CN110028743B - Recyclable nano carbon composite material and preparation method and application thereof - Google Patents
Recyclable nano carbon composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a recyclable nano carbon composite material and a preparation method and application thereof. The nanocarbon composite material comprises: a two-dimensional or three-dimensional aggregation structure formed by densely interweaving a plurality of carbon nano tubes; two-dimensional graphene-like polymers and high molecular polymers distributed in the two-dimensional or three-dimensional aggregation structure. The nano-carbon composite material provided by the invention has the advantages of cyclic reutilization and the like, particularly the multifunctional composite paper disclosed by the invention not only can be self-repaired and recycled, but also has the advantages of good mechanical strength, flexibility, bending resistance and the like, and the nano-carbon composite material provided by the invention is simple in preparation process, easy in raw material obtaining, free of harmful waste gas, waste liquid and the like, green, environment-friendly and easy for large-scale production.
Description
Technical Field
The invention relates to a nano carbon composite material, in particular to a recyclable nano carbon composite material (such as multifunctional composite paper) and a preparation method and application thereof.
Background
At the present stage, the high-electric-conductivity and heat-conduction Baji paper is obtained mainly by a vacuum filtration method, a chemical vapor deposition growth method and other methods. Compared with common paper, the bucky paper with special performance due to the existence of the carbon nano-tubes has potential application value in many fields such as energy Sources, sensing and the like, but the popularization and the application of the bucky paper in the actual industrial production are limited due to the defects of brittleness, mechanical strength, unrecyclability and the like of the bucky paper (see Journal of Power Sources 2013,237,325 and 331; J.Phys.chem.C 2012,116,3903-3909.Electrochemistry Communications 2009,11,186 and 189).
Disclosure of Invention
The invention mainly aims to provide a repairable and recyclable nano carbon composite material as well as a preparation method and application thereof, thereby overcoming the defects in the prior art.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a recyclable nano carbon composite material, which comprises the following components:
a two-dimensional or three-dimensional aggregation structure formed by densely interweaving a plurality of carbon nano tubes;
two-dimensional graphene-like polymers and high molecular polymers distributed in the two-dimensional or three-dimensional aggregation structure.
The embodiment of the invention also provides a preparation method of the recyclable nano carbon composite material, which comprises the following steps:
providing a mixed solution containing uniformly dispersed carbon nanotubes, a two-dimensional graphene-like polymer and a high molecular polymer;
and separating the solvent in the mixed solution to form the nano carbon composite material.
Further, the preparation method may comprise:
uniformly dispersing carbon nanotubes in a two-dimensional graphene-like polymer solution to form a uniform dispersion liquid;
and dissolving a high molecular polymer into the uniform dispersion liquid to form the mixed liquid.
Further, the preparation method may comprise: and treating the mixed solution in a filtering mode to form the nano carbon composite material.
Further, the preparation method may include: and removing the solvent in the mixed solution by natural evaporation to form the nanocarbon composite material.
Further, the solvent in the mixed solution includes water.
Further, the two-dimensional graphene-like polymer includes a sulfonated graphene-like polymer, a carboxylated graphene-like polymer, and the like.
Further, the polymer is selected from water-soluble polymers, such as polyvinyl alcohol, polyethylene glycol, or aqueous polyurethane, without being limited thereto.
Further, in the nanocarbon composite material, the mass ratio of the two-dimensional graphene-like polymer to the carbon nanotubes is preferably (3-8) to (2-7).
The embodiment of the invention also provides a recyclable nano carbon composite material prepared by any one of the methods.
Further, the nano carbon composite material is flexible bending-resistant multifunctional composite paper. Further, the maximum tensile strength of the multifunctional composite bucky paper is above 100 MPa.
The embodiment of the invention also provides a method for repairing any one of the multifunctional composite bucky papers, which comprises the following steps: and applying force to the gap of the multifunctional composite bucky paper to ensure that the corresponding broken ends are kept spliced, and applying a specified solvent to the spliced position, thereby realizing the self-repairing of the composite bucky paper.
