CN105536762A - C/TiO mesoporous composite photocatalyst and preparation method thereof - Google Patents
C/TiO mesoporous composite photocatalyst and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000011941 photocatalyst Substances 0.000 title abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 48
- 238000003756 stirring Methods 0.000 claims abstract description 30
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000005011 phenolic resin Substances 0.000 claims abstract description 19
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 14
- APQHKWPGGHMYKJ-UHFFFAOYSA-N Tributyltin oxide Chemical compound CCCC[Sn](CCCC)(CCCC)O[Sn](CCCC)(CCCC)CCCC APQHKWPGGHMYKJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 38
- 238000010438 heat treatment Methods 0.000 claims description 15
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000012423 maintenance Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 238000000802 evaporation-induced self-assembly Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 68
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 11
- 238000007146 photocatalysis Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 abstract description 3
- 229910003074 TiCl4 Inorganic materials 0.000 abstract 1
- 238000001354 calcination Methods 0.000 abstract 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 abstract 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 10
- 238000006555 catalytic reaction Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000012719 thermal polymerization Methods 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 238000003912 environmental pollution Methods 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- XQAXGZLFSSPBMK-UHFFFAOYSA-M [7-(dimethylamino)phenothiazin-3-ylidene]-dimethylazanium;chloride;trihydrate Chemical compound O.O.O.[Cl-].C1=CC(=[N+](C)C)C=C2SC3=CC(N(C)C)=CC=C3N=C21 XQAXGZLFSSPBMK-UHFFFAOYSA-M 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000000696 nitrogen adsorption--desorption isotherm Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
Abstract
The invention discloses a C/TiO mesoporous composite photocatalyst and a preparation method thereof, and belongs to the field of photocatalysis. The photocatalyst is mainly characterized in that mesoporous carbon has a strong absorption effect for visible light, and at the same time the mesoporous carbon reduces TiO2 to TiO at high temperature, and the C/TiO mesoporous composite photocatalyst is formed. The preparation method of the C/TiO mesoporous composite photocatalyst comprises the following steps: (1) preparation of phenolic resin: phenol is dissolved into a NaOH solution of a certain concentration, formaldehyde is added, pH value is adjusted to 6.0, and vacuum drying is carried out; (2) preparation of a phenolic resin-ethanol solution: a proper amount of P123 is dissolved into ethanol and is mixed with a proper amount of the phenolic resin uniformly; (3) TiCl4 and TBOT are added into the solution obtained in the step (2) with uniformly stirring and are poured into a culture dish, and the culture dish is placed in a baking oven; (4) a sample obtained in the step (3) is grinded into powder, the power is placed in a tubular furnace at nitrogen atmosphere for segmented calcinations, and the C/TiO mesoporous composite photocatalyst is obtained. The preparation method has simple and practicable processes, and the prepared C/TiO mesoporous composite photocatalyst is a novel high-efficient composite visible light catalyst.
Description
Technical field
The present invention adopts evaporation-induced self-assembly method to prepare C/TiO presoma, calcines removed template method P123 under presoma being placed in tube furnace nitrogen atmosphere, and phenolic resin carbonized forms mesoporous carbon, and makes titanium source TiCl
4tiO is formed with TBOT crystallization
2, under utilizing high temperature, mesoporous carbon is to TiO
2reduction form TiO, thus obtain the composite mesoporous photochemical catalyst of C/TiO with visible light-responded property.
Background technology
Deepen continuously along with industrialized, problem of environmental pollution is on the rise, and the solution seeking to alleviate problem of environmental pollution has become focus and the focus of scientists study at present.Compared to traditional method, photocatalysis technology makes full use of solar energy, and can be the small-molecule substance of no pollution by producing the organic matter degradation polluted to environment, be a kind of environmentally friendly technology having broad prospect of application.
