CN102078806A - Method for preparing doped mesoporous titanium photocatalyst - Google Patents
Method for preparing doped mesoporous titanium photocatalyst Download PDFInfo
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Abstract
The invention discloses a method for preparing doped mesoporous titanium photocatalyst, which is to prepare the doped mesoporous titanium photocatalyst by using triblock copolymer, namely polyethylene glycol-polypropylene glycol-polyethylene glycol(P123), as a template agent, a tetrabutyl titanate as a titanium source, and a boron, nitrogen or tervalent titanium-containing compound as a doping element-containing precursor, synthesizing by a process of evaporation-induced self-assembly at a certain temperature and humidity, drying and roasting. The catalyst prepared by the method has high catalytic activity in visible light and can quickly degrade organic pollutants in dye waste water.
Description
Technical field
The present invention relates to a kind of preparation method of photochemical catalyst, relate to a kind of preparation method of doped mesoporous TiO 2 photochemical catalyst particularly, the catalyst that the inventive method makes is the organic pollution in the energy degradation water under visible light.
Background technology
Titanium dioxide is a kind of important inorganic semiconductor functional material, and stable, the strong oxidation-reduction quality of chemical property, anti-photoetch, nontoxic, low cost and other advantages are arranged, and is in the core status of photocatalysis research always.But its band gap bigger (Eg=3.2eV), can only be less than or equal to the ultraviolet excitation of 387nm, thereby lower, its photo-generated carrier (e in addition to the utilization ratio of solar energy (ultraviolet light that contains 3-5%) by wavelength
-, h
+) be easy to compoundly, be 10 the compound of catalyst surface
-9Finish in the time of second, thereby limited the practicality of titanium dioxide in catalytic oxidation.Therefore, how reducing the recombination probability of photo-generated carrier, the photoresponse scope of expansion titanium dioxide optical catalyst, is the key of research with the visible light photocatalysis performance that improves titanium dioxide.Discover that since calendar year 2001 nonmetal doping titanium dioxide has good visible absorption and photocatalytic activity, mix and become a kind of important method for preparing high efficiency photocatalyst rapidly, mix promptly by changing the electronic structure and the surface nature of TiO 2 particles, enlarge the photoresponse scope, suppress the compound of photo-generated carrier, improve the stability and the photocatalytic activity of catalysis material simultaneously to improve quantum efficiency.
The present invention is intended to solve key difficult problems such as the low and visible light catalytic efficient of the solar energy utilization ratio of titanium dioxide optical catalyst is low, a kind of preparation method of doped mesoporous TiO 2 photochemical catalyst is provided, and it is simple to have method, easy to operate, cost, equipment requires characteristics such as low.
Summary of the invention
The invention provides a kind of preparation method of doped mesoporous TiO 2 photochemical catalyst, may further comprise the steps successively:
1) triblock copolymer polyethylene glycol-propane diols-polyethylene glycol is mixed with absolute ethyl alcohol, stirring is fully dissolved triblock copolymer polyethylene glycol-propane diols-polyethylene glycol, drip butyl titanate then, continue to stir the yellow solution that obtains homogeneous transparent;
2) precursor that will contain doped chemical is dissolved in the absolute ethyl alcohol, adds entry and glacial acetic acid then, forms colourless transparent solution;
3) step 2) the gained drips of solution is added in the step 1) gained solution, and stirring mixes it; Pour culture dish then into, at room temperature induce into membranaceous gel through volatilization;
4) above-mentioned gel is dried in baking oven, gets xerogel, through roasting, gets described doped mesoporous TiO 2 photochemical catalyst.
Among the present invention, the mixing time that triblock copolymer polyethylene glycol-propane diols-polyethylene glycol mixes with absolute ethyl alcohol in the described step 1) is 2-3h, and mixing time is 30-60 min behind the dropping butyl titanate.
Among the present invention, splash into titanium trichloride in the whipping process in the described step 1) after dripping butyl titanate.
