CN101073769A - Method for producing nano-titanic oxide light catalyst by steam hydrolysis - Google Patents
Method for producing nano-titanic oxide light catalyst by steam hydrolysis Download PDFInfo
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- CN101073769A CN101073769A CN 200710011845 CN200710011845A CN101073769A CN 101073769 A CN101073769 A CN 101073769A CN 200710011845 CN200710011845 CN 200710011845 CN 200710011845 A CN200710011845 A CN 200710011845A CN 101073769 A CN101073769 A CN 101073769A
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- titanic oxide
- light catalyst
- tio
- oxide light
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Abstract
The invention is concerned with a vapour hydrolysis to prepare nano-TiO_2 photocatalyst, relating using TiCl4 to prepare nano-TiO2 particle in ethanol solution. Take certain amount of TiCl4, Low-carbon-ester and dispersant to three neck flask in turn, heat up and reflux with air having some amount of water vapour. React for 0.5 to 4 h and get the production mixture. Mix the production enough and take centrifugation to get wide production, after washing some times and removing chlorine ion and get out. Dry at about 100 degree and put it into muffle furnace to heat for 2 to 6 h and get nano-TiO2 powder. It takes new technology with easy production process and short periods, and the ethanol can be reused. It reduces the cost and the production has good photocatalytic capability.
Description
Technical field
The present invention relates to a kind of preparation nano-TiO
2Method, particularly relate to the method for a kind of direct hydrolysis method preparation than the high light catalytic active titanium oxide.
Background technology
Nano-TiO
2Be a kind of novel inorganic functional material, have particular performances such as specific area is big, surface-active is high, absorbing properties is good, be widely used in fields such as fine ceramics raw material, catalyst, sensor, semiconductor, high-grade automobile finish and cosmetics; Simultaneously, nano-TiO
2Have suitable energy gap, bigger surface area, stronger oxidation-reduction quality and nontoxic, low cost and other advantages are widely used as the catalyst of light-catalyzed reaction.Therefore, nano-TiO
2Become a synthetic research focus of ultrafine inorganic powder in recent years
[1]
At present, preparation nano-TiO
2Method kinds more than ten such as sol-gal process, sluggish precipitation, micro emulsion method and hydro-thermal method are arranged.In the preparation method of various titanium dioxide nanocrystalline photochemical catalysts, sol-gel process is widely adopted.This method has the equipment less investment, synthesis temperature is low and multiple advantage such as easy controlled doping.Adopt this method to prepare TiO
2Nano particle is normally with Ti (OR)
4Be raw material, by control Ti (OR)
4Hydrolysis speed obtain suitable presoma, and then roasting obtains nano-TiO at a certain temperature
2Because Ti (OR)
4At normal temperatures hydrolysis can take place rapidly, in order to make Ti (OR)
4Hydrolysis carry out with suitable speed, common way is at first with Ti (OR)
4Mix the solution that obtains debita spissitudo and pH value with absolute ethyl alcohol equal solvent and appropriate amount of acid, then water is mixed the alcohol solution that obtains suitable acidity with absolute ethyl alcohol equal solvent and appropriate amount of acid, again the latter is added drop-wise among the former with proper speed, obtain making it be transformed into gel again behind the colloidal sol, again with gel drying, roasting gets TiO at last
2Nano-powder.Make and prepare nano-TiO in this way
2Exist cycle long (generally at least 4～5 days), alcohols equal solvent to be difficult to shortcomings such as recovery, contaminated environment, production cost height.
Summary of the invention
The object of the present invention is to provide a kind of nano titanium oxide preparation method, it is stock that this method is selected titanium tetrachloride for use, and lower alcohol is a solvent, adds certain dispersant, adopts Hydrolyze method, is prepared into the titanium dioxide with photocatalytic activity.
The objective of the invention is to be achieved through the following technical solutions:
The method of producing nano-titanic oxide light catalyst by steam hydrolysis, this method comprises the steps:
A. in having the reaction unit that stirs that refluxes, take by weighing a certain amount of titanium tetrachloride, lower alcohol and dispersant in proportion and drop into successively in the there-necked flask, add hot reflux, contain the air of suitable quantity of water steam simultaneously in feeding, react 0.5～4h at a certain temperature, obtain product mixture.
B. the above-mentioned product mixture that makes is dipped in the ethanolic solution, it is fully mixed, isolate thick product through high speed centrifugation, repeatedly washing behind the removal chlorion, is taken out.
C. the above-mentioned thick product that makes is placed in the baking oven, baking is done down about 100 ℃, makes solvent evaporates, and gained titanium dioxide is put into muffle furnace roasting 2～6h and promptly got nano-TiO
2Powder.
The method of aforesaid producing nano-titanic oxide light catalyst by steam hydrolysis, described lower alcohol comprises methyl alcohol, ethanol, propyl alcohol, n-butanol and isopropyl alcohol.
