CN106629580A - Preparation method of graphite oxide/silicon dioxide/carbon nanotube multi-dimension composite nanomaterial - Google Patents
Preparation method of graphite oxide/silicon dioxide/carbon nanotube multi-dimension composite nanomaterial Download PDFInfo
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- CN106629580A CN106629580A CN201610979669.9A CN201610979669A CN106629580A CN 106629580 A CN106629580 A CN 106629580A CN 201610979669 A CN201610979669 A CN 201610979669A CN 106629580 A CN106629580 A CN 106629580A
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- graphite oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a preparation method of a graphite oxide/silicon dioxide/carbon nanotube multi-dimension composite nanomaterial. The method comprises the following steps: compounding zero-dimension silicon dioxide, one-dimension carbon nanotube and two-dimension graphite oxide nanoparticles through isocyanate to obtain multi-dimension composite nanoparticles; performing terminal group modification on the composite nanoparticles to obtain a series of hydrophilic, hydrophobic, super-hydrophobic, even oleophobic and super-oleophobic graphite oxide/silicon dioxide/carbon nanotube multi-dimension composite nanomaterials. The obtained graphite oxide/silicon dioxide/carbon nanotube multi-dimension composite nanomaterials can be applied to composite material enhancement, composite material functionalization, surface modification, material waterproofness, corrosion prevention and self-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
Nanoparticle have higher specific surface area and excellent performance thus widely paid attention to.From on micro-scale
From the point of view of, nano material can be divided into the sheet layer material of the spheroidal material, one-dimensional bar-shaped or tubular material and two dimension of zero dimension.These three
The material of dimension each has its unique performance and different applications.But in some application-specifics 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.At present the research of this aspect is less, and many being used in mixed way based on different nanoparticles.
Nano SiO 2 particle is the good zero-dimension nano particle of low cost, high intensity, corrosion-resistant, biocompatibility,
And the easy hydroxylating in its surface, thus with good hydrophilic.CNT is a kind of one-dimensional tubulose with high length-diameter ratio
Nano-carbon material, it has good electric conductivity and intensity, and can introduce carboxyl and part hydroxyl on its surface by oxidation modification
Base.Graphite oxide is a kind of two-dimensional slice stratiform nano-carbon material widely studied in recent years, and it has good conduction after reduction
And heat conductivility, and graphite oxide surface has substantial amounts of carboxyl and hydroxyl.Therefore, it is possible to use isocyanates are in certain bar
Under part these three particles are connected to form the composite nanoparticle with various dimensions structure, so that the bonding between particle is more
Closely, it is nanometer particle-modified to be applied to high filler loading capacity various dimensions, and the coating of various dimensions nanoparticle surface.
In addition, can be surface-treated to compound particle so as to change the surface of compound particle using different chemical reagent
Can be improving its compatibility to different matrix material.
The content of the invention
Present invention offer one kind prepares graphite oxide/silicon/carbon dioxide nanotube various dimensions and answers by isocyanates grafting
The method for closing nano material, and by different surface modifications, give composite nano materials different surface propertys.
The present invention by isocyanates by the silicon dioxide of zero dimension, receive by one-dimensional CNT and the graphene oxide of two dimension
Rice corpuscles are combined in anhydrous solvent, obtain the composite nanoparticle with various dimensions, and during the course of the reaction according to applying need
The nanoparticle ratio of regulation and control different dimensions is sought, the composite nano materials with different performance are prepared.
