CN104262953B - A kind of Graphene coated glass fiber strengthens polymer matrix composites and preparation method - Google Patents
A kind of Graphene coated glass fiber strengthens polymer matrix composites and preparation method Download PDFInfo
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Abstract
The invention provides a kind of Graphene coated glass fiber and strengthen polymer matrix composites, it is prepared via a method which to obtain: first will form finely dispersed aqueous dispersions in water through silane coupler modified graphene dispersion；Again by glass fiber impregnated in the aqueous dispersions of modified graphene, by electrostatic adsorption, form uniform and fine and close Graphene coat at fiberglass surfacing；The last glass fibre with Graphene coat forms composite with resin matrix through composite molding；The present invention constructs Graphene coat at fiberglass surfacing, not only can the interaction area of increased fiber and matrix and interface binding power, can also effectively solve the scattering problem of Graphene, the mechanical property making composite is more excellent, preparation method technique of the present invention is simple simultaneously, with low cost, practicality is good.
Description
(1) technical field
The invention belongs to field of compound material, be specifically related to a kind of Graphene coated glass fiber and strengthen polymer matrix composites and preparation method thereof.
(2) background technology
Graphene (Graphene) is the allotrope that the carbon of discovered in recent years is new, there is the monolayer Two-dimensional Carbon material being bonded with sp2 hybrid orbital by carbon atom, its basic structural unit is most stable of benzene hexatomic ring in organic material, is material the thinnest in the world at present.Graphene is due to its typical two-dimensional structure, and (room temperature electron mobility is up to 200000cm to have excellent electric property2·V-1·S-1), (thermal conductivity reaches 5000W m to thermal property-1·K-1), mechanical performance (Young's modulus is 1100GPa, and fracture strength is 125GPa), and special quantum hall effect and quantum tunneling effect etc..Owing to possessing above-mentioned various performance, Graphene has broad application prospects in field of compound material, obtains the widely studied of lot of domestic and foreign scholar.
At present, the preparation method having been disclosed for graphite alkene composite, such as application number be 201110042410.9 Chinese patent disclose a kind of graphene composite material and preparation method thereof, the method is to obtain silane coupler modified Graphene with silane coupler after first being reacted by Graphene, then obtains graphene composite material with polymer mixed again.Application number is the Chinese patent preparation method that discloses a kind of graphene oxide/CNT modified synergic glass fiber reinforcement epoxy based composites of 201310186014.2, the active function groups on its mechanical property utilizing graphene oxide and CNT excellence itself and surface, it is effectively improved the mechanical property of epoxy resin-base and the interface bond strength of matrix and glass fibre, thus improving the interlaminar shear strength of glass fiber compound material efficiently.Aforementioned published method is all that Graphene is added to reach the performance of modified whole composite in composite system as inorganic nano-filler, and after Graphene is coated in fiberglass surfacing, the method for reinforced composite yet there are no and is disclosed again.
(3) summary of the invention
It is an object of the invention to provide a kind of Graphene coated glass fiber and strengthen polymer matrix composites and preparation method thereof, composite prepared by the inventive method has more excellent mechanical property.
Graphene coated glass fiber of the present invention strengthens polymer matrix composites and is prepared via a method which: first will form finely dispersed aqueous dispersions in water through silane coupler modified graphene dispersion；Again by glass fiber impregnated in the aqueous dispersions of modified graphene, by electrostatic adsorption, form uniform and fine and close Graphene coat at fiberglass surfacing；The last glass fibre with Graphene coat forms composite with resin matrix through composite molding.Owing to Graphene has higher intensity, bigger specific surface area and matsurface, engage each other with resin matrix and form higher interface cohesion, it is possible to significantly improve the bending strength of galss fiber reinforced resin.
