CN106629580B - A kind of preparation method of graphite oxide/silicon/carbon dioxide nanotube various dimensions composite nano materials - Google Patents
A kind of preparation method of graphite oxide/silicon/carbon dioxide nanotube various dimensions composite nano materials Download PDFInfo
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- CN106629580B CN106629580B CN201610979669.9A CN201610979669A CN106629580B CN 106629580 B CN106629580 B CN 106629580B CN 201610979669 A CN201610979669 A CN 201610979669A CN 106629580 B CN106629580 B CN 106629580B
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- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a kind of preparation methods of graphite oxide/silicon/carbon dioxide nanotube various dimensions composite nano materials.This method, by the silica of zero dimension, one-dimensional carbon nanotube and two-dimensional graphite oxide Nanocomposites, obtains the composite nanoparticle with various dimensions by isocyanates；Terminal groups modification is carried out to composite nanoparticle, obtains a series of hydrophilic, hydrophobic, super-hydrophobic or even oleophobics, superoleophobic graphite oxide/silicon/carbon dioxide nanotube various dimensions composite nano materials.Graphite oxide obtained/silicon/carbon dioxide nanotube various dimensions composite nano materials can be used for including composite material enhancing, composite material functionalization, surface modification and material waterproofing, anti-corrosion, automatic cleaning coating.
Description
Technical field
The invention belongs to composite nano materials field, more particularly to graphite oxide/silicon/carbon dioxide nanotube various dimensions are multiple
Close nano material and preparation method thereof.
Background technology
Nano-particle have higher specific surface area and excellent performance thus widely paid attention to.From micro-scale
From the point of view of, nano material can be divided into the spheroidal material, one-dimensional rodlike or tubular material and two-dimensional sheet layer material of zero dimension.These three
The material of dimension respectively has its unique performance and different applications.However in certain specific applications various dimensions nanometer material
Material or being used in mixed way for different dimensions nano material tend to bring more excellent performance, or even provide unexpected property
Energy.The research of this aspect is less at present, and mostly being used in mixed way based on different nano-particles.
Nano SiO 2 particle is low cost, high intensity, corrosion-resistant, the good zero-dimension nano particle of biocompatibility,
And its surface is easy hydroxylating, thus there is good hydrophily.Carbon nanotube is a kind of one-dimensional tubulose with high length-diameter ratio
Nano-carbon material can introduce carboxyl and part hydroxyl with good electric conductivity and intensity, and by oxidation modification on its surface
Base.Graphite oxide is a kind of two-dimensional slice stratiform nano-carbon material studied extensively in recent years, it is with good conduction after reduction
And heat conductivility, and there is a large amount of carboxyl and hydroxyls on graphite oxide surface.Therefore, it is possible to use isocyanates is in certain item
These three particles are connected to form the composite nanoparticle with various dimensions structure under part, to make the bonding between particle more
Closely, to be applied to, high filler loading capacity various dimensions are nanometer particle-modified and various dimensions nanoparticle surface coats.
In addition, different chemical reagent can be used to be surface-treated to change the surface of compound particle to compound particle
It can be to improve its compatibility to different matrix material.
Invention content
Present invention offer one kind preparing graphite oxide/silicon/carbon dioxide nanotube various dimensions by isocyanates grafting and answers
The method for closing nano material, and by different surface modifications, assign composite nano materials different surface propertys.
The present invention is received the silica of zero dimension, one-dimensional carbon nanotube and two-dimensional graphene oxide by isocyanates
Rice corpuscles is compound in anhydrous solvent, obtains the composite nanoparticle with various dimensions, and during the reaction according to using need
The nano-particle ratio of regulation and control different dimensions is sought, the composite nano materials with different performance are prepared.
