CN108752611A - A kind of aramid nano-fiber hybrid film of high strength and preparation method thereof - Google Patents
A kind of aramid nano-fiber hybrid film of high strength and preparation method thereof Download PDFInfo
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- CN108752611A CN108752611A CN201810424080.1A CN201810424080A CN108752611A CN 108752611 A CN108752611 A CN 108752611A CN 201810424080 A CN201810424080 A CN 201810424080A CN 108752611 A CN108752611 A CN 108752611A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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Abstract
The invention discloses aramid nano-fiber hybrid film of a kind of high strength and preparation method thereof, the film is in terms of mass parts, including following component：100 parts of aramid nano-fiber, 3-15 parts of graphene oxide.The present invention while promoting the structural rearrangement of aramid nano-fiber, induces the ordered gel self assembly of nanofiber using proton hydrate effect, easily regulates and controls the thickness of thin-film material；1-dimention nano fibrous matrix is filled with two dimensional oxidation graphene reinforced phase, the interface effectively played between phase component is compatible with advantage, greatly improves the mechanical mechanics property of aramid fiber composite film material.
Description
Technical field
The invention belongs to fiber-like polymer composites preparing technical fields, especially a kind of to have high mechanical mechanics
The aramid fiber hybrid film and preparation method thereof of energy.
Background technology
Polymer composite film is one kind of polymer composites, relative to the material of macroscopic three dimensional size, is gathered
Conjunction object film can in two-dimensional directional, there are anisotropy again while keeping block material property, in capacitor
Part, the directions such as biological filter, photoelectric characteristic and anticorrosive heat insulating are widely used.To adapt to practical harsh application environment, promotion makes
With the service life, the thin polymer film for preparing high mechanical mechanics property using the synthetic method being simple and efficient has great practical valence
Value.
Poly(p-phenylene terephthalamide) (PPTA) is a kind of high-performance para-aramid fiber, basic repetitive unit is-[-
CO-C6H4-CONH-C6H4NH-]-.Exist between PPTA strands and conjugation is stacked by hydrogen bond, π-π and Van der Waals force is formed
Powerful active force, imparts that macroscopical aramid fiber yarn high intensity, high-modulus, high temperature resistant, resistant to chemical etching, anti-flammability is strong, anti-
Fatigue, many advantages, such as stability is strong, superior specific strength have surmounted general fiber-like material with specific modulus.To widen virtue
Application of the synthetic fibre fibrous composite in industrial circle, it is necessary to destroy the hydrogen bond and π-π active forces between fiber, aramid fiber is made to receive
Rice functionalization.Document《ACS nano,2015,9(3):2489-2501》In report using carbon nanotube as mechanics reinforced filling,
The higher p-aramid fiber nanofiber/carbon nano-tube hybridization film of mechanical strength has been prepared using suction method self-assembling technique
Material.Document《ACS nano,2017,11(7):6682-6690》Equally it has been prepared with aramid fiber with filtering self-assembling technique
Nanofiber is the redox graphene hybrid film material of reinforcement phase.Wherein, when the mass fraction of aramid nano-fiber is
When 25%, the tensile strength of hybrid film reaches as high as 100.6MPa.The tensile strength of this thin-film material is relative to pure oxygen reduction
Graphite alkene film improves 350%, however, be not improved compared with aramid nano-fiber film, and elongation at break
Reduce 60%.
Invention content
The purpose of the present invention is to provide a kind of aramid nano-fiber hybrid films and preparation method thereof.
Realize that the technical solution of the object of the invention is：
A kind of aramid nano-fiber hybrid film, in terms of mass parts, including following component：
100 parts of aramid nano-fiber, 3-15 parts of graphene oxide.
Further, the average-size of aramid nano-fiber is：Diameter 30-40nm, 5-10 μm of length.
