CN101433828A - Aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst and preparation method - Google Patents
Aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst and preparation method Download PDFInfo
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- CN101433828A CN101433828A CNA2008101542948A CN200810154294A CN101433828A CN 101433828 A CN101433828 A CN 101433828A CN A2008101542948 A CNA2008101542948 A CN A2008101542948A CN 200810154294 A CN200810154294 A CN 200810154294A CN 101433828 A CN101433828 A CN 101433828A
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Abstract
The invention discloses an aluminum-doped titanium dioxide nanotube visible light catalyst and a preparation method thereof. The aluminum-doped titanium dioxide nanotube visible light catalyst is prepared by the following method: (1) titanium dioxide powder and aluminum oxide powder are added into a sodium hydroxide water solution to be stirred, heated and react; (2) the mixture is cooled to normal temperature and is washed until the pH value is between 6.5 and 7.5; (3) an inorganic acid aqueous solution is used to adjust the pH value, the soaking is performed, and then the washing is performed until the pH value is between 6.5 and 7.5; (4) a trapped concentrated solution is dried to obtain a solid after the filtration; and (5) the calcination is performed for 5 to 7 hours at a temperature of between 300 and 700 DEG C to obtain the aluminum-doped titanium dioxide nanotube visible light catalyst. The catalyst can reduce the treatment cost for photocatalytic reactions, and fully utilize solar resources; the removal rate of the catalyst to humic acid TOC under visible light irradiation is high up to more than 70 percent and is only reduced by 10 percent or so compared with that of under ultraviolet lamp condition, thereby showing a good visible light excitation function.
Description
Technical field
The present invention relates to a kind of photochemical catalyst and preparation method, especially relate to a kind of visible light catalyst and preparation method.
Background technology
Because photocatalysis can produce the very strong hydroxyl radical free radical of oxidability, it can non-selectivity ground be degraded the polluter reaction, so the exploitation of at present new and effective photochemical catalyst becomes focus.As a kind of photochemical catalyst, titania nanotube becomes the research focus of photochemical catalyst and ozone catalytic agent as the product that specific area is bigger in the titanium dioxide series.
But, because catalyst restriction, be used to study that the lamp source of light-catalyzed reaction is most is the uviol lamp source, in actual use, processing cost is bigger than normal, and human body is had certain injury, and practical value is restricted.At present, the way of head it off is generally carries out element doping to catalyst, make catalyst under excited by visible light, carry out catalytic reaction, research focuses mostly in powdery or film titanium deoxide catalyst are mixed, and does not still have and the titania nanotube of high-specific surface area is carried out the research that aluminium mixes.
Summary of the invention
It is higher to the objective of the invention is to solve in the photocatalytic process processing cost, and catalyst needs carry out light-catalysed problem under ultraviolet light, and a kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst is provided.
Second purpose of the present invention provides a kind of preparation method of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst.
Technical scheme of the present invention is summarized as follows:
A kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst is to make with following method:
(1) is to add 0.5-1.0g titanium dioxide powder and 0.03-0.30g aluminium oxide powder in the sodium hydrate aqueous solution of 10mol/L or the potassium hydroxide aqueous solution in 15-20mL concentration, stirs 0.5-1h; Be heated to 100-120 ℃, reaction 20-30h;
(2) be cooled to normal temperature, it is 6.5-7.5 that products therefrom is washed to pH;
(3) use the pH of the solution that inorganic aqueous acid regulating step (2) obtains to be 1-3, soak 0.4-1h, being washed to pH again is 6.5-7.5;
(4) solution with step (3) preparation filters, with the concentrate that is retained down under 50-70 ℃, the down dry 5-7h of normal pressure, solid;
(5),, promptly make a kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst with the described solid calcining of step (4) 5-7h at 300-700 ℃.
Aqueous hydrochloric acid solution, aqueous sulfuric acid, phosphate aqueous solution or aqueous solution of nitric acid that described inorganic aqueous acid is 0.1-0.5mol/L.
A kind of preparation method of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst comprises the steps:
(1) is to add 0.5-1.0g titanium dioxide powder and 0.03-0.30g aluminium oxide powder in the sodium hydrate aqueous solution of 10mol/L or the potassium hydroxide aqueous solution in 15-20mL concentration, stirs 0.5-1h; Be heated to 100-120 ℃, reaction 20-30h;
(2) be cooled to normal temperature, it is 6.5-7.5 that products therefrom is washed to pH;
(3) use the pH of the solution that inorganic aqueous acid regulating step (2) obtains to be 1-3, soak 0.4-1h, being washed to pH again is 6.5-7.5;
(4) solution with step (3) preparation filters, with the concentrate that is retained down under 50-70 ℃, the down dry 5-7h of normal pressure, solid;
(5),, promptly make a kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst with the described solid calcining of step (4) 5-7h at 300-700 ℃.
