CN102701276A - Hollow TiO2 microsphere synthesizing method - Google Patents
Hollow TiO2 microsphere synthesizing method Download PDFInfo
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- CN102701276A CN102701276A CN201210172919XA CN201210172919A CN102701276A CN 102701276 A CN102701276 A CN 102701276A CN 201210172919X A CN201210172919X A CN 201210172919XA CN 201210172919 A CN201210172919 A CN 201210172919A CN 102701276 A CN102701276 A CN 102701276A
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Abstract
The invention discloses a hollow TiO2 microsphere synthesizing method, and belongs to the field of solar energy utilizing photovoltaic technology and photocatalysts. In the hollow TiO2 microsphere synthesizing method, through hydrothermal treatment, tetrabutyl titanate is directly taken as an oil phase and forms an emulsion dispersion system with water to obtain a TiO2 hollow spherical particle; a hollow characteristic is obtained through simple change in the mixing sequence of raw materials; the substantial part of the TiO2 hollow spherical particle has a three-dimensional interpenetrating network structure formed by a nano TiO2 crystal grain and a nano-sized space; the average diameter of the spherical particle is 0.5-1.5 microns and can be adjusted by changing the adding amount of a surfactant; the specific surface area of the spherical particle is 32-97 m2/g; the apparent density of the spherical particle is 1.91 g/cm3. When the hollow spherical particle is used as an electrode material of a dye-sensitized TiO2 solar cell, the optical path can be elongated and the utilization efficiency of light energy can be improved; and when the hollow spherical particle is used as a photocatalyst, the photocatalytic activity is high and the hollow spherical particle is easily separated from a liquid medium.
Description
Technical field
The present invention relates to a kind of hollow TiO
2The preparation method of microballoon belongs to photovoltaic technology and photocatalyst field that sun power utilizes.
Background technology
The major objective of solar cell research is to be devoted to improve light-photoelectric transformation efficiency.For dye sensitization TiO
2Solar cell, its photoelectric transformation efficiency and TiO
2The microstructure of electrode has confidential relation.As the TiO that forms electrode
2Size of particles increases to visible wavelength when suitable, owing to its enhancing to the visible light scattering process has prolonged light path, thereby helps improving the capture rate of dye molecule to light.But TiO
2When being beneficial to scattering of light, the increase of size of particles also reduced TiO
2Specific surface area.And the TiO of little nano-scale
2Particle has big specific surface area, but is unfavorable for the scattering effect of visible light.Therefore, formed naturally and utilized nanoparticle and macrobead TiO
2The thinking of combined preparation electrode.Research shows, for macrobead TiO
2Microballoon is a hollow microsphere if inside can form cavity, and the scattering that then utilizes its spherical shell and cavity can further prolong light path and increase the assimilated efficiency of light, thereby helps improving the light-photoelectric transformation efficiency of solar cell.On the other hand, at TiO
2As the application facet of photocatalyst, nano-TiO
2Powder has showed relative advantages of high catalytic activity because of its nanometer size effect and high specific surface area, but nano-TiO
2Powder in use with the separation difficulty of medium liquid.Therefore, also need still can not obviously reduce its specific surface area through the size that increases particle.Synthesizing porous property TiO
2Microballoon can address this problem equally.
