CN101327438B - Method for preparing AgI/TiO2 nano compound photocatalyst - Google Patents

Method for preparing AgI/TiO2 nano compound photocatalyst Download PDF

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CN101327438B
CN101327438B CN2008100466701A CN200810046670A CN101327438B CN 101327438 B CN101327438 B CN 101327438B CN 2008100466701 A CN2008100466701 A CN 2008100466701A CN 200810046670 A CN200810046670 A CN 200810046670A CN 101327438 B CN101327438 B CN 101327438B
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agi
solution
lii
tio
catalyst
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CN101327438A (en
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李远志
张华�
郭智敏
赵修建
韩建军
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Wuhan University of Technology WUT
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Abstract

The present invention relates to a preparation method of a nanometer-scale composite photocatalyst. The preparation method of AgI/TiO2 nanometer-scale composite photocatalyst is characterized by comprising the steps as follows: firstly, two raw materials of AgNO3 and LiI.3H2 or LiI are selected for using according to the mol ratio of 1 to 1 of the AgNO3 to the LiI.3H2 or the LiI; secondly, the LiI.3H2 or the LiI is added into waterless ethanol to be processed by ultrasound to be dissolved, solution A with weight concentration of 1 percent to 10 percent is obtained, the AgNO3 is added into thewaterless ethanol to be processed by the ultrasound to be dissolved, solution B with the weight concentration of 0.1 percent to 2 percent is obtained; thirdly, when being stirred by magnetic force, the solution A is dripped into the solution B to be mixed uniformly, butyl titanate is dripped; fourthly, the waterless ethanol is added, water is added for washing and to be dried, calcined and coolednaturally to obtain the AgI/TiO2 nanometer-scale composite photocatalyst. The preparation method has easily obtained raw material and simple technology and is easy to be industrialized; the prepared AgI/TiO2 nanometer-scale composite photocatalyst has stable performance and good visible photocatalysis activity.

Description

AgI/TiO 2The preparation method of nano composite photo-catalyst
Technical field
The present invention relates to a kind of preparation method who is used for the visible light-responded nano composite photo-catalyst of photocatalysis water treatment and air cleaning, belong to nano material and depollution of environment field.
Background technology
In the past 20 years are because nano-TiO 2Low price, nontoxic, have an ability of degrade efficiently toxic gas and sewage, therefore obtained extensive studies.Under the exciting of light, TiO 2The valence band electronics of photochemical catalyst is excited to its conduction band, produces photohole and electronics respectively in valence band and conduction band, and these photo-generated carriers migrate to TiO 2The surface of particle is also caught by surface species (as-OH, adsorbed water and oxygen etc.), and it is extremely strong to generate oxidisability such as hydroxyl radical free radical, the active oxygen species that reactivity is very high, and pollutant (mainly being organic pollution) is oxidized to CO by these active oxygen species 2, H 2O and simple inorganic acid reach the purpose that purifies water and air.
But because its energy gap big (anatase 3.2ev, rutile 3.0ev) can only be excited by ultraviolet radiation.Yet ultraviolet light only accounts for about 5% of solar energy, and 95% sunshine is to TiO 2Photochemical catalyst all is useless, and this point has limited TiO widely 2Application in curbing environmental pollution.So the task of at present crucial also tool challenge is exactly: pass through TiO 2Modification and modification technology obtain visible light-responded photochemical catalyst, and this also is a global hot issue in photocatalysis field.In the past several years, in order to reach this purpose, the scientific worker has carried out a large amount of research, to dwindle energy gap or to improve photostability.These work mainly divide three aspects: (1) transient metal doped TiO 2, as Pt, Au, Ag, Cr, V or the like; (2) non-metallic atom doped Ti O 2, as N, C, S, B, I, Br, F or the like; (3) surface sensitizing of organic dye molecule.As: Chinese patent CN 1565721 has proposed employing colloidal sol～gel method, under lower temperature with nitrogen-doping in titanium dioxide sample, preparation nitrogen doping type titanium dioxide; It is visible light catalyst of matrix and preparation method thereof that Chinese patent CN 1431051 proposes with sial mesopore molecular sieve MCM～41 and AlMCM～41, and the effect of this photochemical catalyst under λ＞420nm visible light is quite active with the ultraviolet light catalyst (Degussa P25) of the marketization; The cyclohexane that proposes with ammonium metavanadate and metatitanic acid fourth fat among the Chinese patent CN 1792425 is an initiation material, in microemulsion system, has synthesized the V with nucleocapsid clad structure through hydro-thermal reaction 2O 5/ TiO 2The preparation method of nano composite material.But still there is following problem: metal-doped TiO 2Instability, the TiO of nonmetal doping 2Absorption coefficient is lower in the visible region, the poisonous and degraded certainly of dyestuff.Therefore seeking and can effectively utilizing the novel composite catalyst of visible light is a challenge that faces at present.
