CN103272588A - Recoverable float type Pt-TiO2/ floating bead photocatalyst and preparation method thereof - Google Patents
Recoverable float type Pt-TiO2/ floating bead photocatalyst and preparation method thereof Download PDFInfo
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- CN103272588A CN103272588A CN2013102320902A CN201310232090A CN103272588A CN 103272588 A CN103272588 A CN 103272588A CN 2013102320902 A CN2013102320902 A CN 2013102320902A CN 201310232090 A CN201310232090 A CN 201310232090A CN 103272588 A CN103272588 A CN 103272588A
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Abstract
The invention discloses a recoverable float type Pt-TiO2/ floating bead photocatalyst and a preparation method thereof. The carrier of the catalyst is regular cenosphere, and TiO2 with the deposition of Pt is loaded on in a film layer form. The preparation comprises the steps that at a room temperature, defined amount of distilled water is added into a butyl titanate and absolute ethyl alcohol mixed solution, and the mixture is stirred to form a TiO2 sol; the floating beads are taken as the carrier, a titanium dioxide film layer is loaded on the surface through a sol-gel method, and TiO2/ floating bead is prepared after drying and calcination; and TiO2/ floating bead is mixed with a chloroplatinic acid solution, and platinum is loaded to the surface of TiO2/ floating bead through a photodeposition method to obtain the photocatalyst. According to the recoverable float type Pt-TiO2/ floating bead photocatalyst and the preparation method thereof, the particle size of the carrier is adjustable, the thickness of the titanium dioxide layer is controllable, good photocatalytic activity is provided, UV-vis results prove that the photoresponse range is expanded to a visible region, so that conditions are created for photocatalytic degradation of pollutants by using sunlight in industry.
Description
Technical field
The present invention relates to field of photocatalytic material, be specifically related to a kind of callable float type Pt-TiO
2/ float the pearly-lustre Catalysts and its preparation method.
Background technology
In oxide semiconductor, Detitanium-ore-type TiO
2Photocatalytic activity be the strongest, be a kind of inexpensive, nontoxic, energy-conservation, material of organic pollution in the empty G﹠W of photocatalytic degradation efficiently.But because TiO
2Wideer band gap can only be by ultraviolet excitation, and only contains the ultraviolet ray about 4% in the solar spectrum, and this has just greatly limited its application in depollution of environment reality, thereby improves TiO
2The modification technology of photocatalysis performance has become the focus of research under visible light.It is to influence TiO by the electron distributions in the change system that platinum is modified
2Surface nature, and then improve light-catalyzed reaction efficient.Work as TiO
2When contacting with platinum, because the influence of Schottky barrier, the noble metal platinum of precipitation becomes effective trap of trapped electrons, can impel light induced electron to separate with the hole, thereby has improved the catalytic activity of photochemical catalyst.In addition, platinum is modified and can also be made catalyst that the response range of light is expanded to visible region, makes more solar energy obtain utilizing.But the TiO that in wastewater treatment process, relates to
2Mostly be nano-scale particle, reclaim difficulty, cause the waste of resource easily.
Floating pearl is a kind of cenosphere that can bubble through the water column in the flyash, and its chemical analysis has multiple functions such as particle is thin, the thin hollow of wall, quality is light, high-strength, wear-resisting, high temperature resistant, insulation is insulated, insulation is fire-retardant based on silica and alundum (Al.Float the good physical and chemical performance of pearl and provide good platform for its resource recycling that realizes refuse.Be that the composite photo-catalyst of preparing carriers can float on the water surface for a long time to float pearl, fully absorb luminous energy, its good adsorption performance also can improve the degradation efficiency of photochemical catalyst, and its recyclable and repeatedly recycling, has broad application prospects.
Summary of the invention
Technical problem solved by the invention provides a kind of float type Pt-TiO
2/ floating the pearly-lustre Catalysts and its preparation method, this catalyst diameter and titanium oxide film layer are all adjustable, can realize visible-light response type, can float on the water surface long period simultaneously, and are convenient to reclaim and repeatedly recycling.
