CN104190449B - The preparation method of the hollow nanostructured catalysis material of a kind of Ag/AgCl - Google Patents
The preparation method of the hollow nanostructured catalysis material of a kind of Ag/AgCl Download PDFInfo
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Abstract
The invention belongs to nano material and photocatalysis technology field, be specifically related to the preparation method that a kind of Ag/AgCl is hollow nanostructured.Innovation of the present invention is to adopt the hollow AgCl nanostructured of one pot process, have employed CCl first
4as chlorine source; Reacted in ethanol by silver nitrate and NaOH; take polyvinylpyrrolidone as the crystal seed of protective agent preparation silver; then seed-solution is mixed with carbon tetrachloride; in polytetrafluoroethylene (PTFE) reactor, heated sealed is to 90-100 DEG C; reaction 3-5h; prepare silver chlorate hollow cubic block, and obtain Ag/AgCl hollow nanostructured material by irradiation.Ag/AgCl product prepared by the present invention is the hollow cubic block of rule, and size is even, length of side 800-900nm, inner aperture 500-600nm.This material has good photocatalytic degradation effect to methyl orange under simulated solar irradiation irradiates, and is a kind of desirable catalysis material.This preparation method's technique is simple, easy to operate, reproducible, is easy to industrializing implementation.
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 directly affecting human survival and development, and institute's facing challenges is particularly severe in this respect in China.Photocatalysis technology directly can 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 environment and the most promising approach of energy problem, there is vast potential for future development.The core of photocatalysis technology is catalysis material, and traditional catalysis material generally adopts the metal oxide or sulfide semiconductor compound that have compared with large band gap, and this kind of material has the weak point being difficult to overcome: (l) photoresponse narrow range.Be that traditional catalysis material (band-gap energy is greater than 3.0eV) of representative only just has photocatalytic activity under UV-irradiation with titanium dioxide.And the main energetic of sunshine is visible region (accounting for 46% of solar energy), the energy of ultraviolet region only accounts for 4%.Break the bottleneck of restriction catalysis material application, the photoresponse scope of catalysis material must be widened, improve catalysis material to the utilization rate of visible ray.(2) quantum yield is low.Light-catalysed general principle is that semiconductor produces electron-hole pair under optical excitation, and photo-generate electron-hole is owing to having high reduction and oxidability and can degradation of contaminant or hydrone.But due to the restriction of material itself, the electron-hole pair negligible amounts of generation, or electron-hole pair produces rear compound rapidly, causes the quantum conversion of catalysis material entirety low.Therefore, explore and there is visible light-responded novel semiconductor material system, widen the photoresponse scope of photochemical catalyst, promote that being separated of light induced electron and hole is the research focus of photocatalysis field always.
As everyone knows, the performance of catalysis material and its size, pattern and micro-structural closely related.The appearance structure of catalyst is regulated to be 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, and the raising for catalytic performance has unique advantage.Therefore, controlledly the hollow nanostructured study hotspot having become current nano material and catalytic field is constructed.
Silver halide AgX(X=Cl, Br, I) be the novel catalysis material of a class.Golden cypress marks in 2008 etc. propose the concept of novel plasma catalysis material, and opening one by metal surface plasma bulk effect carries out finishing 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, namely Ag/AgX catalyst has excellent catalytic performance under visible light, and catalytic activity is far away higher than the TiO of N doping
2, and the load of metal A g makes original photosensitive AgX become quite stable.AgX is made hollow Nano particle, its specific area can be increased, 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 the hollow crystallite of Template preparation Ag/AgCl with sodium chloride, and preparing Ag/AgCl with simple one kettle way, hollow nanostructured there is not been reported so far.
There is the defects such as complex process, manufacturing cycle length, the Ag/AgCl pattern obtained and particle diameter systematicness difference in the preparation method that the present invention is directed to current Ag/AgCl catalysis material, proposes the preparation method of the hollow nanostructured catalysis material of a kind of quick, easy Ag/AgCl.Catalysis material prepared by the method can realize the efficient degradation of organic pollution.
