CN110054222A - It is a kind of to prepare mesoporous single crystals TiO2The method of nanoparticle - Google Patents
It is a kind of to prepare mesoporous single crystals TiO2The method of nanoparticle Download PDFInfo
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- CN110054222A CN110054222A CN201910497186.9A CN201910497186A CN110054222A CN 110054222 A CN110054222 A CN 110054222A CN 201910497186 A CN201910497186 A CN 201910497186A CN 110054222 A CN110054222 A CN 110054222A
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- 239000013078 crystal Substances 0.000 title claims abstract description 32
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 23
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 22
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 18
- 150000007524 organic acids Chemical class 0.000 claims abstract description 15
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 12
- 239000012498 ultrapure water Substances 0.000 claims abstract description 12
- 238000000151 deposition Methods 0.000 claims abstract description 11
- 230000008021 deposition Effects 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 10
- 238000005119 centrifugation Methods 0.000 claims abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 9
- 239000010935 stainless steel Substances 0.000 claims abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 21
- 230000007062 hydrolysis Effects 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 5
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- KBIWNQVZKHSHTI-UHFFFAOYSA-N 4-n,4-n-dimethylbenzene-1,4-diamine;oxalic acid Chemical compound OC(=O)C(O)=O.CN(C)C1=CC=C(N)C=C1 KBIWNQVZKHSHTI-UHFFFAOYSA-N 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Natural products OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N Propionic acid Chemical compound CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 abstract description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 11
- 239000000463 material Substances 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000527 sonication Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 230000010148 water-pollination Effects 0.000 description 2
- -1 Butyl titanate Chemical compound 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000013265 porous functional material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
Mesoporous single crystals TiO is prepared the invention discloses a kind of2The method of nanoparticle, butyl titanate is added drop-wise in organic acid by this method dropwise, ultrapure water is then added and hydrofluoric acid causes butyl titanate prehydrolysis, and mixture is stirred at room temperature, then mixture is transferred in stainless steel autoclave, and reaction kettle is put into baking oven cooling after heat preservation a period of time, after reaction kettle is cooled to room temperature, centrifuge washing is carried out to mixture and obtains white depositions, sonicated and use dehydrated alcohol and water washing are for several times, it is finally collected by centrifugation up to the nanoparticle, the present invention has the advantages that method is simple, it is low in cost, by controlling reaction condition, the mesoporous single crystals TiO of different-shape can be obtained2Nanoparticle.
Description
Technical field
The application belongs to photochemical catalyzing field, and in particular to a kind of to prepare mesoporous single crystals TiO2The side of nanoparticle
Method, the method in the application is simple, low in cost, and by controlling reaction condition, the mesoporous single crystals of different-shape can be obtained
TiO2Nanoparticle.
Background technique
It is well known that global industry rapid development and economy are fast after World War II and the industrial revolution
Sagitar flies, and pollution situation caused by industrial pollution and the discharge of " three wastes " but can not be ignored, the demand to clean reproducible energy
And increase increasingly；With the fast development of scientific and technological level, photocatalysis achieved in terms of solving energy demand it is huge into
Exhibition, especially reaps in abundant in photocatalysis Decomposition aquatic products hydrogen field；Under simulated solar irradiation or UV-visible radiation, urging
Water can be decomposed under the action of agent generates hydrogen；Therefore, so far, more and more researchs concentrate on novel nano photochemical catalyst
Selection and preparation on, with preferably be applied to photocatalysis Decomposition aquatic products hydrogen field.
Mesoporous material is the porous functional material that a kind of pore size belongs to mesoporous scope, and pore size distribution is uniformly and the ruler in aperture
Very little accurately to regulate and control, specific surface area is higher, and pore volume is larger；Titanium dioxide (TiO2) it is in basic research and industrial application
It is excellent to be primarily due to its physical and chemical performance for one of most important inorganic material, and this cost is needed in practice
Low, nontoxic, the features such as property is stable and physical and chemical performance is excellent；The crystallization of monocrystal material is perfect, is conducive to charge
Quickly transmission, therefore all shows excellent performance in many application fields, especially in the conversion of the energy such as solar battery and
The fields such as field of storage and photocatalysis and lithium ion battery；Mesoporous single crystals material is a kind of unique functional material, is had good
Good mesoporosity and high mono-crystalline structures, show excellent performance in various applications.
