CN102826597B - Method for preparing nanometer titanium dioxide - Google Patents
Method for preparing nanometer titanium dioxide Download PDFInfo
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- CN102826597B CN102826597B CN201210292798.2A CN201210292798A CN102826597B CN 102826597 B CN102826597 B CN 102826597B CN 201210292798 A CN201210292798 A CN 201210292798A CN 102826597 B CN102826597 B CN 102826597B
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Abstract
The invention provides a method for preparing nanometer titanium dioxide, and belongs to the technical field of photocatalysis materials. The method comprises the following steps: preparing a titanate solution, and a gelatin solution with a mass percent concentration of 0.5%-1.5%, adding the gelatin solution into the titanate solution, stirring to obtain gel, drying the gel to obtain uniformly-distributed white powder, boiling, washing with water, washing with ethanol, and naturally drying in the air to obtain the nanometer titanium dioxide. The invention overcomes the deficiencies in current nanometer titanium dioxide sol-gel preparation technology, and provides a simple low-temperature preparation technology; the obtained nanometer titanium dioxide has uniform particle size distribution, and good dispersibility; the method of the invention prevents the nanometer titanium dioxide particles from agglomeration.
Description
Technical field
The invention belongs to photocatalyst material technical field, be specifically related to a kind of low temperature preparation method with the nano titanium oxide of anatase crystal.
Background technology
Environmentally friendly photocatalysis technology has the features such as less energy-consumption, easy to operate, non-secondary pollution, and is expected to utilize sun power, in fields such as organic synthesis, photodissociation water, environmental improvements, shows wide application prospect.Titanium dioxide (TiO
2) have that photocatalytic activity is high, stable performance, non-secondary pollution and the feature such as cheap and easy to get, be considered to the photocatalyst of tool application prospect.In photocatalysis technology field, how to improve the quantum yield of light-catalyzed reaction, be the main bugbear that application faces.The optical absorption edge band border blue shift of the titanium dioxide of nanoscale, has higher Eo+; The nano-crystalline titanium dioxide that particle diameter is little can reduce the compound of light induced electron and photohole effectively, makes more electronics and cavity energy participate in oxidation-reduction reaction; Meanwhile, the surface that nano titanium oxide is huge can by reactant absorption from the teeth outwards, also be conducive to the carrying out of reaction.Therefore, the great interest of nano titanium dioxide photocatalyst preparation work person in recent years.
At present, the preparation method of relevant nano titanium oxide mainly contains: hydrothermal synthesis method, controlled hydrolysis method, sol-gel method, microemulsion method, the precipitator method, chemical Vapor deposition process etc.Wherein sol-gel method is to take titanium alkoxide as raw material, is hydrolyzed, polycondensation in organic medium, makes solution after colloidal sol, gelation process, and gel drying is sintered into the method for powder.The standby nano titanium oxide particle diameter of this legal system is little, is evenly distributed, and good dispersity.But owing to will take titanium alkoxide as raw material, add again a large amount of organic reagents, cost is high.And this method directly calcines the dry precursor obtaining, product is easily reunited, and has limited the performance of the many excellent properties of product.
Summary of the invention
The present invention, in order to overcome the deficiency in existing nano titanic oxide sol-gel technology of preparing, provides a kind of simple low temperature preparation technology, and the nano titanium oxide size distribution obtaining is even, and good dispersity has been avoided the reunion between nano-titania particle.
The invention provides a kind of method of preparing nano titanium oxide, comprise the steps:
A. by the volume ratio of titanate and solvent, be 1:2～5, preparation titanate solution;
B. gelatin is dissolved in in the water of 75 ℃～85 ℃, to prepare mass percent concentration be 0.5%～1.5% gelatin solution;
C. by described gelatin solution with titanate liquor capacity than 1:3～5, gelatin solution is added to titanate solution, after stirring, with acid-conditioning solution pH value to 2～4, stirring is until obtain gel;
D. described gel is put to 45 ℃～50 ℃ oven drying 4-6 hour, obtained finely dispersed white powder;
E. described white powder is put into water and boil 10～30min, cross leaching precipitation, this precipitation is washed with water, then use washing with alcohol, seasoning in air, obtains nano titanium oxide.
Titanate in step a is one or more the mixture in butyl (tetra) titanate, titanium propanolate and titanium ethanolate.
Solvent in step a is methyl alcohol, ethanol or propyl alcohol
Described in step c, acid is nitric acid or hydrochloric acid.
In step e, the number of times of washing with alcohol is 3 times.
beneficial effect:
(1) preparation method of the present invention uses gelatin on nano titanium oxide surface, to form one deck organic protective film as tensio-active agent; the hypertrophy that has suppressed nano titanium oxide crystal grain; hinder being in contact with one another between nanoparticle simultaneously, alleviated the reunion between nano-titania particle.The titanium dioxide nanoparticle size distribution obtaining is even.