A kind of preparation method of graphite oxide/silicon/carbon dioxide nanotube various dimensions composite nano materials, including walk as follows
Suddenly：
（1）Graphite oxide, silica and carbon nanotube are mixed and are packed into dry three-necked flask, anhydrous solvent is added,
It seals, composite nanoparticle is obtained after ultrasonic disperse；Isocyanates is added, is passed through drying nitrogen, is reacted under heating stirring；
（2）Excessive alcohol or distilled water is added, keeps rotating speed, continues to be stirred to react, composite nanoparticle is modified,
And neutralize the isocyanates not reacted；It is hydrophobic, super-hydrophobic that the addition of monohydric alcohol makes composite nanoparticle surface have, even
Oleophobic, superoleophobic characteristic；And the amino that the addition of distilled water keeps composite nanoparticle Surface Creation hydrophilic, to make composite Nano
Particle can disperse in water, and maintain good reactivity, be suitable for including that surface spraying is modified；
（3）After reaction, solution is transferred in centrifuge tube and is centrifuged, remove supernatant liquor；Ethyl alcohol and ultrasound is added
Dispersion 1 ~ 4 hour, makes small molecule dissolve, centrifuges again, removes supernatant liquor；After repeating 3 ~ 5 times, collection obtains the oxidation stone
Ink/silicon/carbon dioxide nanotube various dimensions composite nano materials.
Further, step（1）In, the mass ratio of the graphite oxide, silica and carbon nanotube is 1:0.5~2:
0.1~2。
Further, step（1）In, the anhydrous solvent is to be suitble to graphite oxide, silica and carbon nanotube point
The polar solvent for dissipating and not reacted with isocyanates, including dimethylformamide or dimethyl sulfoxide.
Further, step（1）In, the time of the ultrasonic disperse is 1 ~ 2 hour.
Further, step（1）In, the isocyanates includes toluene di-isocyanate(TDI), diphenylmethane diisocyanate
Ester, hexamethylene diisocyanate, isophorone diisocyanate or dicyclohexyl methyl hydride diisocyanate.
Further, step（1）In, the addition of the isocyanates be after first isocyanates is dissolved with anhydrous solvent again
It is added；The mass ratio of the isocyanates and composite nanoparticle is 5% ~ 20%.
Further, step（1）In, the rotating speed of the stirring is 500 ~ 1000 r/min.
Further, step（1）In, the temperature of the reaction is 60 ~ 80 DEG C, and the time of reaction is 3 ~ 12 hours.
Further, step（2）In, the alcohol includes Long carbon chain monohydric alcohol, branched alcohol or fluorination monohydric alcohol.
Further, the branched alcohol includes isopropanol, isoamyl alcohol or neopentyl alcohol；The Long carbon chain monohydric alcohol packet
Include n-hexyl alcohol, n-heptanol or n-octyl alcohol；The fluorination monohydric alcohol includes trifluoroethanol, tetrafluoropropanol, hexafluoro butanol, octafluoro penta
Alcohol, ten difluoro enanthol or ten trifluoro octanols.
Further, step（2）In, it is described that continue to be stirred to react reacted 1 ~ 3 hour at 50 ~ 70 DEG C.
Further, step（3）In, the rotating speed of the centrifugation is 4000 ~ 8000 r/min, and centrifugation time is 5 ~ 15min.
Further, step（3）In, the collected mode is vacuum filtration or freeze-drying.
Compared with prior art, the invention has the advantages that and advantageous effect：
The present invention is by isocyanates by the silica of zero dimension, one-dimensional carbon nanotube and two-dimensional graphite oxide nanometer
Particle is compound, obtains the composite nanoparticle with various dimensions, and is obtained by terminal groups modification a series of hydrophilic, hydrophobic, super thin
Water or even oleophobic, superoleophobic various dimensions composite nano materials, can be used for include composite material enhancing, composite material functionalization,
Surface is modified and material waterproofing, anti-corrosion, automatic cleaning coating.
Description of the drawings
Fig. 1 is graphite oxide/silicon/carbon dioxide nanotube various dimensions that the Isopropanol An prepared in embodiment 1 is modified
The transmission electron microscope photo of composite nano materials.
Fig. 2 is graphite oxide/silicon/carbon dioxide nanotube various dimensions that the Isopropanol An prepared in embodiment 1 is modified
The x-ray photoelectron spectroscopy C1s curves of composite nano materials.
Fig. 3 is that graphite oxide/silicon/carbon dioxide nanotube various dimensions of the amino-terminated modification prepared in embodiment 2 are multiple
Close the transmission electron microscope photo of nano material.