The preparation method of a kind of graphite oxide/silicon/carbon dioxide nanotube various dimensions composite nano materials, including following step
Suddenly:
(1)Graphite oxide, silicon dioxide and CNT are mixed and load dry there-necked flask, add anhydrous solvent, sealed,
Composite nanoparticle is obtained after ultrasonic disperse;Isocyanates are added, drying nitrogen is passed through, is reacted under heated and stirred;
(2)Excessive alcohol or distilled water is added, rotating speed is kept, continues stirring reaction, composite nanoparticle is modified, and in
The isocyanates not reacted;It is hydrophobic, super-hydrophobic that the addition of monohydric alcohol has composite nanoparticle surface, or even dredges
Oily, superoleophobic characteristic;And the addition of distilled water makes the hydrophilic amino of composite nanoparticle Surface Creation, so that composite nano-granule
Son can disperse in water, and maintain good reactivity, it is adaptable to modified including surface spraying;
(3)After reaction terminates, solution is proceeded in centrifuge tube and is centrifuged, remove the supernatant;Add ethanol and ultrasonic disperse 1
~ 4 hours, dissolve small molecule, recentrifuge removes the supernatant;After repeating 3 ~ 5 times, collection obtains graphite oxide/bis-
Silicon oxide/CNT various dimensions composite nano materials.
Further, step(1)In, the mass ratio of the graphite oxide, silicon dioxide and CNT is 1:0.5~2:
0.1~2。
Further, step(1)In, the anhydrous solvent divides to be adapted to graphite oxide, silicon dioxide and CNT
The polar solvent for dissipating and not reacting 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 include 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 first by after the dissolving of isocyanates anhydrous solvent again
Add;The isocyanates are 5% ~ 20% with the mass ratio of composite nanoparticle.
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, described 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 bag
Include hexanol, n-heptanol or n-octyl alcohol;The fluorination monohydric alcohol includes trifluoroethanol, C3-Fluoroalcohol., hexafluoro butanol, octafluoro penta
Alcohol, ten difluoro enanthol or ten trifluoro capryl alcohol.
Further, step(2)In, the continuation stirring reaction is 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 mode of the collection is vacuum filtration or lyophilization.
Compared with prior art, the invention has the advantages that and beneficial effect:
The present invention passes through isocyanates by the graphite oxide nanoparticle of the silicon dioxide of zero dimension, one-dimensional CNT and two dimension
It is compound, the composite nanoparticle with various dimensions is obtained, and obtain a series of hydrophilic, hydrophobic, super-hydrophobic by terminal groups modification, very
To oleophobic, superoleophobic various dimensions composite nano materials, can be used to include composite enhancing, composite functionalization, surface
Modified and material waterproofing, anti-corrosion, automatic cleaning coating.
Description of the drawings
Fig. 1 is the modified graphite oxide/silicon/carbon dioxide nanotube various dimensions of the Isopropanol An prepared in embodiment 1
The transmission electron microscope photo of composite nano materials.
Fig. 2 is the modified graphite oxide/silicon/carbon dioxide nanotube various dimensions of the Isopropanol An prepared in embodiment 1
The x-ray photoelectron power spectrum C1s curve of composite nano materials.
Fig. 3 is that the amino-terminated modified graphite oxide/silicon/carbon dioxide nanotube various dimensions prepared in embodiment 2 are answered
Close the transmission electron microscope photo of nano material.
Fig. 4 is that the amino-terminated modified graphite oxide/silicon/carbon dioxide nanotube various dimensions prepared in embodiment 2 are answered
Close the x-ray photoelectron power spectrum C1s curve of nano material.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the invention is not restricted to following examples.
Embodiment 1
(1)Graphite oxide 50mg, silica 1 00mg, CNT 50mg are weighed respectively, load dry there-necked flask, plus
Enter 50mg anhydrous dimethyl formamides, ultrasound 2 hours, make nanoparticle be dispersed in solvent after sealing;By 10mg toluene
Diisocyanate is completely dissolved in 5ml anhydrous dimethyl formamides, in adding there-necked flask;Dry nitrogen is passed through into flask
Gas, was heated to 80 DEG C, with 500r/min stirring reactions 8 hours;
(2)After being cooled to 60 DEG C, 10ml isopropanols are added in there-necked flask, continue to stir 2 hours, to carry out compound particle
It is modified, and the toluene di-isocyanate(TDI) that neutralization does not react;
(3)Reacted solution is moved in centrifuge tube, is centrifuged 10 minutes with the rotating speed of 5000r/min, remove the supernatant;
Ethanol is added in centrifuge tube and ultrasonic disperse dissolves small molecule, recentrifuge, remove the supernatant;So clean repeatedly compound
After particle 3 times, graphite oxide/silicon/carbon dioxide nanotube various dimensions composite nano materials are obtained by the method for vacuum filtration.
