CN102527381A - Preparation method of nano-sized gold/ titanium dioxide compound mesoporous microspheric photocatalyst - Google Patents

Preparation method of nano-sized gold/ titanium dioxide compound mesoporous microspheric photocatalyst Download PDF

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CN102527381A
CN102527381A CN2012100181421A CN201210018142A CN102527381A CN 102527381 A CN102527381 A CN 102527381A CN 2012100181421 A CN2012100181421 A CN 2012100181421A CN 201210018142 A CN201210018142 A CN 201210018142A CN 102527381 A CN102527381 A CN 102527381A
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gold
titanium dioxide
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oil phase
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刘军枫
王冠男
孙晓明
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Beijing University of Chemical Technology
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Abstract

The invention discloses a preparation method of nano-sized gold/titanium dioxide compound mesoporous microspheric photocatalyst, and belongs to the technical field of catalysts. The preparation method comprises the following steps: mixing monodisperse oil-phase titanium dioxide nanocrystal and a monodisperse oil-phase gold nanocrystal in a mass ratio of gold to titanium dioxide of (0.5-15): 100; adding the mixture into an aqueous solution in which sodium dodecyl sulfate is dissolved; crushing the mixture by using an ultrasonic crushing device to obtain a microemulsion; completely evaporating an organic solvent in an oil bath at 50-80 DEG C, centrifugating, eluting and drying; and calcining dried powder to obtain the gold-doped nano-sized titanium dioxide mesoporous sphere. Components of the prepared nano-sized gold/titanium dioxide compound mesoporous microsphere keep respective microscopic shapes; and the two nanocrystals are assembled by the microemulsion method to form a special mesoporous structure, so that the specific surface is large, the mass transfer is easy and the photocatalysis easily occurs on the surface of the catalyst.

Description

The preparation method of a kind of nm of gold/titanium dioxide composite mesopore microsphere photocatalyst
Technical field
The invention belongs to catalyst technical field, the prepared photochemical catalyst of preparation method of a kind of nm of gold/titanium dioxide composite mesopore microsphere photocatalyst can effectively be used for visible light photocatalytic degradation organic dye waste water field.
Background technology
Along with the quickening of process of industrialization, problem of environmental pollution increases the weight of day by day, and wherein water pollutes the extensive attention that particularly causes in the global range.It is any discharging owing to organic pollution that water pollutes most, and there are characteristics not easily separated and degraded in organic matter.The chemical method degradable organic pollutant of development in recent years is a big focus, and wherein photocatalytic degradation has low, the abundant degraded of energy consumption, do not produce advantages such as toxic products.Therefore researching and developing new nano-photocatalyst more efficiently is an important direction handling the organic pollution development from now on.
Research at present photochemical catalyst the most widely is nano-TiO 2Because of its photocatalysis technology technology simple, with low cost; Utilize natural daylight to get final product the catalytic decomposition pollutant; Having characteristics such as high catalytic activity, good chemical stability and heat endurance, non-secondary pollution, nonirritant, safety non-toxic, and can be of value to the ecological natural environment for a long time, is one of environmental protection catalyst that has most DEVELOPMENT PROSPECT.But from TiO 2Utilize the efficient of solar energy, also have many shortcomings: the one, to light to absorb wave-length coverage narrow, mainly at ultraviolet region, visible and infrared light district are not had photocatalysis performance, light utilization efficiency is low; The 2nd, the semiconductor carriers recombination rate is high, and quantum efficiency is lower.Because common titanium dioxide can only utilize ultraviolet light, and the energy that the generation of ultraviolet light needs is very high, needs to consume extra energy, and the target of this and energy savings and sustainable development is runed counter to.So high energy consumption has limited titanium dioxide in the application aspect the photocatalysis to the poor efficiency of visible light.