Step 2) precursor that contains doped chemical described in is meant the compound of boracic, nitrogen or titanous.Among the present invention, the described precursor that contains doped chemical is boric acid preferably, or boric acid and triethanolamine, or boric acid and titanium trichloride.
Mixing time described in the step 3) is 30-60 min.
The temperature of drying in the step 4) is 80 ℃, and sintering temperature is 400-600 ℃, and roasting time is 4h.
Among the present invention, the mol ratio of butyl titanate, absolute ethyl alcohol, water, glacial acetic acid is 1:18-22:3:1-1.2.
Among the present invention, the compound by adding boracic, nitrogen or titanous is realized the purpose that preparation is titania-doped as the precursor that contains doped chemical.Among the present invention, preferably be the boron source with boric acid, triethanolamine is a nitrogenous source, and titanium trichloride is the titanous source.When mixing, because triethanolamine density is bigger, therefore earlier it is dissolved in the absolute ethyl alcohol with boric acid, mix with step 1) gained solution again.And titanium trichloride is a liquid, therefore directly is added drop-wise in the yellow solution of gained in the step 1).
The preparation method of a kind of doped mesoporous TiO 2 photochemical catalyst that The present invention be directed to the deficiencies in the prior art and provide, this method is induced self-assembly method for volatilization, with triblock copolymer polyethylene glycol-propane diols-polyethylene glycol (P
123) be the template agent, butyl titanate is the titanium source, boric acid is the boron source, triethanolamine is a nitrogenous source, and titanium trichloride is the titanous source, and absolute ethyl alcohol is a solvent, acetic acid is inhibitor, induces the method for self assembly synthetic by volatilization under certain temperature and humidity, obtains through super-dry and roasting then.The catalyst that the present invention prepares has reasonable response effect to visible light, fast degrading organic contaminant in wastewater.
The preparation method of doped mesoporous TiO 2 photochemical catalyst of the present invention comprises following concrete steps:
A, with triblock copolymer polyethylene glycol-propane diols-polyethylene glycol (P
123) mix with an amount of absolute ethyl alcohol, stir 2-3 h and make triblock copolymer polyethylene glycol-propane diols-polyethylene glycol (P
123) fully dissolving, drip tetraethyl titanate then, continue to stir the yellow solution that 30-60 min obtains homogeneous transparent;
B, boric acid is dissolved in an amount of ethanol, adds an amount of water and inhibitor glacial acetic acid then, form colourless transparent solution;
C, b is added drop-wise among a, and stirs 30-60 min it is mixed; Pour culture dish then into, at room temperature induce into membranaceous gel through volatilization;
D, above-mentioned gel are dried in 80 ℃ of baking ovens, get xerogel, then at 400-600 ℃ of following roasting 4 h, get the doped mesoporous TiO 2 photochemical catalyst.
Wherein, the mol ratio of butyl titanate, absolute ethyl alcohol, water and glacial acetic acid is 1:18-22:3:1-1.2.。
The beneficial effect that the present invention has comprises: nonmetalloid boron has obtained the photochemical catalyst of high catalytic activity to the doping of titanium dioxide, for the degraded of organic pollution in the industrial wastewater provides catalysis material; Nonmetal boron and nonmetal nitrogen have obtained the more visible-light photocatalyst of high catalytic activity to the codope of titanium dioxide, have improved the degradation efficiency to organic pollution widely; This catalyst produces effect under visible light, can improve the utilization ratio of sunshine greatly; This method for preparing catalyst is simple, and equipment requires low, and process conditions are simple.
The specific embodiment:
In conjunction with following specific embodiment, the present invention is described in further detail, and protection content of the present invention is not limited to following examples.Under the spirit and scope that do not deviate from inventive concept, variation and advantage that those skilled in the art can expect all are included among the present invention, and are protection domain with the appending claims.
