CN102861600A - Graphene oxide/silver phosphate/P25 composite material and preparation method thereof - Google Patents
Graphene oxide/silver phosphate/P25 composite material and preparation method thereof Download PDFInfo
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- CN102861600A CN102861600A CN2012103804477A CN201210380447A CN102861600A CN 102861600 A CN102861600 A CN 102861600A CN 2012103804477 A CN2012103804477 A CN 2012103804477A CN 201210380447 A CN201210380447 A CN 201210380447A CN 102861600 A CN102861600 A CN 102861600A
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Abstract
The invention discloses a graphene oxide/silver phosphate/P25 composite material and a preparation method thereof, and belongs to the technical field of composites and photocatalysis for environmental management. The preparation method includes steps of dissolving graphene oxide into water to obtain graphene oxide dispersion under ultrasonic treatment; ultrasonically dispersing silver phosphate and P25 into deionized water to obtain mixed solution, adding the mixed solution into the graphene oxide dispersion drop by drop while stirring so as to obtain a mixed precursor; dripping a prepared phosphate solution into the mixed precursor of the graphene oxide, the silver phosphate and the P25 slowly while stirring continuously so as to obtain a celadon product through reaction, centrifugally separating the celadon product, washing the product with the deionized water and absolute ethyl alcohol multiple times, and drying the product in vacuum so as to obtain the composite material. The graphene oxide/silver phosphate/P25 composite material prepared by the method has high photocatalysis degradation effect to organic dye Rhodamine-B after being initiated by visible light, and also has excellent broad-spectrum bactericidal activity to various common bacteria.
Description
Technical field
The present invention relates to a kind of graphene oxide/silver orthophosphate/P25 composite and preparation method thereof, refer to that especially a kind of solution system ion-exchange based on the electric charge self assembly prepares the method for graphene oxide/silver orthophosphate/P25 composite, belongs to the fields such as composite, catalysis material, environment-friendly materials and pollution control.
Background technology
Titanium dioxide obtains extensive concern as conductor photocatalysis material, but, titanium dioxide light abstraction width narrower (only limiting to ultraviolet region), quantum efficiency are lower, and particularly its visible light-responded degree is low causes its photocatalytic activity under radiation of visible light limited; Guo etc. [
Nat Mater, 2010,9,559-564] to have reported under excited by visible light, silver orthophosphate is owing to having the band structure of dispersion, energy gap relative narrower, the recombination rate of photo-generated carrier reduces greatly, and quantum efficiency is greatly improved, thereby shows excellent visible light photocatalysis active; Silver orthophosphate is as a kind of compound of silver in addition, and silver orthophosphate also has preferably bactericidal activity, but preparing silver orthophosphate has used the compound of argentiferous so that preparation cost is higher, and the size of the silver orthophosphate material of preparing in addition all bigger than normal and pattern is difficult to control.
Graphene oxide is a kind of two-dimensional sheet nano material, have the advantages such as specific area is large, high adsorption capacity, simultaneously, graphene oxide shows to have more hydrophile function group, graphene oxide is applied in the composite manufacture, its surface with negative electrical charge more reflecting point not only can be provided for positively charged silver ion, thereby the nucleation of silver orthophosphate and growth can be controlled at the surface of graphene oxide, thereby reach the effect of effective control silver orthophosphate size and pattern; On the other hand because the good dissolution dispersity of Graphene, the effective compound dispersing and dissolving performance that can significantly improve composite of itself and silver orthophosphate, along with the improvement of preparation graphene oxide technique and the reduction of cost, also can so that the cost of preparation graphene oxide/silver orthophosphate composite greatly reduce.
P25 is the titanic oxide material that a kind of rutile-type and Detitanium-ore-type mix, studies show that its visible light-responded degree is poor, we are effectively compound by silver orthophosphate and P25's, construct the silver orthophosphate of micro nano structure/P25 heterojunction structure, further widen material to visible Optical Absorption and utilization ratio, simultaneously, hydrophilic functional groups large in conjunction with the graphene oxide specific area mainly with and the architectural characteristic such as dispersing and dissolving is good, the multifunctional composite that preparation size and pattern be controlled, have the bactericidal activity of efficient visible light photocatalysis performance, excellence; At present, with graphene oxide, silver nitrate, silver orthophosphate and P25 are that solion exchange process that raw material adopts electric charge to drive self assembly prepares graphene oxide/silver orthophosphate/P25 composite and is applied to photocatalysis degradation organic contaminant and the sterilization field has no report.
