CN104785280A - Flaky titanium dioxide/bismuth oxybromide composite photocatalyst and preparation method thereof - Google Patents
Flaky titanium dioxide/bismuth oxybromide composite photocatalyst and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a flaky titanium dioxide/bismuth oxybromide composite photocatalyst and a preparation method thereof. The composite photocatalyst is a heterogeneous composite material formed by depositing bismuth oxybromide on a titanium dioxide nanometer sheet. The preparation method comprises the following steps: dispersing the titanium dioxide nanometer sheet, thioglycollic acid, potassium bromide in deionized water in an ultrasonic manner, uniformly mixing to obtain a solution, and dissolving bismuth nitrate in ethylene glycol to obtain a solution; mixing the two solutions obtained in the former step to obtain a milky emulsion, stirring, leaving the emulsion to stand, and performing centrifugal separation and washing to obtain the composite photocatalyst. In the preparation process, through adjusting ratio of titanium dioxide to bismuth oxybromide, composite structures in different particle diameters can be obtained. The composite photocatalyst is simple in preparation technology; particularly, through thioglycollic acid, bismuth oxybromide can be uniformly distributed on the titanium dioxide (TiO2) sheet; the composite photocatalyst shows a more excellent photocatalytic activity compared with that of the titanium dioxide nanometer sheet under visible light, and has the potential practical application prospect of photocatalytic degration of organic pollutants through solar power light in the processing technology.
Description
Technical field
The present invention relates to a kind of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst and preparation method thereof, belong to photocatalysis field.
Background technology
In recent years, along with developing rapidly of global industry process, problem of environmental pollution becomes increasingly conspicuous.Photocatalytic Oxidation With Semiconductors technology, because having the advantages such as simple to operate, reaction condition is gentle, energy consumption is low and secondary pollution is few, receives much concern in field of environmental improvement.In numerous semiconductor light-catalyst, TiO
2because having high chemism, Strong oxdiative ability, the advantages such as nontoxic and high stability, become one of desirable photocatalyst material.But TiO
2a kind of wide bandgap semiconductor (anatase TiO
2e
g=3.2
ev), only can absorb the ultraviolet light that sunshine medium wavelength is less than 387nm, and ultraviolet light ratio in sunshine is approximately 4%, low to the utilization rate of sunshine.Meanwhile, the recombination rate in the electronics that optical excitation produces and hole is high, and photo-quantum efficiency is poor.These two bottleneck factor limit its practical application.Therefore, research and development possess the TiO of efficient sunlight utilization ratio and high catalytic activity
2expand its key in photochemical catalytic oxidation practical application.
At TiO
2study on the modification in, narrow gap semiconductor and wide bandgap semiconductor TiO
2carrying out compound is important research topic.BiOBr is as a kind of novel narrow bandgap semiconductor material, and its energy gap is only about 2.5eV, and be conducive to photoelectronic under visible light exciting, light abstraction width can cover whole solar spectrum.And BiOBr has the open lamellar structure of high anisotropy uniqueness, for atom polarization and atomic orbital polarization provide sufficient space, make both hole and electron avoid rapid compound at interlayer, be conducive to the right effective separation of hole-electron and Charger transfer.In addition, BiOBr is indirect band gap, and after electronics is excited to conduction band, want to come back to valence band and just have to pass through K layer and could arrive, this angle from energy also effectively reduces the right compound of photo-generate electron-hole.Therefore BiOBr is regulation and control TiO
2the ideal material of photo-catalysis capability.
Chinese patent application (CN103908972A) discloses a kind of BiOX/titanium dioxide composite photocatalyst and preparation method thereof, the composite catalyst of preparation is that nano titania sieve is by solvent thermal reaction surface deposition BiOX, the method length consuming time, and because just simply deposit, BiOX deposition is very uneven, subsequent processes is loaded down with trivial details, therefore, research and develop a kind of preparation method simple, BiOX depositing homogeneous, the excellent titanium dioxide/bismuth oxybromide composite photo-catalyst of photocatalysis performance has great importance.
Summary of the invention
For prior art Problems existing, the invention provides a kind of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst, the present invention utilizes TGA to connect agent, bismuth oxybromide is made to be deposited on titanium dioxide nanoplate surface equably, be conducive to improving its photocatalysis property, sunshine utilization rate is high and effectively solve the high problem of hole-electron pair recombination rate, has potential using value at catalytic field.
