CN104785280B - A kind of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst and preparation method thereof - Google Patents
A kind of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst and preparation method thereof Download PDFInfo
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- CN104785280B CN104785280B CN201510176532.5A CN201510176532A CN104785280B CN 104785280 B CN104785280 B CN 104785280B CN 201510176532 A CN201510176532 A CN 201510176532A CN 104785280 B CN104785280 B CN 104785280B
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Abstract
The invention discloses a kind of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst and preparation method thereof, the composite photo-catalyst is deposited on the heterogeneous material compound formed on titanium dioxide nanoplate by bismuth oxybromide, and its preparation process includes：By titanium dioxide nanoplate, TGA, KBr ultrasonic disperse in deionized water, uniform solution is mixed to obtain, bismuth nitrate is dissolved in ethylene glycol；Then above two solution is mixed to get milky emulsion, stood after stirring, centrifuge washing.The composite construction of different-grain diameter can be obtained in preparation process by adjusting the ratio of titanium dioxide and bismuth oxybromide.Preparation technology of the present invention is simple, particularly can make bismuth oxybromide in TiO with TGA2It is uniformly distributed on piece, the photocatalytic activity more excellent than simple titanium dioxide nanoplate is shown under visible light, there is potential actual application prospect in using solar energy photocatalytic degradable organic pollutant treatment 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 light and urge
Change field.
Background technology
In recent years, developing rapidly with global industry process, problem of environmental pollution becomes increasingly conspicuous.Conductor photocatalysis
Oxidation technology is because having the advantages that simple to operate, reaction condition is gentle, energy consumption is low and secondary pollution is few, standby in field of environmental improvement
It is concerned.In numerous semiconductor light-catalysts, TiO2Because having high chemism, Strong oxdiative ability, nontoxic and high stability
The advantages of, as one of preferable photocatalyst material.But TiO2It is a kind of wide bandgap semiconductor（Anatase TiO2Eg=
3.2eV）, it is only capable of absorbing the ultraviolet light that sunshine medium wavelength is less than 387nm, and ultraviolet light ratio in sunshine is about
4%, the utilization rate to sunshine is low.Meanwhile, light excites the electronics of generation and the recombination rate height in hole, and photo-quantum efficiency is poor.This two
Individual bottleneck factor limits its practical application.Therefore, research and development possess efficient sunlight utilization ratio and high catalytic activity
TiO2It is the key for expanding it in photochemical catalytic oxidation practical application.
In TiO2Study on the modification in, narrow gap semiconductor and wide bandgap semiconductor TiO2It is important research to carry out compound
Problem.BiOBr is only 2.5eV or so as a kind of new narrow bandgap semiconductor material, its energy gap, is conducive to visible
Photoelectronic under light to excite, light abstraction width can cover whole solar spectrum.And BiOBr has high anisotropy uniqueness
Open lamellar structure, is that atom polarization and atomic orbital polarization provide sufficient space, both hole and electron is avoided in interlayer
It is rapid compound, be conducive to efficiently separating and electric charge transfer for hole-electron pair.In addition, BiOBr is indirect band gap, when electronics quilt
It is energized into after conduction band, wants to come back to valence band and just have to pass through K layers and get to, this is also effectively reduced for angle from energy
Photo-generate electron-hole is to being combined.Therefore BiOBr is regulation and control TiO2The ideal material of photo-catalysis capability.
Chinese patent application（CN103908972A）Disclose a kind of BiOX/titanium dioxide composite photocatalyst and its
Preparation method, the composite catalyst of preparation deposits BiOX, the party for nano titania sieve by solvent thermal reaction surface
Time-consuming for method, and because simply simple deposit, BiOX deposition is very uneven, and subsequent processes are cumbersome, therefore, research and development
A kind of preparation method is simple, BiOX depositing homogeneous, the excellent titanium dioxide of photocatalysis performance/bismuth oxybromide composite photocatalyst
Agent has great importance.
The content of the invention
The problem of existing for prior art, urges the invention provides a kind of plate-like titanium dioxide/bismuth oxybromide complex light
Agent, the present invention makees bridging agent using TGA, bismuth oxybromide is uniformly deposited on titanium dioxide nanoplate surface, favorably
In improving its photocatalysis property, sun light utilization efficiency is high and effectively solves the problem of hole-electron pair recombination rate is high, is urging
Change field has potential application value.
Present invention also offers a kind of preparation method of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst, this method
Operation preparation technique is simple, prepares gained composite photo-catalyst and shows excellent photocatalysis performance under visible light.
The technical scheme that is used to achieve these goals of the present invention for：
The invention provides a kind of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst, it is by bismuth oxybromide particle
Titanium dioxide nanoplate surface is deposited to by TGA and forms nano-heterogeneous structure, the titanium dioxide nanoplate is averaged
Size is 150nm × 100nm, and the thickness of bismuth oxybromide sedimentary is 5-15 nm.
