CN115341306A - Graphene aerogel fiber and preparation method thereof - Google Patents
Graphene aerogel fiber and preparation method thereof Download PDFInfo
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- CN115341306A CN115341306A CN202211161888.8A CN202211161888A CN115341306A CN 115341306 A CN115341306 A CN 115341306A CN 202211161888 A CN202211161888 A CN 202211161888A CN 115341306 A CN115341306 A CN 115341306A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The invention relates to a graphene aerogel fiber and a preparation method thereof. The preparation method specifically comprises the steps of obtaining a mixed solution of graphene oxide and polyvinyl alcohol by means of solution blending, concentrating the mixed solution into a spinning solution, discharging the spinning solution into an ethanol bath for freeze spinning, and performing freeze drying to obtain graphene oxide/polyvinyl alcohol aerogel fibers, wherein the graphene oxide/polyvinyl alcohol aerogel fibers are obtained by chemical reduction.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a graphene aerogel fiber and a preparation method thereof.
Background
Aerogel is a light porous material with a three-dimensional nano-network structure, high specific surface area, low density and high porosity, and is also a solid material with the lowest thermal conductivity coefficient reported at present. Therefore, the aerogel is used for high-efficiency heat insulation in the fields of manned space flight, aviation, fire protection, construction, chemical engineering and the like. Based on the demand of special clothes such as space suits, fire-fighting suits and the like for high-performance heat-insulating fabrics, researchers have developed related researches on aerogel fibers. In addition, the aerogel fiber has the characteristic of large external surface area, and has wide application prospects in the fields of quick adsorption, catalytic loading, energy storage and the like. The prior art discloses that GO solution is discharged into liquid nitrogen as spinning solution, liquid nitrogen is used as a cold source to form frozen Fibers, the frozen Fibers are freeze-dried by a freeze-drying machine to obtain GO Aerogel Fibers, and the GO is annealed in a tube furnace to reduce GO to obtain final rGO Aerogel Fibers (Xu, Z.; zhang, Y.; li, P.; gao, C., strong, decrease, lightweight, new Graphene Aerogel Fibers with Aligned pores. ACS Nano 2012,6 (8), 7103-7113).
The current preparation methods of aerogel fibers mainly comprise two types: the first method is that spinning solution is discharged into liquid nitrogen to form frozen fibers by taking simple liquid nitrogen as a cold source, and the frozen fibers are freeze-dried by a freeze-drying machine to remove water under the condition of keeping an in-fiber network structure to obtain aerogel fibers; and the other method needs a cooling device specially designed to achieve the purpose of freezing the fiber, and has the problems of complicated process and the like.
The present invention has been made in view of the above circumstances.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the graphene aerogel fiber and the preparation method thereof.
The first purpose of the invention is to provide a method for preparing graphene aerogel fibers in low-temperature liquid, which comprises the step of carrying out freeze spinning on graphene oxide spinning solution in an ethanol bath, wherein the ethanol bath is formed by mixing ethanol and liquid nitrogen.
Furthermore, the ethanol bath is prepared by mixing ethanol and liquid nitrogen according to a volume ratio of 1-5.
Furthermore, the temperature of the ethanol bath is-100 to-30 ℃.
The freezing point of the ethanol is-114 ℃, and the ethanol can be frozen after the freezing point is lower than-100 ℃, so the temperature of the ethanol bath is controlled to be-100 to-30 ℃.
Further, the method specifically comprises the following steps:
(1) Mixing the graphene oxide solution and the polyvinyl alcohol solution, stirring and concentrating to obtain a spinning solution;
(2) Discharging the spinning solution into an ethanol bath for freeze spinning to obtain frozen fibers, and freeze-drying the frozen fibers to obtain graphene oxide/polyvinyl alcohol aerogel fibers;
(3) And reducing the graphene oxide/polyvinyl alcohol aerogel fiber, washing with water, soaking with ethanol, and naturally drying to obtain the graphene aerogel fiber.
Further, in the step (1), the concentration of the graphene oxide in the graphene oxide solution is 4-6mg/ml, and the concentration of the polyvinyl alcohol in the polyvinyl alcohol solution is 18-22mg/ml.
Further, the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution in the step (1) is 7-11.
The graphene oxide should occupy a main body in the application, and the polyvinyl alcohol is excessively occupied, so that various properties, such as conductivity, of subsequent materials are affected. Too little polyvinyl alcohol will affect the viscosity of the spinning solution and thus the formation of gel fibers and the mechanical properties of subsequent fibers.
Further, in the step (1), stirring is carried out for 4-5 days, and concentration is carried out until the concentration of the graphene oxide is 23-27mg/ml.