Summary of the invention
The present invention adopts the hollow Ag/AgCl nanostructured of one pot process; And adopt carbon tetrachloride as chlorine source first; 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 is formed.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; NaOH is dissolved in absolute ethyl alcohol, forms solution B; Solution B is joined in solution A fast, vigorous stirring 1h, form solution C;
(2) by the solution C that step (1) obtains, mix with carbon tetrachloride, 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 terminates, naturally cools to room temperature;
(3) by the sediment centrifugation that step (2) obtains, then respectively with absolute ethyl alcohol and distilled water washing, vacuum drying, obtains the AgCl hollow cubic block of white;
(4) silver chlorate hollow cubic block is dispersed in water, with 500W tungsten lamp 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 0.6-0.8g/L; PVP concentration is 2.5-7.5g/L; In described solution B, naoh concentration is 0.3-0.6g/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 DEG C, and the reaction time is 3-5h.
The hollow nanostructured catalysis material of silver/silver chlorate prepared by described method, pattern is a cube bulk, length of side 800-900nm, inner aperture 500-600nm.
Technique effect of the present invention is embodied in:
1, adopt silver nitrate and carbon tetrachloride as reactant, one pot process 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 of the Ag/AgCl of preparation is regular, size is even, good dispersion.Compared with traditional non-hollow-core construction Ag/AgCl material, this hollow structure material absorption property significantly strengthens, and has good application prospect in fields such as photocatalysis.
accompanying drawing illustrates:
Fig. 1 is SEM and the transmission electron microscope photo of the hollow nanostructured catalysis material of Ag/AgCl prepared by embodiment 1.
Fig. 2 is the hollow nanostructured XRD collection of illustrative plates of AgCl prepared by embodiment 1.
Fig. 3 is that the hollow nanostructured catalysis material of Ag/AgCl of embodiment 1 preparation is to the photocatalytic degradation curve map of organic dyestuff MO.
Detailed description of the invention
The present embodiment implements under premised on technical solution of the present invention; give detailed embodiment; following non-limiting example is used for explaining and the present invention is described; instead of limit the invention; in the protection domain of spirit of the present invention and claim; the any amendment make the present invention and change, all belong to protection scope of the present invention.
Embodiment 1
0.03g silver nitrate and 0.2gPVP are dissolved in as solution A in 40mL absolute ethyl alcohol, 0.008g NaOH is dissolved in 20mL absolute ethyl alcohol as solution B.B solution is added in solution A, under magnetic agitation, reacts 1h.Add 50mL carbon tetrachloride in above-mentioned solution, be transferred in the steel bomb of 5 25mL tetrafluoroethene inner bags after stirring, 93 DEG C of heating 4h.Product after hydro-thermal reaction, after centrifugation, washs by absolute ethyl alcohol and deionized water respectively, and is placed in the dry 12h of vacuum drying oven 45 DEG C of lucifuges.The product obtained is scattered in deionized water, with 500W tungsten lamp 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 prepared by embodiment 1.Can be observed sample topography for cube bulk, length of side 800-900nm, inner aperture 500-600nm.
Fig. 2 is the hollow nanostructured XRD collection of illustrative plates of AgCl prepared by embodiment 1, and wherein abscissa is the angle of diffraction (2
θ), unit is degree (deg.), and ordinate is diffracted intensity, and unit is a.u..
Silver prepared by the present invention/silver chlorate hollow Nano catalysis material applies to the photocatalysis experiment of organic dyestuff MO, concrete steps are as follows: be scattered in the MO solution of 100mL10ppm by 100mg hollow Nano catalysis material, continue to stir until reach adsorption equilibrium under dark-state.After light-catalyzed reaction starts, extract the postradiation mixed solution of 4mL every 5min syringe, and be transferred in centrifuge tube, centrifugation, utilize ultraviolet-visible spectrophotometer to measure the absorbance of supernatant liquor, with the change of detection reaction liquid concentration.
