CN102764649A - Metal-silver-supported titanium dioxide photocatalyst and preparation method thereof - Google Patents
Metal-silver-supported titanium dioxide photocatalyst and preparation method thereof Download PDFInfo
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- CN102764649A CN102764649A CN201210234760XA CN201210234760A CN102764649A CN 102764649 A CN102764649 A CN 102764649A CN 201210234760X A CN201210234760X A CN 201210234760XA CN 201210234760 A CN201210234760 A CN 201210234760A CN 102764649 A CN102764649 A CN 102764649A
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Abstract
The invention discloses a metal-silver-supported titanium dioxide photocatalyst and a preparation method thereof. The photocatalyst material is composed of metal-silver-supported titanium dioxide microspheres, wherein the diameter of the titanium dioxide microspheres is 300-500nm; the supported metal silver is dispersed in the titanium dioxide microspheres in a bulk phase homogenization manner; the diameter of the metal silver particles is 5-15nm; and the photocatalyst material has very high photocatalysis efficiency for simulated organic pollutant rhodamine B in water body under the irradiation of ultraviolet and visible light. The preparation method is simple in process, safe to operate and low in cost; and all the used reagents are cheap and accessible, and are free of substances poisonous/harmful to human body or environment.
Description
Technical field
The invention belongs to the Composite Preparation technical field, relate to a kind of titanium dioxide based photocatalytic material, be specifically related to a kind of argent load type titania photocatalyst, the invention still further relates to the preparation method of this argent load type titania photocatalyst.
Background technology
In recent years the titanium dioxide semiconductor catalysis material because of cheapness that it had, be easy to get, nontoxic, characteristic development such as chemical property stable, anti-photoetch property is strong rapidly, and obtain huge economic benefit in practical application area such as water pollution control, air cleaning and anti-bacteria ceramics.But, TiO in actual application
2Photocatalysis degradation organic contaminant exists that the photo-generated carrier recombination rate is high, quantum yield is low and the band gap of itself broad and can not effectively utilize shortcoming such as visible light and become the bottleneck of its large-scale industrial application of restriction.
Research shows, modifies TiO with the nano-noble metal material
2Can promote effective separation in electronics-hole Deng conductor photocatalysis material, improve photocatalytic activity, prolong the service time of catalyst.Behind its area load nano metal material, because metal and semiconductor TiO
2Have different fermi levels, in the light-catalyzed reaction process, semiconductor TiO
2The conduction band that the valence band electronics is extremely empty with induced transition, and because the effect of metal fermi level, electronics will finally transit to fermi level, thereby make TiO
2Hole-duplet takes place effectively to separate, and forming the semiconductor valence band will be main with the hole, and the metal fermi level is main system with the electronics; In the photocatalytic process; The organic group (hydroxyl, carboxyl) that is adsorbed onto semiconductor surface is oxidized with valence band hole generation redox reaction; Simultaneously will accept the electronics that fermi level provides and be reduced, improve light-catalyzed reaction efficient with this as the group of electron acceptor.The load of metal simultaneously can also improve the effective absorption of TiO 2-base optical catalyst material to visible light, and its range of application is expanded to visible region.
The method of existing preparation argent load type titania photocatalyst material mainly contains three types of electronation, light deposition and high-temperature calcinations; (1) chemical reduction method; Mainly flood the method for reduction, the reduction of high energy light source irradiation or reducing agent reduction, but its efficient is lower, not easy to operate through silver-colored source precursor solution; (2) high-temperature calcination mainly through slaine is decomposed, and is realized the apposition growth of metal nanoparticle at titanium dioxide surface in hot environment, this method power consumption is high and be difficult for realizing the uniform load of noble metal; (3) light deposition method mainly adopts the light source irradiation precious metal salt of different-energy, and it is decomposed, and reaches the effect of deposition, and this method is loaded down with trivial details, strict to reaction condition.
Summary of the invention
The purpose of this invention is to provide a kind of argent load type titania photocatalyst material, realized that the argent nano particle is at TiO
2Uniform load on the microballoon, and the particle diameter of titanium dioxide and argent is controlled, and employed reagent is all cheap and easy to get, and does not contain human body or environment poisonous and harmful substances.
Another object of the present invention provides the preparation method of above-mentioned argent load type titania photocatalyst.