Further, the solvent includes water.
The embodiment of the invention also provides a crease eliminating method of any one of the multifunctional composite bucky papers, which comprises the following steps: applying a specified solvent to the multi-functional composite bucky paper at the crease and applying a force at least at the crease that tends to flatten the multi-functional composite bucky paper, thereby removing the crease.
Further, the solvent includes water.
The embodiment of the invention also provides a recycling method of any one of the nano carbon composite materials, which comprises the following steps:
immersing the used nano carbon composite material into a specified solvent to disintegrate the nano carbon composite material to form a mixed solution; and separating the specified solvent in the mixed solution to reform the nano carbon composite material.
Further, the specified solvent comprises water.
Further, the recycling method may further include: and treating the mixed solution in a filtering mode to form the nano carbon composite material. The nanocarbon composite material may be multifunctional composite bucky paper or the like.
Further, the recycling method may further include: and removing the specified solvent in the mixed solution by natural evaporation to form the nanocarbon composite material.
Compared with the prior art, the nano-carbon composite material provided by the invention has the advantages of cyclic reutilization and the like, particularly, the multifunctional composite paper disclosed by the invention not only can be self-repaired and cyclically recycled, but also has the advantages of good mechanical strength, flexibility, bending resistance and the like, and the nano-carbon composite material provided by the invention is simple in preparation process, easy in obtaining of raw materials, free of harmful waste gas, waste liquid and the like, green, environment-friendly and easy for large-scale production.
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 description of the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and it is also possible for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is a flow diagram of a process for making a recyclable multifunctional composite bucky paper in accordance with an exemplary embodiment of the present invention;
FIG. 2 is a schematic diagram of a process for making a recyclable multifunctional composite bucky paper in accordance with an exemplary embodiment of the present invention;
fig. 3 is a photograph of a multifunctional composite bucky paper in accordance with an embodiment of the present invention.
Fig. 4 a-4 b are mechanical property test results of the multifunctional composite paper formed by using different raw material ratios according to an embodiment of the invention.
Fig. 5 is a diagram illustrating the repair of creases and cuts in a multifunctional composite bucky paper in accordance with an embodiment of the present invention.
Fig. 6 is a graph comparing the mechanical properties of the multifunctional composite bucky paper of fig. 5 before the cuts are made and after the cuts have been self-repaired.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention provides a recyclable nano carbon composite material, which comprises the following components:
a two-dimensional or three-dimensional aggregation structure formed by densely interweaving a plurality of carbon nano tubes;
two-dimensional graphene-like polymers and high molecular polymers distributed in the two-dimensional or three-dimensional aggregation structure.
Further, the two-dimensional graphene-like polymer includes a super-hydrophilic graphene-like polymer, such as a sulfonated graphene-like polymer, a carboxylated graphene-like polymer, and the like. The two-dimensional graphene-based polymer contributes to better dispersion of the carbon nanotubes. Further, the high molecular polymer may be selected from water-soluble high molecular polymers, such as polyvinyl alcohol, polyethylene glycol, or aqueous polyurethane, and the like, without being limited thereto. The hydrophilic group contained in the water-soluble high polymer, such as a hydroxyl group contained in polyvinyl alcohol, can form strong bonding force with a sulfonic group or a carboxylic group contained in the two-dimensional graphene polymer, and then the hydrophilic group can cooperate with the two-dimensional graphene polymer to remarkably improve the mechanical property of the nanocarbon composite material.
Furthermore, the mass ratio of the two-dimensional graphene-like polymer to the carbon nano tube is preferably (3-8): 2-7.
The preparation method of the recyclable nano carbon composite material provided by the embodiment of the invention comprises the following steps:
providing a mixed solution containing uniformly dispersed carbon nanotubes, a two-dimensional graphene-like polymer and a high molecular polymer;
and separating the solvent in the mixed solution to form the nano carbon composite material.