The present invention specifically adopts the following technical scheme that
A kind of Graphene coated glass fiber strengthens polymer matrix composites, and described composite is prepared via a method which and obtains:
(1) Graphene and silane coupler react in the mixed solvent of second alcohol and water, reaction products therefrom is first by washing with alcohol, it is washed with water and washs, be 1:5～10 finally by the centrifugal mass ratio obtaining silane coupler modified Graphene, described Graphene and silane coupler；
(2) the silane coupler modified graphene dispersion obtained in step (1) is formed in water aqueous dispersions, then glass fibre is put into dipping in gained aqueous dispersions, after taking-up, prepare the glass fibre of Graphene coating through overbaking；
(3) glass fibre being coated with by the Graphene obtained in step (2) and resin compounded, obtain Graphene coated glass fiber and strengthen polymer matrix composites.
The conventional forming method of the glass fibre of described Graphene coating and Combined Mining this area galss fiber reinforced resin of resin: if thermosetting resin, complex method adopts hand pasting forming method, the advantage of hand pasting forming method is that equipment is simple, and the suitability is wide；If thermoplastic resin, complex method adopts extrusion, injection moulding process.
Graphene coated glass fiber of the present invention strengthens polymer matrix composites, in described preparation method step (1), described silane coupler adopts the one in 4 kinds of types that glass fibre field is the most frequently used, and respectively vinyl type is (such as VTES, vinyltrimethoxy silane, vinyl three tert-butoxy silane, vinyl silane tri-butyl peroxy, vinyltriacetoxy silane etc.), epoxy radicals type is (such as γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane, γ-(2,3-epoxy the third oxygen) propyl-triethoxysilicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane etc.), amine type is (such as gamma-aminopropyl-triethoxy-silane, γ-aminopropyltrimethoxysilane, N-β (aminoethyl)-γ-aminopropyltrimethoxysilane, N-β (aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane, N-β (aminoethyl)-gamma-aminopropyl-triethoxy-silane, N-β (aminoethyl)-γ-aminopropyltriethoxy diethoxy silane, phenylaminomethyl triethoxysilane, phenylaminomethyl trimethoxy silane etc.), or methacryloxy type is (such as γ-methacryloxypropyl trimethoxy silane, vinyl trimethoxy Ethoxysilane etc.) silane coupler.
In described step (1), the mass ratio of described Graphene and silane coupler is preferably 1:7～9.In the mixed solvent of described second alcohol and water, the volume ratio of second alcohol and water can be 0.5～2:1, it is preferred to 1:1.The volumetric usage of described ethanol and water mixed solvent can for 100～300mL/g with the quality meter of Graphene, it is preferred to 150～200mL/g.
Reaction temperature in described step (1) can be 55～70 DEG C, it is preferred to 60 DEG C；Response time can be 20～24h, it is preferred to 24h.
In described step (1), described centrifugal method is: centrifugal 15～20min under the centrifugation rate of 8000～10000r/min.
In the preparation method step (2) of composite of the present invention, described silane coupler modified Graphene mass fraction in aqueous dispersions can be 0.01%～1%, it is preferred to 0.1%～0.8%.
Dip time in described step (2) can be 0.5～2h, it is preferred to 1h.
Baked temperature in described step (2) can be 100～105 DEG C, and baking time is 10～15h.
The present invention specifically recommends described composite to be prepared via a method which and obtain:
(1) Graphene and silane coupler are in the mixed solution of second alcohol and water, 24h is reacted at 60 DEG C, reaction products therefrom, first by washing with alcohol, is washed with water and washs, and finally under the centrifugation rate of 8000～10000r/min, centrifugal 15～20min obtains silane coupler modified Graphene；Described silane coupler is VTES, vinyltrimethoxy silane, vinyl three tert-butoxy silane, vinyl silane tri-butyl peroxy, vinyltriacetoxy silane, γ-(2, 3-epoxy the third oxygen) propyl trimethoxy silicane, γ-(2, 3-epoxy the third oxygen) propyl-triethoxysilicane, β-(3, 4-epoxycyclohexyl) ethyl trimethoxy silane, gamma-aminopropyl-triethoxy-silane, γ-aminopropyltrimethoxysilane, N-β (aminoethyl)-γ-aminopropyltrimethoxysilane, N-β (aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane, N-β (aminoethyl)-gamma-aminopropyl-triethoxy-silane, N-β (aminoethyl)-γ-aminopropyltriethoxy diethoxy silane, phenylaminomethyl triethoxysilane, phenylaminomethyl trimethoxy silane, γ-methacryloxypropyl trimethoxy silane or vinyl trimethoxy Ethoxysilane；The mass ratio of described Graphene and silane coupler is 1:7～9；In the mixed solution of described second alcohol and water, the volume ratio of second alcohol and water is 1:1；The volumetric usage of described ethanol and water mixed solution is calculated as 150～200mL/g with the quality of Graphene；
(2) the silane coupler modified graphene dispersion obtained in step (1) is formed the aqueous dispersions that mass fraction is 0.1%～0.8% in water, again glass fibre is put into dipping 1h in gained aqueous dispersions, at 100～105 DEG C, bake 10～15h after taking-up obtain the glass fibre of Graphene coating；
(3) glass fibre being coated with by the Graphene obtained in step (2) and resin compounded, obtain Graphene coated glass fiber and strengthen polymer matrix composites.
