CN102826597A - Method for preparing nanometer titanium dioxide - Google Patents
Method for preparing nanometer titanium dioxide Download PDFInfo
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- CN102826597A CN102826597A CN2012102927982A CN201210292798A CN102826597A CN 102826597 A CN102826597 A CN 102826597A CN 2012102927982 A CN2012102927982 A CN 2012102927982A CN 201210292798 A CN201210292798 A CN 201210292798A CN 102826597 A CN102826597 A CN 102826597A
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- titanium oxide
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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 the photocatalyst material technical field, be specifically related to a kind of low temperature preparation method with nano titanium oxide of anatase crystal.
Background technology
Environmentally friendly photocatalysis technology has characteristics such as less energy-consumption, easy to operate, non-secondary pollution, and is expected to utilize sun power, shows wide application prospect in fields such as organic synthesis, photodissociation water, environmental improvements.Titanium oxide (TiO
2) have photocatalytic activity height, stable performance, non-secondary pollution and characteristics such as cheap and easy to get, be considered to the photocatalyst of tool application prospect.In the photocatalysis technology field, how to improve the quantum yield of light-catalyzed reaction, be to use a main difficult problem that is faced.The optical absorption edge boundary blue shift of the titanium oxide 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; Simultaneously, the surface energy that nano titanium oxide is huge adsorbs reactant from the teeth outwards, also helps the carrying out that reacts.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, control hydrolysis method, sol-gel method, microemulsion method, the precipitator method, chemical Vapor deposition process etc.Wherein sol-gel method is to be raw material with the titanium alkoxide, in organic medium, is hydrolyzed, polycondensation, makes solution behind colloidal sol, gelation process, and gel drying is sintered into the method for powder.The nano titanium oxide particle diameter of this method preparation is little, is evenly distributed good dispersivity.But owing to will be raw material with the titanium alkoxide, add a large amount of organic reagents again, cost is high.And this method directly calcines the precursor that drying obtains, and product is prone to reunite, and has limited the performance of the many excellent properties of product.
Summary of the invention
The present invention provides a kind of simple low temperature preparation technology in order to overcome the deficiency in existing nano titanic oxide sol-preparing gel technology, and the nano titanium oxide size distribution that obtains is even, and good dispersivity has been avoided the reunion between nano-titania particle.
The present invention provides a kind of method for preparing nano titanium oxide, comprises the steps:
A. the volume ratio by titanate and solvent is 1:2～5, preparation titanate solution;
B. gelatin being dissolved in preparation mass percent concentration in 75 ℃～85 ℃ the water is 0.5%～1.5% gelatin solution;
C. by said gelatin solution and titanate liquor capacity than 1:3～5, gelatin solution is added titanate solution, after stirring, with acid-conditioning solution pH value to 2～4, stirring is until obtaining gel;
D. with said gel put 45 ℃～50 ℃ oven drying 4-6 hour, obtain finely dispersed white powder;
E. said white powder is put into water and boil 10～30min, cross the leaching deposition, should precipitate and use water washing, use washing with alcohol then, seasoning in the air obtains nano titanium oxide.
Titanate among the step a is one or more the mixture in butyl(tetra)titanate, titanium propanolate and the titanium ethanolate.
Solvent among the step a is methyl alcohol, ethanol or propyl alcohol
Acid is nitric acid or hydrochloric acid described in the step c.
The number of times of washing with alcohol is 3 times among the step e.
Beneficial effect:
(1) preparation method of the present invention uses gelatin to form one deck organic protective film as tensio-active agent on the nano titanium oxide surface; 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 that obtains is even.
(2) the creative hydrothermal method (using water boil, then washing) of using of preparation method of the present invention is removed the impurity such as gelatin in the dry precursor, and process washing and alcohol are washed and obtained nano-titanium dioxide powder.Only adopt the Air drying process in the method and, do not have high-temperature calcination technology, further avoided the reunion that high-temperature calcination produces between nano-titania particle with the water-heat process that deionized water boils.Prepared nano titanium oxide good dispersivity.
Description of drawings
Fig. 1 is the XRD figure spectrum of the embodiment of the invention 1 gained nano titanium oxide;
Fig. 2 is the transmission electron microscope photo of the embodiment of the invention 1 gained nano titanium oxide.
Embodiment
Below through specific embodiment the preparation process of nano titanium oxide of the present invention is described further, but be not limited thereto.
