CN102863021B - 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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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 a kind of hydro-thermal surface reaction and prepare the method for 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, there is both at home and abroad a lot of relevant reports, 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, due to its nanoscale, make nanometer titanic oxide material be easy to same organic polymer or small molecule material and carry out compoundly, by revolving the methods such as way, prepare the devices such as solar cell.Nano-titanium dioxide powder be prepared with many methods, as sol-gel process, coprecipitation method, atomizing thermolysis process etc.But the general particle diameter of the titanium dioxide nano-particle of synthesized is larger, synthetic particle size distribution is wide.On the interface forming at profit, synthesis of titanium dioxide nano-particles size is little, narrow size distribution.
Content of the present invention
The present invention utilizes organic solvent and water to form 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.Between BET result demonstration internal particle, form meso-hole structure.Synthesis device of the present invention is simple, easy to operate, and condition is loose, and raw material is simple and easy to get, and the product simultaneously obtaining 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 the titanium dioxide nano material of not showing on year-on-year basis long-pending porous.
Technical scheme of the present invention is:
Hydro-thermal surface reaction is prepared a method for anatase-phase nano titanium dioxide, comprises the following steps:
A) by water and toluene according to volume ratio water: the proportioning of toluene=0 ~ 1:1 ~ 2 adds in reactor, under normal temperature, stir, the ethanol solution of metatitanic acid four fourth fat is being joined in reactor lentamente, proportioning is the metatitanic acid four fourth fat that every milliliter of toluene adds 0.1g, in whole adding procedure, keeping the pH value of solution is 4.0, obtains mixture;
B) said mixture stirs 2h at normal temperatures, proceeds to reaction in reactor, and the standing aging 24h of thermostatic drying chamber that puts into 140~180 ° of C temperature, obtains liquid-solid mixture;
C) liquid-solid mixture is taken out to rear filtration, water and ethanol is washing alternately, and washing is arrived neutral, and filtration product, at thermostatic drying chamber inner drying, is obtained to white powder, and roasting 5h in retort furnace, finally obtains titania powder afterwards.
In described step a), keeping pH is that 4.0 method is to drip wherein hydrochloric acid soln.
In described step a), the concentration of the ethanol solution of metatitanic acid four fourth fat is 0.6mol/L.
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 advantages of following: preparation process has reaction conditions gentleness, need not specific installation, without any waste liquid, produce, the feature that method is simple, and preparation cycle is short, thereby be easy to realize industrialization.
2. can be by regulating 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 the methylene blue dyestuff of degrading under the irradiation of UV-light), has good industrial application value.
Accompanying drawing explanation
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 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 titanium dioxide and commodity P25 prepared by the present invention degrades in methylene blue process under the irradiation of UV-light, 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 beaker, start to stir simultaneously.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 reactor lentamente, by the pH value of hydrochloric acid conditioning solution, remaining 4.0, at room temperature stirring 2h, mixture is being proceeded to in teflon-lined stainless steel cauldron.The standing aging 24h of thermostatic drying chamber that puts into 140 ° of C, liquid-solid mixture is taken out and filtered with vacuum pump using circulatory water, the washing that hockets of the solution of water and ethanol, washing is to neutral, by 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 completely 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 there is no other impurity peaks, sample belongs to Anatase (Fig. 1).Nitrogen adsorption show sample specific surface area is 93.333m
2/ g, pore volume is 0.191cm
3/ g, aperture is 3.99nm.Utilizing Scherrer formula to calculate particle diameter is 10.99nm.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 beaker, start to stir simultaneously, 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 reactor lentamente.PH value to 4.0 with hydrochloric acid conditioning solution, at room temperature stirs 2h, and mixture is proceeded to in teflon-lined stainless steel cauldron.The standing aging 24h of thermostatic drying chamber that puts into 180 ° of C, liquid-solid mixture is taken out and filtered with vacuum pump using circulatory water, the washing that hockets of the solution of water and ethanol, washing is to neutral, by 60 ° of C thermostatic drying chamber inner dryings of product, then 500 ° of C roastings 5 hours, obtain white titania powder.X-ray diffracting spectrum can be completely 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 there is no 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 is 0.199cm
3/ g, aperture is 4.3nm.Utilizing Scherrer formula to calculate particle diameter is 13.19nm.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, on the interface of oil and water formation, hydrolysis slowly occur and polycondensation forms larger titanium complexing ion polymerization cluster, and because interface is sphere, thereby optimization synthesis condition can form spherical coacervate.
Embodiment 3:
25ml water and 50ml toluene are added in beaker, start to stir simultaneously, 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 reactor lentamente.PH value to 4 with hydrochloric acid conditioning solution, at room temperature stirs 2h, and mixture is proceeded to in teflon-lined stainless steel cauldron.The standing aging 24h of thermostatic drying chamber that puts into 160 ° of C, liquid-solid mixture is taken out and filtered with vacuum pump using circulatory water, the washing that hockets of the solution of water and ethanol, washing is to neutral, by 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 completely 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 there is no 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 is 0.224cm
3/ g, aperture is 3.55nm.Utilizing Scherrer formula to calculate particle diameter is 12.69nm.Scanning Electron Microscope photos reveal synthetic sample is comprised of the nano particle of assembling, the comparison homogeneous of dispersion.
