CN100360227C - Method for preparing load type photocatalyst of titania modified by Argentine - Google Patents
Method for preparing load type photocatalyst of titania modified by Argentine Download PDFInfo
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- CN100360227C CN100360227C CNB2005100493688A CN200510049368A CN100360227C CN 100360227 C CN100360227 C CN 100360227C CN B2005100493688 A CNB2005100493688 A CN B2005100493688A CN 200510049368 A CN200510049368 A CN 200510049368A CN 100360227 C CN100360227 C CN 100360227C
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 10
- AILDTIZEPVHXBF-UHFFFAOYSA-N Argentine Natural products C1C(C2)C3=CC=CC(=O)N3CC1CN2C(=O)N1CC(C=2N(C(=O)C=CC=2)C2)CC2C1 AILDTIZEPVHXBF-UHFFFAOYSA-N 0.000 title claims description 9
- 244000308495 Potentilla anserina Species 0.000 title claims description 9
- 235000016594 Potentilla anserina Nutrition 0.000 title claims description 9
- 238000000034 method Methods 0.000 title abstract description 9
- 239000007789 gas Substances 0.000 claims abstract description 25
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims abstract description 20
- 229940071536 silver acetate Drugs 0.000 claims abstract description 20
- 239000010936 titanium Substances 0.000 claims abstract description 18
- 239000011261 inert gas Substances 0.000 claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010453 quartz Substances 0.000 claims abstract description 12
- 229910052709 silver Inorganic materials 0.000 claims abstract description 11
- 239000004332 silver Substances 0.000 claims abstract description 10
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 238000000151 deposition Methods 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000012159 carrier gas Substances 0.000 claims description 15
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 230000008021 deposition Effects 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 13
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000741 silica gel Substances 0.000 claims description 4
- 229910002027 silica gel Inorganic materials 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 11
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 230000032683 aging Effects 0.000 abstract description 2
- 239000000969 carrier Substances 0.000 abstract 2
- 238000001354 calcination Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- -1 silver modified titanium dioxide Chemical class 0.000 abstract 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 19
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000007592 spray painting technique Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
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Abstract
The present invention relates to a method for preparing supported photocatalysts of silver modified titanium dioxide. The method has the following steps: 1) carriers are put into a quartz reactor, maintained for 15 to 60 minutes after being heated to 373 to 573K, and then maintained at the level of 673 to 1073K after being continuously heated; titanium predecessors are heated to 323 to 523K, inert gas is taken as the supporting gas, the titanium predecessors are carried into the quartz reactor, and TiO2 is deposited on the surfaces of the carriers; 3) silver acetate is heated to 373 to 473K, inert gas is also taken as the supporting gas, the silver acetate is carried into the reactor, silver is deposited on the surface of titanium dioxide, and calcination is carried out for 1 to 3 hours under the protection of the inert gas. The method omits the steps of saturation, drying, ageing, reduction, etc. in traditional methods for preparing catalysts, greatly simplifies the process for preparing catalysts and has the advantages of simple equipment and easy industrialization. In addition, Ag particles are small, which can greatly improve the photocatalytic activity of TiO2.
Description
Technical field
The present invention relates to the preparation method of load type photocatalyst of titania modified by Argentine.
Background technology
In 20 years of past, utilize titanium dioxide (TiO
2) the catalyst research of removing water pollutant causes people's attention gradually.But TiO
2In application, there are many problems: (1) TiO
2Recovery very the difficulty; (2) TiO
2Dosage when big, TiO
2Powder is assembled easily, thereby has reduced catalytic activity.Therefore, preparation supported titanium
2Research become the focus of photocatalysis field research.
