CN103599802A - Preparation method of silver phosphate/graphene nanocomposite - Google Patents
Preparation method of silver phosphate/graphene nanocomposite Download PDFInfo
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Abstract
The invention discloses a preparation method of a silver phosphate/graphene nanocomposite. The method has the advantages that a light-assisted reducing process is adopted, the process is simple, and the cost is low, so that the method is suitable for large-scale production and industrial production. The prepared silver phosphate/graphene nanocomposite consists of silver phosphate nanoparticles and graphene nanosheets, wherein the graphene nanosheets cover the surfaces of the spherical silver phosphate nanoparticles with sizes of about 200nm, and the two are in close interface contact. The silver phosphate/graphene nanocomposite disclosed by the invention is a novel visible-light-driven photocatalyst which is more efficient and stable.
Description
Technical field
The present invention relates to a kind of preparation method of silver orthophosphate/graphene nanocomposite material, belong to nano composite material and photocatalysis technology field.
Background technology
Along with the lasting deterioration of exhaustive exploitation and the natural environment of natural resources, human society is faced with increasingly serious energy shortage, the problems such as environmental pollution.Photocatalysis technology, because required energy consumption is low, simple to operate, nontoxic, non-secondary pollution, is developing solar energy, and the aspects such as sewage disposal have broad application prospects.Semiconductor nano material has opto-electronic conversion effect, it is the basic composition material of photochemical catalyst, yet the photochemical catalyst of practical application is as titanium dioxide, zinc oxide etc. are wide band gap semiconducter mostly, their light absorption wavelength scope is narrow, mainly be positioned at ultra-violet (UV) band, low to the utilization ratio of solar spectrum, photoelectric transformation efficiency is low.Therefore, the efficient visible light catalyst of development of new becomes the focus in catalyst research gradually.
Silver orthophosphate is a kind ofly in 2010, by Ye group, to wait people (Nature Mater., 2010,9,559-564) visible light catalyst that find and that be subject to extensive concern, their research shows that silver orthophosphate has very strong photooxidation ability under radiation of visible light, effectively the organic pollution in photodissociation water or rapid degradation water.But researchers subsequently also find the easy photoetch of silver orthophosphate, poor stability, and silver orthophosphate has certain dissolubility, recovery use difficulty in solution.
Patent of invention (CN102580714 A) has been reported a kind of graphene oxide/silver phosphate composite photocatalyst and preparation method thereof, patent of invention (CN102631939 A) has been reported a kind of Graphene/silver phosphate composite photocatalyst and preparation method thereof, but the composite that these patent reports are crossed some adopt graphene oxide as the substitute of Graphene, electronics is separated poor with transmission performance, some adopts hydrothermal reduction method that Graphene and silver orthophosphate nano particle are mixed, but nanoparticle agglomerates is serious, interface contact is poor, photocatalysis efficiency needs to promote.Up to now, also do not retrieve in the literature about utilizing the auxiliary reducing process of light to prepare the relevant report of silver orthophosphate/Graphene composite nano materials.
Summary of the invention
The object of the invention is for the problems referred to above, a kind of preparation method of silver orthophosphate/graphene nanocomposite material is provided, solved in prior art photocatalysis efficiency low, the problem of poor stability.
For achieving the above object, the present invention has adopted following technical scheme: a kind of preparation method of silver orthophosphate/graphene nanocomposite material, comprises the following steps:
(1) preparation of graphene oxide dispersion liquid: weigh graphene oxide and be dissolved in deionized water, obtaining concentration after ultrasonic being uniformly dispersed is 0.5 mg/ml graphene oxide dispersion liquid;
(2) preparation of disodium phosphate soln: weigh sodium hydrogen phosphate solid and be dissolved in deionized water, obtain the disodium phosphate soln that concentration is 0.01-0.1mol/L after ultrasonic being uniformly dispersed;
(3) preparation of precursor solution: weigh silver nitrate dissolution of solid in graphene oxide dispersion liquid, the concentration of silver nitrate is 0.03-0.3 mol/L, obtains precursor solution A after magnetic agitation is even; The disodium phosphate soln of preparation in step 2 is added drop-wise in the precursor solution A of same volume under lasting magnetic agitation and dark condition, and sodium hydrogen phosphate is 1:3 with the ratio of the amount of substance of silver nitrate, dropwise rear mixed solution and at room temperature continue magnetic agitation 0.5-2 hour, deionized water will be used after sediment centrifugation, absolute ethyl alcohol cleans repeatedly repeatedly, sediment is dissolved in absolute ethyl alcohol after vacuum drying, and after ultrasonic being uniformly dispersed, obtaining concentration is 1-5 mg/ml precursor solution B;
(4) preparation of silver orthophosphate/graphene nanocomposite material: the precursor solution B in step 3 is placed in to illumination 10-30 min under visible ray under magnetic agitation, after illumination finishes by sediment centrifugation, use respectively deionized water, absolute ethyl alcohol repeatedly eccentric cleaning repeatedly, sediment vacuum drying obtains silver orthophosphate/graphene nanocomposite material.