The preparation method of above-mentioned aramid nano-fiber hybrid film, includes the following steps：
The DMSO dispersion liquids of graphene oxide are blended with the DMSO solution of aramid nano-fiber, stir at room temperature by step 1
Mix 1h or more, wherein in blended liquid, aramid nano-fiber is 100 mass parts, and graphene oxide is 3-15 mass parts；
Step 2, is added deionized water into the blended liquid of step 1, and heating stirring 2 hours or more, then room temperature are aged 2h；
Step 3 obtains gelatinous graphene oxide/aramid nano-fiber composite wood through solvent is removed by suction filtration under vacuum
Material peels off after drying at room temperature from miillpore filter, is dried in vacuo 6h, and the aramid nano-fiber hybrid film is made.
Further, in step 2,125~200mL deionized waters are added in every 100mL blended liquids.
Further, in step 2,80 ± 5 DEG C of stirrings 2 hours or more are warming up to.
Further, in step 3, Vacuum filtration device prepares the miillpore filter of a diameter of 47mm using sand core funnel.
Further, in step 3, vacuum filtration pressure is -0.1MPa.
Compared with prior art, the present invention its remarkable advantage is：(1) proton hydrate effect is utilized to promote aramid fiber nanometer
While the structural rearrangement of fiber, the ordered gel self assembly of nanofiber is induced, easily regulates and controls the thickness of thin-film material；
(2) 1-dimention nano fibrous matrix is filled with two dimensional oxidation graphene reinforced phase, effectively plays the interface compatibility between phase component
Advantage greatly improves the mechanical mechanics property of aramid fiber composite film material, such as when filling 15 parts of graphene oxides,
The tensile strength of polymer composite film reaches 441.48MPa, and Young's modulus reaches 7.59GPa, and elongation at break is up to 19.21%.
Compared with the aramid nano-fiber film for being not filled by graphene oxide, tensile strength, Young's modulus and elongation at break carry respectively
It is high by 140%, 59% and 131%.
Present invention is further described in detail below in conjunction with the accompanying drawings.
Description of the drawings
Fig. 1 is the flow diagram of the polymer hybrid method for manufacturing thin film the present invention is based on aramid nano-fiber.
Fig. 2 is the stress-strain curve of the polymer hybrid film the present invention is based on aramid nano-fiber.
Specific implementation mode
Below by embodiment and comparative example, the invention will be further described.
As common mechanics reinforcing filler, the maximum characteristic of graphene oxide is its high intensity and high-modulus (≈
40GPa), the mechanical mechanics property of material can significantly be improved by adding graphene oxide into polymeric matrix.It utilizes
The para-aramid fiber of graphene oxide and high intensity with ultra high modulus carries out effectively compound, it should can make thin polymer film
Mechanical mechanics property have breakthrough.
The present invention is based on the flow diagram of the polymer hybrid method for manufacturing thin film of aramid nano-fiber is as shown in Figure 1.
Embodiment 1
It weighs 1g aramid fibers yarn and 1.5g potassium hydroxide is put into reactor, DMSO solution is added, is in temperature
It is stirred 7 days under conditions of 25 DEG C, obtains aramid nano-fiber solution.
It weighs 3g graphite powders and 18g potassium permanganate is put into reactor, be slowly added to the nitration mixture (concentrated sulfuric acid：360mL is dense
Phosphoric acid：40mL), it stirs to uniformly mixed.Reaction system is transferred in water-bath, constant temperature stirs 12h at 50 DEG C.It then will be anti-
It answers liquid to be poured into 400mL on ice, continues to stir, and hydrogen peroxide (30wt.%) is added dropwise until reaction solution becomes glassy yellow.While hot
Filtering reacting liquid is used in combination 1:10 dilute hydrochloric acid washing.Product is washed by high speed centrifugation and repeatedly until close to neutrality, at ultrasound
1h or more is managed, power 100W obtains graphene oxide water slurry.