Adopt sol-gel, spray-painting, reactive sputtering technology, liquid-phase deposition technique can be with TiO
2Load on the carrier, thereby realize TiO
2Recovery, but the TiO of load
2Because its catalytic activity of minimizing of active surface is usually far below Powdered TiO
2Therefore catalyst improves supported titanium
2Catalytic activity have practical meaning.By at TiO
2Surface deposition Ag particle quickens TiO
2Conduction band electron promotes separating of light induced electron and hole to as electron acceptor molecule oxygen transfer velocity, improves quantum yield, is the raising TiO that is widely adopted
2The method of catalytic activity.Big (greater than 10nm) can obstruction TiO for the Ag particle that the employing conventional method deposits such as the light deposition method
2To the absorption of light, TiO
2The raising of photocatalytic activity very limited.Conventional method of modifying such as infusion process complex process are difficult to industrialization, and can cause TiO during modification
2Loss and active the reduction.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology, and cost is lower, the preparation method of high activity loading type photocatalyst of titania modified by Argentine.
The preparation method of load type photocatalyst of titania modified by Argentine of the present invention, employing be Metalorganic Chemical Vapor Deposition, may further comprise the steps:
1) carrier is put into quartz reactor, feed inert gas in reactor, the control gas flow is 50-200ml/min, is heated to 373-573K then and keeps 15-60 minute, continues heating and also remains on 673-1073K;
2) the titanium precursor thing being heated to 323-523K, is carrier gas with the inert gas, and the control gas flow is 100-800ml/min, the titanium precursor thing is downloaded in the quartz reactor, at carrier surface depositing Ti O
2, behind the deposition 1-20h, stopping to be written into the titanium precursor thing, logical inert gas is calcined 1-3h to remove residual part titanium precursor thing under inert gas shielding in reactor;
3) silver acetate being heated to 373-473K, is carrier gas with the inert gas, and the control flow rate of carrier gas is 100-500ml/min; silver acetate is downloaded in the reactor, at the titanium dioxide surface depositing silver, behind the deposition 1-10h; stop to be written into silver acetate, under inert gas shielding, calcine 1-3h.
Among the present invention, said inert gas is nitrogen, argon gas or their mixed gas.The titanium precursor thing is isopropyl titanate or butyl titanate.Said carrier is active carbon, silica gel, molecular sieve, aluminium oxide, stainless steel, carbon fiber or pottery.
The present invention is by control TiO
2With the sedimentation time of silver, can obtain having the catalyst of different Ag/Ti atomic ratios.
Beneficial effect of the present invention is:
1) the present invention has omitted traditional TiO
2Steps such as saturated in the method for preparing catalyst, dry, aging, reduction have been simplified catalyst preparation process greatly.
2) because metal organic chemical vapor deposition (MOCVD) adopts the gas phase predecessor, this makes the Ag particle of deposition have smaller particle size, and is dispersed in TiO
2The surface, thus help to improve TiO
2Photocatalytic activity;
3) equipment is simple, is easy to industrialization.
Description of drawings
Fig. 1 is the X-ray diffractogram of the catalyst of preparation, among the figure, and zero expression Detitanium-ore-type TiO
2Characteristic peak, ● the expression argent characteristic peak;
Fig. 2 is the TEM figure of the catalyst of preparation;
Fig. 3 is the influence of the Ag/Ti atomic ratio of preparation to modified effect, and among the figure: a represents unmodified TiO
2Photochemical catalyst is removed the degradation curve of methyl orange; B, c, d, e, f represent that respectively the Ag/Ti atomic ratio is 0.0198,0.0387,0.0595,0.0792,0.149 silver medal modification TiO
2Photochemical catalyst is removed the degradation curve of methyl orange.
