CN107216486A - A kind of nano hybridization filler of surface of graphene oxide growth in situ silica and preparation method thereof - Google Patents
A kind of nano hybridization filler of surface of graphene oxide growth in situ silica and preparation method thereof Download PDFInfo
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- CN107216486A CN107216486A CN201710511497.7A CN201710511497A CN107216486A CN 107216486 A CN107216486 A CN 107216486A CN 201710511497 A CN201710511497 A CN 201710511497A CN 107216486 A CN107216486 A CN 107216486A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of nano hybridization filler of surface of graphene oxide growth in situ silica and preparation method thereof.This method is first by graphene oxide ultrasonic disperse into water and ethanol, then ammoniacal liquor and catalyst are added, and silicon source monomer is slowly added dropwise, stirring reaction 28 hours at 30 80 DEG C, it is scrubbed, dry, obtain nano hybridization filler of the silicon dioxide granule homoepitaxial in surface of graphene oxide.The nano hybridization filler surface is the nanometer projection formed by silicon dioxide granule, the stacking between graphene oxide layer can be prevented, the specific surface area of hydridization filler can be improved again, be expected to significantly improve the interface interaction between dispersity and polymer hybrid filler of the hydridization filler in polymeric matrix.Therefore, the present invention is respectively provided with potential application value in the preparation field of functionalization filler and high-performance composite materials.
Description
Technical field
The present invention relates to the preparing technical field of material, and in particular to a kind of surface of graphene oxide growth in situ titanium dioxide
Nano hybridization filler of silicon and preparation method thereof.
Background technology
With continuing to develop for material science, led with high-performance and multifunctional nano hybrid material in scientific research and engineering
Domain all obtains extensive concern, and the development of polymer composite is even more the extensive use for be unableing to do without Nano filling.Nanometer
The addition of filler, is not only able to significantly reduce the cost of polymer composite, moreover it is possible to effectively improve mechanical strength, the heat of material
The performances such as stability, heat conduction, conduction.Common Nano filling can be divided into 1-dimention nano filler according to its geometry（Carbon nanometer
Pipe, halloysite nanotubes etc.）, two-dimensional nano filler（Such as graphene, montmorillonite）With three-dimensional manometer particle（Such as silica
Deng）.Generally, the geometry and architectural feature of Nano filling have very big shadow to the final performance of composite
Ring.Compared with single Nano filling, by receiving that the filler of different nanometer dimensions is combined together by physically or chemically acting on
Rice hydridization filler is to the lifting of polymer composites performance with more excellent synergy.
Graphene is a kind of two-dimentional conjugated structure nano material being made up of single layer of carbon atom, mechanics and pole with superelevation
The characteristics such as good heat conduction, conduction.Based on its unique chemical constitution and excellent combination property, graphene is in new energy, biology
The fields such as science and technology, new material obtain extensive concern and applied.Compared with graphene, graphene oxide is contained due to its surface
The oxy radicals such as abundant hydroxyl, carboxyl, epoxy radicals, it is easy to carry out chemical bond with other materials.The present invention utilizes silicon source
Monomer carries out sol gel reaction on the surface of graphene oxide, by chemical bond one on the area load of graphene oxide
Layer Nano particles of silicon dioxide.This method is simple to operate, convenient post-treatment, it is easy to accomplish industrialization, and the graphite oxide obtained
Alkene-silica（GO-SiO2）It is that, by chemical bonds, therefore silica dioxide granule will not be rear between nano hybridization filler
Come off in continuous polymer processing from graphene oxide, there is very big potential application in polymer composites field
Value.