(2) the creative hydrothermal method (with water boil, then washing) of using of preparation method of the present invention is removed the impurity such as gelatin in dry precursor, through washing and alcohol wash, obtains nano-titanium dioxide powder.The water-heat process that only adopts Air drying process and boil with deionized water in method, does not have high-temperature calcination technique, has further avoided the reunion that between nano-titania particle, high-temperature calcination produces.Prepared nano titanium oxide good dispersity.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the embodiment of the present invention 1 gained nano titanium oxide;
Fig. 2 is the transmission electron microscope photo of the embodiment of the present invention 1 gained nano titanium oxide.
Embodiment
By specific embodiment, further describe below the preparation process of nano titanium oxide of the present invention, but be not limited to this.
Embodiment 1
A. take butyl (tetra) titanate as raw material, ethanol is solvent, 10ml butyl (tetra) titanate is slowly splashed under magnetic stirring apparatus rapid stirring in 30ml ethanol to preparation butyl (tetra) titanate solution;
B. 1g gelatin is dissolved in to 49g, temperature and is that in the deionized water of 85 ℃, to be mixed with mass percent concentration be 1% gelatin solution;
C. gelatin solution described in 10ml is slowly added in 40ml butyl (tetra) titanate solution, after stirring, the salt slow acid that is 20% by mass percent is added dropwise to mixing solutions, regulator solution pH=2.7, and rapid stirring, until solution loses flowability, obtains light yellow gel;
D. described yellow gel is put to 50 ℃ of oven dryings 5 hours, obtain finely dispersed white powder;
E. described white powder is put into deionized water and boil 10min, cross leaching precipitation, by precipitate with deionized water washing 3 times, and then by washing with alcohol 3 times, seasoning in air (volatilization ethanol), obtains nano titanium oxide.
Adopt X ray powder diffracting technology (XRD) and the crystalline phase of transmission electron microscope (TEM) to nano titanium oxide, pattern characterizes.Fig. 1 is the XRD figure spectrum of nano titanium oxide, the PDF standard diagram that diffraction peak is #782486 with JCPDS card number is consistent, obvious dephasign peak do not detected, and is respectively 25.39 ° at 2 θ, 37.94 °, 48.06 °, the peak of 54.36 ° and 54.96 °, with [101] of anatase titania, [004], [200], [105] and [211] crystal face diffraction peak is corresponding one by one, and interpret sample is anatase titanium dioxide.According to the peak width of 5 diffraction peaks, the average grain size with Scherrer formula estimation sample, is about 57nm.Fig. 2 is the TEM photo of nano titanium oxide, its epigranular, and good dispersity, has avoided the reunion between nano-titania particle, and particle size is about 40-70nm, and this is consistent with the result of XRD figure spectrum estimation.
These results suggest that the technical solution used in the present invention can successfully obtain even particle size distribution, the nano-titanium dioxide powder of good dispersity.
Embodiment 2
A. take titanium ethanolate as raw material, methyl alcohol is solvent, 10ml titanium ethanolate is slowly splashed under magnetic stirring apparatus rapid stirring in 50ml ethanol to preparation titanium ethanolate solution;
B. 0.25g gelatin is dissolved in to 49.75g, temperature and is that in the deionized water of 80 ℃, to be mixed with mass percent concentration be 0.5% gelatin solution;
C. gelatin solution described in 20ml is slowly added in 60ml titanium ethanolate solution, after stirring, the nitric acid that is 20% by mass percent is slowly added dropwise to mixing solutions, regulator solution pH=2.1, and rapid stirring, until solution loses flowability, obtains light yellow gel;
D. described yellow gel is put to 45 ℃ of oven dryings 6 hours, obtain finely dispersed white powder;
E. described white powder is put into deionized water and boil 20min, cross leaching precipitation, by precipitate with deionized water washing, and then by washing with alcohol 3 times, seasoning in air (volatilization ethanol), obtains nano titanium oxide.
Adopt X ray powder diffracting technology (XRD) and the crystalline phase of transmission electron microscope (TEM) to nano titanium oxide, pattern characterizes.The demonstration of XRD figure spectrum, the product making is anatase titanium dioxide.Average grain size is about 65nm.The demonstration of TEM photo, the product granularity making is even, and good dispersity has been avoided the reunion between nano-titania particle, and particle size is about 40-70nm, and this is consistent with the result of XRD figure spectrum estimation.
These results suggest that the technical solution used in the present invention can successfully obtain even particle size distribution, the nano-titanium dioxide powder of good dispersity.
Embodiment 3
A. take titanium propanolate as raw material, propyl alcohol is solvent, 10ml titanium propanolate is slowly splashed under magnetic stirring apparatus rapid stirring in 20ml ethanol to preparation titanium propanolate solution;
B. 0.75g gelatin is dissolved in to 49.25g, temperature and is that in the deionized water of 75 ℃, to be mixed with mass percent concentration be 1.5% gelatin solution;
C. gelatin solution described in 6ml is slowly added in 30ml titanium propanolate solution, after stirring, the salt slow acid that is 20% by mass percent is added dropwise to mixing solutions, regulator solution pH=3.8, and rapid stirring, until solution loses flowability, obtains light yellow gel;
D. described yellow gel is put to 50 ℃ of oven dryings 4 hours, obtain finely dispersed white powder;
E. described white powder is put into deionized water and boil 10min, cross leaching precipitation, by precipitate with deionized water washing, and then by washing with alcohol 3 times, seasoning in air (volatilization ethanol), obtains nano titanium oxide.