The invention has the beneficial effects as follows: utilize the auxiliary reducing process of light, can simply and effectively silver orthophosphate nano particle and the Graphene with numerous excellent properties be combined with each other, form interface contact closely, not only can suppress photoetch, improve the stability of silver orthophosphate, also, by the separation contributing in photo-generated carrier, improve photoelectric transformation efficiency.Therefore, utilize the synergy between nano material, silver orthophosphate/graphene nanocomposite material is a kind of novel efficient, stable visible light catalyst.
Accompanying drawing explanation
Fig. 1 is the X-ray diffraction picture of silver orthophosphate/graphene nanocomposite material of the present invention;
Fig. 2 is the x-ray photoelectron spectroscopy picture of silver orthophosphate/graphene nanocomposite material of the present invention;
Fig. 3 is the scanning electron microscope diagram sheet of silver orthophosphate/graphene nanocomposite material of the present invention;
Fig. 4 is the transmission electron micrograph of silver orthophosphate/graphene nanocomposite material of the present invention;
Fig. 5 is silver orthophosphate/graphene nanocomposite material of the present invention photocatalytic degradation curve map to rhodamine B during as visible light catalyst.
The specific embodiment
Embodiment 1:
Get 25 mg graphene oxides and be dissolved in 50 ml deionized waters, after ultrasonic being uniformly dispersed, obtaining concentration is 0.5 mg/ml graphene oxide dispersion liquid; Weigh 0.0711g sodium hydrogen phosphate solid and be dissolved in deionized water, after ultrasonic being uniformly dispersed, obtain the disodium phosphate soln that concentration is 0.01mol/L; Weigh 0.2548 g silver nitrate dissolution of solid in above-mentioned graphene oxide dispersion liquid, wherein the concentration of silver nitrate is 0.03 mol/L, after magnetic agitation is even, obtain precursor solution A. is slowly added drop-wise to the above-mentioned disodium phosphate soln of 50 ml in the precursor solution A of 50 ml under lasting magnetic agitation and dark condition, dropwising rear mixed solution at room temperature continues to stir 0.5 hour, deionized water will be used after sediment centrifugation, absolute ethyl alcohol repeatedly eccentric cleaning repeatedly, vacuum drying; Weigh the dried powder of 0.05 g and be dissolved in 50 ml ethanol solutions, after ultrasonic being uniformly dispersed, obtain precursor solution B.Under lasting magnetic agitation condition, precursor solution B is placed in to illumination 10 min under visible ray, after illumination finishes, by sediment centrifugation, uses respectively deionized water, absolute ethyl alcohol repeatedly eccentric cleaning repeatedly, obtains silver orthophosphate/graphene nanocomposite material after vacuum drying.
Fig. 1 is the X-ray diffraction picture of the prepared silver orthophosphate/graphene nanocomposite material of this example, diffraction maximum in figure and cubic system silver orthophosphate fit like a glove, and Graphene due to content in nano composite material seldom, diffraction peak intensity is relatively very weak, cannot observe in the drawings.