A kind of callable float type Pt-TiO of the present invention
2/ float the pearly-lustre catalyst, it is characterized in that described carrier floats the cenosphere that pearl is rule, the TiO of deposition Pt
2With the form load of rete on it.Above-mentioned callable float type Pt-TiO
2/ float pearly-lustre Preparation of catalysts method, may further comprise the steps:
1) float the pearl preliminary treatment: will float pearl with rare nitric acid dousing 4h, and use the distilled water rinsing afterwards, and be neutral until the water that flows out, the oven dry back is standby;
2) be raw material with butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water, regulate its pH to 4 ~ 6 with red fuming nitric acid (RFNA), stirring is fully reacted it, add polyethylene glycol then, the mol ratio that makes butyl titanate and polyethylene glycol is 800 ~ 1200:1, heating and stirring make it abundant dissolving, namely obtain the TiO of yellow transparent
2Colloidal sol;
3) to TiO
2Add in the colloidal sol step 1) pretreated float bead carrier, making butyl titanate and the mass ratio that floats pearl is 5 ~ 10:1, stirring makes it to mix, filter behind dipping 12 ~ 36h, filtrate constant temperature is preserved, and the sample oven dry that leaches places Muffle furnace in 350 ℃ ~ 550 ℃ temperature lower calcination 2 ~ 4h again, be cooled to room temperature, thereby make the TiO of a load
2/ float pearl;
4) loading process repeatedly: the sample that obtains with above-mentioned step 3) is carrier, repeating step 2) and step 3), to make the TiO of secondary load
2/ float pearl; Repeat above-mentioned experiment, to finish repeatedly load;
5) with after the step 4) TiO that makes
2/ to float pearl to join in the platinum acid chloride solution and stir, chloroplatinic acid measures with platinum in the synthetic system, wherein platinum and TiO
2/ float contained TiO in the pearl
2Mass ratio is 1:1000 ~ 50, at last product is placed under the ultraviolet light to shine some hours, finally obtains callable float type Pt-TiO
2/ float the pearly-lustre catalyst.
Above-mentioned steps 2) mol ratio of butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water is 1:25:1:1 ~ 4.5 in.
The addition of floating bead carrier above-mentioned steps 3) is TiO
2Butyl titanate is 5 ~ 10:1 with the mass ratio that floats pearl in the colloidal sol.
Above-mentioned steps 4) TiO in
2/ load the number of times that floats pearl is 2 ~ 4 times.
Above-mentioned steps 5) light-struck time of medium ultraviolet is 12 ~ 18h.
The present invention compared with prior art has following advantage:
1, it is simple that the present invention has preparation, and cost is low, advantages of environment protection.
2, carrier of the present invention is for floating pearl, and is cheap and easy to get, can float on the long period on the water surface, easily accepts illumination, and is convenient to reclaim and can repeatedly reuse.
3, the present invention is visible-light-responsive photocatalyst, is conducive to the follow-up sunshine degradation of contaminant that utilizes in commercial Application; And traditional photochemical catalyst can only utilize ultraviolet light, and the present invention can reduce the commercial Application cost by contrast.
4, the present invention can prepare the photochemical catalyst of different-diameter by the adjustment to technical process, and the titanium dioxide film layer thickness is also adjustable, to satisfy different demands.
Description of drawings
Fig. 1 is callable float type Pt-TiO involved in the present invention
2/ float the sem photograph of pearly-lustre catalyst.As can be seen from Figure, Pt-TiO
2/ the profile of floating the pearly-lustre catalyst is the spherical of rule, floats bead surface and has formed rete, and rete distributes more even relatively, but the rete non-uniform phenomenon has also appearred in a few regions.
Fig. 2 is callable float type Pt-TiO involved in the present invention
2/ float pearly-lustre catalyst and unmodified TiO
2/ float the ultraviolet-visible absorption spectroscopy figure of pearl, as can be seen from the figure, Pt-TiO
2/ floating pearl compares TiO to the response intensity of light
2/ float pearl to be significantly improved, and the photoresponse scope has extended to visible region.
