CN101147859A - Method for preparing porous bismuth titanate photocatalyst - Google Patents
Method for preparing porous bismuth titanate photocatalyst Download PDFInfo
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- CN101147859A CN101147859A CNA2007101662201A CN200710166220A CN101147859A CN 101147859 A CN101147859 A CN 101147859A CN A2007101662201 A CNA2007101662201 A CN A2007101662201A CN 200710166220 A CN200710166220 A CN 200710166220A CN 101147859 A CN101147859 A CN 101147859A
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Abstract
The present invention belongs to the field of environmental science and engineering technology, in the concrete, it relates to a preparation method of new-type mesopore bismuth titanate photacatalyst for degrading organic pollutant. Said method includes the following steps: using bismuth nitrate and titanate as main raw material, using block interpolymer surfactant as structure guide agent, adopting acetic acid as hydrolysis catalyst, utilizing solvent thermal synthesis method to prepare titanium-bismuth composite oxide gel, making said gel undergo the processes of filtering, drying, high-temperature calcining and crystallizing so as to obtain the mesopore bismuth titanate material with photocatalytic activity.
Description
Technical field
The invention belongs to the Environmental Science and Engineering ambit, be specially a kind of preparation method who is used for the porous bismuth titanate photocatalyst of photocatalysis degradation organic contaminant.
Background technology
In recent years, the conductor photocatalysis technology has obtained at aspects such as environmental protection and photolysis water hydrogens using very widely.Photochemical catalyst commonly used is an anatase titanium oxide, but because the greater band gap of titanium oxide, can only be by the ultraviolet excitation of wavelength less than 386.5nm, if with uviol lamp as the photocatalysis light source, can cause a large amount of energy wastes; In addition, it is too tiny to use more TiOx nano powder particle at present, if be used for water body purification, then be difficult for separating from water body and reclaim.Therefore the development of new semiconductor light-catalyst requires its granularity bigger, reclaims easily, and can be activated by visible light, has high photocatalytic activity, becomes two big research directions of present photocatalysis research field.
Polynary metal oxide is because of the diversity of its crystal and electronic structure, might possess band structure that responding to visible light excites and high photo-generated carrier mobility simultaneously, is used as potential high-efficiency photocatalysis material and obtained broad research.The compound composite oxides with multiple crystal phase structure that form of bismuth oxide and titanium oxide are commonly referred to as the bismuth titanates compound.Bi wherein
4Ti
3O
12And Bi
2Ti
2O
7Because its outstanding ferroelectric and high dielectric property matter often is used to the preparation of microelectronic component.Bismuth titanates compound functions character depends on their structure particularity, all has TiO in their crystal structure
6Octahedron or TiO
4Tetrahedron exists because of having 6s and be attached thereto in the BiOn polyhedron that connects
2Lone pair electrons to and have a three-dimensional active Bi
3+Ion, this makes it to have the ability as the photocatalytic activity center.
Bismuth titanates (Bi
12TiO
20) be typical sillenite crystalline compounds, belong to broadband semiconductor, it has character such as photoelectricity, electric light, fluorescence, magneto-optic, acousto-optic, optically-active and piezoelectricity simultaneously.Particularly its good photoelectricity and electrooptical property make it in fields such as photoelectron, optics, optical information processing materials extremely wide application prospect be arranged all.In this year, the research worker is introduced into photocatalysis field: document " Bi
12TiO
20The preparation of nano-powder and optical absorption characteristics research Zhou Aiqiu thereof, Xu Xiaohong, Yao Weifeng, all brightening Acta Physica Sinicas 2006, Vol.17 No.3 " studied the optical absorption characteristics of bismuth titanates nano-powder morning, indicated its potentiality as the photo-catalysis function material; Document " Photocatalytic Performance Study of bismuth titanates based compound permitted to imitate red, Yao Weifeng, Zhang Yin, Zhou Aiqiu, Hou Yun, Wang Min, chemical journal 2005, Vol.63 No.1,5-10 " compared the degradation capability of the bismuth titanates of different crystal forms structure, and it is analyzed; Document " Photocatalytic properties of bismuth titanateBi12TiO20 prepared by co-precipitation processing Shihong Xu; Wenfeng Shangguan; Jian Yuan; Jianwei Shi; Mingxia Chen Materials Science and Engineering B 137 (2007) 108-111 " is studied the visible absorption spectra of nanometer bismuth titanate, and has estimated the effect of its photocatalytic degradation phenol.