Recently, the TiO by the photosensitive processing of various inorganic material 2Paid close attention to widely, this is because it is more stable and have relatively stronger absorption at visible-range.The I with clad structure of Usseglio etc. (S.Usseglio, A.Damin, D.Scarano, S.Bordiga, A.Zecchina, C.Lamberti, J.Am.Chem.Soc.2007,129,2822.) preparation 2/ TiO 2The catalyst methylene blue of degrading under solar radiation is because I 2Activate TiO 2And make its photocatalytic activity be higher than the commercial P25 (TiO of P25:Degussa company 2Its trade names are P25).Silver halide is well-known photosensitive material, is widely used as photosensitive material.Silver halide is the following variation of main generation in photo-process: absorb a photon and produce a light induced electron and a hole; Light induced electron combines with the lattice silver ion and produces a silver atoms; Constantly absorb photon, finally form silver atom cluster.If photo-process is effectively suppressed, light induced electron and hole can be used for photocatalytic process.This point is confirmed: carriers such as zeolite can come stabilisation of halogenated silver by suppressing photo-process, make it have photocatalytic activity.Bibliographical information be that the AgBr of matrix has visible light catalysis activity and photostability (S.Rodrigues, S.Uma, I.N.Martyanov, K.J.Klabunde, J.Catal.2005,233,405.) with AlMCM-41.Hu etc. are by the AgBr/P25 (TiO of load method preparation 2) and AgI/P25 (TiO 2) photocatalytic activity is highly stable under illumination, and can degrade efficiently nitrogenous dyestuff and killing bacteria (C.Hu, Y.Q.Lan, J.H.Qu, X.X.H u, A.M.Wang, J.Phys.Chem.B2006,110,4066.C.Hu, X.X.Hu, L.S.Wang, J.H.Qu, A.M.Wang, Environ.Sci.Technol.2006,40,7903.).
Summary of the invention
The purpose of this invention is to provide a kind of AgI/TiO 2The preparation method of nano composite photo-catalyst, this preparation method's raw material is easy to get, technology simple, be easy to industrialization, the AgI/TiO that makes 2The nano composite photo-catalyst stable performance, has good visible light catalysis activity.
To achieve these goals, technical scheme of the present invention is as follows: AgI/TiO 2The preparation method of nano composite photo-catalyst is characterized in that it comprises the steps:
1) according to AgNO 3With LiI.3H 2The mol ratio of O or LiI is 1: 1, chooses following two kinds of raw materials: (1) AgNO 3, (2) LiI.3H2O or LiI, standby;
2) with LiI.3H 2O or LiI join in the absolute ethyl alcohol ultrasonic to dissolving, mass concentration is 1%～10% A solution;
With AgNO 3Join in the absolute ethyl alcohol ultrasonic to dissolving, mass concentration is 0.1%～2% B solution;
3) under magnetic agitation, the A drips of solution is added in the B solution, produce yellow mercury oxide, the back of waiting to stir drips metatitanic acid fourth fat; Metatitanic acid fourth fat and AgNO 3Mass ratio be 5.9～61;
4) continuing heating is stirred near doing, 0.5～2h is continued to stir to dried fully in the cooling back, add absolute ethyl alcohol again and make that solids content is 5～10% (quality) in the gained suspension, ultrasonic dispersion adds entry under magnetic agitation, the mass ratio of water and metatitanic acid fourth fat is 0.2～2.0, after Buchner funnel suction filtration, the washing, 90 ℃～150 ℃ baking 1～4h, 300 ℃～500 ℃ roasting 2～4h, 2～20 ℃/min of heating rate gets AgI/TiO naturally after the cooling 2Nano composite photo-catalyst.