Present invention also offers the preparation method of a kind of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst, preparation technology is simple in the method operation, prepares gained composite photo-catalyst and shows excellent photocatalysis performance under visible light.
The technical scheme that the present invention is adopted to achieve these goals is:
The invention provides a kind of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst, it deposits to titanium dioxide nanoplate surface by bismuth oxybromide particle by TGA to form nano-heterogeneous structure, the average-size of described titanium dioxide nanoplate is 150nm × 100nm, and the thickness of bismuth oxybromide sedimentary deposit is 5-15 nm.
Above-mentioned composite photo-catalyst adopts following methods to obtain: titanium dioxide nanoplate and TGA, bromine raw material are joined deionized water for ultrasonic and disperses fully to mix, bismuth nitrate is dissolved in alcoholic solvent, then by two kinds of solution mixing, abundant stirring leaves standstill 3h afterwards, eventually passes the heterojunction structure that centrifugation washing obtains plate-like titanium dioxide/bismuth oxybromide.
The preparation method of plate-like titanium dioxide in the present invention/bismuth oxybromide composite photo-catalyst specifically comprises the following steps:
(1) in alcoholic solvent, add titanium source butyl titanate, then add derivant, stir and obtain precursor solution;
(2) transferred in reactor by precursor solution and carry out solvent thermal reaction, centrifugation after completion of the reaction, washing, obtain titanium dioxide nanoplate;
(3) titanium dioxide nanoplate and TGA, KBr are added in deionized water, ultrasonic disperse 30min, obtain homogeneous transparent solution;
(4) bismuth nitrate is dissolved in alcoholic solvent, stirs, the bismuth nitrate solution after dissolving is joined in the homogeneous transparent solution of titanium dioxide nanoplate, at room temperature carry out fully stirring obtaining uniform milky emulsion;
(5) milky emulsion is at room temperature left standstill 3h, after terminating, obtain plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst through centrifugation washing.
Further, in step (1), the volume ratio of described alcoholic solvent and butyl titanate is 125:1, and derivant is 4:1 with the volume ratio of butyl titanate.
Further, described alcoholic solvent is isopropyl alcohol, and derivant is hydrofluoric acid.
Further, in step (2), described solvent thermal reaction for react 20h under temperature is 180 ° of C conditions.
Further, the mol ratio of titanium dioxide nanoplate and TGA, KBr is 0.625-5:0.01:1 in step (3).
Further, in step (4), described alcoholic solvent is ethylene glycol.
Further, in the present invention, the concentration of bismuth source bismuth nitrate solution is 1.5 × 10
-3-6.2 × 10
-3mol/L.
Further, described bismuth nitrate is 1:2-8 with the mol ratio of titanium dioxide nanoplate; Optimize the most, bismuth nitrate is 1:2 with the mol ratio of titanium dioxide nanoplate.
The composite photo-catalyst that the present invention obtains is by TiO
2nanometer sheet and bismuth oxybromide (BiOBr) composition, preparation process is simple, and the time is short, has very strong operability and practicality.Plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst, compared with conventional method, can make bismuth oxybromide at TiO by utilizing TGA
2nanometer sheet is uniformly distributed, improves photocatalysis effect.This product shows excellent photocatalysis performance under visible light.
Advantage of the present invention is:
(1) plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst, bismuth oxybromide is evenly distributed, show excellent photocatalytic activity under visible light, sunshine utilization rate is high and effectively solve the high problem of hole-electron pair recombination rate, has potential actual application prospect utilizing in solar energy photocatalytic degradable organic pollutant;
(2) preparation method provided by the invention is simple, consuming time short, is applicable to large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is diffraction (XRD) figure of the X-ray of the titanium dioxide nanoplate that embodiment 1 is synthesized.
Fig. 2 is ESEM (SEM) figure of the plate-like titanium dioxide that embodiment 1 is synthesized.
Fig. 3 is X-ray diffraction (XRD) collection of illustrative plates of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst that embodiment 1 is synthesized.
Fig. 4 is ESEM (SEM) figure of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst that embodiment 1 is synthesized.
Fig. 5 be in effect example different photochemical catalyst to the degradation effect figure of rhodamine B.