But above-mentioned bismuth titanate photocatalytic material is nano-powder, and granularity is less, still can't solve the problem that catalyst separates from water body, therefore need further improve its structure and form, makes it better application in the water body purification field.
Summary of the invention
The objective of the invention is to propose a kind of porous bismuth titanate photocatalyst that is used for degradable organic pollutant and preparation method thereof with highlight catalytic active, bigger serface and micron order aggregate particle size.This photochemical catalyst separates recovery easily, and has kept the high catalytic activity of nanometer bismuth titanate powder, so have better industrial prospect.
The porous bismuth titanate photocatalyst that is used for degradable organic pollutant that the present invention proposes, has unique meso-hole structure, specific area is in 20～60 meters squared per gram, the aperture is about 1.7 nanometers, the aggregate particle size is 5～20 microns, and what form aggregate is the bismuth titanates nanometer crystal grain (seeing accompanying drawing 1) of sillenite crystal formation.The microstructure of this photochemical catalyst is seen accompanying drawing 2.
The preparation method of porous bismuth titanate photocatalyst among the present invention, comprise solvent thermal synthesis process and last handling process, utilize bismuth nitrate and titanate esters to be raw material, the block interpolymers surfactant is a structure directing agent, the employing glacial acetic acid is a hydrolyst, at first prepares the titanium bismuth composite oxide with solvent-thermal method, pass through washing, filtration, drying again after, high-temperature roasting removes the block interpolymers surfactant and makes it crystallization, forms by the sillenite crystalline phase to pile up the porous bismuth titanate photocatalyst that forms.
This mesoporous photocatalytic agent adopts solvent-thermal method synthetic, wherein the source of titanium is a titanate esters, the source of bismuth is five water bismuth nitrates, and the mol ratio of each component is a titanate esters when synthetic: bismuth nitrate: acetate: block interpolymers surfactant=1: 10～14: 350: 0.17～0.34.
The preparation method of porous bismuth titanate photocatalyst of the present invention, wherein the titanium bismuth composite oxide is prepared by three-step approach:
(a) add five water bismuth nitrates in concentration is the acetic acid solution of block interpolymers surfactant of 50～100 grams per liters, the mass ratio that makes five water bismuth nitrates and acetate is 17: 50, constantly is stirred to five water bismuth nitrates and dissolves fully;
(b) be that 1: 10 to 1: 14 titanate esters dropwise joins in above-mentioned (a) solution with titanium/bismuth mol ratio, constantly stir and obtain complex sol;
(c), be transferred in the autoclave of sealing 140 ℃～160 ℃ following solvent thermal crystallisations 12～36 hours, after the gel that forms is taken out, through washing, filter, be drying to obtain the titanium bismuth composite oxide with complex sol ageing at room temperature after 12 hours.
The concrete preparation method of the porous bismuth titanate photocatalyst that is used for degradable organic pollutant that the present invention proposes is as follows: be that to add the mass ratio that five water bismuth nitrates make it with acetate be 17: 50 for the acetic acid solution of the block interpolymers surfactant of 50～100 grams per liters in concentration, constantly be stirred to dissolving fully, with mol ratio is titanium: bismuth is that 1: 10～14 titanate esters dropwise joins in the above-mentioned solution, constantly stirs and obtains complex sol.The ageing at room temperature of this complex sol is transferred to 140～160 ℃ of lower seal crystallization in the autoclave after 12 hours, after 12～36 hours, the taking-up of composite oxides sediment is washed with deionized water, filter, behind 120～150 ℃ of following drying and dehydratings,, remove the block interpolymers surfactant in 380～550 ℃ of insulation high-temperature roastings in 3 hours down, and make the bismuth titanates crystallization, promptly get target product.
Among the present invention, used titanate esters is a kind of of butyl titanate, isopropyl titanate; Structure directing agent is a kind of of block interpolymers surfactant P123, F108, F127.Wherein, the molecular formula of P123 is PEO20-PPO70-PEO20, and molecular weight is 5750 gram/moles; The molecular formula of F108 is PEO132-PPO50-PEO132, and molecular weight is 15500 gram/moles; The molecular formula of F127 is PEO106-PPO70-PEO106, and molecular weight is 14600 gram/moles.