The present invention AgI/TiO of method for preparing 2Nano composite photo-catalyst has following characteristics: 1) nanometer Ag I is that (5～30nm), subshell is little metal Ag and simple substance I to kernel 2(0.6nm～1nm), outermost layer is TiO 2(3.7nm); 2) principal crystalline phase of titanium oxide is the anatase phase, and the principal crystalline phase of AgI is β～AgI, and TiO 2Coat AgI and suppress its light decomposition; 3) photochemical catalyst has strong absorption in the visible region, and wherein AgI, Ag, I 2, TiO 2There is synergy between the component, thereby the light induced electron of its generation and hole-recombination rate are descended, therefore have visible light catalysis activity efficiently; 4) in this composite photo-catalyst, nanometer Ag I can stable existence, has good light resistance.
The invention has the beneficial effects as follows: raw materials used being easy to get, preparation technology is simple, be easy to industrialization, has very high practical value; The AgI/TiO that makes 2The nano composite photo-catalyst stable performance, has good visible light catalysis activity; But organic pollution such as dye solution such as efficient degradation crystal violet and parachlorophenol solution under radiation of visible light; Only need solar light irradiation, energy savings.
Description of drawings
(A) among Fig. 1 is the AgI/TiO of embodiment 1 2The TEM figure of nano composite photo-catalyst; (B) be AgI and the TiO of embodiment 1 2The HRTEM figure at nano particle interface.
Fig. 2 is AgI/TiO 2, AgI/P25, P25, AgI/SiO 2, Ag/TiO 2The ultraviolet of powder～visible light diffuse reflection collection of illustrative plates.As can be seen from this figure, P25 does not absorb at visible region, and strong absorption is arranged in the ultra-violet (UV) band, and composite A gI/TiO 2, AgI/P25 all has strong absorption at ultraviolet, visible region, photoresponse is widened visible region from ultraviolet, and new absworption peak occurred about 420 nm, and at whole visible region absorption is arranged all.AgI/SiO 2Very strong absworption peak is also arranged, because SiO near 420nm 2In 200～700nm scope, do not absorb, so near the strong absworption peak of 420nm is owing to the absorption of AgI.Ag/TiO 2Photochemical catalyst has the absorption Bao Feng of disperse at 400～800nm.I 2/ TiO 2Photochemical catalyst also has very strong absorption at 400～800nm.The made AgI/TiO of the present invention in visible region 400～800nm scope 2The absworption peak of nano composite photo-catalyst is apparently higher than AgI/P25.
Fig. 3 is at AgI/TiO 2On the nano composite photo-catalyst, the ultraviolet-visible light absorption of crystal violet solution is with visible light (the variation relation figure of light application time of λ＞420nm).After this figure illustrated radiation of visible light 120min, crystal violet solution did not have absworption peak at visible region, and crystal violet solution is degraded fully.
Fig. 4 is at AgI/TiO 2, AgI/P25, P25, AgI/SiO 2, Ag/TiO 2On the catalyst, the concentration of crystal violet solution is with the variation relation figure of visible light (λ＞420 nm) light application time.
Fig. 5 is at AgI/TiO 2, on the P25, AgI/P25 catalyst, the parachlorophenol solution concentration is with visible light (the variation relation figure of light application time of λ＞420nm).
The specific embodiment
Further set forth substantive distinguishing features of the present invention and obvious improvement below in conjunction with embodiment, but the cited case does not limit protection domain of the present invention.
Embodiment 1:
AgI/TiO 2The preparation method of nano composite photo-catalyst, it comprises the steps:
Take by weighing 0.188g LiI.3H 2O (three hydration lithium iodides), add the 4ml absolute ethyl alcohol ultrasonic to dissolve A solution; Take by weighing 0.169g AgNO 3And add the ultrasonic extremely dissolving of 15ml absolute ethyl alcohol, prepare B solution thus.Under magnetic stirs, the A drips of solution is added in the B solution, produce yellow mercury oxide, drip 1ml metatitanic acid fourth fat after waiting to stir, heating is stirred near doing, and cools off the back and continues to stir 1h to dried fully, add 8ml absolute ethyl alcohol ultrasonic dissolution again, under magnetic agitation, add 1ml water, Buchner funnel suction filtration, the back 90 ℃ of baking 2h of washing, 450 ℃ of roasting 2h, 10 ℃/min of heating rate gets AgI/TiO naturally after the cooling 2Nano composite photo-catalyst.
