CN102101697A - Rapid preparation method of high-dispersible TiO2 nano crystal sol - Google Patents
Rapid preparation method of high-dispersible TiO2 nano crystal sol Download PDFInfo
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- CN102101697A CN102101697A CN 201110000380 CN201110000380A CN102101697A CN 102101697 A CN102101697 A CN 102101697A CN 201110000380 CN201110000380 CN 201110000380 CN 201110000380 A CN201110000380 A CN 201110000380A CN 102101697 A CN102101697 A CN 102101697A
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Abstract
The invention relates to a rapid preparation method of a high-dispersible TiO2 nano crystal sol, belonging to the technical field of semi-conductor nano crystal preparation. The preparation method is as follows: dissolving inorganic titanium salt serving as a titanium source in a corresponding solvent so that a solution with a certain concentration is prepared; adding alkali liquor to regulate the pH value to 7.5-8.5 and generate a precipitate; washing the precipitate, carrying out complexing reflux dispergation by utilizing H2O2 so as to obtain a peroxotitauium acid sol; and transferring the peroxotitauium acid sol into a hermetic high-temperature kettle of a microwave sampling system, and crystallizing for a while at a certain power and temperature, so that finally, the TiO2 nano crystal sol is prepared. The advantages of solvent heat and microwave methods are integrated in the method provided by the invention, the zeta potential of the obtained sol is between 50 and 70 mV, and the obtained sol has higher dispersibility; and in the preparation process, no surfactant is introduced, high-temperature calcination is not needed, and the obtained sol has a wide application prospect in the field of photocatalysis.
Description
Technical field
The present invention relates to a kind of polymolecularity TiO
2The fast preparation method of nanocrystalline colloidal sol belongs to low temperature and prepares the semiconductor nano material field.This preparation process is simple, quick, and energy consumption is low, the TiO of preparation
2The nanocrystalline colloidal sol good dispersity, the photocatalytic activity height.
Background technology
TiO
2Be a kind of important conductor photocatalysis material, it has higher photocatalytic activity and acid and alkali-resistance and photochemical corrosion, and cost is low, advantages such as nontoxicity, and in purifying air, aspects such as sewage disposal have extensively and potential is used.Common nano-TiO
2The preparation method be divided into vapor phase process and liquid phase method.Wherein vapor phase process is because energy consumption is big, and reasons such as cost height and complex process cause use range less, and the liquid phase rule is because its energy consumption is less, and advantage such as cost is relatively low, and required equipment is comparatively simple has obtained using widely.In the liquid phase method the most frequently used to be hydrolysis method, colloidal sol-coagulate method, chemical precipitation method, methods such as hydrothermal method, these methods mostly need high-temperature calcination to promote its crystallization, cause particle agglomeration serious.And utilize hydro-thermal or solvent thermal to prepare semiconductor nano, can obtain dispersiveness nanocrystalline colloidal sol preferably, but this method needs the time longer.Use at present microwave heating can shorten the preparation time of semiconductor nano greatly, and microwave heating have homogeneous heating, selective, do not have thermograde, cleaning and many reaction systems had the advantages such as effect of quickening chemical reaction.Chinese patent CN1287099A has introduced a kind of microwave heating titanium solution and has prepared nano-TiO
2Method, this method makes its hydrolysis with the microwave heating titanium solution, throw out is through separating, washing, drying, calcining obtains the spheric nano-TiO
2Though the deficiency of this method is that microwave has been accelerated hydrolytic process, the high-temperature calcination of products therefrom ultimate demand is handled to promote its crystallization.Chinese patent CN101054203A has introduced a kind of preparation method of no-agglomeration nano of ceramic, with TiCl
4Be the titanium source,, obtain nano level TiO by microwave heating with mineral acid or inorganic salt dilution
2Emulsion removes water with the carboxylic acid component distillation again and organic acid obtains nano level TiO
2, it is to keep intergranular electrostatic repulsion that this method is used the effect of carboxylic acid, prevents to reunite to improve dispersiveness.Chinese patent CN101468812A then passes through nano-TiO
2Particle and alkali metal compound, organic solvent and tensio-active agent contact, and prepare the TiO of club shaped structure by microwave heating
2Nanocrystalline, but this method need add the dispersiveness that tensio-active agent could improve product.As seen how under cold condition, the semiconductor nanocrystalline sol that obtains polymolecularity is still the problem that is worth research.The present invention adopts the method for microwave-assisted solvent heat, has prepared neutral TiO at low temperature, in the short period of time
2Nanocrystalline colloidal sol, good product dispersibility, narrow diameter distribution, and preparation process need not to add tensio-active agent, and the nanocrystalline colloidal sol of acquisition has embodied good photocatalysis performance.