Fig. 4 is that graphite oxide/silicon/carbon dioxide nanotube various dimensions of the amino-terminated modification prepared in embodiment 2 are multiple
Close the x-ray photoelectron spectroscopy C1s curves of nano material.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following embodiments.
Embodiment 1
（1）Graphite oxide 50mg, silica 1 00mg, carbon nanotube 50mg are weighed respectively, are packed into three mouthfuls of dry burnings
50mg anhydrous dimethyl formamides are added in bottle, and ultrasound 2 hours, make nano-particle be dispersed in solvent after sealing；By 10mg
Toluene di-isocyanate(TDI) is completely dissolved in 5ml anhydrous dimethyl formamides, is added in three-necked flask；It is passed through into flask dry
Dry nitrogen is heated to 80 DEG C, is stirred to react 8 hours with 500r/min；
（2）After being cooled to 60 DEG C, 10ml isopropanols are added into three-necked flask, continue stirring 2 hours, with to compound particle
It is modified, and neutralizes the toluene di-isocyanate(TDI) not reacted；
（3）Solution after reaction is moved into centrifuge tube, is centrifuged 10 minutes with the rotating speed of 5000r/min, it is clear to remove upper layer
Liquid；Ethyl alcohol is added in centrifuge tube and ultrasonic disperse makes small molecule dissolve, centrifuges again, removes supernatant liquor；It is clear repeatedly
After washing compound particle 3 times, graphite oxide/silicon/carbon dioxide nanotube various dimensions are compound is obtained by the method for vacuum filtration and is received
Rice material.
The transmission electron microscopy of the graphite oxide being prepared/silicon/carbon dioxide nanotube various dimensions composite nano materials
For mirror photo as shown in Figure 1, being connected with each other as seen from Figure 1 by isocyanates after three kinds of particle reactions, formation pattern and scale are rich
The nanoscale of richness, sub-micron particulate.
The water contact angle of the graphite oxide being prepared/silicon/carbon dioxide nanotube various dimensions composite nano materials powder
It is 102 °.
The x-ray photoelectron energy of the graphite oxide being prepared/silicon/carbon dioxide nanotube various dimensions composite nano materials
C1s curves are composed as shown in Fig. 2, the intensity of the particle C-C keys of Isopropanol An is higher as shown in Figure 2, illustrate that particle surface is hydrophobic
The introducing of group.
Embodiment 2
（1）Graphite oxide 50mg, silica 25mg, carbon nanotube 5mg are weighed respectively, are packed into dry three-necked flask,
50mg anhydrous dimethyl sulfoxides are added, ultrasound 1 hour, makes nano-particle be dispersed in solvent after sealing；By 16mg diphenyl
Methane diisocyanate is completely dissolved in 5ml anhydrous dimethyl formamides, is added in three-necked flask；It is passed through into flask dry
Dry nitrogen is heated to 60 DEG C, is stirred to react 3 hours with 1000r/min；
（2）After being cooled to 50 DEG C, 10ml deionized waters are added into three-necked flask, continue stirring 1 hour, with to compound grain
Son is modified, and neutralizes the methyl diphenylene diisocyanate not reacted；
（3）Solution after reaction is moved into centrifuge tube, is centrifuged 15 minutes with the rotating speed of 4000r/min, it is clear to remove upper layer
Liquid；Ethyl alcohol is added in centrifuge tube and ultrasonic disperse makes small molecule dissolve, centrifuges again, removes supernatant liquor；It is clear repeatedly
After washing compound particle 3 times, graphite oxide/silicon/carbon dioxide nanotube various dimensions are compound is obtained by the method for vacuum filtration and is received
Rice material.
The transmission electron microscopy of the graphite oxide being prepared/silicon/carbon dioxide nanotube various dimensions composite nano materials
For mirror photo as shown in figure 3, being connected with each other as seen from Figure 3 by isocyanates after three kinds of particle reactions, formation pattern and scale are rich
The nanoscale of richness, sub-micron particulate.
The water contact angle of the graphite oxide being prepared/silicon/carbon dioxide nanotube various dimensions composite nano materials powder
It is 0 °.