The beneficial effects of the present invention is:
With the composite that the glass fibre of Graphene coat is formed with resin matrix, owing to Graphene has higher intensity, bigger specific surface area and matsurface, to engage each other ability more excellent with resin matrix, thus forming higher interface cohesion, it is possible to significantly improve the bending strength of galss fiber reinforced resin.In the prior art, Graphene is usually used as a kind of composite enhancement component, but the scattering problem of Graphene is never well solved, and eventually results in composite materials property not good.The inventive method constructs Graphene coat at fiberglass surfacing, not only can the interaction area of increased fiber and matrix and interface binding power, moreover it is possible to effectively solving the scattering problem of Graphene, the mechanical property making composite is more excellent.Additionally the present invention adopts the method for modified graphene dispersion to prepare glass fiber compound material, and technique is simple, and with low cost, practicality is good.
(4) Figure of description
In Fig. 1, (a) is the fiberglass surfacing SEM figure being not impregnated with Graphene, and the fiberglass surfacing SEM that (b) is impregnated graphite alkene schemes；
In Fig. 2, the SEM that (c) is glass fibre/PA66 composite section schemes, and the SEM that (d) is Graphene coated glass fiber/PA66 composite section schemes；
In Fig. 3, the SEM that (e) is glass fiber/epoxy composite material section schemes, and the SEM that (f) is Graphene coated glass fiber/epoxy resin composite material section schemes.
(5) detailed description of the invention
Below by specific embodiment, the present invention is further described, but protection scope of the present invention is not limited to that.
Embodiment 1:
1. silane coupler modified Graphene: be dissolved in the mixed solvent of 200mL distilled water and 150mL dehydrated alcohol by 2g graphene powder, forms uniform dispersion after ultrasonic 1h；The dehydrated alcohol that then 50mL contains 15g aminopropyl triethoxysilane (A1100) is added slowly with stirring in the dispersion liquid of aforementioned gained, at 60 DEG C, 24h is reacted after adding, the paste product obtained first uses absolute ethanol washing 3 times, to remove unnecessary A1100, using distilled water wash 3 times again, finally under 8000r/min, centrifugal 15min obtains the modified Graphene 1.5g of A1100.
2. the aqueous dispersions of glass fiber impregnated silane coupler modified Graphene: take the step Graphene 1g that 1. middle gained is silane coupler modified and be scattered in 1000mL distilled water, obtain the silane coupler modified aqueous dispersions that Graphene mass fraction is 0.1%, after ultrasonic 1h, form uniform dispersion.Take 600g short glass fiber to put in the aqueous dispersions of silane coupler modified Graphene and take out after dipping 1h, at 100 DEG C, bake 10h obtain the glass fibre of Graphene coating.
3. glass fibre and PA66 resin compounded: prepare two groups of materials respectively: short glass fiber 500g, PA66 resin 1015g being coated with Graphene is a group；Glass fibre 500g, PA66 resin 1015g of uncoated Graphene is one group.Respectively by the pelletize of above-mentioned two groups of material elder generations, then send in double screw extruder, screw rod shearing and mixing under, material melting, compound, obtain composite batten then through extrusion, cold cut.
4. Compound Material Engineering test: 3. step being extruded the batten obtained and does bending strength test respectively, result is shown in table 1 below.
