CN102962088A - Composite visible-light catalyst for TiO2 microsphere and g-C3N4, as well as preparation method and application of catalyst - Google Patents
Composite visible-light catalyst for TiO2 microsphere and g-C3N4, as well as preparation method and application of catalyst Download PDFInfo
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- CN102962088A CN102962088A CN2012104398663A CN201210439866A CN102962088A CN 102962088 A CN102962088 A CN 102962088A CN 2012104398663 A CN2012104398663 A CN 2012104398663A CN 201210439866 A CN201210439866 A CN 201210439866A CN 102962088 A CN102962088 A CN 102962088A
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Abstract
The invention discloses a composite visible-light catalyst for TiO2 microsphere and g-C3N4, as well as a preparation method and an application of the catalyst. The preparation method comprises the following steps of: putting a cleaned titanium sheet to a mixed aqueous solution of melamine and ammonium fluoride to carry out a hydrothermal reaction; and collecting precipitate in a reaction solution after the reaction solution is cooled, cleaning the precipitate, drying and burning the cleaned precipitate to acquire the composite visible-light catalyst for TiO2 microsphere and g-C3N4. The composite visible-light catalyst overcomes the defects of low photo-transformation efficiency and low activity of a single material, has the advantages of an extensive photo-response range, high visible light catalytic activity and the like, and can be applied to the environment-friendly field, in particular an occasion that visible light catalyzes and degrades organic pollutants in water and kills pathogenic microorganisms in the water, thus the application prospect is extensive.
Description
Technical field
The present invention relates to the visible light catalytic material technical field, particularly a kind of TiO
2Microballoon and g-C
3N
4Composite visible light catalyst and preparation method and application.
Background technology
The organic pollution of a large amount of accumulations and pathogenic microorganism are to cause the human arch-criminal who catches in a large number always in the water body.Healthy and safe in order to ensure human drinking water, traditional processing method are to add the purpose that a large amount of chlorine or ozone reach the sterilization oxidation in drinking water, but this method produces easily toxic byproduct is arranged.And the high-level oxidation technology that developed recently gets up such as photocatalysis technology especially the optically catalytic TiO 2 technology be considered in the Water Disinfection one of the most promising new technology.Photocatalysis technology is that semi-conducting material produces the active oxygen species with very strong oxidability under light-catalysed condition, can non-selectivity in the ground degradation water organic pollution and kill microorganism in the water body, be a kind of cheaply environmentally friendly water treatment and disinfection technology.But because titanium dioxide (TiO
2) greater band gap (3.2eV), only can accept wavelength less than ultraviolet excitation generation light induced electron and the hole of 387nm, thus lower to the sunshine utilization ratio, therefore cause energy consumption larger, photo-quantum efficiency is low.For solving the problems such as the ultraviolet catalytic energy consumption is relatively large, need to carry out modification to its catalyst, improve it to the utilization ratio of visible light, reduce energy consumption in use.The C-N material is C material one of most potential candidate in every field is used because of its unique performance such as mechanics electricity, and there is multiple isomers in it, graphite-phase-C
3N
4(g-C
3N
4) be its allotrope the most stable in environment, existing pertinent literature is reported its synthetic and source at present.Recently, people are by the synthetic g-C of various common organic monomer thermal polymerizations
3N
4Material, and find that it has higher chemical stability, good electrophilic structure and visible light response activity, it is a kind of good organic semiconductor, and its aspect such as photocatalytic degradation of carrying out photolysis water hydrogen, photosynthesis and dye molecule under the driving of visible light has obtained certain effect, yet its most critical issue that exists in using is that its specific activity is lower.Therefore, seek to prepare high activity, g-C cheaply
3N
4Associated materials has good challenge.And prepare TiO by simple hydrothermal synthesis method
2Microballoon and g-C
3N
4Composite visible light catalysis material and be applied to organic matter degradation and the sterilization aspect yet there are no relevant report so far.
Summary of the invention
The shortcoming that primary and foremost purpose of the present invention is to overcome prior art provides a kind of TiO with not enough
2Microballoon and g-C
3N
4The preparation method of composite visible light catalyst.
Another object of the present invention is to provide the TiO for preparing by said method
2Microballoon and g-C
3N
4Composite visible light catalyst.This composite visible light catalyst has overcome single TiO
2Only under ultraviolet excitation, just have photocatalytic activity and single g-C
3N
4Therefore the shortcomings such as activity is lower have higher visible light catalysis activity.
