CN108752611B - Aramid nanofiber hybrid film with high mechanical strength and preparation method thereof - Google Patents
Aramid nanofiber hybrid film with high mechanical strength and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an aramid fiber nanofiber hybrid film with high mechanical strength and a preparation method thereof, wherein the film comprises the following components in parts by mass: 100 parts of aramid nano-fiber and 3-15 parts of graphene oxide. According to the method, the structural recombination of the aramid nano-fiber is promoted by utilizing a hydration protonation effect, and meanwhile, the ordered gelation self-assembly of the nano-fiber is induced, so that the thickness of a film material is conveniently regulated and controlled; the one-dimensional nanofiber matrix is filled with the two-dimensional graphene oxide reinforced phase, so that the interface compatibility advantage among phase components is effectively exerted, and the mechanical property of the aramid fiber composite film material is greatly improved.
Description
Technical Field
The invention belongs to the technical field of preparation of fiber polymer composite materials, and particularly relates to an aramid fiber hybrid film with high mechanical property and a preparation method thereof.
Background
A polymer composite film is a polymer composite material that is polymerized relative to a macroscopically three dimensional size of the material
The compound film can maintain the performance of the block material and has anisotropy in two-dimensional direction, and is widely applied in the directions of capacitance devices, biological permeation, photoelectric characteristics, corrosion prevention, heat insulation and the like. In order to adapt to the actual harsh application environment and prolong the service life, the polymer film with high mechanical property prepared by adopting a simple and efficient synthesis method has great practical value.
Poly-p-phenylene terephthamide (PPTA) is a high-performance para-aramidA fiber having a basic repeating unit of- [ -CO-C6H4-CONH-C6H4NH-]-. The strong acting force consisting of hydrogen bonds, pi-pi stacking conjugation and van der Waals force exists among PPTA molecular chains, so that the macroscopic aramid fiber yarn has the advantages of high strength, high modulus, high temperature resistance, chemical corrosion resistance, strong flame retardance, fatigue resistance, strong stability and the like, and the superior specific strength and specific modulus of the macroscopic aramid fiber yarn exceed those of common fiber materials. In order to widen the application of the aramid fiber composite material in the industrial field, the hydrogen bond and the pi-pi acting force between fibers must be destroyed to enable the aramid fiber to be nano-functionalized. The document ACS nano,2015,9(3):2489-2501 reports that the carbon nano tube is used as a mechanical reinforcing filler, and a para-aramid nano fiber/carbon nano tube hybrid film material with higher mechanical strength is prepared by adopting a suction filtration self-assembly technology. The reduced graphene oxide hybrid film material taking the aramid nano-fiber as a reinforcing phase is prepared by the suction filtration self-assembly technology in ACS nano,2017,11(7):6682 and 6690. Wherein, when the mass fraction of the aramid nano-fiber is 25%, the tensile strength of the hybrid film can reach 100.6MPa at most. The tensile strength of the film material is improved by 350% compared with that of a pure reduced graphene oxide film, however, the tensile strength is not improved compared with that of an aramid nano-fiber film, and the elongation at break is reduced by 60%.
Disclosure of Invention
The invention aims to provide an aramid nanofiber hybrid film and a preparation method thereof.
The technical solution for realizing the purpose of the invention is as follows:
the aramid nanofiber hybrid film comprises the following components in parts by mass:
100 parts of aramid nano-fiber and 3-15 parts of graphene oxide.
Further, the average size of the aramid nanofibers is: the diameter is 30-40nm, and the length is 5-10 μm.
The preparation method of the aramid nanofiber hybrid film comprises the following steps:
step one, mixing a DMSO dispersion solution of graphene oxide and a DMSO solution of aramid nano-fibers, and stirring at room temperature for more than 1h, wherein in the mixed solution, the mass parts of the aramid nano-fibers are 100, and the mass parts of the graphene oxide are 3-15;
step two, adding deionized water into the blending liquid obtained in the step one, heating and stirring for more than 2 hours, and then aging for 2 hours at room temperature;
and step three, removing the solvent through vacuum filtration to obtain the gelatinous graphene oxide/aramid nano-fiber composite material, drying at room temperature, peeling off the material from the microporous filter membrane, and drying in vacuum for 6 hours to obtain the aramid nano-fiber hybrid film.
