CN104472542A - Method for preparing graphene/silver/titanium dioxide composite material - Google Patents
Method for preparing graphene/silver/titanium dioxide composite material Download PDFInfo
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- CN104472542A CN104472542A CN201410783020.0A CN201410783020A CN104472542A CN 104472542 A CN104472542 A CN 104472542A CN 201410783020 A CN201410783020 A CN 201410783020A CN 104472542 A CN104472542 A CN 104472542A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
Abstract
The invention discloses a method for preparing a graphene/silver/titanium dioxide composite material. The method comprises the following steps: (1) weighing graphene sheets; (2) dispersing the graphene sheets weighed in the step (1) into an aqueous solution of a proper amount of surfactants (PVP or SDS), and performing ultrasonic dispersion; (3) adding silver nitrate in a calculated amount into the graphene sheet solution treated in the step (2), preserving the constant temperature in an oil bath pan, dripping a reducing agent (N2H4, NaBH4 or vitamin C) in a corresponding calculated amount, and preserving the constant temperature for a period of time, thereby obtaining a graphene/silver composite material solution; and (4) heating the graphene/silver composite material solution prepared in the step (3) to another temperature, preserving the constant temperature for a certain time, slowly adding a chlorotitanate solution (TiCl3 or TiCl4) of a calculated amount, and performing suction filtration, washing, vacuum drying treatment, thereby obtaining the graphene/silver/titanium dioxide composite material powder. The method is simple in preparation process and easy to popularize and apply.
Description
Technical field
The invention belongs to the preparation field of carbon composite, specifically, relate to the technology of preparing of a kind of Graphene/silver/titanium dioxide composite.
Background technology
Graphene is a kind of SP
2hydridization has cellular material with carbon element, and the thickness of single-layer graphene only has 0.334nm, is the thinnest known material at present.The specific surface area that Graphene has super large can reach about 2600m
2/ g, so large specific surface area makes grapheme material become the first-selection of energy storage material, finds that it may be used in Chu Qing, ultracapacitor or fuel cell in research in the past; Simultaneously in view of the characteristic of the specific surface area of its superelevation, grapheme material also obtains extensive research in environment absorption and air cleaning; And because grapheme material itself is highly stable, in material science research, usually chooses the carrier that it is composite, be used for preparing graphene-based composite.Graphene also because having very high conductive performance and carrier's rate performance, can be applicable in electronic information technology; And because it has thermal conductivity (~ 5000 W/m of super large
*k), Graphene also result in the great interest of the researcher of heat transfer aspect, applies it in heat-conducting medium, the heat transfer medium of preparation high heat conductance.
In research in the past, find that Graphene has certain anti-microbial property, such as, report a kind of graphene paper of being reduced by graphene oxide at " American Chemical Society-nanometer " (ACS-Nano, the 4th volume 4317 pages in 2010) and there is certain antibiotic property.Occur a series of Graphene/silver nanoparticle composite antibacterial material with better anti-microbial property subsequently, research finds that this type of material all has certain complexity or result of use has certain limitation in the technique of preparation.
So in research process; have chosen titanium dioxide and carry out the collaborative anti-microbial property promoting Graphene/silver; as everyone knows; titanium dioxide has high photocatalytic activity; and itself is nontoxic; its stable chemical nature simultaneously; the features such as anti-light corrosive nature is strong are the most widely used a kind of catalysis materials; and reports existing a large amount of in research in the past proves that titanium dioxide can be used for (as: air cleaning in field of environment protection; the sterilization etc. of water); therefore, titanium dioxide is a kind of catalyzer with exploitation future.Considering that the agglomeration of nano titanium oxide directly can affect its catalytic performance, the Graphene selecting specific surface area large, as carrier, can make it effectively can be dispersed in graphene sheet layer and represent better catalytic antimicrobial performance.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, the preparation method of a kind of Graphene/silver/titanium dioxide composite is provided.