The specific embodiment
Embodiment 1
1) active carbon is put into quartz reactor, feed nitrogen in reactor, the control gas flow is 100ml/min, is heated to 473K then and keeps 60 minutes, continues heating and also remains on 873K;
2) butyl titanate being heated to 423K, is carrier gas with nitrogen, and the control gas flow is 400ml/min, and butyl titanate is downloaded in the quartz reactor, and butyl titanate decomposes the back at activated carbon surface depositing Ti O
2, behind the deposition 10h, stopping to be written into butyl titanate, logical nitrogen is calcined 3h to remove residual part butyl titanate under nitrogen protection in reactor;
3) silver acetate being heated to 473K, is carrier gas with nitrogen, and the control flow rate of carrier gas is 200ml/min, and silver acetate is downloaded in the reactor, and silver acetate decomposes, and at the titanium dioxide surface depositing silver, behind the deposition 5h, stops to be written into silver acetate, calcines 3h under nitrogen protection.
Embodiment 2
1) silica gel is put into quartz reactor, feed argon gas in reactor, the control gas flow is 100ml/min, is heated to 473K then and keeps 30 minutes, continues heating and also remains on 1073K;
2) butyl titanate being heated to 323K, is carrier gas with the argon gas, and the control gas flow is 200ml/min, and butyl titanate is downloaded in the quartz reactor, and butyl titanate decomposes the back at silica gel surface deposition TiO
2, behind the deposition 10h, stopping to be written into butyl titanate, logical argon gas is calcined 1h to remove residual part butyl titanate under argon shield in reactor;
3) silver acetate being heated to 373K, is carrier gas with the argon gas, and the control flow rate of carrier gas is 400ml/min, and silver acetate is downloaded in the reactor, and silver acetate decomposes, and at the titanium dioxide surface depositing silver, behind the deposition 10h, stops to be written into silver acetate, calcines 2h under argon shield.
Embodiment 3
1) stainless steel is put into quartz reactor, feed argon gas in reactor, the control gas flow is 50ml/min, is heated to 373K then and keeps 60 minutes, continues heating and also remains on 773K;
2) isopropyl titanate being heated to 373K, is carrier gas with the argon gas, and the control gas flow is 600ml/min, and isopropyl titanate is downloaded in the quartz reactor, and isopropyl titanate decomposes the back at stainless steel surfaces depositing Ti O
2, behind the deposition 8h, stopping to be written into isopropyl titanate, logical argon gas is calcined 2h to remove residual part isopropyl titanate under argon shield in reactor;
3) silver acetate being heated to 523K, is carrier gas with the argon gas, and the control flow rate of carrier gas is 100ml/min, and silver acetate is downloaded in the reactor, and silver acetate decomposes, and at the titanium dioxide surface depositing silver, behind the deposition 4h, stops to be written into silver acetate, calcines 3h under argon shield.
Fig. 1 is for the X-ray diffractogram of the load type photocatalyst of titania modified by Argentine of employing the present invention preparation, from scheming as seen the TiO of load
2Crystal formation be anatase, silver exist with metallic state.As can be seen from Figure 2, be deposited on TiO
2The Ag particle grain size on surface is 1-5nm.Fig. 3 shows, the TiO after the Ag modification
2Before photocatalytic activity is far longer than modification, and modified effect is best when the atom ratio of Ag and Ti is 0.0595.
Claims (3)
1. the preparation method of load type photocatalyst of titania modified by Argentine is characterized in that may further comprise the steps:
1) carrier is put into quartz reactor, feed inert gas in reactor, the control gas flow is 50-200ml/min, is heated to 373-573K then and keeps 15-60 minute, continues heating and also remains on 673-1073K;
2) the titanium precursor thing being heated to 323-523K, is carrier gas with the inert gas, and the control gas flow is 100-800ml/min, the titanium precursor thing is downloaded in the quartz reactor, at carrier surface depositing Ti O
2, behind the deposition 1-20h, stopping to be written into the titanium precursor thing, logical inert gas is calcined 1-3h to remove residual part titanium precursor thing under inert gas shielding in reactor, and said titanium precursor thing is isopropyl titanate or butyl titanate;
3) silver acetate being heated to 373-473K, is carrier gas with the inert gas, and the control flow rate of carrier gas is 100-500ml/min; silver acetate is downloaded in the reactor, at the titanium dioxide surface depositing silver, behind the deposition 1-10h; stop to be written into silver acetate, under inert gas shielding, calcine 1-3h.