In recent years, it is continually striving to due to scientific research personnel, there has also been remarkable progress for the research of mesoporous single crystals material；Lin etc.1
The mesoporous anatase TiO with mesoporous single crystals characteristic is successfully prepared by hydro-thermal method2, imitated in dye-sensitized solar cells
Rate may be up to 8.7%；2013, Crossland etc.2It is put forward for the first time with SiO2For hard template and to be successfully prepared anatase mesoporous
Monocrystalline TiO2, with preferable electric conductivity, electron mobility is very fast, therefore shows in low temp fuel sensitization solar battery
Excellent photoelectric conversion performance out；HF acid can reduce the surface energy of (001) crystal face, thus have good crystal face adjustment effect；
However, simple under the action of HF, Wang etc.3Fail the monocrystalline TiO that preparation has mesoporous characteristic2；Wherein:
1.Lin,J.；Zhao,L.；Heo,Y.-U.；Wang,L.；Bijarbooneh,F.H.；Mozer,A.J.；
Nattestad,A.；Yamauchi,Y.；Dou,S.X.；Kim,J.H.Nano Energy 2015,11,557-567.
2.Crossland,E.J.；Noel,N.；Sivaram,V.；Leijtens,T.；Alexander-Webber,
J.A.；Snaith,H.J.Nature 2013,495,(7440),215-9.
3.Wang,Y.；Zhang,H.；Han,Y.；Liu,P.；Yao,X.；Zhao,H.Chemical
communications 2011,47,(10),2829-31.
The present invention using organic acid as solvent and pore creating material, by chemical method on nanoscale accurately controllable preparation pattern
Controllably, size adjustable, the nanoscale mesoporous single crystals TiO that dispersibility is high and hydrophily is strong2Material is expected in wider emerging neck
Domain plays a significant role, such as photocatalysis and lithium ion battery field.
Summary of the invention
For overcome the deficiencies in the prior art, the purpose of the present invention, which is intended to provide, a kind of prepares mesoporous single crystals TiO2Nanoparticle
The method of son；The method of the present invention is simple, low in cost, and by controlling reaction condition, different-shape mesoporous single crystals can be obtained
TiO2Nanoparticle.
For achieving the above object, the present invention adopts the following technical scheme that:
It is a kind of to prepare mesoporous single crystals TiO2Butyl titanate is added drop-wise to organic acid by the method for nanoparticle, this method dropwise
In, ultrapure water is then added and hydrofluoric acid causes butyl titanate prehydrolysis, and mixture is stirred at room temperature, then will mix
It closes object to be transferred in stainless steel autoclave, and reaction kettle is put into baking oven cooling after heat preservation a period of time, to reaction kettle
After being cooled to room temperature, centrifuge washing is carried out to mixture and obtains white depositions, it is sonicated and using dehydrated alcohol and
Water washing for several times, is finally collected by centrifugation up to the nanoparticle.The present invention, which provides, a kind of prepares mesoporous single crystals TiO2Nanoparticle
The method of son, the specific steps are as follows:
(a) butyl titanate of 1-10mL is added drop-wise in the organic acid of 10-50mL dropwise, ultrapure water and 0- is then added
10% hydrofluoric acid causes the hydrolysis of butyl titanate；
(b) mixture is then transferred to not by mixture at room temperature with faster speed magnetic agitation 5-20 minutes
In rust steel autoclave, and autoclave is put into 100-200 DEG C of baking oven, is kept for 6-24 hours；
(c) it is cooled to room temperature to autoclave temperature, mixture described in centrifuge washing obtains white depositions, will be upper
It is sonicated to state white depositions, and for several times using dehydrated alcohol and water washing, finally by being collected by centrifugation, collecting product is
Mesoporous single crystals TiO can be obtained2Nanoparticle.
It is preferred that wherein in the hydrolytic process of step (a), the volume of organic acid, the volume of ultrapure water, the quality of hydrofluoric acid
The ratio of score three is x:y:z, wherein 10≤x≤50；0<y≤2；0≤z≤1.
It is preferred that the organic acid in formic acid, acetic acid, methyl acetic acid or ethanedioic acid any one.
It is preferred that wherein in step (c) during being collected by centrifugation, centrifugal rotational speed is that 3000-14000 turns/min, when centrifugation
Between be 1-10 minutes.
It is preferred that wherein the magnetic agitation rotating speed in step (a) is that 800-1400 turns/min.