The content of the invention
It is an object of the invention to the method using easy growth in situ, in the Surface Creation nanometer two of graphene oxide
Silica, prepares a kind of nano hybridization filler.In this hydridization filler, silica is by chemical bonds in oxidation stone
The surface of black alkene.The unique architectural feature of hydridization filler, can prevent the stacking between graphene oxide layer（Silicon dioxide granule
Buffer action）With the reunion of silicon dioxide granule（Homoepitaxial promotes hydridization filler in polymer in surface of graphene oxide
It is dispersed in matrix）, the specific surface area of filler can be significantly increased again, strengthen the interface cohesion between polymer, in addition,
GO-SiO2Substantial amounts of hydroxyl is contained on nano hybridization filler surface, to realize that the functional modification of filler provides feasibility.
The present invention is achieved through the following technical solutions.
A kind of method that surface of graphene oxide growth in situ silica prepares nano hybridization filler, including following step
Suddenly：
（1）Ultrasonic disperse in water is added graphene oxide into, ethanol is added, graphene oxide dispersion is obtained；
（2）To step（1）Ammoniacal liquor and catalyst, then ultrasonic disperse are added in gained graphene oxide dispersion, mixed liquor is obtained；
（3）At 30-80 DEG C, to step（2）Silicon source monomer, stirring reaction are added dropwise in gained mixed liquor；
（4）By step（3）Products therefrom washing, drying, the nanometer for obtaining surface of graphene oxide growth in situ silica are miscellaneous
Change filler, labeled as GO-SiO2Nano hybridization filler.
It is preferred that, step（1）The graphene oxide is prepared using existing modified Hummer methods.
It is preferred that, step（1）The time of the ultrasonic disperse is 2h.
It is preferred that, step（1）Described water is deionized water, and described ethanol is absolute ethyl alcohol；The water and ethanol
Volume ratio is 1:1.
It is preferred that, step（1）The solid content of the graphene oxide dispersion is 0.01%-0.1%.
It is preferred that, step（2）In, to step（1）Added in gained graphene oxide dispersion after ammoniacal liquor, ultrasonic disperse,
Add catalyst.
It is preferred that, step（2）The ultrasonic time is 1h.
It is preferred that, step（2）The catalyst is Bis(lauroyloxy)dioctyltin, dibutyl tin laurate and the tetrabutyl
One or more of ammonium bromide；The addition of the catalyst is 5-15mg, more preferably 5-10mg.
It is preferred that, step（2）The addition of the ammoniacal liquor is 5-15ml.
It is preferred that, step（3）The silicon source monomer is one kind in methyl silicate, tetraethyl orthosilicate and sodium metasilicate.
It is preferred that, step（3）The time of the stirring reaction is 2-8h, more preferably 4-6 hours.
It is preferred that, step（3）The silicon source monomer accounts for the 400wt%-640 wt% of graphene oxide.
It is preferred that, step（3）The middle speed that silicon source monomer is added dropwise is 3-10 drops/sec.
A kind of nano hybridization filler as made from the process described above.
The present invention is by sol-gal process, using silicon source monomer hydrolytic condensation in one layer of surface of graphene oxide growth in situ
Nano-silicon dioxide particle.
Compared with prior art, the present invention has the advantage that and characteristic：
（1）GO-SiO prepared by the present invention2The surface of nano hybridization filler is the nanometer projection formed by silicon dioxide granule, both
The stacking between graphene oxide layer can be prevented, the specific surface area of hydridization filler can be improved again, can be formed with polymeric matrix
Stronger interface cohesion effect, and there are many active groups on surface, and the further modification and functionalization for filler provide base
Plinth.
（2）The GO-SiO that the present invention is prepared using growth in situ2Nano hybridization filler realizes graphene oxide and dioxy
The chemical bonds of SiClx, it is to avoid occur coming off for silicon dioxide granule in follow-up polymer processing, are expanded
The application of the nano hybridization filler.
（3）Operation is simple and feasible for the preparation method of the present invention, it is not necessary to complicated preparation process and post-processing step, favorably
In realizing industrialization.
Brief description of the drawings
Fig. 1 a, Fig. 1 b be respectively in embodiment 1 graphene oxide and surface of graphene oxide growth in situ silica receive
The TEM figures of rice hydridization filler.