Titanium and oxygen react and can generate a series of titanium oxygen compound, as TiO, TiO
2, Ti
2o
3, Ti
3o
5deng, these titanium oxygen compounds have stable phase structure, and wherein modal titanium oxygen compound is TiO
2.TiO
2be widely used in processing and produce the organic pollution of environmental pollution, it has the features such as nontoxic, oxidisability strong, stable chemical nature.But, due to TiO
2band gap width is comparatively large, can only absorb the ultraviolet that energy is higher, effectively can not utilize solar energy, and photo-generated carrier recombination rate is high, limit its extensive use.TiO is a kind of conductive oxide, not only has lower resistivity, also has and intercepts Al efficiently, the ability of the Elements Diffusion such as Si, its function and metal oxide containing precious metals RuO
2similar, in layer-stepping microelectronic structure device, piezoelectric structure device, there is important application prospect.In addition TiO also has application study in the field such as electrode material, imitation gold copper-base alloy.But the concern that generally speaking, TiO is subject to also can not show a candle to TiO
2so extensively with deep, particularly about TiO doping vario-property and the research also rare report based on first principle thereof.Mesoporous carbon has larger specific area, homogeneous adjustable aperture, chemical stability, mechanical stability, good electric conductivity and being paid close attention to widely.These advantages become the ideal material of absorption, separation, catalysis.In addition, mesoporous carbon can produce strong absorption to visible ray, and has stronger adsorption capacity and make it have potential application in photocatalysis field.After C doped Ti O, its metallic conduction band structure does not change, just near Fermi surface, there is the impurity energy level that C2p state provides, impurity energy level extends the conduction band width of TiO and the density of electronic states that improve near Fermi surface, thus TiO conductance is increased, resistivity reduces, thus improves photocatalysis performance.
Summary of the invention
The object of the present invention is to provide composite mesoporous photochemical catalyst of a kind of C/TiO and preparation method thereof, utilize mesoporous carbon at high temperature by TiO
2be reduced to TiO, and form the composite mesoporous photochemical catalyst of C/TiO with TiO.The prepared composite mesoporous photochemical catalyst of C/TiO has efficient photocatalytic activity.
The preparation method of the composite mesoporous photochemical catalyst of a kind of C/TiO provided by the invention, utilize mesoporous carbon to the strong absorption effect of visible ray, both the spectral response range of TiO had significantly been widened, make it have visible light catalysis activity, being separated of the light induced electron of photocatalyst surface and hole can be promoted again, thus significantly improve the photocatalytic activity of TiO photochemical catalyst.Comprise the steps:
(1) phenolic resins is prepared: a certain amount of phenol being dissolved in concentration is in the NaOH solution of 20wt%, stirs 10min continuously after mixing, is dropwise added by a certain amount of formaldehyde in above-mentioned mixed solution, stirs 60min at 60 ~ 70 DEG C.After being cooled to room temperature, with the HCl of 2mol/L, the pH value of solution is adjusted to 6.0,50 DEG C of vacuum drying;
(2) configure phenolic resins-ethanolic solution, 0.5 ~ 1.5gPluronicP123 is dissolved in 20g ethanol, mixes with the phenolic resins prepared by 0.5 ~ 5g above-mentioned steps (1), stir, obtain phenolic resins-ethanolic solution;
(3) by 0.5 ~ 1gTiCl
4pour in the phenolic resins-ethanolic solution of step (2) after 2 ~ 3g butyl titanate (TBOT) mixes, pour in culture dish after stirring 30 ~ 60min, under environment temperature, place 5 ~ 10h, then react 10 ~ 15h at being placed in 100 ~ 120 DEG C, baking oven;
(4) preparation of the composite mesoporous photochemical catalyst of C/TiO: by the orange-yellow sample grind into powder of above-mentioned steps (3) gained, be placed in tube furnace, under nitrogen atmosphere, 350 ~ 450 DEG C of heating 2 ~ 5h with removed template method, then are warming up to 700 ~ 800 DEG C of maintenance 2 ~ 5h.
In the preparation method of the composite mesoporous photochemical catalyst of the C/TiO described in the present invention, the mass ratio of each material is P123: phenolic resins: TiCl
4: TBOT=1: (0.5 ~ 5): (0.5 ~ 1): (2 ~ 3).Evaporation-induced self-assembly method is adopted to prepare the composite mesoporous photochemical catalyst presoma of C/TiO.