The technical scheme that the present invention adopted is; A kind of argent load type titania photocatalyst; This photocatalyst material is made up of the titanium dioxide microballoon sphere of argent load; Wherein the diameter of titanium dioxide microballoon sphere is 300 ~ 500nm, and the argent of institute's load is body and evenly disperses mutually in titanium dioxide microballoon sphere, and the particle diameter of metallic silver particles is 5 ~ 15nm.
Another technical scheme that the present invention adopted is; A kind of method for preparing the argent load type titania photocatalyst; The photocatalyst material for preparing is made up of the titanium dioxide microballoon sphere of argent load, and wherein the diameter of titanium dioxide microballoon sphere is 300 ~ 500nm; The argent of institute's load is body and evenly disperses mutually in titanium dioxide microballoon sphere, the particle diameter of metallic silver particles is 5 ~ 15nm;
Specifically implement according to following steps,
Step 1: be 1-2:300 with molar concentration according to volume ratio be that the inorganic salt solution of 0.1 ~ 1.0mmol/L joins in the absolute ethyl alcohol; Magnetic agitation 20min slowly splashes into tetrabutyl titanate, and the volume ratio of tetrabutyl titanate and inorganic salt solution is 1-2:5.4; Vigorous stirring reaction 10min; Ageing 1 ~ 6h centrifugalizes and cleans successively with absolute ethyl alcohol and deionized water, obtains the pure white powder;
Step 2: according to quality-volumetric concentration is that 1/400-1/600g/ml is dispersed in the pure white powder that step 1 makes in the absolute ethyl alcohol, and ultrasonic dispersion 20min is to wherein adding the AgNO that concentration is 0.1 ~ 1.5g/100mL
3Solution, AgNO
3The volume ratio of solution and absolute ethyl alcohol is 1:2-12, and constant temperature magnetic agitation to solution evaporate to dryness obtains the sepia powder under 30 ~ 50 ℃ of conditions;
Step 3: the sepia powder that step 2 is obtained places Muffle furnace in the air atmosphere calcination processing, makes the argent load type titania photocatalyst.
Characteristic of the present invention also is,
Calcination processing in the step 3 wherein, temperature increasing schedule is: heating rate is 2 ℃/min before 300 ℃, and 300 ℃ to 500 ℃ heating rates are 1 ℃/min, and in 500 ℃ of maintenances 2 hours, naturally cools to room temperature subsequently.
Inorganic salt solution in the step 1 is wherein selected the one or more kinds of mixtures among LiCl, KCl or the NaCl for use.
The invention has the beneficial effects as follows: successful preparation a kind of argent load type titania photocatalyst material, realized that the argent nano particle is at TiO
2Uniform load on the microballoon, and the particle diameter of titanium dioxide and argent is controlled, and employed reagent is all cheap and easy to get, and does not contain human body or environment poisonous and harmful substances.In addition, this photocatalyst material under ultraviolet and radiation of visible light to water body in simulation organic pollution rhodamine B all have very high photocatalysis efficiency.
The amount of positive four butyl esters of metatitanic acid, absolute ethyl alcohol, inorganic salt solution, deionized water and digestion time etc. have considerable influence to the pattern of titanium dioxide microballoon sphere among the present invention.The addition of liquor argenti nitratis ophthalmicus, constant temperature whipping temp etc. also have certain influence to the size and the pattern of silver-colored particle.
Description of drawings
Fig. 1 be the argent load type titania photocatalyst different amplification that makes of the embodiment of the invention 1 transmission electron microscope photo;
Fig. 2 is the X ray diffracting spectrum of the argent load type titania photocatalyst that makes of the embodiment of the invention 2;
Fig. 3 is the degradation curve of argent load type titania photocatalyst rhodamine B in UV-irradiation goes down except that water body of making of the embodiment of the invention 3;
Fig. 4 is the degradation curve of argent load type titania photocatalyst rhodamine B in radiation of visible light goes down except that water body of making of the embodiment of the invention 3.
The specific embodiment
Below in conjunction with the accompanying drawing and the specific embodiment the present invention is elaborated.