The transmission electron microscopy of the graphite oxide for preparing/silicon/carbon dioxide nanotube various dimensions composite nano materials
Mirror photo by isocyanates after three kinds of particle reactions as shown in figure 1, be connected with each other as seen from Figure 1, formation pattern and yardstick are rich
Rich nanoscale, sub-micron particulate.
The water contact angle of the graphite oxide for preparing/silicon/carbon dioxide nanotube various dimensions composite nano materials powder
For 102 °.
The x-ray photoelectron energy of the graphite oxide for preparing/silicon/carbon dioxide nanotube various dimensions composite nano materials
Spectrum C1s curves illustrate that particle surface is hydrophobic as shown in Fig. 2 as shown in Figure 2 the intensity of the particle C-C keys of Isopropanol An is higher
The introducing of group.
Embodiment 2
(1)Graphite oxide 50mg, silicon dioxide 25mg, CNT 5mg are weighed respectively, loads dry there-necked flask, add
50mg anhydrous dimethyl sulfoxides, ultrasound 1 hour, makes nanoparticle be dispersed in solvent after sealing;By 16mg diphenyl methanes
Diisocyanate is completely dissolved in 5ml anhydrous dimethyl formamides, in adding there-necked flask;Dry nitrogen is passed through into flask
Gas, was heated to 60 DEG C, with 1000r/min stirring reactions 3 hours;
(2)After being cooled to 50 DEG C, 10ml deionized waters are added in there-necked flask, continue to stir 1 hour, to enter compound particle
Row is modified, and the methyl diphenylene diisocyanate that neutralization does not react;
(3)Reacted solution is moved in centrifuge tube, is centrifuged 15 minutes with the rotating speed of 4000r/min, remove the supernatant;
Ethanol is added in centrifuge tube and ultrasonic disperse dissolves small molecule, recentrifuge, remove the supernatant;So clean repeatedly compound
After particle 3 times, graphite oxide/silicon/carbon dioxide nanotube various dimensions composite nano materials are obtained by the method for vacuum filtration.
The transmission electron microscopy of the graphite oxide for preparing/silicon/carbon dioxide nanotube various dimensions composite nano materials
Mirror photo by isocyanates after three kinds of particle reactions as shown in figure 3, be connected with each other as seen from Figure 3, formation pattern and yardstick are rich
Rich nanoscale, sub-micron particulate.
The water contact angle of the graphite oxide for preparing/silicon/carbon dioxide nanotube various dimensions composite nano materials powder
For 0 °.
The x-ray photoelectron energy of the graphite oxide for preparing/silicon/carbon dioxide nanotube various dimensions composite nano materials
As shown in figure 4, the intensity of particle C-C keys amino-terminated as shown in Figure 4 is relatively low, C-N bond strengths are raised spectrum C1s curves, and are had
CO2Absorption, illustrate the introducing of particle surface hydrophile amino.
