CN102211033A - Method for preparing platinum and nitrogen codoped active carbon supported titanium dioxide photocatalyst - Google Patents
Method for preparing platinum and nitrogen codoped active carbon supported titanium dioxide photocatalyst Download PDFInfo
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- CN102211033A CN102211033A CN2011100939270A CN201110093927A CN102211033A CN 102211033 A CN102211033 A CN 102211033A CN 2011100939270 A CN2011100939270 A CN 2011100939270A CN 201110093927 A CN201110093927 A CN 201110093927A CN 102211033 A CN102211033 A CN 102211033A
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Abstract
The invention discloses a method for preparing a platinum and nitrogen codoped active carbon supported titanium dioxide photocatalyst, which comprises the following steps of: adding tetrabutyl titanate into absolute ethanol, stirring for a period of time, slowing dripping into distilled water, adding acetylacetone and polyethylene glycol, regulating a pH value, and strongly stirring for complete hydrolysis to obtain a clear and transparent sol; adding urea with stirring, reacting, adding treated active carbon, continuously stirring, and performing ultrasonic dispersion, standing, filtration, washing, drying and roasting to obtain a nitrogen-doped active carbon supported TiO2 photocatalyst; immersing the nitrogen-doped active carbon supported TiO2 photocatalyst in a chloroplatinic acid solution, adding sodium borohydride for reduction, and drying to obtain a platinum and nitrogen codoped active carbon supported titanium dioxide photocatalyst. The invention solves the problem that a titanium dioxide catalyst in a suspension system is difficult to recover, the photocatalytic efficiency of the platinum and nitrogen codoped active carbon supported titanium dioxide photocatalyst on a liquid phase dye is further improved, and the platinum and nitrogen codoped active carbon supported titanium dioxide photocatalyst has stronger response under the condition of visible light.
Description
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Technical field
The invention belongs to activated carbon supported type catalyst preparation technical field, relate generally to the preparation method that loaded photocatalyst is used in a kind of visible light-responded liquid dyes decolouring.
Background technology
Semiconductor TiO
2Be to use maximum photochemical catalysts at present, have nontoxic, cheap, steady performance.Yet, TiO
2Be broadband semiconductor, only just have catalytic activity taking up an area of under 3%～4% the ultraviolet light of ball surface sunshine, simultaneously, TiO
2Have powder in, the suspension system low to the low concentration pollutant catalytic activity again and very easily reunite and be difficult for shortcoming such as recovery, these shortcomings have all limited TiO
2Practical application.If with TiO
2Load on the porous carrier, can play absorption and act synergistically mutually, realize that target contaminant is at TiO with catalytic oxidation
2Enrichment on every side improves photocatalysis efficiency, has also solved the problem that reclaims difficulty simultaneously.
Can improve TiO by doped metal ion or nonmetallic ion
2Photocatalytic activity, the doping of some metal ion and non-metallic atom can make TiO by changing energy gap
2Under visible light, show certain photocatalytic activity.At present, to activated carbon supported TiO
2The ion doping structure of system has more research in gas phase degraded field, also fails to solve visible light catalytic problem, the shortcoming that the ubiquity catalytic activity is low in the liquid phase field of polluting.
Summary of the invention
In order to solve the activated carbon supported TiO that prior art exists
2The ion doping structure of system is polluted the low problem of field catalytic activity in liquid phase, the invention provides the preparation method of a kind of platinum, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst, the active carbon for preparing has good catalytic effect at visible light, can be applied to the liquid-phase catalysis field.
Technical scheme of the present invention is: the preparation method of a kind of platinum, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst, and step is:
Butyl titanate is added in the absolute ethyl alcohol, splash in the distilled water after stirring, adding acetylacetone,2,4-pentanedione and polyethylene glycol then and regulating the pH value is 2～3, and strong agitation gets clear colloidal sol fully until hydrolysis; Under agitation add urea, reaction back adds through washing, oven dry back active carbon continues to stir, then through after the ultrasonic dispersion through the leaving standstill of routine, filter, wash, obtain the activated carbon supported type TiO that nitrogen mixes behind dry, the calcination steps
2Photochemical catalyst; Activated carbon supported type TiO with the nitrogen doping
2Photochemical catalyst is dried behind the adding sodium borohydride reduction after flooding with platinum acid chloride solution by equi-volume impregnating, obtains platinum, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst.
According to the volume ratio butyl titanate: absolute ethyl alcohol: distilled water: acetylacetone,2,4-pentanedione: polyethylene glycol=12.5:45:100:10:2, quality is than butyl titanate: the ratio of urea=1.6 adds raw material.