Summary of the invention
The invention provides a kind of is the titanium source with inorganic titanium salt, and through complexing, backflow and microwave-assisted solvent thermal process prepare TiO
2The process of nanocrystalline colloidal sol.Control particulate size and shape by the conditions such as temperature, reaction times and reaction solvent of regulating microwave-assisted solvent thermal process.The reaction raw materials cost is low, and technology is simple to operation.The product of preparation is the neutral nanocrystalline colloidal sol of high dispersive, can be widely used in photocatalysis field.
The present invention for a kind of be presoma with self-control pertitanic acid colloidal sol, by the neutral TiO of microwave-assisted solvent hot preparation
2The nanocrystalline colloidal sol method, it adopts following technical scheme:
With inorganic titanium salt is the titanium source, is dissolved in coordinative solvent and is configured to certain density solution, adds alkali lye and regulates pH=7.5-8.5, and generate precipitation, with washing of precipitate, with H
2O
2Complexing backflow dispergation obtains pertitanic acid colloidal sol, above-mentioned pertitanic acid colloidal sol is moved in the airtight pyroreaction still of microwave sampling system, and under certain power and temperature, the crystallization certain hour finally makes TiO
2Nanocrystalline colloidal sol.
The inorganic titanium salt that is used for disposing titanium salt solution is a kind of of titanyl sulfate, titanium sulfate; Used solvent is a kind of in deionized water, ethanol, propyl alcohol, the butanols, and perhaps both mix; The inorganic titanium concentration of salt solution of preparation is 0.1～0.4M, and its representative value is 0.1M.
Microwave-assisted solvent thermal crystallisation process is as follows: pertitanic acid colloidal sol is transferred in the airtight pyroreaction still of microwave sampling system, microwave power is 600-1000W; Temperature of reaction is 120～180 ℃; Crystallization time is 15～60 minutes.
TiO with preparation
2Nanocrystalline colloidal sol revolves to steam and obtains powder, in the self-control photocatalysis apparatus of packing into, and the TiO by photocatalytic degradation methylene blue or reactive brilliant red to preparing
2The nano-crystalline photocatalysis performance is investigated.
Advantage of the present invention and effect are:
(1) TiO of the inventive method preparation
2Nanocrystalline colloidal sol has higher dispersiveness, the zeta current potential between 50～70mV, colloidal sol stable homogeneous, crystallization degree height.
(2) the inventive method is preparation TiO
2The technological process of the quick preparation of nanocrystalline colloidal sol was compared with the conventional solvent thermal process, and the time has shortened to tens minutes from tens hours, and the reaction process energy consumption is low, and is simple to operate easy to control.
(3) TiO of the inventive method preparation
2Nanocrystalline colloidal sol is analyzed it by x-ray diffractometer and is pure anatase octahedrite phase, and utilizing electronic lens to observe pattern is bar-shaped, spherical and cube type structure, and size distribution is narrower, between 25-30nm.
(4) the inventive method prepares TiO
2Do not introduce tensio-active agent in the process of nanocrystalline colloidal sol, and the preparation colloidal sol pH be neutrality, help environmental protection, have broad application prospects in fields such as photochemical catalysis.
(5) obtained colloidal sol has higher photocatalytic activity, all can reach more than 90% in 120min the degradation rate of cationic dyestuff methylene blue and anionic dyestuff reactive brilliant red.
Description of drawings
Fig. 1 is the colloidal sol sample of 160 ℃ of following microwave hydrothermal 30min preparations.
Fig. 2 is the TEM figure that 160 ℃ of following microwave hydrothermal 30min prepare colloidal sol.
Fig. 3 is the XRD figure that 160 ℃ of following microwave hydrothermal 30min prepare colloidal sol.
Embodiment
The present invention is described in detail below in conjunction with embodiment:
Embodiment one:Concrete steps are as follows:
A. dispose the Ti (SO of 0.1M
4)
2The aqueous solution.