Embodiment 2:
Get 25 mg graphene oxides and be dissolved in 50 ml deionized waters, after ultrasonic being uniformly dispersed, obtaining concentration is 0.5 mg/ml graphene oxide dispersion liquid; Weigh 0.3555 g sodium hydrogen phosphate solid and be dissolved in deionized water, after ultrasonic being uniformly dispersed, obtain the disodium phosphate soln that concentration is 0.05 mol/L; Weigh 1.274 g silver nitrate dissolution of solids in above-mentioned graphene oxide dispersion liquid, wherein the concentration of silver nitrate is 0.15 mol/L, after magnetic agitation is even, obtain precursor solution A. is slowly added drop-wise to the above-mentioned disodium phosphate soln of 50 ml in the precursor solution A of 50 ml under lasting magnetic agitation and dark condition, dropwising rear mixed solution at room temperature continues to stir 1 hour, deionized water will be used after sediment centrifugation, absolute ethyl alcohol repeatedly eccentric cleaning repeatedly, vacuum drying.Weigh the dried powder of 0.1 g and be dissolved in 50 ml ethanol solutions, after ultrasonic being uniformly dispersed, obtain precursor solution B.Under lasting magnetic agitation condition, precursor solution B is placed in to illumination 20 min under visible ray, after illumination finishes, by sediment centrifugation, uses respectively deionized water, absolute ethyl alcohol repeatedly eccentric cleaning repeatedly, obtains silver orthophosphate/graphene nanocomposite material after vacuum drying.
Fig. 2 is the x-ray photoelectron spectroscopy picture of the prepared silver orthophosphate/graphene nanocomposite material of this embodiment, as can be seen from the figure oxygen-containing functional group (C-O, C=O) integral area at peak is much smaller than carbon-carbon bond (C-C, C=C) integral area at peak, illustrate that most of oxygen-containing functional groups are removed after the auxiliary reduction of light, graphene oxide is reduced to Graphene effectively.
Embodiment 3:
Get 25 mg graphene oxides and be dissolved in 50 ml deionized waters, after ultrasonic being uniformly dispersed, obtaining concentration is 0.5 mg/ml graphene oxide dispersion liquid; Weigh 0.7107 g sodium hydrogen phosphate solid and be dissolved in deionized water, after ultrasonic being uniformly dispersed, obtain the disodium phosphate soln that concentration is 0.1 mol/L; Weigh 2.548 g silver nitrate dissolution of solids in above-mentioned graphene oxide dispersion liquid, wherein the concentration of silver nitrate is 0.3 mol/L, after magnetic agitation is even, obtain precursor solution A. is slowly added drop-wise to the above-mentioned disodium phosphate soln of 50 ml in the precursor solution A of 50 ml under lasting magnetic agitation and dark condition, dropwising rear mixed solution at room temperature continues to stir 2 hours, deionized water will be used after sediment centrifugation, absolute ethyl alcohol repeatedly eccentric cleaning repeatedly, vacuum drying; Weigh the dried powder of 0.5 g and be dissolved in 50 ml ethanol solutions, after ultrasonic being uniformly dispersed, obtain precursor solution B.Under lasting magnetic agitation condition, precursor solution B is placed in to illumination 30 min under visible ray, after illumination finishes, by sediment centrifugation, uses respectively deionized water, absolute ethyl alcohol repeatedly eccentric cleaning repeatedly, obtains silver orthophosphate/graphene nanocomposite material after vacuum drying.
Fig. 3 is the scanning electron microscope diagram sheet of the prepared silver orthophosphate/graphene nanocomposite material of this example, can clearly find out that graphene nanometer sheet is closely coated on the spherical silver orthophosphate nano grain surface that particle diameter is about 200 nm from figure.
Fig. 4 is the transmission electron micrograph of the prepared silver orthophosphate/graphene nanocomposite material of example, from figure, can clearly find out that the spherical silver orthophosphate nano particle that particle diameter is about 200 nm is closely coated by transparent graphene nanometer sheet, form interface contact closely.
It should be noted that in Fig. 3 and Fig. 4 and all on the surface of silver orthophosphate, found a small amount of silver nano-grain, may be that slight photoetch generation occurs silver orthophosphate in the auxiliary reduction process of light, these silver nano-grains have surface plasma resonance effect, will contribute to the lip-deep carrier of silver orthophosphate excite and produce.
