CN101837300B - Photocatalysis coupled catalyst based on ozone and preparation method thereof - Google Patents
Photocatalysis coupled catalyst based on ozone and preparation method thereof Download PDFInfo
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- CN101837300B CN101837300B CN2010101702588A CN201010170258A CN101837300B CN 101837300 B CN101837300 B CN 101837300B CN 2010101702588 A CN2010101702588 A CN 2010101702588A CN 201010170258 A CN201010170258 A CN 201010170258A CN 101837300 B CN101837300 B CN 101837300B
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- molecular sieve
- aqueous solution
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- ozone
- deionized water
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Abstract
The invention relates to a photocatalysis coupled catalyst based on ozone in the technical field of photocatalysis and a preparation method thereof. The preparation method comprises the following steps of: steeping molecular sieve water solution into metal ion soluble precursor solution, obtaining an oxide molecular sieve catalyst through filter washing and drying processing, adding the oxide molecular sieve catalyst to ethanol and dropwise adding tetrabutyl titanate and deionized water sequentially, and obtaining the photocatalysis coupled catalyst based on ozone through calcinations after mixing and filtering. The catalyst has efficient, continuous and lasting purification functions to organic volatile matters, such as formaldehyde, benzene series, and the like and bacilli in room air.
Description
Technical field
What the present invention relates to is the Catalysts and its preparation method in a kind of photocatalysis technology field, specifically is a kind of photocatalysis coupled catalyst based on ozone and preparation method thereof.
Background technology
Because the City Building syndrome that modern residential environment and interior decoration etc. cause, room conditioning disease, organic contamination etc. directly have influence on people's health and lives safety.Because of central air conditioner system can not be regular cleaning and sterilization, its internal system becomes the bacteria breed place and the environmental pollution that brings, paid more and more attention.Present air purifier adopts mainly that charcoal absorption technology, ozone purification are technological, anion dedusting technology and high voltage electrostatic technique.The charcoal absorption technology can only store nuisance absorption, and can not its decomposition or removal just be shifted pollution sources, and adsorption capacity is limited, in case saturated then lose effect.Ozone technology has sterilization, deodorization, but low to the removal efficient of organic pollution, and ozone itself is harmful to human body and environment.Anion and high voltage electrostatic technique are a kind of physical action processes, can remove airborne flue dust, but can't remove purification to the pollution that chemistry, biology and microorganism etc. are caused.
Retrieval through to the prior art document finds that Chinese invention patent application number 200810064975.5 has been put down in writing a kind of " loaded photocatalyst and preparation method thereof ", and it is the TiO of carrier with the NACF that this technology discloses a kind of
2Photochemical catalyst has improved photochemical catalyst ability has been removed in the degraded of benzene in the water.Nano-TiO
2Photochemical catalyst oxidation or reduction effectively is adsorbed on its lip-deep pernicious gas molecule, and kill bacteria suppresses virus, and can harmful organic substance, bacterium etc. be converted into innocuous substances such as water and carbon dioxide, and has no secondary pollution.TiO
2The absorption property of photochemical catalyst is relatively poor, and the photocatalysis carrier that need to adopt is fit to is to improve the absorption of pollutant and to catch.But TiO
2Photochemical catalyst loses activity owing to organic matter decomposes the intermediate product that produces in the process of degradation of organic substances easily; Therefore present technique adopts drop ozone to avoid the generation of intermediate product as cooxidant; Ozone is a kind of strong oxidizer; The oxide of zinc, copper or manganese can decompose the extremely strong active oxygen atom of generation oxidability by catalysis ozone, thereby further organic matter and intermediate product thereof is carried out oxidation Decomposition, avoids TiO
2The inactivation of photochemical catalyst, concrete reaction as shown in the formula as show:
TiO
2+hv→h
++e
- R1
h
++OH
-→OH
· R2
h
++H
2O→OH
·+H
+ R3
O
3+e
-→O
3 ·- R4
H
++O
3 ·-→HO
3 · R5
HO
3 ·→O
2+OH
· R6
O
3+hv(λ＜310nm)→O
·+O
2 R7
O
·+HO
2→2OH
· R8
O
3+OH
·→HO
2 ·+O
2 R9
h
++ organic matter → organic matter intermediate R10
Organic matter has mesosome+O
2 -→ CO
2+ H
2O R11
Organic matter has mesosome+OH
→ CO
2+ H
2O R12
Summary of the invention
The present invention is directed to the above-mentioned deficiency that prior art exists, a kind of photocatalysis coupled catalyst based on ozone and preparation method thereof is provided, utilize the oxide of zinc, copper or manganese that ozone is had catalyticing decomposition action and TiO
2Photocatalytic activity, a kind of coupled catalyst that is used for the depollution of environment and preparation method thereof is provided.The present invention can form purifier with uviol lamp, and the drop ozone auxiliary catalysis that can utilize uviol lamp or high-pressure electrostatic to discharge has efficient, continuous, lasting purification function to organic volatile such as the formaldehyde in the room air, benzene series thing and bacterium.
