CN109384243A - Mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite and its preparation - Google Patents
Mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite and its preparation Download PDFInfo
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Abstract
It is three-decker the invention proposes a kind of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite and its preparation, the composite material, is followed successively by mesoporous silicon oxide, graphene, mesoporous silicon oxide from top to bottom.Preparation includes: that surfactant and catalyst are dissolved into water by (1), and graphene film is added；Silicon source is dissolved in organic solvent；The organic solution is added to the upper layer of the dark solution, obtains two phase stratification system；(2) it is reacted in 35-70 DEG C of temperature；(3) oxygen-containing group of surfactant and graphene film surface therein is removed.Present invention employs oil-water two-phase reaction systems, due to ultralow graphene content and catalyst concn, the hydrolysis of silicon source and the formation of mesoporous silicon oxide are mainly based on heterogeneous nucleation, therefore gained meso-porous titanium dioxide silicon components can uniformly be grown in the two sides of graphene film, form mesoporous silicon oxide/graphene/mesoporous silicon oxide sandwich structure.
Description
Technical field
The present invention relates to technical field of nano material, particularly relate to a kind of mesoporous silicon oxide/graphene/meso-porous titanium dioxide
Silicon composite and its preparation.
Background technique
Mesoporous silicon oxide/graphene nanocomposite material is a kind of important complex mesoporous material, has near infrared light
It the features such as response, stable, inexpensive porosity height, large specific surface area, chemical property, is answered extensively in fields such as biological medicines
With.In recent years, mesoporous silicon oxide/graphene composite material was prepared very universal, was obtained in terms of the treatment of tumour cell
Remarkable progress, graphene film heat production under harmless near infrared light can kill cancer cell, and mesoporous two
The high load and controlled release of anticancer drug may be implemented in silica portion, but due to the limitation of preparation method, there are many
Disadvantage: 1, the aperture of meso-porous titanium dioxide silicon wafer is smaller (~3nm), can only selectivity load small molecule anti-cancer drug, can not apply
The anticancer drug of Yu Geng great or the load of large biological molecule.2, it is limited by template, the aperture of mesopore silicon oxide piece can only
Modulation (2.0~4.0nm) to a very small extent cannot achieve the load and release of two or more different size pharmaceutical molecules
Deng.Mesoporous silicon oxide/graphene synthetic method how is improved, the limitation of template size itself is broken, is realized to mesoporous
Silica/graphene composite material aperture freely regulates and controls, and has become the hot spot studied now.
Summary of the invention
The present invention proposes a kind of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite and its preparation, solves
In the prior art the problem of template size limiting aperture, realize to mesoporous silicon oxide/graphene composite material aperture certainly
By regulating and controlling.
The technical scheme of the present invention is realized as follows:
A kind of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite, the composite material is three-layered node
Structure is followed successively by mesoporous silicon oxide, graphene, mesoporous silicon oxide from top to bottom.
Above-mentioned mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite is prepared by the following method, system
Preparation Method includes:
(1) surfactant and catalyst are dissolved into water, stir to clarify solution；Surface-active in the clear solution
The concentration of agent is 0.5-20wt%；Graphene film is added in the clear solution, ultrasonic disperse, continues to stir, obtain black
Solution；
Silicon source is dissolved in organic solvent, organic solution is obtained；Wherein the concentration of silicon source is 2.5-30wt%；
The organic solution is added to the upper layer of the dark solution, upper oil phase is formed, obtains two phase stratification system；
The graphene film and the mass ratio of silicon source are 0.0002-0.00095, and the mass ratio of surfactant and silicon source is
0.25-8.0；
(2) the two phase stratification system is reacted in 35-70 DEG C of temperature；Obtain be grown in graphene film two sides mesoporous two
Oxidized silicon chip；
(3) under inert gas atmosphere by the product of step (2), 400-1000 DEG C of temperature is risen to from room temperature, removal is wherein
Surfactant and graphene film surface oxygen-containing group, obtain mesoporous silicon oxide/graphene/mesoporous silicon oxide Sanming City
Control the nanocomposite of structure.
As a preferred technical solution, the surfactant in quaternary cationic surfactant one
Kind is several；Including but not limited to hexadecyltrimethylammonium chloride, cetyl trimethylammonium bromide, octadecyl trimethyl
Ammonium chloride or Cetyltrimethylammonium bromide.
The catalyst is selected from ammonium hydroxide, fatty amine, hydramine, aromatic amine, amide, fragrance as a preferred technical solution,
One or more of amine, aliphatic cyclic amine；Including but not limited to octylame, lauryl amine, triethanolamine, diethanol amine.
The concentration of catalyst described in solution is 0.2-0.5wt% as a preferred technical solution,.
