CN104190449A - Preparation method for hollow Ag/AgCl nano-structure photocatalysis material - Google Patents
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Abstract
The invention belongs to the technical fields of nano materials and photocatalysis and particularly relates to a preparation method for a hollow Ag/AgCl nano-structure photocatalysis material. The preparation method is innovatively characterized in that a hollow AgCl nano structure is synthesized by adopting a one-pot method and CCl4 is used as a chlorine source for the first time; silver nitrate and sodium hydroxide react in ethanol in the presence of polyvinylpyrrolidone used as a protective agent to prepare a seed crystal of silver; then a seed crystal solution is uniformly mixed with CCl4 so as to obtain a mixture; the mixture is sealed in a polytetrafluoroethylene reaction kettle, is heated to 90-100 DEG C to have a reaction for three to five hours to prepare a hollow silver chloride cubic block; and the hollow Ag/AgCl nano-structure material is obtained by radiating the hollow silver chloride cubic block. A Ag/AgCl product prepared by the invention is a regular hollow cubic block, is uniform in size and has the edge length being 800nm-900nm and the inner pore diameter being 500nm-600nm. The material has a good photocatalytic degradation effect on methyl orange under the simulated sunlight irradiation and is an ideal photocatalysis material. The preparation method is simple, convenient to operate and good in repeatability and can be put into the industrialized implementation easily.
Description
Technical field
The invention belongs to nano material and photocatalysis technology field, be specifically related to the preparation method of the hollow nanostructured catalysis material of a kind of Ag/AgCl.
Background technology
Environment and the energy are the significant problems that directly affects human survival and development, and the challenge that China faced is in this respect particularly severe.Photocatalysis technology can directly utilize the various organic and inorganic pollution in solar energy degraded and mineralising environment, low-density solar energy can be changed into the storable Hydrogen Energy of high density, be considered to solve one of most promising approach of environment and energy problem, there is vast potential for future development.The core of photocatalysis technology is catalysis material, and general employing of traditional catalysis material has compared with the metal oxide of large band gap or sulfide semiconductor compound, and this class material has the weak point that is difficult to overcome: (l) photoresponse narrow range.Traditional catalysis material that the titanium dioxide of take is representative (band-gap energy is greater than 3.0 eV) only just has photocatalytic activity under UV-irradiation.And the main energy of sunshine is visible region (account for solar energy 46%), the energy of ultraviolet region only accounts for 4%.Break the bottleneck of restriction catalysis material application, must widen the photoresponse scope of catalysis material, improve the utilization rate of catalysis material to visible ray.(2) quantum yield is low.Light-catalysed basic principle is that semiconductor produces electron-hole pair under optical excitation, and light induced electron-hole can degradation of contaminant or hydrone owing to having high reduction and oxidability.But due to the restriction of material itself, the electron-hole pair negligible amounts of generation, or compound rapidly after electron-hole pair generation, cause the quantum conversion of catalysis material integral body low.Therefore, explore the photoresponse scope, the promotion light induced electron that have visible light-responded novel semiconductor material system, widen photochemical catalyst is the research focus of photocatalysis field with the separated of hole always.
As everyone knows, the performance of catalysis material and its size, pattern and micro-structural are closely related.The appearance structure that regulates catalyst is to improve the effective ways of its photocatalysis efficiency.In this respect, hollow nanostructured material is owing to having larger specific area and more avtive spot, for the raising of catalytic performance, has unique advantage.Therefore, controlledly construct the hollow nanostructured study hotspot that has become current nano material and catalytic field.
Silver halide AgX(X=Cl, Br, I) be the novel catalysis material of a class.Golden cypress marks in 2008 etc. have proposed the concept of novel plasma catalysis material, and having opened up one carries out finishing by metal surface plasma bulk effect to conductor photocatalysis material, and then improve the new way of catalysis material performance.After a certain amount of metal A g of AgX area load, due to the surface plasmon resonance effect of Ag, Ag/AgX catalyst has excellent catalytic performance under visible ray, the TiO that catalytic activity is adulterated higher than nitrogen far away
2, and the load of metal A g makes original photosensitive AgX quite stable that becomes.AgX is made to hollow Nano particle, can increase its specific area, and grain surface activity improves greatly, be conducive to its absorption to organic pollution, effectively improve its photocatalytic activity simultaneously.At present, the preparation method of Ag/AgCl hollow-core construction rarely has report, and an only example is to be that template is prepared the hollow crystallite of Ag/AgCl with sodium chloride, and prepares the hollow nanostructured report that there is not yet so far of Ag/AgCl with simple one kettle way.