Summary of the invention
To above-mentioned this requirement, the present invention proposes a kind of stable dispersion system of tensio-active agent that utilizes and synthesizes hollow TiO
2The method of microballoon.Adopt the method (being about to water adds in the oil phase) that changes reinforced order to obtain the stable double-deck interface dispersion system of tensio-active agent, thereby realize the synthetic of hollow sphere; This method is compared with the emulsion system of routine, because of the organic solvent that do not use other as oil phase, avoided follow-up Recovery of Organic Solvent problem, so technology is simple, with low cost, and environmental protection; The synthetic TiO of institute
2The spherical shell of microballoon is a kind of low density and has the random network structure in a large amount of nano-scales cavity, and whole structures is made up of nanocrystal and nanometer space; The size of spherolite can be regulated through changing amount of surfactant; Prepared hollow TiO
2The microballoon specific surface area is 97 m
2/ g, apparent density is 1.91 g/cm
3
The present invention realizes above-mentioned TiO
2The technical scheme of hollow microsphere is: carry out complexing with methyl ethyl diketone (ACAC) earlier before tetrabutyl titanate (TBOT) uses and stablize, and with it as oil phase.Then the aqueous solution with tensio-active agent in the slow above-mentioned oil phase that adds, forms milky dispersion system under stirring condition.After the aqueous solution gets into oil phase on a small quantity, under influence of surfactant, at first formed the emulsion of w/o type.Along with the further increase of aqueous solution add-on, emulsion system is converted into the O/W type from w/o type.Original globule in oil phase that forms has formed the kernel water in the dispersed oil droplets.In fact promptly formed W/O/W type emulsion.Then this emulsion system is placed hydrothermal treatment consists 24 h under 100~200 ℃ the condition, dispersive TBOT particle generation hydrolysis-condensation reaction forms anatase titanium dioxide TiO
2, the kernel water that comprises volatilization and form the cavity of spherolite in subsequently drying and heat treatment process.In this reaction, because titanium hydrolysis of alkoxide speed is very high, so it is stable to adopt the ACAC complexing agent in advance it to be carried out complexing.
A kind of hollow TiO
2The preparation method of microballoon, carry out according to following step:
(1) tetrabutyl titanate (TBOT) and methyl ethyl diketone (ACAC) are pressed the amount of substance ratio
n(ACAC)/
n(TBOT)=1~5 be mixed into oil phase liquid, stirring reaction 0.5 h.
(2) aqueous solution of getting the Witco 1298 Soft Acid of certain volume slowly joins under condition of stirring in the above-mentioned oil phase liquid, forms milky dispersion system; The water volume ratio of wherein said oil phase and adding does
V o/
V w=0.05~0.6;
(3) above-mentioned dispersion system is transferred in the reaction kettle that has cup in the tetrafluoroethylene reaction 24 h under 100~200 ℃ temperature;
(4) reacted product is after processes such as spinning, water washing and washing with alcohol, dry 2 h under 100 ℃ temperature.
(5) at last with sample 550 ℃ of thermal treatment 0.5 h in retort furnace, can obtain hollow TiO
2Microballoon.
Wherein the concentration of the aqueous solution of the described Witco 1298 Soft Acid of step (1) is 72~800 mg/L.
Advantage of the present invention:
1. synthetic TiO of the present invention
2Hollow sphere can utilize the surfaces externally and internally of its spherical shell the incident scattering of light to be improved the efficiency of light absorption of dye sensitization solar battery.While synthetic TiO of the present invention
2Hollow sphere sedimentation in aqueous media is easy, uses as photocatalyst, can improve TiO
2The repeat usage of photocatalyst.
2. the present invention's employing prepares TiO to the one step that the emulsification dispersion system carries out hydrothermal treatment consists
2Hollow sphere, synthesis technique is simple.
3. the emulsification system that adopts of the present invention is compared with the emulsion system of routine, because of the organic solvent that do not use other as oil phase, avoided follow-up Recovery of Organic Solvent problem, so not only technology is simply but also with low cost for this compound method.
4. the synthetic TiO of institute of the present invention
2The hollow sphere size has certain distribution density, can mate the monochromatic ray of various wavelength in the sunshine, thereby can further increase incident scattering of light degree, improves the efficiency of light absorption of dye sensitization solar battery.
5. the synthetic TiO of institute of the present invention
2The spherical shell of microballoon presents a kind of low density and has the random network structure in a large amount of nano-scales cavity on microcosmic; And whole structures is made up of nanocrystal and nanometer space; Therefore photocatalytic activity is high, also can be applicable to industrial dyeing waste water, contains the processing of greasy dirt waste water etc.
6. the prepared TiO of the present invention
2The mean sizes of microballoon can be regulated through changing amount of surfactant within the specific limits.
Description of drawings:
The TiO that Fig. 1: embodiment 1 is prepared
2The electron micrograph of hollow sphere, its right-of-center in political views figure are the photo of the bigger magnification of respective left figure sample.