Above-mentioned composite photo-catalyst is made using following methods：Titanium dioxide nanoplate is added with TGA, bromine raw material
Enter into deionized water ultrasonic disperse to be sufficiently mixed, bismuth nitrate is dissolved in alcoholic solvent, then mix two kinds of solution, fully
3h is stood after stirring, eventually passes and centrifuges the heterojunction structure that washing obtains plate-like titanium dioxide/bismuth oxybromide.
The preparation method of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst specifically includes following steps in the present invention：
（1）Titanium source butyl titanate is added in alcoholic solvent, derivant is then added, is uniformly mixing to obtain presoma molten
Liquid；
（2）Precursor solution is transferred in reactor and carries out solvent thermal reaction, centrifuges, wash after completion of the reaction,
Obtain titanium dioxide nanoplate；
（3）Titanium dioxide nanoplate and TGA, KBr are added in deionized water, ultrasonic disperse 30min is obtained
Homogeneous transparent solution；
（4）Bismuth nitrate is dissolved in alcoholic solvent, stirs, the bismuth nitrate solution after dissolving is added to titanium dioxide nanoplate
Homogeneous transparent solution in, at room temperature carry out be sufficiently stirred for obtaining uniform milky emulsion；
（5）Milky emulsion is stood into 3h at room temperature, sheet dioxy is obtained by centrifuging washing after terminating
Change titanium/bismuth oxybromide composite photo-catalyst.
Further, step（1）In, the volume ratio of the alcoholic solvent and butyl titanate is 125：1, the same metatitanic acid of derivant
The volume ratio of four butyl esters is 4：1.
Further, the alcoholic solvent is isopropanol, and derivant is hydrofluoric acid.
Further, step（2）In, it in temperature is to react 20h under the conditions of 180 °C that the solvent thermal reaction, which is,.
Further, step（3）The mol ratio of middle titanium dioxide nanoplate and TGA, KBr is 0.625-5：
0.01：1.
Further, step（4）In, the alcoholic solvent is ethylene glycol.
Further, the concentration of bismuth source bismuth nitrate solution is 1.5 × 10 in the present invention-3-6.2×10-3mol/L。
Further, the bismuth nitrate is 1 with the mol ratio of titanium dioxide nanoplate:2-8；Optimize the most, bismuth nitrate
Mol ratio with titanium dioxide nanoplate is 1:2.
Composite photo-catalyst produced by the present invention is by TiO2Nanometer sheet and bismuth oxybromide（BiOBr）Composition, preparation process letter
Single, the time is short, with very strong operability and practicality.Plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst, with tradition
Method is compared, and can make bismuth oxybromide in TiO by using TGA2It is uniformly distributed in nanometer sheet, improves photocatalysis effect.Should
Product shows excellent photocatalysis performance under visible light.
Advantages of the present invention is：
（1）Plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst, bismuth oxybromide is evenly distributed, shown under visible light
Go out excellent photocatalytic activity, sun light utilization efficiency is high and effectively solves the problem of hole-electron pair recombination rate is high, in profit
With in solar energy photocatalytic degradable organic pollutant have potential actual application prospect；
（2）The preparation method that the present invention is provided is simple, takes short, suitable large-scale industrial production.
Brief description of the drawings
Fig. 1 is the diffraction of the X-ray for the titanium dioxide nanoplate that embodiment 1 is synthesized（XRD）Figure.
Fig. 2 is the ESEM for the plate-like titanium dioxide that embodiment 1 is synthesized（SEM）Figure.
Fig. 3 is the X-ray diffraction for plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst that embodiment 1 is synthesized（XRD）Figure
Spectrum.
Fig. 4 is the ESEM for plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst that embodiment 1 is synthesized（SEM）Figure.
Fig. 5 is degradation effect figure of the different photochemical catalysts to rhodamine B in effect example.
Embodiment
Below by embodiment, the present invention will be further elaborated, it should be appreciated that, the description below merely to
The present invention is explained, its content is not defined.