Modification TiO how 2Make it under the exciting of visible light or even indoor light source, produce activity is TiO always 2The focus of photochemical catalyst research.Research shows, a kind of method is through to semi-conducting material TiO 2Carry out (M.Anpo, M.Takeuchi, J.Catal.2003,216,505 such as compound, transient metal doped, the organic dye sensitized and nonmetal doping of semiconductor; R.Asahi, T.Morikawa, T.Ohwaki, K.Aoki, Y.Taga, Science2001,293,269), can improve TiO 2Visible absorption and photocatalysis usefulness.But existing synthetic method can not improve visible light catalysis activity largely.Research show nano particle particularly noble metal gold and silver etc. can be used as a kind of visible light photoactivated dose; Utilize its strong surface plasma resonance effect can help the absorption of catalyst in the ultraviolet-visible-near-infrared spectrum scope, improve the visible light catalysis activity of catalyst with this.But Au/TiO in the existing research 2The research of photocatalytic activity is still very rare.A kind of in addition method is: utilize the physicochemical properties of control titanium dioxide, and size and pattern, design recombination catalyst microcosmic nanostructured increases to improve its photocatalysis performance (C.Chen the surface area of titanium dioxide; Y.Li; Angew.Chem.Int.Ed.2011,50,3725; C.Liu, S.Yang, ACS Nano 2009,3,1025; X.Han, Q.Kuang, M.Jin, Z.Xie, L.Zheng, J.Am.Chem.Soc.2009,131,3152).This kind method mainly is to form special hole, can make fully mass transfer and participate in reacting at catalyst surface of the gas of participating in reaction or liquid.According to above-mentioned two kinds of methods that improve catalyst activity, a kind of desirable light-catalysed synthesizing be both advantages of set, makes it reach synergy.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of nm of gold/titanium dioxide composite mesopore microsphere photocatalyst.The present invention mainly is through design reaction scheme synthesis of nano TiO 2Colloidal spheres, control the fine structure of colloidal spheres, form mesoporously, increasing specific surface area improves TiO to reach 2Photocatalytic activity; Through gold doping nano particle technology, utilize nm of gold to be used for making catalyst under visible light, to excite degradation of organic substances at the plasma resonance of visible region, through some change the visible-light photocatalyst that forms a kind of novelty like this, improve TiO 2Using value, can degradation of sewage curb environmental pollution and reached the purpose of energy efficient.
Mono-dispersed nano gold and titanium dioxide nanocrystalline that the present invention adopts microemulsion method to synthesize in advance are assembled into Au/TiO 2Colloidal spheres is after high-temperature roasting obtains having meso-hole structure, crystallinity good, the nm of gold/titanium dioxide composite mesopore microballoon of Large ratio surface.
For achieving the above object, the present invention adopts following technical scheme:
The preparation method of nm of gold/titanium dioxide composite mesopore microballoon is characterized in that the concrete steps of this method are:
A. utilize the synthetic in advance monodispersed oil phase titanium dioxide nanocrystalline of existing solvent-thermal method.
B. utilize the synthetic in advance monodispersed oil phase gold nanocrystals of existing solvent-thermal method.
C. with step a and the brilliant mixing of two kinds of mono-dispersed nanos of b gained, preferably make gold and TiO 2Mass ratio be (0.5-15): 100, join in the aqueous solution that is dissolved with surfactant, utilize the Ultrasonic Pulverization appearance broken, obtain microemulsion, in 50-80 ℃ of oil bath, make organic solvent evaporation complete, centrifuge washing is dry;
D. step c gained is dry powder is calcined, get final product the mesoporous ball of nano titanium oxide of golden doping.
The synthetic of monodispersed oil phase titanium dioxide nanocrystalline can be with reference to X.L.Li among the step a, Q.Peng, J.X.Yi, X.Wang, Y.Li, Chem.Eur.J.2006,12,2383.Utilization is dissolved in the titanium source in the mixed solution of oleic acid and cyclohexane, adds triethylamine then, stirs, and the volume ratio of oleic acid, cyclohexane and triethylamine is 7: 20: (5-10), obtain a clear solution.This solution is transferred in the water heating kettle of polytetrafluoroethylliner liner, the kettle cover of screwing, high-temperature water heat treatment 12-48h adds the ethanolic solution deposition, and uses cyclohexane Hui Rong, deposition is scattered in obtains monodispersed oil phase titanium dioxide nanocrystalline in the cyclohexane solution;
Further described titanium source is a butyl titanate, and wherein the volume ratio of titanium source and oleic acid is 1: 5-1: 10.The heat treated temperature of high-temperature water is 160-180 ℃.
