CN103769165A - Preparation method and application of surface-loaded linear silver photocatalyst - Google Patents
Preparation method and application of surface-loaded linear silver photocatalyst Download PDFInfo
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- CN103769165A CN103769165A CN201410075403.2A CN201410075403A CN103769165A CN 103769165 A CN103769165 A CN 103769165A CN 201410075403 A CN201410075403 A CN 201410075403A CN 103769165 A CN103769165 A CN 103769165A
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Abstract
The invention provides a preparation method and application of a surface-loaded linear silver photocatalyst, relating to the field of novel catalysts. The preparation method comprises the following steps of sequentially adding a copper microwire, hexamethylenetetramine and polyvinylpyrrolidone into water, and performing ultrasonic oscillation to obtain copper dispersion liquid; adding a silver nitrate aqueous solution into the copper dispersion liquid for displacement reaction; performing centrifugation after the reaction, extracting precipitates, and performing washing, drying and roasting to obtain the surface-loaded linear silver photocatalyst. The preparation method is simple and easy; heating is not required, so that energy resources are saved; the prepared photocatalyst is novel in texture and high in photocatalysis activity, is linearly loaded on the surface of the copper microwire, and can be applied to the degradation of organic pollutants.
Description
Technical field
The present invention relates to new catalyst field, preparation method and the application thereof of concrete a kind of surface-assembled wire silver catalyst.
Background technology
In light-catalysed research, 1972, Japanese scientist Fujishima etc. found TiO
2monocrystalline electricity level can realize photochemical catalyzing (Fujishima, 1972), finds again afterwards nano-TiO
2there is the ability of photocatalysis to degrade organic matter, and have advantages of that higher stability, nontoxic pollution-free etc. are outstanding, obtain extensive and deep research in photocatalysis field.But titanium dioxide is only to ultraviolet-responsive, in order to utilize to a greater extent in sunlight 43% visible ray, people expect to develop more efficient visible-light-responsive photocatalyst.
Summary of the invention
The object of this invention is to provide the preparation method of a kind of surface-assembled wire silver photochemical catalyst, the method is simple, be beneficial to and commercially produce.
Another object of the present invention is to provide surface-assembled wire silver photochemical catalyst prepared by said method, has higher photocatalytic activity under visible ray.
A further object of the present invention is to provide the application of above-mentioned surface-assembled wire silver photochemical catalyst aspect organic pollutant degradation.
A preparation method for surface-assembled wire silver photochemical catalyst, comprises the steps: copper micro wire, methenamine and polyvinylpyrrolidone to be added to the water successively, and ultrasonic concussion, obtains copper dispersion liquid; Silver nitrate aqueous solution is added in described copper dispersion liquid, carry out displacement reaction; After reaction finishes, centrifuging and taking precipitation, washing, dry, roasting, obtains described surface-assembled wire silver catalyst.
Copper simple substance in copper micro wire and the mol ratio of silver nitrate are preferably 1:1-3.In described copper dispersion liquid, the concentration of methenamine is preferably 0.02-0.04mol/L, and the concentration of polyvinylpyrrolidone is preferably 0.4-0.6mmol/L.Described baking temperature is preferably 50-70 ℃, is preferably 1-5h drying time.Described sintering temperature is preferably 400-500 ℃, and roasting time is preferably 1-3h.
Surface-assembled wire silver photochemical catalyst and the application aspect degradable organic pollutant thereof that the present invention also provides described method to prepare.
At room temperature, take water as solvent, under stirring condition, add successively copper micro wire, methenamine, polyvinylpyrrolidone and liquor argenti nitratis ophthalmicus, prepared the wire silver photochemical catalyst in copper micro wire surface-assembled.Reaction of the present invention is to carry out under room temperature (10 ℃-20 ℃) condition, and the reaction time is only 1s-60s, and when reaction finishes, solution becomes black gray expandable from clear, so can change to judge whether reaction finishes according to solution colour.Preparation method of the present invention is simple, does not need heating and the saving energy.Therefore, preparation method of the present invention is conducive to preparation in enormous quantities, and the catalyst of preparing has very high catalytic activity.
Photochemical catalyst prepared by the present invention, has novel pattern, is the wire forming in copper micro wire surface-assembled, decomposition that can efficient catalytic hydrogen peroxide under visible ray, thus greatly accelerate the oxidation Decomposition speed of hydrogen peroxide catalyzed organic pollution.
