CN1562463A - Method for preparing load type T102 photocatalyst in plasma under low temperature and atmospheric pressure - Google Patents
Method for preparing load type T102 photocatalyst in plasma under low temperature and atmospheric pressure Download PDFInfo
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- CN1562463A CN1562463A CN 200410021241 CN200410021241A CN1562463A CN 1562463 A CN1562463 A CN 1562463A CN 200410021241 CN200410021241 CN 200410021241 CN 200410021241 A CN200410021241 A CN 200410021241A CN 1562463 A CN1562463 A CN 1562463A
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- Prior art keywords
- atmospheric pressure
- photochemical catalyst
- barrier discharge
- supported titanium
- low temperature
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- 238000000034 method Methods 0.000 title claims description 20
- 239000011941 photocatalyst Substances 0.000 title abstract description 3
- 230000004888 barrier function Effects 0.000 claims abstract description 37
- 239000002243 precursor Substances 0.000 claims abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 28
- 239000010936 titanium Substances 0.000 claims description 28
- 229910052719 titanium Inorganic materials 0.000 claims description 28
- 239000003054 catalyst Substances 0.000 claims description 18
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000003595 mist Substances 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 6
- 238000007599 discharging Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 67
- 239000007789 gas Substances 0.000 description 10
- 230000008859 change Effects 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000002294 plasma sputter deposition Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000003483 aging Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- -1 oxonium ion Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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Abstract
A process for preparing the carried TiO2 photocatalyst by low-temp plasma under atmosphere pressure features that under the condition of atmosphere pressure and low temp (ordinary temp -300 deg.C), it is directly prepared from the mixture of Ti-contained precursor vapor and O2 or water vapour by use of medium to barrier discharging plasma. The carrier is loaded in the discharge gap or is just the barrier medium.
Description
Technical field
The invention belongs to the conductor photocatalysis technical field, relate to a kind of preparation method of load type titania photocatalyst.
Background technology
TiO
2Because of have the high and anti-photoetch of photocatalytic activity, chemical property is stable, indissoluble is nontoxic and advantage such as applied range, so be at present generally acknowledged comparatively ideal photochemical catalyst.It generates electron-hole pair under ultraviolet light irradiation, produce corresponding active oxygen (as OH base, mistake oxonium ion), and its oxidability is also higher than ozone, so TiO
2Photochemical catalyst have from clean, eliminate multiple functions such as environmental contaminants, antibiotic and deodorizing.Yet Powdered TiO
2In use there is easily cohesion, easily runs off, separates and reclaims between difficulty, powder particle problems such as covering of light.The effective way that addresses this problem is to use support type (being also referred to as film-type) TiO
2Photochemical catalyst.Supported titanium
2The preparation method of photochemical catalyst can be divided into liquid phase method and vapor phase method two big classes.
The main sol-gel process that adopts in liquid phase method, this method generally is predecessor with the titanium salt, makes the stable film sol that is coated with through hydrolysis, stirring and ageing, then this colloidal sol is coated on the matrix, last drying roasting makes.This technology is time-consuming loaded down with trivial details, and the performance of load layer is all multifactor relevant with the size of polymer, the degree of branching, the degree of cross linking and sintering temperature and atmosphere etc., deals with improperly slightly, will occur that photocatalytic activity reduces, film has the crack or with problems such as matrix bond is not firm.Chinese patent 03118762.5 provides a kind of method for preparing titanium deoxid film with sol-gel process on porous ceramics.Chinese patent 02125716.7 is to add the pore creating material carbon black in the process of preparation colloidal sol, is made into coating and is coated on the substrate, can obtain porous photocatalytic titania film after the roasting.
Vapor phase method mainly utilizes technology such as chemical vapor deposition (CVD), plasma activated chemical vapour deposition (PCVD), plasma sputtering.Wherein, utilize plasma chemical vapor deposition technique or plasma sputtering technology, can prepare supported titanium at low temperatures
2Photochemical catalyst.Provide a kind of method of utilizing magnetron sputtering at surface preparation optically catalytic TiO 2 films such as glass, metal, potteries as Chinese patent 01134335.4.Existing plasma prepares supported titanium
2The method of photochemical catalyst mainly is to utilize low pressure (10
-1～10
2Pa) plasma technique, there are problems such as sedimentation rate is low, energy consumption height in electric discharge device and vacuum system investment cost height.This will be very limited on commercial Application.
Summary of the invention
The purpose of this invention is to provide and a kind ofly under atmospheric pressure and low temperature, utilize dielectric barrier discharge plasma technique to prepare supported titanium
2The new method of photochemical catalyst.