The TiO that Fig. 2: embodiment 2 is prepared
2The electron micrograph of hollow sphere, its right-of-center in political views figure are the photo of the bigger magnification of respective left figure sample.
Fig. 3: the TiO that the present invention is prepared
2Hollow sphere is to the photocatalytic degradation effect of methylene blue.
Fig. 4: the TiO that the present invention is prepared
2The digital camera photo of hollow sphere water system suspension liquid before leaving standstill and after leaving standstill 1.5 h.Experiment shows that spherolite has good settling character in water.
Fig. 5: TiO
2The relation of the transmittance of hollow microsphere electrode film and the number of plies of filming.
Concrete embodiment
With concrete embodiment the present invention is further specified below.
Embodiment 1:
(1) 5 mL tetrabutyl titanates is mixed stirring reaction 0.5 h with 2 mL methyl ethyl diketones.This reaction is thermopositive reaction.When reverting to room temperature, the temperature of treating system just can carry out next step operation.
(2) get 50 mL, the aqueous solution of 72 mg/L Witco 1298 Soft Acids slowly joins in the aforesaid liquid under condition of stirring, forms milky dispersion system.Continue to stir 1 h.
(3) above-mentioned dispersion system is transferred in the reaction kettle that has cup in the tetrafluoroethylene reaction 24 h under 150 ℃ temperature.
(4) reacted product is after processes such as spinning, water washing and washing with alcohol, dry 2 h under 100 ℃ temperature.
(5) at last sample 550 ℃ of thermal treatment 0.5 h in retort furnace are obtained TiO
2Microspherical catalyst.Its electron micrograph such as Fig. 1.Can see that particle appearance is spherical, the surface shows comparatively coarse on microcosmic; Have dispersed preferably; The size of particle has the certain distributed width, and the mean diameter of being added up by microscopic is 1.5 microns; Simultaneously can observe spherolite and be the hollow form, the similar Pericarppium arachidis hypogaeae structure of ball wall.By N
2The surface-area that adsorption experiment records is 97 m
2/ g.
(6) prepared TiO
2The photocatalysis performance test process of microballoon is following:
(a) with 40 mg hollow TiO
2The microballoon powder is scattered in 50 mL, and concentration is in the aqueous solution of methylene blue of 5 mg/L, adopts magnetic agitation that powder granule is dispersed in the solution.
(b) the suspension-s system with above-mentioned steps (a) configuration places the uv lamp of 30 W to shine down, and fluorescent tube is apart from liquid level 14 cm.Adopt the regularly concentration of methylene blue solution in the mensuration system of spectrophotometer.Before measuring methylene blue concentration, must adopt centrifugal separation method that system is carried out solid-liquid separation earlier, the clear solution of getting the upper strata then carries out the mensuration of absorbancy.
(c) by the photocatalytic degradation rate of the change calculations methylene blue of methylene blue concentration in the system.The degradation rate of methylene blue and UV-irradiation time relation are as shown in Figure 3.When shining 4 h, the degradation rate of methylene blue is 92%.
(7) prepared TiO
2The separation performance evaluation procedure of hollow microsphere and water is following:
(a) the configuration solid content is the TiO of 20 g/L
2The hollow microsphere aqueous suspension places the test tube that fills 8 these suspension liquids of mL on the test-tube stand.In the process of leaving standstill; Because of particles settling; It is Clear & Transparent that the top of test tube becomes gradually; Bottom then solid content increases, and the observation suspension liquid is tapered to by the muddy system of homogeneous and obvious transparent layer and needed time of white solid layering occur, and Fig. 3 has represented that suspension liquid leaves standstill the digital camera photo of 1.5 h front and back.The photo of Fig. 3 shows: in 1.5 h, the spherolite in the suspension liquid almost all deposits, and good natural deposition characteristics is arranged.
(b) system after the layering is separated, the wet solid after the separation is dry 2 h under 100 ℃, carry out weighing after the cooling.By the operation before and after microballoon Mass Calculation TiO
2The recovery after hollow microsphere uses is 99%.