The graphene film is selected from graphene oxide, redox graphene, graphene as a preferred technical solution,
One or more of.
The time that the step (1) continues stirring as a preferred technical solution, controls in 0.05-5h.
As a preferred technical solution, the silicon source in sodium metasilicate, fumed silica, ethyl orthosilicate one
Kind is several.
The organic solvent is selected from dioxane, hexamethylene, n-hexane, decahydronaphthalene, alkene as a preferred technical solution,
One or more of hydrocarbon.
The time reacted in the step (2) as a preferred technical solution, is 2-12h；Heating in the step (3)
Rate is 0.2-5 DEG C/min, keeps 3-12h when rising to 400-1000 DEG C of temperature.
The two sides of material obtained above are by the mesoporous of the tightly packed formation of silica as a preferred technical solution,
Nanometer sheet, piece size are 40~2500nm, and with a thickness of 20~100nm, specific surface area is 350~1800m2/ g, aperture 2.5
0.35~2.25cm of~20nm, Kong Rongwei3/g。
Beneficial effect
(1) present invention employs oil-water two-phase reaction system, due to ultralow graphene content and catalyst concn,
The hydrolysis of silicon source and the formation of mesoporous silicon oxide are mainly based on heterogeneous nucleation, therefore gained meso-porous titanium dioxide silicon components meeting
The two sides of graphene film are uniformly grown in, mesoporous silicon oxide/graphene/mesoporous silicon oxide sandwich structure is formed, and
Simple growth of the non-mesoporous silica spheres body on graphene film.
(2) during the reaction, reaming effect, therefore gained composite material intermediary hole dioxy can be achieved in the incorporation of organic phase
The aperture of SiClx component obviously increases, and is much higher than 3nm (reaching as high as 20nm).More importantly aperture can 2.5~
Regulated and controled between 20nm.
Detailed description of the invention
It, below will be to embodiment in order to illustrate more clearly of embodiment of the present invention or technical solution in the prior art
Or attached drawing needed to be used in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description is only
It is some embodiments of the invention, for those of ordinary skill in the art, in the premise of not making the creative labor property
Under, it is also possible to obtain other drawings based on these drawings.
Fig. 1 is graphene film mark scanning electron microscope (SEM) figure (250nm) and thickness distribution in embodiment 1.
Fig. 2 is mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite mark scanning electronics in embodiment 1
Microscope (SEM) figure (500nm).
Fig. 3 is mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite mark scanning electronics in embodiment 1
Microscope (SEM) figure (100nm).
Fig. 4 is mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite feature nitrogen adsorption-in embodiment 1
Desorption isotherm and pore size distribution curve.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Substance involved in following embodiments is commercially available.
Embodiment 1
A kind of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite, the composite material is three-layered node
Structure is followed successively by mesoporous silicon oxide, graphene, mesoporous silicon oxide from top to bottom.
Above-mentioned mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite is prepared by the following method, system
Preparation Method includes:
(1) aqueous phase system:
1.5g hexadecyltrimethylammonium chloride and 0.060mL triethanolamine are successively dissolved into 20mL deionized water,
It stirs evenly to form colorless and transparent solution；By the colorless and transparent solution to entering in reactor, 0.62mg oxidation stone is added
Black alkene, ultrasonic disperse, continues to stir 0.5h, obtains dark solution later；
Oil-based system: ethyl orthosilicate is dissolved in hexamethylene, obtains 7mL organic solution；Wherein ethyl orthosilicate is dense
Degree is 10wt%；
Organic solution is added dropwise to the upper surface of dark solution, forms water-oil phase layered system；
(2) the two phase stratification system in step (1) is reacted into 3h in the oil bath of temperature 60 C；Obtain meso-porous titanium dioxide
Silicon/graphene oxide/meso-porous titanium dioxide silicon composite；
(3) above-mentioned mesoporous silicon oxide/graphene oxide/meso-porous titanium dioxide silicon composite is placed in tube furnace,
Under inert gas atmosphere, 600 DEG C of temperature are risen to from room temperature with 1 DEG C/min, and 3h is kept to remove surfactant and oxygen therein
Oxygen-containing group on graphite alkene obtains mesoporous silicon oxide/graphene/mesoporous silicon oxide sandwich structure composite wood
Material.
