CN102861600B - 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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- CN102861600B CN102861600B CN201210380447.7A CN201210380447A CN102861600B CN 102861600 B CN102861600 B CN 102861600B CN 201210380447 A CN201210380447 A CN 201210380447A CN 102861600 B CN102861600 B CN 102861600B
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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 phosphate// P25 composite and preparation method thereof, refer to that a kind of solution system ion-exchange based on electric charge self assembly prepares the method for graphene oxide/silver phosphate// P25 composite especially, belong 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 (being only limitted to ultraviolet region), quantum efficiency are lower, and particularly its visible light-responded degree is low causes it photocatalytic activity is limited under visible light illumination; Guo etc. [
nat Mater, 2010,9,559-564] report under excited by visible light, silver orthophosphate 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, thus shows excellent visible light photocatalysis active; In addition silver orthophosphate is as a kind of compound of silver, and silver orthophosphate also has good bactericidal activity, but preparing the compound that silver orthophosphate employs argentiferous makes preparation cost higher, and all bigger than normal and pattern of the size of the silver orthophosphate material prepared in addition is difficult to control.
Graphene oxide is a kind of two-dimensional sheet nano material, there is 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 preparation of composite, its surface with negative electrical charge can not only provide more reflecting point for positively charged silver ion, thus the coring and increment of silver orthophosphate can be controlled the surface at graphene oxide, thus reach the effect effectively controlling silver orthophosphate size and pattern; On the other hand due to dissolution dispersity that Graphene is good, it significantly can improve the dispersing and dissolving performance of composite with effective compound of silver orthophosphate, along with the reduction of the improvement and cost of preparing graphene oxide technique, the cost preparing graphene oxide/silver phosphate/composite also can be made greatly to reduce.
P25 is the titanic oxide material of a kind of rutile-type and Detitanium-ore-type mixing, research shows that its visible light-responded degree is poor, we are by effective compound of silver orthophosphate and P25, construct the silver orthophosphate/P25 heterojunction structure of micro nano structure, widen material further to the absorption of visible ray and utilization ratio, simultaneously, hydrophilic functional groups large in conjunction with graphene oxide specific area mainly with and the architectural characteristic such as solubility to dispersion is good, preparation size and morphology controllable, there is the multifunctional composite of bactericidal activity of efficient visible light photocatalysis performance, excellence; At present, with graphene oxide, silver nitrate, silver orthophosphate and P25 are that raw material adopts electric charge to drive the solion exchange process of self assembly to prepare graphene oxide/silver phosphate// P25 composite and is applied to photocatalysis degradation organic contaminant and sterilization field has no report.
Summary of the invention
The object of the invention is to develop that a kind of with low cost, method is simple, the technology of preparing of the preparation graphene oxide/silver phosphate// P25 multifunctional composite of environmental protection, the sterilizing that prepared material has good appearance structure, efficiently visible light photocatalysis performance and excellence is active.
Realizing the technical solution adopted in the present invention is: take graphene oxide as presoma, the silver orthophosphate particle of micrometer structure and P25 nano particle are effectively assembled on graphene oxide lamella, 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 its concrete steps are:
(1) graphene oxide is dissolved in deionized water for ultrasonic and obtains the graphene oxide dispersion that concentration is 0.04-0.1 wt%;
(2) be dissolved in deionized water by silver nitrate and P25, obtain the mixed solution A of silver nitrate and P25 after ultrasonic process, in mixed solution A, the concentration of silver nitrate is the concentration of 0.15 mol/L, P25 is 0.5-1.5wt%; Mixed solution A be added drop-wise under magnetic agitation condition in above-mentioned graphene oxide dispersion, the mass ratio of graphene oxide and P25 is 1:6 ~ 30, dropwises rear solution and at room temperature continues stirring 30 ~ 60 min, obtains mixing precursor solution B;
(3) phosphate is dissolved in deionized water, obtains the phosphate solution that concentration is 0.15 mol/L;
(4) phosphate solution prepared by step (3) is dropwise slowly added in mixing precursor solution B prepared by step (2) under the condition of magnetic agitation, until occur in reaction system that celadon is muddy, still aging after dropwising rear mixed solution continuation stirring 30 ~ 60 min, after using absolute ethyl alcohol and deionized water cyclic washing repeatedly after product centrifugation, vacuum drying obtains graphene oxide/silver phosphate// P25 composite.
Phosphate described in step 3 is sodium hydrogen phosphate, sodium dihydrogen phosphate or sodium phosphate.