A further object of the present invention is to have overcome described TiO
2Microballoon and g-C
3N
4The application of composite visible light catalyst.
Purpose of the present invention is achieved through the following technical solutions: a kind of TiO
2Microballoon and g-C
3N
4The preparation method of composite visible light catalyst, may further comprise the steps:
(1) the titanium sheet that cleans up places melamine and ammonium fluoride mixed aqueous solution to carry out hydro-thermal reaction; Wherein melamine and ammonium fluoride in mass ratio (1～2) in melamine and the ammonium fluoride mixed aqueous solution: (0.2～1) proportioning;
(2) after the reaction solution cooling of step (1), collect the sediment in the reaction solution, washing precipitate, oven dry, calcining gets TiO
2Microballoon and g-C
3N
4Composite visible light catalyst;
The titanium sheet that cleans up described in the step (1) preferably prepares by the following method: with titanium sheet successively ultrasonic cleaning in acetone, isopropyl alcohol and ethanol, and oven dry, the titanium sheet that obtains cleaning up; The titanium sheet that cleans up is not hung the globule;
The length of described titanium sheet is preferably 5～100mm, and width is preferably 5～100mm, and thickness is preferably 0.05～0.5mm;
Melamine described in the step (1) and ammonium fluoride mixed aqueous solution adopt following methods to prepare: melamine and ammonium fluoride be added to the water, and ultrasonic, and get final product;
The described ultrasonic time is preferably 30min;
The condition of the hydro-thermal reaction described in the step (1) is preferably in 150 ℃ of reaction 24～120h;
Washing precipitate described in the step (2) adopts the following methods washing: water is the centrifuge washing sediment repeatedly, until the pH value of washing lotion is 6～7;
The condition of the oven dry described in the step (2) is preferably in 80 ℃ of oven dry 12h;
The condition of the calcining described in the step (2) is preferably 550 ℃ of calcining 4h;
Described water is deionized water.
A kind of TiO
2Microballoon and g-C
3N
4Composite visible light catalyst, prepare by said method;
Described TiO
2Microballoon and g-C
3N
4Composite visible light catalyst can at the photochemical catalyst of field of Environment Protection as degradable organic pollutant and killing microorganisms, have wide environmental protection application prospect.
The present invention is compared with existing technology, and has following advantage and effect:
(1) the present invention is with TiO
2Microballoon and g-C
3N
4Carry out compoundly, overcome the inefficient and SA shortcoming of homogenous material; As radiation of visible light g-C
3N
4The time, the light induced electron that is produced by excited by visible light can promptly be transmitted on the titanium dioxide, and g-C also can promptly be transferred in the hole of titanium dioxide
3N
4On, effectively improve light induced electron-hole to the separation on composite material interface, thereby improved the visible light catalysis activity of material.
(2) TiO provided by the invention
2Microballoon and g-C
3N
4The preparation technology of composite visible light catalyst simple, easy to operate.
(3) TiO provided by the invention
2Microballoon and g-C
3N
4Composite visible light catalyst, have photoresponse wide ranges, visible light catalysis activity advantages of higher, can be applicable to field of Environment Protection, particularly be applied to the visible light photocatalytic degradation Organic Pollutants In Water and remove pathogenic microorganism in the water body.
Description of drawings
Fig. 1 is TiO
2Microballoon and g-C
3N
4The scanning electron microscope (SEM) photograph of composite visible light catalyst.
Fig. 2 is TiO
2Microballoon and g-C
3N
4X-ray powder diffraction (XRD) collection of illustrative plates of composite visible light catalyst; Wherein, ■: TiO
2The anatase characteristic peak.▲: g-C
3N
4Characteristic peak.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited to this.
Embodiment 1
(1) titanium sheet preliminary treatment: titanium sheet preliminary treatment: (length * wide * thick=48mm * 15mm * 0.16mm) distinguish successively ultrasonic cleaning 15min in acetone, isopropyl alcohol and ethanol at last 80 ℃ of oven dry, obtains clean titanium sheet with the titanium sheet.
