CN111074380B - Graphene oxide/sodium polyacrylate stretching fluid and application thereof in preparation of graphene - Google Patents
Graphene oxide/sodium polyacrylate stretching fluid and application thereof in preparation of graphene Download PDFInfo
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- CN111074380B CN111074380B CN201911418115.1A CN201911418115A CN111074380B CN 111074380 B CN111074380 B CN 111074380B CN 201911418115 A CN201911418115 A CN 201911418115A CN 111074380 B CN111074380 B CN 111074380B
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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
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Abstract
The invention discloses a graphene oxide/sodium polyacrylate stretching fluid which is prepared by the following method: preparing a sodium polyacrylate aqueous solution with the concentration of more than 0.1 wt% and a graphene oxide aqueous solution with the concentration of more than 0.1 wt%, and uniformly mixing the sodium polyacrylate aqueous solution and the graphene oxide aqueous solution according to the mass ratio of more than 1:3 to obtain the graphene oxide/sodium polyacrylate stretching fluid. The invention discloses a method for adding a small amount of sodium polyacrylate solution into a graphene oxide aqueous solution to enable the graphene oxide aqueous solution to have ultrahigh tensile property, which is simple in process, environment-friendly and efficient, is a novel method for improving the processability of the graphene oxide solution, and can be applied to the field of preparation of graphene.
Description
Technical Field
The invention belongs to the field of nano materials, and particularly relates to a graphene oxide/sodium polyacrylate stretching fluid and application thereof in preparation of graphene.
Technical Field
In 2004, professor a.k.geom, university of manchester, uk, successfully prepared graphene by using a mechanical exfoliation method and hung on a miniature gold frame, and the conclusion that a perfect two-dimensional crystal structure cannot stably exist at a non-absolute zero degree is overcome. In other words, the graphene in a free state can exist stably at room temperature; under the same conditions, any other known material is oxidized or decomposed and becomes unstable even at a thickness 10 times its monolayer thickness. Structurally, Graphene (Graphene) is an sp2 hybridized monolayer carbon atom crystal which is tightly packed into a two-dimensional honeycomb lattice structure, carbon atoms in the layer are connected in a covalent bond mode and have ultrahigh strength (120GPa), so that the carbon-based material with a specific structure is constructed by taking the Graphene as a source material, and the design, controllability and macroscopic preparation of the carbon-based functional material nanostructure are gradually attracted by global scientists.
The graphene oxide fiber has the characteristics of high strength, high modulus, high electric conductivity, high heat conductivity, multiple functions and the like, and has attracted wide attention of scholars at home and abroad. Graphene is a typical two-dimensional polymer, and in a dispersion system, due to the fact that the distance between sheet layers is large and chain entanglement similar to linear polymers is avoided, the graphene mainly shows viscosity, gel fibers are extremely poor in stretchability and are extremely easy to break when being stressed, so that the spinning speed is extremely low, only wet spinning can be performed generally, and the speed is not more than 5 m/min. Graphene fibers have been widely researched and focused since the continuous wet spinning process thereof has been reported due to excellent mechanical properties, thermal conductivity and electrical conductivity, but cannot be applied on a large scale all the time due to the limitation of the spinning speed thereof.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a graphene oxide/sodium polyacrylate stretching fluid and application thereof in preparation of graphene.
The purpose of the invention is realized by the following technical scheme: a graphene oxide/sodium polyacrylate drawing fluid prepared by the following method: preparing a sodium polyacrylate aqueous solution with the concentration of more than 0.2wt% and a graphene oxide aqueous solution with the concentration of more than 0.2wt%, and uniformly mixing the graphene oxide aqueous solution and the sodium polyacrylate aqueous solution according to the mass ratio of more than 3 times to obtain the graphene oxide/sodium polyacrylate stretching fluid. Wherein the weight average molecular weight of the sodium polyacrylate is 3000 ten thousand.
The invention also provides application of the stretching fluid in preparation of graphene.
And further, carrying out air flow auxiliary spinning by taking the stretching fluid of the graphene oxide/sodium polyacrylate as a precursor, and directly drying to obtain the graphene oxide/sodium polyacrylate non-woven fabric.
Further, airflow-assisted spinning is carried out by taking a stretching fluid of graphene oxide/sodium polyacrylate as a precursor, and the graphene oxide/sodium polyacrylate composite fiber is collected by using a coagulating bath.
Further, the coagulation bath is selected from poor solvents of graphene oxide and sodium polyacrylate.
Further, the coagulation bath is preferably ethanol, isopropanol, ethyl acetate and aqueous solutions thereof.
Further, the method also comprises the step of filtering the collected graphene oxide/sodium polyacrylate composite fibers to prepare the non-woven fabric.