Embodiment 1
Present embodiment preparation be doped titanium dioxide photocatalyst not, employing be preparation condition and the method identical with other embodiment.
A, with 1 g triblock copolymer polyethylene glycol-propane diols-polyethylene glycol (P
123) mix with 30 mL absolute ethyl alcohols, stir 3h and make P
123Be dissolved in fully in the ethanol, drip 11.3 g butyl titanates then, and continue to stir 40 min, obtain the yellow solution of homogeneous transparent;
B, 1.8 mL water and 2 mL inhibitor glacial acetic acids and 5 mL absolute ethyl alcohols are mixed;
C, b is added drop-wise among a, and it is mixed; Pour culture dish then into, at room temperature induce into membranaceous gel through volatilization;
D, above-mentioned gel are dried in 80 ℃ of baking ovens, get xerogel, then at 500 ℃ of following roasting 4 h, get mesopore titania photocatalyst.
The above not doped mesoporous TiO 2 photochemical catalyst for preparing is reacted, promptly, methylene blue solution 50 mL that get above-mentioned photochemical catalyst 0.1 g, 10 mg/L join in the reactor, dark reaction 40 min, and then be to carry out illumination 4 h under the 300 W halogen tungsten lamps (simulated solar irradiation) with light source, experimental result shows that the percent of decolourization of methylene blue reaches 23.6 %, shows that the doped titanium dioxide photocatalyst catalytic efficiency is not lower.
Embodiment 2
A, with 1 g triblock copolymer polyethylene glycol-propane diols-polyethylene glycol (P
123) mix with 30 mL absolute ethyl alcohols, stir 3h and make P
123Be dissolved in fully in the ethanol, drip 11.3 g butyl titanates then, and continue to stir 40 min, obtain the yellow solution of homogeneous transparent;
B, 0.02 g boric acid is dissolved in the 5 mL absolute ethyl alcohols, adds 1.8 mL water and 2 mL inhibitor glacial acetic acids then, form colourless transparent solution;
C, b is added drop-wise among a, and it is mixed; Pour culture dish then into, at room temperature induce into membranaceous gel through volatilization;
D, above-mentioned gel are dried in 80 ℃ of baking ovens, get xerogel, then at 500 ℃ of following roasting 4 h, get boron doped mesoporous TiO 2 photochemical catalyst.
The above boron doped mesoporous TiO 2 photochemical catalyst for preparing is reacted, promptly, methylene blue solution 50 mL that get above-mentioned photochemical catalyst 0.1 g, 10 mg/L join in the reactor, dark reaction 40 min, and then be to carry out illumination 4 h under the 300 W halogen tungsten lamps (simulated solar irradiation) with light source, experimental result shows that the percent of decolourization of methylene blue reaches 74.8%.What use in the present embodiment is the titanium dioxide optical catalyst of the mol ratio of boron and titanium as 1:100, and its catalytic efficiency is compared with unadulterated catalyst among the embodiment 1 and is significantly improved.
Embodiment 3
A, with 1 g P
123Mix with 30 mL absolute ethyl alcohols, stir 3 h and make P
123Be dissolved in fully in the ethanol, drip 11.3 g butyl titanates then, and continue to stir 40 min, obtain the yellow solution of homogeneous transparent;
B, 0.04 g boric acid is dissolved in the 5 mL absolute ethyl alcohols, adds 1.8 mL water and 2 mL inhibitor acetate then, form colourless transparent solution;
C, b is added drop-wise among a, and it is mixed; Pour culture dish then into, at room temperature through evaporating into membranaceous gel;
D, above-mentioned gel are dried in 80 ℃ of baking ovens, get xerogel, then at 500 ℃ of following roasting 4 h, get boron doped mesoporous TiO 2 photochemical catalyst.