In some embodiments, the preparation method may specifically comprise:
uniformly dispersing carbon nanotubes in a two-dimensional graphene polymer solution to form a uniform dispersion liquid;
and dissolving a high molecular polymer into the uniform dispersion liquid to form the mixed liquid.
Further, the preparation method can further comprise the following steps: mixing the solution of sulfonated graphene polymer or carboxylated graphene polymer with carbon nanotube powder, and then carrying out ultrasonic treatment on the formed mixed solution to uniformly disperse the carbon nanotubes with the aid of the sulfonated graphene polymer or the carboxylated graphene polymer, thereby forming the uniform dispersion liquid. In some embodiments, the preparation method may specifically comprise: and treating the mixed solution in a filtering mode to form the nano carbon composite material. The filtration may be performed by a method known in the art, such as vacuum filtration. The nanocarbon composite material may be multifunctional composite bucky paper or the like.
In some embodiments, the preparation method specifically may comprise: and removing the solvent in the mixed solution by natural evaporation to form the nanocarbon composite material.
Further, the solvent in the mixed solution includes water.
Further, the two-dimensional graphene-like polymer includes a sulfonated graphene-like polymer or a carboxylated graphene-like polymer. Further, the high molecular polymer may be selected from water-soluble high molecular polymers, such as polyvinyl alcohol, polyethylene glycol, or aqueous polyurethane, and the like, without being limited thereto.
The amount of the high molecular polymer used may be arbitrary.
Furthermore, the mass ratio of the two-dimensional graphene-like polymer to the carbon nano tube in the mixed solution is (3-8) to (2-7).
Furthermore, the mass ratio of the two-dimensional graphene-like polymer to the carbon nanotube high molecular polymer can be selected from the group consisting of:
8/2/5,8/2/10,8/2/15,8/2/20,7/3/5,7/3/10,7/3/15,7/3/20,6/4/5,6/4//10,6/4//15,6/4//20, 5/5/5,5/5/10,5/5/15,5/5/20, 4/6/5,4/6/10,4/6/15,4/6/20, 3/7/5,3/7/10,3/7/15,3/7/20, but is not limited thereto.
The embodiment of the invention also provides a recyclable nano carbon composite material prepared by any one of the methods.
Furthermore, the recyclable nano carbon composite material is flexible bending-resistant multifunctional composite bucky paper, and the maximum tensile strength of the flexible bending-resistant multifunctional composite bucky paper is more than 100 MPa.
The embodiment of the invention also provides a mixed solution for preparing the recyclable nano carbon composite material, which comprises uniformly dispersed carbon nano tubes, two-dimensional graphene-like polymers and high molecular polymers.
The repairing method of the recyclable multifunctional composite bucky paper provided by the embodiment of the invention comprises the following steps: and applying force to the gap of the multifunctional composite bucky paper to keep the corresponding broken ends spliced, and applying a specified solvent to the spliced position, thereby realizing the self-repairing of the composite bucky paper.
Furthermore, in the repairing method, after the corresponding fracture ends at the fracture are spliced, a certain amount of solvent is sprayed, sprayed and coated at the splicing position, and a certain pressure action is applied to reconstruct the carbon nanotube network at the fracture, so that the traceless repairing of the fracture is realized.
Further, the solvent includes water.
Furthermore, the multifunctional composite bucky paper treated by the repairing method still basically keeps the original shape and characteristics, such as good flexibility, bending resistance, high mechanical strength and the like, and also has the advantages of self-repairing, recycling and the like.
The crease eliminating method of the recyclable multifunctional composite bucky paper provided by the embodiment of the invention comprises the following steps: applying a specified solvent to the multi-functional composite bucky paper at the fold and applying a force at least at the fold tending to flatten the multi-functional composite bucky paper thereby eliminating the fold.
Further, the method for removing the crease specifically may include: and spraying, spraying and coating a certain amount of specified solvent at the crease of the multifunctional composite bucky paper, and applying force at the crease by pressing and other modes to ensure that the multifunctional composite bucky paper tends to be flat at the crease, thereby eliminating the crease.