The preparation method who the present invention is directed to current Ag/AgCl catalysis material exists that complex process, manufacturing cycle are long, the Ag/AgCl pattern that obtains and the defect such as particle diameter systematicness is poor, proposes a kind of preparation method of quick, the easy hollow nanostructured catalysis material of Ag/AgCl.Catalysis material prepared by the method can be realized the efficient degradation of organic pollution.
Summary of the invention
The present invention adopts one kettle way to synthesize hollow Ag/AgCl nanostructured; And adopt first carbon tetrachloride as chlorine source; The Nano silver grain that Ag/AgCl catalysis material of the present invention is formed by hollow square shape silver chlorate and its surface in situ forms.The preparation method of described catalyst, comprises the following steps:
(1) silver nitrate and protective agent polyvinylpyrrolidone (PVP) are dissolved in absolute ethyl alcohol, form solution A; Dissolution of sodium hydroxide, in absolute ethyl alcohol, is formed to solution B; Solution B is joined in solution A fast, and vigorous stirring 1 h, forms solution C;
(2) solution C step (1) being obtained, mixes with carbon tetrachloride, and mixed liquor is transferred in the polytetrafluoroethylliner liner of stainless steel cauldron, and liquid volume accounts for 4/5 of inner bag volume.Inner bag is placed in stainless steel outer sleeve, and after sealing, reaction, after reaction kettle for reaction finishes, naturally cools to room temperature;
(3) sediment centrifugation step (2) being obtained, then, respectively with absolute ethyl alcohol and distilled water washing, vacuum drying, obtains white AgCl hollow cubic block;
(4) silver chlorate hollow cubic block is dispersed in water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtain the hollow nanostructured catalysis material of silver/silver chlorate.
In step (1), in described solution A, silver nitrate concentration is 0.6-0.8 g/L; PVP concentration is 2.5-7.5 g/L; In described solution B, naoh concentration is 0.3-0.6 g/L.
In step (1), in described solution C, the mol ratio of silver nitrate and NaOH is 0.7-1.0.
In step (2), the volume ratio of described solution C and carbon tetrachloride is 0.5-2.
In step (2), the reaction temperature in described reactor is 90-100 ℃, and the reaction time is 3-5 h.
The hollow nanostructured catalysis material of silver/silver chlorate prepared by described method, pattern is a cube bulk, length of side 800-900 nm, inner aperture 500-600 nm.
Technique effect of the present invention is embodied in:
1, adopt silver nitrate and carbon tetrachloride as reactant, one kettle way has synthesized silver chlorate hollow cubic block.Reaction condition is gentle, and operating procedure is simple, and raw material is easy to get, and is easy to industrializing implementation.
2, the hollow nanostructured pattern rule of the Ag/AgCl of preparation, big or small even, good dispersion.Compare with traditional non-hollow-core construction Ag/AgCl material, this hollow structure material absorption property significantly strengthens, and in fields such as photocatalysis, has good application prospect.
accompanying drawing explanation:
Fig. 1 is SEM and the transmission electron microscope photo of the hollow nanostructured catalysis material of Ag/AgCl of embodiment 1 preparation.
Fig. 2 is the hollow nanostructured XRD collection of illustrative plates of AgCl of embodiment 1 preparation.
Fig. 3 is the hollow nanostructured catalysis material of Ag/AgCl of the embodiment 1 preparation photocatalytic degradation curve map to organic dyestuff MO.
The specific embodiment
The present embodiment is under prerequisite, to implement take technical solution of the present invention; provided detailed embodiment; following non-limiting example is used for the present invention that explains; rather than limit the invention; in the protection domain of spirit of the present invention and claim; any modification and change that the present invention is made, all belong to protection scope of the present invention.
Embodiment 1
0.03 g silver nitrate and 0.2 g PVP are dissolved in 40 mL absolute ethyl alcohols as solution A, using 0.008 g dissolution of sodium hydroxide in 20 mL absolute ethyl alcohols as solution B.B solution is added in A solution, under magnetic agitation, reacts 1 h.In above-mentioned solution, add 50 mL carbon tetrachloride, after stirring, be transferred in the steel bomb of 5 25 mL tetrafluoroethene inner bags, 93 ℃ of heating 4 h.Product after hydro-thermal reaction, after centrifugation, respectively with absolute ethyl alcohol and deionized water washing, and is placed in dry 12 h of 45 ℃ of lucifuges of vacuum drying oven.The product of obtaining is scattered in deionized water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Fig. 1 is SEM and the transmission electron microscope photo of the hollow nanostructured catalysis material of Ag/AgCl of embodiment 1 preparation.Can be observed sample topography for cube bulk, length of side 800-900 nm, inner aperture 500-600 nm.