B. the pH value that adds the ammoniacal liquor regulator solution is 7.5-8.5, and generates precipitation, with washing of precipitate, with H
2O
2Complexing backflow dispergation obtains pertitanic acid colloidal sol.
C. above-mentioned pertitanic acid colloidal sol is moved in the airtight pyroreaction still of microwave sampling system, under the temperature of 800W power and 160 ℃, crystallization 30min makes TiO
2Nanocrystalline colloidal sol
D. carry out the catalyzed degradation methylene blue with homemade photocatalysis apparatus.
Embodiment two:Present embodiment and embodiment one are basic identical, and different is: used solvent is an ethanol.
Embodiment three:Present embodiment and embodiment one are basic identical, and different is: used solvent is a propyl alcohol.
Embodiment four:Present embodiment and embodiment one are basic identical, and different is: used solvent is a butanols.
Embodiment five:Present embodiment and embodiment one are basic identical, and different is: used solvent is a water: ethanol=1:1.
According to Fig. 1,2, colloidal sol does not have coagulation as can be seen, can stable existence, and the dispersing property in water is fine.XRD figure by Fig. 3 as can be known, the colloidal sol that makes is pure anatase octahedrite phase colloidal sol, and the crystallinity of colloidal sol is better.
Claims (3)
1. polymolecularity TiO
2The fast preparation method of nanocrystalline colloidal sol is characterized in that this method has following process:
With inorganic titanium salt is the titanium source, is dissolved in coordinative solvent and is configured to certain density solution, adds alkali lye and regulates pH=7.5～8.5, and generate precipitation, with washing of precipitate, with H
2O
2Complexing backflow dispergation obtains pertitanic acid colloidal sol, above-mentioned pertitanic acid colloidal sol is moved in the airtight pyroreaction still of microwave sampling system, and under certain power and temperature, the crystallization certain hour finally makes TiO
2Nanocrystalline colloidal sol.
2. as right 1 described polymolecularity TiO
2The fast preparation method of nanocrystalline colloidal sol, the inorganic titanium salt that it is characterized in that being used for disposing titanium salt solution is a kind of of titanyl sulfate, titanium sulfate; Used solvent is a kind of in deionized water, ethanol, propyl alcohol, the butanols, and perhaps both mix; The inorganic titanium concentration of salt solution of preparation is 0.1～0.4M, and its representative value is 0.1M.
3. as right 1 described polymolecularity TiO
2The fast preparation method of nanocrystalline colloidal sol is characterized in that, microwave power is 600～1000W; Temperature of reaction is 120～180 ℃; Crystallization time is 15～60 minutes.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584219A (en) * | 2012-02-22 | 2012-07-18 | 上海大学 | Method for quickly compounding barium titanate nano-powder |
| CN104338522A (en) * | 2013-08-01 | 2015-02-11 | 京程科技股份有限公司 | Preparing method of titanium dioxide sol photocatalyst and applications of the titanium dioxide sol photocatalyst in decontamination and self-cleaning |
| CN104594534A (en) * | 2014-12-24 | 2015-05-06 | 南京倍立达新材料系统工程股份有限公司 | Nanometer photocatalysis GRC curtain wall plate product and production method of nanometer photocatalysis GRC curtain wall plate product |
| CN106185832A (en) * | 2016-06-30 | 2016-12-07 | 攀枝花学院 | A kind of stably-doped peroxo titanic acid sol and preparation method thereof |
| CN107913693A (en) * | 2017-11-23 | 2018-04-17 | 中国科学院福建物质结构研究所 | The oxygen-enriched state titanium oxide in surface and preparation method for high-activity treatment of textile dye waste |
| CN108675343A (en) * | 2018-04-28 | 2018-10-19 | 西安前沿材料研究院有限公司 | Metallic oxide nanocrystal unitary and multiple elements design aqueous sol or powder low-temperature synthetic method |
| CN108927125A (en) * | 2018-08-06 | 2018-12-04 | 攀枝花学院 | The method for preparing photocatalysis nano titania slurry as raw material using positive metatitanic acid |