Argent load type titania photocatalyst of the present invention; Titanium dioxide microballoon sphere by the argent load is formed; Wherein the diameter of titanium dioxide microballoon sphere is 300 ~ 500nm; The argent of institute's load is body and evenly disperses mutually in titanium dioxide microballoon sphere, the particle diameter of metallic silver particles is 5 ~ 15nm, and this photocatalyst material is simulated the organic pollution rhodamine B in to water body and all had very high photocatalysis efficiency under ultraviolet and radiation of visible light.
The present invention prepares the method for argent load type titania photocatalyst, specifically carries out according to following steps:
Step 1: with 1 ~ 2mL concentration is that 0.1 ~ 1.0mmol/L inorganic salt solution joins in the 300mL absolute ethyl alcohol; Magnetic agitation 20min; Slowly splash into the tetrabutyl titanate of 5.4mL, vigorous stirring reaction 10min, ageing 1 ~ 6h; Centrifugalize and clean successively, obtain a kind of pure white powder with absolute ethyl alcohol and deionized water.
Step 2: the prepared pure white powder of 0.1g step 1 is dispersed in 40 ~ 60mL absolute ethyl alcohol, and ultrasonic dispersion 20min is to wherein adding the AgNO that 5 ~ 15mL concentration is 0.1 ~ 1.5g/100mL
3Solution, constant temperature magnetic agitation to solution evaporate to dryness obtains the sepia powder under 30 ~ 50 ℃ of conditions.
Step 3: place Muffle furnace in the air atmosphere calcination processing the resulting brown powder of step 2.Wherein temperature increasing schedule is that heating rate is 2 ℃/min before 300 ℃, and 300 ℃ to 500 ℃ heating rates are 1 ℃/min, and in 500 ℃ of maintenances 2 hours, naturally cools to room temperature subsequently, can make argent load type titania photocatalyst material.
Wherein used inorganic salt solution can be a kind of or its mixture among LiCl, KCl and the NaCl in the step 1.
Embodiment 1
With 1.0mL concentration is that 0.1mmol/L KCl solution joins in the 300mL absolute ethyl alcohol, and magnetic agitation 20min slowly splashes into the butyl titanate of 5.4mL; Vigorous stirring reaction 10min; Ageing 2h, centrifugal and clean successively with absolute ethyl alcohol and deionized water, obtain lily powder.Above-mentioned resulting pure white powder is dispersed in the 50mL absolute ethyl alcohol, and ultrasonic dispersion 20min is to wherein adding the AgNO that 10mL concentration is 0.1g/100mL
3Solution, constant temperature magnetic agitation certain hour obtains tan powder to the solution evaporate to dryness under 35 ℃ of conditions.Place Muffle furnace in the air atmosphere calcination processing above-mentioned resulting brown powder.Wherein temperature increasing schedule is that heating rate is 2 ℃/min before 300 ℃, and 300 ℃ to 500 ℃ heating rates are 1 ℃/min, and in 500 ℃ of maintenances 2 hours, naturally cools to room temperature subsequently, can obtain the Ag-carried nanometer titanium dioxide photochemical catalyst.Fig. 1 be the argent load type titania photocatalyst different amplification that makes transmission electron microscope photo.
Embodiment 2
With 1.3mL concentration is that 0.8mmol/L KCl solution joins in the 300mL absolute ethyl alcohol, and magnetic agitation 20min slowly splashes into the butyl titanate of 5.4mL; Vigorous stirring reaction 10min; Ageing 1h, centrifugal and clean successively with absolute ethyl alcohol and deionized water, obtain lily powder.Above-mentioned resulting pure white powder is dispersed in the 40mL absolute ethyl alcohol, and ultrasonic dispersion 20min is to wherein adding the AgNO that 12mL concentration is 1.3g/100mL
3Solution, constant temperature magnetic agitation certain hour obtains tan powder to the solution evaporate to dryness under 40 ℃ of conditions.Place Muffle furnace in the air atmosphere calcination processing above-mentioned resulting brown powder.Wherein temperature increasing schedule is that heating rate is 2 ℃/min before 300 ℃, and 300 ℃ to 500 ℃ heating rates are 1 ℃/min, and in 500 ℃ of maintenances 2 hours, naturally cools to room temperature subsequently, can obtain the Ag-carried nanometer titanium dioxide photochemical catalyst.Fig. 2 is the X ray diffracting spectrum of the argent load type titania photocatalyst that makes.