The synthetic of monodispersed oil phase gold nanocrystals can be with reference to C.M.Shen among the step b, C.Hui, T.Z.Yang, C.W.Xiao, J.F.Tian, L.H.Bao, S.T.Chen, H.Ding, H.J.Gao, Chem.Mater.2008,20,6939.Gold chloride is dissolved in the oleyl amine, processes the oleyl amine solution of gold chloride, get this gold solution and toluene with 1: 1-1: transfer in the water heating kettle after 5 mixing and stirring; Low-temperature hydrothermal is handled 1-12h; After reaction finishes, add the ethanolic solution deposition, and use cyclohexane Hui Rong; Precipitation is dispersed in the cyclohexane, obtains monodispersed gold nanocrystals.
Further, the low-temperature hydrothermal treatment temperature is 80-100 ℃.
Further, the surfactant described in the step c is lauryl sodium sulfate (SDS), the preferred 3g/L of concentration.
Further, the calcination condition described in the steps d is an air atmosphere, 300-400 ℃.
The nm of gold that makes/titanium dioxide composite mesopore microspherical catalyst is applied to the visible light photocatalytic degradation organic dye waste water.In having the reactor of condensing plant, carry out the photocatalysis experiment, add the 50-100mg catalyst in the AO7 solution of 100mL, lucifuge stirs 30-60min and reaches adsorption equilibrium; Open the visible light source irradiation, sampling is centrifugal at regular intervals; Get supernatant liquor; The ultraviolet absorption spectrum of test sample article is drawn out concentration curve over time, whereby to characterize the visible light catalytic effect of the catalyst for preparing.
The invention has the advantages that: the nanocrystalline assembling that (1) utilizes microemulsion method to make monodispersed surface have the oiliness group becomes hydrophilic mesoporous ball; Because the surface can hydrophilicly can make catalyst effectively be dispersed in the water solution system, can also be widely used in aspects such as photodissociation water, solar cell, lithium battery except the photocatalytic applications system.Various component units in nm of gold/titanium dioxide composite mesopore microballoon have kept microscopic pattern separately; And formed special pore structure after utilizing two kinds of this microemulsion method assemblings nanocrystalline; Had big specific surface; Mass transfer is more prone to, and light-catalyzed reaction is taken place at catalyst surface more easily.(2) mix the certain amount of nano gold grain, gold has very strong corrosion resistance in catalytic process, catalyst can be reused.Utilize the plasma resonance effect of nm of gold, the visible light catalysis activity of catalyst is significantly strengthened, having solved traditional catalysis material must be in the problem of catalysis under the ultraviolet light conditions.(3) this invention is effectively combined two kinds of methods that improve the photocatalysis effect, realizes both synergies, makes the cost of disposing of sewage reduce energy savings.
Description of drawings
Fig. 1 is the TEM figure of the prepared structural catalyst of embodiment 1.
Fig. 2 is the TEM figure of the prepared structural catalyst of embodiment 2.
Fig. 3 is that the SEM and the EDX of the prepared structural catalyst of embodiment 2 can spectrogram.
Fig. 4 is the graph of pore diameter distribution of the prepared structural catalyst of embodiment 2.
Fig. 5 is the TEM figure of the prepared structural catalyst of embodiment 3.
Fig. 6 is the TEM figure of the prepared structural catalyst of embodiment 4.
Fig. 7 is the visible light photocatalytic degradation design sketch of the prepared structural catalyst of embodiment 1-4.
The specific embodiment
Below in conjunction with specific embodiment the present invention is further described, but the present invention is not limited to following examples.