Specific embodimentEmbodiment 1
1) float the pearl preliminary treatment: that will extract from flyash floats pearl with 10% rare nitric acid dousing 4h, uses the distilled water rinsing afterwards, is neutral until the water that flows out, and the oven dry back is standby;
2) be raw material with butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water, the mol ratio of butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water is 1:25:1:4.5, regulate its pH to 4 with red fuming nitric acid (RFNA), stirring is fully reacted it, add Macrogol 2000 0 then, the mol ratio that makes butyl titanate and polyethylene glycol is 800:1, and heating and stirring make it abundant dissolving, namely obtain the TiO of yellow transparent
2Colloidal sol;
3) to TiO
2Add in the colloidal sol step 1) pretreated float bead carrier, making butyl titanate and the mass ratio that floats pearl is 5:1, stirring makes it to mix, filter behind the dipping 12h, filtrate constant temperature is preserved, and the sample oven dry that leaches places Muffle furnace in 350 ℃ of temperature lower calcination 2h again, be cooled to room temperature, thereby make the TiO of a load
2/ float pearl;
4) secondary load process: the sample that obtains with above-mentioned step 3) is carrier, repeating step 2) and step 3), to make the TiO of secondary load
2/ float pearl;
5) with after the step 4) TiO that makes
2/ to float pearl to join in the platinum acid chloride solution and stir, chloroplatinic acid measures with platinum in the synthetic system, wherein platinum and TiO
2/ float contained TiO in the pearl
2Mass ratio is 1:1000, product is placed under the ultraviolet light shine 12h at last, finally obtains callable float type Pt-TiO
2/ float the pearly-lustre catalyst.
Embodiment 2
1) float the pearl preliminary treatment: that will extract from flyash floats pearl with 10% rare nitric acid dousing 4h, uses the distilled water rinsing afterwards, is neutral until the water that flows out, and the oven dry back is standby;
2) be raw material with butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water, the mol ratio of butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water is 1:25:1:3, regulate its pH to 5 with red fuming nitric acid (RFNA), stirring is fully reacted it, add Macrogol 2000 0 then, the mol ratio that makes butyl titanate and polyethylene glycol is 800:1, and heating and stirring make it abundant dissolving, namely obtain the TiO of yellow transparent
2Colloidal sol;
3) to TiO
2Add in the colloidal sol step 1) pretreated float bead carrier, making butyl titanate and the mass ratio that floats pearl is 7:1, stirring makes it to mix, filter behind the dipping 12h, filtrate constant temperature is preserved, and the sample oven dry that leaches places Muffle furnace in 450 ℃ of temperature lower calcination 2h again, be cooled to room temperature, thereby make the TiO of a load
2/ float pearl;
4) secondary load process: the sample that obtains with above-mentioned step 3) is carrier, repeating step 2) and step 3), to make the TiO of secondary load
2/ float pearl;
5) with after the step 4) TiO that makes
2/ to float pearl to join in the platinum acid chloride solution and stir, chloroplatinic acid measures with platinum in the synthetic system, wherein platinum and TiO
2/ float contained TiO in the pearl
2Mass ratio is 1:200, product is placed under the ultraviolet light shine 12h at last, finally obtains callable float type Pt-TiO
2/ float the pearly-lustre catalyst.