Accompanying drawing explanation
Fig. 1 is that material 1 amplifies electron microscope (SEM) shape appearance figure of 500 times.
Fig. 2 is that material 1 amplifies electron microscope (SEM) shape appearance figure of 7000 times.
Fig. 3 is that material 1 amplifies electron microscope (SEM) shape appearance figure of 3200 times.
Fig. 4 is the X ray image K-M (XRD) of material 1.
Fig. 5 is the curve map of material 1 catalysis rhodamine B degraded, and wherein A is material 1, and B is body silver mutually, C
0for the initial concentration of Luo Dan Ming B, C is the Luo Dan Ming B concentration value of measuring after 1 catalytic degradation rhodamine B a period of time of material, and t is the time.
The specific embodiment
Room temperature of the present invention is 10 ℃-20 ℃.
Copper micro wire in the present invention refers to the copper cash of Micro-scale length, and its preparation method is that 201310505999.0(is on January 8th, 2014 in open day with application number) application for a patent for invention in positive pentagonal prism shape copper micro wire.
?embodiment 1
Under room temperature, get the water of 30mL, pour in beaker, under stirring condition, add the copper micro wire (molal quantity of copper simple substance is 0.7874mmol) of 0.05g, add again 0.1575g(1.092mmol) methenamine, 0.8g(0.016mmol) polyvinylpyrrolidone (K-30, Chemical Reagent Co., Ltd., Sinopharm Group), ultrasonic oscillation is dispersed in system elemental copper uniformly, obtains copper dispersion liquid.
The silver nitrate aqueous solution that is 3.08% by 10ml mass percentage concentration (0.1872mol/L) is disposable to be poured in copper dispersion liquid, carries out displacement reaction, and reaction temperature is 10 ℃.In the time that solution becomes black gray expandable, reaction finishes, centrifuging and taking precipitation, washing, and dry 5h under 50 ℃ of conditions, then 450 ℃ of roasting 2h obtain material 1.Can find out the silver-colored simple substance that material 1 is pure phase from the X ray image K-M (Fig. 4) of material 1.Can find out from electron microscope (SEM) shape appearance figure (Fig. 1,2 and 3) of material 1, in the surface-assembled of copper micro wire wire silver simple substance.
Embodiment 2
Under room temperature, get the water of 30mL, pour in beaker, under stirring condition, add the copper micro wire (molal quantity of copper simple substance is 0.6236mmol) of 0.0396g, add again 0.1731g(0.0012mol) methenamine, 0.9g(0.018mmol) polyvinylpyrrolidone (K-30, Chemical Reagent Co., Ltd., Sinopharm Group), ultrasonic oscillation is dispersed in system elemental copper uniformly, obtains copper dispersion liquid.
The liquor argenti nitratis ophthalmicus that is 3.08% by 10ml mass percentage concentration (0.1872mol/L) is disposable to be poured in copper dispersion liquid, carries out displacement reaction, and reaction temperature is 15 ℃.In the time that solution becomes black gray expandable, reaction finishes, centrifuging and taking precipitation, washing, and under 70 ℃ of conditions, drying time, 1h was dried, and then 500 ℃ of roasting 1h obtain material 2.Can find out the silver-colored simple substance that material 2 is pure phase from the X ray image K-M (XRD) of material 2.Can find out from electron microscope (SEM) shape appearance figure of material 2, in the surface-assembled of copper micro wire wire silver simple substance.
Embodiment 3
Under room temperature, get the water of 30mL, pour in beaker, under stirring condition, add the copper micro wire (molal quantity of copper simple substance is 1.87mmol) of 0.1189g, add again 0.0865g(0.5998mmol) methenamine, 0.6g(0.012mmol) polyvinylpyrrolidone (K-30), ultrasonic oscillation is dispersed in system elemental copper uniformly, obtains copper dispersion liquid.
The liquor argenti nitratis ophthalmicus that is 3.08% by 10ml mass percentage concentration (0.1872mol/L) is disposable to be poured in copper dispersion liquid, carries out displacement reaction, and reaction temperature is 20 ℃.In the time that solution becomes black gray expandable, reaction finishes, centrifuging and taking precipitation, washing, and under 60 ℃ of conditions, drying time, 3h was dried, and 400 ℃ of roasting 3h obtain material 3.Can find out the silver-colored simple substance that material 3 is pure phase from the X ray image K-M (XRD) of material 3.Can find out from electron microscope (SEM) shape appearance figure of material 3, in the surface-assembled of copper micro wire wire silver simple substance.