Embodiment 1:
A. utilize the synthetic in advance monodispersed oil phase titanium dioxide nanocrystalline of existing solvent-thermal method.The 1mL butyl titanate is dissolved in the mixed solution of 7mL oleic acid and 20mL cyclohexane, adds about 5mL triethylamine then, stir, obtain a clear solution.This solution is transferred in the water heating kettle of polytetrafluoroethylliner liner, the kettle cover of screwing, 160 ℃ of hydrothermal treatment consists 24h of high temperature add the ethanolic solution deposition, and use cyclohexane Hui Rong, obtain monodispersed oil phase titanium dioxide nanocrystalline;
B. utilize the synthetic in advance monodispersed oil phase gold nanocrystals of existing solvent-thermal method.Gold chloride is dissolved in the oleyl amine, processes the oleyl amine solution of 20g/L gold chloride, get this gold solution and toluene and transferred to after the mixing and stirring in the water heating kettle, 90 ℃ of hydrothermal treatment consists 10h of low temperature with 1: 2.After reaction finishes, add the ethanolic solution deposition, and use cyclohexane Hui Rong, obtain monodispersed gold nanocrystals;
C. with step a and two kinds of mono-dispersed nano crystalline substances of b gained with Au: TiO 2Mix at=1: 200, joins in the SDS aqueous solution of 3g/L, utilizes the broken 10min of Ultrasonic Pulverization appearance; Obtain microemulsion, in 70 ℃ of oil baths, make organic solvent evaporation complete, centrifuge washing is dry; The transmission electron microscope photo of gained sample is shown in accompanying drawing 1; The about 100nm of titanium dioxide ball size, the pore that wherein contrast is bigger in the spheroid is a gold nano grain, can see that titanium dioxide nanocrystalline and gold nanocrystals effectively are assembled in the Nano microsphere;
D. step c gained is dry powder is at 350 ℃ of calcinings of Muffle furnace air atmosphere 6h, get final product 0.5% nm of gold/titanium dioxide composite mesopore microballoon.
0.5% nm of gold that makes/titanium dioxide composite mesopore microspherical catalyst is applied to visible light photocatalytic degradation organic dyestuff AO7 simulated sewage.Experiment condition is to add the 50mg catalyst in the AO7 solution of 100mL, and lucifuge stirs 30min and reaches adsorption equilibrium, opens the visible light source irradiation, whenever use the ultraviolet-visible analysis of spectrum at a distance from the 30min sampling, the curve that drafting AO7 concentration reduces in time.Through illumination in four hours, 87.0%AO7 was degraded.This degradation curve is to be denoted as Au0.5/TiO in the accompanying drawing 7 2Curve.
Embodiment 2:
A. utilize the synthetic in advance monodispersed oil phase titanium dioxide nanocrystalline of existing solvent-thermal method.The 1mL butyl titanate is dissolved in the mixed solution of 7mL oleic acid and 20mL cyclohexane, adds about 5mL triethylamine then, stir, obtain a clear solution.This solution is transferred in the water heating kettle of polytetrafluoroethylliner liner, the kettle cover of screwing, high-temperature water heat treatment 24h adds the ethanolic solution deposition, and uses cyclohexane Hui Rong, obtains monodispersed oil phase titanium dioxide nanocrystalline;
B. utilize the synthetic in advance monodispersed oil phase gold nanocrystals of existing solvent-thermal method.Gold chloride is dissolved in the oleyl amine, processes the oleyl amine solution of 20g/L gold chloride, get this gold solution and toluene and transferred to after the mixing and stirring in the water heating kettle with 1: 2, low-temperature hydrothermal is handled 10h.After reaction finishes, add the ethanolic solution deposition, and use cyclohexane Hui Rong, obtain monodispersed gold nanocrystals;
C. with step a and two kinds of mono-dispersed nano crystalline substances of b gained with Au: TiO 2Mix at=1: 100, joins in the aqueous solution of SDS of 3g/L, utilizes the broken 10min of Ultrasonic Pulverization appearance; Obtain microemulsion, in 70 ℃ of oil baths, make organic solvent evaporation complete, centrifuge washing is dry; The transmission electron microscope photo of gained sample is shown in accompanying drawing 2; The about 100nm of titanium dioxide ball size, the pore that wherein contrast is bigger in the spheroid is a gold nano grain, can see that titanium dioxide nanocrystalline and gold nanocrystals effectively are assembled in the Nano microsphere;
D. step c gained is dry powder is at 350 ℃ of calcinings of Muffle furnace air atmosphere 6h, get final product 1% nm of gold/titanium dioxide composite mesopore microballoon.Shown in SEM figure among the accompanying drawing 3A, sample is through after calcining, and spherical structure does not change, and has formed the accumulation hole between ball and the ball.This sample is further done the EDX energy spectrum analysis, and the basic element that obtains sample is formed, and is mainly Ti, O, Au, and wherein gold content probably is 1%.