Embodiment 3
1) float the pearl preliminary treatment: that will extract from flyash floats pearl with 10% rare nitric acid dousing 4h, uses the distilled water rinsing afterwards, is neutral until the water that flows out, and the oven dry back is standby;
2) be raw material with butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water, the mol ratio of butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water is 1:25:1:2, regulate its pH to 6 with red fuming nitric acid (RFNA), stirring is fully reacted it, add Macrogol 2000 0 then, the mol ratio that makes butyl titanate and polyethylene glycol is 1000:1, and heating and stirring make it abundant dissolving, namely obtain the TiO of yellow transparent
2Colloidal sol;
3) to TiO
2Add in the colloidal sol step 1) pretreated float bead carrier, making butyl titanate and the mass ratio that floats pearl is 10:1, stirring makes it to mix, filter behind the dipping 24h, filtrate constant temperature is preserved, and the sample oven dry that leaches places Muffle furnace in 450 ℃ of temperature lower calcination 3h again, be cooled to room temperature, thereby make the TiO of a load
2/ float pearl;
4) secondary load process: the sample that obtains with above-mentioned step 3) is carrier, repeating step 2) and step 3), to make the TiO of secondary load
2/ float pearl;
5) with after the step 4) TiO that makes
2/ to float pearl to join in the platinum acid chloride solution and stir, chloroplatinic acid measures with platinum in the synthetic system, wherein platinum and TiO
2/ float contained TiO in the pearl
2Mass ratio is 1:100, product is placed under the ultraviolet light shine 15h at last, finally obtains callable float type Pt-TiO
2/ float the pearly-lustre catalyst.
Embodiment 4
1) float the pearl preliminary treatment: that will extract from flyash floats pearl with 10% rare nitric acid dousing 4h, uses the distilled water rinsing afterwards, is neutral until the water that flows out, and the oven dry back is standby;
2) be raw material with butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water, the mol ratio of butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water is 1:25:1:1, regulate its pH to 5 with red fuming nitric acid (RFNA), stirring is fully reacted it, add Macrogol 2000 0 then, the mol ratio that makes butyl titanate and polyethylene glycol is 1200:1, and heating and stirring make it abundant dissolving, namely obtain the TiO of yellow transparent
2Colloidal sol;
3) to TiO
2Add in the colloidal sol step 1) pretreated float bead carrier, making butyl titanate and the mass ratio that floats pearl is 10:1, stirring makes it to mix, filter behind the dipping 36h, filtrate constant temperature is preserved, and the sample oven dry that leaches places Muffle furnace in 550 ℃ of temperature lower calcination 4h again, be cooled to room temperature, thereby make the TiO of a load
2/ float pearl;
4) secondary load process: the sample that obtains with above-mentioned step 3) is carrier, repeating step 2) and step 3), to make the TiO of secondary load
2/ float pearl;
5) with after the step 4) TiO that makes
2/ to float pearl to join in the platinum acid chloride solution and stir, chloroplatinic acid measures with platinum in the synthetic system, wherein platinum and TiO
2/ float contained TiO in the pearl
2Mass ratio is 1:100, product is placed under the ultraviolet light shine 18h at last, finally obtains callable float type Pt-TiO
2/ float the pearly-lustre catalyst.
Embodiment 5
1) float the pearl preliminary treatment: that will extract from flyash floats pearl with 10% rare nitric acid dousing 4h, uses the distilled water rinsing afterwards, is neutral until the water that flows out, and the oven dry back is standby;
2) be raw material with butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water, the mol ratio of butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water is 1:25:1:1, regulate its pH to 5 with red fuming nitric acid (RFNA), stirring is fully reacted it, add Macrogol 2000 0 then, the mol ratio that makes butyl titanate and polyethylene glycol is 1000:1, and heating and stirring make it abundant dissolving, namely obtain the TiO of yellow transparent
2Colloidal sol;
3) to TiO
2Add in the colloidal sol step 1) pretreated float bead carrier, making butyl titanate and the mass ratio that floats pearl is 7:1, stirring makes it to mix, filter behind the dipping 24h, filtrate constant temperature is preserved, and the sample oven dry that leaches places Muffle furnace in 450 ℃ of temperature lower calcination 2h again, be cooled to room temperature, thereby make the TiO of a load
2/ float pearl;
4) secondary load process: the sample that obtains with above-mentioned step 3) is carrier, repeating step 2) and step 3), to make the TiO of secondary load
2/ float pearl;
5) with after the step 4) TiO that makes
2/ to float pearl to join in the platinum acid chloride solution and stir, chloroplatinic acid measures with platinum in the synthetic system, wherein platinum and TiO
2/ float contained TiO in the pearl
2Mass ratio is 1:100, product is placed under the ultraviolet light shine 15h at last, finally obtains callable float type Pt-TiO
2/ float the pearly-lustre catalyst.