The method of aforesaid producing nano-titanic oxide light catalyst by steam hydrolysis, its described reaction temperature is: 50～100 ℃.
The method of aforesaid producing nano-titanic oxide light catalyst by steam hydrolysis, its described sintering temperature is: 300～700 ℃.。
Advantage of the present invention and effect are:
The present invention has studied first and has directly utilized TiCl
4Hydrolysis prepares TiO in ethanolic solution
2The new technology of nano particle has been investigated the gained nano-TiO
2The performance that is used for catalytic degradation dyestuff under the UV-irradiation.Experimental result shows, adopts this technology, and production process is simple, and the cycle is short, and ethanol can be realized recycling, and has reduced the pollution of environment.Reduce nano-TiO
2Production cost, the photocatalysis performance of products obtained therefrom is good.
The specific embodiment
Embodiment 1
The steam hydrolysis legal system is equipped with nano-TiO
2The preparation of photochemical catalyst: have in the reaction unit that stirs that refluxes, in there-necked flask, add titanium tetrachloride, ethanol, dispersant successively by certain raw material proportioning, ratio is 1: 3: 0.05, add hot reflux, contain the air of suitable quantity of water steam simultaneously in feeding, react 2h at a certain temperature, then with reactant mixture, separating, is solvent clean with alcohol, drying; Promptly get nano-TiO in 300 ℃ of following roasting 3h of uniform temperature behind the porphyrize
2Powder.
The said goods is carried out the photocatalysis performance test.This experiment is a tester with the ZBF dyestuff.Measurement result, the removal efficient in 60 minutes is 97.2%.
Embodiment 2
The steam hydrolysis legal system is equipped with nano-TiO
2The preparation of photochemical catalyst: have in the reaction unit that stirs that refluxes, in there-necked flask, add titanium tetrachloride, ethanol, dispersant successively by certain raw material proportioning, ratio is 1: 4: 0.05, add hot reflux, contain the air of suitable quantity of water steam simultaneously in feeding, react 2h at a certain temperature, then with reactant mixture, separating, is solvent clean with alcohol, drying; Promptly get nano-TiO in 300 ℃ of following roasting 3h of uniform temperature behind the porphyrize
2Powder.
The said goods is carried out the photocatalysis performance test.This experiment is a tester with the ZBF dyestuff.Measurement result, the removal efficient in 60 minutes is 96.7%.
Embodiment 3
The steam hydrolysis legal system is equipped with nano-TiO
2The preparation of photochemical catalyst: have in the reaction unit that stirs that refluxes, in there-necked flask, add titanium tetrachloride, ethanol, dispersant successively by certain raw material proportioning, ratio is 1: 3: 0.05, add hot reflux, contain the air of suitable quantity of water steam simultaneously in feeding, react 2h at a certain temperature, then with reactant mixture, separating, is solvent clean with alcohol, drying; Promptly get nano-TiO in 400 ℃ of following roasting 3h of uniform temperature behind the porphyrize
2Powder.
The said goods is carried out the photocatalysis performance test.This experiment is a tester with the ZBF dyestuff.Measurement result, the removal efficient in 60 minutes is 97.7%.
Embodiment 4
The steam hydrolysis legal system is equipped with nano-TiO
2The preparation of photochemical catalyst: have in the reaction unit that stirs that refluxes, in there-necked flask, add titanium tetrachloride, ethanol, dispersant successively by certain raw material proportioning, ratio is 1: 3: 0.05, add hot reflux, contain the air of suitable quantity of water steam simultaneously in feeding, react 2h at a certain temperature, then with reactant mixture, separating, is solvent clean with alcohol, drying; Promptly get nano-TiO in 500 ℃ of following roasting 3h of uniform temperature behind the porphyrize
2Powder.
The said goods is carried out the photocatalysis performance test.This experiment is a tester with the ZBF dyestuff.Measurement result, the removal efficient in 60 minutes is 98.7%.
Embodiment 5
The steam hydrolysis legal system is equipped with nano-TiO
2The preparation of photochemical catalyst: have in the reaction unit that stirs that refluxes, in there-necked flask, add titanium tetrachloride, ethanol, dispersant successively by certain raw material proportioning, ratio is 1: 4: 0.05, add hot reflux, contain the air of suitable quantity of water steam simultaneously in feeding, react 2h at a certain temperature, then with reactant mixture, separating, is solvent clean with alcohol, drying; Promptly get nano-TiO in 400 ℃ of following roasting 3h of uniform temperature behind the porphyrize
2Powder.
The said goods is carried out the photocatalysis performance test.This experiment is a tester with the ZBF dyestuff.Measurement result, the removal efficient in 60 minutes is 99.7%.
