CN102489242B - Method for preparing titanium dioxide by integrating adsorption and photocatalysis - Google Patents
Method for preparing titanium dioxide by integrating adsorption and photocatalysis Download PDFInfo
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- CN102489242B CN102489242B CN 201110389743 CN201110389743A CN102489242B CN 102489242 B CN102489242 B CN 102489242B CN 201110389743 CN201110389743 CN 201110389743 CN 201110389743 A CN201110389743 A CN 201110389743A CN 102489242 B CN102489242 B CN 102489242B
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Abstract
The invention discloses a method for preparing titanium dioxide by integrating adsorption and photocatalysis, which is characterized in that dodecyl-2-pyridine-methylamine is taken as a template, performed hydro-thermal reaction under ethanol-water system condition, an ethanol-hydrochloric acid solution is used for extracting the template to obtain an intermediate, a water passivation method is used for processing to obtain the titanium dioxide by integrating adsorption and photocatalysis. Compared with current materials, the adsorption, catalysis and moisture resistance of the prepared material under high wind speed (short connection time) condition possess substantial superiority, the method of the invention possesses wide application prospect in the indoor air pollution treatment field.
Description
Technical field
The invention belongs to the photocatalysis technology field, relate in particular to the preparation method of the absorption-photocatalysis integrated titanium dioxide of gaseous organic pollutant in a kind of clean room.
Background technology
The health of the seriously polluted harm humans of light concentration gas such as room air pollution, its purification techniques are subjected to people and more and more pay close attention to.Light catalytic purifying is considered to an indoor air purification technology of tool application prospect, have can utilize that luminous energy, cost are low, nonhazardous and extensive advantage such as degradation of contaminant.But do not drop into practical application on this technological world as yet in a large number, China does not then have relevant product.This mainly is because there are several problems in this technology: when one, being applied to equipment such as clarifier or air-conditioning, because air quantity is very big, the time of contact of gaseous contamination molecule and catalysis material is very short, contaminant molecule becomes conditioning step by gas phase to the mass transfer of catalyst surface, thereby the efficient of common catalysis material purifying low-concentration pollutant is lower, does not reach requirement of actual application; Two, the purification efficiency of catalysis material can descend with the humidity increase, and part material catalytic efficiency when high humility descends very obvious.Our south and coastal area are generally moist, thereby photocatalysis technology is used in these areas and had restriction.The present invention prepares novel microporous material by the improvement of synthetic method, improves material than catalytic efficiency under the short contacting time condition and anti humility performance.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, the preparation method of a kind of absorption-photocatalysis integrated titanium dioxide is provided.
The objective of the invention is to be achieved through the following technical solutions: the preparation method of a kind of absorption-photocatalysis integrated titanium dioxide, this method may further comprise the steps:
(1) mixes the mixed liquor of winning with under dodecyl-2-pyridine-methylamine of volume ratio 1 ~ 4:50 and the absolute ethyl alcohol and stirring condition;
(2) be butyl titanate and the absolute ethyl alcohol mixing of 1 ~ 2:30 with volume ratio, get second mixed liquor;
(3) second mixed liquor with step 2 is added drop-wise in first mixed solution of step 1, gets the 3rd mixed liquor, and the volume ratio of second mixed liquor and first mixed solution is 1:0.5 ~ 2;
(4) add entry in the 3rd mixed liquor that step 3 obtains under stirring, the volume ratio of water and the 3rd mixed liquor is 1 ~ 3:3, obtains the 4th mixed liquor after stirring 2 h;
(5) the 4th mixed solution that step 4 is obtained adds the reactor of tool tetrafluoro inner bag, and 80 ℃ of hydro-thermal reaction 24 h and centrifugal obtain first solid;
(6) solid that step 5 is won is joined in the absolute ethyl alcohol, ethanol and solid masses are regulated pH to 3 ~ 4 than 10 ~ 250:1 with concentrated hydrochloric acid, stir (or vibration) 1 ~ 4 h, and be centrifugal, second solid;
(7) operation 3 times of repeating step 6 again obtains material intermediate (TiO
2-P);
(8) material intermediate that step 7 is obtained adds in the entry, and intermediate is 1:1 ~ 250 with the water quality ratio, stirs (or vibration) 1 ~ 60 min, and is centrifugal; Repeat this step and be 6 ~ 8 until pH value of solution, centrifugal, natural air drying or 40 ~ 100 ℃ are dried to such an extent that have a highly active titanic oxide material (TiO
2-W).