Composite material obtained above is combined closely and is formed by mesoporous silicon oxide-graphene-mesoporous silicon oxide
Sandwich structure.Its piece size is 40~2500nm, and with a thickness of 20~100nm, specific surface area is 350~1800m2/ g, aperture
For 2.5~20nm, 0.35~2.25cm of Kong Rongwei3/g。
Embodiment 2
A kind of mesoporous silicon oxide/graphene/mesoporous silicon oxide composite material and preparation method, comprising:
(1) aqueous phase system:
0.5g hexadecyltrimethylammonium chloride and 0.075mL triethanolamine are successively dissolved into 20mL deionized water,
It stirs evenly to form colorless and transparent solution；By the colorless and transparent solution to entering in reactor, 0.13mg oxidation stone is added
Black alkene, ultrasonic disperse, continues to stir 0.5h, obtains dark solution later；
Oil-based system: fumed silica is dissolved in n-hexane, obtains 8mL organic solution；Wherein fumed silica
Concentration be 2.5wt%；
Organic solution is added dropwise to the upper surface of dark solution, forms water-oil phase layered system；
(2) the two phase stratification system in step (1) is reacted into 5h in the oil bath of temperature 60 C；Obtain meso-porous titanium dioxide
Silicon/graphene oxide/meso-porous titanium dioxide silicon composite；
(3) above-mentioned mesoporous silicon oxide/graphene oxide/meso-porous titanium dioxide silicon composite is placed in tube furnace,
Under inert gas atmosphere, rise to 400 DEG C of temperature from room temperature with 0.2 DEG C/min, and keep 6h remove surfactant therein and
Oxygen-containing group on graphene oxide obtains mesoporous silicon oxide/graphene/mesoporous silicon oxide sandwich structure composite wood
Material.
Composite material obtained above is combined closely and is formed by mesoporous silicon oxide-graphene-mesoporous silicon oxide
Sandwich structure.
Embodiment 3
A kind of mesoporous silicon oxide/graphene oxide/mesoporous silicon oxide composite material and preparation method, comprising:
(1) aqueous phase system:
4.0g octadecyltrimethylammonium chloride and 0.15mL ammonium hydroxide are successively dissolved into 20mL deionized water, stirring is equal
It is even to form colorless and transparent solution；By the colorless and transparent solution to entering in reactor, 0.31mg reduction-oxidation graphite is added
Alkene, ultrasonic disperse, continues to stir 1.0h, obtains dark solution later；
Oil-based system: ethyl orthosilicate is dissolved in n-hexane, obtains 8mL organic solution；Wherein the concentration of solvent is
30wt%；
Organic solution is added dropwise to the upper surface of dark solution, forms water-oil phase layered system, and continue at this
10h is reacted under part；
(2) the two phase stratification system in step (1) is reacted in 35 DEG C of temperature of oil bath；Obtain mesoporous silicon oxide/
Redox graphene/meso-porous titanium dioxide silicon composite；
(3) above-mentioned mesoporous silicon oxide/redox graphene/meso-porous titanium dioxide silicon composite is placed in tube furnace
In, under inert gas atmosphere, 800 DEG C of temperature are risen to from room temperature with 2.5 DEG C/min, and 4h is kept to remove surface-active therein
Agent obtains mesoporous silicon oxide/graphene/mesoporous silicon oxide sandwich structure composite material.
Composite material obtained above is combined closely and is formed by mesoporous silicon oxide-graphene-mesoporous silicon oxide
Sandwich structure.
Embodiment 4
A kind of mesoporous silicon oxide/graphene oxide/mesoporous silicon oxide composite material and preparation method, comprising:
(1) aqueous phase system:
0.5g Cetyltrimethylammonium bromide and 0.1mL diethanol amine are successively dissolved into 20mL deionized water, stirred
It mixes and is formed uniformly colorless and transparent solution；By the colorless and transparent solution to entering in reactor, 0.17mg graphene is added, it
Ultrasonic disperse afterwards continues to stir 1.5h, obtains dark solution；
Oil-based system: sodium metasilicate is dissolved in decahydronaphthalene, obtains 10mL organic solution；Wherein the concentration of solvent is 4wt%；
Organic solution is added dropwise to the upper surface of dark solution, forms water-oil phase layered system, and continue at this
5h is reacted under part；
(2) the two phase stratification system in step (1) is reacted in the oil bath of temperature 70 C；Obtain mesoporous silicon oxide/
Graphene/meso-porous titanium dioxide silicon composite；
(3) above-mentioned mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite is placed in tube furnace, in inertia
Under gas atmosphere, 1000 DEG C of temperature are risen to from room temperature with 5 DEG C/min, and 3h is kept to remove surfactant therein, is situated between
Hole silica/graphene/mesoporous silicon oxide sandwich structure composite material.
Composite material obtained above is combined closely and is formed by mesoporous silicon oxide-graphene-mesoporous silicon oxide
Sandwich structure.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite, which is characterized in that the composite material
For three-decker, it is followed successively by mesoporous silicon oxide, graphene, mesoporous silicon oxide from top to bottom.