The above boron doped mesoporous TiO 2 photochemical catalyst for preparing is reacted, promptly, methylene blue solution 50 mL that get above-mentioned photochemical catalyst 0.1 g, 10 mg/L join in the reactor, dark reaction 40 min, light source is 300 W halogen tungsten lamps (simulated solar irradiation), behind illumination 4 h, experimental result shows that the percent of decolourization of methyl blue reaches 96 %.What use in the present embodiment is the titanium dioxide optical catalyst of the mol ratio of boron and titanium as 2:100, and its catalytic efficiency is compared with embodiment 2 specimen in use and further raising arranged.
Embodiment 4
A, with 1 g P
123Mix with 30 mL absolute ethyl alcohols, stir 3 h and make P
123Be dissolved in fully in the ethanol, drip 11.3 g butyl titanates then, and continue to stir 40 min, obtain the yellow solution of homogeneous transparent;
B, 0.06 g boric acid is dissolved in the 5 mL absolute ethyl alcohols, adds 1.8 mL water and 2 mL inhibitor acetate then, form colourless transparent solution;
C, b is added drop-wise among a, and it is mixed; Pour culture dish then into, at room temperature through evaporating into membranaceous gel;
D, above-mentioned gel are dried in 80 ℃ of baking ovens, get xerogel, then at 500 ℃ of following roasting 4 h, get boron doped mesoporous TiO 2 photochemical catalyst.
The above boron doped mesoporous TiO 2 photochemical catalyst for preparing is reacted, promptly, methylene blue solution 50 mL that get above-mentioned photochemical catalyst 0.1 g, 10 mg/L join in the reactor, dark reaction 40 min, light source is 300 W halogen tungsten lamps (simulated solar irradiation), behind illumination 4 h, the percent of decolourization of methyl blue reaches 91.6%.Present embodiment preparation be that the mol ratio of boron and titanium is the titanium dioxide optical catalyst of 3:100, though the sample of the boron in its catalytic efficiency comparing embodiment 2 and the mol ratio 2:100 of titanium descends to some extent, but compare with unadulterated catalyst among the embodiment 1, the catalytic efficiency of present embodiment products obtained therefrom still is significantly increased.
Embodiment 5
A, with 1 g P
123Mix with 30 mL absolute ethyl alcohols, stir 3 h and make P
123Be dissolved in fully in the ethanol, drip 11.3 g butyl titanates then, and continue to stir 40 min, obtain the yellow solution of homogeneous transparent;
B, 0.1g boric acid is dissolved in the 5mL absolute ethyl alcohol, adds 1.8mL water and 2mL inhibitor acetate then, form colourless transparent solution;
C, b is added drop-wise among a, and it is mixed; Pour culture dish then into, at room temperature through evaporating into membranaceous gel;
D, above-mentioned gel are dried in 80 ℃ of baking ovens, get xerogel, then at 500 ℃ of following roasting 4h, get boron doped mesoporous TiO 2 photochemical catalyst.
The above boron doped mesoporous TiO 2 photochemical catalyst for preparing is reacted, promptly, methylene blue solution 50 mL that get above-mentioned photochemical catalyst 0.1 g, 10 mg/L join in the reactor, dark reaction 40 min, light source is 300 W halogen tungsten lamps (simulated solar irradiation), behind illumination 4 h, the percent of decolourization of methyl blue reaches 78%.This experiment is that the mol ratio of boron and titanium is the titanium dioxide optical catalyst of 5:100, though its catalytic efficiency descends to some extent than the mol ratio 3:100 sample of boron among the embodiment 4 and titanium, but compare with unadulterated catalyst among the embodiment 1, the catalytic efficiency of present embodiment products obtained therefrom still is significantly increased.