Embodiment 3
With 1.5mL concentration is that 0.5mmol/L KCl solution joins in the 300mL absolute ethyl alcohol, and magnetic agitation 20min slowly splashes into the butyl titanate of 5.4mL; Vigorous stirring reaction 10min; Ageing 3h, centrifugal and clean successively with absolute ethyl alcohol and deionized water, obtain lily powder.Above-mentioned resulting pure white powder is dispersed in the 45mL absolute ethyl alcohol, and ultrasonic dispersion 20min is to wherein adding the AgNO that 14mL concentration is 0.8g/100mL
3Solution, constant temperature magnetic agitation certain hour obtains tan powder to the solution evaporate to dryness under 30 ℃ of conditions.Place Muffle furnace in the air atmosphere calcination processing above-mentioned resulting brown powder.Wherein temperature increasing schedule is that heating rate is 2 ℃/min before 300 ℃, and 300 ℃ to 500 ℃ heating rates are 1 ℃/min, and in 500 ℃ of maintenances 2 hours, naturally cools to room temperature subsequently, can obtain the Ag-carried nanometer titanium dioxide photochemical catalyst.Fig. 3 is the degradation curve of argent load type titania photocatalyst rhodamine B in UV-irradiation goes down except that water body of making, and Fig. 4 is the degradation curve of argent load type titania photocatalyst rhodamine B in radiation of visible light goes down except that water body of making.
Embodiment 4
With 1.8mL concentration is that 0.2mmol/L KCl solution joins in the 300mL absolute ethyl alcohol, and magnetic agitation 20min slowly splashes into the butyl titanate of 5.4mL; Vigorous stirring reaction 10min; Ageing 5h, centrifugal and clean successively with absolute ethyl alcohol and deionized water, obtain lily powder.Above-mentioned resulting pure white powder is dispersed in the 55mL absolute ethyl alcohol, and ultrasonic dispersion 20min is to wherein adding the AgNO that 5mL concentration is 0.2g/100mL
3Solution, constant temperature magnetic agitation certain hour obtains tan powder to the solution evaporate to dryness under 50 ℃ of conditions.Place Muffle furnace in the air atmosphere calcination processing above-mentioned resulting brown powder.Wherein temperature increasing schedule is that heating rate is 2 ℃/min before 300 ℃, and 300 ℃ to 500 ℃ heating rates are 1 ℃/min, and in 500 ℃ of maintenances 2 hours, naturally cools to room temperature subsequently, can obtain the Ag-carried nanometer titanium dioxide photochemical catalyst.
Embodiment 5
With 2.0mL concentration is that 1.0mmol/L KCl solution joins in the 300mL absolute ethyl alcohol, and magnetic agitation 20min slowly splashes into the butyl titanate of 5.4mL; Vigorous stirring reaction 10min; Ageing 6h, centrifugal and clean successively with absolute ethyl alcohol and deionized water, obtain lily powder.Above-mentioned resulting pure white powder is dispersed in the 60mL absolute ethyl alcohol, and ultrasonic dispersion 20min is to wherein adding the AgNO that 15mL concentration is 1.5g/100mL
3Solution, constant temperature magnetic agitation certain hour obtains tan powder to the solution evaporate to dryness under 45 ℃ of conditions.Place Muffle furnace in the air atmosphere calcination processing above-mentioned resulting brown powder.Wherein temperature increasing schedule is that heating rate is 2 ℃/min before 300 ℃, and 300 ℃ to 500 ℃ heating rates are 1 ℃/min, and in 500 ℃ of maintenances 2 hours, naturally cools to room temperature subsequently, can obtain the Ag-carried nanometer titanium dioxide photochemical catalyst.
Claims (4)
1. argent load type titania photocatalyst; It is characterized in that; This photocatalyst material is made up of the titanium dioxide microballoon sphere of argent load; Wherein the diameter of titanium dioxide microballoon sphere is 300 ~ 500nm, and the argent of institute's load is body and evenly disperses mutually in titanium dioxide microballoon sphere, and the particle diameter of metallic silver particles is 5 ~ 15nm.