Embodiment 1
A. be raw material with the butyl(tetra)titanate, ethanol is solvent, the 10ml butyl(tetra)titanate is slowly splashed in the 30ml ethanol preparation butyl(tetra)titanate solution under magnetic stirring apparatus stirs fast;
B. the 1g gelatin being dissolved in 49g, temperature is that to be mixed with mass percent concentration in 85 ℃ the deionized water be 1% gelatin solution;
C. the said gelatin solution of 10ml slowly being added in the 40ml butyl(tetra)titanate solution, after stirring, is that 20% salt slow acid is added dropwise to mixing solutions with mass percent, and regulator solution pH=2.7 stirs fast and loses flowability until solution, obtains light yellow gel;
D. said yellow gel is put 50 ℃ of oven dryings 5 hours, obtain finely dispersed white powder;
E. said white powder is put into deionized water and boil 10min, cross the leaching deposition, with precipitate with deionized water washing 3 times, and then with washing with alcohol 3 times, seasoning in the air (volatilization ethanol) obtains nano titanium oxide.
Adopt X ray powder diffracting technology (XRD) and transmission electron microscope (TEM) crystalline phase to nano titanium oxide, pattern characterizes.Fig. 1 is the XRD figure spectrum of nano titanium oxide, and diffraction peak and JCPDS card number are that the PDF standard diagram of #782486 is consistent, do not detect tangible dephasign peak; And be respectively 25.39 ° at 2 θ, 37.94 °, 48.06 °; 54.36 ° and 54.96 ° peak, with [101] of anatase titania, [004]; [200], [105] and [211] crystal face diffraction peak is corresponding one by one, and interpret sample is an 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 dispersivity has been avoided the reunion between nano-titania particle, and particle size is about 40-70nm, and this result with the XRD figure spectrum estimation is consistent.
The technical scheme that above presentation of results the present invention adopts can successfully obtain even particle size distribution, the nano-titanium dioxide powder of good dispersivity.
Embodiment 2
A. be raw material with the titanium ethanolate, methyl alcohol is solvent, the 10ml titanium ethanolate is slowly splashed in the 50ml ethanol preparation titanium ethanolate solution under magnetic stirring apparatus stirs fast;
B. the 0.25g gelatin being dissolved in 49.75g, temperature is that to be mixed with mass percent concentration in 80 ℃ the deionized water be 0.5% gelatin solution;
C. the said gelatin solution of 20ml slowly being added in the 60ml titanium ethanolate solution, after stirring, is that 20% nitric acid slowly is added dropwise to mixing solutions with mass percent, and regulator solution pH=2.1 stirs fast and loses flowability until solution, obtains light yellow gel;
D. said yellow gel is put 45 ℃ of oven dryings 6 hours, obtain finely dispersed white powder;
E. said white powder is put into deionized water and boil 20min, cross the leaching deposition, with the precipitate with deionized water washing, and then with washing with alcohol 3 times, seasoning in the air (volatilization ethanol) obtains nano titanium oxide.
Adopt X ray powder diffracting technology (XRD) and transmission electron microscope (TEM) crystalline phase to nano titanium oxide, pattern characterizes.The XRD figure spectrum shows that the product that makes is an anatase titanium dioxide.Average grain size is about 65nm.The TEM photo shows that the product granularity that makes is even, and good dispersivity has been avoided the reunion between nano-titania particle, and particle size is about 40-70nm, and this result with the XRD figure spectrum estimation is consistent.
The technical scheme that above presentation of results the present invention adopts can successfully obtain even particle size distribution, the nano-titanium dioxide powder of good dispersivity.
Embodiment 3
A. be raw material with the titanium propanolate, propyl alcohol is a solvent, the 10ml titanium propanolate is slowly splashed in the 20ml ethanol preparation titanium propanolate solution under magnetic stirring apparatus stirs fast;
B. the 0.75g gelatin being dissolved in 49.25g, temperature is that to be mixed with mass percent concentration in 75 ℃ the deionized water be 1.5% gelatin solution;
C. the said gelatin solution of 6ml slowly being added in the 30ml titanium propanolate solution, after stirring, is that 20% salt slow acid is added dropwise to mixing solutions with mass percent, and regulator solution pH=3.8 stirs fast and loses flowability until solution, obtains light yellow gel;
D. said yellow gel is put 50 ℃ of oven dryings 4 hours, obtain finely dispersed white powder;
E. said white powder is put into deionized water and boil 10min, cross the leaching deposition, with the precipitate with deionized water washing, and then with washing with alcohol 3 times, seasoning in the air (volatilization ethanol) obtains nano titanium oxide.
