CN102863021A - Method for preparing anatase phase nanometer titanium dioxide through hydrothermal interface reaction - Google Patents
Method for preparing anatase phase nanometer titanium dioxide through hydrothermal interface reaction Download PDFInfo
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- CN102863021A CN102863021A CN2012103334236A CN201210333423A CN102863021A CN 102863021 A CN102863021 A CN 102863021A CN 2012103334236 A CN2012103334236 A CN 2012103334236A CN 201210333423 A CN201210333423 A CN 201210333423A CN 102863021 A CN102863021 A CN 102863021A
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Abstract
The invention discloses a method for preparing anatase phase nanometer titanium dioxide through hydrothermal interface reaction. The method comprises the following steps: (a), water and toluene are added to a reactor and stirred according to the volume ratio of 0-1:1-2 of water and toluene, absolute ethyl alcohol solution containing butyl titanate is added to the reactor, and the pH value of the solution is maintained to be 4.0, so that mixture is obtained; (b), the mixture is stirred for two hours, the mixture is reacted in a reaction kettle and is then stilled and placed at the temperature of 140-1800 DEG C to be aged for 24 hours, and liquid-solid mixture is obtained; and (c), the liquid-solid mixture is taken out and filtered, and is alternately rinsed by water and ethanol, the liquid-solid mixture is rinsed to be neutral, the filtration product is dried to obtain white powder, then the white powder is rotated for 5 hours, and titanium dioxide powder is finally obtained. Compared with the prior art, the method has the following advantages: in the preparation process, the reaction conditions are mild, no special equipment is needed, no waste liquid is generated, the method is simple and feasible, meanwhile the preparation cycle is short, and the industrial production can be realized easily.
Description
Technical field
The present invention relates to the method that a kind of hydro-thermal surface reaction prepares anatase-phase nano titanium dioxide, belong to inorganic porous material and field of nanometer material technology.
Background technology
About the preparation of nano titanium oxide, a lot of relevant reports has been arranged both at home and abroad, titanium dioxide nano-particle is by the oxide compound of broad research, because it is in photochemical catalysis, sensor, solar cell, the aspects such as mesopore film have a wide range of applications.In addition, because its nanoscale, so that nanometer titanic oxide material is easy to carry out with organic polymer or small molecule material is compound, prepare the devices such as solar cell by revolving the methods such as way.Nano-titanium dioxide powder be prepared with many methods, such as sol-gel process, coprecipitation method, atomizing thermolysis process etc.But the general particle diameter of the titanium dioxide nano-particle that is synthesized is larger, and synthetic particle size distribution is wide.The synthesis of titanium dioxide nano-particles size is little on the interface that profit forms, narrow size distribution.
Content of the present invention
The present invention utilizes organic solvent and water to form the interface, utilizes the principle of surface reaction to prepare titanium dioxide nanoparticle, and the nano particle of titanium dioxide can cluster become titanium dioxide nanometer microballoons.Utilize scanning electronic microscope, X-ray diffraction (XRD), N
2Adsorption/desorption (BET) characterizes sample.BET result shows and forms meso-hole structure between the internal particle.Synthesis device of the present invention is simple, and is easy to operate, and condition is loose, and raw material is simple and easy to, and the product that obtains simultaneously is pure anatase phase titanium dioxide, and the particle diameter of particle is between 10-20nm, and size is homogeneous relatively.By regulating the ratio of water and organic solvent, can obtain not show on year-on-year basis the titanium dioxide nano material of the porous amassed.
Technical scheme of the present invention is:
A kind of hydro-thermal surface reaction prepares the method for anatase-phase nano titanium dioxide, may further comprise the steps:
A) with water and toluene according to volume ratio water: the proportioning of toluene=0 ~ 1:1 ~ 2 adds in the reactor, stir under the normal temperature, joining the ethanol solution of metatitanic acid four fourth fat lentamente in the reactor, proportioning is the metatitanic acid four fourth fat that every milliliter of toluene adds 0.1g, keeping the pH value of solution in whole adding procedure is 4.0, obtains mixture;
B) said mixture stirs 2h at normal temperatures, changes the reactor internal reaction over to, leaves standstill the aging 24h of the thermostatic drying chamber of putting into 140～180 ° of C temperature, obtains liquid-solid mixture;
C) liquid-solid mixture is taken out rear the filtration, water and ethanol is washing alternately, and washing is arrived neutral, and filtration product at the thermostatic drying chamber inner drying, is obtained the powder of white, and roasting 5h in retort furnace obtains titania powder at last afterwards.