The amount of used active carbon is according to butyl titanate: active carbon=1.3(mass ratio).
Sintering temperature is 400～600 ℃.
Time of repose is 24 h.
Beneficial effect:
1. employing sol-gel process realizes Pt/N/TiO by codope
2Load on active carbon, the preparation loaded photocatalyst has improved the photocatalytic degradation rate, has solved and has reclaimed difficult problem, simultaneously visible light is had a provisioning response, can good degradation effect be arranged to the liquid phase methylene blue dye under visible light.。
2. this preparation method is easy to operate, and equipment is simple, is easy to promote.
Description of drawings
Fig. 1 is methylene blue solution photocatalytic degradation reaction unit figure of the present invention.
Wherein: 1 air intake, 2 condensing water inlets, 3 light sources, 4 magnetic stirring apparatus, 5 condensation-water drains, 6 sample taps, 7 gas vents, 8 methylene blue solutions
Fig. 2 is the XRD figure of the catalyst for preparing of the present invention.
Fig. 3 is the SEM figure of the catalyst for preparing of the present invention.
Fig. 4 Pt/N/TiO
2Ultraviolet-visible absorption spectroscopy figure.
Fig. 5 is that the catalyst for preparing of the present invention is to methylene blue solution degradation rate figure.
The specific embodiment
The invention provides a kind of visible light-responded liquid dyes decolouring platinum, the preparation method of nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst, to solve the problem that the liquid phase photocatalysis efficiency is low and photochemical catalyst reclaims, concrete steps are as follows:
1) 12.5 mL butyl titanates is joined in the 45 mL absolute ethyl alcohols, under vigorous stirring, slowly splash in the 100mL distilled water, add the 10mL acetylacetone,2,4-pentanedione simultaneously with timely 2mL polyethylene glycol, and to be adjusted to pH with the hydrochloric acid of 1mol/L be 2.0-3.0, strong agitation 2h makes hydrolysis complete, gets the colloidal solution of clear;
2) with 1) in the TiO that makes
2Colloidal sol adds urea 7.6g under magnetic agitation, add through the active carbon after washing, the oven dry behind the reaction 30min and continue to stir 1h, ultrasonic 20 min, filter after leaving standstill 24h, with absolute ethyl alcohol and deionized water washing several, with the dry 2h under 120 ℃ of the active carbon after the load,, obtain the activated carbon supported type TiO of different nitrogen dopings by the control sintering temperature then in 400～600 ℃ of following roasting 2h
2Photochemical catalyst;
3) nano-TiO that nitrogen is mixed
2Behind equi-volume impregnating usefulness platinum acid chloride solution (5g/L) dipping, add sodium borohydride reduction, dry behind the certain hour, obtain platinum, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst.
Under the visible light condition, in liquid phase photocatalytic reaction device as shown in Figure 1, degradation of methylene blue solution calculates degradation rate to investigate the photocatalysis performance of obtained catalyst by solution absorbance before and after the reaction.The jacketed reactor for ultraviolet catalytic reaction usefulness is identical on the used liquid phase photocatalytic reaction device surface structure with on the market, but inner bag adopts filter uviol material, in addition, adopt 350W xenon lamp effect light source, therefore on the basis of traditional jacketed reactor, in place light source the glass tube bottom set up an air intake to carry the heat that light source produces.During the experiment beginning, open magnetic stirring apparatus earlier, make catalyst behind pre-absorption 1h under the lucifuge condition, open condensation water and air pump, open light source then and carry out light-catalyzed reaction.
Fig. 2 is the XRD figure of the catalyst for preparing of the present invention, and it the obvious diffraction peak occurs near 25 °, illustrate that the photochemical catalyst crystal formation that makes is a Detitanium-ore-type;
Fig. 3 is the SEM figure of the catalyst for preparing of the present invention, as can be seen from Figure, and nano-TiO
2Present distribution more uniformly on the surface of active carbon;
Fig. 4 is Pt/N/TiO
2Ultraviolet-visible absorption spectroscopy figure, as seen from the figure, platinum, nitrogen co-doped nano-TiO
2Still at ultraviolet region good absorption is arranged, simultaneously at the more single TiO of visible region
2Also show tangible absorption, this also is preparation-obtained catalyst has a provisioning response to visible light a immediate cause;
Fig. 5 is the degradation rate figure of the catalyst for preparing of the present invention to methylene blue solution, experiment showed, when the methylene blue solution initial concentration be 10mg/L, after 6 h were carried out in light-catalyzed reaction, degradation rate can reach 94%.