Detailed description of the invention
Below by embodiment, the present invention will be further elaborated, it is to be understood that following explanation is only to explain the present invention, do not limit its content.
embodiment 1
The butyl titanate of 0.2mL is added in 25mL isopropyl alcohol by 1.1, fully stirs and makes it mix, then add 0.8mL derivant hydrofluoric acid slowly, stir and obtain uniform white emulsion, i.e. precursor solution;
Precursor solution is transferred in reactor by 1.2, under the condition of 180 ° of C, react 20 h, centrifugation after completion of the reaction, washing, obtain titanium dioxide nanoplate, Fig. 1 is the X ray diffracting spectrum of titanium dioxide nanoplate, and Fig. 2 is the scanning electron microscope (SEM) photograph of gained titanium dioxide nanoplate.As can be seen from Figure 1, products obtained therefrom is anatase phase titanium dioxide; As can be seen from Figure 2, the average-size of this titanium dioxide nanoplate is 150nm × 100nm, and pattern is homogeneous;
0.02g titanium dioxide nanoplate and 0.05g KBr, 0.004mmol TGA add in deionized water by 1.3, and ultrasonic disperse 30min, obtains homogeneous transparent solution;
0.06g bismuth nitrate is dissolved in 20ml ethylene glycol by 1.4, stirs, and joins in the homogeneous transparent solution of titanium dioxide nanoplate by the bismuth nitrate solution after dissolving, and at room temperature carries out fully stirring obtaining uniform milky emulsion;
Milky emulsion is at room temperature left standstill 3h by 1.5, and after terminating, obtain plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst through centrifugation washing, Fig. 3 is the X ray diffracting spectrum of this composite photo-catalyst; Fig. 4 is the scanning electron microscope (SEM) photograph of this composite photo-catalyst.
As can be seen from Figure 3, gained composite photo-catalyst is the composite of titanium dioxide and bismuth oxybromide; As can be seen from Figure 4, deposition one deck bismuth oxybromide of titanium dioxide nanoplate surface uniform, the average thickness of bismuth oxybromide sedimentary deposit is 15nm.
embodiment 2
The preparation method of 2.1 titanium dioxide nanoplates is identical with embodiment 1;
0.02g titanium dioxide nanoplate and 0.0252g KBr, 0.002mmol TGA add in deionized water by 2.2, and ultrasonic disperse 30min, obtains homogeneous transparent solution;
0.0304g bismuth nitrate is dissolved in 20ml ethylene glycol by 2.3, stirs, and joins in the homogeneous transparent solution of titanium dioxide nanoplate by the bismuth nitrate solution after dissolving, and at room temperature carries out fully stirring obtaining uniform milky emulsion;
Milky emulsion is at room temperature left standstill 3h by 2.4, after terminating, obtain plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst through centrifugation washing.
The average thickness of 2.5 gained composite photo-catalyst bismuth oxybromide sedimentary deposits is 10 nm.
embodiment 3
The preparation method of 3.1 titanium dioxide nanoplates is identical with embodiment 1;
0.02g titanium dioxide nanoplate and 0.0119g KBr, 0.001mmol TGA add in deionized water by 3.2, and ultrasonic disperse 30min, obtains homogeneous transparent solution;
0.0202g bismuth nitrate is dissolved in 20ml ethylene glycol by 3.3, stirs, and joins in the homogeneous transparent solution of titanium dioxide nanoplate by the bismuth nitrate solution after dissolving, and at room temperature carries out fully stirring obtaining uniform milky emulsion;
Milky emulsion is at room temperature left standstill 3h by 3.4, after terminating, obtain plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst through centrifugation washing.
The average thickness of 3.5 gained composite photo-catalyst bismuth oxybromide sedimentary deposits is 8 nm.
embodiment 4
The preparation method of 4.1 titanium dioxide nanoplates is identical with embodiment 1;
0.02g titanium dioxide nanoplate and 0.0060g KBr, 0.0005mmol TGA add in deionized water by 4.2, and ultrasonic disperse 30min, obtains homogeneous transparent solution;
0.0152g bismuth nitrate is dissolved in 20ml ethylene glycol by 4.3, stirs, and joins in the homogeneous transparent solution of titanium dioxide nanoplate by the bismuth nitrate solution after dissolving, and at room temperature carries out fully stirring obtaining uniform milky emulsion;
Milky emulsion is at room temperature left standstill 3h by 4.4, after terminating, obtain plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst through centrifugation washing.
The average thickness of 4.5 gained composite photo-catalyst bismuth oxybromide sedimentary deposits is 5 nm.
Comparative example 1
A kind of titanium dioxide/bismuth oxybromide composite photo-catalyst, the method that this catalyst utilizes Chinese patent CN103908972A to provide is prepared.Bismuth oxybromide sedimentary deposit skewness in the composite photo-catalyst prepared, and length consuming time.
effect example
Plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst that the titanium dioxide nanoplate prepare embodiment 1 and plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst are prepared with embodiment 2-4 and comparative example 1 carries out catalytic effect test.