Compared with prior art, tool of the present invention has the following advantages:
A) due to by graphene oxide for the preparation of process, obtained graphene oxide/Ag
3pO
4/ P25 composite has larger specific area, uniform size and controlled composite construction;
B) graphene oxide composite material utilizing specific area large can not only effectively be adsorbed with organic dye and organic pollution, and effectively can 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, and sunshine utilization rate significantly promotes, and photocatalysis efficiency strengthens, can all kinds of target contaminant of efficient degradation;
D) utilize the synergy between graphene oxide, silver orthophosphate, titanium dioxide, make prepared material have excellent broad-spectrum antibacterial action, common bacteria in environment can be killed fast;
E) process route adopted is simple, raw material is easy to get, with low cost, non-secondary pollution, economical and efficient.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of graphene oxide/silver phosphate// P25 composite;
Fig. 2 is the transmission electron microscope figure of graphene oxide/silver phosphate// P25 composite;
Fig. 3 is the X ray diffracting spectrum of graphene oxide/silver phosphate// P25 composite;
Fig. 4 is the UV-vis DRS spectrogram of graphene oxide/silver phosphate// P25 composite;
Fig. 5 is graphene oxide/silver phosphate// P25 composite photocatalytic degradation curve map to rhodamine B under visible light conditions.
Detailed description of the invention
Illustrate content of the present invention further below in conjunction with specific embodiment, but these embodiments do not limit the scope of the invention.
Embodiment 1
20 mg graphene oxides are scattered in 50 ml deionized water for ultrasonic and within 5 hours, obtain graphene oxide dispersion, take 1.529 g silver nitrates and 300 mg P25 were dissolved in 50 ml deionized water for ultrasonic after 30 minutes, obtain mixed solution A; Mixed solution A is added drop-wise under magnetic stirring in above-mentioned graphene oxide dispersion, after continuation is stirred and obtained mixing precursor solution B half an hour; Take 0.426 g Na
2hPO
4solid is dissolved in 20 ml deionized waters, obtain disodium phosphate soln, under stirring condition, the disodium phosphate soln prepared is added drop-wise in mixing precursor solution B, until occur in reaction system that celadon is muddy, dropwise rear mixed solution continuation stirring still aging after 30 minutes, after using absolute ethyl alcohol and deionized water cyclic washing repeatedly after product centrifugation, vacuum drying.
The scanning electron microscope (SEM) photograph of Fig. 1 graphene oxide/silver phosphate/prepared by embodiment 1/P25 composite, as can be seen from figure we, P25 nano particle is wrapped on micron-sized silver orthophosphate particle, also there is part P25 particle deposition on thin graphene oxide lamella simultaneously, high-visible micron-sized silver orthophosphate in Fig. 2 transmission electron microscope, the graphene oxide sheet of nanometer P25 particle and covering, the X-ray diffractogram of Fig. 3 graphene oxide/silver phosphate/prepared by embodiment 1/P25 composite, diffraction maximums all in diffraction pattern all well corresponds to silver orthophosphate and the P25 material of response, graphene oxide doped amount is less and diffraction peak intensity is relatively weak, so do not observe the diffraction maximum deriving from graphene oxide in X ray diffracting spectrum, the UV-vis DRS spectrogram of Fig. 4 graphene oxide/silver phosphate/prepared by embodiment 1/P25 composite, as can be seen from figure we, this composite all has good absorption at whole ultraviolet-visible district (200-800 nm), absorbance is more than 0.4.
Embodiment 2-12
The difference of following examples and embodiment 1 is that used graphene oxide quality, P25 quality, phosphate kind and quality are different, and be specifically shown in Table 1, all the other are identical with described in embodiment 1.
Table 1
| Embodiment | Graphene oxide quality | P25 quality | Phosphate kind | Phosphate quality |
| Embodiment 2 | 50 mg | 300 mg | Na 2HPO 4 | 0.426 g |
| Embodiment 3 | 20 mg | 400 mg | Na 2HPO 4 | 0.426 g |
| Embodiment 4 | 50 mg | 400 mg | Na 2HPO 4 | 0.426 g |
| Embodiment 5 | 20 mg | 600 mg | Na 2HPO 4 | 0.426 g |
| Embodiment 6 | 50 mg | 600 mg | Na 2HPO 4 | 0.426 g |
| Embodiment 7 | 20 mg | 300 mg | NaH 2PO 4 | 0.36 g |
| Embodiment 8 | 50 mg | 300 mg | NaH 2PO 4 | 0.36 g |
| Embodiment 9 | 20 mg | 400 mg | NaH 2PO 4 | 0.36 g |
| 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
By the composite prepared by embodiment 1-18 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 bacterial classification used 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's professional standard regulation: can regard as without antibacterial action when compound antibacterial circle diameter is less than 7 milliliters; It is weak antibacterial activity time between inhibition zone between 7-10mm; It is better antibacterial activity when antibacterial circle diameter is between 10-20mm; Antibacterial circle diameter represents to have very strong antibacterial activity more than 20mm, antibacterial circle diameter is larger, show that the antibacterial activity of this material is better, as can be seen from Table 2: all embodiments for the antibacterial circle diameter of all bacteria tested all at 10 more than mm, part antibacterial circle diameter is even more than 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 values is less, represent restraining and sterilizing bacteria effect better, as can be seen from Table 3, the minimal inhibitory concentration of composite to test bacterial classification that all embodiments are prepared all is no more than 100 ppm, MBC is all 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 excellent antibiotic and sterilizing active.