Further, the fiber forming linear velocity of the air flow assisted spinning was 350 m/min.
Further, the method comprises the steps of reducing the graphene oxide/sodium polyacrylate composite fiber or non-woven fabric in a mixed solution of hydriodic acid and acetic acid for 12 hours at the reduction temperature of 95 ℃, cleaning the composite fiber by using 3vt% ammonia water, and carrying out heat treatment at 3000 ℃ for 1 hour. Wherein, the hydriodic acid and the acetic acid are mixed according to the volume ratio of 1: 1.
Compared with the prior art, the invention has the following beneficial effects: the viscoelasticity of the graphene oxide aqueous solution is effectively changed by adding a proper amount of sodium polyacrylate solution, so that the graphene oxide aqueous solution has viscoelasticity similar to polymerization, and therefore, the graphene oxide aqueous solution can show ultrahigh tensile property (the tensile ratio is more than 8 times), the fiber diameter can be reduced to a great extent, the relaxation is weakened, the fiber orientation degree is increased, and the mechanical property, the thermal conductivity, the electric conductivity and the like of the finally obtained fiber material or the derivative material thereof are improved. Because the graphene oxide/sodium polyacrylate stretching fluid has the ultrahigh stretching performance similar to a polymer, the graphene oxide/sodium polyacrylate composite fiber non-woven fabric can be processed by using airflow auxiliary spinning, and the fiber is collected by using a substrate, so that the graphene oxide/sodium polyacrylate composite fiber non-woven fabric can be quickly prepared. And reducing the graphene oxide/sodium polyacrylate composite fiber, and washing away the water-soluble sodium polyacrylate to obtain the pure graphene fiber non-woven fabric which can be applied to gas adsorption, filter membranes, capacitors, battery electrodes, gas diffusion layers of fuel cells and the like. And (3) carrying out solvent replacement on the obtained gel fiber bundle, replacing water in the fiber with n-hexane, and drying to obtain the porous aerogel fiber. The porous aerogel fiber can be applied to gas adsorption, electrodes, catalyst carriers, and the like.
Drawings
Figure 1 comparison of tensile properties of aqueous graphene oxide solutions and graphene oxide/sodium polyacrylate drawing fluids: (a) the tensile property of the graphene oxide aqueous solution, (b) the tensile property of the graphene oxide/sodium polyacrylate tensile fluid;
FIG. 2 is a drawing fluid of graphene oxide/sodium polyacrylate with a different drawing ratio corresponding to the mass ratio of graphene oxide to sodium polyacrylate;
in fig. 3, the mass ratio of graphene oxide to sodium polyacrylate in the mixed solution is controlled to be 7:3, changing the stretching ratio of the stretching fluid obtained by changing the concentration of the graphene oxide;
FIG. 4 scanning electron microscope picture of gel fiber cross section;
FIG. 5 is a photograph of a nonwoven fabric obtained by directly drying and collecting blown fibers with a hot air flow;
FIG. 6 is a photograph of a gel fiber bundle collected by coagulation with isopropyl alcohol;
FIG. 7 is a schematic view of a nonwoven fabric obtained by filtering collected fiber bundles;
FIG. 8 is an electron scanning microscope photograph of a nonwoven fabric.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Example 1
(1) Preparing a graphene oxide aqueous solution with the concentration of 1.0 wt% and a sodium polyacrylate aqueous solution with the concentration of 2.0 wt%.
(2) And uniformly mixing the graphene oxide aqueous solution and the sodium polyacrylate aqueous solution according to the mass ratio of 7:3 to obtain the graphene oxide/sodium polyacrylate ultrahigh-tensile solution. Wherein the weight average molecular weight of the adopted sodium polyacrylate is 3000 ten thousand.
As shown in fig. 1, in order to compare the tensile properties of the aqueous graphene oxide solution and the aqueous graphene oxide/sodium polyacrylate drawing fluid, fig. 1(a) is a drawing property test performed only with the aqueous graphene oxide solution having a concentration of 1.0 wt%, and it can be seen that the tensile property is only 1 time, while fig. 1(b) is a drawing fluid prepared by the above method, and the tensile property is 8 times.
Example 2
(1) Preparing a graphene oxide aqueous solution with the concentration of 2.0 wt% and a sodium polyacrylate aqueous solution with the concentration of 2.0 wt%;
(2) respectively mixing the sodium polyacrylate aqueous solution and the graphene oxide aqueous solution according to the mass ratio of 10:0, 9.5:0.5, 9:1, 8.5:1.5, 8:2, 7.5:2.5, 7:3 and 6.5: 3.5, 6:4, 5:5 and 0: 1' are uniformly mixed, the concentration of the graphene oxide in the mixed solution is adjusted to 12mg/g, and the graphene oxide/sodium polyacrylate stretching fluid is obtained and adjusted to the concentration. Wherein the weight average molecular weight of the adopted sodium polyacrylate is 3000 ten thousand.