The present invention realizes through following technical scheme:
The present invention relates to a kind of photocatalysis coupled catalyst based on ozone, its component and percentage by weight are: the oxide of 0.5%～5.0% zinc, copper or manganese, 20.0% TiO
2Photochemical catalyst, surplus are molecular sieve, wherein:
Described molecular sieve is a type ZSM 5 molecular sieve, and molecular formula is Na
nAl
nSi
96-nO
19216H
2O (0＜n＜27); Has high stability; Very wide silica alumina ratio excursion is arranged; Can the modulation surface acidity, unique three-dimensional straight channel system and ten-ring perforate are close with many organic molecule sizes, and the excellent shape adsorptivity of selecting is arranged; And through ion-exchange with the element of different nature skeleton that induces one, to regulate its aperture, surface nature.
The oxide of described zinc, copper or manganese is meant: through carrying out ZnO, CuO, the Al that ion-exchange process prepares with molecular sieve
2CuO
4, MnO, Mn
2O
3Or MnO
2In a kind of or its combination.
Described TiO
2Photochemical catalyst is meant: load on the nano-TiO on the molecular sieve through what immersion process for preparing obtained
2Photochemical catalyst.
The present invention relates to the preparation method of above-mentioned photocatalysis coupled catalyst based on ozone; Through the molecular sieve aqueous solution being immersed in the metal ion solubility precursor aqueous solution; After handling, washing and oven dry obtain oxide molecular sieve catalyzer through filtering; Oxide molecular sieve catalyzer is joined in the ethanol and dropwise adding tetrabutyl titanate and deionized water successively, and calcining obtains the photocatalysis coupled catalyst based on ozone after agitation and filtration.
Described metal ion solubility precursor aqueous solution is: contain Zn
2+, Cu
2+Or Mn
2+In a metal ion species, concentration is the aqueous solution of nitrate, chlorate or the acetate of 0.1mol/L.
The described molecular sieve aqueous solution is meant: concentration is the aqueous solution of the ZSM-5 molecular sieve of 60g/L.
Described immersion is meant: under the stirring environment of 200rpm, the molecular sieve aqueous solution is added dropwise to metal ion solubility precursor aqueous solution;
Described oven dry is handled and is meant: heat drying 3-5h under 550 ℃ environment.
Described calcination processing is meant: calcining 3-5h under 350～700 ℃ environment.
The present invention has following beneficial effect: raw material resources of the present invention is abundant, low price; Simple, the control easily of preparation technology of the present invention.The depollution of environment coupled catalyst that the present invention obtained; Integrating absorption concentrates-the photocatalysis-oxidation catalysis; Form purifier with uviol lamp or high-pressure electrostatic; The drop ozone auxiliary catalysis that can utilize uviol lamp or high-pressure electrostatic to discharge has the function of formaldehyde, benzene series thing and bacterium in efficient, continuous, lasting the purifying the air of a room.
The specific embodiment
Elaborate in the face of embodiments of the invention down, present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Embodiment 1
Step 1 is the solubility solution that contains zinc ion with zinc acetate, and the molar concentration of zinc acetate is 0.1mol/L; The preparation process of precursor aqueous solution: take by weighing zinc acetate 0.1mol and join in the deionized water; After stirring and dissolving is complete, move in the 1L volumetric flask, be mixed with 1L solution.
Step 2 is added to 30g molecular sieve ZSM-5 in the 500ml deionized water, slowly drips the final gained solution of step 1 1000ml while stirring; After 3h drips; Continue to stir 12h, the suspension of gained is filtered washing repeatedly after, 110 ℃ of dry 12h down; In Muffle furnace, calcine 5h then under 550 ℃, promptly obtain the Zn/ZSM-5 coupled catalyst.