table 3
In addition, the graphene oxide/silver phosphate// P25 composite simultaneously prepared by the present invention is used to the photocatalytic degradation experiment of organic dyestuff rhodamine B, detailed process and step as follows:
The last the graphene oxide/silver phosphate/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 mixed is transferred in the quartzy bottle in xenon lamp catalytic reactor, stir under dark condition after within 30 minutes, making it reach adsorption equilibrium and open xenon source, extracting the postradiation mixed dispersion liquid of 4 mL every 2 minutes with syringe transfers in the centrifuge tube of mark, xenon source is closed after radiation of visible light certain hour, by the sample centrifugation in all centrifuge tubes, centrifugal rear obtained supernatant liquor transfers in quartz colorimetric utensil the absorbance measured on ultraviolet-visible spectrophotometer under the different photocatalysis time further, thus under obtaining each time period composite under visible light illumination to the photocatalytic degradation curve map of rhodamine B.
Fig. 5 graphene oxide/silver phosphate/prepared by embodiment 1/P25 composite under visible light conditions to the photocatalytic degradation curve map of rhodamine B, as can be seen from Figure 5, this composite radiation of visible light after 2 minutes to the degradation rate of rhodamine B more than 80%, be 100% to the degradation rate of methylene blue at radiation of visible light after 6 minutes, photocatalytic degradation curve map shows that graphene oxide/silver phosphate// P25 composite has good photocatalytic degradation effect to organic dyestuff rhodamine B under visible light illumination.
Claims (3)
1. graphene oxide/silver phosphate// P25 composite, it is characterized in that: described composite is formed by graphene oxide, silver orthophosphate and P25 tri-kinds of Material claddings, 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 are all deposited on graphene oxide lamella surface; Described composite not only has efficient photocatalytic degradation effect to organic dyestuff rhodamine B under excited by visible light: to rhodamine B solution 2 minutes degradation rates of 25 ppm more than 80%, 6 minutes degradable; And Escherichia coli, staphylococcus aureus, bacillus pumilus and Pseudomonas aeruginosa are had to the bactericidal activity of wide spectrum: antibacterial circle diameter >=10 mm, minimal inhibitory concentration≤100 ppm, MBC all≤200 ppm.
2. the preparation method of a kind of graphene oxide/silver phosphate// P25 composite as claimed in claim 1, is characterized in that comprising the steps:
(1) graphene oxide is dissolved in deionized water for ultrasonic and obtains the graphene oxide dispersion that concentration is 0.04-0.1 wt%;
(2) be dissolved in deionized water by silver nitrate and P25, obtain the mixed solution A of silver nitrate and P25 after ultrasonic process, in mixed solution A, the concentration of silver nitrate is the concentration of 0.15 mol/L, P25 is 0.5-1.5wt%; Mixed solution A be added drop-wise under magnetic agitation condition in above-mentioned graphene oxide dispersion, the mass ratio of graphene oxide and P25 is 1:6 ~ 30, dropwises rear solution and at room temperature continues stirring 30 ~ 60 min, obtains mixing precursor solution B;
(3) phosphate is dissolved in deionized water, obtains the phosphate solution that concentration is 0.15 mol/L;
(4) phosphate solution prepared by step (3) is dropwise slowly added in mixing precursor solution B prepared by step (2) under the condition of magnetic agitation, until occur in reaction system that celadon is muddy, still aging after dropwising rear mixed solution continuation stirring 30 ~ 60 min, after using absolute ethyl alcohol and deionized water cyclic washing repeatedly after product centrifugation, vacuum drying obtains graphene oxide/silver phosphate// P25 composite.
3. the preparation method of a kind of graphene oxide/silver phosphate// P25 composite as claimed in claim 2, is characterized in that: described phosphate comprises sodium hydrogen phosphate, sodium dihydrogen phosphate and sodium phosphate.
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| CN103480399B (en) * | 2013-09-22 | 2015-06-10 | 江苏大学 | Micronano-structured and silver phosphate based composite visible light catalytic material and preparing method thereof |
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| CN104826639B (en) * | 2015-04-03 | 2016-11-23 | 浙江理工大学 | Silver phosphate/reduced graphene/titanic oxide nano compound material and preparation method |
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| CN109433030B (en) * | 2018-11-23 | 2021-08-10 | 山东大学 | Preparation method of graphene oxide quantum dot-silver phosphate composite material modified reverse osmosis composite membrane |
| CN109759065A (en) * | 2019-01-14 | 2019-05-17 | 中国人民解放军火箭军工程大学 | The laminated film of titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide, preparation method and its application in the treatment of waste water |
| CN115970719A (en) * | 2022-12-19 | 2023-04-18 | 达斯玛环境科技（北京）有限公司 | Magnetic graphene-loaded photocatalyst and preparation method and application thereof |
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