Because the spinning solution is subjected to shear orientation by mechanical stirring, and the concentration of the spinning solution mainly depends on natural evaporation, the stirring period is long and needs 4-5 days; the graphene oxide concentration of 23-27mg/ml is mainly used for ensuring that the viscosity of the spinning solution is high enough to obtain the gel fiber.
Further, the discharge speed of the spinning solution in the step (2) is 50-100ml/h, the inner diameter of a spinning needle is 1050-1550 mu m, the temperature of freeze drying is-65 to-45 ℃, and the pressure is 4-12Pa.
The discharge speed is 50-100ml/h and the inner diameter of the spinning needle is 1050-1550 μm, so as to ensure the formation of the gel fiber, and the freeze drying condition parameter is the working parameter range of a freeze dryer.
And further, the step (3) is reduced to be that the graphene oxide/polyvinyl alcohol aerogel fibers are placed in 55-57% hydriodic acid by mass, reduced for 10-14h at 75-85 ℃, washed until the solution is colorless, soaked for 0.8-1.2h with absolute ethyl alcohol, and repeated for a plurality of times until the absolute ethyl alcohol is colorless.
Reducing for 10-14h at 75-85 ℃ to ensure that the graphene oxide is fully reduced, and washing with water and soaking with absolute ethyl alcohol to wash off iodine elementary substances remained on the fibers.
The graphene oxide solution can be prepared by an improved Hummers method, and can also be prepared by other methods.
The second purpose of the invention is to provide the graphene aerogel fiber prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
the graphene aerogel fiber is prepared by using low-temperature liquid prepared by ethanol under the non-liquid nitrogen ultralow-temperature condition, specifically, a mixed solution of graphene oxide and polyvinyl alcohol is obtained by means of solution blending, the mixed solution is concentrated into a spinning solution, the spinning solution is discharged into an ethanol bath for freeze spinning, and the graphene oxide/polyvinyl alcohol aerogel fiber is obtained by freeze drying and is obtained by chemical reduction.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic process flow diagram of the present invention for preparing graphene aerogel fibers in a cryogenic liquid;
FIG. 2 is a cross-sectional profile of graphene aerogel fibers prepared in comparative example 1 and examples 1-5 before reduction;
FIG. 3 is a cross-sectional profile of graphene aerogel fibers prepared in comparative example 1 and examples 1-5 after reduction;
FIG. 4 is a graph of tensile strength versus temperature for the graphene aerogel fibers prepared in comparative example 1 and examples 1-5;
FIG. 5 is a cross-sectional profile of the graphene aerogel fiber prepared in comparative example 2 before and after reduction;
fig. 6 is a stress-strain graph of the graphene aerogel fibers prepared in comparative example 2 and example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The method for preparing the graphene aerogel fibers in the low-temperature liquid in the embodiment specifically comprises the following steps:
(1) Mixing a graphene oxide solution with a polyvinyl alcohol solution, wherein the concentration of graphene oxide in the graphene oxide solution is 4mg/ml, the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 18mg/ml, the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution is 9;
(2) Discharging the spinning solution into an ethanol bath for freeze spinning, wherein the ethanol bath is formed by mixing ethanol and liquid nitrogen in a volume ratio of 1;
(3) And putting the graphene oxide/polyvinyl alcohol aerogel fiber into 55% hydriodic acid by mass, reducing for 12 hours at 80 ℃, washing with water until the solution is colorless, soaking for 1 hour with absolute ethyl alcohol, repeating for several times until the absolute ethyl alcohol is colorless, and naturally drying to obtain the graphene aerogel fiber.
Example 2
The method for preparing the graphene aerogel fibers in the low-temperature liquid in the embodiment specifically comprises the following steps:
(1) Mixing a graphene oxide solution with a polyvinyl alcohol solution, wherein the concentration of graphene oxide in the graphene oxide solution is 4mg/ml, the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 20mg/ml, the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution is 9;
(2) Discharging the spinning solution into an ethanol bath for freeze spinning, wherein the ethanol bath is formed by mixing ethanol and liquid nitrogen in a volume ratio of 11, the temperature of the ethanol bath is-80 ℃, the discharge speed of the spinning solution is 50ml/h, the inner diameter of a spinning needle is 1050 mu m, so as to obtain frozen fibers, and freeze-drying the frozen fibers in a freeze-drying machine at-65 ℃ under the pressure of 4Pa, so as to obtain graphene oxide/polyvinyl alcohol aerogel fibers;
(3) And putting the graphene oxide/polyvinyl alcohol aerogel fiber into 55% hydriodic acid by mass, reducing for 12 hours at 80 ℃, washing with water until the solution is colorless, soaking for 1 hour with absolute ethyl alcohol, repeating for several times until the absolute ethyl alcohol is colorless, and naturally drying to obtain the graphene aerogel fiber.