The present invention before crystallization process with acetate as solvent and hydrolysis acid catalyst, hydrolysis is relaxed more, and the hydrolytic process of titanate esters and bismuth nitrate is suppressed mutually, obtain more uniform composite oxide sol easily.Activity to photochemical catalyst provided by the invention can be tested with the following method:
Accurately take by weighing 0.05～0.2 gram porous bismuth titanate powder, it is joined in the organic aqueous solution that 100 ml concns are 10～30 mg/litre then, under the ultrasonic wave effect, make suspension, under xenon lamp (simulated solar spectrum, 500 watts) irradiation, react.4 milliliters of samplings in per 20 minutes, catalyst is removed with high speed centrifugation.The ultraviolet-visible spectrum of surplus solution is analyzed on ultraviolet specrophotometer (Varian, Cary50 type).Degradation rate (%)=residual organic substances concentration/initial organic concentration) * 100.
Photochemical catalyst provided by the invention has following advantage:
1. have unique meso-hole structure, aggregate is of a size of 5～20 microns, and crystal grain is the nano particle with sillenite crystal formation, and its specific area is 20～60 meters squared per gram.
2. be light source with the xenon lamp, having in the future directly, the application sunshine is the potentiality of light source; Need not oxidant applying and auxiliary agent, can a step degradable organic pollutant.
3. the catalytic activity height of this catalyst can be applicable to have better industrial application prospects in the multiple organic photocatalytic degradation reaction.
4. this catalyst reaction preparation technology is simple, and the reaction condition gentleness is low to the reaction unit requirement, is a kind of pervasive multifunctional photocatalysis agent.
Description of drawings
Fig. 1 is the Large-angle X-ray diffraction spectrogram of porous bismuth titanate photocatalyst;
Fig. 2 is the scanning electron microscope image of porous bismuth titanate photocatalyst under different resolution;
Fig. 3 is the ultraviolet-visible light diffuse reflection absorption spectrum with the porous bismuth titanate photocatalyst of the inventive method preparation;
Fig. 4～6 are that the uv-visible absorption spectroscopy of its aqueous solution is penetrated the variation of time with illumination in the process of using porous bismuth titanate photocatalyst photocatalytic degradation acridine orange of the present invention, xylenol orange, dimethyl diaminophenazine chloride.
The specific embodiment
5 gram P123 block interpolymers surfactant dissolves are in 50 milliliters of acetate (CH
3COOH) form the solution of concentration 100 grams per liters in, add 17 grams, five water bismuth nitrate (Bi (NO
3)
35H
2O), constantly be stirred to dissolving fully, dropwise add 0.85 gram butyl titanate (Ti (OC then
4H
9)
4), this moment, titanium/bismuth mol ratio was 1: 14.Vigorous stirring forms uniform sol.Ageing moved to aforementioned colloidal sol in the autoclave after 12 hours, 150 ℃ of following crystallization 24 hours, took out the composite oxides gel precipitation, spent deionised water, 120 ℃ of evaporation oven dry down, obtained the titanium bismuth composite oxide.The gained precursor powder is roasting 3 hours in the atmospheric air atmosphere under 550 ℃ temperature, promptly obtains porous bismuth titanate photocatalyst, is designated as the 1# sample.This sample is measured through nitrogen adsorption-desorption specific surface pore size distribution determination method, and its specific area is 21 meters squared per gram, and the aperture is about 1.7 nanometers.
Embodiment 2
2.5 gram F108 block interpolymers surfactant dissolves forms the solution of concentration 50 grams per liters in 50 milliliters of acetate, add 17 grams, five water bismuth nitrates, constantly is stirred to dissolving fully, dropwise adds 0.71 gram isopropyl titanate (Ti (OC then
3H
7)
4), this moment, titanium/bismuth mol ratio was 1: 14.Vigorous stirring forms uniform sol.Ageing moved to aforementioned colloidal sol in the autoclave after 12 hours, 140 ℃ of following crystallization 12 hours, took out gel precipitation, and washing 140 ℃ of evaporation oven dry down, obtains the titanium bismuth composite oxide.The gained precursor powder is roasting 3 hours in the atmospheric air atmosphere under 550 ℃ temperature, promptly obtains porous bismuth titanate photocatalyst, is designated as the 2# sample.Its specific area is 25.4 meters squared per gram, and the aperture is about 1.6 nanometers.