(2) in the 40mL deionized water, add 1.0g-melamine and 1.0g NH
4F, with the ultrasonic (frequency: 40kHz) 30min of this mixed system, obtain being transferred in the 70mL autoclave behind the milky suspension mixed system, and add clean titanium sheet, airtight after at 150 ℃ of hydro-thermal reaction 72h, the collecting precipitation thing and with the deionized water washing repeatedly to neutral and at 80 ℃ of oven dry 12h, then add in the crucible and seal with aluminium paper, speed with 20 ℃/min is warming up to 550 ℃ of maintenance 4h, naturally cools to room temperature, namely obtains catalyst.Electronic Speculum detects: detect by the catalyst of Electronic Speculum to preparation, the result calcines behind the hydro-thermal 72h and can form obvious titanium dioxide microballoon sphere and the curling g-C of layer structure as shown in Figure 1
3N
4Form.Carry out XRD analysis, there is g-C in the result in the gained catalyst as shown in Figure 2
3N
4And TiO
2The anatase characteristic peak, this shows and has successfully prepared TiO
2Microballoon and g-C
3N
4Composite visible light catalyst.
(3) ACV degraded: the ACV take the Photocatalytic Activity for Degradation initial concentration as 10mg/L comes evaluate catalysts to organic photocatalytic activity.Concrete steps are: light source is the xenon lamp of 300W, and optical filter filters the following ultraviolet light of 420nm; Take by weighing TiO
2Microballoon and g-C
3N
4Composite visible light catalyst 0.03g to drop into the 100mL initial concentration be in the ACV solution of 10mg/L, lucifuge stirs 30min to reach the adsorption/desorption balance before the reaction, get at regular intervals the 1mL reactant liquor, filter, utilize the liquid-phase chromatographic analysis concentration of substrate to change.Adopt C/C
0Estimate degradation rate, wherein C is the concentration of solution behind the illumination tmin, C
0Initial concentration for solution.The photocatalytic degradation experimental result shows that behind the illumination 90min, the ACV degradation rate can reach 100%.
(4) the visible light photocatalysis deactivation visible light photocatalysis deactivation of Escherichia coli E.coli k-12: Escherichia coli E.coli k-12(CGSC, The Coli Genetic Stock Center): take visible light photocatalysis deactivation initial concentration as 10
7The Escherichia coli E.coli k-12 of cfu/ml comes evaluate catalysts to the photocatalytic activity of microorganism.Concrete steps are: light source is the Xe lamp of 300W, and optical filter filters the following ultraviolet light of 420nm; Take by weighing TiO
2Microballoon and g-C
3N
4Composite visible light catalyst 0.03g to drop into 50mLE.coli k-12(initial concentration be 10
7Cfu/ml) in the suspension, under radiation of visible light, get at regular intervals the 2mL reactant liquor, be applied on agar-nutrient broth solid medium behind the dilution different multiples, behind 37 ℃ of cultivation 16h, record clump count.Experimental result shows, can make 10 behind the illumination 180min
7The Escherichia coli E.coli k-12 of cfu/ml reaches the deactivation of 7-log.
(1) titanium sheet preliminary treatment: with embodiment 1, difference only is that selected titanium sheet is of a size of length * wide * thick=10mm * 10mm * 0.05mm.
(2) in the 100mL deionized water, add 2.0g-melamine and 1.0g NH
4F, with the ultrasonic 30min of this mixed system, obtain being transferred in the 70mL autoclave behind the milky suspension mixed system, and add clean titanium sheet, airtight after at 150 ℃ of hydro-thermal reaction 48h, the collecting precipitation thing and with the deionized water washing repeatedly to neutral and at 80 ℃ of oven dry 12h, then add in the crucible and seal with aluminium paper, speed with 20 ℃/min is warming up to 550 ℃ of maintenance 4h, naturally cools to room temperature, namely obtains catalyst.Can learn that by SEM and XRD products therefrom is TiO
2Microballoon and g-C
3N
4Composite.
(3) ACV degraded: with embodiment 1.The photocatalytic degradation experimental result shows that behind the illumination 240min, the ACV degradation rate can reach 100%.
(4) the visible light photocatalysis deactivation of Escherichia coli E.coli k-12: with embodiment 1.Experimental result shows, can make 10 behind the illumination 240min
7The Escherichia coli E.coli k-12 of cfu/ml reaches the deactivation of 7-log.
Embodiment 3
(1) with embodiment 1, difference only is that selected titanium sheet is of a size of length * wide * thick=5mm * 5mm * 0.5mm.