Summary of the invention
The object of the invention is to develop a kind of with low cost, method simple, the technology of preparing of the preparation graphene oxide/silver orthophosphate of environmental protection/P25 multifunctional composite, prepared material has appearance structure preferably, visible light photocatalysis performance and excellent sterilizing are active efficiently.
The realization the technical solution adopted in the present invention is: take graphene oxide as presoma, silver orthophosphate particle and the P25 nano particle of micrometer structure effectively is assembled on the graphene oxide lamella, its concrete steps are:
(1) graphene oxide is dissolved in deionized water for ultrasonic and obtains the graphene oxide dispersion liquid that concentration is 0.04-0.1 wt%;
(2) silver nitrate and P25 are dissolved in the deionized water, obtain the mixed solution A of silver nitrate and P25 after the ultrasonic processing, the concentration of silver nitrate is 0.15 mol/L in the mixed solution A, and the concentration of P25 is 0.5-1.5wt%; Mixed solution A is added drop-wise under the magnetic agitation condition in the above-mentioned graphene oxide dispersion liquid, and the mass ratio of graphene oxide and P25 is 1:6 ~ 30, dropwises rear solution and at room temperature continues to stir 30 ~ 60 min, obtains mixing precursor solution B;
(3) phosphate is dissolved in the deionized water, obtains the phosphate solution that concentration is 0.15 mol/L;
(4) phosphate solution that under the condition of magnetic agitation step (3) is prepared dropwise slowly adds among the mixing precursor solution B of step (2) preparation, until occur the celadon muddiness in the reaction system, dropwising rear mixed solution continues to stir behind 30 ~ 60 min still aging, after using absolute ethyl alcohol and deionized water cyclic washing repeatedly after the product centrifugation, vacuum drying obtains graphene oxide/silver orthophosphate/P25 composite.
Phosphate described in the step 3 is sodium hydrogen phosphate, sodium dihydrogen phosphate or sodium phosphate.
Compared with prior art, the present invention has following advantage:
A) since with graphene oxide for the preparation of process, prepared graphene oxide/Ag
3PO
4/ P25 composite has larger specific area, uniform size and controlled composite construction;
B) utilize the large graphene oxide material of specific area not only can effectively adsorb organic dyestuff and organic pollution, and can effectively strengthen the absorbability to light;
C) by the regulating and controlling effect of silver orthophosphate, the visible light-responded scope of titanium dioxide is widened, the sunshine utilization rate significantly promotes, and photocatalysis efficiency strengthens, can all kinds of target contaminants of efficient degradation;
D) utilize synergy between graphene oxide, silver orthophosphate, the titanium dioxide, make prepared material have excellent broad-spectrum antibacterial action, can kill fast common bacteria in the environment;
E) process route that adopts is simple, raw material is easy to get, with low cost, non-secondary pollution, economical and efficient.
Description of drawings
Fig. 1 is the scanning electron microscope diagram of graphene oxide/silver orthophosphate/P25 composite;
Fig. 2 is the transmission electron microscope figure of graphene oxide/silver orthophosphate/P25 composite;
Fig. 3 is the X ray diffracting spectrum of graphene oxide/silver orthophosphate/P25 composite;
Fig. 4 is the UV-vis DRS spectrogram of graphene oxide/silver orthophosphate/P25 composite;
Fig. 5 is graphene oxide/silver orthophosphate/P25 composite photocatalytic degradation curve map to rhodamine B under the visible light condition.
The specific embodiment
Further illustrate content of the present invention below in conjunction with specific embodiment, but these embodiment do not limit protection scope of the present invention.
Embodiment 1
20 mg graphene oxides are scattered in 50 ml deionized water for ultrasonic obtained the graphene oxide dispersion liquid in 5 hours, take by weighing 1.529 g silver nitrates and 300 mg P25 and be dissolved in 50 ml deionized water for ultrasonic after 30 minutes, obtain mixed solution A; Mixed solution A is added drop-wise under magnetic agitation in the above-mentioned graphene oxide dispersion liquid, after continuation is stirred and obtained mixing precursor solution B half an hour; Take by weighing 0.426 g Na
2HPO
4Solid is dissolved in the 20 ml deionized waters, obtain disodium phosphate soln, under the stirring condition disodium phosphate soln for preparing is added drop-wise among the mixing precursor solution B, until occur the celadon muddiness in the reaction system, dropwising rear mixed solution continues to stir after 30 minutes still aging, after using absolute ethyl alcohol and deionized water cyclic washing repeatedly after the product centrifugation, vacuum drying.