The graphene oxide water slurry of 3 parts by weight, ultrasonic disperse 0.5h or more, power 100W is taken to be added isometric
DMSO solution handles 4h through vacuum distillation at 80 DEG C, obtains the DMSO suspension of graphene oxide.By itself and aramid nano-fiber
Solution, which is uniformly mixed, is made the blended liquid of 40mL, and 50mL deionized waters is added (water is that the protonation of aramid nano-fiber promotes
Agent induces the structural rearrangement of nanofiber), 2h or more is stirred at 80 DEG C, obtains the mixing of graphene oxide/aramid nano-fiber
Object.Each component proportioning is in system：100 parts of aramid nano-fiber, graphene oxide：3 parts.Mixture is in 0.01MPa air pressure items
It is aged 2h under part, removes bubble, is handled through vacuum filtration and graphene oxide/aramid nano-fiber plural gel film is made.Finally
6h is dried under vacuum, obtains the aramid nano-fiber hybrid film containing 3 parts of graphene oxides.The thickness of the film is 28
μm, tensile strength 275.77MPa, Young's modulus 4.70GPa, elongation at break 17.73%.
Embodiment 2
It weighs 1g aramid fibers yarn and 1.5g potassium hydroxide is put into reactor, DMSO solution is added, is in temperature
It is stirred 7 days under conditions of 25 DEG C, obtains aramid nano-fiber solution.
It weighs 3g graphite powders and 18g potassium permanganate is put into reactor, be slowly added to the nitration mixture (concentrated sulfuric acid：360mL is dense
Phosphoric acid：40mL), it stirs to uniformly mixed.Reaction system is transferred in water-bath, constant temperature stirs 12h at 50 DEG C.It then will be anti-
It answers liquid to be poured into 400mL on ice, continues to stir, and hydrogen peroxide (30wt.%) is added dropwise until reaction solution becomes glassy yellow.While hot
Filtering reacting liquid is used in combination 1:10 dilute hydrochloric acid washing.Product is washed by high speed centrifugation and repeatedly until close to neutrality, at ultrasound
1h or more is managed, power 100W obtains graphene oxide suspension.
Take 5 parts of graphene oxide suspensions, ultrasonic disperse 0.5h or more, power 100W that isometric DMSO solution is added,
4h is handled through vacuum distillation at 80 DEG C, obtains the DMSO suspension of graphene oxide.It is mixed with aramid nano-fiber solution
The blended liquid of 40mL uniformly is made, and 80mL deionized waters are added, 2h or more is stirred at 80 DEG C, obtains graphene oxide/aramid fiber
The mixture of nanofiber.Each component proportioning is in system：100 parts of aramid nano-fiber, graphene oxide：5 parts.Mixture exists
It is aged 2h under 0.01MPa air pressure conditions, removes bubble, it is multiple to handle obtained graphene oxide/aramid nano-fiber through vacuum filtration
Close gel mould.6h is finally dried under vacuum, obtains the aramid nano-fiber hybrid film containing 5 parts of graphene oxides.It should
The thickness of film is 30 μm, tensile strength 365.32MPa, Young's modulus 5.98GPa, elongation at break 21.12%.
Embodiment 3
It weighs 1g aramid fibers yarn and 1.5g potassium hydroxide is put into reactor, DMSO solution is added, is in temperature
It is stirred 7 days under conditions of 25 DEG C, obtains aramid nano-fiber solution.
It weighs 3g graphite powders and 18g potassium permanganate is put into reactor, be slowly added to the nitration mixture (concentrated sulfuric acid：360mL is dense
Phosphoric acid：40mL), it stirs to uniformly mixed.Reaction system is transferred in water-bath, constant temperature stirs 12h at 50 DEG C.It then will be anti-
It answers liquid to be poured into 400mL on ice, continues to stir, and hydrogen peroxide (30wt.%) is added dropwise until reaction solution becomes glassy yellow.While hot
Filtering reacting liquid is used in combination 1:10 dilute hydrochloric acid washing.Product is washed by high speed centrifugation and repeatedly until close to neutrality, at ultrasound
1h or more is managed, power 100W obtains graphene oxide suspension.