(2) in the 40mL deionized water, add 1.0g-melamine and 1.0g NH
4F, with the ultrasonic 30min of this mixed system, obtain being transferred in the 70mL autoclave behind the milky suspension mixed system, and add clean titanium sheet, airtight after at 150 ℃ of hydro-thermal reaction 24h, the collecting precipitation thing and with the deionized water washing repeatedly to neutral and at 80 ℃ of oven dry 12h, then add in the crucible and seal with aluminium paper, speed with 20 ℃/min is warming up to 550 ℃ of maintenance 4h, naturally cools to room temperature, namely obtains catalyst.Can learn that by SEM and XRD products therefrom is TiO
2Microballoon and g-C
3N
4Composite.
(3) ACV degraded: with embodiment 1.The photocatalytic degradation experimental result shows that behind the illumination 300min, the ACV degradation rate can reach 100%.
(4) the visible light photocatalysis deactivation of Escherichia coli E.coli k-12: with embodiment 1.Experimental result shows, can make 10 behind the illumination 300min
7The Escherichia coli E.coli k-12 of cfu/ml reaches the deactivation of about 2-log.
Embodiment 4
(1) titanium sheet preliminary treatment: with embodiment 1, difference only is that selected titanium sheet is of a size of length * wide * thick=5mm * 5mm * 0.5mm.
(2) in the 40mL deionized water, add 1.0g-melamine and 0.2g NH
4F, with the ultrasonic 30min of this mixed system, obtain being transferred in the 70mL autoclave behind the milky suspension mixed system, and add clean titanium sheet, airtight after at 150 ℃ of hydro-thermal reaction 24h, the collecting precipitation thing and with the deionized water washing repeatedly to neutral and at 80 ℃ of oven dry 12h, then add in the crucible and seal with aluminium paper, speed with 20 ℃/min is warming up to 550 ℃ of maintenance 4h, naturally cools to room temperature, namely obtains catalyst.Can learn that by SEM and XRD products therefrom is TiO
2Microballoon and g-C
3N
4Composite.
(3) ACV degraded: with embodiment 1.The photocatalytic degradation experimental result shows that behind the illumination 150min, the ACV degradation rate can reach 100%.
(4) the visible light photocatalysis deactivation of Escherichia coli E.coli k-12: with embodiment 1.Experimental result shows, can make 10 behind the illumination 240min
7The Escherichia coli E.coli k-12 of cfu/ml reaches the deactivation of 7-log.
Embodiment 5
(1) titanium sheet preliminary treatment: with embodiment 1, difference only is that selected titanium sheet is of a size of length * wide * thick=48mm * 15mm * 0.16mm.
(2) in the 40mL deionized water, add 1.0g-melamine and 0.8g NH
4F, with the ultrasonic 30min of this mixed system, obtain being transferred in the 70mL autoclave behind the milky suspension mixed system, and add the cleaning titan sheet, airtight after at 150 ℃ of hydro-thermal reaction 24h, the collecting precipitation thing and with the deionized water washing repeatedly to neutral and at 80 ℃ of oven dry 12h, then add in the crucible and seal with aluminium paper, speed with 20 ℃/min is warming up to 550 ℃ of maintenance 4h, naturally cools to room temperature, namely obtains catalyst.Can learn that by SEM and XRD products therefrom is TiO
2Microballoon and g-C
3N
4Composite.
(3) ACV degraded: with embodiment 1.The photocatalytic degradation experimental result shows that behind the illumination 240min, the ACV degradation rate can reach 100%.
(4) the visible light photocatalysis deactivation of Escherichia coli E.coli k-12: with embodiment 1.Experimental result shows, can make 10 behind the illumination 300min
7The Escherichia coli E.coli k-12 of cfu/ml reaches the deactivation of about 6-log.
Embodiment 6
(1) titanium sheet preliminary treatment: with embodiment 1, difference only is that selected titanium sheet is of a size of length * wide * thick=48mm * 15mm * 0.16mm.
(2) in the 40mL deionized water, add 1.0g-melamine and 1g NH
4F, with the ultrasonic 30min of this mixed system, obtain being transferred in the 40mL autoclave behind the milky suspension mixed system, and add the cleaning titan sheet, airtight after at 150 ℃ of hydro-thermal reaction 120h, the collecting precipitation thing and with the deionized water washing repeatedly to neutral and at 80 ℃ of oven dry 12h, then add in the crucible and seal with aluminium paper, speed with 20 ℃/min is warming up to 550 ℃ of maintenance 4h, naturally cools to room temperature, namely obtains catalyst.Can learn that by SEM and XRD products therefrom is TiO
2Microballoon and g-C
3N
4Composite.