Technical scheme of the present invention is that a certain amount of titanium precursor thing steam is carried in carrier gas (as argon gas etc.), and mixes at the dielectric barrier discharge reactor with the gas that contains oxygen or moisture vapor.The high-field electrode of this dielectric barrier discharge reactor and earth electrode adopt coaxial-type or plate-plank frame, and two electrodes are blanket dielectric layer or wherein an electrode blanket dielectric layer or a dielectric impedance are placed between two electrodes simultaneously.Carrier fills in the discharge air-gap, or directly with block media as TiO
2The carrier of photochemical catalyst.Ac high-voltage or the burst pulse square wave direct current high pressure of 50Hz-50kHz are put on this dielectric barrier discharge reactor.Under atmospheric pressure and low temperature (room temperature--300 ℃) condition, mist through action of plasma, is promptly directly prepared TiO on carrier surface in this dielectric barrier discharge reactor
2Photochemical catalyst.
Effect of the present invention and benefit provide under atmospheric pressure utilizes dielectric barrier discharge plasma to prepare supported titanium
2The new method of photochemical catalyst, preparation technology is simple, the needing no vacuum device, energy consumption is low, and the unstripped gas consumption is few, need not high-temperature roasting.Utilize this method can under atmospheric pressure and low temperature, prepare highly active supported titanium
2Photochemical catalyst.
The specific embodiment
Below in conjunction with technical scheme, be described in detail the specific embodiment of the present invention.
Embodiment 1
One coaxial-type dielectric barrier discharge reactor: the stainless steel high-field electrode of diameter 6mm places the axle center of the quartz glass tube of internal diameter 17mm, and the stainless (steel) wire earth electrode closely is wrapped in the quartz glass tube outside.Effectively region of discharge length is 30mm.With 6ml γ-Al
2O
3Fill in this dielectric barrier discharge reactor.Reactor is heated to 150 ℃.By flow is that the Ar gas of 10ml/min carries TiCl at normal temperatures
4Steam and flow are the O of 20ml/min
2Carry H at normal temperatures
2O steam mixes in the dielectric barrier discharge reactor.Frequency is 50Hz, and peak-to-peak value is that the sine wave AC high pressure of 27.2kV puts on this dielectric barrier discharge reactor, under atmospheric pressure discharges 1 hour, makes supported titanium
2/ γ-Al
2O
3Get the prepared supported titanium of 3ml then
2/ γ-Al
2O
3, put in the 10ml initial concentration is the HCHO solution of 0.87 μ g/ml and estimate.At 8W, the uv light irradiation of 253.7nm was according to 0.5 hour, and the formaldehyde conversion ratio is 61%.Other gets 3ml γ-Al
2O
3Carrier, also put to the 10ml initial concentration be in the HCHO solution of 0.87 μ g/ml, and equally at 8W, the uv light irradiation of 253.7nm 0.5 hour, concentration of formaldehyde do not have to change substantially.
Embodiment 2
Adopt embodiment 1 used medium barrier discharge reactor.With 6ml γ-Al
2O
3Fill in this dielectric barrier discharge reactor.Reactor is heated to 200 ℃.By flow is that the Ar gas of 10ml/min carries TiCl at normal temperatures
4Steam and flow are the O of 20ml/min
2Carry H at normal temperatures
2O steam mixes in the dielectric barrier discharge reactor.Frequency is 50Hz, and peak-to-peak value is that the sine wave AC high pressure of 27.2kV puts on this dielectric barrier discharge reactor, under atmospheric pressure discharges 1 hour, makes supported titanium
2/ γ-Al
2O
3Get the prepared supported titanium of 3ml then
2/ γ-Al
2O
3, put in the 10ml initial concentration is the HCHO solution of 0.87 μ g/ml and estimate.At 8W, the uv light irradiation of 253.7nm was according to 0.5 hour, and the formaldehyde conversion ratio is 75%.Other gets 3ml γ-Al
2O
3Carrier, also put to the 10ml initial concentration be in the HCHO solution of 0.87 μ g/ml, and equally at 8W, the uv light irradiation of 253.7nm 0.5 hour, concentration of formaldehyde do not have to change substantially.