The invention has the beneficial effects as follows:
1, The present invention be directed to the actual requirement of light concentration gas removing pollutants such as room air, exploitation can be in the titanium dioxide synthetic method than short contacting time efficient degradation pollutant.With the cyclohexanone is the purifying property that indoor air pollutants is represented evaluating material, the result show synthetic material under low time of contact condition (0.036 ~ 0.07 s) than current material having clear superiority aspect absorption and the photocatalysis performance, show moisture resistance preferably simultaneously.
2, the material that synthesizes of the present invention can be applicable to indoor air purification, and for example: with the material is that core prepares clean air package, is installed on air purifier, can effectively remove as the pollutant of generations such as finishing, smoking or kills airborne germ; Be installed on air-conditioning equipment, then can be implemented in and remove indoor pollutant or germ in the process of Air conditioner air exchange, effectively reduce because the indoor healthy risk that new wind deficiency is caused; Material preparation is become coating, can realize long-term adsorption cleaning being pollutant in the room air.This material field of employment is extensive, and, hospital indoor as the resident, school and factory etc. are with a wide range of applications in the light concentration gas field of purification.
Description of drawings
Fig. 1 is TiO
2-W electromicroscopic photograph;
Fig. 2 is XRD spectrum figure;
Fig. 3 is time of contact 0.036 P25, TiO when s, humidity 20%
2-P and TiO
2-W is to the absorption spirogram of cyclohexanone;
Fig. 4 is P25, TiO under humidity 20%, difference condition time of contact
2-P and TiO
2-W is to the removal rate diagram of cyclohexanone;
Fig. 5 is P25, TiO under time of contact 0.036 s, the different humidity condition
2-P and TiO
2-W is to the removal rate diagram of cyclohexanone.
The specific embodiment
The preparation method of the present invention's absorption-photocatalysis integrated titanium dioxide may further comprise the steps:
1, mixes the mixed liquor of winning with under dodecyl-2-pyridine-methylamine of volume ratio 1 ~ 4:50 and the absolute ethyl alcohol and stirring condition;
2, be butyl titanate and the absolute ethyl alcohol mixing of 1 ~ 2:30 with volume ratio, get second mixed liquor;
3, second mixed liquor with step 2 is added drop-wise in first mixed solution of step 1, gets the 3rd mixed liquor, and the volume ratio of second mixed liquor and first mixed solution is 1:0.5 ~ 2;
4, add entry in the 3rd mixed liquor that step 3 obtains under stirring, the volume ratio of water and the 3rd mixed liquor is 1 ~ 3:3, obtains the 4th mixed liquor after stirring 2 h;
5, the 4th mixed solution that step 4 is obtained adds the reactor of tool tetrafluoro inner bag, and 80 ℃ of hydro-thermal reaction 24 h and centrifugal obtain first solid;
6, solid that step 5 is won is joined in the absolute ethyl alcohol, ethanol and solid masses are regulated pH to 3 ~ 4 than 10 ~ 250:1 with concentrated hydrochloric acid, stir (or vibration) 1 ~ 4 h, and be centrifugal, second solid;
7, the operation 3 times of repeating step 6 again obtains material intermediate (TiO
2-P);
8, the material intermediate that step 7 is obtained adds in the entry, intermediate is 1:1 ~ 250 with the water quality ratio, stir (or vibration) 1 ~ 60 min, centrifugal, repeating as preceding washing operation is 6 ~ 8 until pH value of solution, centrifugal, natural air drying or 40 ~ 100 ℃ are dried to such an extent that have a highly active titanic oxide material (TiO
2-W).
Unique micropore result of the titanic oxide material that the present invention synthesizes makes material obtain stronger adsorption capacity, has strengthened pollutant from the mass transfer of gas phase to catalyst surface, and then has improved catalytic efficiency.The material of the present invention's preparation is all having obvious lifting than the relative existing product effect with catalytic effect of the adsorbance under the short contacting time condition, and anti humility performance significantly is better than current material simultaneously.