Embodiment 3
(1)Graphite oxide 50mg, the mg of silica 1 00, the mg of CNT 100 are weighed respectively, load dry there-necked flask,
100 mg anhydrous dimethyl sulfoxides are added, ultrasound 2 hours, make nanoparticle be dispersed in solvent after sealing;25 mg six are sub-
Methyl diisocyanate is completely dissolved in 10 ml anhydrous dimethyl formamides, in adding there-necked flask;It is passed through into flask
Drying nitrogen, was heated to 70 DEG C, with 800r/min stirring reactions 12 hours;
(2)After being cooled to 70 DEG C, 20ml hexanol is added in there-necked flask, continue to stir 3 hours, to carry out compound particle
It is modified, and the hexamethylene diisocyanate that neutralization does not react;
(3)Reacted solution is moved in centrifuge tube, is centrifuged 5 minutes with the rotating speed of 8000r/min, remove the supernatant;
Ethanol is added in centrifuge tube and ultrasonic disperse dissolves small molecule, recentrifuge, remove the supernatant;So clean repeatedly compound
After particle 3 times, graphite oxide/silicon/carbon dioxide nanotube various dimensions composite nano materials are obtained by the method for vacuum filtration.
The graphite oxide for preparing/silicon/carbon dioxide nanotube various dimensions composite nano materials end is n-hexyl, its
The water contact angle of powder is 128 °.
Embodiment 4
(1)Graphite oxide 50mg, the mg of silicon dioxide 25, the mg of CNT 5 are weighed respectively, load dry there-necked flask, plus
Enter 50 mg anhydrous dimethyl sulfoxides, ultrasound 1.5 hours, make nanoparticle be dispersed in solvent after sealing;By the different Fo Er of 8mg
Ketone diisocyanate is completely dissolved in 10 ml anhydrous dimethyl formamides, in adding there-necked flask;It is passed through into flask dry
Dry nitrogen, was heated to 70 DEG C, with 700r/min stirring reactions 8 hours;
(2)After being cooled to 60 DEG C, 15ml n-octyl alcohols are added in there-necked flask, continue to stir 2 hours, to carry out compound particle
It is modified, and the isophorone diisocyanate that neutralization does not react;
(3)Reacted solution is moved in centrifuge tube, is centrifuged 10 minutes with the rotating speed of 6000r/min, remove the supernatant;
Ethanol is added in centrifuge tube and ultrasonic disperse dissolves small molecule, recentrifuge, remove the supernatant;So clean repeatedly compound
After particle 3 times, graphite oxide/silicon/carbon dioxide nanotube various dimensions composite nano materials are obtained by the method for vacuum filtration.
The graphite oxide for preparing/silicon/carbon dioxide nanotube various dimensions composite nano materials end is n-octyl, its
The water contact angle of powder is 146 °.
Embodiment 5
(1)Graphite oxide 50mg, the mg of silicon dioxide 50, the mg of CNT 100 are weighed respectively, load dry there-necked flask,
50 mg anhydrous dimethyl formamides are added, ultrasound 2 hours, make nanoparticle be dispersed in solvent after sealing;By 20 mg
Hexamethylene diisocyanate is completely dissolved in 10 ml anhydrous dimethyl formamides, in adding there-necked flask;Into flask
Drying nitrogen is passed through, 80 DEG C are heated to, with 600r/min stirring reactions 10 hours;
(2)After being cooled to 70 DEG C, the trifluoro capryl alcohol of 15ml ten is added in there-necked flask, continue to stir 2 hours, with to compound particle
It is modified, and the hexamethylene diisocyanate that neutralization does not react;
(3)Reacted solution is moved in centrifuge tube, is centrifuged 10 minutes with the rotating speed of 5000r/min, remove the supernatant;
Ethanol is added in centrifuge tube and ultrasonic disperse dissolves small molecule, recentrifuge, remove the supernatant;So clean repeatedly compound
After particle 3 times, graphite oxide/silicon/carbon dioxide nanotube various dimensions composite nano materials are obtained by the method for vacuum filtration.
The graphite oxide for preparing/silicon/carbon dioxide nanotube various dimensions composite nano materials end is that ten trifluoros are pungent
Base, the water contact angle of its powder is 159 °.