Embodiment 3
5 gram P123 block interpolymers surfactant dissolves form the solution of concentration 100 grams per liters in 50 milliliters of acetate, add 17. grams, five water bismuth nitrates, constantly be stirred to dissolving fully, dropwise add 0.88 gram butyl titanate then, this moment, titanium/bismuth mol ratio was 1: 13.5.Vigorous stirring forms uniform sol.Ageing moved to aforementioned colloidal sol in the autoclave after 12 hours, 150 ℃ of following crystallization 24 hours, took out the composite oxides gel precipitation, and washing 130 ℃ of evaporation oven dry down, obtains the titanium bismuth composite oxide.The gained precursor powder is roasting 3 hours in the atmospheric air atmosphere under 550 ℃ temperature, promptly obtains porous bismuth titanate photocatalyst, is designated as the 3# sample.Its specific area is 20.2 meters squared per gram, and the aperture is about 1.7 nanometers.
Embodiment 4
3 gram F127 block interpolymers surfactant dissolves form the solution of concentration 60 grams per liters in 50 milliliters of acetate, add 17 grams, five water bismuth nitrates, constantly are stirred to dissolving fully, dropwise add 0.99 gram butyl titanate then, and this moment, titanium/bismuth mol ratio was 1: 12.Vigorous stirring forms uniform sol.Ageing moved to aforementioned colloidal sol in the autoclave after 12 hours, 150 ℃ of following crystallization 36 hours, took out the composite oxides gel precipitation, and washing 130 ℃ of evaporation oven dry down, obtains the titanium bismuth composite oxide.The gained precursor powder is roasting 3 hours in the atmospheric air atmosphere under 450 ℃ temperature, promptly obtains porous bismuth titanate photocatalyst, is designated as the 4# sample.Its specific area is 46.5 meters squared per gram, and the aperture is about 1.9 nanometers.
Embodiment 5
3.2 gram P123 block interpolymers surfactant dissolves forms the solution of concentration 64 grams per liters in 50 milliliters of acetate, add 17 grams, five water bismuth nitrates, constantly be stirred to dissolving fully, dropwise add 1.19 gram butyl titanates then, this moment, titanium/bismuth mol ratio was 1: 10.Vigorous stirring forms uniform sol.Ageing moved to aforementioned colloidal sol in the autoclave after 12 hours, 160 ℃ of following crystallization 36 hours, took out the composite oxides gel precipitation, and washing 150 ℃ of evaporation oven dry down, obtains the titanium bismuth composite oxide.The gained precursor powder is roasting 3 hours in the atmospheric air atmosphere under 380 ℃ temperature, promptly obtains porous bismuth titanate photocatalyst, is designated as the 5# sample.Its specific area is 58.1 meters squared per gram, and the aperture is about 1.7 nanometers.
Above-mentioned catalyst is applied to respectively in the different light-catalyzed reactions, and for example down, table 1 is the detailed experiments result to active fructufy:
Reaction 1: take by weighing 0.1 gram 1# sample, it is joined in the methyl orange aqueous solution that 100 ml concns are 15 mg/litre, under ultrasonication, make suspension, magnetic agitation is reacted under xenon lamp (simulated solar spectrum, 500 watts) irradiation, 4 milliliters of samplings in per 20 minutes, high speed centrifugation separates, and (Varian analyzes on cary50) at ultraviolet-visible spectrometer to get supernatant liquor.
Reaction 2: take by weighing 0.05 gram 1# sample, it is joined in the methyl orange aqueous solution of 100 milliliter of 15 mg/litre react, surplus person is with reaction 1.
Reaction 3: take by weighing 0.1 gram 2# sample, it is joined in the methyl orange aqueous solution of 100 milliliter of 15 mg/litre react, surplus person is with reaction 1.
Reaction 4: take by weighing 0.1 gram 3# sample, it is joined in the methyl orange aqueous solution of 100 milliliter of 15 mg/litre react, surplus person is with reaction 1.
Reaction 5: take by weighing 0.15 gram 4# sample, it is joined in the methyl orange aqueous solution of 100 milliliter of 30 mg/litre react, surplus person is with reaction 1.