Fig. 1 is the scanning electron microscope (SEM) photograph of the prepared graphene oxide/silver orthophosphate of embodiment 1/P25 composite, we can find out from figure, the P25 nano particle is wrapped on the micron-sized silver orthophosphate particle, simultaneously part P25 particle deposition is also arranged on thin graphene oxide lamella, high-visible micron-sized silver orthophosphate in Fig. 2 transmission electron microscope, the graphene oxide sheet of nanometer P25 particle and covering, Fig. 3 is the X-ray diffractogram of the prepared graphene oxide/silver orthophosphate of embodiment 1/P25 composite, diffraction maximums all in the diffraction pattern are all well corresponding to the silver orthophosphate and the P25 material that respond, less and the diffraction peak intensity of graphene oxide doped amount relatively a little less than, so in X ray diffracting spectrum, do not observe the diffraction maximum that derives from graphene oxide, Fig. 4 is the UV-vis DRS spectrogram of the prepared graphene oxide/silver orthophosphate of embodiment 1/P25 composite, we can find out from figure, this composite all has preferably absorption at whole ultraviolet-visible district (200-800 nm), and absorbance surpasses 0.4.
Embodiment 2-12
The difference of following examples and embodiment 1 is that employed graphene oxide quality, P25 quality, phosphate kind and quality are different, specifically is shown in Table 1, and all the other are with identical described in the embodiment 1.
Table 1
| Embodiment | The graphene oxide quality | The P25 quality | The phosphate kind | The |
| Embodiment | ||||
| 2 | 50 mg | 300 mg | Na 2HPO 4 | 0.426 g |
| Embodiment 3 | 20 mg | 400 mg | Na 2HPO 4 | 0.426 |
| Embodiment | ||||
| 4 | 50 mg | 400 mg | Na 2HPO 4 | 0.426 g |
| Embodiment 5 | 20 mg | 600 mg | Na 2HPO 4 | 0.426 |
| Embodiment | ||||
| 6 | 50 mg | 600 mg | Na 2HPO 4 | 0.426 g |
| Embodiment 7 | 20 mg | 300 mg | NaH 2PO 4 | 0.36 |
| Embodiment | ||||
| 8 | 50 mg | 300 mg | NaH 2PO 4 | 0.36 g |
| Embodiment 9 | 20 mg | 400 mg | NaH 2PO 4 | 0.36 |
| Embodiment | ||||
| 10 | 50 mg | 400 mg | NaH 2PO 4 | 0.36 g |
| Embodiment 11 | 20 mg | 600 mg | NaH 2PO 4 | 0.36 g |
| Embodiment 12 | 50 mg | 600 mg | NaH 2PO 4 | 0.36 g |
| Embodiment 13 | 20 mg | 300 mg | Na 3PO 4 | 0.49 g |
| Embodiment 14 | 50 mg | 300 mg | Na 3PO 4 | 0.49 g |
| Embodiment 15 | 20 mg | 400 mg | Na 3PO 4 | 0.49 g |
| Embodiment 16 | 50 mg | 400 mg | Na 3PO 4 | 0.49 g |
| Embodiment 17 | 20 mg | 600 mg | Na 3PO 4 | 0.49 g |
| Embodiment 18 | 50 mg | 600 mg | Na 3PO 4 | 0.49 g |
Embodiment 19
The composite that embodiment 1-18 is prepared respectively with Escherichia coli, staphylococcus aureus, bacillus pumilus and Pseudomonas aeruginosa co-incubation, carry out flat band method, minimal inhibitory concentration and Minimum Bactericidal.Test method is according to Ministry of Health of the People's Republic of China's " disinfection technology standard " operation, and used bacterial classification is provided by pharmaceutical college of Jiangsu University.
Table 2
Flat band method inhibition zone result of the test is as shown in table 2, People's Republic of China (PRC) industry standard regulation: the compound antibacterial circle diameter can be regarded as without antibiotic effect during less than 7 milliliters; Be weak antibacterial activity between 7-10mm the time between the inhibition zone; Antibacterial circle diameter is better antibacterial activity between 10-20mm the time; Antibacterial circle diameter surpasses 20mm and represents to have very strong antibacterial activity, antibacterial circle diameter is larger, the antibacterial activity that shows this material is better, as can be seen from Table 2: all embodiment for the antibacterial circle diameter of all bacteria tested all more than 10 mm, part antibacterial circle diameter even surpass 20 mm, show that composite has the anti-microbial property of wide spectrum to different strain, and antibacterial activity is excellent.
