CN101920991A - Method for preparing nanometer titanium dioxide - Google Patents
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- CN101920991A CN101920991A CN 201010250196 CN201010250196A CN101920991A CN 101920991 A CN101920991 A CN 101920991A CN 201010250196 CN201010250196 CN 201010250196 CN 201010250196 A CN201010250196 A CN 201010250196A CN 101920991 A CN101920991 A CN 101920991A
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Abstract
The invention discloses a method for preparing nanometer titanium dioxide with excellent photochemical catalytic activity by taking technical grade titanium acetylacetonate as titanium source, belonging to the technical filed of nanometer titanium dioxide preparation. The method comprises the following steps: hydrolyzing the titanium acetylacetonate under the hydrothermal condition to prepare nanometer amorphous titanium dioxide; and calcining the nanometer amorphous titanium dioxide in a muffle furnace so as to enable the nanometer amorphous titanium dioxide to convert into an anatase type. The photocatalytic degradation dye experiment proves that the prepared titanium dioxide has excellent photochemical catalytic activity. The invention has simple and convenient process and low cost, and is easy to carry out production in large scale.
Description
Technical field
The present invention relates to a kind of is the method that the titanium source prepares nano titanium oxide with the technical grade titanium acetylacetone, and especially a kind of preparation technology is simple, with low cost, product have the good light catalytic activity the preparation method of nano titanium oxide.
Background technology
As a kind of green, stable, semiconductor light-catalyst efficiently, titanium dioxide is widely used in the processing and the organic degraded of inorganic wastewater.In three kinds of crystal formations of titanium dioxide, Detitanium-ore-type becomes the main selection that people prepare photocatalyst because of its excellent photoelectric performance, and simple preparation technology, clean the manufacturing raw material of nontoxic non-secondary pollution, be applicable to the equipment requirements of scale operation, become the major objective that the optically catalytic TiO 2 preparation producers are pursued.The titanium source that is used to prepare nano titanium oxide at present mainly is a butyl (tetra) titanate, titanium tetrachloride, and titanyl sulfate etc., synthetic method mainly is sol-gel and hydrothermal method etc.In the US5330953 patent, be the titanium source with the titanyl sulfate, hydro-thermal has been synthesized anatase-type nanometer titanium dioxide.People such as Sugimoto (Colloid Interface Sci.2003,259 (1): 53-61.) utilize the method for sol-gel, the kind through changing the amine that is added and regulate the nano titanium oxide that the pH value is prepared the different-shape size.People such as Jun (J.Am.Chem.Soc., 2003,125:15981-15985.) utilize non-hydrolytic sol-gelation process, prepare the spherical of favorable dispersity and rod-like nano titanium dioxide by the surfactivity selective agent.People such as Ding (J.Am.Chem.Soc., 2007, be that presoma microwave method in ionic liquid synthesizes high-quality anatase-type nanometer titanium dioxide with the titanium isopropoxide 129:6362-6363.).
Titanium acetylacetone is the inner complex of a kind of titanium and methyl ethyl diketone, is mainly used in the properties-correcting agent of products such as coating, printing ink, varnish; Curing catalyst, surface treatment agent, tackifier etc.Up to now, still finding no the people uses titanium acetylacetone to prepare nano titanium oxide as the titanium source.The titanium acetylacetone chemical property is relatively stable, and is cheap, and toxicity is low, and it is simple to prepare the nano titanium oxide method with it as the titanium source, and the products obtained therefrom photocatalytic activity is good, is expected to large-scale industrial production.
Summary of the invention
The object of the invention provides a kind of method of using new technical grade titanium source to synthesize the nano titanium oxide with good light catalytic activity.
The present invention realizes by following steps:
(1) titanium acetylacetone is dissolved in the dehydrated alcohol, add concentrated hydrochloric acid, the volume ratio of titanium acetylacetone and dehydrated alcohol is 1: 8～1: 12, the volume ratio of titanium acetylacetone and concentrated hydrochloric acid is 3: 1～5: 1, and magnetic agitation mixes reaction solution, and the reaction solution of yellow transparent is poured in the water heating kettle, obtain unbodied titanium dioxide powder after the hydro-thermal reaction, clean product with dehydrated alcohol, centrifugal, oven dry.
(2) the amorphous nano titanium oxide with gained places the retort furnace roasting.
(3) temperature of hydro-thermal reaction is at least 120 ℃ among the present invention, and the reaction times is more than the 10h.
(4) maturing temperature is 300～600 ℃ among the present invention, and roasting time is more than the 3h.
(5) the prepared nano-titanium dioxide powder of the present invention is a Detitanium-ore-type, and crystallization is complete, and diameter of particle is less than 50nm, pattern rule, favorable dispersity.