2. method for preparing the argent load type titania photocatalyst; It is characterized in that; The photocatalyst material for preparing is made up of the titanium dioxide microballoon sphere of argent load, and wherein the diameter of titanium dioxide microballoon sphere is 300 ~ 500nm; The argent of institute's load is body and evenly disperses mutually in titanium dioxide microballoon sphere, the particle diameter of metallic silver particles is 5 ~ 15nm;
Specifically implement according to following steps,
Step 1: be 1-2:300 with molar concentration according to volume ratio be that the inorganic salt solution of 0.1 ~ 1.0mmol/L joins in the absolute ethyl alcohol; Magnetic agitation 20min slowly splashes into tetrabutyl titanate, and the volume ratio of tetrabutyl titanate and inorganic salt solution is 1-2:5.4; Vigorous stirring reaction 10min; Ageing 1 ~ 6h centrifugalizes and cleans successively with absolute ethyl alcohol and deionized water, obtains the pure white powder;
Step 2: according to quality-volumetric concentration is that 1/400-1/600g/ml is dispersed in the pure white powder that step 1 makes in the absolute ethyl alcohol, and ultrasonic dispersion 20min is to wherein adding the AgNO that concentration is 0.1 ~ 1.5g/100mL
3Solution, AgNO
3The volume ratio of solution and absolute ethyl alcohol is 1:2-12, and constant temperature magnetic agitation to solution evaporate to dryness obtains the sepia powder under 30 ~ 50 ℃ of conditions;
Step 3: the sepia powder that step 2 is obtained places Muffle furnace in the air atmosphere calcination processing, makes the argent load type titania photocatalyst.
3. the method for preparing the argent load type titania photocatalyst according to claim 2; It is characterized in that; Calcination processing in the described step 3, temperature increasing schedule is: heating rate is 2 ℃/min before 300 ℃, and 300 ℃ to 500 ℃ heating rates are 1 ℃/min; And, naturally cool to room temperature subsequently in 500 ℃ of maintenances 2 hours.
4. the method for preparing the argent load type titania photocatalyst according to claim 2 is characterized in that, the inorganic salt solution in the described step 1 is selected the one or more kinds of mixtures among LiCl, KCl or the NaCl for use.
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CN103272592A (en) * | 2013-05-08 | 2013-09-04 | 陕西科技大学 | Preparation method of one-dimensional silver-loaded titanium dioxide nanorod photocatalyst |
CN103394343A (en) * | 2013-08-16 | 2013-11-20 | 河海大学 | Preparation method and application of metal-doped titanium dioxide material |
JP2016059878A (en) * | 2014-09-18 | 2016-04-25 | 国立大学法人 筑波大学 | Photocatalyst, coating and sterilization device |
CN109529823A (en) * | 2018-12-07 | 2019-03-29 | 武汉工程大学 | A kind of silver carried titanium dioxide hollow sphere and preparation method thereof |
CN109529832A (en) * | 2018-12-07 | 2019-03-29 | 武汉工程大学 | Double shell hollow spheres of a kind of silver carried titanium dioxide/yttrium oxide and preparation method thereof |
CN110201667A (en) * | 2019-07-15 | 2019-09-06 | 重庆理工大学 | The preparation method of Ag/GO catalysis material for sterilization |
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CN103272592A (en) * | 2013-05-08 | 2013-09-04 | 陕西科技大学 | Preparation method of one-dimensional silver-loaded titanium dioxide nanorod photocatalyst |
CN103272592B (en) * | 2013-05-08 | 2015-09-02 | 陕西科技大学 | One dimension carries the preparation method of silver-colored titanium dioxide nano-rod photo-catalyst |
CN103394343A (en) * | 2013-08-16 | 2013-11-20 | 河海大学 | Preparation method and application of metal-doped titanium dioxide material |
JP2016059878A (en) * | 2014-09-18 | 2016-04-25 | 国立大学法人 筑波大学 | Photocatalyst, coating and sterilization device |
CN109529823A (en) * | 2018-12-07 | 2019-03-29 | 武汉工程大学 | A kind of silver carried titanium dioxide hollow sphere and preparation method thereof |
CN109529832A (en) * | 2018-12-07 | 2019-03-29 | 武汉工程大学 | Double shell hollow spheres of a kind of silver carried titanium dioxide/yttrium oxide and preparation method thereof |
CN110201667A (en) * | 2019-07-15 | 2019-09-06 | 重庆理工大学 | The preparation method of Ag/GO catalysis material for sterilization |
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