Further, the solvent includes water.
Furthermore, the multifunctional composite bucky paper treated by the crease removing method still maintains the original shape and characteristics, such as good flexibility, bending resistance, high mechanical strength and the like, and also has the advantages of self-repairing, recycling and the like.
The recycling method of the recyclable nanocarbon composite material provided by the embodiment of the invention comprises the following steps:
immersing the used nano carbon composite material into a specified solvent to disintegrate the nano carbon composite material to form a mixed solution; and separating the specified solvent in the mixed solution to reform the nano carbon composite material.
In some embodiments, the recycling method specifically comprises: and (3) immersing the used nano carbon composite material into a specified solvent, and disintegrating the nano carbon composite material by heating and/or continuously stirring to form the mixed solution. Further, the recycling method may include: the heating temperature used therein may be relatively low, for example, about 50 ℃, about 70 ℃ or the like, and is lower than the vaporization temperature of the solvent. Further, during the aforementioned heating process, the nano carbon composite material can be disintegrated more rapidly and a mixed solution in which the carbon nanotubes are dispersed more uniformly can be formed more rapidly with continuous stirring of the mixed system.
Obviously, in the process of disintegrating the nanocarbon composite material, ultrasound and the like can be used as an auxiliary operation.
Further, the specified solvent comprises water.
Further, the recycling method may further include: and (3) treating the mixed solution by a filtration mode (such as vacuum filtration) to form the nano carbon composite material.
Further, the recycling method may further include: and removing the specified solvent in the mixed solution by natural evaporation to form the nanocarbon composite material.
Furthermore, the nanocarbon composite material reformed by the recycling method can still maintain the original characteristics, for example, the formed multifunctional composite bucky paper can still maintain the original characteristics, such as good flexibility, bending resistance, high mechanical strength and the like, and also has the advantages of self-repairing, recycling and the like.
The technical solution of the present invention will be described in more detail with reference to some specific embodiments and the accompanying drawings.
Referring to fig. 1, some more specific embodiments of the present invention relate to a method for preparing multifunctional composite bucky paper, which may include the following steps:
1) firstly, mixing a Sulfonated Graphene Polymer (SGP) solution with a certain concentration and carbon nanotube powder (CNTs) according to different proportions, and then carrying out ultrasonic dispersion treatment (the ultrasonic time can be more than 4 hours, for example) on the formed mixed solution so as to uniformly disperse carbon nanotubes with the aid of the sulfonated graphene polymer, thereby forming the uniform dispersion liquid;
2) mixing a polyvinyl alcohol (PVA) solution with a certain concentration and the uniform dispersion liquid according to different proportions to form a mixed solution;
3) and carrying out vacuum filtration treatment on the mixed solution to obtain the multifunctional composite bucky paper.
In the step 3), the mixed solution may be naturally evaporated to dryness to obtain the multifunctional composite bucky paper or the nanocarbon composite material in the form of film, sheet, block, or the like.
Fig. 2 is a schematic diagram illustrating a forming principle of a multifunctional composite bucky paper in the foregoing embodiment of the present invention, in which the sulfonated graphene polymer exhibits a function of a carbon nanotube dispersant to a certain extent, and after being combined with a carbon nanotube, the sulfonated graphene polymer facilitates uniform dispersion of the carbon nanotube in a mixed system in a subsequent process, so as to obtain a high-concentration carbon nanotube dispersed system; and then, adding PVA and the like into a system containing the sulfonated graphene polymer/carbon nano tube compound, and then assisting in vacuum filtration to tightly combine the sulfonated graphene polymer, the carbon nano tube and the polyvinyl alcohol to form the multifunctional composite bucky paper. The Sulfonated Graphene Polymers (SGP), carbon nanotube powders (CNTs), polyvinyl alcohol (PVA), and the like can be obtained from a wide variety of sources, and can be obtained, for example, from commercial sources.
The concentration of the Sulfonated Graphene Polymer (SGP) solution may be any suitable concentration, and may be, for example, preferably 10 wt%.