Fig. 2 is the hollow nanostructured XRD collection of illustrative plates of AgCl of embodiment 1 preparation, and wherein abscissa is the angle of diffraction (2
θ), unit is degree (deg.), and ordinate is diffracted intensity, and unit is a.u..
Prepared silver/silver chlorate hollow Nano the catalysis material of the present invention applies to the photocatalysis experiment of organic dyestuff MO, concrete steps are as follows: 100 mg hollow Nano catalysis materials are scattered in the MO solution of 100 mL 10 ppm, under dark state, continue to stir until reach adsorption equilibrium.After light-catalyzed reaction starts, extract the postradiation mixed solution of 4 mL, and be transferred in centrifuge tube every 5 min with syringe, centrifugation, utilizes ultraviolet-visible spectrophotometer to measure the absorbance of supernatant liquor, with the variation of detection reaction liquid concentration.
Fig. 3 is that the prepared silver/silver chlorate hollow Nano catalysis material of embodiment 1 is to the absorption of MO and photocatalytic degradation curve map, as can be seen from the figure, reach after adsorption equilibrium, silver/silver chlorate hollow Nano catalysis material is under simulated solar irradiation, absorption ratio to organic dyestuff MO reaches 17%, meanwhile, after illumination 35min, the degradation rate of MO surpasses 95%.
Fig. 3 is the hollow nanostructured catalysis material of Ag/AgCl of the embodiment 1 preparation photocatalytic degradation curve map to organic dyestuff MO, ● be T
25the silver chlorate hollow cubic block of not irradiation of, ▲ be, ■ is Ag/AgCl sample.Abscissa is the catalytic reaction time, and unit is minute; Ordinate be MO residual concentration (
c) and original concentration (
c 0) ratio (
c/
c 0).
Embodiment 2
0.04 g silver nitrate and 0.2 g PVP are dissolved in 50 mL absolute ethyl alcohols as solution A, using 0.010 g dissolution of sodium hydroxide in 20 mL absolute ethyl alcohols as solution B.B solution is added in A solution, under magnetic agitation, react 1 h.In above-mentioned solution, add 35mL carbon tetrachloride, after stirring, be transferred in the steel bomb of 5 25 mL tetrafluoroethene inner bags, 100 ℃ of heating 3 h.The product of hydro-thermal reaction, after centrifugation, respectively with absolute ethyl alcohol and deionized water washing, and is placed in dry 12 h of 45 ℃ of lucifuges of vacuum drying oven.The product of obtaining is scattered in deionized water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 3
0.04 g silver nitrate and 0.2 g PVP are dissolved in 60 mL absolute ethyl alcohols as solution A, using 0.012 g dissolution of sodium hydroxide in 20 mL absolute ethyl alcohols as solution B.B solution is added in A solution, under magnetic agitation, react 1 h.In above-mentioned solution, add 40 mL carbon tetrachloride, after stirring, be transferred in the steel bomb of 3 50 mL tetrafluoroethene inner bags, 90 ℃ of heating 5 h.Product after hydro-thermal reaction, through centrifugation, respectively with absolute ethyl alcohol and deionized water washing, and is placed in dry 12 h of 45 ℃ of lucifuges of vacuum drying oven.The product of obtaining is scattered in deionized water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 4
0.03 g silver nitrate and 0.3 g PVP are dissolved in 40 mL absolute ethyl alcohols as solution A, using 0.008 g dissolution of sodium hydroxide in 20 mL absolute ethyl alcohols as solution B.B solution is added in A solution, under magnetic agitation, react 1 h.In above-mentioned solution, add 30mL carbon tetrachloride, after stirring, be transferred in the steel bomb of 100 mL tetrafluoroethene inner bags, 95 ℃ of heating 5 h.Product after hydro-thermal reaction, after centrifugation, respectively with absolute ethyl alcohol and deionized water washing, and is placed in dry 12 h of 45 ℃ of lucifuges of vacuum drying oven.The product of obtaining is scattered in deionized water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 5
0.04 g silver nitrate and 0.3 g PVP are dissolved in 60 mL absolute ethyl alcohols as solution A, using 0.010 g dissolution of sodium hydroxide in 30 mL absolute ethyl alcohols as solution B.B solution is added to A solution, under magnetic agitation, react 1 h.In above-mentioned solution, add 90 mL carbon tetrachloride, after stirring, be transferred in the steel bomb of 2 100 mL tetrafluoroethene inner bags, 95 ℃ of heating 4 h.Product after hydro-thermal reaction, after centrifugation, respectively with absolute ethyl alcohol and deionized water washing, and is placed in dry 12 h of 45 ℃ of lucifuges of vacuum drying oven.The product of obtaining is scattered in deionized water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 6