Furthermore, in the second step, 125-200 mL of deionized water is added to every 100mL of the blending solution.
Further, in the second step, the temperature is increased to 80 +/-5 ℃ and the mixture is stirred for more than 2 hours.
Further, in the third step, the vacuum filtration device adopts a sand core funnel to prepare a microporous filter membrane with the diameter of 47 mm.
Further, in the third step, the vacuum filtration pressure is-0.1 MPa.
Compared with the prior art, the invention has the following remarkable advantages: (1) the structural recombination of the aramid nano-fiber is promoted by utilizing the hydration protonation effect, and meanwhile, the ordered gelation self-assembly of the nano-fiber is induced, so that the thickness of the film material is conveniently regulated and controlled; (2) the one-dimensional nanofiber matrix is filled with the two-dimensional graphene oxide reinforced phase, so that the interface compatibility advantage among phase components is effectively exerted, and the mechanical property of the aramid fiber composite film material is greatly improved, for example, when 15 parts of graphene oxide is filled, the tensile strength of the polymer composite film reaches 441.48MPa, the Young modulus reaches 7.59GPa, and the elongation at break reaches 19.21%. Compared with the aramid nano-fiber film which is not filled with graphene oxide, the tensile strength, the Young modulus and the elongation at break are respectively improved by 140 percent, 59 percent and 131 percent.
The present invention is described in further detail below with reference to the attached drawing figures.
Drawings
Fig. 1 is a flow chart of the preparation method of the polymer hybrid film based on the aramid nano-fiber.
Fig. 2 is a stress-strain curve diagram of the polymer hybrid film based on aramid nanofibers according to the present invention.
Detailed Description
The present invention is further illustrated by the following examples and comparative examples.
As a common mechanical reinforcing filler, graphene oxide is characterized by high strength and high modulus (approximately 40GPa), and the mechanical properties of the material can be obviously improved by adding the graphene oxide into a polymer matrix. The graphene oxide with ultrahigh modulus and the high-strength para-aramid fiber are effectively compounded, so that the mechanical property of the polymer film is broken through.
The flow schematic diagram of the preparation method of the polymer hybrid film based on the aramid nano-fiber is shown in figure 1.
Example 1
Weighing 1g of aramid fiber yarn and 1.5g of potassium hydroxide, putting into a reactor, adding a DMSO solution, and stirring for 7 days at the temperature of 25 ℃ to obtain an aramid nanofiber solution.
3g of graphite powder and 18g of potassium permanganate are weighed and put into a reactor, mixed acid (concentrated sulfuric acid: 360mL, concentrated phosphoric acid: 40mL) is slowly added, and the mixture is stirred until the mixture is uniformly mixed. The reaction system is transferred to a water bath kettle and stirred for 12 hours at the constant temperature of 50 ℃. The reaction was then poured onto 400mL of ice, stirring was continued, and hydrogen peroxide (30 wt.%) was added dropwise until the reaction turned bright yellow. The reaction solution was filtered while hot and washed with dilute hydrochloric acid at a ratio of 1: 10. And (3) performing high-speed centrifugation and repeated water washing on the product until the product is close to neutrality, and performing ultrasonic treatment for more than 1h at the power of 100W to obtain the graphene oxide water suspension.
Taking 3 parts by weight of graphene oxide aqueous suspension, carrying out ultrasonic dispersion for more than 0.5h at a power of 100W, adding an equal volume of DMSO solution, and carrying out reduced pressure distillation treatment for 4h at 80 ℃ to obtain the DMSO suspension of graphene oxide. The graphene oxide/aramid nano-fiber composite material is uniformly mixed with an aramid nano-fiber solution to prepare 40mL of blending solution, 50mL of deionized water (water is a protonation promoter of the aramid nano-fiber and induces the structural recombination of the nano-fiber) is added, and the mixture is stirred at 80 ℃ for more than 2 hours to obtain a graphene oxide/aramid nano-fiber mixture. The system comprises the following components in proportion: 100 parts of aramid nanofiber, graphene oxide: and 3 parts. And aging the mixture for 2h under the condition of 0.01MPa of air pressure, removing bubbles, and performing vacuum filtration treatment to obtain the graphene oxide/aramid nano-fiber composite gel film. And finally, drying for 6 hours under a vacuum condition to obtain the aramid nano-fiber hybrid film containing 3 parts of graphene oxide. The film had a thickness of 28 μm, a tensile strength of 275.77MPa, a Young's modulus of 4.70GPa, and an elongation at break of 17.73%.