| CN109336172A (en) * | 2018-10-30 | 2019-02-15 | 攀枝花学院 | The method for preparing photocatalysis nano-titanium dioxide as raw material using metatitanic acid |
| CN109364961A (en) * | 2018-11-21 | 2019-02-22 | 黄冈师范学院 | A kind of Ag3PO4/TiO2Composite photo-catalyst and its microwave synthesis method |
| CN110292918A (en) * | 2019-07-10 | 2019-10-01 | 西北师范大学 | A kind of preparation and application of oxygen defect titanium dioxide/Palygorskite Composite Materials |
| CN111170282A (en) * | 2020-01-07 | 2020-05-19 | 北京科技大学 | Preparation method of inorganic peroxotitanic acid dispersant |
| CN111484072A (en) * | 2020-04-23 | 2020-08-04 | 河北工业大学 | Method for preparing titanate or titanium-based composite oxide material by low-temperature crystalline phase conversion |
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| CN2568626Y (en) * | 2002-08-22 | 2003-08-27 | 西北有色金属研究院 | Appts. for prepn. of anatase type nano titania sol |
| CN101559979A (en) * | 2009-05-22 | 2009-10-21 | 东华大学 | Method for preparing extrafine anatase titanium dioxide nano rods |
| CN101597084A (en) * | 2009-07-03 | 2009-12-09 | 东华大学 | The method of synthesizing anatase phase titanium dioxide nanometer particle by microreactor |
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2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN2568626Y (en) * | 2002-08-22 | 2003-08-27 | 西北有色金属研究院 | Appts. for prepn. of anatase type nano titania sol |
| CN101559979A (en) * | 2009-05-22 | 2009-10-21 | 东华大学 | Method for preparing extrafine anatase titanium dioxide nano rods |
| CN101597084A (en) * | 2009-07-03 | 2009-12-09 | 东华大学 | The method of synthesizing anatase phase titanium dioxide nanometer particle by microreactor |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584219A (en) * | 2012-02-22 | 2012-07-18 | 上海大学 | Method for quickly compounding barium titanate nano-powder |
| CN104338522A (en) * | 2013-08-01 | 2015-02-11 | 京程科技股份有限公司 | Preparing method of titanium dioxide sol photocatalyst and applications of the titanium dioxide sol photocatalyst in decontamination and self-cleaning |
| CN104594534A (en) * | 2014-12-24 | 2015-05-06 | 南京倍立达新材料系统工程股份有限公司 | Nanometer photocatalysis GRC curtain wall plate product and production method of nanometer photocatalysis GRC curtain wall plate product |
| CN106185832A (en) * | 2016-06-30 | 2016-12-07 | 攀枝花学院 | A kind of stably-doped peroxo titanic acid sol and preparation method thereof |
| CN107913693A (en) * | 2017-11-23 | 2018-04-17 | 中国科学院福建物质结构研究所 | The oxygen-enriched state titanium oxide in surface and preparation method for high-activity treatment of textile dye waste |
| CN108675343A (en) * | 2018-04-28 | 2018-10-19 | 西安前沿材料研究院有限公司 | Metallic oxide nanocrystal unitary and multiple elements design aqueous sol or powder low-temperature synthetic method |
| CN108927125A (en) * | 2018-08-06 | 2018-12-04 | 攀枝花学院 | The method for preparing photocatalysis nano titania slurry as raw material using positive metatitanic acid |
| CN109336172A (en) * | 2018-10-30 | 2019-02-15 | 攀枝花学院 | The method for preparing photocatalysis nano-titanium dioxide as raw material using metatitanic acid |
| CN109364961A (en) * | 2018-11-21 | 2019-02-22 | 黄冈师范学院 | A kind of Ag3PO4/TiO2Composite photo-catalyst and its microwave synthesis method |
| CN109364961B (en) * | 2018-11-21 | 2021-12-03 | 黄冈师范学院 | Ag3PO4/TiO2Composite photocatalyst and microwave synthesis method thereof |
| CN110292918A (en) * | 2019-07-10 | 2019-10-01 | 西北师范大学 | A kind of preparation and application of oxygen defect titanium dioxide/Palygorskite Composite Materials |
| CN111170282A (en) * | 2020-01-07 | 2020-05-19 | 北京科技大学 | Preparation method of inorganic peroxotitanic acid dispersant |
| CN111484072A (en) * | 2020-04-23 | 2020-08-04 | 河北工业大学 | Method for preparing titanate or titanium-based composite oxide material by low-temperature crystalline phase conversion |
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Application publication date: 20110622 |