Fig. 2 a, Fig. 2 b are respectively graphene oxide and surface of graphene oxide growth in situ titanium dioxide sila in embodiment 2
Change the SEM figures of filler.
Fig. 3 is SiO2The GO-SiO prepared with embodiment 32The thermogravimetric curve figure of nano hybridization filler.
Fig. 4 is SiO2The GO-SiO prepared with embodiment 42The infrared spectrum of nano hybridization filler.
Fig. 5 is with graphene oxide and silicon source single silica acid ethyl ester to prepare GO-SiO in embodiment 12Nano hybridization filler
Synthetic route chart.
Embodiment
In order to preferably describe and understand the present invention, with reference to embodiment and accompanying drawing, the invention will be further described,
But the scope of protection of present invention is not limited to the scope of embodiment statement.
Embodiment 1
50mg is crushed into dry graphene oxide to be distributed in 28ml deionized waters, ultrasonic disperse 2h, is added at 30 DEG C
28ml absolute ethyl alcohols, and 5ml25wt% ammoniacal liquor is added, 5mg dibutyl tin laurates are then added dropwise, the ultrasound point at 30 DEG C
30min is dissipated, at 30 DEG C, 200mg tetraethyl orthosilicate is added dropwise（Rate of addition is 3 drops/sec）, stirring reaction 4 hours, through washing
Wash, be dried to obtain GO-SiO2Nano hybridization filler, the i.e. nano hybridization of surface of graphene oxide growth in situ silica is filled out
Material, synthetic route is as shown in Figure 5.Fig. 1 a, Fig. 1 b are respectively graphene oxide and surface of graphene oxide growth in situ titanium dioxide
The TEM figures of silicon nano hybridization filler.One layer of the superficial growth that comparison diagram 1a, Fig. 1 b can be seen that in graphene oxide is not advised
Nano-silicon dioxide particle then.
Embodiment 2
50mg is crushed into dry graphene oxide and is distributed to 154ml deionized waters, ultrasonic disperse 2h, is added at 30 DEG C
126.5ml absolute ethyl alcohols, and 10ml25wt% ammoniacal liquor is added, then the ultrasonic disperse 30min at 30 DEG C is added dropwise the fourths of 10mg tetra-
Base ammonium bromide, at 55 DEG C, is added dropwise 260mg methyl silicate（Rate of addition is 6.5 drops/sec）, stirring reaction 5 hours, warp
Wash, be dried to obtain GO-SiO2Nano hybridization filler, i.e. surface of graphene oxide growth in situ SiO 2 hybrid filler.Figure
2a, Fig. 2 b are respectively the graphene oxide and surface of graphene oxide growth in situ SiO 2 hybrid filler of the present embodiment
SEM schemes.Comparison diagram 2a, Fig. 2 b can with it is further seen that, silicon dioxide granule is uniformly distributed in surface of graphene oxide, rather than
Simple mechanical mixture.
Embodiment 3
In 1000 ml three-necked flasks, add 50mg and crush dry graphene oxide, then add 280ml deionized waters,
Ultrasonic disperse 2h at 30 DEG C, adds 280ml absolute ethyl alcohols, and add 15 ml25wt% ammoniacal liquor, the ultrasonic disperse at 30 DEG C
1h, is then added dropwise 15mg dibutyl tin laurates, at 80 DEG C, and 320mg methyl silicates are added dropwise（Rate of addition be 10 drop/
Second）, stirring reaction 6 hours is scrubbed, be dried to obtain GO-SiO2Nano hybridization filler.Fig. 3 is GO-SiO2Nano hybridization filler
Thermogravimetric curve figure, the Thermogravimetric Data of the figure shows that the silicon dioxide granule in the surface attachment of graphene oxide is 93.0wt%.