The x-ray photoelectron energy of the graphite oxide being prepared/silicon/carbon dioxide nanotube various dimensions composite nano materials
C1s curves are composed as shown in figure 4, the intensity of amino-terminated particle C-C keys is relatively low as shown in Figure 4, C-N bond strengths increase, and have
CO2Absorption, illustrate the introducing of particle surface hydrophile amino.
Embodiment 3
（1）Graphite oxide 50mg, 00 mg of silica 1,100 mg of carbon nanotube are weighed respectively, are packed into dry three mouthfuls
100 mg anhydrous dimethyl sulfoxides are added in flask, and ultrasound 2 hours, make nano-particle be dispersed in solvent after sealing；By 25
Mg hexamethylene diisocyanates are completely dissolved in 10 ml anhydrous dimethyl formamides, are added in three-necked flask；To flask
It is inside passed through drying nitrogen, is heated to 70 DEG C, is stirred to react 12 hours with 800r/min；
（2）After being cooled to 70 DEG C, 20ml n-hexyl alcohols are added into three-necked flask, continue stirring 3 hours, with to compound particle
It is modified, and neutralizes the hexamethylene diisocyanate not reacted；
（3）Solution after reaction is moved into centrifuge tube, is centrifuged 5 minutes with the rotating speed of 8000r/min, it is clear to remove upper layer
Liquid；Ethyl alcohol is added in centrifuge tube and ultrasonic disperse makes small molecule dissolve, centrifuges again, removes supernatant liquor；It is clear repeatedly
After washing compound particle 3 times, graphite oxide/silicon/carbon dioxide nanotube various dimensions are compound is obtained by the method for vacuum filtration and is received
Rice material.
The graphite oxide being prepared/silicon/carbon dioxide nanotube various dimensions composite nano materials end is n-hexyl,
The water contact angle of powder is 128 °.
Embodiment 4
（1）Graphite oxide 50mg, 25 mg of silica, 5 mg of carbon nanotube are weighed respectively, are packed into three mouthfuls of dry burnings
50 mg anhydrous dimethyl sulfoxides are added in bottle, and ultrasound 1.5 hours, make nano-particle be dispersed in solvent after sealing；8mg is different
Isophorone diisocyanate is completely dissolved in 10 ml anhydrous dimethyl formamides, is added in three-necked flask；Lead into flask
Enter drying nitrogen, be heated to 70 DEG C, is stirred to react 8 hours with 700r/min；
（2）After being cooled to 60 DEG C, 15ml n-octyl alcohols are added into three-necked flask, continue stirring 2 hours, with to compound particle
It is modified, and neutralizes the isophorone diisocyanate not reacted；
（3）Solution after reaction is moved into centrifuge tube, is centrifuged 10 minutes with the rotating speed of 6000r/min, it is clear to remove upper layer
Liquid；Ethyl alcohol is added in centrifuge tube and ultrasonic disperse makes small molecule dissolve, centrifuges again, removes supernatant liquor；It is clear repeatedly
After washing compound particle 3 times, graphite oxide/silicon/carbon dioxide nanotube various dimensions are compound is obtained by the method for vacuum filtration and is received
Rice material.
The graphite oxide being prepared/silicon/carbon dioxide nanotube various dimensions composite nano materials end is n-octyl,
The water contact angle of powder is 146 °.
Embodiment 5
（1）Graphite oxide 50mg, 50 mg of silica, 100 mg of carbon nanotube are weighed respectively, are packed into three mouthfuls of dry burnings
50 mg anhydrous dimethyl formamides are added in bottle, and ultrasound 2 hours, make nano-particle be dispersed in solvent after sealing；By 20
Mg hexamethylene diisocyanates are completely dissolved in 10 ml anhydrous dimethyl formamides, are added in three-necked flask；To flask
It is inside passed through drying nitrogen, is heated to 80 DEG C, is stirred to react 10 hours with 600r/min；
（2）After being cooled to 70 DEG C, ten trifluoro octanols of 15ml are added into three-necked flask, continue stirring 2 hours, with to compound
Particle is modified, and neutralizes the hexamethylene diisocyanate not reacted；
（3）Solution after reaction is moved into centrifuge tube, is centrifuged 10 minutes with the rotating speed of 5000r/min, it is clear to remove upper layer
Liquid；Ethyl alcohol is added in centrifuge tube and ultrasonic disperse makes small molecule dissolve, centrifuges again, removes supernatant liquor；It is clear repeatedly
After washing compound particle 3 times, graphite oxide/silicon/carbon dioxide nanotube various dimensions are compound is obtained by the method for vacuum filtration and is received
Rice material.