Embodiment 4:
50ml water and 50ml toluene are added in beaker, start to stir simultaneously, 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 reactor lentamente.PH value to 4 with hydrochloric acid conditioning solution, at room temperature stir 2h, mixture is proceeded to in teflon-lined stainless steel cauldron, the standing aging 24h of thermostatic drying chamber that puts into 160 ° of C, for liquid-solid mixture is taken out, vacuum pump using circulatory water filters, the washing that hockets of the solution of water and ethanol, washing is to neutral, by 60 ° of C thermostatic drying chamber inner dryings of product, then, at 500 ° of C roasting 5h, obtain white titania powder.X-ray diffracting spectrum can be completely 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 there is no 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 is 0.162cm
3/ g, aperture is 3.57nm.Utilizing Scherrer formula to calculate particle diameter is 12.67nm.
Embodiment 5:
5ml water and 50ml toluene are added in beaker, start to stir simultaneously, 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 reactor lentamente.PH value to 4 with hydrochloric acid conditioning solution, at room temperature stir 2h, mixture is proceeded to in teflon-lined stainless steel cauldron, the standing aging 24h of thermostatic drying chamber that puts into 160 ° of C, for liquid-solid mixture is taken out, vacuum pump using circulatory water filters, the washing that hockets of the solution of water and ethanol, washing is to neutral, by 60 ° of C thermostatic drying chamber inner dryings of product, then, at 500 ° of C roasting 5h, obtain white titania powder.X-ray diffracting spectrum can be completely 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 there is no 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 is 0.190cm
3/ g, aperture is 3.1nm.Utilizing Scherrer formula to calculate particle diameter is 13.14nm.
Embodiment 6:
0ml water and 50ml toluene are added in beaker, start to stir simultaneously, 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 reactor lentamente.PH value to 4.0 with hydrochloric acid conditioning solution, at room temperature stir 2h, mixture is proceeded to in teflon-lined stainless steel cauldron, the standing aging 24h of thermostatic drying chamber that puts into 160 ° of C, for liquid-solid mixture is taken out, vacuum pump using circulatory water filters, the washing that hockets of the solution of water and ethanol, washing is to neutral, by 60 ° of C thermostatic drying chamber inner dryings of product, then roasting 5h under 500 ° of C, obtains titania powder.X-ray diffracting spectrum can be completely 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 there is no 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 is 0.187cm
3/ g, aperture is 3.56nm.Utilizing Scherrer formula to calculate particle diameter is 16.73nm.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 beaker, start to stir simultaneously.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 reactor lentamente.The pH value of solution is 6.0, at room temperature stirs 2h, and mixture is proceeded to in teflon-lined stainless steel cauldron.The standing aging 24h of thermostatic drying chamber that puts into 140 ° of C, liquid-solid mixture is taken out and filtered with vacuum pump using circulatory water, the washing that hockets of the solution of water and ethanol, washing is to neutral, by product at 60 ° of C thermostatic drying chamber inner dryings, then roasting 5h under 500 ° of C of retort furnace, obtains titania powder.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 beaker, start to stir simultaneously.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 reactor lentamente, by the pH value of hydrochloric acid conditioning solution, remaining 4.0, at room temperature stirring 2h, mixture is being proceeded to in teflon-lined stainless steel cauldron.The standing aging 48h of thermostatic drying chamber that puts into 140 ° of C, liquid-solid mixture is taken out and filtered with vacuum pump using circulatory water, the washing that hockets of the solution of water and ethanol, washing is to neutral, by 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 completely 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 there is no other impurity peaks, sample belongs to Anatase.Scanning Electron Microscope photos reveal sample is comprised of nanoparticle agglomerates, and particle diameter ratio is larger.
From embodiment above, can find out, the inventive method is simple, and without 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 changing the volume ratio of water and toluene, the difference of aging temperature, can obtain different-shape, does not show on year-on-year basis the poriferous titanium dioxide material of long-pending and particle diameter.
Claims (1)
1. hydro-thermal surface reaction is prepared a method for anatase-phase nano titanium dioxide, it is characterized by and comprises the following steps:
A) by water and toluene according to volume ratio water: the proportioning of toluene=0~1:1~2 adds in reactor, under normal temperature, stir, the ethanol solution of metatitanic acid four fourth fat is being joined in reactor lentamente, proportioning is the metatitanic acid four fourth fat that every milliliter of toluene adds 0.1g, in whole adding procedure, keeping the pH value of solution is 4.0, obtains mixture;
B) said mixture stirs 2h at normal temperatures, proceeds to reaction in reactor, and the standing aging 24h of thermostatic drying chamber that puts into 140~180 ℃ of temperature, obtains liquid-solid mixture;
C) liquid-solid mixture is taken out to rear filtration, water and ethanol is washing alternately, and washing is arrived neutral, and filtration product, at thermostatic drying chamber inner drying, is obtained to white powder, and roasting 5h in retort furnace, finally obtains titania powder afterwards;
It is to drip wherein hydrochloric acid soln that described step keeps the method that pH is 4.0 in a);
The described step a) concentration of the ethanol solution of middle metatitanic acid four fourth fat is 0.6mol/L.
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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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