In the preparation method of the composite mesoporous photochemical catalyst of the C/TiO described in the present invention, less than 350 ~ 450 DEG C heating rates are 1 DEG C/min, and more than 350 ~ 450 DEG C heating rates are 5 DEG C/min.
The present invention compared with prior art, has remarkable advantage:
(1) the present invention utilizes mesoporous carbon at high temperature by TiO
2be reduced to TiO, and form the composite mesoporous photochemical catalyst of C/TiO with TiO, preparation technology's simple possible, the method preparing TiO than tradition has significant advantage.
(2) photocatalytic activity of the composite mesoporous photochemical catalyst of C/TiO prepared by the present invention is higher, utilize mesoporous carbon to the synergic sorption of visible ray, significantly widen the spectral response range of TiO, make it have visible light catalysis activity, promote the light induced electron of photocatalyst surface and being separated of hole, thus significantly improve the photocatalytic activity of TiO photochemical catalyst.
Accompanying drawing explanation
The X-ray diffraction style of the composite mesoporous photochemical catalyst of Fig. 1 C/TiO;
Nitrogen adsorption-the desorption isotherm of the composite mesoporous photochemical catalyst of Fig. 2 C/TiO;
The pore size distribution curve of the composite mesoporous photochemical catalyst of Fig. 3 C/TiO;
The photocatalysis performance test of the composite mesoporous photochemical catalyst of Fig. 4 C/TiO
Detailed description of the invention
The invention provides composite mesoporous photochemical catalyst of a kind of C/TiO and preparation method thereof, this composite photo-catalyst is used for degradable organic pollutant, it is characterized in that: utilize mesoporous carbon to the synergic sorption of visible ray, significantly widen the spectral response range of TiO, make it have visible light catalysis activity, promote the light induced electron of photocatalyst surface and being separated of hole, make composite photo-catalyst have efficient visible light catalytic performance.
The preparation method of the composite mesoporous photochemical catalyst of a kind of C/TiO of the present invention, comprises the steps:
(1) phenolic resins is prepared: a certain amount of phenol being dissolved in concentration is in the NaOH solution of 20wt%, stirs 10min continuously after mixing, is dropwise added by a certain amount of formaldehyde in above-mentioned mixed solution, stirs 60min at 60 ~ 70 DEG C.After being cooled to room temperature, with the HCl of 2mol/L, the pH value of solution is adjusted to 6.0,50 DEG C of vacuum drying;
(2) configure phenolic resins-ethanolic solution, 0.5 ~ 1.5gPluronicP123 is dissolved in 20g ethanol, mixes with the phenolic resins prepared by 0.5 ~ 5g above-mentioned steps (1), stir, obtain phenolic resins-ethanolic solution;
(3) by 0.5 ~ 1gTiCl
4pour in the phenolic resins-ethanolic solution of step (2) after 2 ~ 3g butyl titanate (TBOT) mixes, pour in culture dish after stirring 30 ~ 60min, under environment temperature, place 5 ~ 10h, then react 10 ~ 15h at being placed in 100 ~ 120 DEG C, baking oven;
(4) preparation of the composite mesoporous photochemical catalyst of C/TiO: by the orange-yellow sample grind into powder of above-mentioned steps (3) gained, be placed in tube furnace, under nitrogen atmosphere, 350 ~ 450 DEG C of heating 2 ~ 5h with removed template method, then are warming up to 700 ~ 800 DEG C of maintenance 2 ~ 5h.
For a better understanding of the present invention, illustrate content of the present invention further below in conjunction with example, but the example that content of the present invention is given below being not limited to.