Aqueous hydrochloric acid solution, aqueous sulfuric acid, phosphate aqueous solution or aqueous solution of nitric acid that described inorganic aqueous acid is 0.1-0.5mol/L.
A kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst of the present invention can reduce the processing cost of light-catalyzed reaction, make full use of the sunshine resource, its under radiation of visible light to the clearance of humic acid TOC up to more than 70%, than under the uviol lamp condition, only having reduced about 10%, shown good excited by visible light function.
Description of drawings
Fig. 1 is the microstructure of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst;
Fig. 2 is the degradation effect of photocatalysis to humic acid TOC.
The specific embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
A kind of preparation method of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst comprises the steps:
(1) is to add 0.7g titanium dioxide powder and 0.10g aluminium oxide powder in the sodium hydrate aqueous solution of 10mol/L in 17mL concentration, stirs 0.8h; Change the reactor of inner liner polytetrafluoroethylene over to, be heated to 110 ℃, reaction 25h;
(2) be cooled to normal temperature, it is 7 that products therefrom is washed to pH;
(3) using the pH of the solution that the aqueous hydrochloric acid solution regulating step (2) of 0.1mol/L obtains is 2, soaks 0.5h, and being washed to pH again is 7;
(4) solution with step (3) preparation filters, with the concentrate that is retained down under 60 ℃, dry 6h under the normal pressure, solid;
(5),, promptly make a kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst with the described solid calcining of step (4) 6h at 500 ℃.
It is that the titania powder (trade name is P25) of 25 nanometers is prepared that present embodiment adopts business-like particle diameter.
The microstructure of a kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst of present embodiment preparation is seen Fig. 1.Degradation effect to humic acid TOC is seen Fig. 2.
Embodiment 2
A kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst is to make with following method:
(1) is to add 1.0g titanium dioxide powder and 0.30g aluminium oxide powder in the potassium hydroxide aqueous solution of 10mol/L in 15mL concentration, stirs 0.5h; Be heated to 120 ℃, reaction 20h;
(2) be cooled to normal temperature, it is 7.5 that products therefrom is washed to pH;
(3) using the pH of the solution that the aqueous sulfuric acid regulating step (2) of 0.5mol/L obtains is 3, soaks 1h, and being washed to pH again is 7.5;
(4) solution with step (3) preparation filters, with the concentrate that is retained down under 70 ℃, dry 5h under the normal pressure, solid;
(5),, promptly make a kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst with the described solid calcining of step (4) 6h at 400 ℃.
Embodiment 3
A kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst is to make with following method:
(1) is to add 0.5g titanium dioxide powder and 0.20g aluminium oxide powder in the potassium hydroxide aqueous solution of 10mol/L in 20mL concentration, stirs 0.8h; Be heated to 100 ℃, reaction 30h;
(2) be cooled to normal temperature, it is 6.5 that products therefrom is washed to pH;
(3) using the pH of the solution that the phosphate aqueous solution regulating step (2) of 0.3mol/L obtains is 1, soaks 0.4h, and being washed to pH again is 6.5;
(4) solution with step (3) preparation filters, with the concentrate that is retained down under 50 ℃, dry 7h under the normal pressure, solid;
(5),, promptly make a kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst with the described solid calcining of step (4) 5h at 700 ℃.
Embodiment 4
A kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst is to make with following method:
(1) is to add 0.8g titanium dioxide powder and 0.03g aluminium oxide powder in the sodium hydrate aqueous solution of 10mol/L in 18mL concentration, stirs 1h; Be heated to 110 ℃, reaction 25h;
(2) be cooled to normal temperature, it is 7 that products therefrom is washed to pH;
(3) using the pH of the solution that the aqueous solution of nitric acid regulating step (2) of 0.2mol/L obtains is 2, soaks 0.5h, and being washed to pH again is 7;
(4) solution with step (3) preparation filters, with the concentrate that is retained down under 60 ℃, dry 6h under the normal pressure, solid;
(5),, promptly make a kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst with the described solid calcining of step (4) 7h at 300 ℃.