The concentration of the polyvinyl alcohol (PVA) solution may be any suitable concentration, and may preferably be 1 wt%, for example. The mass ratio of the Sulfonated Graphene Polymer (SGP), the carbon nanotube powder (CNTs), and the polyvinyl alcohol (PVA) may be a suitable ratio, for example, it may be preferably (3-8): 2-7, and more specifically, the mass ratio of the SGP/CNTs/PVA may be selected from the following group:
8/2/5,8/2/10,8/2/15,8/2/20,7/3/5,7/3/10,7/3/15,7/3/20,6/4/5,6/4//10,6/4//15,6/4//20，5/5/5,5/5/10,5/5/15,5/5/20，4/6/5,4/6/10,4/6/15,4/6/20，3/7/5,3/7/10,3/7/15,3/7/20。
referring to fig. 3, a photograph of a multifunctional composite bucky paper obtained according to the previous embodiment of the present invention is shown. The other multifunctional composite bucky paper obtained in the embodiment also shows basically the same shape. These composite bucky papers are flexible and can be bent without breakage.
Referring to fig. 4a, in the previous embodiment, when the mass ratio of SGP/CNT/PVA is 7: 3: 10. 5: 5: 10. 3: 7: 10. 5: 5: and 5, according to the mechanical property test result of the formed multifunctional composite paper, the composite paper has higher mechanical strength which can reach 100MPa at most. The composite bucky paper formed by adopting other SGP/CNT/PVA ratios is proved to have better mechanical strength through the same mechanical test.
Fig. 4b shows mechanical property test results of the multifunctional composite paper base paper formed in the foregoing embodiment when the mass ratio of SGP/CNT/PVA is other ratios, and it can be seen that the composite paper base paper has better mechanical strength. The multifunctional composite bucky paper obtained by the embodiment of the invention has the self-repairing capability of the crease and the cut. For example, as shown in fig. 5, for a plain white paper (commercially available a4 paper), the crease is still very noticeable and substantially not completely eliminated after spraying deionized water with pressure.
Similarly, referring to fig. 5, for any of the samples of composite bucky paper according to the previous embodiments of the present invention, after forming the crease, the crease is substantially removed by spraying deionized water at the crease with a light press.
Referring to fig. 5, for any one of the composite bucky paper samples according to the previous embodiments of the present invention, if a cut is formed at any position, the corresponding broken end at the cut is spliced, and then a certain amount of deionized water is sprayed at the spliced position, and the pressure is continuously applied for a period of time, so that the cut can heal by itself, and no cut mark is left. The mechanical strength of the composite bucky paper sample before the notch is formed and the mechanical strength of the repaired composite bucky paper sample are respectively tested, and as shown in fig. 6, the mechanical strength can still be well maintained (the mechanical strength can be recovered to about 70% of the original mechanical strength).
In addition, for each composite bucky paper sample obtained in the previous examples, it can also be recycled. For example, as shown in fig. 1, the used composite paper may be soaked in deionized water, and then the solution is stirred at a temperature of about 50 ℃ (preferably about 70 ℃) for 4-5 hours, so as to dissolve the composite paper, and then the formed mixed solution is vacuum filtered again, so as to form the composite paper again. The composite paper can maintain the original characteristics.
Similarly, the nanocarbon composite materials of other forms obtained in the foregoing examples can be recycled in substantially the same manner. In other embodiments of the present invention, a carboxylated graphene polymer is used to replace the sulfonated graphene polymer, and polyethylene glycol, aqueous polyurethane, etc. are used to replace the polyvinyl alcohol, so as to obtain composite bucky paper or other nanocarbon composite materials with similar properties.