0.03 g silver nitrate and 0.3 g PVP are dissolved in 40 mL absolute ethyl alcohols as solution A, using 0.008 g dissolution of sodium hydroxide in 20 mL absolute ethyl alcohols as solution B.B solution is added in A solution, under magnetic agitation, react 1 h.In above-mentioned solution, add 60 mL carbon tetrachloride, after stirring, be transferred in the steel bomb of 3 50 mL tetrafluoroethene inner bags, 93 ℃ of heating 4 h.Product after hydro-thermal reaction, after high speed centrifugation separation, respectively with absolute ethyl alcohol and deionized water washing, and is placed in dry 12 h of 45 ℃ of lucifuges of vacuum drying oven.The product of obtaining is scattered in deionized water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 7
0.03 g silver nitrate and 0.2 g PVP are dissolved in 50 mL absolute ethyl alcohols as solution A, using 0.008 g dissolution of sodium hydroxide in 20 mL absolute ethyl alcohols as solution B.B solution is added in A solution, under magnetic agitation, react 1 h.In above-mentioned solution, add 50 mL carbon tetrachloride, after stirring, be transferred in the steel bomb of 3 50 mL tetrafluoroethene inner bags, 93 ℃ of heating 4 h.Product after hydro-thermal reaction, after centrifugation, respectively with absolute ethyl alcohol and deionized water washing, and is placed in dry 12 h of 45 ℃ of lucifuges of vacuum drying oven.The product of obtaining is scattered in deionized water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 8
0.03 g silver nitrate and 0.1 g PVP are dissolved in 40 mL absolute ethyl alcohols as solution A, 0.008 g NaOH is dissolved in 20 mL absolute ethyl alcohols as solution B.B solution is added in A solution, under magnetic agitation, react 1 h.In above-mentioned solution, add 120 mL carbon tetrachloride, after stirring, be transferred in the steel bomb of 2 100 mL tetrafluoroethene inner bags, 90 ℃ of heating 3 h.Product after hydro-thermal reaction, after centrifugation, washs in deionized water with absolute ethyl alcohol respectively, and is placed in dry 12 h of 45 ℃ of lucifuges of vacuum drying oven.The product of obtaining is scattered in deionized water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 9
0.03 g silver nitrate and 0.2 g PVP are dissolved in 40 mL absolute ethyl alcohols as solution A, 0.009 g NaOH is dissolved in 20 mL absolute ethyl alcohols as solution B.B solution is added in A solution, under magnetic agitation, react 1 h.In above-mentioned solution, add 40 mL carbon tetrachloride, after stirring, be transferred in the steel bomb of 5 25 mL tetrafluoroethene inner bags, 93 ℃ of heating 4 h.Product after hydro-thermal reaction, after centrifugation, respectively with absolute ethyl alcohol and deionized water washing, and is placed in dry 12 h of 45 ℃ of lucifuges of vacuum drying oven.The product of obtaining is scattered in deionized water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 10
0.03 g silver nitrate and 0.2 g PVP are dissolved in 40 mL absolute ethyl alcohols as solution A, 0.010 g NaOH is dissolved in 20 mL absolute ethyl alcohols as solution B.B solution is added in A solution, under magnetic agitation, react 1 h.In above-mentioned solution, add 120 mL carbon tetrachloride, after stirring, be transferred in the steel bomb of 2 100 mL tetrafluoroethene inner bags, 95 ℃ of heating 3 h.Product after hydro-thermal reaction, after centrifugation, respectively with absolute ethyl alcohol and deionized water washing, and is placed in dry 12 h of 45 ℃ of lucifuges of vacuum drying oven.The product of obtaining is scattered in deionized water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 11
0.03 g silver nitrate and 0.2 g PVP are dissolved in 50 mL absolute ethyl alcohols as solution A, 0.010 g NaOH is dissolved in 30 mL absolute ethyl alcohols as solution B.B solution is added in A solution, under magnetic agitation, react 1 h.In above-mentioned solution, add 40 mL carbon tetrachloride, after stirring, be transferred in the steel bomb of 3 50 mL tetrafluoroethene inner bags, 97 ℃ of heating 3 h.Product after hydro-thermal reaction, after high speed centrifugation separation, respectively with absolute ethyl alcohol and deionized water washing, and is placed in dry 12 h of 45 ℃ of lucifuges of vacuum drying oven.The product of obtaining is scattered in deionized water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 12