Take 10 parts of graphene oxide suspensions, ultrasonic disperse 0.5h or more, power 100W that it is molten that isometric DMSO is added
Liquid handles 4h through vacuum distillation at 80 DEG C, obtains the DMSO suspension of graphene oxide.Itself and aramid nano-fiber solution are mixed
Uniformly the blended liquid of 40mL is made in conjunction, and 50mL deionized waters are added, and 2h or more is stirred at 80 DEG C, obtains graphene oxide/virtue
The mixture of synthetic fibre nanofiber.Each component proportioning is in system：100 parts of aramid nano-fiber, graphene oxide：10 parts.Mixing
Object is aged 2h under 0.01MPa air pressure conditions, removes bubble, is handled through vacuum filtration and graphene oxide/aramid fiber Nanowire is made
Tie up plural gel film.6h is finally dried under vacuum, and it is thin to obtain the aramid nano-fiber hydridization containing 10 parts of graphene oxides
Film.The thickness of the film is 32 μm, tensile strength 399.82MPa, Young's modulus 7.21GPa, elongation at break 12.53%.
Embodiment 4
It weighs 1g aramid fibers yarn and 1.5g potassium hydroxide is put into reactor, DMSO solution is added, is in temperature
It is stirred 7 days under conditions of 25 DEG C, obtains aramid nano-fiber solution.
It weighs 3g graphite powders and 18g potassium permanganate is put into reactor, be slowly added to the nitration mixture (concentrated sulfuric acid：360mL is dense
Phosphoric acid：40mL), it stirs to uniformly mixed.Reaction system is transferred in water-bath, constant temperature stirs 12h at 50 DEG C.It then will be anti-
It answers liquid to be poured into 400mL on ice, continues to stir, and hydrogen peroxide (30wt.%) is added dropwise until reaction solution becomes glassy yellow.While hot
Filtering reacting liquid is used in combination 1:10 dilute hydrochloric acid washing.Product is washed by high speed centrifugation and repeatedly until close to neutrality, at ultrasound
1h or more is managed, power 100W obtains graphene oxide suspension.
Take 15 parts of graphene oxide suspensions, ultrasonic disperse 0.5h or more, power 100W that it is molten that isometric DMSO is added
Liquid handles 4h through vacuum distillation at 80 DEG C, obtains the DMSO suspension of graphene oxide.Itself and aramid nano-fiber solution are mixed
Uniformly the blended liquid of 40mL is made in conjunction, and 64mL deionized waters are added, and 2h or more is stirred at 80 DEG C, obtains graphene oxide/virtue
The mixture of synthetic fibre nanofiber.Each component proportioning is in system：100 parts of aramid nano-fiber, graphene oxide：15 parts.Mixing
Object is aged 2h under 0.01MPa air pressure conditions, removes bubble, is handled through vacuum filtration and graphene oxide/aramid fiber Nanowire is made
Tie up plural gel film.6h is finally dried under vacuum, and it is thin to obtain the aramid nano-fiber hydridization containing 15 parts of graphene oxides
Film.The thickness of the film is 33 μm, tensile strength 441.48MPa, Young's modulus 7.59GPa, elongation at break 19.21%.
Comparative example 1
According to the method that specified each component content repeats embodiment 1, but graphene oxide is free of in formula.The film
Thickness be 25 μm, tensile strength 184.57MPa, Young's modulus 4.78GPa, elongation at break 8.31%.
Comparative example 2
According to the method that specified each component content repeats embodiment 1, but aramid nano-fiber is free of in formula.It obtains
Graphene oxide film thickness be 25 μm, tensile strength 92.97MPa, Young's modulus 8.54GPa, elongation at break
1.30%.
Comparative example 3
According to the method that specified each component content repeats comparative example 2, but contain 20 parts of aramid nano-fibers in formula.It should
The tensile strength 140.24MPa of film, Young's modulus 8.06GPa, elongation at break 2.15%.
Comparative example 4
According to the method that specified each component content repeats comparative example 2, but contain 50 parts of aramid nano-fibers in formula.It should
The tensile strength 85.67MPa of film, Young's modulus 7.91GPa, elongation at break 1.93%.
Table 1 and the performance test data that Fig. 2 is embodiment 1-4 and comparative example 1-4.