Embodiment 1
1.1 are added to 0.2mL butyl titanate in 25mL isopropanols, are sufficiently stirred for being well mixed it, then slowly
Addition 0.8mL derivant hydrofluoric acid, stirring obtains uniform white emulsion, i.e. precursor solution；
1.2 are transferred to precursor solution in reactor, and 20 h are reacted under conditions of 180 °C, are centrifuged after completion of the reaction
Separation, washing, obtain titanium dioxide nanoplate, and Fig. 1 is the X ray diffracting spectrum of titanium dioxide nanoplate, and Fig. 2 is gained titanium dioxide
The scanning electron microscope (SEM) photograph of titanium nanometer sheet.From figure 1 it appears that products obtained therefrom is anatase phase titanium dioxide；Can from Fig. 2
Go out, the average-size of the titanium dioxide nanoplate is 150nm × 100nm, and pattern is homogeneous；
1.3 add 0.02g titanium dioxide nanoplates and 0.05g KBr, 0.004mmol TGA in deionized water,
Ultrasonic disperse 30min, obtains homogeneous transparent solution；
1.4 are dissolved in 0.06g bismuth nitrates in 20ml ethylene glycol, stirring, and the bismuth nitrate solution after dissolving is added into dioxy
In the homogeneous transparent solution for changing titanium nanometer sheet, carry out being sufficiently stirred for obtaining uniform milky emulsion at room temperature；
Milky emulsion is stood 3h by 1.5 at room temperature, and sheet dioxy is obtained by centrifuging washing after terminating
Change titanium/bismuth oxybromide composite photo-catalyst, Fig. 3 is the X ray diffracting spectrum of the composite photo-catalyst；Fig. 4 is that the complex light is urged
The scanning electron microscope (SEM) photograph of agent.
From figure 3, it can be seen that gained composite photo-catalyst is the composite of titanium dioxide and bismuth oxybromide；From Fig. 4
In as can be seen that titanium dioxide nanoplate surface uniformly deposition one layer of bismuth oxybromide, the average thickness of bismuth oxybromide sedimentary
For 15nm.
Embodiment 2
The preparation method be the same as Example 1 of 2.1 titanium dioxide nanoplates is identical；
0.02g titanium dioxide nanoplates and 0.0252g KBr, 0.002mmol TGA are added deionized water by 2.2
In, ultrasonic disperse 30min obtains homogeneous transparent solution；
2.3 are dissolved in 0.0304g bismuth nitrates in 20ml ethylene glycol, stirring, and the bismuth nitrate solution after dissolving is added into two
In the homogeneous transparent solution of TiOx nano piece, carry out being sufficiently stirred for obtaining uniform milky emulsion at room temperature；
Milky emulsion is stood 3h by 2.4 at room temperature, and sheet dioxy is obtained by centrifuging washing after terminating
Change titanium/bismuth oxybromide composite photo-catalyst.
The average thickness of 2.5 gained composite photo-catalyst bismuth oxybromide sedimentaries is 10 nm.
Embodiment 3
The preparation method be the same as Example 1 of 3.1 titanium dioxide nanoplates is identical；
0.02g titanium dioxide nanoplates and 0.0119g KBr, 0.001mmol TGA are added deionized water by 3.2
In, ultrasonic disperse 30min obtains homogeneous transparent solution；
3.3 are dissolved in 0.0202g bismuth nitrates in 20ml ethylene glycol, stirring, and the bismuth nitrate solution after dissolving is added into two
In the homogeneous transparent solution of TiOx nano piece, carry out being sufficiently stirred for obtaining uniform milky emulsion at room temperature；
Milky emulsion is stood 3h by 3.4 at room temperature, and sheet dioxy is obtained by centrifuging washing after terminating
Change titanium/bismuth oxybromide composite photo-catalyst.
The average thickness of 3.5 gained composite photo-catalyst bismuth oxybromide sedimentaries is 8 nm.
Embodiment 4
The preparation method be the same as Example 1 of 4.1 titanium dioxide nanoplates is identical；
0.02g titanium dioxide nanoplates and 0.0060g KBr, 0.0005mmol TGA are added deionized water by 4.2
In, ultrasonic disperse 30min obtains homogeneous transparent solution；
4.3 are dissolved in 0.0152g bismuth nitrates in 20ml ethylene glycol, stirring, and the bismuth nitrate solution after dissolving is added into two
In the homogeneous transparent solution of TiOx nano piece, carry out being sufficiently stirred for obtaining uniform milky emulsion at room temperature；
Milky emulsion is stood 3h by 4.4 at room temperature, and sheet dioxy is obtained by centrifuging washing after terminating
Change titanium/bismuth oxybromide composite photo-catalyst.
The average thickness of 4.5 gained composite photo-catalyst bismuth oxybromide sedimentaries is 5 nm.
Comparative example 1
A kind of titanium dioxide/bismuth oxybromide composite photo-catalyst, the catalyst is carried using Chinese patent CN103908972A
It is prepared by the method for confession.Bismuth oxybromide sedimentary skewness in the composite photo-catalyst prepared, and time-consuming.
Effect example
Titanium dioxide nanoplate and plate-like titanium dioxide prepared by embodiment 1/bismuth oxybromide composite photo-catalyst is with real
Apply plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst progress catalytic effect experiment prepared by a 2-4 and comparative example 1.