Fig. 2 is a drawing ratio corresponding to a change in the mass ratio of graphene oxide to sodium polyacrylate in the mixed solution, and it can be seen from the drawing that when the content of sodium polyacrylate exceeds 25%, the drawing performance of the mixed solution is significantly improved, and is improved with the increase of the content of sodium polyacrylate. When the solid contents are all 1.2 wt%, the loss factor of the sodium polyacrylate aqueous solution is about 0.42, and the loss factor of the graphene oxide aqueous solution is only 0.12, which shows that the sodium polyacrylate is closer to a viscoelastic fluid (the loss factor is equal to 1) and has excellent tensile property, and the graphene oxide aqueous solution is closer to an elastic solid, so the tensile ratio is small. The sodium polyacrylate can be added into the cured graphene aqueous solution to improve the loss factor of the graphene aqueous solution, so that the graphene oxide aqueous solution is endowed with an ultrahigh tensile ratio, the processing performance can be greatly improved, and the sodium polyacrylate can be used for quickly and efficiently preparing graphene materials by airflow-assisted spinning and the like.
Example 3
(1) Preparing a 2.0 wt% aqueous solution of sodium polyacrylate and a 2.0 wt% aqueous solution of graphene oxide, and adjusting the concentration of graphene oxide in the mixed solution to 0.2wt%, 0.4 wt%, 0.6 wt%, 0.8 wt%, 1.0 wt%, 1.2 wt%, 1.4 w%, 1.6 wt% and 1.8 wt% at a time.
(2) And uniformly mixing the sodium polyacrylate aqueous solution and the graphene oxide aqueous solution according to the mass ratio of 3:7 respectively to obtain the graphene oxide/sodium polyacrylate stretching fluid. Wherein the weight average molecular weight of the adopted sodium polyacrylate is 3000 ten thousand.
Fig. 3 shows the draw ratio corresponding to the drawing fluid with the changed graphene oxide concentration, and it can be seen from the graph that the draw ratio increases first and then decreases as the content of graphene oxide in the mixed solution increases. The graphene oxide concentration is too low, so that the distance between internal molecules is larger, the polymer chain entanglement is less, the intermolecular interaction is weaker, the fluid is more prone to be generated, and the loss factor is larger. However, if the concentration is too large, the intermolecular interaction is too strong, and the loss factor is small similarly to a solid, so that the tensile properties are deteriorated.
Example 4
(1) Preparing a graphene oxide aqueous solution with the concentration of 0.2wt% and a sodium polyacrylate aqueous solution with the concentration of 0.2 wt%.
(2) And uniformly mixing the graphene oxide aqueous solution and the sodium polyacrylate aqueous solution according to the mass ratio of 3:1 to obtain the graphene oxide/sodium polyacrylate ultrahigh-tensile solution. Wherein the weight average molecular weight of the adopted sodium polyacrylate is 3000 ten thousand.
The stretching fluid also had good stretching properties, with a stretch of 6.8 times.
Example 5
The stretched fluid obtained in example 1 was placed in a defoaming machine to be defoamed for 10min, and then air-assisted spinning was performed, wherein the fiber forming linear velocity of the air-assisted spinning was 350 m/min, the flow velocity ratio of the coaxial needle outer flow channel to the inner flow channel was 12, and the graphene oxide/sodium polyacrylate nonwoven fabric was obtained by directly drying the fiber bundle, as shown in fig. 5.
And reducing the graphene oxide/sodium polyacrylate non-woven fabric in a hydriodic acid/acetic acid mixed solution for 12 hours at the reduction temperature of 95 ℃, cleaning the composite fiber by using 3vt% ammonia water, and performing heat treatment at 3000 ℃ for 1 hour to obtain the graphene non-woven fabric. Wherein, the hydriodic acid and the acetic acid are mixed according to the volume ratio of 1: 1.
The nonwoven fabric can be used for sensors, Gas Diffusion Layers (GDLs) for fuel cells, battery electrodes, catalyst carriers, capacitor electrodes, and the like.
Example 6
Placing the stretching fluid in the embodiment 4 into a defoaming machine to perform defoaming treatment for 10min, and then performing air-assisted spinning, wherein the linear velocity of the air-assisted spinning is 350 m/min, the flow velocity ratio of the coaxial needle outer flow channel to the inner flow channel is 12, collecting graphene oxide/sodium polyacrylate composite fibers by using an isopropanol solidification bath, and as shown in fig. 6, collecting a gel fiber bundle photo by using isopropanol solidification, performing solvent replacement on the obtained composite fibers, replacing the isopropanol in the fibers with n-hexane, and filtering and drying to obtain the porous fiber aerogel material. FIG. 4 is a scanning electron micrograph of a cross section of the gel fiber, and it can be seen that the inside thereof is hollow.