Example 3
The method for preparing the graphene aerogel fibers in the low-temperature liquid in the embodiment specifically comprises the following steps:
(1) Mixing a graphene oxide solution with a polyvinyl alcohol solution, wherein the concentration of graphene oxide in the graphene oxide solution is 4mg/ml, the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 22mg/ml, the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution is 9;
(2) Discharging the spinning solution into an ethanol bath for freeze spinning, wherein the ethanol bath is formed by mixing ethanol and liquid nitrogen in a volume ratio of 6;
(3) And putting the graphene oxide/polyvinyl alcohol aerogel fiber into 55% hydriodic acid by mass, reducing for 12 hours at 80 ℃, washing with water until the solution is colorless, soaking for 1 hour with absolute ethyl alcohol, repeating for several times until the absolute ethyl alcohol is colorless, and naturally drying to obtain the graphene aerogel fiber.
Example 4
The method for preparing the graphene aerogel fiber in the low-temperature liquid in the embodiment specifically comprises the following steps:
(1) Mixing a graphene oxide solution with a polyvinyl alcohol solution, wherein the concentration of graphene oxide in the graphene oxide solution is 4mg/ml, the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 20mg/ml, the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution is 9;
(2) Discharging the spinning solution into an ethanol bath for freeze spinning, wherein the ethanol bath is formed by mixing ethanol and liquid nitrogen in a volume ratio of 2;
(3) And putting the graphene oxide/polyvinyl alcohol aerogel fiber into 55% hydriodic acid by mass, reducing for 12 hours at 80 ℃, washing with water until the solution is colorless, soaking for 1 hour with absolute ethyl alcohol, repeating for several times until the absolute ethyl alcohol is colorless, and naturally drying to obtain the graphene aerogel fiber.
Example 5
The method for preparing the graphene aerogel fiber in the low-temperature liquid in the embodiment specifically comprises the following steps:
(1) Mixing a graphene oxide solution with a polyvinyl alcohol solution, wherein the concentration of graphene oxide in the graphene oxide solution is 4mg/ml, the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 19mg/ml, the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution is 9;
(2) Discharging the spinning solution into an ethanol bath for freeze spinning, wherein the ethanol bath is formed by mixing ethanol and liquid nitrogen in a volume ratio of 5;
(3) And putting the graphene oxide/polyvinyl alcohol aerogel fiber into 55% hydriodic acid by mass, reducing for 12 hours at 80 ℃, washing with water until the solution is colorless, soaking for 1 hour with absolute ethyl alcohol, repeating for several times until the absolute ethyl alcohol is colorless, and naturally drying to obtain the graphene aerogel fiber.
Comparative example 1
The preparation method of the graphene aerogel fiber of the present comparative example was the same as that of example 2, except that the ethanol bath in step (2) was replaced with liquid nitrogen at a temperature of-196 ℃.
Comparative example 2
The preparation method of the graphene aerogel fiber of the comparative example is the same as that of example 3, except that the spinning solution in the step (1) is a pure GO solution instead of a mixed solution of graphene oxide and polyvinyl alcohol.
Test example 1
The graphene aerogel fibers prepared in examples 1 to 5 were tested for pore size and tensile strength as shown in table 1.
TABLE 1
It can be seen from table 1 that as the volume ratio of ethanol to liquid nitrogen increases, the temperature of the ethanol bath increases from-100 ℃ to-30 ℃ and the pore size increases from 1.65 μm to 8.25 μm, mainly due to the effect of the freezing rate on ice crystal nucleation and growth, and as the temperature of the ethanol bath gradually decreases, the freezing rate increases, resulting in more ice crystal nucleation and thus more and smaller pores. The final fiber tensile strength increased from 0.38Mpa to 0.90Mpa and then decreased to 0.29Mpa, demonstrating that the ordered porous structure can improve the mechanical properties of the fiber.
Test example 2
The cross-sectional topography of the graphene aerogel fibers prepared in comparative example 1 and examples 1 to 5 before and after reduction are respectively shown in fig. 2 and fig. 3, a-f in fig. 2 are respectively the cross-sectional topography of the graphene oxide/polyvinyl alcohol aerogel fibers before reduction in comparative example 1 and examples 1 to 5, and a-f in fig. 3 are respectively the cross-sectional topography of the graphene oxide/polyvinyl alcohol aerogel fibers after reduction in comparative example 1 and examples 1 to 5.