(8) TiO
2The preparation of hollow microsphere electrode and the test process of transmittance thereof are following:
(a) 0.5 g hollow sphere is disperseed in the mixed solvent of 4.5 mL water and 4.5 mL absolute ethyl alcohols composition, stir suspension liquid and make solvent evaporates to system have suitable viscosity, adopt the frictioning method to form coating at glass basic surface.
(b) carry out the repetition coating operation after the coating drying.
(c) adopt the absorbancy of ultraviolet-visible light spectrophotometry different thickness film, and calculate the transmittance of film thus.Fig. 4 has represented the relation of transmittance and its thickness of film.Filming 1~2 layer time, film has higher transmittance, but when the number of plies was increased to more than 3 layers, the transmittance of film reduced to about 1%.Therefore use as membrane electrode, film and to have satisfied request for utilization 3 layers time.
Embodiment 2:
(1) 5 mL tetrabutyl titanates is mixed stirring reaction 0.5 h with 2 mL methyl ethyl diketones.This reaction is thermopositive reaction.When reverting to room temperature, the temperature of treating system just can carry out next step operation.
(2) get 50 mL, the aqueous solution of 800 mg/L Witco 1298 Soft Acids slowly joins in the aforesaid liquid under condition of stirring, forms milky dispersion system.Continue to stir 1 h.
(3) above-mentioned dispersion system is transferred in the reaction kettle that has cup in the tetrafluoroethylene reaction 24 h under 150 ℃ temperature.
(4) reacted product is after processes such as spinning, water washing and washing with alcohol, dry 2 h under 100 ℃ temperature.
(5) at last sample 550 ℃ of thermal treatment 0.5 h in retort furnace are obtained TiO
2Microspherical catalyst.Its electron micrograph such as Fig. 2.The particle profile is similar to the product that embodiment 1 obtains, and except spheroidal particle, has also generated the powder of some nano-scales in the system.Spheroidal particle mean diameter by the microscopic statistics is 0.5 micron.By N
2The surface-area that adsorption experiment records is 32 m
2/ g.
(6) prepared TiO
2The photocatalysis performance test process of microballoon is following:
(a) with 40 mg TiO
2The microballoon powder is scattered in 50 mL, and concentration is in the aqueous solution of methylene blue of 5 mg/L, adopts magnetic agitation that powder granule is dispersed in the solution.
(b) the suspension-s system with above-mentioned steps (a) configuration places the uv lamp of 30 W to shine down, and fluorescent tube is apart from liquid level 14 cm.Adopt the regularly concentration of methylene blue in the mensuration system of spectrophotometer.Before measuring methylene blue concentration, must adopt centrifugal separation method that system is carried out solid-liquid separation earlier, the clear solution of getting the upper strata then carries out the mensuration of absorbancy.
(c) by the degradation rate of the change calculations methylene blue of methylene blue concentration in the system.Fig. 3 has shown the hollow TiO that embodiment 2 is prepared
2Microballoon is to the photocatalytic degradation effect of methylene blue.Behind UV-irradiation 4 h, the degradation rate of methylene blue reaches 99 %.
Claims (2)
1. hollow TiO
2The preparation method of microballoon is characterized in that carrying out according to following step:
(1) be 1~5 to be mixed into oil phase liquid, stirring reaction 0.5 h with tetrabutyl titanate and methyl ethyl diketone by the amount of substance ratio;
(2) aqueous solution of getting the Witco 1298 Soft Acid of certain volume slowly joins under condition of stirring in the above-mentioned oil phase liquid, forms milky dispersion system; The water volume ratio of wherein said oil phase and adding is 0.05~0.6;
(3) above-mentioned dispersion system is transferred in the reaction kettle that has cup in the tetrafluoroethylene reaction 24 h under 100~200 ℃ temperature;
(4) reacted product is after processes such as spinning, water washing and washing with alcohol, dry 2 h under 100 ℃ temperature;
(5) at last with sample 550 ℃ of thermal treatment 0.5 h in retort furnace, can obtain hollow TiO
2Microballoon.
2. a kind of hollow TiO according to claim 1
2The preparation method of microballoon is characterized in that wherein the concentration of the aqueous solution of the described Witco 1298 Soft Acid of step (1) is 72~800 mg/L.