In order further to confirm the pore structure of 1% nm of gold/titanium dioxide composite mesopore microballoon, accompanying drawing 4 is the graph of pore diameter distribution of this sample, by the N of sample 2The adsorption/desorption data can know that this figure is an IV type curve, and the hole shape that shows sample is an ink bottle type structure, and can know that by graph of pore diameter distribution the aperture is approximately about 5nm, belong to mesoporous, and the specific surface that records this sample is 303m 2g -1
1% nm of gold that makes/titanium dioxide composite mesopore microspherical catalyst is applied to visible light photocatalytic degradation organic dyestuff AO7 simulated sewage.Experiment condition is to add the 50mg catalyst in the AO7 solution of 100mL, and lucifuge stirs 30min and reaches adsorption equilibrium, opens the visible light source irradiation, whenever use the ultraviolet-visible analysis of spectrum at a distance from the 30min sampling, the curve that drafting AO7 concentration reduces in time.Through illumination in four hours, 96.2%AO7 was degraded.This degradation curve is to be denoted as Au1/TiO in the accompanying drawing 7 2Curve.
Embodiment 3:
A. utilize the synthetic in advance monodispersed oil phase titanium dioxide nanocrystalline of existing solvent-thermal method.The 1mL butyl titanate is dissolved in the mixed solution of 7mL oleic acid and 20mL cyclohexane, adds about 5mL triethylamine then, stir, obtain a clear solution.This solution is transferred in the water heating kettle of polytetrafluoroethylliner liner, the kettle cover of screwing, high-temperature water heat treatment 24h adds the ethanolic solution deposition, and uses cyclohexane Hui Rong, obtains monodispersed oil phase titanium dioxide nanocrystalline;
B. utilize the synthetic in advance monodispersed oil phase gold nanocrystals of existing solvent-thermal method.Gold chloride is dissolved in the oleyl amine, processes the oleyl amine solution of 20g/L gold chloride, get this gold solution and toluene and transferred to after the mixing and stirring in the water heating kettle with 1: 2, low-temperature hydrothermal is handled 10h.After reaction finishes, add the ethanolic solution deposition, and use cyclohexane Hui Rong, obtain monodispersed gold nanocrystals;
C. with step a and two kinds of mono-dispersed nano crystalline substances of b gained with Au: TiO 2Mix at=1: 40, joins in the aqueous solution of SDS of 3g/L, utilizes the broken 10min of Ultrasonic Pulverization appearance; Obtain microemulsion, in 70 ℃ of oil baths, make organic solvent evaporation complete, centrifuge washing is dry; The transmission electron microscope photo of gained sample is shown in accompanying drawing five; The about 100nm of titanium dioxide ball size, the pore that wherein contrast is bigger in the spheroid is a gold nano grain, can see that titanium dioxide nanocrystalline and gold nanocrystals effectively are assembled in the Nano microsphere;
D. step c gained is dry powder is at 350 ℃ of calcinings of Muffle furnace air atmosphere 6h, get final product 2.5% nm of gold/titanium dioxide composite mesopore microballoon.
2.5% nm of gold that makes/titanium dioxide composite mesopore microspherical catalyst is applied to visible light photocatalytic degradation organic dyestuff AO7 simulated sewage.Experiment condition is to add the 50mg catalyst in the AO7 solution of 100mL, and lucifuge stirs 30min and reaches adsorption equilibrium, opens the visible light source irradiation, whenever use the ultraviolet-visible analysis of spectrum at a distance from the 30min sampling, the curve that drafting AO7 concentration reduces in time.Through illumination in four hours, 96.5%AO7 was degraded.This degradation curve is to be denoted as Au2.5/TiO in the accompanying drawing 7 2Curve.