The maintenance pH is that 4.0 method is to wherein dripping hydrochloric acid soln in the described step a).
The concentration of the ethanol solution of metatitanic acid four fourth fat is 0.6mol/L in the described step a).
The present invention has following features:
1. the technology of preparing of anatase-phase nano titanium dioxide provided by the present invention, compare with present technology, have following advantage: preparation process has the reaction conditions gentleness, need not specific installation, produce without any waste liquid, the characteristics that method is simple, and preparation cycle is short, thereby be easy to realize industrialization.
2. can be by regulating the water-oil ratio example, the difference of aging temperature can obtain different-grain diameter, the TiO 2 porous material of the mesoporous anatase phase of different specific surface areas.
3. preparation technology and equipment are simple, easy control of reaction conditions, and controlled titanium dioxide is long-pending and pore distribution than table.
4. the material of preparation has good photocatalytic activity (seeing the test of degraded methylene blue dyestuff under the irradiation of UV-light), has good industrial application value.
Description of drawings
Fig. 1 is sample XRD figure sheet (a) embodiment 1, and (b) embodiment 2, and (c) embodiment 3, and (d) embodiment 4, and (e) embodiment 5, and (f) embodiment 6.
Fig. 2 is the nitrogen adsorption-desorption isotherm of sample and the graph of pore diameter distribution that the DFT method is calculated, and (a) embodiment 1, and (c) embodiment 3, and (d) embodiment 4, and (f) embodiment 6.
Fig. 3 is the scanning electron microscope (SEM) photograph of sample, and (a) embodiment 1, and (b) embodiment 2, and (c) embodiment 3, and (f) embodiment 5.
Fig. 4 is that the titanium dioxide for preparing of the present invention and commodity P25 degrade under the irradiation of UV-light in the methylene blue process, and degradation rate is with the variation of light application time.(a) embodiment 3, (b) commodity P25, and (c) embodiment 1, and (d) embodiment 2.
Embodiment
Embodiment 1
25ml water and 50ml toluene are added in the beaker, begin simultaneously to stir.Claim 5g metatitanic acid four fourth liposoluble (wherein, the concentration of the ethanol solution of metatitanic acid four fourth fat is 0.6mol/L) in the solution of the dehydrated alcohol of 25ml, form the solution of homogeneous transparent.The ethanol solution of metatitanic acid four fourth fat is being joined in the reactor lentamente, remaining 4.0 with the pH value of hydrochloric acid conditioning solution, at room temperature stirring 2h, mixture is being changed over to in the teflon-lined stainless steel cauldron.Leave standstill the aging 24h of the thermostatic drying chamber of putting into 140 ° of C, the liquid-solid mixture taking-up is filtered with vacuum pump using circulatory water, the washing that hockets of the solution of water and ethanol, washing is to neutral, with product at 60 ° of C thermostatic drying chamber inner dryings, then roasting 5h under 500 ° of C of retort furnace obtains titania powder.
As can be seen from Figure 1 the X-ray diffracting spectrum of sample can be fully corresponding with anatase titania standard spectrogram, 8 corresponding anatase octahedrite TiO of diffraction peak difference
2(101), (004), (200), (105), the diffraction peak (JCPDS No.21-1271) of (116) (200) and (215) crystal face and do not have other impurity peaks, sample belongs to Anatase (Fig. 1).Nitrogen adsorption show sample specific surface area is 93.333m
2/ g, pore volume are 0.191cm
3/ g, the aperture is 3.99nm.Utilize the Scherrer formula to calculate particle diameter and be 10.99nm.The Scanning Electron Microscope photos reveal synthetic sample is comprised of the nano particle of assembling.