(3) ACV degraded: with embodiment 1.The photocatalytic degradation experimental result shows that behind the illumination 120min, the ACV degradation rate can reach 100%.
(4) the visible light photocatalysis deactivation of Escherichia coli E.coli k-12: with embodiment 1.Experimental result shows, can make 10 behind the illumination 240min
7The Escherichia coli E.coli k-12 of cfu/ml reaches the 7-log deactivation.
Comparative Examples 1:
Use embodiment 1 described preparation method to prepare material, difference is that hydrothermal temperature is 180 ℃.Can learn that by SEM and XRD products therefrom is mainly by flower-shaped TiO
2Consist of.The photocatalytic degradation experimental result shows that behind the illumination 300min, the ACV degradation rate is 0%.Can make 10 behind the illumination 300min
7The Escherichia coli E.coli k-12 of cfu/ml only has the deactivation of 1-log.
Comparative Examples 2:
Use embodiment 3 described preparation methods to prepare material, difference is the NH that adds
4The F amount is 1.5g.Can learn that by SEM and XRD products therefrom is mainly by TiO
2Microballoon consists of.
The photocatalytic degradation experimental result shows that behind the illumination 300min, the ACV degradation rate is about 10%.Can make 10 behind the illumination 300min
7The Escherichia coli E.coli k-12 of cfu/ml only has the deactivation of 3-log.
Above-described embodiment is the better embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under Spirit Essence of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. TiO
2Microballoon and g-C
3N
4The preparation method of composite visible light catalyst, it is characterized in that may further comprise the steps:
(1) the titanium sheet that cleans up places melamine and ammonium fluoride mixed aqueous solution to carry out hydro-thermal reaction; Wherein melamine and ammonium fluoride in mass ratio (1～2) in melamine and the ammonium fluoride mixed aqueous solution: (0.2～1) proportioning;
(2) after the reaction solution cooling of step (1), collect the sediment in the reaction solution, washing precipitate, oven dry, calcining gets TiO
2Microballoon and g-C
3N
4Composite visible light catalyst.
2. TiO according to claim 1
2Microballoon and g-C
3N
4The preparation method of composite visible light catalyst, it is characterized in that: the titanium sheet that cleans up described in the step (1) prepares by the following method: with titanium sheet successively ultrasonic cleaning in acetone, isopropyl alcohol and ethanol, oven dry, the titanium sheet that obtains cleaning up.
3. TiO according to claim 1
2Microballoon and g-C
3N
4The preparation method of composite visible light catalyst, it is characterized in that: described titanium sheet is of a size of: length is 5～100mm, width is 5～100mm, thickness is 0.05～0.5mm.
4. TiO according to claim 1
2Microballoon and g-C
3N
4The preparation method of composite visible light catalyst, it is characterized in that: the melamine described in the step (1) and ammonium fluoride mixed aqueous solution adopt following methods to prepare: melamine and ammonium fluoride are added to the water, ultrasonic, and get final product.
5. TiO according to claim 1
2Microballoon and g-C
3N
4The preparation method of composite visible light catalyst, it is characterized in that: the condition of the hydro-thermal reaction described in the step (1) is in 150 ℃ of reaction 24～120h.
6. TiO according to claim 1
2Microballoon and g-C
3N
4The preparation method of composite visible light catalyst, it is characterized in that: the washing precipitate described in the step (2) adopts the following methods washing: water is the centrifuge washing sediment repeatedly, until the pH value of washing lotion is 6～7.
7. TiO according to claim 1
2Microballoon and g-C
3N
4The preparation method of composite visible light catalyst, it is characterized in that: the condition of the oven dry described in the step (2) is in 80 ℃ of oven dry 12h.
8. TiO according to claim 1
2Microballoon and g-C
3N
4The preparation method of composite visible light catalyst, it is characterized in that: the condition of the calcining described in the step (2) is 550 ℃ of calcining 4h.
9. TiO
2Microballoon and g-C
3N
4Composite visible light catalyst, each described preparation method obtains by claim 1～8.
10. TiO claimed in claim 9
2Microballoon and g-C
3N
4The application of composite visible light catalyst, it is characterized in that: described TiO
2Microballoon and g-C
3N
4Composite visible light catalyst be used for degradable organic pollutant and killing microorganisms at field of Environment Protection.
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| XIFENG LU ETAL.: "《Preparation and Photocatalytic Properties of g-C3N4/TiO2 Hybrid Composite》", 《J. MATER. SCI. TECHNOL.》 * |
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