Test method: get 10 mg samples respectively, adds in the rhodamine B solution of 25 mL 10 mg/L respectively; Rhodamine B solution is stirred 60min at dark place, solution is made to be in adsorption equilibrium state, then irradiate under visible ray (light source 18W), take out 2 mL samples every 30min and carry out absorption test, measure the absorbance of rhodamine B in now solution, calculate concentration according to langbobier law, calculate sampling concentration and initial rhodamine B concentration proportion; Take time as abscissa, sampling concentration and initial concentration ratio are ordinate, curve plotting, concrete outcome as shown in Figure 5, as can be seen from Figure 5: compared with composite photo-catalyst prepared by plate-like titanium dioxide of the present invention/bismuth oxybromide composite photo-catalyst and simple plate-like titanium dioxide and comparative example, all there is good photocatalysis effect, and when titanium dioxide is 2 to 1 with bismuth nitrate mol ratio, photocatalysis effect is best.
Claims (10)
1. plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst, it is characterized in that, deposit to titanium dioxide nanoplate surface by bismuth oxybromide particle by TGA to form nano-heterogeneous structure, the average-size of described titanium dioxide nanoplate is 150nm × 100nm, and the thickness of bismuth oxybromide sedimentary deposit is 5-15 nm.
2. plate-like titanium dioxide according to claim 1/bismuth oxybromide composite photo-catalyst, it is characterized in that: this composite photo-catalyst adopts following methods to obtain: titanium dioxide nanoplate and TGA, bromine raw material are joined deionized water for ultrasonic and disperses fully to mix, bismuth nitrate is dissolved in alcoholic solvent, then by two kinds of solution mixing, abundant stirring leaves standstill 3h afterwards, eventually passes the heterojunction structure that centrifugation washing obtains plate-like titanium dioxide/bismuth oxybromide.
3. the preparation method of a kind of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst as claimed in claim 1, is characterized in that, comprise the following steps:
(1) in alcoholic solvent, add titanium source butyl titanate, then add derivant, stir and obtain precursor solution;
(2) transferred in reactor by precursor solution and carry out solvent thermal reaction, centrifugation after completion of the reaction, washing, obtain titanium dioxide nanoplate;
(3) titanium dioxide nanoplate and TGA, KBr are added in deionized water, ultrasonic disperse 30min, obtain homogeneous transparent solution;
(4) bismuth nitrate is dissolved in alcoholic solvent, stirs, the bismuth nitrate solution after dissolving is joined in the homogeneous transparent solution of titanium dioxide nanoplate, at room temperature carry out fully stirring obtaining uniform milky emulsion;
(5) milky emulsion is at room temperature left standstill 3h, after terminating, obtain plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst through centrifugation washing.
4. preparation method according to claim 3, is characterized in that: in step (1), and the volume ratio of described alcoholic solvent and butyl titanate is 125:1, and derivant is 4:1 with the volume ratio of butyl titanate.
5. the preparation method according to claim 3 or 4, is characterized in that: in step (1), and described alcoholic solvent is isopropyl alcohol, and derivant is hydrofluoric acid.
6. preparation method according to claim 3, is characterized in that: in step (2), described solvent thermal reaction for react 20h under temperature is 180 ° of C conditions.
7. preparation method according to claim 3, is characterized in that: the mol ratio of titanium dioxide nanoplate and TGA, KBr is 0.625-5:0.01:1 in step (3).
8. preparation method according to claim 3, is characterized in that: in step (4), and described alcoholic solvent is ethylene glycol.
9. the preparation method according to claim 3 or 8, is characterized in that: the concentration of described bismuth nitrate solution is 1.5 × 10
-3-6.2 × 10
-3mol/L.
10. preparation method according to claim 3, is characterized in that: described bismuth nitrate is 1:2-8 with the mol ratio of titanium dioxide nanoplate, and the mol ratio of optimization is 1:2.