Embodiment 4 effects
In photocatalysis experiment, the organic absorption spectrum that is degraded uses ultraviolet-visible spectrophotometer to measure.According to Lambert – Beer law, according to the variation of organic matter characteristic absorption peak intensity, can quantitatively calculate its change in concentration.Because Luo Dan Ming B has a characteristic absorption peak at 553 nm places, so can utilize the variation of absorbance to weigh the change in concentration of Luo Dan Ming B in solution, drafting C/C0 is for the curve of time, to characterize the catalytic activity of photochemical catalyst.
Concrete contrast experiment is as follows: material 1 prepared by embodiment 1 and body mutually silver (commercial filamentary silver, purchased from Xi'an western electrical-optical cable Co., Ltd) do respectively rhodamine B degradation experiment as photochemical catalyst.By 0.1g material 1 or body mutually silver add in 40mL rhodamine B solution (10mg/L), then adding 10ml mass percentage concentration is 30% aqueous hydrogen peroxide solution, add water to 200ml, under visible ray (being greater than 420nm), carry out light-catalyzed reaction, extract reaction solution every a few minutes, after centrifugation, get supernatant liquor, with spectrophotometer detection, according to testing result, make the curve map (Fig. 5) of catalysis rhodamine B degraded.As can be seen from Figure 5, with body mutually compared with silver, material 1 prepared by embodiment 1 is as photochemical catalyst, decomposition that can efficient catalytic hydrogen peroxide under visible ray, thus greatly accelerate the oxidation Decomposition speed of hydrogen peroxide catalyzed rhodamine B organic pollution.
Claims (7)
1. a preparation method for surface-assembled wire silver photochemical catalyst, is characterized in that comprising the steps: copper micro wire, methenamine and polyvinylpyrrolidone are added to the water successively, and ultrasonic concussion, obtains copper dispersion liquid; Silver nitrate aqueous solution is added in described copper dispersion liquid, carry out displacement reaction; After reaction finishes, centrifuging and taking precipitation, washing, dry, roasting, obtains described surface-assembled wire silver catalyst.
2. the preparation method of surface-assembled wire silver photochemical catalyst according to claim 1, is characterized in that copper simple substance in described copper micro wire and the mol ratio of silver nitrate are 1:1-3.
3. the preparation method of surface-assembled wire silver photochemical catalyst according to claim 2, the concentration that it is characterized in that methenamine in described copper dispersion liquid is 0.02-0.04mol/L, the concentration of polyvinylpyrrolidone is 0.4-0.6mmol/L.
4. the preparation method of surface-assembled wire silver photochemical catalyst according to claim 3, is characterized in that described baking temperature is 50-70 ℃, drying time 1-5h.
5. the preparation method of surface-assembled wire silver photochemical catalyst according to claim 4, is characterized in that described sintering temperature is 400-500 ℃, roasting time 1-3h.
6. the surface-assembled wire silver photochemical catalyst that prepared by the described method of one of claim 1-5.
7. the application of surface-assembled wire silver photochemical catalyst aspect degradable organic pollutant described in claim 6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104258876A (en) * | 2014-10-21 | 2015-01-07 | 南京信息工程大学 | Silver micrometer line photocatalyst, and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709791A (en) * | 2005-07-05 | 2005-12-21 | 华东理工大学 | Method for preparing silver nano line |
| CN103252246A (en) * | 2013-06-07 | 2013-08-21 | 南京信息工程大学 | Shuttle-type silver phosphate photocatalyst and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709791A (en) * | 2005-07-05 | 2005-12-21 | 华东理工大学 | Method for preparing silver nano line |
| CN103252246A (en) * | 2013-06-07 | 2013-08-21 | 南京信息工程大学 | Shuttle-type silver phosphate photocatalyst and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| PENG PENG ET AL.: "Room-temperature pressureless bonding with silver nanowire paste: towards organic electronic and heat-sensitive functional devices packaging", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
| PENG PENG ET AL.: "Room-temperature pressureless bonding with silver nanowire paste: towards organic electronic and heat-sensitive functional devices packaging", 《JOURNAL OF MATERIALS CHEMISTRY》, vol. 22, 31 December 2012 (2012-12-31), pages 12997 - 13001 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104258876A (en) * | 2014-10-21 | 2015-01-07 | 南京信息工程大学 | Silver micrometer line photocatalyst, and preparation method and application thereof |
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