CN100441512C - Prepn process of nanometer titania ring - Google Patents
Prepn process of nanometer titania ring Download PDFInfo
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- CN100441512C CN100441512C CNB2006101301641A CN200610130164A CN100441512C CN 100441512 C CN100441512 C CN 100441512C CN B2006101301641 A CNB2006101301641 A CN B2006101301641A CN 200610130164 A CN200610130164 A CN 200610130164A CN 100441512 C CN100441512 C CN 100441512C
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Abstract
The present invention discloses preparation process of nanometer TiO2 ring, and features that through emulsion polymerization process to synthesize nanometer polystyrene ball, the subsequent sol-gel process to coat the nanometer polystyrene ball with colloidal TiO2 particle in the thickness of 40-500 nm, and final heat treatment to eliminate nanometer polystyrene ball, nanometer TiO2 ring is prepared. The present invention prepares nanometer polystyrene ball of different diameters as template so as to prepare nanometer TiO2 ring of required size, and the preparation process of nanometer TiO2 ring is simple, low in cost and suitable for large scale production. The said process may be also applied in preparing nanometer ring of ZnO, SnO2, Al2O3 and other oxides.
Description
[technical field]
The present invention relates in chemistry, chemical field, particularly a kind of preparation method of nano material nanometer titania ring.
[background technology]
In recent years, various ring-type nanostructures are subjected to paying close attention to widely because of its unique physics, chemical property and the potential using value in fields such as light, electricity, storages.So far, people have prepared several nano-rings, as ZnO and SnO
2Nano-rings, Au nano-rings, however aspect the nano-rings material preparation, existing technological line requires to use expensive plant and instrument usually, and cost is higher, also also has many technological difficulties to overcome simultaneously.
[summary of the invention]
Purpose of the present invention is intended to for overcoming the deficiencies in the prior art, and provides a kind of based on the preparation method of pipe/polyhenylethylene nano ball as the nanometer titania ring of template.
The present invention addresses the above problem the preparation method that the scheme that is adopted is a kind of nanometer titania ring of design, it is characterized in that with emulsion polymerisation process synthetic polystyrene nanometer ball, the TiO that is 40～500nm at its surface coverage thickness by sol-gel process then
2Colloidal particle is removed the pipe/polyhenylethylene nano ball by thermal treatment again, prepares TiO
2Nano-rings.
Superiority of the present invention is: (1) the present invention is based on pipe/polyhenylethylene nano ball template method and prepares nanometer titania ring, and preparation technology is simple, and cost is low, is easy to scale operation; (2) this method can also further be expanded to preparing and comprise ZnO, SnO
2, Al
2O
3, SiO
2Etc. multiple oxidate nano ring.
[description of drawings]
Fig. 1 is the stereoscan photograph of the polystyrene spheres that forms on the substrate of glass;
Fig. 2 is the stereoscan photograph of nanometer titania ring.
[embodiment]
TiO of the present invention
2The preparation method of nano-rings is made by following steps:
(1) prepare pipe/polyhenylethylene nano ball emulsion with emulsion polymerization: pipe/polyhenylethylene nano ball emulsion is prepared by emulsion polymerisation process in 80 ℃ of waters bath with thermostatic control by monomer styrene, emulsifier sodium lauryl sulfate, buffer reagent sodium bicarbonate, water and initiator potassium persulfate, and the mol ratio of vinylbenzene, sodium lauryl sulphate, sodium bicarbonate, water and Potassium Persulphate is 1: 0.001～0.01: 0.005～0.05: 20～60: 0.005～0.05.In emulsion, the size homogeneous of polystyrene spheres, diameter is between 40～100nm.
(2) adopt sol-gel method to prepare TiO
2Colloidal sol: with butyl (tetra) titanate, dehydrated alcohol and diethanolamine is 1: 2～10: 0.2～0.5 ratio in molar ratio, obtains TiO mix 2～3h under constantly stirring after
2Colloidal sol.
(3) with polystyrene emulsion and TiO
2Colloidal sol is after 1: 0.1～0.5 ratio mixes by volume, and the method that adopts dipping to lift forms polystyrene spheres-TiO in substrate
2After colloidal particle composite membrane, composite membrane dried naturally, the thermal treatment between 400-600 ℃ obtained TiO again
2Nano-rings.TiO
2The internal diameter of nano-rings is between 40～100nm, and external diameter is between 60～140nm.
Principle of work of the present invention is: at first prepare monodispersity pipe/polyhenylethylene nano ball emulsion preferably with emulsion polymerization, then with TiO
2Colloidal sol mixes makes polystyrene spheres surface coverage one deck TiO
2Colloidal particle is removed the pipe/polyhenylethylene nano ball with preparation TiO by thermal treatment again
2Nano-rings.
The invention will be further described in conjunction with the embodiments:
1. the preparation of monodispersed polystyrene spheres: in water bath with thermostatic control, place a there-necked flask, connect electric mixer, condensing works, constant pressure funnel respectively.Measure the 225ml deionized water, add in the there-necked flask, and make the temperature of water bath with thermostatic control be raised to 80 ℃, add emulsifier sodium lauryl sulfate (SDS) and the 0.125g buffer reagent sodium bicarbonate (NaHCO of 0.24g then
3), open mechanical electric mixer, it is mixed, after 10 minutes, add 27.55ml styrene monomer (St) with constant pressure funnel, react after one hour, add initiator potassium persulfate (KPS) 0.125g, polyreaction 18 hours.Fig. 1 is the stereoscan photograph of prepared polystyrene spheres, and as seen from Figure 1, the polystyrene spheres monodispersity is better, size unanimity, the about 80nm of the diameter of ball.