Embodiment 6
A, with 1 g P
123Mix with 30 mL absolute ethyl alcohols, stir 3 h and make P
123Be dissolved in fully in the ethanol, drip 11.3 g butyl titanates then, and continue to stir 40 min, obtain the yellow solution of homogeneous transparent;
B, 0.04 g boric acid and 0.1 g triethanolamine are dissolved in the 5 mL absolute ethyl alcohols, add 1.8 mL water and 2 mL inhibitor glacial acetic acids then, form colourless transparent solution;
C, b is added drop-wise among a, and it is mixed; Pour culture dish then into, at room temperature induce into membranaceous gel through volatilization;
D, above-mentioned gel are dried in 80 ℃ of baking ovens, xerogel, then at 500 ℃ of following roasting 4 h, boron, nitrogen co-doped mesopore titania photocatalyst.
The above boron doped mesoporous TiO 2 photochemical catalyst for preparing is reacted, promptly, methylene blue solution 50 mL that get above-mentioned photochemical catalyst 0.1 g, 10 mg/L join in the reactor, dark reaction 40 min, light source is 300 W halogen tungsten lamps (simulated solar irradiation), behind illumination 3 h, the percent of decolourization of methyl blue reaches 97.6%.This sample is to have mixed nonmetalloid nitrogen on the basis of best boron-doping amount (0.04 g boric acid), and the catalyst of the single doped with boron that obtains with embodiment 2,3,4,5 is compared, and its photocatalysis efficiency has obtained further raising.
Embodiment 7
A, with 1 g P
123Mix with 30 mL absolute ethyl alcohols, stir 3 h and make P
123Be dissolved in fully in the ethanol, drip 11.3 g butyl titanates then, and continue to stir 40 min, obtain the yellow solution of homogeneous transparent, under agitation drip the titanium trichloride of 0.25 mL then;
B, 0.04 g boric acid is dissolved in the 5 mL absolute ethyl alcohols, adds 1.8 mL water and 2 mL inhibitor glacial acetic acids then, form clear solution;
C, b is added drop-wise among a, and it is mixed; Pour culture dish then into, at room temperature induce into membranaceous gel through volatilization;
D, above-mentioned gel are dried in 80 ℃ of baking ovens, get xerogel, then at 500 ℃ of following roasting 4 h, get boron doped mesoporous TiO 2 photochemical catalyst.
The above boron doped mesoporous TiO 2 photochemical catalyst for preparing is reacted, promptly, methylene blue solution 50 mL that get above-mentioned photochemical catalyst 0.1 g, 10 mg/L join in the reactor, dark reaction 40 min, light source is 300 W halogen tungsten lamps (simulated solar irradiation), behind illumination 3 h, the percent of decolourization of methyl blue reaches 82%.This sample is to have mixed the titanous atom on the basis of best boron-doping amount, its photocatalysis efficiency increases than the catalyst of single doped with boron of embodiment 2,5, and is significantly increased than the catalytic efficiency of the not doped mesoporous TiO 2 photochemical catalyst of preparation among the embodiment 1.
Claims (8)
1. the preparation method of a doped mesoporous TiO 2 photochemical catalyst is characterized in that, described method may further comprise the steps successively:
1) triblock copolymer polyethylene glycol-propane diols-polyethylene glycol is mixed with absolute ethyl alcohol, stirring is fully dissolved triblock copolymer polyethylene glycol-propane diols-polyethylene glycol, drip butyl titanate then, continue to stir the yellow solution that obtains homogeneous transparent;
2) precursor that will contain doped chemical is dissolved in the absolute ethyl alcohol, adds entry and glacial acetic acid then, forms colourless transparent solution;
3) step 2) the gained drips of solution is added in the step 1) gained solution, stirs it is mixed; Pour culture dish then into, at room temperature induce into membranaceous gel through volatilization;
4) above-mentioned membranaceous gel is dried in baking oven, obtain xerogel,, obtain described doped mesoporous TiO 2 photochemical catalyst through roasting.
2. preparation method as claimed in claim 1 is characterized in that, the mixing time that triblock copolymer polyethylene glycol-propane diols-polyethylene glycol mixes with absolute ethyl alcohol in the described step 1) is 2-3h; Mixing time behind the dropping Butyl Phthalate is 30-60 min.