Fig. 1, Fig. 2 are respectively TEM figure and the ultraviolet～visible light diffuse reflection collection of illustrative plates of embodiment 1.
The AgI/TiO that said method is made 2Nano composite photo-catalyst carries out the visible light photocatalysis performance test.
(1) gets the made AgI/TiO of 0.2000g the present invention 2Nano composite photo-catalyst is put into the 100ml beaker, measures 10ml crystal violet solution (1 * 10 with graduated cylinder ～3The ml/L water as solvent), 40ml distilled water adds beaker, in photocatalysis instrument camera bellows magnetic agitation to adsorption equilibrium, the sampling and measuring initial concentration of solution.On beaker, add a cover the 420nm optical filter then, and open the 125W high-pressure sodium lamp, and pick up counting, respectively at 5min, 10min, 20min, 40min, 60min, 80min, 100min, 120min sampling, after institute's sample thief centrifugation, get supernatant 0.9ml respectively and inject vial, and add the 3ml distilled water diluting respectively.With the absorbance of ultraviolet-uisible spectrophotometer survey crystal violet solution, the comparative catalyst has AgI/P25, P25, AgI/SiO 2, Ag/TiO 2, method is the same, the results are shown in Figure 3, Fig. 4.
(2) get the made AgI/TiO of 0.2000g the present invention 2Nano composite photo-catalyst is put in the 100ml beaker, measures 10ml parachlorophenol solution (1 * 10 with graduated cylinder ～3The ml/L water as solvent), 40ml distilled water adds beaker, in photocatalysis instrument camera bellows magnetic agitation to adsorption equilibrium, the sampling and measuring initial concentration of solution.On beaker, add a cover the 420nm optical filter then, and open the 125W high-pressure sodium lamp, and pick up counting, respectively at 5min, 10min, 20min, 40min, 60min, 80min, 100min, 120min sampling, after institute's sample thief centrifugation, get supernatant 0.9ml respectively and inject vial, and add the 3ml distilled water diluting respectively.Survey the parachlorophenol solution absorbency with ultraviolet-uisible spectrophotometer, the comparative catalyst has AgI/P25, and P25 the results are shown in Figure 5.
Comparative Examples 1
Pure TiO 2: under magnetic agitation and heating, in the 60ml absolute ethyl alcohol, add the 3ml butyl titanate, heating evaporation to volume is 20ml, after being cooled to room temperature, add the 20ml absolute ethyl alcohol, continue to stir and add 3ml distilled water under the room temperature, continue to stir 30min, Buchner funnel suction filtration, the back 90 ℃ of baking 5h of washing, 450 ℃ of roasting 2h, heating rate are 10 ℃/min, get pure TiO naturally after the cooling 2
Comparative Examples 2
Ag/TiO 2: the 1ml concentrated ammonia liquor joins and gets A solution in the 9ml absolute ethyl alcohol; Accurately take by weighing the 0.34g silver nitrate and add the ultrasonic extremely dissolving of 34ml absolute ethyl alcohol, under magnetic agitation,, add the 2ml butyl titanate again to wherein dripping 1.4ml A solution, heating evaporation is to the 10ml, be cooled to room temperature and add 16ml ethanol, and under the magnetic agitation condition, drip 2ml water, continue to stir 10min, the Buchner funnel vacuum filtration, washing, 90 ° of baking 5h, 450 ℃ of roasting 2h, 10 ℃/min of heating rate gets Ag/TiO naturally after the cooling 2
Comparative Examples 3
AgI/P25: accurately take by weighing 0.21g AgNO 3And the concentrated ammonia liquor that adds 2.3ml 25% gets A solution; Take by weighing 1g P25 and add the ultrasonic 20min of 100ml water, 30min is stirred in continuation behind the adding 0.205g KI, adds A solution fast, stirs 16h under the room temperature, the Buchner funnel vacuum filtration, and washing, 90 ℃ of baking 4h get AgI/P25 after cooling off naturally.