Embodiment 6
The steam hydrolysis legal system is equipped with nano-TiO
2The preparation of photochemical catalyst: have in the reaction unit that stirs that refluxes, in there-necked flask, add titanium tetrachloride, ethanol, dispersant successively by certain raw material proportioning, ratio is 1: 4: 0.05, add hot reflux, contain the air of suitable quantity of water steam simultaneously in feeding, react 2h at a certain temperature, then with reactant mixture, separating, is solvent clean with alcohol, drying; Promptly get nano-TiO in 500 ℃ of following roasting 3h of uniform temperature behind the porphyrize
2Powder.
The said goods is carried out the photocatalysis performance test.This experiment is a tester with the ZBF dyestuff.Measurement result, the removal efficient in 60 minutes is 99.8%.
Claims (4)
1. the method for producing nano-titanic oxide light catalyst by steam hydrolysis is characterized in that, this method comprises the steps:
A. in having the reaction unit that stirs that refluxes, take by weighing a certain amount of titanium tetrachloride, lower alcohol and dispersant in proportion and drop into successively in the there-necked flask, add hot reflux, contain the air of suitable quantity of water steam simultaneously in feeding, react 0.5～4h at a certain temperature, obtain product mixture.
B. the above-mentioned product mixture that makes is dipped in the ethanolic solution, it is fully mixed, isolate thick product through high speed centrifugation, repeatedly washing behind the removal chlorion, is taken out.
C. the above-mentioned thick product that makes is placed in the baking oven, baking is done down about 100 ℃, makes solvent evaporates, and gained titanium dioxide is put into muffle furnace roasting 2～6h and promptly got the nano TiO 2 powder.
2. the method for aforesaid producing nano-titanic oxide light catalyst by steam hydrolysis, described lower alcohol comprises methyl alcohol, ethanol, propyl alcohol, n-butanol and isopropyl alcohol.
3. the method for aforesaid producing nano-titanic oxide light catalyst by steam hydrolysis, its described reaction temperature is: 50～100 ℃.
4. the method for aforesaid producing nano-titanic oxide light catalyst by steam hydrolysis, its described sintering temperature is: 300～700 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100118450A CN100569358C (en) | 2007-06-25 | 2007-06-25 | The method of producing nano-titanic oxide light catalyst by steam hydrolysis |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100118450A CN100569358C (en) | 2007-06-25 | 2007-06-25 | The method of producing nano-titanic oxide light catalyst by steam hydrolysis |
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| CN101073769A true CN101073769A (en) | 2007-11-21 |
| CN100569358C CN100569358C (en) | 2009-12-16 |
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| CNB2007100118450A Expired - Fee Related CN100569358C (en) | 2007-06-25 | 2007-06-25 | The method of producing nano-titanic oxide light catalyst by steam hydrolysis |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102389785A (en) * | 2011-09-26 | 2012-03-28 | 武汉理工大学 | Method for preparing TiO2 nano crystals with high photocatalytic activity |
| CN103120933A (en) * | 2011-11-18 | 2013-05-29 | 中国石油化工股份有限公司 | Preparation method of nanometer TiO2/ZrO2 composite material |
| CN111545186A (en) * | 2020-05-14 | 2020-08-18 | 江西宝弘纳米科技有限公司 | Attapulgite loaded TiO2And preparation method and application thereof |
| CN112226264A (en) * | 2020-10-19 | 2021-01-15 | 中国科学院兰州化学物理研究所 | Attapulgite-titanium dioxide modified ultra-high molecular weight polyethylene composite material and preparation method and application thereof |
| CN114956155A (en) * | 2022-06-21 | 2022-08-30 | 中国船舶重工集团公司第七二五研究所 | Composite anti-fouling agent and preparation method thereof |
-
2007
- 2007-06-25 CN CNB2007100118450A patent/CN100569358C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102389785A (en) * | 2011-09-26 | 2012-03-28 | 武汉理工大学 | Method for preparing TiO2 nano crystals with high photocatalytic activity |
| CN103120933A (en) * | 2011-11-18 | 2013-05-29 | 中国石油化工股份有限公司 | Preparation method of nanometer TiO2/ZrO2 composite material |
| CN111545186A (en) * | 2020-05-14 | 2020-08-18 | 江西宝弘纳米科技有限公司 | Attapulgite loaded TiO2And preparation method and application thereof |
| CN112226264A (en) * | 2020-10-19 | 2021-01-15 | 中国科学院兰州化学物理研究所 | Attapulgite-titanium dioxide modified ultra-high molecular weight polyethylene composite material and preparation method and application thereof |
| CN112226264B (en) * | 2020-10-19 | 2021-07-23 | 中国科学院兰州化学物理研究所 | Attapulgite-titanium dioxide modified ultra-high molecular weight polyethylene composite material and preparation method and application thereof |
| CN114956155A (en) * | 2022-06-21 | 2022-08-30 | 中国船舶重工集团公司第七二五研究所 | Composite anti-fouling agent and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100569358C (en) | 2009-12-16 |
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Granted publication date: 20091216 Termination date: 20120625 |