Fig. 1 is the related callable float type Pt-TiO of embodiment 5
2/ float the sem photograph of pearly-lustre catalyst.As can be seen from Figure, Pt-TiO
2/ the profile of floating the pearly-lustre catalyst is the spherical of rule, floats bead surface and has formed rete, and rete distributes more even relatively, but the rete non-uniform phenomenon has also appearred in a few regions.
Fig. 2 is the related callable float type Pt-TiO of embodiment 5
2/ float pearly-lustre catalyst and unmodified TiO
2/ float the ultraviolet-visible absorption spectroscopy figure of pearl, as can be seen from the figure, Pt-TiO
2/ floating pearl compares TiO to the response intensity of light
2/ float pearl to be significantly improved, and the photoresponse scope has extended to visible region.
Embodiment 6
1) float the pearl preliminary treatment: that will extract from flyash floats pearl with 10% rare nitric acid dousing 4h, uses the distilled water rinsing afterwards, is neutral until the water that flows out, and the oven dry back is standby;
2) be raw material with butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water, the mol ratio of butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water is 1:25:1:2, regulate its pH to 6 with red fuming nitric acid (RFNA), stirring is fully reacted it, add Macrogol 2000 0 then, the mol ratio that makes butyl titanate and polyethylene glycol is 1200:1, and heating and stirring make it abundant dissolving, namely obtain the TiO of yellow transparent
2Colloidal sol;
3) to TiO
2Add in the colloidal sol step 1) pretreated float bead carrier, making butyl titanate and the mass ratio that floats pearl is 10:1, stirring makes it to mix, filter after flooding 12 h, filtrate constant temperature is preserved, and the sample oven dry that leaches places Muffle furnace in 450 ℃ of temperature lower calcination 4h again, be cooled to room temperature, thereby make the TiO of a load
2/ float pearl;
4) secondary load process: the sample that obtains with above-mentioned step 3) is carrier, repeating step 2) and step 3), to make the TiO of secondary load
2/ float pearl;
Three loading processes: the sample with secondary load is carrier, repeating step 2) and step 3), to make the TiO of three loads
2/ float pearl;
5) with after the step 4) TiO that makes
2/ to float pearl to join in the platinum acid chloride solution and stir, chloroplatinic acid measures with platinum in the synthetic system, wherein platinum and TiO
2/ float contained TiO in the pearl
2Mass ratio is 1:50, product is placed under the ultraviolet light shine 15h at last, finally obtains callable float type Pt-TiO
2/ float the pearly-lustre catalyst.
Embodiment 7
1) float the pearl preliminary treatment: that will extract from flyash floats pearl with 10% rare nitric acid dousing 4h, uses the distilled water rinsing afterwards, is neutral until the water that flows out, and the oven dry back is standby;
2) be raw material with butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water, the mol ratio of butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water is 1:25:1:3, regulate its pH to 5 with red fuming nitric acid (RFNA), stirring is fully reacted it, add Macrogol 2000 0 then, the mol ratio that makes butyl titanate and polyethylene glycol is 1000:1, and heating and stirring make it abundant dissolving, namely obtain the TiO of yellow transparent
2Colloidal sol;
3) to TiO
2Add in the colloidal sol step 1) pretreated float bead carrier, making butyl titanate and the mass ratio that floats pearl is 7:1, stirring makes it to mix, filter behind the dipping 24h, filtrate constant temperature is preserved, and the sample oven dry that leaches places Muffle furnace in 450 ℃ of temperature lower calcination 3h again, be cooled to room temperature, thereby make the TiO of a load
2/ float pearl;
4) secondary load process: the sample that obtains with above-mentioned step 3) is carrier, repeating step 2) and step 3), to make the TiO of secondary load
2/ float pearl;
Three loading processes: the sample with secondary load is carrier, repeating step 2) and step 3), to make the TiO of three loads
2/ float pearl;
Four loading processes: the sample with three loads is carrier, repeating step 2) and step 3), to make the TiO of four loads
2/ float pearl;
5) with after the step 4) TiO that makes
2/ to float pearl to join in the platinum acid chloride solution and stir, chloroplatinic acid measures with platinum in the synthetic system, wherein platinum and TiO
2/ float contained TiO in the pearl
2Mass ratio is 1:200, product is placed under the ultraviolet light shine 18h at last, finally obtains callable float type Pt-TiO
2/ float the pearly-lustre catalyst.