The side's of enforcement example 1: the preparation method of the composite mesoporous photochemical catalyst of a kind of C/TiO of the present invention, comprises the following steps:
(1) phenolic resins is prepared: 10g phenol being dissolved in 2.13g concentration is in the NaOH solution of 20wt%, stirs 10min continuously after mixing, is dropwise added by the formaldehyde of 17.7g in above-mentioned mixed solution, stirs 60min at 70 DEG C.After being cooled to room temperature, with the HCl of 2mol/L, the pH value of solution is adjusted to 6.0, moisture is removed in 50 DEG C of vacuum drying;
(2) phenolic resins-ethanolic solution is configured: be dissolved in by 1gPluronicP123 in 20g ethanol, mix with the above-mentioned phenolic resins of 1g, stir;
(3) by 0.95gTiCl
4, pour into after 2.85g butyl titanate (TBOT) mixes in the solution of step (2), stir after 30min and pour in culture dish, under environment temperature, place 6h, then be placed in thermal polymerization 12h at 100 DEG C, baking oven;
(4) preparation of the composite mesoporous photochemical catalyst of C/TiO: by the orange-yellow sample grind into powder of step (3) gained, under being placed in tube furnace nitrogen atmosphere, heat 2h at 350 DEG C with removed template method, then be warming up to 750 DEG C of maintenance 2h.Less than 350 DEG C heating rates are 1 DEG C/min, and more than 350 DEG C heating rates are 5 DEG C/min.The composite mesoporous photochemical catalyst of C/TiO of gained is labeled as C/TiO-1.
Embodiment 2: the preparation method of the composite mesoporous photochemical catalyst of a kind of C/TiO of the present invention, comprises the following steps:
(1) phenolic resins is prepared: 10g phenol being dissolved in 2.13g concentration is in the NaOH solution of 20wt%, stirs 10min continuously after mixing, is dropwise added by the formaldehyde of 17.7g in above-mentioned mixed solution, stirs 60min at 70 DEG C.After being cooled to room temperature, with the HCl of 2mol/L, the pH value of solution is adjusted to 6.0, moisture is removed in 50 DEG C of vacuum drying;
(2) phenolic resins-ethanolic solution is configured: be dissolved in by 1gPluronicP123 in 20g ethanol, mix with the above-mentioned phenolic resins of 2g, stir;
(3) by 0.9gTiCl
4, pour into after 2.7g butyl titanate (TBOT) mixes in the solution of step (2), stir after 30min and pour in culture dish, under environment temperature, place 6h, then be placed in thermal polymerization 12h at 100 DEG C, baking oven;
(4) preparation of the composite mesoporous photochemical catalyst of C/TiO: by the orange-yellow sample grind into powder of step (3) gained, under being placed in tube furnace nitrogen atmosphere, heat 2h at 350 DEG C with removed template method, then be warming up to 750 DEG C of maintenance 2h.Less than 350 DEG C heating rates are 1 DEG C/min, and more than 350 DEG C heating rates are 5 DEG C/min.The composite mesoporous photochemical catalyst of C/TiO of gained is labeled as C/TiO-2.
Embodiment 3: the preparation method of the composite mesoporous photochemical catalyst of a kind of C/TiO of the present invention, comprises the steps:
(1) phenolic resins is prepared: 10g phenol being dissolved in 2.13g concentration is in the NaOH solution of 20wt%, stirs 10min continuously after mixing, is dropwise added by the formaldehyde of 17.7g in above-mentioned mixed solution, stirs 60min at 70 DEG C.After being cooled to room temperature, with the HCl of 2mol/L, the pH value of solution is adjusted to 6.0, moisture is removed in 50 DEG C of vacuum drying;
(2) configure phenolic resins-ethanolic solution, 1gPluronicP123 is dissolved in 20g ethanol, mixes with the above-mentioned phenolic resins of 3g, stir;
(3) by 0.85gTiCl
4, pour into after 2.55g butyl titanate (TBOT) mixes in the solution of step (2), stir after 30min and pour in culture dish, under environment temperature, place 6h, then be placed in thermal polymerization 12h at 100 DEG C, baking oven;
(4) preparation of the composite mesoporous photochemical catalyst of C/TiO: by the orange-yellow sample grind into powder of step (3) gained, under being placed in tube furnace nitrogen atmosphere, heat 2h at 350 DEG C with removed template method, then be warming up to 750 DEG C of maintenance 2h.Less than 350 DEG C heating rates are 1 DEG C/min, and more than 350 DEG C heating rates are 5 DEG C/min.The composite mesoporous photochemical catalyst of C/TiO of gained is labeled as C/TiO-3.