0.03 g silver nitrate and 0.2 g PVP are dissolved in 40 mL absolute ethyl alcohols as solution A, 0.010 g NaOH is dissolved in 20 ml absolute ethyl alcohols as solution B.B solution is added in A solution, under magnetic agitation, react 1 h.In above-mentioned solution, add 120 mL carbon tetrachloride, after stirring, be transferred in the steel bomb of 2 100 mL tetrafluoroethene inner bags, 95 ℃ of heating 4 h.Product after hydro-thermal reaction, after high speed centrifugation separation, respectively with absolute ethyl alcohol and deionized water washing, and is placed in dry 12 h of 45 ℃ of lucifuges of vacuum drying oven.The product of obtaining is scattered in deionized water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Described embodiment is preferred embodiment of the present invention; but the present invention is not limited to above-mentioned embodiment; in the situation that not deviating from flesh and blood of the present invention, any apparent improvement, replacement or modification that those skilled in the art can make all belong to protection scope of the present invention.
Claims (6)
1. a preparation method for the hollow nanostructured catalysis material of Ag/AgCl, is characterized in that, synthetic according to following steps:
(1) silver nitrate and polyvinylpyrrolidone PVP are dissolved in absolute ethyl alcohol, form solution A; Dissolution of sodium hydroxide, in absolute ethyl alcohol, is formed to solution B; Solution B is joined in solution A fast, and vigorous stirring 1 h, forms solution C;
(2) solution C step (1) being obtained, mixes with carbon tetrachloride, and mixed liquor is transferred in the polytetrafluoroethylliner liner of stainless steel cauldron, and liquid volume accounts for 4/5 of inner bag volume; Inner bag is placed in stainless steel outer sleeve, and after sealing, reaction, after reaction kettle for reaction finishes, naturally cools to room temperature;
(3) sediment centrifugation step (2) being obtained, then, respectively with absolute ethyl alcohol and distilled water washing, vacuum drying, obtains white AgCl hollow cubic block;
(4) silver chlorate hollow cubic block is dispersed in water, with 500 W tungsten lamps, as light source, carries out photoreduction, until system becomes blueness from white, obtain the hollow nanostructured catalysis material of silver/silver chlorate.
2. according to the preparation method of the hollow nanostructured catalysis material of a kind of Ag/AgCl described in claim 1, it is characterized in that, in step (1), in described solution A, silver nitrate concentration is 0.6-0.8 g/L; PVP concentration is 2.5-7.5 g/L; In described solution B, naoh concentration is 0.3-0.6 g/L.
3. according to the preparation method of the hollow nanostructured catalysis material of a kind of Ag/AgCl described in claim 1, it is characterized in that, in step (1), in described solution C, the mol ratio of silver nitrate and NaOH is 0.7-1.0.
4. according to the preparation method of the hollow nanostructured catalysis material of a kind of Ag/AgCl described in claim 1, it is characterized in that, in step (2), the volume ratio of described solution C and carbon tetrachloride is 0.5-2.
5. according to the preparation method of the hollow nanostructured catalysis material of a kind of Ag/AgCl described in claim 1, it is characterized in that, the reaction temperature in described reactor is 90-100 ℃, and the reaction time is 3-5 h.
6. according to the preparation method of the hollow nanostructured catalysis material of a kind of Ag/AgCl described in claim 1, it is characterized in that, the hollow nanostructured catalysis material of silver/silver chlorate prepared by described method, pattern is a cube bulk, length of side 800-900 nm, inner aperture 500-600 nm.
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| CN106076372A (en) * | 2016-06-17 | 2016-11-09 | 武汉理工大学 | The efficiently preparation method of the hollow octahedra visible-light photocatalyst of Ag/AgCl |
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