Embodiment 1:
12.5 mL butyl titanates are joined in the 45 mL absolute ethyl alcohols, under vigorous stirring, slowly drip in the people 100mL distilled water, add the 10mL acetylacetone,2,4-pentanedione simultaneously with timely 2mL polyethylene glycol, and to be adjusted to pH with the hydrochloric acid of 1mol/L be 2.0-3.0, strong agitation 2h makes hydrolysis complete, gets the colloidal sol of clear.Then add 6-10 purpose granular active carbon 9.6 g, add urea 7.6g simultaneously, ultrasonic 20 min behind the stirring 1h steep 24h only, filter, with absolute ethyl alcohol and deionized water washing several.With the dry 2h under 120 ℃ of the active carbon after the load, obtain the activated carbon supported type nano-TiO that nitrogen mixes in 400 ℃ of following roasting 2h
2Activated carbon supported type nano-TiO with the nitrogen doping
2By equi-volume impregnating with chloroplatinic acid (is 1% to take by weighing according to Pt mass fraction in catalyst) solution impregnation after, add sodium borohydride reduction, obtain platinum, nitrogen co-doped nano-TiO behind the certain hour
2Obtain platinum, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst, the gained photochemical catalyst is 75.7% to the photocatalytic degradation rate of methylene blue solution.
Embodiment 2:
12.5 mL butyl titanates are joined in the 45 mL absolute ethyl alcohols, under vigorous stirring, slowly drip in the people 100mL distilled water, add the 10mL acetylacetone,2,4-pentanedione simultaneously with timely 2mL polyethylene glycol, and to be adjusted to pH with the hydrochloric acid of 1mol/L be 2.0-3.0, strong agitation 2h makes hydrolysis complete, gets the colloidal sol of clear.Then add 6-10 purpose granular active carbon 9.6 g, add urea 7.6g simultaneously, ultrasonic 20 min behind the stirring 1h steep 24h only, filter, with absolute ethyl alcohol and deionized water washing several.With the dry 2h under 120 ℃ of the active carbon after the load, obtain the activated carbon supported type nano-TiO that nitrogen mixes in 450 ℃ of following roasting 2h
2Activated carbon supported type nano-TiO with the nitrogen doping
2By equi-volume impregnating with chloroplatinic acid (is 1% to take by weighing according to Pt mass fraction in catalyst) solution impregnation after, add sodium borohydride reduction, obtain platinum, nitrogen co-doped nano-TiO behind the certain hour
2Obtain platinum, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst, the gained photochemical catalyst is 94.1% to the photocatalytic degradation rate of methylene blue solution.
Embodiment 3:
12.5 mL butyl titanates are joined in the 45 mL absolute ethyl alcohols, under vigorous stirring, slowly drip in the people 100mL distilled water, add the 10mL acetylacetone,2,4-pentanedione simultaneously with timely 2mL polyethylene glycol, and to be adjusted to pH with the hydrochloric acid of 1mol/L be 2.0-3.0, strong agitation 2h makes hydrolysis complete, gets the colloidal sol of clear.Then add 6-10 purpose granular active carbon 9.6 g, add urea 7.6g simultaneously, ultrasonic 20 min behind the stirring 1h steep 24h only, filter, with absolute ethyl alcohol and deionized water washing several.With the dry 2h under 120 ℃ of the active carbon after the load, obtain the activated carbon supported type nano-TiO that nitrogen mixes in 500 ℃ of following roasting 2h
2Activated carbon supported type nano-TiO with the nitrogen doping
2By equi-volume impregnating with chloroplatinic acid (is 1% to take by weighing according to Pt mass fraction in catalyst) solution impregnation after, add sodium borohydride reduction, obtain platinum, nitrogen co-doped nano-TiO behind the certain hour
2Obtain platinum, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst, the gained photochemical catalyst is 90.4% to the photocatalytic degradation rate of methylene blue solution.
Embodiment 4:
12.5 mL butyl titanates are joined in the 45 mL absolute ethyl alcohols, under vigorous stirring, slowly drip in the people 100mL distilled water, add the 10mL acetylacetone,2,4-pentanedione simultaneously with timely 2mL polyethylene glycol, and to be adjusted to pH with the hydrochloric acid of 1mol/L be 2.0-3.0, strong agitation 2h makes hydrolysis complete, gets the colloidal sol of clear.Then add 6-10 purpose granular active carbon 9.6 g, add urea 7.6g simultaneously, ultrasonic 20 min behind the stirring 1h steep 24h only, filter, with absolute ethyl alcohol and deionized water washing several.With the dry 2h under 120 ℃ of the active carbon after the load, obtain the activated carbon supported type nano-TiO that nitrogen mixes in 550 ℃ of following roasting 2h
2Activated carbon supported type nano-TiO with the nitrogen doping
2By equi-volume impregnating with chloroplatinic acid (is 1% to take by weighing according to Pt mass fraction in catalyst) solution impregnation after, add sodium borohydride reduction, obtain platinum, nitrogen co-doped nano-TiO behind the certain hour
2Obtain platinum, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst, the gained photochemical catalyst is 57.7% to the photocatalytic degradation rate of methylene blue solution.