Example 2
Weighing 1g of aramid fiber yarn and 1.5g of potassium hydroxide, putting into a reactor, adding a DMSO solution, and stirring for 7 days at the temperature of 25 ℃ to obtain an aramid nanofiber solution.
3g of graphite powder and 18g of potassium permanganate are weighed and put into a reactor, mixed acid (concentrated sulfuric acid: 360mL, concentrated phosphoric acid: 40mL) is slowly added, and the mixture is stirred until the mixture is uniformly mixed. The reaction system is transferred to a water bath kettle and stirred for 12 hours at the constant temperature of 50 ℃. The reaction was then poured onto 400mL of ice, stirring was continued, and hydrogen peroxide (30 wt.%) was added dropwise until the reaction turned bright yellow. The reaction solution was filtered while hot and washed with dilute hydrochloric acid at a ratio of 1: 10. And (3) performing high-speed centrifugation and repeated water washing on the product until the product is close to neutrality, performing ultrasonic treatment for more than 1h at the power of 100W, and thus obtaining the graphene oxide suspension.
And (3) taking 5 parts of graphene oxide suspension, carrying out ultrasonic dispersion for more than 0.5h at the power of 100W, adding an isometric DMSO solution, and carrying out reduced pressure distillation treatment for 4h at the temperature of 80 ℃ to obtain the DMSO suspension of graphene oxide. And uniformly mixing the graphene oxide/aramid nano-fiber mixture with an aramid nano-fiber solution to prepare 40mL of blending solution, adding 80mL of deionized water, and stirring at 80 ℃ for more than 2h to obtain a graphene oxide/aramid nano-fiber mixture. The system comprises the following components in proportion: 100 parts of aramid nanofiber, graphene oxide: 5 parts of the raw materials. And aging the mixture for 2h under the condition of 0.01MPa of air pressure, removing bubbles, and performing vacuum filtration treatment to obtain the graphene oxide/aramid nano-fiber composite gel film. And finally, drying for 6 hours under a vacuum condition to obtain the aramid nano-fiber hybrid film containing 5 parts of graphene oxide. The film had a thickness of 30 μm, a tensile strength of 365.32MPa, a Young's modulus of 5.98GPa, and an elongation at break of 21.12%.
Example 3
Weighing 1g of aramid fiber yarn and 1.5g of potassium hydroxide, putting into a reactor, adding a DMSO solution, and stirring for 7 days at the temperature of 25 ℃ to obtain an aramid nanofiber solution.
3g of graphite powder and 18g of potassium permanganate are weighed and put into a reactor, mixed acid (concentrated sulfuric acid: 360mL, concentrated phosphoric acid: 40mL) is slowly added, and the mixture is stirred until the mixture is uniformly mixed. The reaction system is transferred to a water bath kettle and stirred for 12 hours at the constant temperature of 50 ℃. The reaction was then poured onto 400mL of ice, stirring was continued, and hydrogen peroxide (30 wt.%) was added dropwise until the reaction turned bright yellow. The reaction solution was filtered while hot and washed with dilute hydrochloric acid at a ratio of 1: 10. And (3) performing high-speed centrifugation and repeated water washing on the product until the product is close to neutrality, performing ultrasonic treatment for more than 1h at the power of 100W, and thus obtaining the graphene oxide suspension.