The graphite oxide being prepared/silicon/carbon dioxide nanotube various dimensions composite nano materials end is that ten trifluoros are pungent
The water contact angle of base, powder is 159 °.
Claims (5)
1. a kind of preparation method of graphite oxide/silicon/carbon dioxide nanotube various dimensions composite nano materials, which is characterized in that
Include the following steps：
（1）Graphite oxide, silica and carbon nanotube are mixed and are packed into dry three-necked flask, anhydrous solvent is added, is sealed,
Composite nanoparticle is obtained after ultrasonic disperse, the time of the ultrasonic disperse is 1 ~ 2 hour；Isocyanates is added, is passed through drying
Nitrogen reacts under heating stirring；The mass ratio of the graphite oxide, silica and carbon nanotube is 1:0.5~2:0.1~2；Institute
The addition for stating isocyanates is added after isocyanates is first dissolved in the anhydrous solvent；The isocyanates is received with compound
The mass ratio of rice corpuscles is 5% ~ 20%；The rotating speed of the stirring is 500 ~ 1000r/min, and the temperature of the reaction is 60 ~ 80
DEG C, the time of reaction is 3 ~ 12 hours；
（2）It is added excessive alcohol or distilled water, keeps rotating speed, continue to be stirred to react, described to continue to be stirred to react be at 50 ~ 70 DEG C
Under be stirred to react 1 ~ 3 hour；
（3）After reaction, solution is transferred in centrifuge tube and is centrifuged, remove supernatant liquor；Ethyl alcohol and ultrasonic disperse 1 is added
~ 4 hours, small molecule is made to dissolve, centrifuged again, removes supernatant liquor；After repeating 3 ~ 5 times, collection obtains graphite oxide/bis-
Silica/carbon nanotube various dimensions composite nano materials.
2. a kind of system of graphite oxide according to claim 1/silicon/carbon dioxide nanotube various dimensions composite nano materials
Preparation Method, which is characterized in that step（1）In, the anhydrous solvent is to be suitble to graphite oxide, silica and carbon nanotube point
The polar solvent for dissipating and not reacted with isocyanates, including dimethylformamide or dimethyl sulfoxide.
3. a kind of system of graphite oxide according to claim 1/silicon/carbon dioxide nanotube various dimensions composite nano materials
Preparation Method, which is characterized in that step（1）In, the isocyanates includes toluene di-isocyanate(TDI), diphenylmethane diisocyanate
Ester, hexamethylene diisocyanate, isophorone diisocyanate or dicyclohexyl methyl hydride diisocyanate.
4. a kind of system of graphite oxide according to claim 1/silicon/carbon dioxide nanotube various dimensions composite nano materials
Preparation Method, which is characterized in that step（2）In, the alcohol includes Long carbon chain monohydric alcohol, branched alcohol or fluorination monohydric alcohol；
The branched alcohol includes isopropanol, isoamyl alcohol or neopentyl alcohol, and the Long carbon chain monohydric alcohol includes n-hexyl alcohol, n-heptanol or just
Octanol, the fluorination monohydric alcohol include trifluoroethanol, tetrafluoropropanol, hexafluoro butanol, octafluoropentanol, ten difluoro enanthol or ten trifluoros
Octanol.
5. a kind of system of graphite oxide according to claim 1/silicon/carbon dioxide nanotube various dimensions composite nano materials
Preparation Method, which is characterized in that step（3）In, the rotating speed of the centrifugation is 4000 ~ 8000 r/min, centrifugation time is 5 ~
15min；The collected mode is vacuum filtration or freeze-drying.
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| CN110280145B (en) * | 2019-07-02 | 2021-09-14 | 中国科学院宁波材料技术与工程研究所 | Super-hydrophilic-underwater super-oleophobic modified separation membrane, and preparation method and application thereof |
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