium permanganate in total, adding 1 time every 15min, and continuing to react at the medium temperature of 40 ℃ for 24 hours after the potassium permanganate is added; and after the medium-temperature reaction is finished, transferring the beaker to a 98 ℃ water bath kettle, continuously stirring, keeping the temperature of the solution at 98 ℃, then adding hydrogen peroxide until no gas is generated (namely bubbles are not released), then washing for 2 times by using 5% hydrochloric acid, washing by using deionized water until the pH value is =7, and freeze-drying to obtain the graphite oxide powder.
Mixing 200mg of graphite oxide powder with 100ml of deionized water, mechanically stirring for 0.5 h, preparing a graphene oxide solution with the concentration of 2mg/ml, and adjusting the pH to 12; adding 2g of glucose into the solution, stirring for 2h, pouring the solution into a reaction kettle, reacting for 6h at 100 ℃, carrying out solvent replacement for 3 days by using 10% ethanol, replacing the ethanol solution twice a day, freezing at-30 ℃ after the solvent replacement is finished, and drying for 30h under the condition of the drying vacuum degree of 2000 Pa to obtain the high-strength high-resilience graphene aerogel.
As shown in fig. 1, is an SEM image of the graphene aerogel.
As can be seen from the figure, the graphene aerogel is an inorganic conductive aerogel with a three-dimensional network structure formed by two-dimensional graphene cross-linking, and can form an ordered pore structure after hydrothermal reaction after alkali treatment, wherein the pore width is 20-30 μm, which is one of the reasons that the aerogel has high mechanical properties.
Through determination, the aperture of the graphene aerogel is 1nm-100 mu m, the porosity is 75-95%, and the density is 5-50 mg/cm3Compressibility of 0-90%, conductivity of 1-1000S/m, specific surface area of 100-2The stress is 0-60 KPa.
Example 3:
preparing graphene oxide by using an improved Hummers method: mixing 2g of flake graphite with 50ml of concentrated sulfuric acid, and stirring in an ice water bath for 30min to form a suspension; transferring the beaker to a water bath kettle at 40 ℃, adding 1g of potassium permanganate, adding 4g of potassium permanganate totally, adding 1 time every 15min, and continuing to react at the medium temperature of 40 ℃ for 24 hours after the potassium permanganate is added; and after the medium-temperature reaction is finished, transferring the beaker to a 98 ℃ water bath kettle, continuously stirring, keeping the temperature of the solution at 98 ℃, then adding hydrogen peroxide until no gas is generated (namely bubbles are not released), then washing for 2 times by using 5% hydrochloric acid, washing by using deionized water until the pH value is =7, and freeze-drying to obtain the graphite oxide powder.
Mixing 1g of graphene oxide powder with 100ml of deionized water, mechanically stirring for 0.5h, preparing a graphene oxide solution with the concentration of 10mg/ml, and adjusting the pH to 12; adding 1g of sodium borohydride into the solution, stirring for 0.5h, pouring the solution into a reaction kettle, reacting for 3h at 120 ℃, performing solvent replacement for 3 days by using 10% ethanol, replacing the ethanol solution twice a day, freezing at-20 ℃ after the solvent replacement is finished, and drying for 60h under the condition of a drying vacuum degree of 1000 Pa to obtain the high-strength high-resilience graphene aerogel.
As shown in fig. 2, different stress-strain curves for graphene aerogels.
The graphene aerogel with the mass of only 12mg can bear the load of 30KPa under the strain of 70%, which shows the excellent mechanical properties of the graphene aerogel.
Example 4:
preparing graphite oxide by a modified Hummers method: mixing 2g of flake graphite with 50ml of concentrated sulfuric acid, and stirring in an ice water bath for 30min to form a suspension; transferring the beaker to a water bath kettle at 40 ℃, adding 1g of potassium permanganate, adding 4g of potassium permanganate totally, adding 1 time every 15min, and continuing to react at the medium temperature of 40 ℃ for 24 hours after the potassium permanganate is added; and after the medium-temperature reaction is finished, transferring the beaker to a 98 ℃ water bath kettle, continuously stirring, keeping the temperature of the solution at 98 ℃, then adding hydrogen peroxide until no gas is generated (namely bubbles are not released), then washing for 2 times by using 5% hydrochloric acid, washing by using deionized water until the pH value is =7, and freeze-drying to obtain the graphite oxide powder.