And (3) taking 10 parts of graphene oxide suspension, carrying out ultrasonic dispersion for more than 0.5h at the power of 100W, adding an isometric DMSO solution, and carrying out reduced pressure distillation treatment for 4h at the temperature of 80 ℃ to obtain the DMSO suspension of graphene oxide. The graphene oxide/aramid nano-fiber composite material is uniformly mixed with an aramid nano-fiber solution to prepare 40mL of blending solution, 50mL of deionized water is added, and the mixture is stirred for more than 2 hours at 80 ℃ to obtain a graphene oxide/aramid nano-fiber mixture. The system comprises the following components in proportion: 100 parts of aramid nanofiber, graphene oxide: 10 parts. And aging the mixture for 2h under the condition of 0.01MPa of air pressure, removing bubbles, and performing vacuum filtration treatment to obtain the graphene oxide/aramid nano-fiber composite gel film. And finally, drying for 6 hours under a vacuum condition to obtain the aramid nano-fiber hybrid film containing 10 parts of graphene oxide. The film had a thickness of 32 μm, a tensile strength of 399.82MPa, a Young's modulus of 7.21GPa, and an elongation at break of 12.53%.
Example 4
Weighing 1g of aramid fiber yarn and 1.5g of potassium hydroxide, putting into a reactor, adding a DMSO solution, and stirring for 7 days at the temperature of 25 ℃ to obtain an aramid nanofiber solution.
3g of graphite powder and 18g of potassium permanganate are weighed and put into a reactor, mixed acid (concentrated sulfuric acid: 360mL, concentrated phosphoric acid: 40mL) is slowly added, and the mixture is stirred until the mixture is uniformly mixed. The reaction system is transferred to a water bath kettle and stirred for 12 hours at the constant temperature of 50 ℃. The reaction was then poured onto 400mL of ice, stirring was continued, and hydrogen peroxide (30 wt.%) was added dropwise until the reaction turned bright yellow. The reaction solution was filtered while hot and washed with dilute hydrochloric acid at a ratio of 1: 10. And (3) performing high-speed centrifugation and repeated water washing on the product until the product is close to neutrality, performing ultrasonic treatment for more than 1h at the power of 100W, and thus obtaining the graphene oxide suspension.
Taking 15 parts of graphene oxide suspension, carrying out ultrasonic dispersion for more than 0.5h at a power of 100W, adding an isometric DMSO solution, and carrying out reduced pressure distillation treatment for 4h at 80 ℃ to obtain the DMSO suspension of graphene oxide. The graphene oxide/aramid nano-fiber composite material is uniformly mixed with an aramid nano-fiber solution to prepare 40mL of blending solution, 64mL of deionized water is added, and the mixture is stirred for more than 2 hours at 80 ℃ to obtain a graphene oxide/aramid nano-fiber mixture. The system comprises the following components in proportion: 100 parts of aramid nanofiber, graphene oxide: 15 parts. And aging the mixture for 2h under the condition of 0.01MPa of air pressure, removing bubbles, and performing vacuum filtration treatment to obtain the graphene oxide/aramid nano-fiber composite gel film. And finally, drying for 6 hours under a vacuum condition to obtain the aramid nano-fiber hybrid film containing 15 parts of graphene oxide. The film had a thickness of 33 μm, a tensile strength of 441.48MPa, a Young's modulus of 7.59GPa, and an elongation at break of 19.21%.
Comparative example 1
The method of example 1 was repeated with the specified amounts of the components, but without graphene oxide in the formulation. The film had a thickness of 25 μm, a tensile strength of 184.57MPa, a Young's modulus of 4.78GPa, and an elongation at break of 8.31%.
Comparative example 2
The method of example 1 was repeated with the specified amounts of the components, but without the aramid nanofibers in the formulation. The thickness of the obtained graphene oxide film is 25 micrometers, the tensile strength is 92.97MPa, the Young modulus is 8.54GPa, and the elongation at break is 1.30%.
Comparative example 3
The process of comparative example 2 was repeated with the specified amounts of the components, but with 20 parts of aramid nanofibers in the formulation. The tensile strength of the film was 140.24MPa, the Young's modulus was 8.06GPa, and the elongation at break was 2.15%.
Comparative example 4
The process of comparative example 2 was repeated with the specified amounts of the components, but with 50 parts of aramid nanofibers in the formulation. The tensile strength of the film was 85.67MPa, the Young's modulus was 7.91GPa, and the elongation at break was 1.93%.