Adopt X ray powder diffracting technology (XRD) and the crystalline phase of transmission electron microscope (TEM) to nano titanium oxide, pattern characterizes.The demonstration of XRD figure spectrum, the product making is anatase titanium dioxide.Average grain size is about 47nm.The demonstration of TEM photo, the product granularity making is even, and good dispersity has been avoided the reunion between nano-titania particle, and particle size is about 40-70nm, and this is consistent with the result of XRD figure spectrum estimation.
These results suggest that the technical solution used in the present invention can successfully obtain even particle size distribution, the nano-titanium dioxide powder of good dispersity.
Embodiment described in this specification sheets, its formula, title that technique is named etc. can be different.Every equivalence or simple change of doing according to described structure, feature and the principle of patent design of the present invention, is included in the protection domain of patent of the present invention.Those skilled in the art can make various modifications or supplement or adopt similar mode to substitute described embodiment; only otherwise depart from structure of the present invention or surmount the defined scope of this claim, all belong to protection scope of the present invention.
Claims (4)
1. a method of preparing nano titanium oxide, is characterized in that comprising the steps:
A. by one or more mixture and the solvent in butyl (tetra) titanate, titanium propanolate and titanium ethanolate, be 1:2～5 by volume, obtain solution;
B. gelatin is dissolved in in the water of 75 ℃～85 ℃, to prepare mass percent concentration be 0.5%～1.5% gelatin solution;
C. by described gelatin solution with liquor capacity described in step a than 1:3～5, gelatin solution is added to solution described in step a, after stirring, with acid-conditioning solution pH value to 2～4, stirring is until obtain gel;
D. described gel is put to 45 ℃～50 ℃ oven drying 4-6 hour, obtained finely dispersed white powder;
E. described white powder is put into water and boil 10～30min, cross leaching precipitation, this precipitation is washed with water, then use washing with alcohol, seasoning in air, obtains nano titanium oxide.
2. prepare according to claim 1 the method for nano titanium oxide, it is characterized in that the solvent in step a is methyl alcohol, ethanol or propyl alcohol.
3. prepare according to claim 2 the method for nano titanium oxide, it is characterized in that acid described in step c is for nitric acid or hydrochloric acid.
4. prepare according to claim 3 the method for nano titanium oxide, the number of times that it is characterized in that washing with alcohol in step e is 3 times.
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| CN103663548B (en) * | 2013-12-27 | 2015-07-22 | 南京信息工程大学 | Preparation method for anatase titanium dioxide nanocrystalline mesoporous microsphere |
| CN104087995B (en) * | 2014-07-01 | 2016-08-31 | 南京信息工程大学 | A kind of preparation method of titanium dioxide nano-film |
| CN104612369B (en) * | 2014-12-30 | 2017-05-03 | 南京信息工程大学 | Preparing method of anti-microbial plastic-wood floor |
| CN104944455A (en) * | 2015-06-24 | 2015-09-30 | 南京理工大学 | Sol-gel method for preparing aluminum oxide |
| CN105000596B (en) * | 2015-07-24 | 2017-03-22 | 大族激光科技产业集团股份有限公司 | Method for preparing nano-TiO2 gel |
| CN108821335B (en) * | 2018-08-29 | 2020-11-06 | 单潇 | Preparation method of high-dispersion nano titanium dioxide |
| CN113896231B (en) * | 2020-07-06 | 2023-09-29 | 宁波极微纳新材料科技有限公司 | Preparation method of titanium dioxide material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1962458A (en) * | 2005-11-10 | 2007-05-16 | 中国科学院电工研究所 | Method for preparing anatase-like titanium dioxide nanometer powder |
| CN101007651A (en) * | 2006-12-20 | 2007-08-01 | 中国科学院山西煤炭化学研究所 | Synthesis method of nanometer anatase titania under room temperature |
| US20110253012A1 (en) * | 2009-01-06 | 2011-10-20 | Chongqing Kechang Technology Co., Ltd. | Titania composite and preparing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962458A (en) * | 2005-11-10 | 2007-05-16 | 中国科学院电工研究所 | Method for preparing anatase-like titanium dioxide nanometer powder |
| CN101007651A (en) * | 2006-12-20 | 2007-08-01 | 中国科学院山西煤炭化学研究所 | Synthesis method of nanometer anatase titania under room temperature |
| US20110253012A1 (en) * | 2009-01-06 | 2011-10-20 | Chongqing Kechang Technology Co., Ltd. | Titania composite and preparing method thereof |
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