Claims (4)
1. aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst is characterized in that making with following method:
(1) is to add 0.5-1.0g titanium dioxide powder and 0.03-0.30g aluminium oxide powder in the sodium hydrate aqueous solution of 10mol/L or the potassium hydroxide aqueous solution in 15-20mL concentration, stirs 0.5-1h; Be heated to 100-120 ℃, reaction 20-30h;
(2) be cooled to normal temperature, it is 6.5-7.5 that products therefrom is washed to pH;
(3) use the pH of the solution that inorganic aqueous acid regulating step (2) obtains to be 1-3, soak 0.4-1h, being washed to pH again is 6.5-7.5;
(4) solution with step (3) preparation filters, with the concentrate that is retained down under 50-70 ℃, the down dry 5-7h of normal pressure, solid;
(5),, promptly make a kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst with the described solid calcining of step (4) 5-7h at 300-700 ℃.
2. a kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst according to claim 1 is characterized in that described inorganic aqueous acid is the aqueous hydrochloric acid solution of 0.1-0.5mol/L, aqueous sulfuric acid, phosphate aqueous solution or aqueous solution of nitric acid.
3. the preparation method of an aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst is characterized in that comprising the steps:
(1) is to add 0.5-1.0g titanium dioxide powder and 0.03-0.30g aluminium oxide powder in the sodium hydrate aqueous solution of 10mol/L or the potassium hydroxide aqueous solution in 15-20mL concentration, stirs 0.5-1h; Be heated to 100-120 ℃, reaction 20-30h;
(2) be cooled to normal temperature, it is 6.5-7.5 that products therefrom is washed to pH;
(3) use the pH of the solution that inorganic aqueous acid regulating step (2) obtains to be 1-3, soak 0.4-1h, being washed to pH again is 6.5-7.5;
(4) solution with step (3) preparation filters, with the concentrate that is retained down under 50-70 ℃, the down dry 5-7h of normal pressure, solid;
(5),, promptly make a kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst with the described solid calcining of step (4) 5-7h at 300-700 ℃.
4. the preparation method of a kind of aluminum doped titanium dioxide nano tube visible-light responsive photocatalyst according to claim 3 is characterized in that described inorganic aqueous acid is the aqueous hydrochloric acid solution of 0.1-0.5mol/L, aqueous sulfuric acid, phosphate aqueous solution or aqueous solution of nitric acid.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013008209A2 (en) | 2011-07-14 | 2013-01-17 | Centro De Investigación Y De Estudios Avanzados Del Instituto Politécnico Nacional | Methods for the preparation of carbon nanotubes doped with different elements |
| CN103157476A (en) * | 2013-04-01 | 2013-06-19 | 北京科技大学 | Fe-doped TiO2 nanotube photocatalyst, and preparation method and application thereof |
| CN106245092A (en) * | 2016-08-10 | 2016-12-21 | 太原理工大学 | A kind of fast preparation method of black titanium dioxide nano-tube array |
| CN106268765A (en) * | 2016-07-15 | 2017-01-04 | 辽宁大学 | A kind of metal ion doped titanium dioxide method for manufacturing thin film |
-
2008
- 2008-12-19 CN CNA2008101542948A patent/CN101433828A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013008209A2 (en) | 2011-07-14 | 2013-01-17 | Centro De Investigación Y De Estudios Avanzados Del Instituto Politécnico Nacional | Methods for the preparation of carbon nanotubes doped with different elements |
| CN103157476A (en) * | 2013-04-01 | 2013-06-19 | 北京科技大学 | Fe-doped TiO2 nanotube photocatalyst, and preparation method and application thereof |
| CN103157476B (en) * | 2013-04-01 | 2015-03-11 | 北京科技大学 | Fe-doped TiO2 nanotube photocatalyst, and preparation method and application thereof |
| CN106268765A (en) * | 2016-07-15 | 2017-01-04 | 辽宁大学 | A kind of metal ion doped titanium dioxide method for manufacturing thin film |
| CN106268765B (en) * | 2016-07-15 | 2019-01-08 | 辽宁大学 | A kind of metal ion doped titanium dioxide method for manufacturing thin film |
| CN106245092A (en) * | 2016-08-10 | 2016-12-21 | 太原理工大学 | A kind of fast preparation method of black titanium dioxide nano-tube array |
| CN106245092B (en) * | 2016-08-10 | 2018-04-27 | 太原理工大学 | A kind of fast preparation method of black titanium dioxide nano-tube array |
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