Test method：10 mg samples are taken respectively, in the rhodamine B solution for being separately added into the mg/L of 25 mL 10；By Luo Dan
Bright B solution stirs 60min at dark, solution is in adsorption equilibrium state, then in visible ray（Light source 18W）Lower irradiation,
2 mL samples are taken out every 30min and carry out absorption test, the absorbance of rhodamine B in now solution are measured, according to lambert Bill
Law calculates concentration, calculates sampling concentration and initial rhodamine B concentration proportion；Using the time as abscissa, concentration is sampled and initial
Concentration proportion is ordinate, draws curve, concrete outcome is as shown in figure 5, as can be seen from Figure 5：Sheet titanium dioxide of the present invention
Titanium/bismuth oxybromide composite photo-catalyst has compared with composite photo-catalyst prepared by simple plate-like titanium dioxide and comparative example
Have a preferable photocatalysis effect, and titanium dioxide when with bismuth nitrate mol ratio being 2 to 1 photocatalysis effect it is best.
Claims (9)
1. the preparation method of a kind of plate-like titanium dioxide/bismuth oxybromide composite photo-catalyst, it is characterised in that be by bismuth oxybromide
Particle deposits to titanium dioxide nanoplate surface by TGA and forms nano-heterogeneous structure, the titanium dioxide nanoplate
Average-size is 150nm × 100nm, and the thickness of bismuth oxybromide sedimentary is 5-15 nm；
Specifically include following steps：
（1）Titanium source butyl titanate is added in alcoholic solvent, derivant is then added, is uniformly mixing to obtain precursor solution；
（2）Precursor solution is transferred in reactor and carries out solvent thermal reaction, centrifuges, wash after completion of the reaction, obtain two
TiOx nano piece；
（3）Titanium dioxide nanoplate and TGA, KBr are added in deionized water, ultrasonic disperse 30min, obtain uniform
Clear solution；
（4）Bismuth nitrate is dissolved in alcoholic solvent, stirs, the bismuth nitrate solution after dissolving is added to the equal of titanium dioxide nanoplate
In even clear solution, carry out being sufficiently stirred for obtaining uniform milky emulsion at room temperature；
（5）Milky emulsion is stood into 3h at room temperature, after terminating through centrifugation washing obtain plate-like titanium dioxide/
Bismuth oxybromide composite photo-catalyst.
2. preparation method according to claim 1, it is characterised in that：Step（1）In, the alcoholic solvent and butyl titanate
Volume ratio be 125：1, derivant is 4 with the volume ratio of butyl titanate：1.
3. preparation method according to claim 1 or 2, it is characterised in that：Step（1）In, the alcoholic solvent is isopropanol,
Derivant is hydrofluoric acid.
4. preparation method according to claim 1, it is characterized in that：Step（2）In, the solvent thermal reaction is to be in temperature
20h is reacted under the conditions of 180 °C.
5. preparation method according to claim 1, it is characterized in that：Step（3）Middle titanium dioxide nanoplate and TGA,
The mol ratio of KBr is 0.625-5：0.01：1.
6. preparation method according to claim 1, it is characterized in that：Step（4）In, the alcoholic solvent is ethylene glycol.
7. the preparation method according to claim 1 or 6, it is characterised in that：The concentration of the bismuth nitrate solution is 1.5 × 10-3-6.2×10-3mol/L。
8. preparation method according to claim 1, it is characterised in that：Mole of the bismuth nitrate with titanium dioxide nanoplate
Than for 1:2-8.
9. preparation method according to claim 8, it is characterised in that：Mole of the bismuth nitrate with titanium dioxide nanoplate
Than for 1:2.
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| CN105214693B (en) * | 2015-10-13 | 2018-05-15 | 辽宁大学 | Bismuth oxyiodide/poriferous titanium dioxide composite photo-catalyst and its preparation method and application |
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| 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 |
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| CN110813331A (en) * | 2019-08-19 | 2020-02-21 | 西北矿冶研究院 | BiOBr/TiO2 composite photocatalyst and preparation method thereof |
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| 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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| CN1686609A (en) * | 2005-02-18 | 2005-10-26 | 中国科学院上海硅酸盐研究所 | Iron oxide sensitized lamellar titanium oxide visible light catalyst and its preparation method |
| CN103908972A (en) * | 2013-12-19 | 2014-07-09 | 嘉兴学院 | Recyclable BiOX/TiO2 composite photocatalyst and preparation method thereof |
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| CN1686609A (en) * | 2005-02-18 | 2005-10-26 | 中国科学院上海硅酸盐研究所 | Iron oxide sensitized lamellar titanium oxide visible light catalyst and its preparation method |
| CN103908972A (en) * | 2013-12-19 | 2014-07-09 | 嘉兴学院 | Recyclable BiOX/TiO2 composite photocatalyst and preparation method thereof |
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