Embodiment 4
In 1000 ml three-necked flasks, add 50mg and crush dry graphene oxide, then add 280ml deionized waters,
Ultrasonic disperse 2h at 30 DEG C, adds 280ml absolute ethyl alcohols, and add 15ml25wt% ammoniacal liquor, the ultrasonic disperse at 30 DEG C
1h, is then added dropwise 5mg Bis(lauroyloxy)dioctyltins, at 80 DEG C, and 200mg sodium metasilicate is added dropwise（Rate of addition is 10 drops/sec）,
Stirring reaction 6 hours, it is scrubbed, be dried to obtain GO-SiO2Nano hybridization filler.Fig. 4 is SiO2And GO-SiO2Nano hybridization is filled out
The infrared spectrum of material, contrasts the infrared spectrum of the two, it can be seen that GO-SiO2The infrared spectrum of nano hybridization filler
In in 1406 cm-1With 1470 cm-1Place occurs in that stretching vibration peak, illustrates have silicon dioxide granule to pass through chemical bond success table
Face growth in situ generates new GO-SiO to GO surfaces2Nano hybridization filler, and it is grafted to the dioxy on graphene oxide
SiClx particle is a lot.
Claims (10)
1. a kind of preparation method of the nano hybridization filler of surface of graphene oxide growth in situ silica, it is characterised in that
Comprise the following steps：
（1）Ultrasonic disperse in water is added graphene oxide into, ethanol is added, graphene oxide dispersion is obtained；
（2）To step（1）Ammoniacal liquor and catalyst, then ultrasonic disperse are added in gained graphene oxide dispersion, mixed liquor is obtained；
（3）At 30-80 DEG C, to step（2）Silicon source monomer, stirring reaction are added dropwise in gained mixed liquor；
（4）By step（3）Products therefrom washing, drying, the nanometer for obtaining surface of graphene oxide growth in situ silica are miscellaneous
Change filler.
2. according to the method described in claim 1, it is characterised in that step（1）Described water is deionized water, described ethanol
For absolute ethyl alcohol.
3. according to the method described in claim 1, it is characterised in that step（1）The solid content of the graphene oxide dispersion
For 0.01%-0.1%.
4. according to the method described in claim 1, it is characterised in that step（2）In, to step（1）Gained graphene oxide point
Added in dispersion liquid after ammoniacal liquor, ultrasonic disperse, add catalyst.
5. according to the method described in claim 1, it is characterised in that step（2）The catalyst is tin dilaurate di-n-octyl
One or more of tin, dibutyl tin laurate and TBAB；The addition of the catalyst is 5-15mg.
6. according to the method described in claim 1, it is characterised in that step（2）The addition of the ammoniacal liquor is 5-15ml.
7. according to the method described in claim 1, it is characterised in that step（3）The silicon source monomer is methyl silicate, positive silicon
One kind in acetoacetic ester and sodium metasilicate.
8. according to the method described in claim 1, it is characterised in that step（3）The time of the stirring reaction is 2-8h.
9. according to the method described in claim 1, it is characterised in that step（3）The silicon source monomer accounts for graphene oxide
400wt%-640 wt%。
10. a kind of nano hybridization filler as made from the method described in claim any one of 1-9.
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| CN108117811A (en) * | 2018-01-25 | 2018-06-05 | 惠州市栢诗新材料有限公司 | A kind of graphene-silicon electromagnetic shielding filler and electromagnetic screen coating |
| CN108439419A (en) * | 2018-04-02 | 2018-08-24 | 深圳元颉新材料科技有限公司 | Preparation method of mesoporous silica nano hemispherical material |
| CN108589273A (en) * | 2018-04-17 | 2018-09-28 | 东华大学 | A kind of modified quartz fibre and its surface modifying method |
| CN108862265A (en) * | 2018-07-18 | 2018-11-23 | 深圳大学 | A kind of graphene oxide-nanometer silicon dioxide composite material and preparation method thereof |
| CN109135504A (en) * | 2018-07-27 | 2019-01-04 | 山东大学 | A kind of modified graphene oxide/aqueous epoxy resins composite coating and preparation method thereof |
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