Describe the present invention in detail with embodiment with reference to the accompanying drawings below, it is more obvious that purpose of the present invention and effect will become.
Embodiment 1:
1, mixes the mixed liquor of winning with under dodecyl-2-pyridine-methylamine of volume ratio 2:50 and the absolute ethyl alcohol and stirring condition;
2, be butyl titanate and the absolute ethyl alcohol mixing of 1:30 with volume ratio, get second mixed liquor;
3, second mixed liquor with step 2 is added drop-wise in first mixed solution of step 1, gets the 3rd mixed liquor, and the volume ratio of second mixed liquor and first mixed solution is 1:1;
4, add entry in the 3rd mixed liquor that step 3 obtains under stirring, the volume ratio of water and the 3rd mixed liquor is 1:3, obtains the 4th mixed liquor after stirring 2 h;
5, the 4th mixed solution that step 4 is obtained adds the reactor of tool tetrafluoro inner bag, and 80 ℃ of hydro-thermal reaction 24 h and centrifugal obtain first solid;
6, solid that step 5 is won is joined in the absolute ethyl alcohol, ethanol and solid masses are regulated pH to 3 ~ 4 than 50:1 with concentrated hydrochloric acid, stir (or vibration) 4 h, and be centrifugal, second solid;
7, the operation 3 times of repeating step 6 again obtains material intermediate (TiO
2-P);
8, getting 600 μ l dodecyl-2-pyridine-methylamines joins in the 30 ml absolute ethyl alcohols, 1.7 the ml butyl titanate is dissolved in 30 ml absolute ethyl alcohols, slowly is added drop-wise in the ethanolic solution of dodecyl-2-pyridine-methyl amine, adds 20 ml ultra-pure waters, stir 2 h, move into tetrafluoro inner bag hydrothermal reaction kettle, 80 ℃ of hydro-thermal reaction 24 h, cooling and centrifugal naturally, the gained solid disperses with 250 ml absolute ethyl alcohols, regulating pH with concentrated hydrochloric acid is 3, stirs 4 h, centrifugal, repeat again with ethanol-HCl rinse 3 times, centrifugal, the gained solid dispersed stirs 10 min in 250 ml ultra-pure waters, centrifugal, repeat the ultra-pure water rinse and be 7 until pH value of solution, centrifugal, 60 ℃ of oven dry promptly.
As mentioned above, make material structure as Fig. 1,2 and table 1 shown in, TiO
2The aperture of-W broadens, and specific surface significantly reduces, and compares TiO simultaneously
2The impalpable structure of-P, TiO
2-W has produced the crystalline structure of part anatase.Under humidity 20% condition, material to the adsorbance of cyclohexanone as shown in Figure 3, TiO
2-W〉TiO
2-P〉P25.Catalytic performance result under different times of contact and the humidity shown in Fig. 4,5, under low time of contact and high humidity, TiO
2-W compares P25 and TiO
2There is clear superiority in-P.
Table 1: the specific area of material, aperture and micro pore volume
Embodiment 2:
Step 1-7 is identical with embodiment 1, step 8 is as follows: get 600 μ l dodecyl-2-pyridine-methylamines and join in the 30 ml absolute ethyl alcohols, 1.7 the ml butyl titanate is dissolved in 30 ml absolute ethyl alcohols, slowly be added drop-wise in the ethanolic solution of dodecyl-2-pyridine-methylamine, add 20 ml ultra-pure waters, stir 2 h, move into tool tetrafluoro inner bag hydrothermal reaction kettle, 80 ℃ of hydro-thermal reaction 24 h, naturally cooling and centrifugal, the gained solid disperses with 250 ml absolute ethyl alcohols, and regulating pH with concentrated hydrochloric acid is 3,4 h vibrate, centrifugal, repeat again with ethanol-HCl rinse 3 times, centrifugal, the gained solid dispersed is in 50 ml ultra-pure waters, stir 30 min, centrifugal, repeating the ultra-pure water rinse is 7 until pH value of solution, centrifugal, 60 ℃ of oven dry promptly.