2. a kind of preparation method of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite characterized by comprising
(1) surfactant and catalyst are dissolved into water, stir to clarify solution；Surfactant in the clear solution
Concentration is 0.5-20wt%；Graphene film is added in the clear solution, ultrasonic disperse, continues to stir, obtain dark solution；
Silicon source is dissolved in organic solvent, organic solution is obtained；Wherein the concentration of silicon source is 2.5-30wt%；
The organic solution is added to the upper layer of the dark solution, upper oil phase is formed, obtains two phase stratification system；
The graphene film and the mass ratio of silicon source are 0.0002-0.00095, and the mass ratio of surfactant and silicon source is
0.25-8.0；
(2) the two phase stratification system is reacted in 35-70 DEG C of temperature；Obtain the meso-porous titanium dioxide for being grown in graphene film two sides
Silicon wafer；
(3) under inert gas atmosphere by the product of step (2), 400-1000 DEG C of temperature is risen to from room temperature, removes table therein
The oxygen-containing group of face activating agent and graphene film surface obtains mesoporous silicon oxide/graphene/mesoporous silicon oxide sandwich knot
The nanocomposite of structure.
3. a kind of preparation side of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite according to claim 2
Method, which is characterized in that the surfactant is selected from one or more of quaternary cationic surfactant；Including
But it is not limited to hexadecyltrimethylammonium chloride, cetyl trimethylammonium bromide, octadecyltrimethylammonium chloride or 18
Alkyl trimethyl ammonium bromide.
4. a kind of preparation side of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite according to claim 2
Method, which is characterized in that the catalyst is in ammonium hydroxide, fatty amine, hydramine, aromatic amine, amide, aromatic amine, aliphatic cyclic amine
It is one or more of；Including but not limited to octylame, lauryl amine, triethanolamine, diethanol amine.
5. a kind of system of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite according to claim 2 or 3
Preparation Method, which is characterized in that the concentration of catalyst described in solution is 0.2-0.5wt%.
6. a kind of preparation side of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite according to claim 2
Method, which is characterized in that the graphene film is selected from one of graphene oxide, redox graphene, graphene or several
Kind.
7. a kind of preparation side of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite according to claim 2
Method, which is characterized in that the time that the step (1) continues stirring controls in 0.05-5h.
8. a kind of preparation side of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite according to claim 2
Method, which is characterized in that the silicon source is selected from one or more of sodium metasilicate, fumed silica, ethyl orthosilicate；It is described
Organic solvent be selected from one or more of dioxane, hexamethylene, n-hexane, decahydronaphthalene, alkene.
9. a kind of preparation side of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite according to claim 2
Method, which is characterized in that the time reacted in the step (2) is 2-12h；Heating rate in the step (3) is 0.2-5
DEG C/min, 3-12h is kept when rising to 400-1000 DEG C of temperature.
10. a kind of preparation of mesoporous silicon oxide/graphene/meso-porous titanium dioxide silicon composite according to claim 2
Method, which is characterized in that the two sides of material obtained are by the meso-porous nano piece of the tightly packed formation of silica, piece size
For 40~2500nm, with a thickness of 20~100nm, specific surface area is 350~1800m2/ g, aperture are 2.5~20nm, Kong Rongwei
0.35~2.25cm3/g。
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| CN112885895A (en) * | 2021-01-25 | 2021-06-01 | 北海惠科光电技术有限公司 | Preparation method of graphene conductive film, thin film transistor and display device |
| CN113385222A (en) * | 2021-06-21 | 2021-09-14 | 复旦大学 | Monodisperse mesoporous silica composite zeolite core-shell material and preparation method thereof |
| CN114572989A (en) * | 2022-05-06 | 2022-06-03 | 北洋研创(天津)科技有限公司 | Silicon dioxide nanosheet and preparation method and laminated structure thereof |
| CN116395678A (en) * | 2023-05-06 | 2023-07-07 | 蜂巢能源科技(马鞍山)有限公司 | 3D graphene and preparation method thereof |
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| CN113385222A (en) * | 2021-06-21 | 2021-09-14 | 复旦大学 | Monodisperse mesoporous silica composite zeolite core-shell material and preparation method thereof |
| CN114572989A (en) * | 2022-05-06 | 2022-06-03 | 北洋研创(天津)科技有限公司 | Silicon dioxide nanosheet and preparation method and laminated structure thereof |
| CN114572989B (en) * | 2022-05-06 | 2022-09-16 | 北洋研创(天津)科技有限公司 | Silicon dioxide nanosheet and preparation method and laminated structure thereof |
| CN116395678A (en) * | 2023-05-06 | 2023-07-07 | 蜂巢能源科技(马鞍山)有限公司 | 3D graphene and preparation method thereof |
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