Step 3: step 2 is obtained the Zn/ZSM-5 coupled catalyst join in the 500ml ethanol; Slow while stirring dropwise adding tetrabutyl titanate 37.5ml; Continue again slowly to drip deionized water 200ml while stirring, after 30 minutes, the gained sample filtered, washes three times repeatedly after; Under 550 ℃, calcine 3h, can obtain TiO
2/ Zn/ZSM-5 coupled catalyst.
Catalytic component and content that present embodiment prepares gained are: the ZnO mass content is 0.74%-0.85%, TiO
2Mass content is 20%.
With above-mentioned TiO
2/ Zn/ZSM-5 coupled catalyst places photo catalysis reactor, feeds 269ppm equilibrium concentration formaldehyde gas, and air speed is 67000h
-1, breakdown 15W uviol lamp (dominant wavelength 254nm) and ozone generator can reach 18.9% to the disposable of acetaldehyde through removing efficient.
Embodiment 2
Step 1 is the solubility solution of copper ions with the Schweinfurt green, and the molar concentration of Schweinfurt green is 0.1mol/L; The preparation process of precursor aqueous solution: take by weighing Schweinfurt green 0.1mol and join in the deionized water; After stirring and dissolving is complete, move in the 1L volumetric flask, be mixed with 1L solution.
Step 2 is added to 30g molecular sieve ZSM-5 in the 500ml deionized water, slowly drips the final gained solution of step 1 1000ml while stirring; After 3h drips; Continue to stir 24h, the suspension of gained is filtered washing repeatedly after, 110 ℃ of dry 12h down; In Muffle furnace, calcine 5h then under 550 ℃, promptly obtain the Cu/ZSM-5 coupled catalyst.
Step 3: step 2 is obtained the Cu/ZSM-5 coupled catalyst join in the 500ml ethanol; Slow while stirring dropwise adding tetrabutyl titanate 37.5ml; Continue again slowly to drip deionized water 200ml while stirring, after 30 minutes, the gained sample filtered, washes three times repeatedly after; Under 550 ℃, calcine 3h, can obtain TiO
2/ Cu/ZSM-5 coupled catalyst.
Catalytic component and content that present embodiment prepares gained are: the CuO mass content is 1.64%-1.86%, TiO
2Mass content is 20%.
With above-mentioned TiO
2/ Cu/ZSM-5 coupled catalyst places photo catalysis reactor, feeds 269ppm equilibrium concentration formaldehyde gas, and air speed is 67000h
-1, breakdown 15W uviol lamp (dominant wavelength 254nm) and ozone generator can reach 30.5% to the disposable of acetaldehyde through removing efficient.
Embodiment 3
Step 1 is the solubility solution that contains manganese ion with manganese acetate, and the molar concentration of manganese acetate is 0.1mol/L; The preparation process of precursor aqueous solution: take by weighing manganese acetate 0.1mol and join in the deionized water; After stirring and dissolving is complete, move in the 1L volumetric flask, be mixed with 1L solution.
Step 2 is added to 30g molecular sieve ZSM-5 in the 500ml deionized water, slowly drips the final gained solution of step 1 1000ml while stirring; After 3h drips; Continue to stir 36h, the suspension of gained is filtered washing repeatedly after, 110 ℃ of dry 12h down; In Muffle furnace, calcine 5h then under 550 ℃, promptly obtain the Mn/ZSM-5 coupled catalyst.
Step 3: step 2 is obtained the Mn/ZSM-5 coupled catalyst join in the 500ml ethanol; Slow while stirring dropwise adding tetrabutyl titanate 37.5ml; Continue again slowly to drip deionized water 200ml while stirring, after 30 minutes, the gained sample filtered, washes three times repeatedly after; Under 550 ℃, calcine 3h, can obtain TiO
2/ Mn/ZSM-5 coupled catalyst.
Catalytic component and content that present embodiment prepares gained are: MnO
xMass content is 2.34%-2.66%, TiO
2Mass content is 20%.
With above-mentioned TiO
2/ Cu/ZSM-5 coupled catalyst places photo catalysis reactor, feeds 269ppm equilibrium concentration formaldehyde gas, and air speed is 67000h
-1, breakdown 15W uviol lamp (dominant wavelength 254nm) and ozone generator can reach 78.9% to the disposable of acetaldehyde through removing efficient.