Embodiment 4: composite mesoporous photochemical catalyst of a kind of C/TiO of the present invention and preparation method thereof, comprises the steps:
(1) phenolic resins is prepared: 10g phenol being dissolved in 2.13g concentration is in the NaOH solution of 20wt%, stirs 10min continuously after mixing, is dropwise added by the formaldehyde of 17.7g in above-mentioned mixed solution, stirs 60min at 70 DEG C.After being cooled to room temperature, with the HCl of 2mol/L, the pH value of solution is adjusted to 6.0, moisture is removed in 50 DEG C of vacuum drying;
(2) configure phenolic resins-ethanolic solution, 1gPluronicP123 is dissolved in 20g ethanol, mixes with the above-mentioned phenolic resins of 4g, stir;
(3) by 0.8gTiCl
4, pour into after 2.4g butyl titanate (TBOT) mixes in the solution of step (2), stir after 30min and pour in culture dish, under environment temperature, place 6h, then be placed in thermal polymerization 12h at 100 DEG C, baking oven;
(4) preparation of the composite mesoporous photochemical catalyst of C/TiO: by the orange-yellow sample grind into powder of step (3) gained, under being placed in tube furnace nitrogen atmosphere, heat 2h at 350 DEG C with removed template method, then be warming up to 750 DEG C of maintenance 2h.Less than 350 DEG C heating rates are 1 DEG C/min, and more than 350 DEG C heating rates are 5 DEG C/min.The composite mesoporous photochemical catalyst of C/TiO of gained is labeled as C/TiO-4.
As shown in Figure 1, characterize mutually the thing of the composite mesoporous photochemical catalyst of C/TiO, the diffraction maximum that plum blossom icon sections out is the TiO of Hongquiite phase, does not find the TiO of anatase or Rutile Type
2, because under high temperature high temperature, TiO
2tiO is reduced into by the C in system.The composite mesoporous photochemical catalyst of C/TiO is carried out to the sign of nitrogen adsorption-desorption, the parameters such as the specific area of test sample and aperture, as can be seen from Figure 2, nitrogen adsorption-desorption isotherm is typical IV type thermoisopleth, shows that sample has meso-hole structure.The type of hysteresis loop is H2 type, shows that mesopore orbit is regular.In addition, as can be seen from the pore size distribution curve of Fig. 3, the pore-size distribution of the sample of different C/TiO ratio all concentrates on about 10nm, further illustrates mesopore orbit rule.The photocatalysis performance of the composite mesoporous photochemical catalyst of C/TiO and commercially available P25 is degradation of methylene blue (methyleneblue under the radiation of visible light provided by 300W xenon lamp, MB) solution is weighed, concrete experimentation is as follows: taking 20mg photochemical catalyst, to add concentration be in the 50mLMB solution of 10mg/L, the solution prepared is placed in dark place dispersed with stirring 20min and makes it reach adsorption equilibrium.Then solution is carried out light-catalyzed reaction, get the solution of about 5mL at regular intervals, catalyst is fallen in centrifugal filtration, measures MB absorbance residual in solution with ultraviolet specrophotometer.The photocatalysis performance of the composite mesoporous photochemical catalyst of C/TiO and commercially available P25 as shown in Figure 4, its result shows that the composite mesoporous photochemical catalyst photocatalysis performance of C/TiO is obviously better than P25 photocatalysis performance under visible light, and along with the increasing of ratio of C in C/TiO compound, visible light photocatalysis effect is become better and better.