Embodiment 2:
25ml water and 50ml toluene are added in the beaker, begin simultaneously to stir, claim 5g metatitanic acid four fourth liposoluble (wherein, the concentration of the ethanol solution of metatitanic acid four fourth fat is 0.6mol/L) in the solution of the dehydrated alcohol of 25ml to form the solution of homogeneous transparent.The ethanol solution of metatitanic acid four fourth fat is being joined in the reactor lentamente.PH value to 4.0 with hydrochloric acid conditioning solution at room temperature stirs 2h, and mixture is changed over to in the teflon-lined stainless steel cauldron.Leave standstill the aging 24h of the thermostatic drying chamber of putting into 180 ° of C, the liquid-solid mixture taking-up is filtered with vacuum pump using circulatory water, the washing that hockets of the solution of water and ethanol, washing is to neutral, with 60 ° of C thermostatic drying chambers of product inner drying, then 500 ° of C roastings 5 hours, obtain the titania powder of white.X-ray diffracting spectrum can be fully corresponding with anatase titania standard spectrogram, 8 corresponding anatase octahedrite TiO of diffraction peak difference
2(101), (004), (200), (105), the diffraction peak (JCPDS No.21-1271) of (116) (200) and (215) crystal face and do not have other impurity peaks, sample belongs to Anatase (Fig. 1 b).Nitrogen adsorption and graph of pore diameter distribution show sample specific surface area 121.557m
2/ g, pore volume are 0.199cm
3/ g, the aperture is 4.3nm.Utilize the Scherrer formula to calculate particle diameter and be 13.19nm.The Scanning Electron Microscope photos reveal synthetic sample is comprised of the nano particle of assembling, and has titanium dioxide microballoon sphere to generate.Metatitanic acid four fourth fat form larger titanium complexing ion polymerization cluster in slowly hydrolysis of interface generation and the polycondensation that oil and water form, because the interface is sphere, thereby optimize the coacervate that synthesis condition can form sphere.
Embodiment 3:
25ml water and 50ml toluene are added in the beaker, begin simultaneously to stir, claim 5g metatitanic acid four fourth liposoluble (wherein, the concentration of the ethanol solution of metatitanic acid four fourth fat is 0.6mol/L) in the solution of the dehydrated alcohol of 25ml to form the solution of homogeneous transparent.The ethanol solution of metatitanic acid four fourth fat is being joined in the reactor lentamente.PH value to 4 with hydrochloric acid conditioning solution at room temperature stirs 2h, and mixture is changed over to in the teflon-lined stainless steel cauldron.Leave standstill the aging 24h of the thermostatic drying chamber of putting into 160 ° of C, the liquid-solid mixture taking-up is filtered with vacuum pump using circulatory water, the washing that hockets of the solution of water and ethanol, washing is to neutral, with product at 60 ° of C thermostatic drying chamber inner dryings, then roasting 5h under 500 ° of C of retort furnace obtains titania powder.X-ray diffracting spectrum can be fully corresponding with anatase titania standard spectrogram, 8 corresponding anatase octahedrite TiO of diffraction peak difference
2(101), (004), (200), (105), the diffraction peak (JCPDS No.21-1271) of (116) (200) and (215) crystal face and do not have other impurity peaks, sample belongs to Anatase (Fig. 1 c).Nitrogen adsorption and graph of pore diameter distribution show sample specific surface area are 89.041m
2/ g, pore volume are 0.224cm
3/ g, the aperture is 3.55nm.Utilize the Scherrer formula to calculate particle diameter and be 12.69nm.The Scanning Electron Microscope photos reveal synthetic sample forms the comparison homogeneous of dispersion by the nano particle of assembling.
Embodiment 4:
50ml water and 50ml toluene are added in the beaker, begin simultaneously to stir, claim 5g metatitanic acid four fourth liposoluble (wherein, the concentration of the ethanol solution of metatitanic acid four fourth fat is 0.6mol/L) in the solution of the dehydrated alcohol of 25ml to form the solution of homogeneous transparent.The ethanol solution of metatitanic acid four fourth fat is being joined in the reactor lentamente.PH value to 4 with hydrochloric acid conditioning solution, at room temperature stir 2h, mixture is changed over to in the teflon-lined stainless steel cauldron, leave standstill the aging 24h of the thermostatic drying chamber of putting into 160 ° of C, liquid-solid mixture is taken out with vacuum pump using circulatory water filter, the washing that hockets of the solution of water and ethanol, washing is to neutral, with 60 ° of C thermostatic drying chambers of product inner drying, then at 500 ° of C roasting 5h, obtain the titania powder of white.X-ray diffracting spectrum can be fully corresponding with anatase titania standard spectrogram, 8 corresponding anatase octahedrite TiO of diffraction peak difference
2(101), (004), (200), (105), the diffraction peak (JCPDSNo.21-1271) of (116) (200) and (215) crystal face and do not have other impurity peaks, sample belongs to Anatase (Fig. 1 d).Nitrogen adsorption and graph of pore diameter distribution show sample specific surface area are 65.970m
2/ g, pore volume are 0.162cm
3/ g, the aperture is 3.57nm.Utilize the Scherrer formula to calculate particle diameter and be 12.67nm.