Comparative Examples 4
I 2/ TiO 2: take by weighing 0.1gI 2Add the 3g butyl titanate, at room temperature magnetic agitation 36h forms powder, 100 ℃ of baking 2h, and 500 ℃ of roasting 6h, 10 ℃/min of heating rate gets I naturally after the cooling 2/ TiO 2
Comparative Examples 5
AgI/SiO 2: take by weighing 0.42g AgNO 3And the concentrated ammonia liquor that adds 4.6ml 25% gets A solution; Take by weighing 2g SiO 2Add extremely dissolving of the ultrasonic 20min of 200ml distilled water, after adding 0.41gKI continues to stir 30min, to wherein adding A solution (the whole adding), stir 16h under the room temperature fast, the Buchner funnel vacuum filtration washs, and 90 ℃ of baking 4h get SiO naturally after the cooling 2/ AgI.
The photocatalysis performance test, the comparative catalyst has AgI/P25, pure TiO 2, AgI/SiO 2, Ag/TiO 2, I 2/ TiO 2, concrete experimentation is with the visible light photocatalysis performance test (1) among the embodiment 1, and the result is as shown in Figure 4.
The photocatalysis performance test, the comparative catalyst has AgI/P25, P25, concrete experimentation is with the visible light photocatalysis performance test (2) among the embodiment 1, and the result is as shown in Figure 5.
Embodiment 2:
AgI/TiO 2The preparation method of nano composite photo-catalyst, it comprises the steps:
1) according to AgNO 3With the mol ratio of LiI be 1: 1, choose following two kinds of raw materials: (1) AgNO 3, (2) LiI, standby;
2) LiI is joined in the absolute ethyl alcohol ultrasonic to dissolving, mass concentration is 1% A solution;
With AgNO 3Join in the absolute ethyl alcohol ultrasonic to dissolving, mass concentration is 0.1% B solution;
3) under magnetic agitation, the A drips of solution is added in the B solution, produce yellow mercury oxide, the back of waiting to stir drips metatitanic acid fourth fat; Metatitanic acid fourth fat and AgNO 3Mass ratio be 5.9;
4) continuing heating is stirred near doing, 0.5h is continued to stir to dried fully in the cooling back, add absolute ethyl alcohol again and make that solids content is 5% (quality) in the gained suspension, ultrasonic dispersion adds entry under magnetic agitation, the addition of water and metatitanic acid fourth fat mass ratio are 1, Buchner funnel suction filtration, the back 90 ℃ of baking 1h of washing, 450 ℃ of roasting 2h, 10 ℃/min of heating rate gets AgI/TiO naturally after the cooling 2Nano composite photo-catalyst.
Embodiment 3:
AgI/TiO 2The preparation method of nano composite photo-catalyst, it comprises the steps:
1) according to AgNO 3With LiI.3H 2The mol ratio of O is 1: 1, chooses following two kinds of raw materials: (1) AgNO 3, (2) LiI.3H 2O, standby;
2) with LiI.3H 2O joins in the absolute ethyl alcohol ultrasonic to dissolving, mass concentration is 10% A solution;
With AgNO 3Join in the absolute ethyl alcohol ultrasonic to dissolving, mass concentration is 2% B solution;
3) under magnetic agitation, the A drips of solution is added in the B solution, produce yellow mercury oxide, the back of waiting to stir drips metatitanic acid fourth fat; Metatitanic acid fourth fat and AgNO 3Mass ratio be 61;
4) continuing heating is stirred near doing, 2h is continued to stir to dried fully in the cooling back, add absolute ethyl alcohol again and make that solids content is 10% in the gained suspension, ultrasonic dispersion adds entry under magnetic agitation, the addition of water and metatitanic acid fourth fat mass ratio are 2.0, Buchner funnel suction filtration, the back 90 ℃ of baking 4h of washing, 500 ℃ of roasting 4h, 5 ℃/min of heating rate gets AgI/TiO naturally after the cooling 2Nano composite photo-catalyst.