Reaction 6: take by weighing 0.1 gram 5# sample, it is joined in the methyl orange aqueous solution of 100 milliliter of 15 mg/litre react, surplus person is with reaction 1.
Reaction 7: take by weighing 0.2 gram 1# sample, it is joined in the bromocresol green aqueous solution of 100 milliliter of 10 mg/litre react, surplus person is with reaction 1.
Reaction 8: take by weighing 0.15 gram 2# sample, it is joined in the acridine orange aqueous solution of 100 milliliter of 20 mg/litre react (see figure 4), surplus person is with reaction 1.
Reaction 9: take by weighing 0.1 gram 1# sample, it is joined in the xylenol orange aqueous solution of 100 milliliter of 20 mg/litre react (see figure 5), surplus person is with reaction 1.
Reaction 10: take by weighing 0.1 gram 1# sample, it is joined in the neutral red aqueous solution of 100 milliliter of 20 mg/litre react (see figure 6), surplus person is with reaction 1.
Table 1
| Reaction | Sample number | Reaction time (hour) | Degradation effect of |
| 1 | 1# | 1.0 | 68% (methyl orange, down together) |
| 2 | 1# | 1.5 | 78％ |
| 3 | 2# | 1.0 | 56％ |
| 4 | 3# | 3 | 95％ |
| 5 | 4# | 2.0 | 34％ |
| 6 | 5# | 2.0 | 89％ |
| 7 | 1# | 1.5 | 31% (bromocresol green) |
| 8 | 2# | 1.0 | 95% (bifurcation is stung orange) |
| 9 | 1# | 1.0 | 98% (xylenol orange) |
| 10 | 1# | 1.0 | 66% (dimethyl diaminophenazine chloride) |
Claims (6)
1. the preparation method of a porous bismuth titanate photocatalyst, comprise solvent thermal synthesis process and last handling process, it is characterized in that: utilize five water bismuth nitrates and titanate esters to be raw material, the block interpolymers surfactant is a structure directing agent, employing acetate is hydrolyst, at first prepare the titanium bismuth composite oxide,, form by the sillenite crystalline phase and pile up the porous bismuth titanate photocatalyst that forms again through removing the block interpolymers surfactant and making it crystallization with solvent-thermal method.
2. the preparation method of photochemical catalyst as claimed in claim 1, wherein the titanium bismuth composite oxide is prepared by three-step approach:
(a) add five water bismuth nitrates in concentration is the acetic acid solution of block interpolymers surfactant of 50～100 grams per liters, the mass ratio that makes five water bismuth nitrates and acetate is 17: 50, constantly is stirred to five water bismuth nitrates and dissolves fully;
(b) be that 1: 10 to 1: 14 titanate esters dropwise joins in above-mentioned (a) solution with titanium/bismuth mol ratio, constantly stir and obtain complex sol;
(c) with complex sol ageing at room temperature after 12 hours.Be transferred in the autoclave of sealing 140 ℃～160 ℃ following solvent thermal crystallisations 12～36 hours, after the gel that forms is taken out, through washing, filter, be drying to obtain the titanium bismuth composite oxide.
3. the preparation method of photochemical catalyst as claimed in claim 1 or 2, wherein said titanate esters is butyl titanate or isopropyl titanate.
4. the preparation method of photochemical catalyst as claimed in claim 1 or 2, wherein said block interpolymers surfactant is P123, F108 or F127, the three is the polyoxyethylene-poly-oxypropylene polyoxyethylene block polyether.
5. the preparation method of photochemical catalyst as claimed in claim 4, the molecular formula of wherein said P123 is PEO20-PPO70-PEO20, molecular weight is 5750 gram/moles; The molecular formula of F108 is PEO132-PPO50-PEO132, and molecular weight is 15500 gram/moles; The molecular formula of F127 is PEO106-PPO70-PEO106, and molecular weight is 14600 gram/moles.
6. the preparation method of photochemical catalyst as claimed in claim 2, wherein from crystallizing kettle, take out, after filtration, Drying of gels temperature after the washing is 120～150 ℃, then in 380～550 ℃ of insulations high-temperature roasting in 3 hours, remove the block interpolymers surfactant, and make the further crystallization of bismuth titanates.
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