Embodiment 5:
5ml water and 50ml toluene are added in the beaker, begin simultaneously to stir, claim 5g metatitanic acid four fourth liposoluble (wherein, the concentration of the ethanol solution of metatitanic acid four fourth fat is 0.6mol/L) in the solution of the dehydrated alcohol of 25ml to form the solution of homogeneous transparent.The ethanol solution of metatitanic acid four fourth fat is being joined in the reactor lentamente.PH value to 4 with hydrochloric acid conditioning solution, at room temperature stir 2h, mixture is changed over to in the teflon-lined stainless steel cauldron, leave standstill the aging 24h of the thermostatic drying chamber of putting into 160 ° of C, liquid-solid mixture is taken out with vacuum pump using circulatory water filter, the washing that hockets of the solution of water and ethanol, washing is to neutral, with 60 ° of C thermostatic drying chambers of product inner drying, then at 500 ° of C roasting 5h, obtain the titania powder of white.X-ray diffracting spectrum can be fully corresponding with anatase titania standard spectrogram, 8 corresponding anatase octahedrite TiO of diffraction peak difference
2(101), (004), (200), (105), the diffraction peak (JCPDS No.21-1271) of (116) (200) and (215) crystal face and do not have other impurity peaks, sample belongs to Anatase (Fig. 1 e).Nitrogen adsorption and graph of pore diameter distribution show sample specific surface area are 87.462m
2/ g, pore volume are 0.190cm
3/ g, the aperture is 3.1nm.Utilize the Scherrer formula to calculate particle diameter and be 13.14nm.
Embodiment 6:
0ml water and 50ml toluene are added in the beaker, begin simultaneously to stir, claim 5g metatitanic acid four fourth liposoluble (wherein, the concentration of the ethanol solution of metatitanic acid four fourth fat is 0.6mol/L) in the solution of the dehydrated alcohol of 25ml to form the solution of homogeneous transparent.The ethanol solution of metatitanic acid four fourth fat is being joined in the reactor lentamente.PH value to 4.0 with hydrochloric acid conditioning solution, at room temperature stir 2h, mixture is changed over to in the teflon-lined stainless steel cauldron, leave standstill the aging 24h of the thermostatic drying chamber of putting into 160 ° of C, liquid-solid mixture is taken out with vacuum pump using circulatory water filter, the washing that hockets of the solution of water and ethanol, washing is to neutral, with 60 ° of C thermostatic drying chambers of product inner drying, then roasting 5h under 500 ° of C obtains titania powder.X-ray diffracting spectrum can be fully corresponding with anatase titania standard spectrogram, 8 corresponding anatase octahedrite TiO of diffraction peak difference
2(101), (004), (200), (105), the diffraction peak (JCPDSNo.21-1271) of (116) (200) and (215) crystal face and do not have other impurity peaks, sample belongs to Anatase (Fig. 1 f).Nitrogen adsorption and graph of pore diameter distribution show sample specific surface area are 67.579m
2/ g, pore volume are 0.187cm
3/ g, the aperture is 3.56nm.Utilize the Scherrer formula to calculate particle diameter and be 16.73nm.The Scanning Electron Microscope photos reveal synthetic sample is comprised of the nano particle of assembling.Granular size has tens nanometers.
Embodiment 7:
25ml water and 50ml toluene are added in the beaker, begin simultaneously to stir.Claim 5g metatitanic acid four fourth liposoluble (wherein, the concentration of the ethanol solution of metatitanic acid four fourth fat is 0.6mol/L) in the solution of the dehydrated alcohol of 25ml to form the solution of homogeneous transparent.The ethanol solution of metatitanic acid four fourth fat is being joined in the reactor lentamente.The pH value of solution is 6.0, at room temperature stirs 2h, and mixture is changed over to in the teflon-lined stainless steel cauldron.Leave standstill the aging 24h of the thermostatic drying chamber of putting into 140 ° of C, the liquid-solid mixture taking-up is filtered with vacuum pump using circulatory water, the washing that hockets of the solution of water and ethanol, washing is to neutral, with product at 60 ° of C thermostatic drying chamber inner dryings, then roasting 5h under 500 ° of C of retort furnace obtains titania powder.The Scanning Electron Microscope photos reveal synthetic sample distributes irregular, and particle diameter ratio is larger, and agglomeration is more serious.