Compared with the prior art, the present invention has the following advantages: experimental implementation is simple, can obtain different-shape and size and
The mesoporous single crystals TiO of good dispersion2Nanoparticle finally shows excellent photochemical catalyzing H2-producing capacity.
Detailed description of the invention
Fig. 1 is elliposoidal mesoporous single crystals TiO prepared by the embodiment of the present invention 12The X ray diffracting spectrum of nanoparticle；
Fig. 2 is elliposoidal mesoporous single crystals TiO prepared by the embodiment of the present invention 12The TEM of nanoparticle schemes；
Fig. 3 is cube shaped mesoporous single crystals TiO prepared by the embodiment of the present invention 62The TEM of nanoparticle schemes.
Specific embodiment
The present invention is described further With reference to embodiment.
Embodiment 1:
Firstly, the butyl titanate of 1mL is added drop-wise to dropwise in the organic acid of 10mL, the ultrapure water of 0.5mL is then added
Hydrofluoric acid with 1.5% causes the hydrolysis of butyl titanate.Mixture is stirred at room temperature with the magnetic force of 1200 turns/min of revolving speed
It mixes 15 minutes, transfers it in stainless steel autoclave, be then put into autoclave in 150 DEG C of baking oven,
It is kept for 12 hours.It is cooled to room temperature to autoclave temperature, centrifuge washing obtains white depositions, dehydrated alcohol and water ultrasound
Processing washing is finally that 14000 turns/min is centrifuged 10 minutes by revolving speed, collecting product can be obtained mesoporous single crystals TiO for several times2
Nanoparticle, major axis dimension are~110nm, and minor axis dimension is~50nm, are prepared as shown in Figure 1 for the embodiment of the present invention 1
Elliposoidal mesoporous single crystals TiO2The X ray diffracting spectrum of nanoparticle；Fig. 2 is that elliposoidal prepared by the embodiment of the present invention 1 is mesoporous
Monocrystalline TiO2The TEM of nanoparticle schemes.
Embodiment 2:
Firstly, the butyl titanate of 1mL is added drop-wise to dropwise in the organic acid of 15mL, the ultrapure water of 0.75mL is then added
Hydrofluoric acid with 1.5% causes the hydrolysis of butyl titanate.Mixture is stirred at room temperature with the magnetic force of 1200 turns/min of revolving speed
It mixes 15 minutes, transfers it in stainless steel autoclave, be then put into autoclave in 150 DEG C of baking oven,
It is kept for 12 hours.It is cooled to room temperature to autoclave temperature, centrifuge washing obtains white depositions, dehydrated alcohol and water ultrasound
Processing washing is finally that 14000 turns/min is centrifuged 10 minutes by revolving speed, collecting product can be obtained the mesoporous of elliposoidal for several times
Monocrystalline TiO2Nanoparticle, major axis dimension are~240nm, and minor axis dimension is~95nm.
Embodiment 3:
Firstly, the butyl titanate of 1mL is added drop-wise to dropwise in the organic acid of 15mL, the ultrapure water of 0.75mL is then added
Cause the hydrolysis of butyl titanate.By mixture at room temperature with faster speed magnetic agitation 15 minutes, then shifted
Into stainless steel autoclave, then autoclave is put into 150 DEG C of baking oven, is kept for 12 hours.To reaction under high pressure
Kettle temperature degree is cooled to room temperature, and centrifuge washing obtains white depositions, and dehydrated alcohol and the washing of water ultrasonic treatment for several times, are finally passed through
Revolving speed is that 14000 turns/min is centrifuged 10 minutes, and collecting product can be obtained mesoporous single crystals TiO2Nanoparticle, major axis dimension are
~258nm, minor axis dimension are~122nm.
Embodiment 4:
Firstly, the butyl titanate of 1mL is added drop-wise to dropwise in the organic acid of 15mL, the ultrapure water of 0.8mL is then added
Hydrofluoric acid with 2.5% causes the hydrolysis of butyl titanate.Mixture is stirred at room temperature with the magnetic force of 1300 turns/min of revolving speed
It mixes 15 minutes, transfers it in stainless steel autoclave, be then put into autoclave in 150 DEG C of baking oven,
It is kept for 16 hours.It is cooled to room temperature to autoclave temperature, centrifuge washing obtains white depositions, super with dehydrated alcohol and water
Sonication is washed for several times, is finally that 14000 turns/min is centrifuged 10 minutes by revolving speed, collecting product can be obtained mesoporous single crystals
TiO2Nanoparticle, major axis dimension are~35nm, and minor axis dimension is~16nm.