Embodiment 4:
AgI/TiO 2The preparation method of nano composite photo-catalyst, it comprises the steps:
1) according to AgNO 3With the mol ratio of LiI be 1: 1, choose following two kinds of raw materials: (1) AgNO 3, (2) LiI, standby;
2) LiI is joined in the absolute ethyl alcohol ultrasonic to dissolving, mass concentration is 5% A solution;
With AgNO 3Join in the absolute ethyl alcohol ultrasonic to dissolving, mass concentration is 1% B solution;
3) under magnetic agitation, the A drips of solution is added in the B solution, produce yellow mercury oxide, the back of waiting to stir drips metatitanic acid fourth fat; Metatitanic acid fourth fat and AgNO 3Mass ratio be 30;
4) continuing heating is stirred near doing, 1h is continued to stir to dried fully in the cooling back, add absolute ethyl alcohol again and make that solids content is 7% in the gained suspension, ultrasonic dispersion adds entry under magnetic agitation, the addition of water and metatitanic acid fourth fat mass ratio are 0.5, Buchner funnel suction filtration, the back 150 ℃ of baking 3h of washing, 350 ℃ of roasting 3h, 10 ℃/min of heating rate gets AgI/TiO naturally after the cooling 2Nano composite photo-catalyst.
The bound value of each raw material of the present invention, and the bound value of technological parameter (as temperature, time) can both realize the present invention, do not enumerate embodiment one by one at this.

Claims (1)

1.AgI/TiO 2The preparation method of nano composite photo-catalyst is characterized in that it comprises the steps:
1) according to AgNO 3With LiI3H 2The mol ratio of O or LiI is 1: 1, chooses following two kinds of raw materials: (1) AgNO 3, (2) LiI3H 2O or LiI, standby;
2) with LiI3H 2O or LiI join in the absolute ethyl alcohol ultrasonic to dissolving, mass concentration is 1%～10% A solution;
With AgNO 3Join in the absolute ethyl alcohol ultrasonic to dissolving, mass concentration is 0.1%～2% B solution;
3) under magnetic agitation, the A drips of solution is added in the B solution, produce yellow mercury oxide, the back of waiting to stir drips metatitanic acid fourth fat; Metatitanic acid fourth fat and AgNO 3Mass ratio be 5.9～61;
4) continuing heating is stirred near doing, 0.5～2h is continued to stir to dried fully in the cooling back, add absolute ethyl alcohol again and make that solids content is 5～10wt% in the gained suspension, ultrasonic dispersion adds entry under magnetic agitation, the mass ratio of water and metatitanic acid fourth fat is 0.2～2.0, Buchner funnel suction filtration, back 90 ℃～150 ℃ baking 1～4h of washing, 300 ℃～500 ℃ roasting 2～4h, 2 ℃～20 ℃/min of heating rate gets AgI/TiO naturally after the cooling 2Nano composite photo-catalyst.
CN2008100466701A 2008-01-10 2008-01-10 Method for preparing AgI/TiO2 nano compound photocatalyst Expired - Fee Related CN101327438B (en)

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CN102527413A (en) * 2012-02-01 2012-07-04 江苏大学 Preparation and using method of Ag@AgI/AgBr modified TiO2 nanometer tube photochemical catalyst
CN102631937B (en) * 2012-03-28 2014-02-19 武汉理工大学 Synthesis method of supported silver iodide nanoparticle visible light photocatalyst
CN103846066A (en) * 2012-11-30 2014-06-11 淮南师范学院 Preparation method of silicon-based photocatalyst with heterostructure
CN108380244B (en) * 2016-04-25 2021-01-29 翟宇学 Composite visible light photocatalyst Ag2CO3/TiO2/UIO-66-(COOH)2And application of organic matter degradation
CN106391067A (en) * 2016-07-01 2017-02-15 上海电力学院 AgI-Ag3PO4/OV-TiO2 compound photocatalyst and preparation method thereof
CN107817339A (en) * 2016-09-13 2018-03-20 太原理工大学 Chitosan-modified AgI/TiO2Compound and its structure colorimetric immunoassay sensor are used for the method for chloramphenicol detection
CN106752113B (en) * 2016-12-14 2019-02-19 浙江恒逸高新材料有限公司 A kind of preparation method and application of modifying titanium dioxide
CN113402111A (en) * 2021-06-03 2021-09-17 哈尔滨工程大学 Biological/photoelectric/solar coupling sewage treatment integrated device

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