The technical solution used in the present invention is with the homemade Graphene in laboratory for raw material, by reduction AgNO
3preparation graphene/silver composite material solution, and then the method for nano titanium oxide is prepared by chlorotitanate hydrolysis, concrete preparation process is as follows:
A preparation method for Graphene/silver/titanium dioxide composite, comprises the steps:
(1) graphene film is taken;
(2) the graphene film aqueous solution is prepared: the graphene film that above-mentioned (1) takes is placed in three hole flasks, then adds deionized water, then add surfactant, then carry out ultrasonic disperse, obtain the graphene film aqueous solution;
(3) graphene/silver composite material solution is prepared: be fixed in thermostatical oil bath by the flask filling the graphene film aqueous solution prepared by above-mentioned (2), setting reaction temperature, the reductant constant pressure funnel taking corresponding amount of calculation is added drop-wise in solution, then obtains graphene/silver composite material solution after constant temperature certain hour;
(4) Graphene/silver/titanium dioxide composite is prepared: the graphene/silver composite material solution warms above-mentioned (3) prepared is to another higher temperature, the chlorine titanium salt solution measuring amount of calculation after constant temperature certain hour is added drop-wise in solution in constant pressure funnel, after dripping chlorine titanium salt, by solution constant temperature certain hour again by solution filter, washing and in vacuum drying chamber drying obtain Graphene/silver/titanium dioxide composite.
In above-mentioned preparation method, the graphene film described in step (1) has laminate structure and lamella is 1 ~ 10 carbon atomic layer thickness, and the size of this lamella is 5 ~ 20 μm.
In above-mentioned preparation method, the amount of the deionized water that step (2) adds is 100 ~ 300 ml; PVP or SDS chosen by the surfactant added, and the deionized water solution measured experimentally determines to take the amount adding PVP or SDS, and the amount of PVP or SDS in aqueous controls at 0.005 ~ 0.05 g/ml.
In above-mentioned preparation method, in step (2), mechanical agitation is introduced in ultrasonic procedure, rotating speed controls at 100 ~ 400 rpm, the power of the ultrasonic dispersing machine that ultrasonic disperse is used is 100 ~ 400 W, ultrasonic time is 20 ~ 60 min, and the concentration of the graphene film solution of preparation is in 0.5 ~ 5 mg/ml scope.
In above-mentioned preparation method, concentration step (2) prepared is fixed in thermostatical oil bath at the flask of 0.5 ~ 5 mg/ml graphene film solution, and the reaction temperature of setting is 70 ~ 90 DEG C, and the reductant taken is N
2h
4, NaBH
4or vitamin C, then be added drop-wise in solution by constant pressure funnel, the rate of addition of control is 0.25 ~ 5 drop/sec, drips rear constant temperature 1 ~ 4 hour, the speed controlling to stir in dropping reductant and thermostatic process is 100 ~ 400 rpm, selects magnetic agitation or mechanical agitation during stirring.
In above-mentioned preparation method, in step (4), the thermostatical oil bath that graphene/silver composite material solution is housed is warmed up to 85 ~ 98 DEG C, measures chlorine titanium salt solution after constant temperature, the chlorine titanium salt selected is TiCl
3or TiCl
4, instill in constant pressure funnel in solution, the rate of addition of control is 0.5 ~ 5 drop/sec, drips rear constant temperature 1 ~ 4 hour, and in dropping chlorine titanium salt and thermostatic process, control mixing speed is 100 ~ 400 rpm, selects magnetic agitation or mechanical agitation during stirring.
In above-mentioned preparation method, in step (4), Graphene/silver/titanium dioxide composite solution after suction filtration, the washing of 3 water washings, 2 ethanol in vacuum drying chamber 60 DEG C, drying in 24 hours obtains Graphene/silver/titanium dioxide composite material powder.
Compared with prior art, the present invention has following beneficial effect: the graphene film that the present invention selects laboratory ultrasonic disperse to prepare is base material, first reduces AgNO by liquid phase method
3preparation graphene/silver composite material solution, and then the method being prepared nano titanium oxide by chlorotitanate hydrolysis, the self assembly composite of Graphene/silver/titanium dioxide, this material has two kinds of material Synergistic antimicrobial performances.
Accompanying drawing explanation
Fig. 1 is the SEM figure of graphene film;
Fig. 2 is the TEM figure of graphene film;
Fig. 3 is graphene film/silver-colored SEM figure;
Fig. 4 is graphene film/silver-colored TEM figure;
Fig. 5 is that graphene film/silver/titanium dioxide SEM schemes;
Fig. 6 is that graphene film/silver/titanium dioxide TEM schemes;
Fig. 7 is graphene film/silver/titanium dioxide preparation flow schematic diagram.
Embodiment
Explain the present invention further below in conjunction with specific embodiment, but embodiment does not limit in any form to invention.