Claims (10)
1. the preparation method of a kind of graphite oxide/silicon/carbon dioxide nanotube various dimensions composite nano materials, it is characterised in that
Comprise the steps:
(1)Graphite oxide, silicon dioxide and CNT are mixed and load dry there-necked flask, add anhydrous solvent, sealed,
Composite nanoparticle is obtained after ultrasonic disperse;Isocyanates are added, drying nitrogen is passed through, is reacted under heated and stirred;
(2)Excessive alcohol or distilled water is added, rotating speed is kept, continues stirring reaction, composite nanoparticle is modified, and in
The isocyanates not reacted;
(3)After reaction terminates, solution is proceeded in centrifuge tube and is centrifuged, remove the supernatant;Add ethanol and ultrasonic disperse 1
~ 4 hours, dissolve small molecule, recentrifuge removes the supernatant;After repeating 3 ~ 5 times, collection obtains graphite oxide/bis-
Silicon oxide/CNT various dimensions composite nano materials.
2. the system of a kind of graphite oxide according to claim 1/silicon/carbon dioxide nanotube various dimensions composite nano materials
Preparation Method, it is characterised in that step(1)In, the mass ratio of the graphite oxide, silicon dioxide and CNT is 1:0.5~2:
0.1~2。
3. the system of a kind of graphite oxide according to claim 1/silicon/carbon dioxide nanotube various dimensions composite nano materials
Preparation Method, it is characterised in that step(1)In, the anhydrous solvent divides to be adapted to graphite oxide, silicon dioxide and CNT
The polar solvent for dissipating and not reacting with isocyanates, including dimethylformamide or dimethyl sulfoxide.
4. the system of a kind of graphite oxide according to claim 1/silicon/carbon dioxide nanotube various dimensions composite nano materials
Preparation Method, it is characterised in that step(1)In, the time of the ultrasonic disperse is 1 ~ 2 hour.
5. the system of a kind of graphite oxide according to claim 1/silicon/carbon dioxide nanotube various dimensions composite nano materials
Preparation Method, it is characterised in that step(1)In, the isocyanates include toluene di-isocyanate(TDI), diphenylmethane diisocyanate
Ester, hexamethylene diisocyanate, isophorone diisocyanate or dicyclohexyl methyl hydride diisocyanate.
6. the system of a kind of graphite oxide according to claim 1/silicon/carbon dioxide nanotube various dimensions composite nano materials
Preparation Method, it is characterised in that step(1)In, the addition of the isocyanates is first by after the dissolving of isocyanates anhydrous solvent
Add;The isocyanates are 5% ~ 20% with the mass ratio of composite nanoparticle.
7. the system of a kind of graphite oxide according to claim 1/silicon/carbon dioxide nanotube various dimensions composite nano materials
Preparation Method, it is characterised in that step(1)In, the rotating speed of the stirring be the temperature reacted described in 500 ~ 1000r/min be 60 ~
80 DEG C, the time of reaction is 3 ~ 12 hours.
8. the system of a kind of graphite oxide according to claim 1/silicon/carbon dioxide nanotube various dimensions composite nano materials
Preparation Method, it is characterised in that step(2)In, described 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 hexanol, n-heptanol or just
Capryl alcohol, the fluorination monohydric alcohol includes trifluoroethanol, C3-Fluoroalcohol., hexafluoro butanol, octafluoropentanol, ten difluoro enanthol or ten trifluoros
Capryl alcohol.
9. the system of a kind of graphite oxide according to claim 1/silicon/carbon dioxide nanotube various dimensions composite nano materials
Preparation Method, it is characterised in that step(2)In, the continuation stirring reaction is stirring reaction 1 ~ 3 hour at 50 ~ 70 DEG C.
10. a kind of graphite oxide according to claim 1/silicon/carbon dioxide nanotube various dimensions composite nano materials
Preparation method, it is characterised in that step(3)In, the rotating speed of the centrifugation is 4000 ~ 8000 r/min, centrifugation time is 5 ~
15min;The mode of the collection is vacuum filtration or lyophilization.
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