More than be thinking of the present invention and implementation method, concrete application approach is a lot, should be understood that; for those skilled in the art; under the prerequisite that does not break away from the principle of the invention, can also make some improvement, these improvement also should be considered as protection scope of the present invention.
Claims (6)
1. callable float type Pt-TiO
2/ float the pearly-lustre catalyst, it is characterized in that described carrier floats the cenosphere that pearl is rule, the TiO of deposition Pt
2With the form load of rete on it.
2. callable float type Pt-TiO
2/ float pearly-lustre Preparation of catalysts method, it is characterized in that may further comprise the steps:
1) float the pearl preliminary treatment: will float pearl with rare nitric acid dousing 4h, and use the distilled water rinsing afterwards, and be neutral until the water that flows out, the oven dry back is standby;
2) be raw material with butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water, regulate its pH to 4 ~ 6 with red fuming nitric acid (RFNA), stirring is fully reacted it, add polyethylene glycol then, the mol ratio that makes butyl titanate and polyethylene glycol is 800 ~ 1200:1, heating and stirring make it abundant dissolving, namely obtain the TiO of yellow transparent
2Colloidal sol;
3) to TiO
2Add in the colloidal sol step 1) pretreated float bead carrier, making butyl titanate and the mass ratio that floats pearl is 5 ~ 10:1, stirring makes it to mix, filter behind dipping 12 ~ 36h, filtrate constant temperature is preserved, and the sample oven dry that leaches places Muffle furnace in 350 ℃ ~ 550 ℃ temperature lower calcination 2 ~ 4h again, be cooled to room temperature, thereby make the TiO of a load
2/ float pearl;
4) loading process repeatedly: the sample that obtains with above-mentioned step 3) is carrier, repeating step 2) and step 3), to make the TiO of secondary load
2/ float pearl; Repeat above-mentioned experiment, to finish repeatedly load;
5) with after the step 4) TiO that makes
2/ to float pearl to join in the platinum acid chloride solution and stir, chloroplatinic acid measures with platinum in the synthetic system, wherein platinum and TiO
2/ float contained TiO in the pearl
2Mass ratio is 1:1000 ~ 50, at last product is placed under the ultraviolet light to shine some hours, finally obtains callable float type Pt-TiO
2/ float the pearly-lustre catalyst.
3. callable float type Pt-TiO according to claim 2
2/ float pearly-lustre Preparation of catalysts method, it is characterized in that step 2) in the mol ratio of butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and distilled water be 1:25:1:1 ~ 4.5.
4. callable float type Pt-TiO according to claim 3
2/ float pearly-lustre Preparation of catalysts method, it is characterized in that the addition of floating bead carrier in the step 3) is TiO
2Butyl titanate is 5 ~ 10:1 with the mass ratio that floats pearl in the colloidal sol.
5. according to claim 2,3 or 4 described callable float type Pt-TiO
2/ float pearly-lustre Preparation of catalysts method, it is characterized in that TiO in the step 3)
2/ load the number of times that floats pearl is 2 ~ 4 times.
6. according to claim 2,3 or 4 described callable float type Pt-TiO
2/ float pearly-lustre Preparation of catalysts method, it is characterized in that light-struck time of step 5) medium ultraviolet is 12 ~ 18h.
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| CN112264069A (en) * | 2020-10-23 | 2021-01-26 | 南京信息工程大学 | Attapulgite photocatalyst and preparation method thereof |
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