Embodiment four:
A. utilize the synthetic in advance monodispersed oil phase titanium dioxide nanocrystalline of existing solvent-thermal method.The 1mL butyl titanate is dissolved in the mixed solution of 7mL oleic acid and 20mL cyclohexane, adds about 5mL triethylamine then, stir, obtain a clear solution.This solution is transferred in the water heating kettle of polytetrafluoroethylliner liner, the kettle cover of screwing, high-temperature water heat treatment 24h adds the ethanolic solution deposition, and uses cyclohexane Hui Rong, obtains monodispersed oil phase titanium dioxide nanocrystalline;
B. utilize the synthetic in advance monodispersed oil phase gold nanocrystals of existing solvent-thermal method.Gold chloride is dissolved in the oleyl amine, processes the oleyl amine solution of 20g/L gold chloride, get this gold solution and toluene and transferred to after the mixing and stirring in the water heating kettle with 1: 2, low-temperature hydrothermal is handled 10h.Add the ethanolic solution deposition, and use cyclohexane Hui Rong, obtain monodispersed gold nanocrystals;
C. with step a and two kinds of mono-dispersed nano crystalline substances of b gained with Au: TiO 2Mix at=1: 20, joins in the aqueous solution of the SDS that is dissolved with 3g/L, utilizes the broken 10min of Ultrasonic Pulverization appearance; Obtain microemulsion, in 70 ℃ of oil baths, make organic solvent evaporation complete, centrifuge washing is dry; The transmission electron microscope photo of gained sample is shown in accompanying drawing six; The about 100nm of titanium dioxide ball size, the pore that wherein contrast is bigger in the spheroid is a gold nano grain, can see that titanium dioxide nanocrystalline and gold nanocrystals effectively are assembled in the Nano microsphere;
D. step c gained is dry powder is at 350 ℃ of calcinings of Muffle furnace air atmosphere 6h, get final product 5% nm of gold/titanium dioxide composite mesopore microballoon.
5% nm of gold that makes/titanium dioxide composite mesopore microspherical catalyst is applied to visible light photocatalytic degradation organic dyestuff AO7 simulated sewage.Experiment condition is to add the 50mg catalyst in the AO7 solution of 100mL, and lucifuge stirs 30min and reaches adsorption equilibrium, opens the visible light source irradiation, whenever use the ultraviolet-visible analysis of spectrum at a distance from the 30min sampling, the curve that drafting AO7 concentration reduces in time.Through illumination in four hours, 91.8%AO7 was degraded.This degradation curve is to be denoted as Au5/TiO in the accompanying drawing 7 2Curve.
To sum up four case along with the increase of golden incorporation, can find out obviously that from four TEM photos the gold content of each sample increases progressively successively.Each case degradation curve gathers contrast and can draw following conclusion in Fig. 7: titanium dioxide (being labeled as P25) and unassembled titanium dioxide nanocrystalline commonly used in (1) industry (are labeled as TiO 2NCs) under visible light, all do not have tangible catalytic activity, mesoporous titanium dioxide microspheres (is labeled as pTiO 2) visible light catalysis activity improve explanation greatly than the above two and utilize microemulsion method to make the brilliant assembling of mono-dispersed nano become hydrophilic mesoporous ball; Formed special pore structure; Had big specific surface, mass transfer is more prone to, and light-catalyzed reaction is taken place at catalyst surface more easily.(2) utilize the plasma resonance effect of nm of gold, the visible light catalysis activity of catalyst is significantly strengthened, having solved traditional catalysis material must be in the problem of catalysis under the ultraviolet light conditions.Can find to strengthen through the contrast of the visible light catalysis activity of sample in four case of this inventive method enforcement along with the increase visible light catalysis activity of golden incorporation; When gold mixes 1%, be the righttest incorporation, surpass the catalytic activity that began to suppress visible light at 2.5% o'clock.Mix a spot of gold and just can reach the effect that improves visible light catalytic.(3) this invention is effectively combined two kinds of methods that improve the photocatalysis effect, realizes both synergies, makes the cost of disposing of sewage reduce energy savings.