Embodiment 4
Step 1 is the solubility solution that contains manganese ion with manganese acetate, and the molar concentration of manganese acetate is 0.1mol/L; The preparation process of precursor aqueous solution: take by weighing manganese acetate 0.1mol and join in the deionized water; After stirring and dissolving is complete, move in the 1L volumetric flask, be mixed with 1L solution.
Step 2 is added to 30g molecular sieve ZSM-5 in the 500ml deionized water, slowly drips the final gained solution of step 1 1000ml while stirring; After 3h drips; Continue to stir 48h, the suspension of gained is filtered washing repeatedly after, 110 ℃ of dry 12h down; In Muffle furnace, calcine 5h then under 700 ℃, promptly obtain the Mn/ZSM-5 coupled catalyst.
Step 3: step 2 is obtained the Mn/ZSM-5 coupled catalyst join in the 500ml ethanol; Slow while stirring dropwise adding tetrabutyl titanate 37.5ml; Continue again slowly to drip deionized water 200ml while stirring, after 30 minutes, the gained sample filtered, washes three times repeatedly after; Under 350 ℃, calcine 3h, can obtain TiO
2/ Mn/ZSM-5 coupled catalyst.
Catalytic component and content that present embodiment prepares gained are: MnO
xMass content is 3.84%-4.06%, TiO
2Mass content is 20%.
With above-mentioned TiO
2/ Mn/ZSM-5 coupled catalyst places photo catalysis reactor, feeds 269ppm equilibrium concentration formaldehyde gas, and air speed is 67000h
-1, breakdown 15W uviol lamp (dominant wavelength 254nm) and ozone generator can reach 68.5% to the disposable of acetaldehyde through removing efficient.
Embodiment 5
Step 1 is the solubility solution that contains manganese ion with manganese chloride, and the molar concentration of manganese chloride is 0.1mol/L; The preparation process of precursor aqueous solution: take by weighing manganese chloride 0.1mol and join in the deionized water; After stirring and dissolving is complete, move in the 1L volumetric flask, be mixed with 1L solution.
Step 2 is added to 30g molecular sieve ZSM-5 in the 500ml deionized water, slowly drips the final gained solution of step 1 1000ml while stirring; After 3h drips; Continue to stir 12h, the suspension of gained is filtered washing repeatedly after, 110 ℃ of dry 12h down; In Muffle furnace, calcine 5h then under 550 ℃, promptly obtain the Mn/ZSM-5 coupled catalyst.
Step 3: step 2 is obtained the Mn/ZSM-5 coupled catalyst join in the 500ml ethanol; Slow while stirring dropwise adding tetrabutyl titanate 37.5ml; Continue again slowly to drip deionized water 200ml while stirring, after 30 minutes, the gained sample filtered, washes three times repeatedly after; Under 450 ℃, calcine 3h, can obtain TiO
2/ Mn/ZSM-5 coupled catalyst.
Catalytic component and content that present embodiment prepares gained are: MnO
xMass content is 0.86%-1.02%, TiO
2Mass content is 20%.
With above-mentioned TiO
2/ Mn/ZSM-5 coupled catalyst places photo catalysis reactor, feeds 269ppm equilibrium concentration formaldehyde gas, and air speed is 67000h
-1, breakdown 15W uviol lamp (dominant wavelength 254nm) and ozone generator can reach 59.3% to the disposable of acetaldehyde through removing efficient.
Embodiment 5
Step 1 is the solubility solution that contains manganese ion with manganese nitrate, and the molar concentration of manganese nitrate is 0.1mol/L; The preparation process of precursor aqueous solution: take by weighing manganese nitrate 0.1mol and join in the deionized water; After stirring and dissolving is complete, move in the 1L volumetric flask, be mixed with 1L solution.
Step 2 is added to 30g molecular sieve ZSM-5 in the 500ml deionized water, slowly drips the final gained solution of step 1 1000ml while stirring; After 3h drips; Continue to stir 24h, the suspension of gained is filtered washing repeatedly after, 110 ℃ of dry 12h down; In Muffle furnace, calcine 5h then under 350 ℃, promptly obtain the Mn/ZSM-5 coupled catalyst.
Step 3: step 2 is obtained the Mn/ZSM-5 coupled catalyst join in the 500ml ethanol; Slow while stirring dropwise adding tetrabutyl titanate 37.5ml; Continue again slowly to drip deionized water 200ml while stirring, after 30 minutes, the gained sample filtered, washes three times repeatedly after; Under 700 ℃, calcine 3h, can obtain TiO
2/ Mn/ZSM-5 coupled catalyst.