(6) utilize X-ray diffractometer (XRD), scanning electronic microscope (SEM), transmission electron microscope (TEM), full-automatic physical and chemical adsorption analyser (BET) isothermal adsorption pattern to survey specific surface area product is carried out the appearance structure analysis, with rhodamine B solution is that the target dyestuff carries out the photocatalytic degradation experiment, measure absorbancy by ultraviolet-visible spectrophotometer, to assess its photocatalytic activity.
Description of drawings
Fig. 1 is the XRD diffraction spectrogram of prepared nano titanium oxide, and diffraction peak is the anatase titanium dioxide characteristic diffraction peak among the figure.
Fig. 2 is the stereoscan photograph of prepared nano titanium oxide.
Fig. 3 is the transmission electron microscope photo of prepared nano titanium oxide.
Fig. 4 be under the different maturing temperatures nano titanium dioxide photocatalysis degraded rhodamine B solution time-the degradation rate graph of a relation.
1、500℃ 2、600℃ 3、400℃ 4、300℃
The preparation of embodiment 1 nano titanium oxide
Add 2mL titanium acetylacetone and 0.6mL concentrated hydrochloric acid in the 20mL dehydrated alcohol, magnetic agitation changes reaction solution in the 25mL water heating kettle over to after the question response thing mixes, and 120 ℃, 10h.
Products therefrom is cleaned with dehydrated alcohol, centrifugal, 60 ℃ of oven dry in the thermostatic drying chamber.
The amorphous nano titanium oxide of oven dry is put into the retort furnace roasting, and temperature is respectively 300,400,500,600 ℃.
The phenetic analysis of resulting nano titanium oxide under the embodiment 2 different maturing temperatures
As shown in Figure 1, resulting nano titanium oxide all presents the characteristic diffraction peak of anatase titanium dioxide under the different maturing temperatures, does not have impurity, and crystallization is complete.
Following table is the specific surface area of nano titanium oxide prepared under the different maturing temperatures and the product particle mean size data of calculating gained by the XRD figure spectrum.
The photocatalytic activity of resulting nano titanium oxide experiment under the embodiment 3 different maturing temperatures
(1) compound concentration is the rhodamine B solution of 10 μ g/L, and the solution for preparing is placed the dark place.
(2) take by weighing titanium dioxide 0.1g under the differing temps roasting, place photo catalysis reactor respectively, add the target degradation solution that 100mL step (1) is prepared, after magnetic agitation 30min treats that titanium dioxide is uniformly dispersed, open the water source, light source carries out the photocatalytic degradation experiment.
(3) every 30min draws the photocatalytic degradation liquid in the reactor, is used for the measurement of ultraviolet-visible absorbancy after centrifugal.
(4) prepared as seen from Figure 4 nano titanium oxide has excellent photocatalysis activity, and especially maturing temperature is that 500 ℃ sample rhodamine B solution degradation rate behind catalyzed reaction 60min surpasses 60%, and the eventual degradation rate reaches 100%.
Claims (4)
1. method for preparing nano titanium oxide, it is characterized in that: be the titanium source with the titanium acetylacetone, dehydrated alcohol is a solvent, and concentrated hydrochloric acid is a hydrolytic accelerating agent, hydro-thermal reaction makes the hydrolysis of titanium source under the normal pressure, and after reaction finished, alcohol was washed, centrifugal, oven dry will obtain nano titanium oxide after the products therefrom roasting.
2. the method for preparing nano titanium oxide as claimed in claim 1, it is characterized in that: concrete steps are as follows:
(1) titanium acetylacetone is dissolved in the dehydrated alcohol, add concentrated hydrochloric acid, the volume ratio of titanium acetylacetone and dehydrated alcohol is 1: 8～1: 12, and the volume ratio of titanium acetylacetone and concentrated hydrochloric acid is 3: 1～5: 1, magnetic agitation mixes reaction solution, the reaction solution of yellow transparent poured into carry out hydro-thermal reaction in the water heating kettle, the temperature of hydro-thermal reaction is at least 120 ℃, and the reaction times is more than the 10h, obtain unbodied titanium dioxide powder after the hydro-thermal reaction, clean product with dehydrated alcohol, centrifugal, oven dry;
(2) with the amorphous nano titanium oxide roasting of gained, maturing temperature is 300～600 ℃, and roasting time is more than the 3h.
3. nano titanium oxide preparation method as claimed in claim 1 or 2 is characterized in that: the mass percentage concentration of concentrated hydrochloric acid is 37%.
4. nano titanium oxide preparation method as claimed in claim 1 or 2 is characterized in that: the bake out temperature of amorphous titania powder is lower than 70 ℃.