Claims (7)

1. the preparation method of nm of gold/titanium dioxide composite mesopore microsphere photocatalyst is characterized in that, may further comprise the steps:
A. utilize the synthetic in advance monodispersed oil phase titanium dioxide nanocrystalline of existing solvent-thermal method;
B. utilize the synthetic in advance monodispersed oil phase gold nanocrystals of existing solvent-thermal method;
C. with step a and the brilliant mixing of two kinds of mono-dispersed nanos of b gained, make gold and TiO 2Mass ratio be (0.5-15): 100, join in the aqueous solution that is dissolved with surfactant, utilize the Ultrasonic Pulverization appearance broken, obtain microemulsion, in 50-80 ℃ of oil bath, make organic solvent evaporation complete, centrifuge washing is dry;
D. step c gained is dry powder is calcined, get final product the mesoporous ball of nano titanium oxide of golden doping;
Described surfactant is lauryl sodium sulfate (SDS).
2. according to the described method of claim 1, it is characterized in that the calcination condition described in the steps d is an air atmosphere, 300-400 ℃.
3. according to the described method of claim 1, it is characterized in that lauryl sodium sulfate (SDS), concentration are 3g/L.
4. according to the described method of claim 1; It is characterized in that; The synthetic method of monodispersed oil phase titanium dioxide nanocrystalline is that the titanium source is dissolved in the mixed solution of oleic acid and cyclohexane, adds triethylamine then, stirs; The volume ratio of oleic acid, cyclohexane and triethylamine is 7: 20: (5-10), obtain a clear solution.This solution is transferred in the water heating kettle of polytetrafluoroethylliner liner the kettle cover of screwing, high-temperature water heat treatment 12-48h; After reaction finishes, add the ethanolic solution deposition, and use cyclohexane Hui Rong, obtain monodispersed oil phase titanium dioxide nanocrystalline.
5. according to the described method of claim 4, it is characterized in that wherein the volume ratio of titanium source and oleic acid is 1: 5-1: 10, the heat treated temperature of high-temperature water is 160-180 ℃.
6. according to the described method of claim 1, it is characterized in that the synthetic of monodispersed oil phase gold nanocrystals is that gold chloride is dissolved in the oleyl amine; Process the oleyl amine solution of gold chloride, get this gold solution and toluene with 1: 1-1: transfer in the water heating kettle after 5 mixing and stirring, low-temperature hydrothermal is handled 1-12h; After reaction finishes; Add the ethanolic solution deposition, and use cyclohexane Hui Rong, obtain monodispersed gold nanocrystals.
7. according to the described method of claim 6, it is characterized in that the low-temperature hydrothermal treatment temperature is 80-100 ℃.
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CN104353456A (en) * 2014-11-14 2015-02-18 上海应用技术学院 Gold-supported titanium dioxide nano-catalyst as well as preparation method and application of gold-supported titanium dioxide nano-catalyst
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CN106519848A (en) * 2016-11-17 2017-03-22 重庆文理学院 Preparation method for nanometer textured paint capable of carrying out photocatalytic purification of aldehyde
CN106519848B (en) * 2016-11-17 2019-08-09 重庆文理学院 A kind of preparation method of the net aldehyde nanometer texture paint of photocatalysis
CN108452800A (en) * 2018-03-27 2018-08-28 中国科学技术大学 The preparation method of nanocrystalline catalyst, preparation method and propylene oxide
CN114540836A (en) * 2022-04-22 2022-05-27 中国长江三峡集团有限公司 Iridium-based multielement composite nano-porous catalyst and preparation method and application thereof
CN114540836B (en) * 2022-04-22 2022-08-02 中国长江三峡集团有限公司 Iridium-based multielement composite nano porous catalyst and preparation method and application thereof
CN116143217A (en) * 2023-01-03 2023-05-23 重庆邮电大学 Preparation method of multifunctional light-heat conversion film with semiconductor-metal nanowire structure

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