Catalytic component and content that present embodiment prepares gained are: MnO
xMass content is 1.25%-1.42%, TiO
2Mass content is 20%.
With above-mentioned TiO
2/ Mn/ZSM-5 coupled catalyst places photo catalysis reactor, feeds 269ppm equilibrium concentration formaldehyde gas, and air speed is 67000h
-1, breakdown 15W uviol lamp (dominant wavelength 254nm) and ozone generator can reach 54.7% to the disposable of acetaldehyde through removing efficient.
Claims (1)
1. preparation method based on the photocatalysis coupled catalyst of ozone, this photocatalysis coupled catalyst component and percentage by weight are: the oxide of 0.5%～5.0% zinc, copper or manganese, 20.0% TiO
2Photochemical catalyst, surplus are molecular sieve, wherein:
Described molecular sieve is a type ZSM 5 molecular sieve, and molecular formula is Na
nAl
nSi
96-nO
19216H
2O, 0＜n＜27;
It is characterized in that; Said method is through being immersed in the molecular sieve aqueous solution in the metal ion solubility precursor aqueous solution; After handling, washing and oven dry obtain oxide molecular sieve catalyzer through filtering; Oxide molecular sieve catalyzer is joined in the ethanol and dropwise adding tetrabutyl titanate and deionized water successively, and calcining obtains the photocatalysis coupled catalyst based on ozone after agitation and filtration;
The oxide of described zinc, copper or manganese is meant: through carrying out ZnO, CuO, the Al that ion-exchange process prepares with molecular sieve
2CuO
4, MnO, Mn
2O
3Or MnO
2In a kind of or its combination;
Described TiO
2Photochemical catalyst is meant: load on the nano-TiO on the molecular sieve through what immersion process for preparing obtained
2Photochemical catalyst;
Described metal ion solubility precursor aqueous solution is: contain Zn
2+, Cu
2+Or Mn
2+In a metal ion species, concentration is the aqueous solution of nitrate, chlorate or the acetate of 0.1mol/L;
The described molecular sieve aqueous solution is meant: concentration is the aqueous solution of the ZSM-5 molecular sieve of 60g/L;
Described immersion is meant: under the stirring environment of 200rpm, the molecular sieve aqueous solution is added dropwise to metal ion solubility precursor aqueous solution;
Described dropwise adding tetrabutyl titanate successively and deionized water are meant: dropwise adding tetrabutyl titanate dropwise while stirring; And then dropwise drip deionized water while stirring and left standstill 30 minutes; Wherein: the consumption of butyl titanate is 0.075 times of said ethanol volume, and the consumption of deionized water is 0.4 times of said ethanol volume;
Described oven dry is handled and is meant: heat drying 3-5h under 550 ℃ environment;
Described calcination processing is meant: calcining 3-5h under 350～700 ℃ environment.
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| CN101837300B true CN101837300B (en) | 2012-06-13 |
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| CN103240115B (en) * | 2012-02-09 | 2015-01-21 | 中国石油天然气股份有限公司 | Supported catalytic ozonation catalyst and its preparation method |
| CN113083302B (en) * | 2021-04-25 | 2023-05-05 | 西南民族大学 | Heterostructure nano-composite and preparation method and application thereof |
| CN116099568A (en) * | 2022-12-30 | 2023-05-12 | 重庆市畜牧科学院 | Cu/ZSM-5/TiO 2 Composite photocatalytic material and preparation method and application thereof |
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2010
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Non-Patent Citations (2)
| Title |
|---|
| Wenfeng Shangguan.《Photocatalytic nanocomposite for hydrogen production from water splitting and environmental purification》.《Nagasaki Symposium on Nano-Dynamics 2010》.2010,第12-13页. * |
| 史文晶等.《TiO2/Mn-ZSM-5复合催化剂的光催化-臭氧耦合降解乙醛》.《分子催化》.2010,第24卷(第1期),摘要,第64页第1节至第66页第2节. * |
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Application publication date: 20100922 Assignee: Zhejiang Minghua air purification technology Co., Ltd. Assignor: Shanghai Jiaotong Univ. Contract record no.: 2016330000158 Denomination of invention: Photocatalysis coupled catalyst based on ozone and preparation method thereof Granted publication date: 20120613 License type: Exclusive License Record date: 20161219 |