Embodiment 5:
12.5 mL butyl titanates are joined in the 45 mL absolute ethyl alcohols, under vigorous stirring, slowly drip in the people 100mL distilled water, add the 10mL acetylacetone,2,4-pentanedione simultaneously with timely 2mL polyethylene glycol, and to be adjusted to pH with the hydrochloric acid of 1mol/L be 2.0-3.0, strong agitation 2h makes hydrolysis complete, gets the colloidal sol of clear.Then add 6-10 purpose granular active carbon 9.6 g, add urea 7.6g simultaneously, ultrasonic 20 min behind the stirring 1h steep 24h only, filter, with absolute ethyl alcohol and deionized water washing several.With the dry 2h under 120 ℃ of the active carbon after the load, obtain the activated carbon supported type nano-TiO that nitrogen mixes in 450 ℃ of following roasting 2h
2Activated carbon supported type nano-TiO with the nitrogen doping
2By equi-volume impregnating with chloroplatinic acid (is 0.5% to take by weighing according to Pt mass fraction in catalyst) solution impregnation after, add sodium borohydride reduction, obtain platinum, nitrogen co-doped nano-TiO behind the certain hour
2Obtain platinum, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst, the gained photochemical catalyst is 82.2% to the photocatalytic degradation rate of methylene blue solution.
Claims (5)
1. the preparation method of a platinum, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst is characterized in that step is:
Butyl titanate is added in the absolute ethyl alcohol, splash in the distilled water after stirring, adding acetylacetone,2,4-pentanedione and polyethylene glycol then and regulating the pH value is 2～3, and strong agitation gets clear colloidal sol fully until hydrolysis; Under agitation add urea, reaction back adds through washing, oven dry back active carbon continues to stir, then through after the ultrasonic dispersion through the leaving standstill of routine, filter, wash, obtain the activated carbon supported type TiO that nitrogen mixes behind dry, the calcination steps
2Photochemical catalyst; Activated carbon supported type TiO with the nitrogen doping
2Photochemical catalyst is dried behind the adding sodium borohydride reduction after flooding with platinum acid chloride solution by equi-volume impregnating, obtains platinum, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst.
2. the preparation method of platinum as claimed in claim 1, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst, it is characterized in that, according to the volume ratio butyl titanate: absolute ethyl alcohol: distilled water: acetylacetone,2,4-pentanedione: polyethylene glycol=12.5:45:100:10:2, quality is than butyl titanate: the ratio of urea=1.6 adds raw material.
3. the preparation method of platinum as claimed in claim 1, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst is characterized in that, the amount of used active carbon is according to butyl titanate: active carbon=1.3(mass ratio).
4. the preparation method of platinum as claimed in claim 1, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst is characterized in that, sintering temperature is 400～600 ℃.
5. the preparation method of platinum as claimed in claim 1, nitrogen co-doped activated carbon supported type titanium dioxide optical catalyst is characterized in that, time of repose is 24 h.
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| CN102989449A (en) * | 2012-11-30 | 2013-03-27 | 复旦大学 | Preparation method of C-Pt-codoped TiO2 nanometer material |
| CN103240110A (en) * | 2013-05-29 | 2013-08-14 | 福建省林业科学研究院 | Iron and nitrogen co-doping titanium dioxide/active carbon photocatalyst |
| CN104772140A (en) * | 2015-04-23 | 2015-07-15 | 于晓颖 | Suspension type preparation method of platinum doped titanium oxide membrane |
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| CN102989449B (en) * | 2012-11-30 | 2015-06-17 | 复旦大学 | Preparation method of C-Pt-codoped TiO2 nanometer material |
| CN103240110A (en) * | 2013-05-29 | 2013-08-14 | 福建省林业科学研究院 | Iron and nitrogen co-doping titanium dioxide/active carbon photocatalyst |
| CN103240110B (en) * | 2013-05-29 | 2015-03-25 | 福建省林业科学研究院 | Iron and nitrogen co-doping titanium dioxide/active carbon photocatalyst |
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| CN109569101B (en) * | 2018-12-10 | 2021-08-06 | 新昌县以琳环保科技有限公司 | Filter screen for air purifier and preparation method thereof |
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Application publication date: 20111012 |