Table 1 short glass fiber/PA66 composite bending strength
5. after can be seen that coated glass fiber Graphene from upper table, bending strength has been risen to 392.6MPa by 314.3MPa, improve 24.9%, this is because the Graphene being coated in fiberglass surfacing has bigger specific surface area and matsurface, better with engaging of resin matrix, thus causing higher interface cohesion.The SEM of two kinds of composite sections schemes as shown in Figure 2.
Embodiment 2:
1. silane coupler modified Graphene: be dissolved in the mixed solvent of 200mL distilled water and 150mL dehydrated alcohol by 2g graphene powder, forms uniform dispersion after ultrasonic 1h；The dehydrated alcohol that then 50mL contains 15g aminopropyl triethoxysilane (A187) is added slowly with stirring in the dispersion liquid of aforementioned gained, at 60 DEG C, 24h is reacted after adding, the paste product obtained first uses absolute ethanol washing 3 times, to remove unnecessary A187, using distilled water wash 3 times again, finally under 8000r/min, centrifugal 15min obtains the modified Graphene 1.5g of A187.
2. the aqueous dispersions of glass fiber impregnated silane coupler modified Graphene: take the step Graphene 1g that 1. middle gained is silane coupler modified and be scattered in 1000mL distilled water, obtain the silane coupler modified aqueous dispersions that Graphene mass fraction is 0.1%, after ultrasonic 1h, form uniform dispersion.Finally equirotal (10cm × 20cm) the glass fibre woven roving cut is put into and take out after the aqueous dispersions of silane coupler modified Graphene impregnates 1h, notice that woven roving is to hang dipping, identical method impregnates 20, then bakes 10h at 100 DEG C and obtains the glass fibre woven roving of Graphene coating.
3. glass fibre woven roving and epoxy resin compound: take the glass fibre woven roving of Graphene coating and each 20 of the glass fibre woven roving of uncoated Graphene, after 1333g epoxy resin adds 325gIPD firming agent, obtain two kinds of composite products by hand pasting forming method.
4. Compound Material Engineering test: according to standard ISO178, step 3. two kinds of composites of gained are cut into batten, finally does bending strength test.Result is shown in table 1 below.
Table 2 woven rovings/epoxy resin composite material bending strength
5., after can be seen that glass fibre woven roving is graphene coated from upper table, warp-wise bending strength improves 21.2%, and the bending strength in broadwise too increases 20.8%.This is because the Graphene being coated in fiberglass surfacing has bigger specific surface area and matsurface, better with engaging of resin matrix, thus forming higher interface cohesion.The SEM of two kinds of composite sections schemes as shown in Figure 3.
Claims (10)
1. a Graphene coated glass fiber strengthens polymer matrix composites, it is characterised in that described composite is prepared via a method which and obtains:
(1) Graphene and silane coupler react in the mixed solvent of second alcohol and water, reaction products therefrom is first by washing with alcohol, it is washed with water and washs, be 1:5～10 finally by the centrifugal mass ratio obtaining silane coupler modified Graphene, described Graphene and silane coupler；
(2) the silane coupler modified graphene dispersion obtained in step (1) is formed in water aqueous dispersions, then glass fibre is put into dipping in gained aqueous dispersions, after taking-up, prepare the glass fibre of Graphene coating through overbaking；
(3) glass fibre being coated with by the Graphene obtained in step (2) and resin compounded, obtain Graphene coated glass fiber and strengthen polymer matrix composites.
2. Graphene coated glass fiber as claimed in claim 1 strengthens polymer matrix composites, it is characterized in that, in described step (1), described silane coupler is the silane coupler of vinyl type, epoxy radicals type, amine type or methacryloxy type.