The silver of Fig. 3 prepared by embodiment 1/silver chlorate hollow Nano catalysis material is to the absorption of MO and photocatalytic degradation curve map, as can be seen from the figure, after reaching adsorption equilibrium, silver/silver chlorate hollow Nano catalysis material is under simulated solar irradiation, 17% is reached to the adsorption ratio of organic dyestuff MO, meanwhile, after illumination 35min the degradation rate of MO more than 95%.
Fig. 3 be embodiment 1 prepare the hollow nanostructured catalysis material of Ag/AgCl to the photocatalytic degradation curve map of organic dyestuff MO, ● be T
25the silver chlorate hollow cubic block of the non-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
0.04g silver nitrate and 0.2gPVP are dissolved in as solution A in 50mL absolute ethyl alcohol, 0.010g NaOH is dissolved in 20mL absolute ethyl alcohol as solution B.B solution is added in solution A, under magnetic agitation, react 1h.Add 35mL carbon tetrachloride in above-mentioned solution, be transferred in the steel bomb of 5 25mL tetrafluoroethene inner bags after stirring, 100 DEG C of heating 3h.The product of hydro-thermal reaction, after centrifugation, washs by absolute ethyl alcohol and deionized water respectively, and is placed in the dry 12h of vacuum drying oven 45 DEG C of lucifuges.The product obtained is scattered in deionized water, with 500W tungsten lamp as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 3
0.04g silver nitrate and 0.2gPVP are dissolved in as solution A in 60mL absolute ethyl alcohol, 0.012g NaOH is dissolved in 20mL absolute ethyl alcohol as solution B.B solution is added in solution A, under magnetic agitation, react 1h.Add 40mL carbon tetrachloride in above-mentioned solution, be transferred in the steel bomb of 3 50mL tetrafluoroethene inner bags after stirring, 90 DEG C of heating 5h.Product after hydro-thermal reaction, through centrifugation, washs by absolute ethyl alcohol and deionized water respectively, and is placed in the dry 12h of vacuum drying oven 45 DEG C of lucifuges.The product obtained is scattered in deionized water, with 500W tungsten lamp as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 4
0.03g silver nitrate and 0.3gPVP are dissolved in as solution A in 40mL absolute ethyl alcohol, 0.008g NaOH is dissolved in 20mL absolute ethyl alcohol as solution B.B solution is added in solution A, under magnetic agitation, react 1h.Add 30mL carbon tetrachloride in above-mentioned solution, be transferred in the steel bomb of 100mL tetrafluoroethene inner bag after stirring, 95 DEG C of heating 5h.Product after hydro-thermal reaction, after centrifugation, washs by absolute ethyl alcohol and deionized water respectively, and is placed in the dry 12h of vacuum drying oven 45 DEG C of lucifuges.The product obtained is scattered in deionized water, with 500W tungsten lamp as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 5
0.04g silver nitrate and 0.3gPVP are dissolved in as solution A in 60mL absolute ethyl alcohol, 0.010g NaOH is dissolved in 30mL absolute ethyl alcohol as solution B.B solution is added solution A, under magnetic agitation, reacts 1h.Add 90mL carbon tetrachloride in above-mentioned solution, be transferred in the steel bomb of 2 100mL tetrafluoroethene inner bags after stirring, 95 DEG C of heating 4h.Product after hydro-thermal reaction, after centrifugation, washs by absolute ethyl alcohol and deionized water respectively, and is placed in the dry 12h of vacuum drying oven 45 DEG C of lucifuges.The product obtained is scattered in deionized water, with 500W tungsten lamp as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 6
0.03g silver nitrate and 0.3gPVP are dissolved in as solution A in 40mL absolute ethyl alcohol, 0.008g NaOH is dissolved in 20mL absolute ethyl alcohol as solution B.B solution is added in solution A, under magnetic agitation, react 1h.Add 60mL carbon tetrachloride in above-mentioned solution, be transferred in the steel bomb of 3 50mL tetrafluoroethene inner bags after stirring, 93 DEG C of heating 4h.Product after hydro-thermal reaction, after high speed centrifugation is separated, washs by absolute ethyl alcohol and deionized water respectively, and is placed in the dry 12h of vacuum drying oven 45 DEG C of lucifuges.The product obtained is scattered in deionized water, with 500W tungsten lamp as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 7