As can be seen from FIGS. 2 and 3, as the gelled fibers gradually enter the low temperature ethanol bath, the water within the fibers first nucleates by crystallization near the fiber surface, then grows in the radial direction to form ordered ice crystals, while the GO/PVA solute is repelled by and compressed by the ice crystals, which are subsequently removed by freeze-drying, resulting in an ordered porous structure with a central outward divergence, and the pore structure after reduction is largely retained with only a slight contraction, with little difference in the morphology of the fibers obtained by freezing in the liquid nitrogen and ethanol baths.
Test example 3
Testing the tensile strength-temperature curves of the graphene aerogel fibers prepared in comparative example 1 and examples 1-5 are shown in fig. 4.
As shown in FIG. 4, as the temperature of the freezing medium was changed from liquid nitrogen to a low temperature ethanol bath and an ethanol bath was gradually increased, the tensile strength of the prepared fiber was increased from 0.36MPa to 0.90MPa and then decreased to 0.29MPa, from which it was concluded that the tensile strength of the prepared fiber was at most 0.90MPa when the temperature of the ethanol bath was-65 ℃.
Test example 4
The cross-sectional topography and stress-strain curves of the graphene aerogel fiber prepared in comparative example 2 before and after reduction are respectively shown in fig. 5 and 6, a and b in fig. 5 are respectively the cross-sectional topography of the graphene oxide aerogel fiber prepared in comparative example 2 before and after reduction, and fig. 6 is the stress-strain curve of the graphene aerogel fiber prepared in comparative example 2 and example 3.
As shown in fig. 5, the cross-sectional morphology before and after the pure GO aerogel fiber is reduced does not change much compared with GO/PVA aerogel fibers, but it can be seen from observation of fig. 6 that the tensile strength of the pure GO aerogel fiber after reduction is only less than 0.2MPa, and is reduced by several times compared with the tensile strength of the GO/PVA aerogel fiber after reduction, from which it is concluded that the addition of PVA contributes to the improvement of the mechanical properties of the fiber.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. The method for preparing the graphene aerogel fiber in the low-temperature liquid is characterized by comprising the step of carrying out freeze spinning on graphene oxide spinning solution in an ethanol bath, wherein the ethanol bath is formed by mixing ethanol and liquid nitrogen.
2. The method for preparing the graphene aerogel fibers in the cryogenic liquid according to claim 1, wherein the ethanol bath is prepared by mixing ethanol and liquid nitrogen according to a volume ratio of 1.
3. The method for preparing graphene aerogel fibers in a cryogenic liquid according to claim 2, wherein the temperature of the ethanol bath is-100 to-30 ℃.
4. The method for preparing graphene aerogel fibers in a cryogenic liquid according to any of claims 1 to 3, characterized in that the method specifically comprises the following steps:
(1) Mixing the graphene oxide solution and the polyvinyl alcohol solution, stirring and concentrating to obtain a spinning solution;
(2) Discharging the spinning solution into an ethanol bath for freeze spinning to obtain frozen fibers, and freeze-drying the frozen fibers to obtain graphene oxide/polyvinyl alcohol aerogel fibers;
(3) And reducing the graphene oxide/polyvinyl alcohol aerogel fiber, washing with water, soaking with ethanol, and naturally drying to obtain the graphene aerogel fiber.
5. The method for preparing the graphene aerogel fibers in the cryogenic liquid according to claim 4, wherein the concentration of graphene oxide in the graphene oxide solution in the step (1) is 4-6mg/ml, and the concentration of polyvinyl alcohol in the polyvinyl alcohol solution is 18-22mg/ml.
6. The method for preparing the graphene aerogel fiber in the cryogenic liquid according to claim 4 or 5, wherein the mass ratio of the graphene oxide solution to the polyvinyl alcohol solution in the step (1) is 7-11.
7. The method for preparing graphene aerogel fibers in a cryogenic liquid according to claim 4, wherein the graphene oxide aerogel fibers are concentrated to a graphene oxide concentration of 23-27mg/ml in step (1) after being stirred for 4-5 days.
8. The method for preparing graphene aerogel fiber in cryogenic liquid according to claim 4, wherein the discharge speed of the spinning solution in the step (2) is 50-100ml/h, the inner diameter of the spinning needle is 1050-1550 μm, the temperature of freeze drying is-65-45 ℃, and the pressure is 4-12Pa.
9. The method for preparing graphene aerogel fibers in a cryogenic liquid according to claim 4, wherein in the step (3), the graphene oxide/polyvinyl alcohol aerogel fibers are put into 55-57% by mass of hydroiodic acid, reduced at 75-85 ℃ for 10-14h, washed with water until the solution is colorless, soaked in absolute ethyl alcohol for 0.8-1.2h, and repeated for several times until the absolute ethyl alcohol is colorless.
10. A graphene aerogel fiber prepared by the method of any of claims 1-9.
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