Embodiment 1:
(1) the PVP powder of 1g graphene film and 2g is taken, two kinds of powders are proceeded in three hole flasks, then 200 ml deionized waters are measured, at the supersonic wave cleaning machine ultrasonic disperse of 200 W, the rotating speed regulating machine mixer is 200 rpm, ultrasonic about 40 min obtain the stable graphene film aqueous solution, and Fig. 1 is the SEM figure of graphene film in experiment, Fig. 2 is that the TEM of graphene film schemes.
(2) take in the graphene film solution that 1g nitric acid silver powder joins in (1), three hole flasks to be fixed in constant temperature oil bath raised temperature to 82 DEG C and constant temperature 10 min, and the rotating speed regulating agitator is 150 rpm, then measures the hydration N of about 3 ml
2h
4solution is in constant pressure funnel, and regulating and dripping rotating speed is 0.5 drop/sec, treats hydration N
2h
4after solution drips under this reaction temperature constant temperature 2 hours, obtain uniform graphene/silver composite material solution, Fig. 3 is the SEM figure of graphene/silver composite material, Fig. 4 is that the TEM of graphene film/silver schemes.
(3) by the graphene/silver composite material solution warms of preparation in (2) to 95 DEG C and constant temperature 10 min, the rotating speed regulating agitator is 120 rpm, measures the TiCl of about 10 ml
3solution is in constant pressure funnel, and controlling rate of addition is 1 drop/sec, treats TiCl
3after solution drips under this reaction temperature constant temperature 2.5 hours, obtain uniform Graphene/silver/titanium dioxide composite solution, sample carried out suction filtration, 3 deionization washings, after 2 ethanol washings, obtain Graphene/silver/titanium dioxide composite material powder.Fig. 5 is the SEM figure of Graphene/silver/titanium dioxide composite, and Fig. 6 is that Graphene/silver/titanium dioxide TEM schemes, and Fig. 7 is the schematic flow sheet of the Graphene/silver/titanium dioxide composite of preparation.
Embodiment 2:
(1) the SDS powder of 1.5 g graphene films and 2 g is taken, two kinds of powders are proceeded in three hole flasks, then 150 ml deionized waters are measured, at the supersonic wave cleaning machine ultrasonic disperse of 200 W, the rotating speed regulating machine mixer is 200 rpm, and ultrasonic about 30 min obtain the stable graphene film aqueous solution.
(2) take in the graphene film solution that 1g nitric acid silver powder joins in (1), three hole flasks to be fixed in constant temperature oil bath raised temperature to 85 DEG C and constant temperature 10 min, and the rotating speed regulating agitator is 150 rpm, then measures the NaBH of about 2.5 ml
4the aqueous solution is in constant pressure funnel, and regulating and dripping rotating speed is 0.5 drop/sec, treats hydration NaBH
4after the aqueous solution drips under this reaction temperature constant temperature 2 hours, obtain uniform graphene/silver composite material solution.
(3) by the graphene/silver composite material solution warms of preparation in (2) to 92 DEG C and constant temperature 10 min, the rotating speed regulating agitator is 150 rpm, measures the TiCl of about 10 ml
3solution is in constant pressure funnel, and controlling rate of addition is 1 drop/sec, treats TiCl
3after solution drips under this reaction temperature constant temperature 3 hours, obtain uniform Graphene/silver/titanium dioxide composite solution, sample carried out suction filtration, 3 deionization washings, after 2 ethanol washings, obtain Graphene/silver/titanium dioxide composite material powder.
Embodiment 3:
(1) the PVP powder of 2 g graphene films and 2 g is taken, two kinds of powders are proceeded in three hole flasks, then 300 ml deionized waters are measured, at the supersonic wave cleaning machine ultrasonic disperse of 250 W, the rotating speed regulating machine mixer is 250 rpm, and ultrasonic about 25 min obtain the stable graphene film aqueous solution.
(2) taking 1.5 g nitric acid silver powder joins in the graphene film solution in (1), three hole flasks to be fixed in constant temperature oil bath raised temperature to 80 DEG C and constant temperature 10 min, and regulate the rotating speed of agitator to be 150 rpm, measure the vitamin C aqueous solution of about 5 ml again in constant pressure funnel, regulating and dripping rotating speed is 1 drop/sec, after the hydration vitamin C aqueous solution drips under this reaction temperature constant temperature 3 hours, obtain uniform graphene/silver composite material solution.