0.03g silver nitrate and 0.2gPVP are dissolved in as solution A in 50mL absolute ethyl alcohol, 0.008g NaOH is dissolved in 20mL absolute ethyl alcohol as solution B.B solution is added in solution A, under magnetic agitation, react 1h.Add 50mL carbon tetrachloride in above-mentioned solution, be transferred in the steel bomb of 3 50mL tetrafluoroethene inner bags after stirring, 93 DEG C of heating 4h.Product after hydro-thermal reaction, after centrifugation, washs by absolute ethyl alcohol and deionized water respectively, and is placed in the dry 12h of vacuum drying oven 45 DEG C of lucifuges.The product obtained is scattered in deionized water, with 500W tungsten lamp as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 8
0.03g silver nitrate and 0.1gPVP are dissolved in as solution A in 40mL absolute ethyl alcohol, 0.008g NaOH is dissolved in 20mL absolute ethyl alcohol as solution B.B solution is added in solution A, under magnetic agitation, react 1h.Add 120mL carbon tetrachloride in above-mentioned solution, be transferred in the steel bomb of 2 100mL tetrafluoroethene inner bags after stirring, 90 DEG C of heating 3h.Product after hydro-thermal reaction, after centrifugation, washs in deionized water with absolute ethyl alcohol respectively, and is placed in the dry 12h of vacuum drying oven 45 DEG C of lucifuges.The product obtained is scattered in deionized water, with 500W tungsten lamp as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 9
0.03g silver nitrate and 0.2gPVP are dissolved in as solution A in 40mL absolute ethyl alcohol, 0.009g NaOH is dissolved in 20mL absolute ethyl alcohol as solution B.B solution is added in solution A, under magnetic agitation, react 1h.Add 40mL carbon tetrachloride in above-mentioned solution, be transferred in the steel bomb of 5 25mL tetrafluoroethene inner bags after stirring, 93 DEG C of heating 4h.Product after hydro-thermal reaction, after centrifugation, washs by absolute ethyl alcohol and deionized water respectively, and is placed in the dry 12h of vacuum drying oven 45 DEG C of lucifuges.The product obtained is scattered in deionized water, with 500W tungsten lamp as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 10
0.03g silver nitrate and 0.2gPVP are dissolved in as solution A in 40mL absolute ethyl alcohol, 0.010g NaOH is dissolved in 20mL absolute ethyl alcohol as solution B.B solution is added in solution A, under magnetic agitation, react 1h.Add 120mL carbon tetrachloride in above-mentioned solution, be transferred in the steel bomb of 2 100mL tetrafluoroethene inner bags after stirring, 95 DEG C of heating 3h.Product after hydro-thermal reaction, after centrifugation, washs by absolute ethyl alcohol and deionized water respectively, and is placed in the dry 12h of vacuum drying oven 45 DEG C of lucifuges.The product obtained is scattered in deionized water, with 500W tungsten lamp as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 11
0.03g silver nitrate and 0.2gPVP are dissolved in as solution A in 50mL absolute ethyl alcohol, 0.010g NaOH is dissolved in 30mL absolute ethyl alcohol as solution B.B solution is added in solution A, under magnetic agitation, react 1h.Add 40mL carbon tetrachloride in above-mentioned solution, be transferred in the steel bomb of 3 50mL tetrafluoroethene inner bags after stirring, 97 DEG C of heating 3h.Product after hydro-thermal reaction, after high speed centrifugation is separated, washs by absolute ethyl alcohol and deionized water respectively, and is placed in the dry 12h of vacuum drying oven 45 DEG C of lucifuges.The product obtained is scattered in deionized water, with 500W tungsten lamp as light source, carries out photoreduction, until system becomes blueness from white, obtains the hollow nanostructured catalysis material of silver/silver chlorate.