2.TiO
2The preparation of colloidal sol: the metatitanic acid fourth fat of 100ml ethanol and 34ml is put into beaker, stir, in beaker, add the diethanolamine of 11ml then.With pouring in the above-mentioned mixed solution after 55ml ethanol and the mixing of 9ml water, stir 3～5h then again, obtain TiO 2 sol.
3. the preparation of nanometer titania ring: with the polystyrene spheres emulsion and the TiO of above-mentioned preparation
2Colloidal sol is filmed on substrate by the method that dipping lifts after mixing by 2: 1 volume ratio, after drying naturally, obtains TiO at 500 ℃ of calcination 3h again
2The nanometer ring-type.Fig. 2 is the stereoscan photograph of prepared nanometer titania ring, and the internal diameter of prepared nanometer titania ring is consistent with the diameter of polystyrene spheres, is about 80nm, and the external diameter of nano-rings is about 120nm.
Claims (2)
1, a kind of preparation method of nanometer titania ring is characterized in that with emulsion polymerisation process synthetic polystyrene nanometer ball, the TiO that is 40～500nm at its surface coverage thickness by sol-gel process then
2Colloidal particle is removed the pipe/polyhenylethylene nano ball by thermal treatment again, prepares TiO
2Nano-rings.
2, the preparation method of nanometer titania ring according to claim 1 is characterized in that said nanometer titania ring may further comprise the steps to make:
(1) prepare pipe/polyhenylethylene nano ball emulsion with emulsion polymerization: pipe/polyhenylethylene nano ball emulsion is to be prepared by emulsion polymerisation process in 80 ℃ of waters bath with thermostatic control by monomer styrene, emulsifier sodium lauryl sulfate, buffer reagent sodium bicarbonate, water and initiator potassium persulfate; The mol ratio of said vinylbenzene, sodium lauryl sulphate, sodium bicarbonate, water and Potassium Persulphate is 1: 0.001-0.01: 0.005-0.05: 20-60: 0.005-0.05; In emulsion, obtain the polystyrene spheres of diameter at 40-100nm;
(2) adopt sol-gel method to prepare TiO
2Colloidal sol: with butyl (tetra) titanate, dehydrated alcohol and diethanolamine is 1 in molar ratio: the ratio of 2-10: 0.2-0.5 obtains TiO behind the mixing 2-3h under constantly stirring
2Colloidal sol;
(3) TiO that obtains of polystyrene emulsion that step (1) is obtained and step (2)
2Colloidal sol is 1 by volume: after the ratio of 0.1-0.5 mixed, the method that adopts dipping to lift formed polystyrene spheres-TiO in substrate
2The colloidal particle composite membrane; After composite membrane dried naturally, the thermal treatment between 400-600 ℃ obtained TiO again
2Nano-rings.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101301641A CN100441512C (en) | 2006-12-14 | 2006-12-14 | Prepn process of nanometer titania ring |
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| CNB2006101301641A CN100441512C (en) | 2006-12-14 | 2006-12-14 | Prepn process of nanometer titania ring |
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| CN1974404A CN1974404A (en) | 2007-06-06 |
| CN100441512C true CN100441512C (en) | 2008-12-10 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102556952B (en) * | 2012-02-14 | 2015-01-07 | 中国人民解放军国防科学技术大学 | Metal cup-cylinder composite nano structure array and preparation method thereof |
| CN103232172B (en) * | 2013-04-16 | 2016-01-20 | 同济大学 | Big area prepares the method for nano titania hollow ball order thin film |
| CN107029695A (en) * | 2017-05-14 | 2017-08-11 | 陈毅忠 | A kind of biodiesel prepares the preparation method of special solid base catalyst |
| CN111205865A (en) * | 2020-02-17 | 2020-05-29 | 内蒙古工业大学 | Template method for preparing hollow spherical Mn4+Doping with Mg2TiO4Method for producing luminescent material |
| CN111962095B (en) * | 2020-08-13 | 2021-11-05 | 沧州信联化工有限公司 | Green preparation method of tetramethylammonium hydroxide |
| CN111962094B (en) * | 2020-08-13 | 2021-07-30 | 沧州信联化工有限公司 | Electrolysis cell for preparing tetramethyl ammonium hydroxide |
| CN111893505B (en) * | 2020-08-13 | 2021-07-02 | 沧州信联化工有限公司 | Method for preparing tetramethyl ammonium hydroxide by electrolysis |
| CN112030186B (en) * | 2020-08-13 | 2021-08-13 | 沧州信联化工有限公司 | Anode for preparing tetramethyl ammonium hydroxide by electrolysis |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1697132A (en) * | 2004-05-12 | 2005-11-16 | 中国科学院长春光学精密机械与物理研究所 | Method for preparing nano zinc oxide tube by assistance of radiofrequency plasma |
| CN1789115A (en) * | 2005-12-20 | 2006-06-21 | 山东大学 | Method for preparing boron nitride nanometer ring and tube |
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2006
- 2006-12-14 CN CNB2006101301641A patent/CN100441512C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1697132A (en) * | 2004-05-12 | 2005-11-16 | 中国科学院长春光学精密机械与物理研究所 | Method for preparing nano zinc oxide tube by assistance of radiofrequency plasma |
| CN1789115A (en) * | 2005-12-20 | 2006-06-21 | 山东大学 | Method for preparing boron nitride nanometer ring and tube |
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