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| CN2010102501961A CN101920991B (en) | 2010-08-10 | 2010-08-10 | Method for preparing nanometer titanium dioxide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491414A (en) * | 2011-11-30 | 2012-06-13 | 姚敏 | Preparation method of titanium dioxide (TiO2) photocatalyst |
| CN103628052A (en) * | 2013-09-04 | 2014-03-12 | 杭州电子科技大学 | Preparation method of titanium dioxide thin film coating on surface of titanium alloy microporous bone |
| CN105905940A (en) * | 2016-04-12 | 2016-08-31 | 渤海大学 | Preparation method of nickel titanate/titanium dioxide composite nanomaterial |
| CN109647418A (en) * | 2018-12-19 | 2019-04-19 | 陕西科技大学 | A kind of preparation method of foamed nickel supported samarium doping titania photocatalyst |
| CN113562804A (en) * | 2021-08-25 | 2021-10-29 | 上海交通大学 | Method for degrading herbicide by visible light |
| CN114054047A (en) * | 2021-11-26 | 2022-02-18 | 江苏科技大学 | Preparation method of titanium dioxide-copper sulfide heterojunction photocatalyst |
| CN116573669A (en) * | 2023-05-04 | 2023-08-11 | 江苏第二师范学院 | Preparation method and application of amorphous titanium dioxide electrochemical nitrate radical reduction catalyst |
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| JPH11269414A (en) * | 1998-03-25 | 1999-10-05 | Central Glass Co Ltd | Photocatalytic membrane-forming ink and method for forming photocatalytic membrane |
| CN101033080A (en) * | 2007-02-26 | 2007-09-12 | 清华大学 | Method of preparing TiO2 nano-tube array |
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2010
- 2010-08-10 CN CN2010102501961A patent/CN101920991B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11269414A (en) * | 1998-03-25 | 1999-10-05 | Central Glass Co Ltd | Photocatalytic membrane-forming ink and method for forming photocatalytic membrane |
| CN101033080A (en) * | 2007-02-26 | 2007-09-12 | 清华大学 | Method of preparing TiO2 nano-tube array |
Non-Patent Citations (2)
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| 《J. Phys. Chem.》 20080524 Liming Shen et al. Hydrothermal Splitting of Titanate Fibers to Single-Crystalline TiO2 Nanostructures with Controllable Crystalline Phase, Morphology, Microstructure, and Photocatalytic Activity pp.8809-8818 1-4 第112卷, 第24期 2 * |
| 《中国博士学位论文全文数据库 工程科技I辑》 20061115 方晓明 TiCl4液相水解制备纳米TiO2粉体的研究 第74页第5.2节 1-4 , 第11期 2 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491414A (en) * | 2011-11-30 | 2012-06-13 | 姚敏 | Preparation method of titanium dioxide (TiO2) photocatalyst |
| CN102491414B (en) * | 2011-11-30 | 2014-03-26 | 西北大学 | Preparation method of titanium dioxide (TiO2) photocatalyst |
| CN103628052A (en) * | 2013-09-04 | 2014-03-12 | 杭州电子科技大学 | Preparation method of titanium dioxide thin film coating on surface of titanium alloy microporous bone |
| CN103628052B (en) * | 2013-09-04 | 2016-01-20 | 杭州电子科技大学 | A kind of preparation method of titanium alloy micropore bone surface titanium deoxid film coating |
| CN105905940A (en) * | 2016-04-12 | 2016-08-31 | 渤海大学 | Preparation method of nickel titanate/titanium dioxide composite nanomaterial |
| CN105905940B (en) * | 2016-04-12 | 2017-03-29 | 渤海大学 | A kind of preparation method of nickel titanate/titanium dioxide composite nano material |
| CN109647418A (en) * | 2018-12-19 | 2019-04-19 | 陕西科技大学 | A kind of preparation method of foamed nickel supported samarium doping titania photocatalyst |
| CN113562804A (en) * | 2021-08-25 | 2021-10-29 | 上海交通大学 | Method for degrading herbicide by visible light |
| CN114054047A (en) * | 2021-11-26 | 2022-02-18 | 江苏科技大学 | Preparation method of titanium dioxide-copper sulfide heterojunction photocatalyst |
| CN116573669A (en) * | 2023-05-04 | 2023-08-11 | 江苏第二师范学院 | Preparation method and application of amorphous titanium dioxide electrochemical nitrate radical reduction catalyst |
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| CN101920991B (en) | 2012-05-23 |
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Inventor after: Chen Min Inventor after: Li Di Inventor after: Wu Wen Inventor after: Jiang Deli Inventor after: Xie Jimin Inventor after: Zhu Jianjun Inventor after: Lv Xiaomeng Inventor after: Huang Chunxia Inventor before: Chen Min Inventor before: Li Di Inventor before: Jiang Deli Inventor before: Xie Jimin Inventor before: Zhu Jianjun Inventor before: Lv Xiaomeng Inventor before: Huang Chunxia |
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Free format text: CORRECT: INVENTOR; FROM: CHEN MIN LI DI JIANG DELI XIE JIMIN ZHU JIANJUN LV XIAOMENG HUANG CHUNXIA TO: CHEN MIN LI DI WU WEN JIANG DELI XIE JIMIN ZHU JIANJUN LV XIAOMENG HUANG CHUNXIA |
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