Claims (4)
1. composite mesoporous photochemical catalyst of C/TiO and preparation method thereof, comprises the steps:
(1) phenolic resins is prepared: a certain amount of phenol being dissolved in concentration is in the NaOH solution of 20wt%, stirs 10min continuously after mixing, is dropwise added by a certain amount of formaldehyde in above-mentioned mixed solution, stirs 60min at 60 ~ 70 DEG C.After being cooled to room temperature, with the HCl of 2mol/L, the pH value of solution is adjusted to 6.0,50 DEG C of vacuum drying;
(2) configure phenolic resins-ethanolic solution, 0.5 ~ 1.5gPluronicP123 is dissolved in 20g ethanol, mixes with the phenolic resins prepared by 0.5 ~ 5g above-mentioned steps (1), stir, obtain phenolic resins-ethanolic solution;
(3) by 0.5 ~ 1gTiCl
4pour in the phenolic resins-ethanolic solution of step (2) after 2 ~ 3g butyl titanate (TBOT) mixes, pour in culture dish after stirring 30 ~ 60min, under environment temperature, place 5 ~ 10h, then react 10 ~ 15h at being placed in 100 ~ 120 DEG C, baking oven;
(4) preparation of the composite mesoporous photochemical catalyst of C/TiO: by the orange-yellow sample grind into powder of above-mentioned steps (3) gained, be placed in tube furnace, under nitrogen atmosphere, 350 ~ 450 DEG C of heating 2 ~ 5h with removed template method, then are warming up to 700 ~ 800 DEG C of maintenance 2 ~ 5h.
2. the preparation method of the composite mesoporous photochemical catalyst of C/TiO according to claim 1, is characterized in that: in step (3), the mass ratio of each material is P123: phenolic resins: TiCl
4: TBOT=1: (0.5 ~ 5): (0.5 ~ 1): (2 ~ 3).Evaporation-induced self-assembly method is adopted to prepare the composite mesoporous photochemical catalyst presoma of C/TiO.
3. the preparation method of the composite mesoporous photochemical catalyst of C/TiO according to claim 1, is characterized in that: in step (4), and less than 350 ~ 450 DEG C heating rates are 1 DEG C/min, and more than 350 ~ 450 DEG C heating rates are 5 DEG C/min.
4. the composite mesoporous photochemical catalyst of C/TiO, is characterized in that: the composite mesoporous photochemical catalyst of described C/TiO obtains according to the preparation method in claims 1 to 3 described in any one.
Priority Applications (1)
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| CN110152654A (en) * | 2019-05-08 | 2019-08-23 | 上海师范大学 | Ordered mesopore carbon-TiO2Composite material loaded palladium catalyst and preparation method thereof, application |
| CN110394175A (en) * | 2019-06-26 | 2019-11-01 | 济南大学 | A kind of template prepares the method and application of Copper-cladding Aluminum Bar mesoporous TiO 2 |
| CN110508275A (en) * | 2019-08-21 | 2019-11-29 | 上海应用技术大学 | A kind of mesoporous material load manganese dioxide-catalyst and preparation method thereof |
| CN112871210A (en) * | 2019-11-29 | 2021-06-01 | 兰州大学 | Preparation method of ordered mesoporous polymer heterogeneous photocatalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107899601A (en) * | 2017-12-05 | 2018-04-13 | 江南大学 | A kind of CuO/ nitridations carbon composite photocatalyst and preparation method thereof |
| CN110152654A (en) * | 2019-05-08 | 2019-08-23 | 上海师范大学 | Ordered mesopore carbon-TiO2Composite material loaded palladium catalyst and preparation method thereof, application |
| CN110152654B (en) * | 2019-05-08 | 2022-08-12 | 上海师范大学 | Ordered mesoporous carbon-TiO 2 Composite material supported palladium catalyst, preparation method and application thereof |
| CN110394175A (en) * | 2019-06-26 | 2019-11-01 | 济南大学 | A kind of template prepares the method and application of Copper-cladding Aluminum Bar mesoporous TiO 2 |
| CN110394175B (en) * | 2019-06-26 | 2022-10-21 | 济南大学 | Method for preparing copper-doped mesoporous titanium dioxide by template method and application |
| CN110508275A (en) * | 2019-08-21 | 2019-11-29 | 上海应用技术大学 | A kind of mesoporous material load manganese dioxide-catalyst and preparation method thereof |
| CN110508275B (en) * | 2019-08-21 | 2022-08-26 | 上海应用技术大学 | Mesoporous material loaded manganese dioxide catalyst and preparation method thereof |
| CN112871210A (en) * | 2019-11-29 | 2021-06-01 | 兰州大学 | Preparation method of ordered mesoporous polymer heterogeneous photocatalyst |
| CN112871210B (en) * | 2019-11-29 | 2023-09-29 | 兰州大学 | Preparation method of ordered mesoporous polymer multiphase photocatalyst |
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