Embodiment 4:
Prepared silver orthophosphate/the graphene nanocomposite material of the present invention can be used as the photocatalytic degradation that visible light catalyst is used to organic dyestuff rhodamine B, and specific experiment process is as follows:
Getting the prepared silver orthophosphate/graphene nano composite nano materials of 25 mg, to be dissolved in 50 ml concentration be in the rhodamine B of 20 mg/ml, the mixed solution obtaining after ultrasonic being uniformly dispersed is transferred in photo catalysis reactor, be placed under dark condition and continue magnetic agitation 30 minutes, when photochemical catalyst and dye molecule reach after adsorption-desorption balance, open the 500W halogen tungsten lamp that is equipped with visible ray filter plate (wavelength >400 nm) and irradiate vertical irradiation mixed solution; Every 5 minutes, with liquid-transfering gun, draw the postradiation mixed solution of 3 ml, transfer in the centrifuge tube of number consecutively mark, after centrifugation, supernatant is further transferred in quartz colorimetric utensil and is utilized the absorbance curve of the mixed solution under measurement of ultraviolet-visible spectrophotometer different time points, thereby draws out silver orthophosphate/graphene nano composite photo-catalyst photocatalytic degradation curve map to rhodamine B under radiation of visible light.
Fig. 5 is silver orthophosphate/graphene nanocomposite material prepared in example 2 photocatalytic degradation curve map to rhodamine B during as visible light catalyst, and the degradation rate of illumination rhodamine B after 30 minutes is 100%.
Claims (1)
1. a preparation method for silver orthophosphate/graphene nanocomposite material, is characterized in that, comprises the following steps:
(1) preparation of graphene oxide dispersion liquid: weigh graphene oxide powder and be dissolved in deionized water, obtaining concentration after ultrasonic being uniformly dispersed is 0.5 mg/ml graphene oxide dispersion liquid;
(2) preparation of disodium phosphate soln: weigh sodium hydrogen phosphate solid and be dissolved in deionized water, obtain the disodium phosphate soln that concentration is 0.01-0.1mol/L after ultrasonic being uniformly dispersed;
(3) preparation of precursor solution: weigh silver nitrate dissolution of solid in graphene oxide dispersion liquid, the concentration of silver nitrate is 0.03-0.3 mol/L, obtains precursor solution A after magnetic agitation is even; The disodium phosphate soln of preparation in step 2 is added drop-wise in the precursor solution A of same volume under lasting magnetic agitation and dark condition, and sodium hydrogen phosphate is 1:3 with the ratio of the amount of substance of silver nitrate, dropwise rear mixed solution and at room temperature continue magnetic agitation approximately 0.5-2 hour, deionized water will be used after sediment centrifugation, absolute ethyl alcohol cleans repeatedly repeatedly, sediment is dissolved in absolute ethyl alcohol after vacuum drying, and after ultrasonic being uniformly dispersed, obtaining concentration is 1-5 mg/ml precursor solution B;
(4) preparation of silver orthophosphate/Graphene/argentum nano composite material: the precursor solution B in step 3 is placed in to illumination approximately 10-30 min under visible ray under magnetic agitation, after illumination finishes by sediment centrifugation, use respectively deionized water, absolute ethyl alcohol repeatedly eccentric cleaning repeatedly, sediment obtains silver orthophosphate/graphene nanocomposite material through vacuum drying.
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| CN106167652A (en) * | 2016-08-29 | 2016-11-30 | 佛山市高明区海帝陶瓷原料有限公司 | A kind of anti-static ceramic ink with leather pattern effect and preparation method thereof |
| CN106242297A (en) * | 2016-08-29 | 2016-12-21 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | A kind of antibacterial and deodouring Ceramic Tiles and preparation method thereof |
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| CN106348600A (en) * | 2016-08-29 | 2017-01-25 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | Method for antibacterial luminous health ceramics and preparing method thereof |
| CN106348601A (en) * | 2016-08-29 | 2017-01-25 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | Radiation-proof healthcare ceramics and preparing method thereof |
| CN106396401A (en) * | 2016-08-29 | 2017-02-15 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | Antistatic health care ceramic and preparation method thereof |
| CN106396405A (en) * | 2016-08-29 | 2017-02-15 | 佛山市高明区明城镇新能源新材料产业技术创新中心 | Photochromic ceramic tile and preparation method thereof |
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| CN102580714A (en) * | 2012-02-09 | 2012-07-18 | 江苏大学 | Graphene oxide/silver phosphate composite visible light catalyst and preparation method thereof |
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Application publication date: 20140226 |