Embodiment 5:
Firstly, the butyl titanate of 1mL is added drop-wise to dropwise in the organic acid of 25mL, the ultrapure water of 1.8mL is then added
Hydrofluoric acid with 2.5% causes the hydrolysis of butyl titanate.Mixture is stirred at room temperature with the magnetic force of 1400 turns/min of revolving speed
It mixes 15 minutes, transfers it in stainless steel autoclave, be then put into autoclave in 150 DEG C of baking oven,
It is kept for 12 hours.It is cooled to room temperature to autoclave temperature, centrifuge washing obtains white depositions, super with dehydrated alcohol and water
Sonication is washed for several times, is finally that 14000 turns/min is centrifuged 10 minutes by revolving speed, collecting product can be obtained mesoporous single crystals
TiO2Nanoparticle, major axis dimension are~266nm, and minor axis dimension is~100nm.
Embodiment 6:
Firstly, the butyl titanate of 1mL is added drop-wise to dropwise in the organic acid of 15mL, the ultrapure water of 0.8mL is then added
2% hydrofluoric acid solution of sum causes the hydrolysis of butyl titanate.By mixture at room temperature with the magnetic of 1100 turns/min of revolving speed
Power stirs 15 minutes, transfers it in stainless steel autoclave, then autoclave is put into 150 DEG C of baking oven
In, it is kept for 12 hours.It is cooled to room temperature to autoclave temperature, centrifuge washing obtains white depositions, dehydrated alcohol and water
It is ultrasonically treated washing for several times, is finally that 14000 turns/min is centrifuged 10 minutes by revolving speed, collection product can be obtained cube shaped
Mesoporous single crystals TiO2Nanoparticle, having a size of~240nm；It is illustrated in figure 3 the cube shaped of the preparation of the embodiment of the present invention 6
Mesoporous single crystals TiO2The TEM of nanoparticle schemes.
Compared with prior art, the positive effect of the present invention is: the application by chemical method on nanoscale accurately
Controllable preparation morphology controllable, size adjustable, the nanoscale mesoporous single crystals TiO that dispersibility is high and hydrophily is strong2Material is expected to more
Extensive emerging field plays a significant role, such as photocatalysis and lithium ion battery field；The method of the present invention is simple, at low cost
It is honest and clean, by controlling reaction condition, different-shape mesoporous single crystals TiO can be obtained2Nanoparticle.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in type of the present invention
Protection scope within.
The preferred technical solution of the present invention is only embodied in summary, and those skilled in the art is to some of them part institute
The some variations that may be made embody the principle of the present invention, all should be technology scope of the invention.
Claims (5)
1. a kind of prepare mesoporous single crystals TiO2The method of nanoparticle, which is characterized in that specific step is as follows:
(a) butyl titanate of 1-10mL is added drop-wise in the organic acid of 10-50mL dropwise, ultrapure water and 0-10% is then added
Hydrofluoric acid cause butyl titanate hydrolysis；
(b) mixture is then transferred to stainless steel at room temperature with faster speed magnetic agitation 5-20 minutes by mixture
In autoclave, and autoclave is put into 100-200 DEG C of baking oven, is kept for 6-24 hours；
(c) it is cooled to room temperature to autoclave temperature, mixture described in centrifuge washing obtains white depositions, will be above-mentioned white
Color sediment is sonicated, and for several times using dehydrated alcohol and water washing, and finally by being collected by centrifugation, collecting product can be obtained
To mesoporous single crystals TiO2Nanoparticle.
2. according to the method described in claim 1, it is characterized by: wherein in the hydrolytic process of step (a), the body of organic acid
The ratio of product, the volume of ultrapure water, the volume fraction three of hydrofluoric acid is x:y:z, wherein 10≤x≤50；0<y≤2；0≤z≤1.
3. according to the method described in claim 1, it is characterized by: the organic acid be selected from formic acid, acetic acid, methyl acetic acid or
Any one in ethanedioic acid.
4. according to the method described in claim 1, it is characterized by: centrifugation turns wherein in step (c) during being collected by centrifugation
Speed is that 3000-14000 turns/min, and centrifugation time is 1-10 minutes.
5. according to the method described in claim 1, it is characterized by: wherein the magnetic agitation rotating speed in step (a) is 800-
1400 turns/min.
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