Mixing 400mg of graphene oxide powder with 100ml of deionized water, mechanically stirring for 0.5 h, preparing a graphene oxide solution with the concentration of 4mg/ml, and adjusting the pH to 12; adding 800mg of sodium citrate into the solution, stirring for 1h, pouring the solution into a reaction kettle, reacting for 6h at 180 ℃, carrying out solvent replacement for 3 days by using ammonia water, replacing an ethanol solution twice a day, freezing at-50 ℃ after the solvent replacement is finished, and drying for 20h under the condition of 50000 Pa of drying vacuum degree to obtain the high-strength high-resilience graphene aerogel.
As shown in fig. 3, the stress-strain curve of the graphene aerogel obtained 50% strain for 500 cycles.
After 500 cycles, the height of the graphene aerogel is kept at 95.6%, the maximum stress is kept at 70.3%, and excellent mechanical properties are shown.
Example 5:
preparing graphite oxide by a modified Hummers method: mixing 2g of flake graphite with 50ml of concentrated sulfuric acid, and stirring in an ice water bath for 30min to form a suspension; transferring the beaker to a water bath kettle at 40 ℃, adding 1g of potassium permanganate, adding 4g of potassium permanganate in total, adding 1g of potassium permanganate every 15min, and continuing to react at the medium temperature of 40 ℃ for 24h after the potassium permanganate is added; and after the medium-temperature reaction is finished, transferring the beaker to a 98 ℃ water bath kettle, continuously stirring, keeping the temperature of the solution at 98 ℃, then adding hydrogen peroxide until no gas is generated (namely bubbles are not released), then washing for 2 times by using 5% hydrochloric acid, washing by using deionized water until the pH value is =7, and freeze-drying to obtain the graphite oxide powder.
Mixing 500mg of graphite oxide powder with 100ml of deionized water, mechanically stirring for 0.5 h, preparing a graphene oxide solution with the concentration of 5mg/ml, and adjusting the pH value to 12; adding an ethylenediamine solution containing 500mg into the solution, stirring for 1h, pouring the solution into a reaction kettle, reacting for 6h at 180 ℃, carrying out solvent replacement for 3 days by using ammonia water, replacing the ethanol solution twice a day, freezing at-30 ℃ after the solvent replacement is finished, and drying for 40h under the condition of drying vacuum degree of 3000 Pa to obtain the high-strength high-resilience graphene aerogel.
The foregoing is merely a preferred embodiment of the invention and all such equivalent alterations and permutations and derivations thereof are intended to be included within the scope of the invention.
Claims (7)
1. A preparation method of a high-strength high-resilience graphene aerogel is characterized by comprising the following steps:
a. adding a certain amount of graphite oxide into the alkaline solution, mechanically stirring for 0.5-6 h, and preparing a graphene oxide solution with a concentration of 2-10 mg/ml and good dispersibility;
b. b, adjusting the temperature of the graphene oxide solution prepared in the step a to be between the freezing point and the boiling point of water, adding a reducing agent, magnetically stirring for 0.5-2h, pouring into a reaction kettle, sealing, and then putting into an oven for hydrothermal reaction to obtain graphene hydrogel;
c. And c, washing the graphene hydrogel prepared in the step b with 2% -20% ethanol solution for multiple times, and freeze-drying to obtain the high-strength high-resilience graphene aerogel.
2. The preparation method of the high-strength high-resilience graphene aerogel according to claim 1, wherein the preparation method comprises the following steps: the drying method in the step c adopts supercritical drying, and specifically comprises the following steps: and (2) carrying out solvent replacement on solvent water, soluble reactants and reaction products existing in the graphene hydrogel by adopting ethanol or ammonia water, freezing, and drying by adopting a supercritical ethanol or supercritical ammonia water mode.