Table 1 and fig. 2 are performance test data of examples 1 to 4 and comparative examples 1 to 4.
TABLE 1
According to the invention, a simple vacuum induction suction filtration self-assembly method is adopted, and graphene oxide is introduced as a mechanical reinforcing agent to fill the aramid nano-fiber film, so that the tensile strength, Young modulus and elongation at break of the film material are greatly improved, and the purpose of remarkably improving the mechanical performance of the aramid nano-fiber film is achieved. Therefore, the invention provides the aramid nano-fiber composite film with high mechanical strength and the preparation method thereof.
Claims (5)
1. The aramid nanofiber hybrid film is characterized by comprising the following components in parts by mass:
100 parts of aramid nano-fiber and 3-15 parts of graphene oxide;
the method comprises the following steps:
step one, mixing a DMSO dispersion solution of graphene oxide and a DMSO solution of aramid nano-fibers, and stirring at room temperature for more than 1h, wherein in the mixed solution, the mass parts of the aramid nano-fibers are 100, and the mass parts of the graphene oxide are 3-15;
step two, adding deionized water into the blending liquid obtained in the step one, heating to 80 +/-5 ℃, stirring for more than 2 hours, aging at room temperature for 2 hours, and adding 125-200 mL of deionized water into every 100mL of blending liquid;
and step three, removing the solvent through vacuum filtration to obtain the gelatinous graphene oxide/aramid nano-fiber composite material, drying at room temperature, peeling off the material from the microporous filter membrane, and drying in vacuum for 6 hours to obtain the aramid nano-fiber hybrid film.
2. The film of claim 1, wherein the aramid nanofibers have an average size of: the diameter is 30-40nm, and the length is 5-10 μm.
3. The preparation method of the aramid nanofiber hybrid film is characterized by comprising the following steps of:
step one, mixing a DMSO dispersion solution of graphene oxide and a DMSO solution of aramid nano-fibers, and stirring at room temperature for more than 1h, wherein in the mixed solution, the mass parts of the aramid nano-fibers are 100, and the mass parts of the graphene oxide are 3-15;
step two, adding deionized water into the blending liquid obtained in the step one, heating to 80 +/-5 ℃, stirring for more than 2 hours, aging at room temperature for 2 hours, and adding 125-200 mL of deionized water into every 100mL of blending liquid;
and step three, removing the solvent through vacuum filtration to obtain the gelatinous graphene oxide/aramid nano-fiber composite material, drying at room temperature, peeling off the material from the microporous filter membrane, and drying in vacuum for 6 hours to obtain the aramid nano-fiber hybrid film.
4. The method of claim 3, wherein in step three, the vacuum filtration apparatus employs a sand core funnel to prepare a microfiltration membrane with a diameter of 47 mm.
5. The process according to claim 3, wherein in the third step, the vacuum filtration pressure is-0.1 MPa.
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| CN110318112B (en) * | 2019-07-23 | 2022-04-29 | 东华大学 | Neutron radiation prevention high-strength graphene oxide composite fiber and preparation method thereof |
| CN110655668B (en) * | 2019-10-25 | 2022-04-26 | 陕西科技大学 | Hydroxyapatite nanowire/ANF composite film and preparation method and application thereof |
| CN113136060B (en) * | 2020-11-16 | 2022-06-17 | 山东理工大学 | Preparation method of aramid nanofiber reinforced sweet sorghum residue composite material |
| CN113416414B (en) * | 2021-07-30 | 2022-04-22 | 湖南大学 | Preparation method and application of aramid nanofiber/porous graphene/polyaniline composition, hydrogel and film with high mechanical strength |
| US12024434B2 (en) | 2021-11-01 | 2024-07-02 | Wisconsin Alumni Research Foundation | Carbon-based composite materials with enhanced dynamic performance |
| CN115448691B (en) * | 2022-09-22 | 2023-06-09 | 东莞华贝电子科技有限公司 | Thermal conductive composite film and preparation method thereof |
| CN117127429A (en) * | 2023-08-30 | 2023-11-28 | 山东聚芳新材料股份有限公司 | Copolymerization fibrid/graphene composite film and preparation method thereof |
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