Embodiment 3
Adopt embodiment 1 used medium barrier discharge reactor.With 6ml γ-Al
2O
3Fill in this dielectric barrier discharge reactor.Reactor is heated to 250 ℃.By flow is that the Ar gas of 10ml/min carries TiCl at normal temperatures
4Steam and flow are the O of 20ml/min
2Carry H at normal temperatures
2O steam mixes in the dielectric barrier discharge reactor.Frequency is 50Hz, and peak-to-peak value is that the sine wave AC high pressure of 27.2kV puts on this dielectric barrier discharge reactor, under atmospheric pressure discharges 1 hour, makes supported titanium
2/ γ-Al
2O
3Get the prepared supported titanium of 3ml then
2/ γ-Al
2O
3, put in the 10ml initial concentration is the HCHO solution of 0.87 μ g/ml and estimate.At 8W, the uv light irradiation of 253.7nm was according to 0.5 hour, and the formaldehyde conversion ratio is 42%.Other gets 3ml γ-Al
2O
3Carrier, also put to the 10ml initial concentration be in the HCHO solution of 0.87 μ g/ml, and equally at 8W, the uv light irradiation of 253.7nm 0.5 hour, concentration of formaldehyde do not have to change substantially.
Embodiment 4
Adopt embodiment 1 used medium barrier discharge reactor.With 6ml γ-Al
2O
3Fill in this dielectric barrier discharge reactor.Reactor is heated to 300 ℃.By flow is that the Ar gas of 10ml/min carries TiCl at normal temperatures
4Steam and flow are the O of 20ml/min
2Carry H at normal temperatures
2O steam mixes in the dielectric barrier discharge reactor.Frequency is 50Hz, and peak-to-peak value is that the sine wave AC high pressure of 27.2kV puts on this dielectric barrier discharge reactor, under atmospheric pressure discharges 1 hour, makes supported titanium
2/ γ-Al
2O
3Get the prepared supported titanium of 3ml then
2/ γ-Al
2O
3, put in the 10ml initial concentration is the HCHO solution of 0.87 μ g/ml and estimate.At 8W, the uv light irradiation of 253.7nm was according to 0.5 hour, and the formaldehyde conversion ratio is 47%.Other gets 3ml γ-Al
2O
3Carrier, also put to the 10ml initial concentration be in the HCHO solution of 0.87 μ g/ml, and equally at 8W, the uv light irradiation of 253.7nm 0.5 hour, concentration of formaldehyde do not have to change substantially.
Embodiment 5
Adopt embodiment 1 used medium barrier discharge reactor.With 6ml γ-Al
2O
3Fill in this dielectric barrier discharge reactor.Reactor is heated to 200 ℃.By flow is that the Ar gas of 10ml/min carries TiCl at normal temperatures
4Steam and flow are the O of 20ml/min
2Carry H at normal temperatures
2O steam mixes in the dielectric barrier discharge reactor.Frequency is 50Hz, and peak-to-peak value is that the sine wave AC high pressure of 30.6kV puts on this dielectric barrier discharge reactor, under atmospheric pressure discharges 1 hour, makes supported titanium
2/ γ-Al
2O
3Get the prepared supported titanium of 3ml then
2/ γ-Al
2O
3, put in the 10ml initial concentration is the HCHO solution of 1.67 μ g/ml and estimate.At 8W, the uv light irradiation of 253.7nm was according to 0.5 hour, and the formaldehyde conversion ratio is 59%.Other gets 3ml γ-Al
2O
3Carrier, also put to the 10ml initial concentration be in the HCHO solution of 1.67 μ g/ml, and equally at 8W, the uv light irradiation of 253.7nm 0.5 hour, concentration of formaldehyde do not have to change substantially.
Embodiment 6
Adopt embodiment 1 used medium barrier discharge reactor.With 6ml γ-Al
2O
3Fill in this dielectric barrier discharge reactor.Reactor is heated to 200 ℃.By flow is that the Ar gas of 10ml/min carries TiCl at normal temperatures
4Steam and flow are the O of 20ml/min
2Carry H at normal temperatures
2O steam mixes in the dielectric barrier discharge reactor.Frequency is 50Hz, and peak-to-peak value is that the sine wave AC high pressure of 34kV puts on this dielectric barrier discharge reactor, under atmospheric pressure discharges 1 hour, makes supported titanium
2/ γ-Al
2O
3Get the prepared supported titanium of 3ml then
2/ γ-Al
2O
3, put in the 10ml initial concentration is the HCHO solution of 1.51 μ g/ml and estimate.At 8W, the uv light irradiation of 253.7nm was according to 0.5 hour, and the formaldehyde conversion ratio is 66%.Other gets 3ml γ-Al
2O
3Carrier, also put to the 10ml initial concentration be in the HCHO solution of 1.51 μ g/ml, and equally at 8W, the uv light irradiation of 253.7nm 0.5 hour, concentration of formaldehyde do not have to change substantially.