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Cited By (9)
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CN103894163A (en) * | 2012-12-24 | 2014-07-02 | 北京有色金属研究总院 | High-performance nanometer TiO2 photocatalyst material and preparation method thereof |
CN103950975A (en) * | 2014-04-17 | 2014-07-30 | 渤海大学 | Method for preparing hollow rutile micron titanium dioxide |
CN104192895A (en) * | 2014-08-12 | 2014-12-10 | 渤海大学 | Method for preparing nanometer TiO2 microspheres |
CN104310466A (en) * | 2014-10-10 | 2015-01-28 | 常州大学 | Hollow titanium dioxide microsphere based on gel sphere precursor and preparation method of hollow titanium dioxide microsphere |
CN104817106A (en) * | 2015-05-07 | 2015-08-05 | 中国科学院合肥物质科学研究院 | Solvothermal synthetic method of TiO2 hollow-structure submicron spheres |
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CN107021522A (en) * | 2017-05-05 | 2017-08-08 | 常州大学 | A kind of single dispersing TiO based on microemulsion2The synthetic method of microballoon |
CN107253735A (en) * | 2017-07-21 | 2017-10-17 | 陕西科技大学 | Hollow nano TiO 2 microballoon and preparation method thereof |
CN113772722A (en) * | 2021-10-28 | 2021-12-10 | 中国科学院合肥物质科学研究院 | TiO with special hollow structure2Preparation method of micro-spheres |
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CN1765511A (en) * | 2005-10-13 | 2006-05-03 | 武汉理工大学 | PH adjusting hydrothermal preparation method of active nano crystal mesoporous titanium dioxide photocatalytic material |
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CN103894163A (en) * | 2012-12-24 | 2014-07-02 | 北京有色金属研究总院 | High-performance nanometer TiO2 photocatalyst material and preparation method thereof |
CN103894163B (en) * | 2012-12-24 | 2016-02-24 | 北京有色金属研究总院 | A kind of high-performance nano TiO 2photocatalyst material and preparation method thereof |
CN103950975A (en) * | 2014-04-17 | 2014-07-30 | 渤海大学 | Method for preparing hollow rutile micron titanium dioxide |
CN103950975B (en) * | 2014-04-17 | 2015-05-06 | 渤海大学 | Method for preparing hollow rutile micron titanium dioxide |
CN104192895A (en) * | 2014-08-12 | 2014-12-10 | 渤海大学 | Method for preparing nanometer TiO2 microspheres |
CN104192895B (en) * | 2014-08-12 | 2018-07-10 | 渤海大学 | A kind of nano-TiO2The preparation method of microballoon |
CN104310466B (en) * | 2014-10-10 | 2016-03-09 | 常州大学 | A kind of hollow titanium dioxide microballoon based on gel ball presoma and preparation method thereof |
CN104310466A (en) * | 2014-10-10 | 2015-01-28 | 常州大学 | Hollow titanium dioxide microsphere based on gel sphere precursor and preparation method of hollow titanium dioxide microsphere |
CN104817106B (en) * | 2015-05-07 | 2017-03-15 | 中国科学院合肥物质科学研究院 | TiO2The solvent process for thermosynthesizing of hollow-core construction sub-micron ball |
CN104817106A (en) * | 2015-05-07 | 2015-08-05 | 中国科学院合肥物质科学研究院 | Solvothermal synthetic method of TiO2 hollow-structure submicron spheres |
CN105348795A (en) * | 2015-12-01 | 2016-02-24 | 仇颖超 | Preparation method of modified titanium dioxide/polyimide resin composite |
CN107021522A (en) * | 2017-05-05 | 2017-08-08 | 常州大学 | A kind of single dispersing TiO based on microemulsion2The synthetic method of microballoon |
CN107253735A (en) * | 2017-07-21 | 2017-10-17 | 陕西科技大学 | Hollow nano TiO 2 microballoon and preparation method thereof |
CN113772722A (en) * | 2021-10-28 | 2021-12-10 | 中国科学院合肥物质科学研究院 | TiO with special hollow structure2Preparation method of micro-spheres |
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