3. Graphene coated glass fiber as claimed in claim 2 strengthens polymer matrix composites, it is characterised in that in described step (1), described silane coupler is VTES, vinyltrimethoxy silane, vinyl three tert-butoxy silane, vinyl silane tri-butyl peroxy, vinyltriacetoxy silane, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane, γ-(2,3-epoxy the third oxygen) propyl-triethoxysilicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, gamma-aminopropyl-triethoxy-silane, γ-aminopropyltrimethoxysilane, N-β (aminoethyl)-γ-aminopropyltrimethoxysilane, N-β (aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane, N-β (aminoethyl)-gamma-aminopropyl-triethoxy-silane, N-β (aminoethyl)-γ-aminopropyltriethoxy diethoxy silane, phenylaminomethyl triethoxysilane, phenylaminomethyl trimethoxy silane, γ-methacryloxypropyl trimethoxy silane or vinyl trimethoxy Ethoxysilane.
4. Graphene coated glass fiber as claimed in claim 1 strengthens polymer matrix composites, it is characterised in that in described step (1), in the mixed solvent of described second alcohol and water, the volume ratio of second alcohol and water is 0.5～2:1；The volumetric usage of described ethanol and water mixed solvent is calculated as 100～300mL/g with the quality of Graphene.
5. Graphene coated glass fiber as claimed in claim 1 strengthens polymer matrix composites, it is characterised in that the reaction temperature in described step (1) is 55～70 DEG C, and the response time is 20～24h.
6. Graphene coated glass fiber as claimed in claim 1 strengthens polymer matrix composites, it is characterised in that in described step (1), described centrifugal method is: centrifugal 15～20min under the centrifugation rate of 8000～10000r/min.
7. Graphene coated glass fiber as claimed in claim 1 strengthens polymer matrix composites, it is characterised in that in described step (2), described silane coupler modified Graphene mass fraction in aqueous dispersions is 0.01%～1%.
8. Graphene coated glass fiber as claimed in claim 1 strengthens polymer matrix composites, it is characterised in that the dip time in described step (2) is 0.5～2h.
9. Graphene coated glass fiber as claimed in claim 1 strengthens polymer matrix composites, it is characterised in that the baked temperature in described step (2) is 100～105 DEG C, and baking time is 10～15h.
10. Graphene coated glass fiber as claimed in claim 1 strengthens polymer matrix composites, it is characterised in that described composite is prepared via a method which and obtains:
(1) Graphene and silane coupler react in the mixed solution of second alcohol and water, 20～24h is reacted at 55～70 DEG C, reaction products therefrom is first by washing with alcohol, it is washed with water and washs, last 15～the 20min that is centrifuged under the centrifugation rate of 8000～10000r/min obtains silane coupler modified Graphene, and described silane coupler is the one in vinyl type, epoxy radicals type, amine type or methacryloxy type；The mass ratio of described Graphene and silane coupler is 1:5～10；In the mixed solvent of described second alcohol and water, the volume ratio of second alcohol and water is 0.5～2:1；The volumetric usage of described ethanol and water mixed solvent is calculated as 100～300mL/g with the quality of Graphene；
(2) the silane coupler modified graphene dispersion obtained in step (1) is formed the aqueous dispersions that mass fraction is 0.01%～1% in water, again glass fibre is put into dipping 0.5～2h in gained aqueous dispersions, at 100～105 DEG C, bake 10～15h after taking-up obtain the glass fibre of Graphene coating；
(3) glass fibre being coated with by the Graphene obtained in step (2) and resin compounded, obtain Graphene coated glass fiber and strengthen polymer matrix composites.
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| GB0710425D0 (en) * | 2007-06-01 | 2007-07-11 | Hexcel Composites Ltd | Improved structural adhesive materials |
| CN102153877B (en) * | 2011-02-22 | 2013-05-01 | 中国科学技术大学 | Graphene composite material and preparation method thereof |
| CN102343239B (en) * | 2011-05-20 | 2013-05-29 | 四川大学 | Oxidized graphene or graphene/inorganic particle core/shell material and preparation method thereof |
| KR20130049444A (en) * | 2011-11-04 | 2013-05-14 | 현대자동차주식회사 | Preparing method for polymer composite coated carbon nano material |
| CN103788413B (en) * | 2014-01-24 | 2015-12-02 | 济南大学 | The method of graphene oxide chemically modified mineral filler, products obtained therefrom and application |
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| CN106977882A (en) * | 2017-05-08 | 2017-07-25 | 北京化工大学 | A kind of heat-conductive composite material and preparation method thereof |
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