3. preparation method as claimed in claim 1 is characterized in that, splashes into titanium trichloride in the whipping process in the described step 1) after dripping butyl titanate.
4. preparation method as claimed in claim 1 is characterized in that step 2) described in contain doped chemical precursor be meant the compound of boracic, nitrogen or titanous.
5. preparation method as claimed in claim 4 is characterized in that step 2) described in contain doped chemical precursor be boric acid, or boric acid and triethanolamine, or boric acid and titanium trichloride.
6. preparation method as claimed in claim 1 is characterized in that, mixing time described in the step 3) is 30-60 min.
7. preparation method as claimed in claim 1 is characterized in that, the temperature of drying in the step 4) is 80 ℃, and sintering temperature is 400-600 ℃, and roasting time is 4 h.
8. preparation method as claimed in claim 1 is characterized in that, the mol ratio of described butyl titanate, absolute ethyl alcohol, water and glacial acetic acid is 1:18-22:3:1-1.2.
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| CN102583529A (en) * | 2012-02-28 | 2012-07-18 | 南京大学 | Method for preparing mesoporous titanium dioxide by template method and application of mesoporous titanium dioxide to preparation of dye-sensitized solar cells |
| CN103949232A (en) * | 2014-04-30 | 2014-07-30 | 上海师范大学 | TiO2 photocatalyst with mesoporous structure, as well as preparation method and applications of photocatalyst |
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| CN102583529B (en) * | 2012-02-28 | 2014-12-10 | 南京大学 | Method for preparing mesoporous titanium dioxide by template method and application of mesoporous titanium dioxide to preparation of dye-sensitized solar cells |
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| CN105013500A (en) * | 2014-04-23 | 2015-11-04 | 同济大学 | Heterogeneous Fenton catalyst for degrading azo dye wastewater as well as preparation method and application of heterogeneous Fenton catalyst |
| CN103949232A (en) * | 2014-04-30 | 2014-07-30 | 上海师范大学 | TiO2 photocatalyst with mesoporous structure, as well as preparation method and applications of photocatalyst |
| CN104128172A (en) * | 2014-07-29 | 2014-11-05 | 南昌航空大学 | Method for regulating and controlling morphology of nano TiO2-CeO2 into ball shape, dumbbell shape or sheet shape |
| CN104843780A (en) * | 2015-04-30 | 2015-08-19 | 景德镇陶瓷学院 | Preparation method of anatase black nano titanium oxide powder |
| CN104843780B (en) * | 2015-04-30 | 2016-06-22 | 景德镇陶瓷大学 | A kind of preparation method of anatase black nano titanium oxide powder |
| CN105435828A (en) * | 2015-12-31 | 2016-03-30 | 北京化工大学 | Fe and N co-doped mesoporous TiO2 microsphere array visible light photocatalyst and preparation method |
| CN105854955A (en) * | 2016-04-25 | 2016-08-17 | 张哲夫 | Preparation method and application of compound visible-light responding catalyst Ag2CO3/TiO2/M-ZIF-8 |
| CN107096556B (en) * | 2017-03-13 | 2019-12-06 | 中国科学院化学研究所 | preparation method of visible light response TiO2 precursor, TiO2 precursor and catalyst |
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| CN107552079A (en) * | 2017-08-16 | 2018-01-09 | 同济大学 | A kind of spongy loose structure titanium dioxide optical catalyst and its preparation and application |
| CN107552079B (en) * | 2017-08-16 | 2019-12-27 | 同济大学 | Titanium dioxide photocatalyst with spongy porous structure and preparation and application thereof |
| CN109019679A (en) * | 2018-09-10 | 2018-12-18 | 济南大学 | A kind of preparation method of mesoporous TiO 2 |
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| CN115318321A (en) * | 2022-07-18 | 2022-11-11 | 西安交通大学 | Preparation method of titanium dioxide/graphite phase carbon nitride nano composite material |
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Application publication date: 20110601 |