The nonwoven fabric can be used for sensors, Gas Diffusion Layers (GDLs) for fuel cells, battery electrodes, catalyst carriers, capacitor electrodes, and the like.
Example 7
Placing the stretching fluid in the embodiment 1 or 3 into a defoaming machine to perform defoaming treatment for 10min, and then performing air-flow assisted spinning, wherein the linear velocity of the air-flow assisted spinning is 350 m/min, the flow velocity ratio of the coaxial needle outer flow channel to the coaxial needle inner flow channel is 12, collecting graphene oxide/sodium polyacrylate composite fibers by using an isopropanol coagulating bath, and filtering to obtain a non-woven fabric material, fig. 7 is a non-woven fabric object diagram obtained by filtering the collected fiber bundles, and fig. 8 is an electron scanning microscope photograph of the non-woven fabric, wherein the non-woven fabric is tightly lapped and has a uniform structure.
Or reducing the non-woven fabric in a hydriodic acid/acetic acid mixed solution for 1 hour at the reduction temperature of 95 ℃, cleaning the composite fiber by using 3vt% ammonia water, and performing heat treatment at 3000 ℃ for 1 hour to obtain the graphene non-woven fabric. Wherein, the hydriodic acid and the acetic acid are mixed according to the volume ratio of 1: 1.
The nonwoven fabric can be used for sensors, Gas Diffusion Layers (GDLs) for fuel cells, battery electrodes, catalyst carriers, capacitor electrodes, and the like.
Claims (9)
1. A graphene oxide/sodium polyacrylate drawing fluid, which is prepared by the following method: preparing a sodium polyacrylate aqueous solution with the concentration of more than 0.2wt% and a graphene oxide aqueous solution with the concentration of more than 0.2wt%, and uniformly mixing the graphene oxide aqueous solution and the sodium polyacrylate aqueous solution according to the mass ratio of more than 3 times to obtain a graphene oxide/sodium polyacrylate stretching fluid; wherein the weight average molecular weight of the sodium polyacrylate is 3000 ten thousand.
2. Use of the drawing fluid of claim 1 for the preparation of graphene fiber-based materials.
3. The application of the graphene oxide/sodium polyacrylate non-woven fabric as claimed in claim 2, wherein the graphene oxide/sodium polyacrylate non-woven fabric is obtained by performing gas flow assisted spinning by using a stretched fluid of graphene oxide/sodium polyacrylate as a precursor and directly drying.
4. The application of the graphene oxide/sodium polyacrylate composite fiber as the core material in the spinning process is characterized in that the graphene oxide/sodium polyacrylate composite fiber is collected by a coagulating bath through gas flow assisted spinning by taking graphene oxide/sodium polyacrylate stretching fluid as a precursor.
5. Use according to claim 4, wherein the coagulation bath is selected from the group consisting of graphene oxide and sodium polyacrylate poor solvents.
6. Use according to claim 5, wherein the coagulation bath is preferably ethanol, isopropanol, ethyl acetate and aqueous solutions thereof.
7. The application of claim 4, further comprising a step of filtering the collected graphene oxide/sodium polyacrylate composite fibers to form a non-woven fabric.
8. Use according to claim 3 or 4, wherein the gas-assisted spinning has a fiber forming linear velocity of 350 m/min.
9. The use according to claim 3, 4 or 7, further comprising the steps of reducing the graphene oxide/sodium polyacrylate composite fiber or non-woven fabric in a mixed solution of hydroiodic acid and acetic acid for 12 hours at a reduction temperature of 95 ℃, washing the composite fiber with 3vt% ammonia water, and then performing heat treatment at 3000 ℃ for 1 hour; wherein, the hydriodic acid and the acetic acid are mixed according to the volume ratio of 1: 1.
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| CN112456476B (en) * | 2020-12-02 | 2022-09-30 | 浙江大学 | Method for rapidly preparing graphene fiber aerogel |
| CN112680957A (en) * | 2020-12-15 | 2021-04-20 | 浙江大学 | Reinforcing method of graphene fiber non-woven fabric and continuous preparation method of high-performance graphene non-woven fabric |
| CN115341301A (en) * | 2022-08-26 | 2022-11-15 | 兰州大学 | Sodium alginate/sodium polyacrylate/graphene oxide composite fiber and preparation method and application thereof |
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