Table 1
。
Self-assembly method is filtered using simple vacuum induced in the present invention, is used as mechanics reinforcement by introducing graphene oxide
Aramid nano-fiber film is filled in agent, is greatly improved thin-film material tensile strength, Young's modulus and elongation at break, is reached
Significantly improve the purpose of the mechanical mechanics property of aramid nano-fiber film.Therefore the present invention provides one kind to have high mechanics strong
Aramid nano-fiber laminated film of degree and preparation method thereof.
Claims (7)
1. a kind of aramid nano-fiber hybrid film, which is characterized in that in terms of mass parts, including following component：
100 parts of aramid nano-fiber, 3-15 parts of graphene oxide.
2. film as described in claim 1, which is characterized in that the average-size of aramid nano-fiber is：Diameter 30-40nm,
5-10 μm of length.
3. a kind of preparation method of aramid nano-fiber hybrid film, which is characterized in that include the following steps：
The DMSO dispersion liquids of graphene oxide are blended with the DMSO solution of aramid nano-fiber, stir 1h at room temperature by step 1
More than, wherein in blended liquid, aramid nano-fiber is 100 mass parts, and graphene oxide is 3-15 mass parts；
Step 2, is added deionized water into the blended liquid of step 1, and heating stirring 2 hours or more, then room temperature are aged 2h；
Step 3 obtains gelatinous graphene oxide/aramid nano-fiber composite material, room through solvent is removed by suction filtration under vacuum
It is peeled off from miillpore filter after the lower drying of temperature, is dried in vacuo 6h, the aramid nano-fiber hybrid film is made.
4. preparation method as claimed in claim 3, which is characterized in that in step 2, per 100mL blended liquids in be added 125~
200mL deionized waters.
5. preparation method as claimed in claim 3, which is characterized in that in step 2, be warming up to 80 ± 5 DEG C stirring 2 hours with
On.
6. preparation method as claimed in claim 3, which is characterized in that in step 3, Vacuum filtration device uses sand core funnel
Prepare the miillpore filter of a diameter of 47mm.
7. preparation method as claimed in claim 3, which is characterized in that in step 3, vacuum filtration pressure is -0.1MPa.
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| CN110318112A (en) * | 2019-07-23 | 2019-10-11 | 东华大学 | A kind of high-strength graphene oxide composite fibre of anti-neutron irradiation and preparation method thereof |
| CN110655668A (en) * | 2019-10-25 | 2020-01-07 | 陕西科技大学 | Hydroxyapatite nanowire/ANF composite film and preparation method and application thereof |
| CN113136060A (en) * | 2020-11-16 | 2021-07-20 | 山东理工大学 | Preparation method of aramid nanofiber reinforced sweet sorghum residue composite material |
| CN113416414A (en) * | 2021-07-30 | 2021-09-21 | 湖南大学 | Preparation method and application of aramid nanofiber/porous graphene/polyaniline composition, hydrogel and film with high mechanical strength |
| CN115448691A (en) * | 2022-09-22 | 2022-12-09 | 东莞华贝电子科技有限公司 | Thermal conductive composite film and preparation method thereof |
| CN115851242A (en) * | 2022-11-11 | 2023-03-28 | 四川龙华光电薄膜股份有限公司 | Aramid fiber carbon nano dispersion liquid 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 |
| US12024434B2 (en) | 2021-11-01 | 2024-07-02 | Wisconsin Alumni Research Foundation | Carbon-based composite materials with enhanced dynamic performance |
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| US12024434B2 (en) | 2021-11-01 | 2024-07-02 | Wisconsin Alumni Research Foundation | Carbon-based composite materials with enhanced dynamic performance |
| CN115448691A (en) * | 2022-09-22 | 2022-12-09 | 东莞华贝电子科技有限公司 | Thermal conductive composite film and preparation method thereof |
| 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 |
| CN115851242A (en) * | 2022-11-11 | 2023-03-28 | 四川龙华光电薄膜股份有限公司 | Aramid fiber carbon nano dispersion liquid 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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