Embodiment 3:
Step 1-7 is identical with embodiment 1, step 8 is as follows: get 600 μ l dodecyl-2-pyridine-methylamines and join in the 30 ml absolute ethyl alcohols, 1.7 the ml butyl titanate is dissolved in 30 ml absolute ethyl alcohols, slowly be added drop-wise in the ethanolic solution of dodecyl-2-pyridine-methyl amine, add 20 ml ultra-pure waters, stir 2 h, move into tool tetrafluoro inner bag hydrothermal reaction kettle, 80 ℃ of hydro-thermal reaction 24 h, naturally cooling and centrifugal, the gained solid disperses with 250 ml absolute ethyl alcohols, and regulating pH with concentrated hydrochloric acid is 3, stir 4 h, centrifugal, repeat again with ethanol-HCl rinse 3 times, centrifugal, the gained solid dispersed is in 250 ml ultra-pure waters, stir 60 min, centrifugal, repeating the ultra-pure water rinse is 7 until pH value of solution, centrifugal, 70 ℃ of oven dry promptly.
Embodiment 4:
Step 1-7 is identical with embodiment 1, step 8 is as follows: get 600 μ l dodecyl-2-pyridine-methylamines and join in the 30 ml absolute ethyl alcohols, 1.7 the ml butyl titanate is dissolved in 30 ml absolute ethyl alcohols, slowly be added drop-wise in the ethanolic solution of dodecyl-2-pyridine-methyl amine, add 20 ml ultra-pure waters, stir 2 h, move into tool tetrafluoro inner bag hydrothermal reaction kettle, 80 ℃ of hydro-thermal reaction 24 h, naturally cooling and centrifugal, the gained solid disperses with 250 ml absolute ethyl alcohols, and regulating pH with concentrated hydrochloric acid is 3, stir 4 h, centrifugal, repeat again with ethanol-HCl rinse 3 times, centrifugal, the gained solid dispersed is in 150 ml ultra-pure waters, stir 10 min, centrifugal, repeating the ultra-pure water rinse is 6 until pH value of solution, centrifugal, 60 ℃ of oven dry promptly.
Embodiment 5:
Step 1-7 is identical with embodiment 1, step 8 is as follows: get 600 μ l dodecyl-2-pyridine-methylamines and join in the 30 ml absolute ethyl alcohols, 1.7 the ml butyl titanate is dissolved in 30 ml absolute ethyl alcohols, slowly be added drop-wise in the ethanolic solution of dodecyl-2-pyridine-methyl amine, add 20 ml ultra-pure waters, stir 2 h, move into tool tetrafluoro inner bag hydrothermal reaction kettle, 80 ℃ of hydro-thermal reaction 24 h, naturally cooling and centrifugal, the gained solid disperses with 250 ml absolute ethyl alcohols, and regulating pH with concentrated hydrochloric acid is 3, stir 4 h, centrifugal, repeat again with ethanol-HCl rinse 3 times, centrifugal, the gained solid dispersed is in 50 ml ultra-pure waters, stir 50 min, centrifugal, repeating the ultra-pure water rinse is 7 until pH value of solution, centrifugal, 100 ℃ of oven dry promptly.
Embodiment 6:
Step 1-7 is identical with embodiment 1, and step 8 is as follows: with the cyclohexanone is the representative of indoor air pollutants, has tested micropore titanium dioxide (TiO of the present invention
2-W) to the adsorption capacity of gaseous contaminant cyclohexanone, and with P25 and TiO
2-P relatively.The initial concentration of cyclohexanone is 1 mg/m
3Material therefor is prepared among the embodiment 1, and service property (quality) is 10 mg, and reactor adopts the fixed-bed type dynamic response device of unidirectional ventilation.Be 0.036 s time of contact, and humidity is 20% o'clock, every gram TiO
2-W, TiO
2The adsorbance of-P and P25 is respectively 21.0 mg, 16.1 mg and 3.9 mg.
Embodiment 7:
Step 1-7 is identical with embodiment 1, and step 8 is as follows: with the cyclohexanone is the representative of indoor air pollutants, has tested micropore titanium dioxide (TiO of the present invention
2-W) to the photocatalysis effect of gaseous contaminant cyclohexanone, and with P25 and TiO
2-P effect relatively.The initial concentration of cyclohexanone is about 1 mg/m
3Using wavelength is that 310 nm uviol lamps are as light source.Material therefor is prepared among the embodiment 1, and service property (quality) is 10 mg, and reactor adopts the fixed-bed type dynamic response device of unidirectional ventilation.Be 0.036 s time of contact, and humidity is 20% o'clock, TiO
2-W, TiO
2-P and P25 cyclohexanone clearance are respectively 69.4%, 63.2% and 57.7%.