(3) by the graphene/silver composite material solution warms of preparation in (2) to 98 DEG C and constant temperature 10 min, the rotating speed regulating agitator is 150 rpm, measures the TiCl of about 10 ml
4solution is in constant pressure funnel, and controlling rate of addition is 1.5 drops/sec, treats TiCl
3after solution drips under this reaction temperature constant temperature 2 hours, obtain uniform Graphene/silver/titanium dioxide composite solution, sample carried out suction filtration, 3 deionization washings, after 2 ethanol washings, obtain Graphene/silver/titanium dioxide composite material powder.
Claims (7)
1. a preparation method for Graphene/silver/titanium dioxide composite, is characterized in that comprising the steps:
(1) graphene film is taken;
(2) the graphene film aqueous solution is prepared: the graphene film that above-mentioned (1) takes is placed in three hole flasks, then adds deionized water, then add surfactant, then carry out ultrasonic disperse, obtain the graphene film aqueous solution;
(3) graphene/silver composite material solution is prepared: be fixed in thermostatical oil bath by the flask filling the graphene film aqueous solution prepared by above-mentioned (2), setting reaction temperature, the reductant constant pressure funnel taking corresponding amount of calculation is added drop-wise in solution, then obtains graphene/silver composite material solution after constant temperature certain hour;
(4) Graphene/silver/titanium dioxide composite is prepared: the graphene/silver composite material solution warms above-mentioned (3) prepared is to another higher temperature, the chlorine titanium salt solution measuring amount of calculation after constant temperature certain hour is added drop-wise in solution in constant pressure funnel, after dripping chlorine titanium salt, by solution constant temperature certain hour again by solution filter, washing and in vacuum drying chamber drying obtain Graphene/silver/titanium dioxide composite.
2. preparation method according to claim 1, is characterized in that, the graphene film described in step (1) has laminate structure and lamella is 1 ~ 10 carbon atomic layer thickness, and the size of this lamella is 5 ~ 20 μm.
3. preparation method according to claim 1, is characterized in that, the amount of the deionized water that step (2) adds is 100 ~ 300 ml; PVP or SDS chosen by the surfactant added, and the deionized water solution measured experimentally determines to take the amount adding PVP or SDS, and the amount of PVP or SDS in aqueous controls at 0.005 ~ 0.05 g/ml.
4. preparation method according to claim 1, it is characterized in that in step (2), mechanical agitation is introduced in ultrasonic procedure, rotating speed controls at 100 ~ 400 rpm, the power of the ultrasonic dispersing machine that ultrasonic disperse is used is 100 ~ 400 W, ultrasonic time is 20 ~ 60 min, and the concentration of the graphene film solution of preparation is in 0.5 ~ 5 mg/ml scope.
5. preparation method according to claim 1, is characterized in that, concentration step (2) prepared is fixed in thermostatical oil bath at the flask of 0.5 ~ 5 mg/ml graphene film solution, and the reaction temperature of setting is 70 ~ 90 DEG C, and the reductant taken is N
2h
4, NaBH
4or vitamin C, then be added drop-wise in solution by constant pressure funnel, the rate of addition of control is 0.25 ~ 5 drop/sec, drips rear constant temperature 1 ~ 4 hour, the speed controlling to stir in dropping reductant and thermostatic process is 100 ~ 400 rpm, selects magnetic agitation or mechanical agitation during stirring.
6. preparation method according to claim 1, it is characterized in that, in step (4), the thermostatical oil bath that graphene/silver composite material solution is housed being warmed up to 85 ~ 98 DEG C, measuring chlorine titanium salt solution after constant temperature, the chlorine titanium salt selected is TiCl
3or TiCl
4, instill in constant pressure funnel in solution, the rate of addition of control is 0.5 ~ 5 drop/sec, drips rear constant temperature 1 ~ 4 hour, and in dropping chlorine titanium salt and thermostatic process, control mixing speed is 100 ~ 400 rpm, selects magnetic agitation or mechanical agitation during stirring.
7. preparation method according to claim 1, it is characterized in that in step (4), Graphene/silver/titanium dioxide composite solution after suction filtration, the washing of 3 water washings, 2 ethanol in vacuum drying chamber 60 DEG C, drying in 24 hours obtains Graphene/silver/titanium dioxide composite material powder.
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| CN201410783020.0A CN104472542A (en) | 2014-12-18 | 2014-12-18 | Method for preparing graphene/silver/titanium dioxide composite material |
| PCT/CN2015/075296 WO2016095358A1 (en) | 2014-12-18 | 2015-03-27 | Method for preparing graphene/silver/titanium dioxide composite |
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