It should be noted that, the technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, however, as long as there is no contradiction between the combinations of the technical features, the scope of the present description should be considered as being included in the present specification.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (9)
1. A method for repairing a flexible, bend-resistant multifunctional composite bucky paper, comprising:
a two-dimensional or three-dimensional aggregation structure formed by densely interweaving a plurality of carbon nano tubes,
the two-dimensional graphene-like polymer and the high polymer are distributed in the two-dimensional or three-dimensional aggregation structure, the two-dimensional graphene-like polymer is selected from a sulfonated graphene-like polymer or a carboxylated graphene-like polymer, the high polymer is selected from a water-soluble high polymer, and the mass ratio of the two-dimensional graphene-like polymer to the carbon nano tube is (3-8) to (2-7);
the repair method includes: and applying force to the split of the multifunctional composite bucky paper to keep the splicing of the corresponding broken ends, and applying a specified solvent to the spliced position, thereby realizing the self-repairing of the composite bucky paper, wherein the specified solvent comprises water.
2. The method of repairing a flexible bend-resistant multifunctional composite bucky paper according to claim 1, characterized in that: the high molecular polymer is selected from polyvinyl alcohol, polyethylene glycol or waterborne polyurethane.
3. A crease eliminating method of flexible bending-resistant multifunctional composite bucky paper is characterized in that the multifunctional composite bucky paper comprises the following steps:
a two-dimensional or three-dimensional aggregation structure formed by densely interweaving a plurality of carbon nano tubes,
the two-dimensional graphene-like polymer and the high polymer are distributed in the two-dimensional or three-dimensional aggregation structure, the two-dimensional graphene-like polymer is selected from a sulfonated graphene-like polymer or a carboxylated graphene-like polymer, the high polymer is selected from a water-soluble high polymer, and the mass ratio of the two-dimensional graphene-like polymer to the carbon nano tube is (3-8) to (2-7);
also, the crease removal method includes: applying a specified solvent to the multi-functional composite bucky paper at the crease, and applying a force at least at the crease that tends to flatten the multi-functional composite bucky paper, thereby eliminating the crease, the specified solvent comprising water.
4. The method for removing creases from a flexible bend-resistant multifunctional composite buckypaper according to claim 3, characterized in that: the high molecular polymer is selected from polyvinyl alcohol, polyethylene glycol or waterborne polyurethane.
5. A recycling method of flexible bending-resistant multifunctional composite base paper is characterized in that the multifunctional composite base paper comprises the following steps:
a two-dimensional or three-dimensional aggregation structure formed by densely interweaving a plurality of carbon nano tubes,
the two-dimensional graphene-like polymer and the high polymer are distributed in the two-dimensional or three-dimensional aggregation structure, the two-dimensional graphene-like polymer is selected from a sulfonated graphene-like polymer or a carboxylated graphene-like polymer, the high polymer is selected from a water-soluble high polymer, and the mass ratio of the two-dimensional graphene-like polymer to the carbon nano tube is (3-8) to (2-7);
the recycling method includes: immersing the used multifunctional composite paper into a specified solvent to disintegrate the multifunctional composite paper to form a mixed solution; and separating the appointed solvent in the mixed solution to reform the multifunctional composite bucky paper, wherein the appointed solvent comprises water.
6. The method of recycling a flexible, bend-resistant multi-functional composite bucky paper according to claim 5, comprising: and (2) immersing the used multifunctional composite paper into a specified solvent, and disintegrating the multifunctional composite paper by heating and/or continuously stirring to form the mixed solution.
7. The method of recycling a flexible, bend-resistant multi-functional composite bucky paper according to claim 6, comprising: and treating the mixed solution in a filtering mode to form the multifunctional composite bucky paper.
8. The method of recycling the flexible bend-resistant multifunctional composite bucky paper according to claim 6, wherein the multifunctional composite bucky paper is formed by removing the specified solvent in the mixed solution by natural evaporation.
9. The method of recycling flexible bend-resistant multifunctional composite buckypaper according to claim 5, characterized in that: the high molecular polymer is selected from polyvinyl alcohol, polyethylene glycol or waterborne polyurethane.
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| CN103319734A (en) * | 2012-03-20 | 2013-09-25 | 沈阳航空航天大学 | Method for preparing carbon nanometer paper enhanced conductive polymer matrix composite material |
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