The result of the test of minimal inhibitory concentration and MBC is as shown in table 3, concentration numerical value is less, represent the restraining and sterilizing bacteria effect better, as can be seen from Table 3, the composite that all embodiment prepare all is no more than 100 ppm to the minimal inhibitory concentration of test bacterial classification, MBC all is no more than 200 ppm, all significantly better than the standard of anti-biotic material 800 ppm of national regulation, shows that prepared composite all has an excellent antibiotic and sterilizing active.
Table 3
In addition, the prepared graphene oxide/silver orthophosphate of simultaneously the present invention/P25 composite is used to the photocatalytic degradation experiment of organic dyestuff rhodamine B, and detailed process and step are as follows:
After graphene oxide/silver orthophosphate of 50 mg/P25 compound material ultrasound being scattered in the rhodamine B solution of 100 milliliter of 25 ppm ultrasonic 10 minutes, the dispersion liquid that mixes is transferred in the quartzy bottle in the xenon lamp catalytic reactor, stirring was opened xenon source after making it reach adsorption equilibrium in 30 minutes under the dark condition, extracting the postradiation mixed dispersion liquid of 4 mL every 2 minutes with syringe transfers in the centrifuge tube of mark, close xenon source behind the radiation of visible light certain hour, with the sample centrifugation in all centrifuge tubes, centrifugal rear resulting supernatant liquor is further transferred in the quartz colorimetric utensil at ultraviolet-visible spectrophotometer and is measured absorbance under the different photocatalysis time, thereby obtains the photocatalytic degradation curve map to rhodamine B under radiation of visible light of composite under each time period.
Fig. 5 is the prepared graphene oxide/silver orthophosphate of embodiment 1/P25 composite photocatalytic degradation curve map to rhodamine B under the visible light condition, as can be seen from Figure 5, this composite surpasses 80% to the degradation rate of rhodamine B at radiation of visible light after 2 minutes, radiation of visible light after 6 minutes the degradation rate to methylene blue be 100%, the photocatalytic degradation curve map shows that graphene oxide/silver orthophosphate/P25 composite has preferably photocatalytic degradation effect to the organic dyestuff rhodamine B under radiation of visible light.
Claims (3)
1. graphene oxide/silver orthophosphate/P25 composite, it is characterized in that: described composite is formed by graphene oxide, silver orthophosphate and three kinds of Material claddings of P25, wherein average-size is that the P25 nano particle of 2-30nm is wrapped in the silver orthophosphate particle surface that particle diameter is 200-400nm, and the P25 of nanometer and micron-scale, silver orthophosphate particle all are deposited on graphene oxide lamella surface; Described composite not only has efficient photocatalytic degradation effect to the organic dyestuff rhodamine B under excited by visible light: the 2 minutes degradation rates of rhodamine B solution to 25 ppm are degradable above 80%, 6 minute; And Escherichia coli, staphylococcus aureus, bacillus pumilus and Pseudomonas aeruginosa are had a bactericidal activity of wide spectrum: antibacterial circle diameter 〉=10 mm, minimal inhibitory concentration≤100 ppm, MBC is ppm all≤200.
2. a kind of graphene oxide/silver orthophosphate as claimed in claim 1/P25 composite manufacture method is characterized in that comprising the steps:
(1) graphene oxide is dissolved in deionized water for ultrasonic and obtains the graphene oxide dispersion liquid that concentration is 0.04-0.1 wt%;
(2) silver nitrate and P25 are dissolved in the deionized water, obtain the mixed solution A of silver nitrate and P25 after the ultrasonic processing, the concentration of silver nitrate is 0.15 mol/L in the mixed solution A, and the concentration of P25 is 0.5-1.5wt%; Mixed solution A is added drop-wise under the magnetic agitation condition in the above-mentioned graphene oxide dispersion liquid, and the mass ratio of graphene oxide and P25 is 1:6 ~ 30, dropwises rear solution and at room temperature continues to stir 30 ~ 60 min, obtains mixing precursor solution B;
(3) phosphate is dissolved in the deionized water, obtains the phosphate solution that concentration is 0.15 mol/L;
(4) phosphate solution that under the condition of magnetic agitation step (3) is prepared dropwise slowly adds among the mixing precursor solution B of step (2) preparation, until occur the celadon muddiness in the reaction system, dropwising rear mixed solution continues to stir behind 30 ~ 60 min still aging, after using absolute ethyl alcohol and deionized water cyclic washing repeatedly after the product centrifugation, vacuum drying obtains graphene oxide/silver orthophosphate/P25 composite.
3. a kind of graphene oxide/silver orthophosphate as claimed in claim 2/P25 composite manufacture method, it is characterized in that: described phosphate comprises sodium hydrogen phosphate, sodium dihydrogen phosphate and sodium phosphate.
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