3. The preparation method of the high-strength high-resilience graphene aerogel according to claim 2, wherein the preparation method comprises the following steps: the freezing is directional freezing or non-directional freezing, the freezing temperature is-10 ℃ to the liquid nitrogen temperature, the drying time is 20-60h, and the drying vacuum degree is 0.1-50000 Pa.
4. The preparation method of the high-strength high-resilience graphene aerogel according to claim 1, wherein the preparation method comprises the following steps: in the step b, the reducing agent is one of L-ascorbic acid, saccharides, ammonia water, sodium citrate, sodium borohydride, hydroiodic acid, sodium bisulfate and ethylenediamine.
5. The preparation method of the high-strength high-resilience graphene aerogel according to claim 1, wherein the preparation method comprises the following steps: the mass ratio of the reducing agent to the graphene oxide in the step b is 1: 1-50: 1.
6. the preparation method of the high-strength high-resilience graphene aerogel according to claim 1, wherein the preparation method comprises the following steps: the temperature of the hydrothermal reaction in the step b is 85-180 ℃, and the time is 1.5-24 h.
7. The utility model provides a high-strength high resilience graphene aerogel which characterized in that: the graphene aerogel is an inorganic conductive aerogel with a three-dimensional network structure formed by mutually crosslinking two-dimensional graphene; the graphene aerogel has the pore diameter of 1 nm-200 mu m, the porosity of 75-95% and the density of 2-50mg/cm3Compressibility of 0-98%, conductivity of 1-4000S/m, specific surface area of 100-2The stress is 0-60 KPa.
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Cited By (6)
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| CN112758917A (en) * | 2021-01-12 | 2021-05-07 | 广州科技职业技术大学 | Preparation method of graphene aerogel with inner parts arranged in circular flow manner |
| CN112794705A (en) * | 2021-01-13 | 2021-05-14 | 兰州大学 | Method for preparing hyperelastic silicon oxide nano ceramic aerogel based on graphene serving as template |
| CN112852386A (en) * | 2021-01-25 | 2021-05-28 | 武汉科技大学 | High-orientation layered graphene aerogel phase-change composite material and preparation method thereof |
| CN112897515A (en) * | 2021-02-26 | 2021-06-04 | 广东墨睿科技有限公司 | Highly-ordered graphene aerogel and preparation method thereof |
| CN115010125A (en) * | 2022-07-27 | 2022-09-06 | 中国科学院兰州化学物理研究所 | Pure graphene aerogel and preparation method thereof |
| CN115874446A (en) * | 2022-12-30 | 2023-03-31 | 浙江凌龙智尚科技股份有限公司 | Finishing agent for cashmere and wool fiber fabrics and preparation method thereof |
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| CN112758917A (en) * | 2021-01-12 | 2021-05-07 | 广州科技职业技术大学 | Preparation method of graphene aerogel with inner parts arranged in circular flow manner |
| CN112794705A (en) * | 2021-01-13 | 2021-05-14 | 兰州大学 | Method for preparing hyperelastic silicon oxide nano ceramic aerogel based on graphene serving as template |
| CN112852386A (en) * | 2021-01-25 | 2021-05-28 | 武汉科技大学 | High-orientation layered graphene aerogel phase-change composite material and preparation method thereof |
| CN112897515A (en) * | 2021-02-26 | 2021-06-04 | 广东墨睿科技有限公司 | Highly-ordered graphene aerogel and preparation method thereof |
| CN115010125A (en) * | 2022-07-27 | 2022-09-06 | 中国科学院兰州化学物理研究所 | Pure graphene aerogel and preparation method thereof |
| CN115010125B (en) * | 2022-07-27 | 2024-04-12 | 中国科学院兰州化学物理研究所 | Pure graphene aerogel and preparation method thereof |
| CN115874446A (en) * | 2022-12-30 | 2023-03-31 | 浙江凌龙智尚科技股份有限公司 | Finishing agent for cashmere and wool fiber fabrics and preparation method thereof |
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Application publication date: 20201030 |