Adopt X ray powder diffracting technology (XRD) and transmission electron microscope (TEM) crystalline phase to nano titanium oxide, pattern characterizes.The XRD figure spectrum shows that the product that makes is an anatase titanium dioxide.Average grain size is about 47nm.The TEM photo shows that the product granularity that makes is even, and good dispersivity has been avoided the reunion between nano-titania particle, and particle size is about 40-70nm, and this result with the XRD figure spectrum estimation is consistent.
The technical scheme that above presentation of results the present invention adopts can successfully obtain even particle size distribution, the nano-titanium dioxide powder of good dispersivity.
Embodiment described in this specification sheets, its prescription, title that technology is named etc. can be different.Everyly conceive equivalence or the simple change that described structure, characteristic and principle are done, include in the protection domain of patent of the present invention according to patent of the present invention.Person of ordinary skill in the field of the present invention can make various modifications or replenishes 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 (5)
1. a method for preparing nano titanium oxide is characterized in that comprising the steps:
A. the volume ratio by titanate and solvent is 1:2～5, preparation titanate solution;
B. gelatin being dissolved in preparation mass percent concentration in 75 ℃～85 ℃ the water is 0.5%～1.5% gelatin solution;
C. by said gelatin solution and titanate liquor capacity than 1:3～5, gelatin solution is added titanate solution, after stirring, with acid-conditioning solution pH value to 2～4, stirring is until obtaining gel;
D. with said gel put 45 ℃～50 ℃ oven drying 4-6 hour, obtain finely dispersed white powder;
E. said white powder is put into water and boil 10～30min, cross the leaching deposition, should precipitate and use water washing, use washing with alcohol then, seasoning in the air obtains nano titanium oxide.
2. according to the said method for preparing nano titanium oxide of claim 1, it is characterized in that titanate among the step a is one or more the mixture in butyl(tetra)titanate, titanium propanolate and the titanium ethanolate.
3. according to the said method for preparing nano titanium oxide of claim 2, it is characterized in that the solvent among the step a is methyl alcohol, ethanol or propyl alcohol.
4. according to the said method for preparing nano titanium oxide of claim 3, it is characterized in that acid described in the step c is nitric acid or hydrochloric acid.
5. according to the said method for preparing nano titanium oxide of claim 4, the number of times that it is characterized in that washing with alcohol among the step e is 3 times.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663548A (en) * | 2013-12-27 | 2014-03-26 | 南京信息工程大学 | Preparation method for anatase titanium dioxide nanocrystalline mesoporous microsphere |
| CN104087995A (en) * | 2014-07-01 | 2014-10-08 | 南京信息工程大学 | Method for preparing titanium dioxide nanometer film |
| CN104612369A (en) * | 2014-12-30 | 2015-05-13 | 南京信息工程大学 | Anti-microbial plastic-wood floor and preparing method thereof |
| CN104944455A (en) * | 2015-06-24 | 2015-09-30 | 南京理工大学 | Sol-gel method for preparing aluminum oxide |
| CN105000596A (en) * | 2015-07-24 | 2015-10-28 | 大族激光科技产业集团股份有限公司 | Method for preparing nano-TiO2 gel |
| CN108821335A (en) * | 2018-08-29 | 2018-11-16 | 佛山市禅城区诺高环保科技有限公司 | A kind of preparation method of high-dispersion nano titanium dioxide |
| CN113896231A (en) * | 2020-07-06 | 2022-01-07 | 宁波极微纳新材料科技有限公司 | Preparation method of titanium dioxide material |
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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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Patent 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 |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663548A (en) * | 2013-12-27 | 2014-03-26 | 南京信息工程大学 | Preparation method for anatase titanium dioxide nanocrystalline mesoporous microsphere |
| CN104087995A (en) * | 2014-07-01 | 2014-10-08 | 南京信息工程大学 | Method for preparing titanium dioxide nanometer film |
| CN104612369A (en) * | 2014-12-30 | 2015-05-13 | 南京信息工程大学 | Anti-microbial plastic-wood floor and preparing method thereof |
| CN104944455A (en) * | 2015-06-24 | 2015-09-30 | 南京理工大学 | Sol-gel method for preparing aluminum oxide |
| CN105000596A (en) * | 2015-07-24 | 2015-10-28 | 大族激光科技产业集团股份有限公司 | Method for preparing nano-TiO2 gel |
| CN108821335A (en) * | 2018-08-29 | 2018-11-16 | 佛山市禅城区诺高环保科技有限公司 | A kind of preparation method of high-dispersion nano titanium dioxide |
| CN113896231A (en) * | 2020-07-06 | 2022-01-07 | 宁波极微纳新材料科技有限公司 | Preparation method of titanium dioxide material |
| 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 |
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