Embodiment 8:
Step 1-7 is identical with embodiment 1, and step 8 is as follows: with the cyclohexanone is the representative of indoor air pollutants, has tested micropore titanium dioxide (TiO of the present invention
2-W) to the photocatalysis effect of gaseous contaminant cyclohexanone, and with P25 and TiO
2-P effect relatively.The initial concentration of cyclohexanone is about 1 mg/m
3Using wavelength is that 310 nm uviol lamps are as light source.Material therefor is prepared among the embodiment 1, and service property (quality) is 10 mg, and reactor adopts the fixed-bed type dynamic response device of unidirectional ventilation.Be 0.036 s time of contact, and humidity is 60% o'clock, TiO
2-W, TiO
2-P and P25 cyclohexanone clearance are respectively 64.3%, 34.7% and 52.6%.
Above embodiment only is described further invention, and scope of the present invention is not limited to by illustrated embodiment.
Claims (1)
1. the preparation method of absorption-photocatalysis integrated titanium dioxide is characterized in that, this method may further comprise the steps:
(1) mixes the mixed liquor of winning with under dodecyl-2-pyridine-methylamine of volume ratio 1 ~ 4:50 and the absolute ethyl alcohol and stirring condition;
(2) be butyl titanate and the absolute ethyl alcohol mixing of 1 ~ 2:30 with volume ratio, get second mixed liquor;
(3) second mixed liquor with step (2) is added drop-wise in first mixed solution of step (1), gets the 3rd mixed liquor, and the volume ratio of second mixed liquor and first mixed solution is 1:0.5 ~ 2;
(4) add entry in the 3rd mixed liquor that step (3) obtains under stirring, the volume ratio of water and the 3rd mixed liquor is 1 ~ 3:3, obtains the 4th mixed liquor after stirring 2 h;
(5) the 4th mixed solution that step (4) is obtained adds the reactor of tool tetrafluoro inner bag, and 80 ℃ of hydro-thermal reaction 24h and centrifugal obtain first solid;
(6) step (5) solid of winning is joined in the absolute ethyl alcohol, ethanol and solid masses are regulated pH to 3 ~ 4 than 10 ~ 250:1 with concentrated hydrochloric acid, stir or 1 ~ 4 h that vibrates, and be centrifugal, second solid;
(7) operation 3 times of repeating step (6) again obtains material intermediate TiO
2-P;
(8) material intermediate that step (7) is obtained adds in the entry, and intermediate is 1:1 ~ 250 with the water quality ratio, stirs or 1 ~ 60 min that vibrates, and is centrifugal; Repeat this step and be 6 ~ 8 until pH value of solution, centrifugal, natural air drying or 40 ~ 100 ℃ are dried to such an extent that have a highly active titanic oxide material TiO
2-W.
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| CN103657620B (en) * | 2013-11-19 | 2015-09-30 | 浙江大学 | A kind of anatase titanium dioxide microporous titania materials preparation method purified the air of a room |
| CN105502484B (en) * | 2015-11-26 | 2017-03-22 | 江南大学 | Preparation method of titanium dioxide composite material for absorption enhanced visible light catalysis of low-concentration VOCs |
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|---|---|---|---|---|
| CN101104525A (en) * | 2007-08-06 | 2008-01-16 | 浙江大学 | Method for preparing anatase type bentonite-base porous titanium dioxide nano material |
| CN101244381A (en) * | 2008-03-07 | 2008-08-20 | 东南大学 | Process for producing TiO2-Al2O3composite nano-powder body material |
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| KR100564136B1 (en) * | 2003-09-19 | 2006-03-27 | 주식회사 나노 | Method for producing titanium oxide particle and method for producing titanium oxide thin layer using the same |
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| CN101104525A (en) * | 2007-08-06 | 2008-01-16 | 浙江大学 | Method for preparing anatase type bentonite-base porous titanium dioxide nano material |
| CN101244381A (en) * | 2008-03-07 | 2008-08-20 | 东南大学 | Process for producing TiO2-Al2O3composite nano-powder body material |
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