Embodiment 7
Adopt embodiment 1 used medium barrier discharge reactor.With 6ml γ-Al
2O
3Fill in this dielectric barrier discharge reactor.Reactor does not heat.By flow is that the Ar gas of 10ml/min carries TiCl at normal temperatures
4Steam and flow are the O of 20ml/min
2Carry H at normal temperatures
2O steam mixes in the dielectric barrier discharge reactor.Frequency is 5kHz, and peak-to-peak value is that the sine wave AC high pressure of 13.0kV puts on this dielectric barrier discharge reactor, under atmospheric pressure discharges 1 hour, makes supported titanium
2/ γ-Al
2O
3Get the prepared supported titanium of 3ml then
2/ γ-Al
2O
3, put in the 10ml initial concentration is the HCHO solution of 2.63 μ g/ml and estimate.At 8W, the uv light irradiation of 253.7nm was according to 0.5 hour, and the formaldehyde conversion ratio is 86%.Other gets 3ml γ-Al
2O
3Carrier, also put to the 10ml initial concentration be in the HCHO solution of 2.63 μ g/ml, and equally at 8W, the uv light irradiation of 253.7nm 0.5 hour, concentration of formaldehyde do not have to change substantially.
Embodiment 8
Get 10mg P-25 powder TiO
2Photochemical catalyst (Degussa company) joins in the formalin that the 40ml initial concentration is 2.34 μ g/ml, stirs 15min, ultrasonic 15min, and getting wherein, 10ml does the photocatalysis experiment.At 8W, the uv light irradiation of 253.7nm 0.5 hour, formaldehyde conversion ratio are 83%.Other gets the above-mentioned 10ml of containing P-25 TiO
2Formalin place 30min (no uv light irradiation), concentration of formaldehyde not have variation substantially.Getting the 10ml initial concentration more in addition is that 2.34 μ g/ml do not have P-25 TiO
2Formalin illumination 0.5 hour under identical uviol lamp, concentration of formaldehyde does not change substantially yet.
Claims (3)
1. low temperature plasma prepares supported titanium under the atmospheric pressure
2The method of photochemical catalyst is characterized in that utilizing the mist that contains titanium precursor thing steam and contain oxygen or moisture vapor, by dielectric barrier discharge plasma, directly prepares supported titanium under atmospheric pressure and cryogenic conditions
2Photochemical catalyst.
2. low temperature plasma prepares supported titanium under a kind of atmospheric pressure according to claim 1
2The method of photochemical catalyst is characterized in that high-field electrode and earth electrode adopt coaxial-type or plate-plank frame, and two electrodes are blanket dielectric layer simultaneously, or an electrode blanket dielectric layer wherein, or a dielectric impedance is placed between two electrodes.
3. prepare supported titanium according to low temperature plasma under claim 1 and the described a kind of atmospheric pressure of claim 2
2The method of photochemical catalyst is characterized in that carrier fills in the discharge air-gap, or directly with block media as TiO
2The carrier of photochemical catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410021241 CN1562463A (en) | 2004-04-05 | 2004-04-05 | Method for preparing load type T102 photocatalyst in plasma under low temperature and atmospheric pressure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410021241 CN1562463A (en) | 2004-04-05 | 2004-04-05 | Method for preparing load type T102 photocatalyst in plasma under low temperature and atmospheric pressure |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1562463A true CN1562463A (en) | 2005-01-12 |
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ID=34479769
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|---|---|---|---|
| CN 200410021241 Pending CN1562463A (en) | 2004-04-05 | 2004-04-05 | Method for preparing load type T102 photocatalyst in plasma under low temperature and atmospheric pressure |
Country Status (1)
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|---|---|
| CN (1) | CN1562463A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106076304A (en) * | 2016-06-16 | 2016-11-09 | 四川理工学院 | Transesterification supported titanium2the preparation method of catalyst |
| CN106192294A (en) * | 2016-07-29 | 2016-12-07 | 东华大学 | A kind of fast method for assisting daily dirt to remove |
| CN106237843A (en) * | 2016-08-29 | 2016-12-21 | 四川环翔科技有限责任公司 | A kind of air purification method based on lower temperature plasma technology |
-
2004
- 2004-04-05 CN CN 200410021241 patent/CN1562463A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106076304A (en) * | 2016-06-16 | 2016-11-09 | 四川理工学院 | Transesterification supported titanium2the preparation method of catalyst |
| CN106076304B (en) * | 2016-06-16 | 2018-10-09 | 四川理工学院 | Transesterification supported titanium2The preparation method of catalyst |
| CN106192294A (en) * | 2016-07-29 | 2016-12-07 | 东华大学 | A kind of fast method for assisting daily dirt to remove |
| CN106237843A (en) * | 2016-08-29 | 2016-12-21 | 四川环翔科技有限责任公司 | A kind of air purification method based on lower temperature plasma technology |
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