Embodiment 12
0.03g silver nitrate and 0.2gPVP are dissolved in as solution A in 40mL absolute ethyl alcohol, 0.010g NaOH is dissolved in 20ml absolute ethyl alcohol as solution B.B solution is added in solution A, under magnetic agitation, react 1h.Add 120mL carbon tetrachloride in above-mentioned solution, be transferred in the steel bomb of 2 100mL tetrafluoroethene inner bags after stirring, 95 DEG C of heating 4h.Product after hydro-thermal reaction, after high speed centrifugation is separated, washs by absolute ethyl alcohol and deionized water respectively, and is placed in the dry 12h of vacuum drying oven 45 DEG C of lucifuges.The product obtained is scattered in deionized water, with 500W tungsten lamp 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; when not deviating from flesh and blood of the present invention, any apparent improvement that those skilled in the art can make, replacement or modification all belong to protection scope of the present invention.
Claims (5)
1. a preparation method for the hollow nanostructured catalysis material of Ag/AgCl, is characterized in that, synthesizes according to following steps:
(1) silver nitrate and polyvinylpyrrolidone PVP are dissolved in absolute ethyl alcohol, form solution A; NaOH is dissolved in absolute ethyl alcohol, forms solution B; Solution B is joined in solution A fast, vigorous stirring 1h, form solution C;
(2) by the solution C that step (1) obtains, mix with carbon tetrachloride, 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, reaction after sealing, after 90-100 DEG C of reaction 3-5h terminates in reactor, naturally cools to room temperature;
(3) by the sediment centrifugation that step (2) obtains, then respectively with absolute ethyl alcohol and distilled water washing, vacuum drying, obtains the AgCl hollow cubic block of white;
(4) silver chlorate hollow cubic block is dispersed in water, with 500W tungsten lamp as light source, carries out photoreduction, until system becomes blueness from white, obtain the hollow nanostructured catalysis material of silver/silver chlorate.
2. the preparation method of the hollow nanostructured catalysis material of a kind of Ag/AgCl according to claim 1, is characterized in that, in step (1), in described solution A, silver nitrate concentration is 0.6-0.8g/L; PVP concentration is 2.5-7.5g/L; In described solution B, naoh concentration is 0.3-0.6g/L.
3. the preparation method of the hollow nanostructured catalysis material of a kind of Ag/AgCl according to claim 1, 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. the preparation method of the hollow nanostructured catalysis material of a kind of Ag/AgCl according to claim 1, is characterized in that, in step (2), the volume ratio of described solution C and carbon tetrachloride is 0.5-2.
5. the preparation method of the hollow nanostructured catalysis material of a kind of Ag/AgCl according to 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 800-900nm, inner aperture 500-600nm.
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| CN105638729B (en) * | 2016-01-18 | 2018-03-20 | 北京林业大学 | A kind of hollow structure spherical silver/chlorination silver composite material and preparation method thereof |
| CN106076372B (en) * | 2016-06-17 | 2018-10-09 | 武汉理工大学 | The preparation method of the efficient hollow octahedra visible-light photocatalysts of Ag/AgCl |
| CN109280423A (en) * | 2018-08-31 | 2019-01-29 | 谭亚 | A kind of preparation method of electrically conductive ink |
| CN112221520B (en) * | 2019-12-10 | 2024-03-29 | 天津科技大学 | Preparation method of silver/silver chloride composite nanocube |
| CN111604068B (en) * | 2020-06-21 | 2022-10-28 | 安徽理工大学 | Ag-AgBr/TiO 2 Method for preparing nano-rod composite array film |
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