Embodiment 8:
25ml water and 50ml toluene are added in the beaker, begin simultaneously to stir.Claim 5g metatitanic acid four fourth liposoluble (wherein, the concentration of the ethanol solution of metatitanic acid four fourth fat is 0.6mol/L) in the solution of the dehydrated alcohol of 25ml to form the solution of homogeneous transparent.The ethanol solution of metatitanic acid four fourth fat is being joined in the reactor lentamente, remaining 4.0 with the pH value of hydrochloric acid conditioning solution, at room temperature stirring 2h, mixture is being changed over to in the teflon-lined stainless steel cauldron.Leave standstill the aging 48h of the thermostatic drying chamber of putting into 140 ° of C, the liquid-solid mixture taking-up is filtered with vacuum pump using circulatory water, the washing that hockets of the solution of water and ethanol, washing is to neutral, with product at 60 ° of C thermostatic drying chamber inner dryings, then roasting 5h under 500 ° of C of retort furnace obtains titania powder.X-ray diffracting spectrum can be fully corresponding with anatase titania standard spectrogram, 8 corresponding anatase octahedrite TiO of diffraction peak difference
2(101), (004), (200), (105), the diffraction peak (JCPDS No.21-1271) of (116) (200) and (215) crystal face and do not have other impurity peaks, sample belongs to Anatase.The Scanning Electron Microscope photos reveal sample is comprised of nanoparticle agglomerates, and particle diameter ratio is larger.
Can find out that from top embodiment the inventive method is simple, need not special equipment, synthesis cycle is short, can make the titanic oxide material of pure anatase crystal, has good photocatalytic activity, can be applied to industrial production.When the volume ratio that changes water and toluene, the difference of aging temperature can obtain different-shape, and table does not amass the poriferous titanium dioxide material that reaches particle diameter on year-on-year basis.
Claims (3)
1. a hydro-thermal surface reaction prepares the method for anatase-phase nano titanium dioxide, it is characterized by may further comprise the steps:
A) with water and toluene according to volume ratio water: the proportioning of toluene=0 ~ 1:1 ~ 2 adds in the reactor, stir under the normal temperature, joining the ethanol solution of metatitanic acid four fourth fat lentamente in the reactor, proportioning is the metatitanic acid four fourth fat that every milliliter of toluene adds 0.1g, keeping the pH value of solution in whole adding procedure is 4.0, obtains mixture;
B) said mixture stirs 2h at normal temperatures, changes the reactor internal reaction over to, leaves standstill and puts into 140
~180
0Aging 24h obtains liquid-solid mixture in the thermostatic drying chamber of C temperature;
C) liquid-solid mixture is taken out rear the filtration, water and ethanol is washing alternately, and washing is arrived neutral, and filtration product at the thermostatic drying chamber inner drying, is obtained the powder of white, and roasting 5h in retort furnace obtains titania powder at last afterwards.
2. hydro-thermal surface reaction as claimed in claim 1 prepares the method for anatase-phase nano titanium dioxide, it is characterized by in the described step a) that to keep pH be that 4.0 method is to wherein dripping hydrochloric acid soln.
3. hydro-thermal surface reaction as claimed in claim 1 prepares the method for anatase-phase nano titanium dioxide, and the concentration of the ethanol solution of metatitanic acid four fourth fat is 0.6 mol/L in the described step a) of its feature.
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| CN113522260A (en) * | 2021-07-27 | 2021-10-22 | 西南化工研究设计院有限公司 | Y molecular sieve coated magnesium oxide-titanium dioxide catalyst and application thereof in ester exchange reaction |
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| CN1526645A (en) * | 2003-09-23 | 2004-09-08 | 翁文剑 | Prepn of nano titania particle |
| CN101070184A (en) * | 2006-05-12 | 2007-11-14 | 中国科学院理化技术研究所 | Method for preparing single dispersing ball-shape mesoporous titanium dioxide colloid particles whose size and apparance are controllable |
| CN101333002A (en) * | 2007-06-27 | 2008-12-31 | 中国科学院合肥物质科学研究院 | Titanium dioxide nanometer powder with special appearance and method for preparing same |
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| CN1526645A (en) * | 2003-09-23 | 2004-09-08 | 翁文剑 | Prepn of nano titania particle |
| CN101070184A (en) * | 2006-05-12 | 2007-11-14 | 中国科学院理化技术研究所 | Method for preparing single dispersing ball-shape mesoporous titanium dioxide colloid particles whose size and apparance are controllable |
| CN101333002A (en) * | 2007-06-27 | 2008-12-31 | 中国科学院合肥物质科学研究院 | Titanium dioxide nanometer powder with special appearance and method for preparing same |
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| CN113522260A (en) * | 2021-07-27 | 2021-10-22 | 西南化工研究设计院有限公司 | Y molecular sieve coated magnesium oxide-titanium dioxide catalyst and application thereof in ester exchange reaction |
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