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| CN105214693A (en) * | 2015-10-13 | 2016-01-06 | 辽宁大学 | Bismuth oxyiodide/poriferous titanium dioxide composite photo-catalyst and its preparation method and application |
| CN105776410A (en) * | 2016-03-28 | 2016-07-20 | 朱连文 | Flexible bismuth oxybromide-titanium oxide/carbon fiber water-purifying material with capillary water supply and photocatalytic adsorption functions and preparation method thereof |
| CN106442671A (en) * | 2016-09-12 | 2017-02-22 | 济南大学 | Preparation method of no-mark insulin sensor based on BiOBr/Ag2S composite material |
| CN107670664A (en) * | 2017-10-31 | 2018-02-09 | 云南健牛生物科技有限公司 | Titanic oxide composite photochemical catalyst system prepares and its application |
| CN110252353A (en) * | 2019-07-02 | 2019-09-20 | 汕头大学 | A kind of BiOI/Bi/TiO of ternary heterojunction structure2Composite photocatalyst material and its preparation and application |
| CN110813331A (en) * | 2019-08-19 | 2020-02-21 | 西北矿冶研究院 | BiOBr/TiO2 composite photocatalyst and preparation method thereof |
| CN111185203A (en) * | 2020-02-11 | 2020-05-22 | 江南大学 | Iodine-doped titanium dioxide-bismuth oxybromide composite photocatalyst and preparation method thereof |
| CN111437854A (en) * | 2020-05-08 | 2020-07-24 | 中国环境科学研究院 | Bismuth oxyiodide/boron carbide catalyst and preparation method and application thereof |
| CN113289646A (en) * | 2021-05-05 | 2021-08-24 | 桂林理工大学 | Core-shell structured nanoflower/nanoparticle bismuth oxybromide/titanium dioxide visible-light-driven photocatalyst and preparation method and application thereof |
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| US11794173B2 (en) | 2021-03-08 | 2023-10-24 | Samsung Electronics Co., Ltd. | Composite photocatalyst structure, and photocatalytic filter and air purification device including the same |
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| CN105214693A (en) * | 2015-10-13 | 2016-01-06 | 辽宁大学 | Bismuth oxyiodide/poriferous titanium dioxide composite photo-catalyst and its preparation method and application |
| CN105776410A (en) * | 2016-03-28 | 2016-07-20 | 朱连文 | Flexible bismuth oxybromide-titanium oxide/carbon fiber water-purifying material with capillary water supply and photocatalytic adsorption functions and preparation method thereof |
| CN106442671A (en) * | 2016-09-12 | 2017-02-22 | 济南大学 | Preparation method of no-mark insulin sensor based on BiOBr/Ag2S composite material |
| CN107670664A (en) * | 2017-10-31 | 2018-02-09 | 云南健牛生物科技有限公司 | Titanic oxide composite photochemical catalyst system prepares and its application |
| CN110252353B (en) * | 2019-07-02 | 2022-05-27 | 汕头大学 | BiOI/Bi/TiO of ternary heterostructure2Composite photocatalytic material and preparation and application thereof |
| CN110252353A (en) * | 2019-07-02 | 2019-09-20 | 汕头大学 | A kind of BiOI/Bi/TiO of ternary heterojunction structure2Composite photocatalyst material and its preparation and application |
| CN110813331A (en) * | 2019-08-19 | 2020-02-21 | 西北矿冶研究院 | BiOBr/TiO2 composite photocatalyst and preparation method thereof |
| CN111185203A (en) * | 2020-02-11 | 2020-05-22 | 江南大学 | Iodine-doped titanium dioxide-bismuth oxybromide composite photocatalyst and preparation method thereof |
| CN111185203B (en) * | 2020-02-11 | 2021-04-20 | 江南大学 | Iodine-doped titanium dioxide-bismuth oxybromide composite photocatalyst and preparation method thereof |
| US11701635B2 (en) | 2020-02-19 | 2023-07-18 | Samsung Electronics Co., Ltd. | Material, filter, and device for removing contaminant |
| CN111437854B (en) * | 2020-05-08 | 2021-08-06 | 中国环境科学研究院 | Bismuth oxyiodide/boron carbide catalyst and preparation method and application thereof |
| CN111437854A (en) * | 2020-05-08 | 2020-07-24 | 中国环境科学研究院 | Bismuth oxyiodide/boron carbide catalyst and preparation method and application thereof |
| US11794173B2 (en) | 2021-03-08 | 2023-10-24 | Samsung Electronics Co., Ltd. | Composite photocatalyst structure, and photocatalytic filter and air purification device including the same |
| CN113289646A (en) * | 2021-05-05 | 2021-08-24 | 桂林理工大学 | Core-shell structured nanoflower/nanoparticle bismuth oxybromide/titanium dioxide visible-light-driven photocatalyst and preparation method and application thereof |
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