2. the preparation method of load type photocatalyst of titania modified by Argentine according to claim 1 is characterized in that said inert gas is nitrogen, argon gas or their mixed gas.
3. the preparation method of load type photocatalyst of titania modified by Argentine according to claim 1 is characterized in that said carrier is active carbon, silica gel, molecular sieve, aluminium oxide, stainless steel, carbon fiber or pottery.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100493688A CN100360227C (en) | 2005-03-15 | 2005-03-15 | Method for preparing load type photocatalyst of titania modified by Argentine |
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|---|---|---|---|
| CNB2005100493688A CN100360227C (en) | 2005-03-15 | 2005-03-15 | Method for preparing load type photocatalyst of titania modified by Argentine |
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| Publication Number | Publication Date |
|---|---|
| CN1695800A CN1695800A (en) | 2005-11-16 |
| CN100360227C true CN100360227C (en) | 2008-01-09 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102941087A (en) * | 2012-10-25 | 2013-02-27 | 常州大学 | Composite silver-titanium catalyst preparation method |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102000566A (en) * | 2010-10-15 | 2011-04-06 | 徐志兵 | Method for preparing photoactivated silver/titanium dioxide complex |
| CN102580727B (en) * | 2011-01-11 | 2013-12-04 | 同济大学 | Preparation method of active carbon loaded titanium dioxide silver-doped photochemical catalyst |
| CN105465899A (en) * | 2014-09-26 | 2016-04-06 | 福建省辉锐材料科技有限公司 | Air disinfection purifier and photocatalytic film preparation method thereof |
| CN104588004A (en) * | 2015-01-06 | 2015-05-06 | 吉林大学 | Catalyst for ultraviolet photocatalytic degradation of organic pollutants and preparation method thereof |
| CN106139222A (en) * | 2015-04-09 | 2016-11-23 | 藍石環球科技（香港）有限公司 | A kind of photocatalysis film preparation method of air disinfection purification apparatus and use thereof |
| CN105771977A (en) * | 2016-03-22 | 2016-07-20 | 济南大学 | Method for preparing graphene oxide coated carbon fiber-silver loaded TiO2 nano-wire array composite materials and application thereof |
| CN106378122A (en) * | 2016-08-26 | 2017-02-08 | 天津南化催化剂有限公司 | Silica gel loaded titanium catalyst, preparation method and application thereof |
| CN109718859A (en) * | 2019-01-08 | 2019-05-07 | 东北师范大学 | A kind of Ag/TiO2/ MIL-125 (Ti) composite material and preparation method and Morphological control |
| CN113332962A (en) * | 2021-03-31 | 2021-09-03 | 陕西科技大学 | Ag-TiO2Preparation method of/CNF/PTFE composite air purification membrane |
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| CN1459476A (en) * | 2002-05-20 | 2003-12-03 | 中山市华铿喷涂有限公司 | Silver phosphate antibacterial modified titanium dioxide composite particle and preparation method and application thereof |
| CN1513595A (en) * | 2003-07-28 | 2004-07-21 | 西南石油学院 | Adsorption-photo catalyst and its preparation method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1459476A (en) * | 2002-05-20 | 2003-12-03 | 中山市华铿喷涂有限公司 | Silver phosphate antibacterial modified titanium dioxide composite particle and preparation method and application thereof |
| CN1513595A (en) * | 2003-07-28 | 2004-07-21 | 西南石油学院 | Adsorption-photo catalyst and its preparation method |
Non-Patent Citations (2)
| Title |
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| 纳米固体的MOCVD法制备及结构性能的研究. 彭冬生等.材料导报，第17卷第6期. 2003 * |
| 负载型纳米TiO2催化剂的制备及其在难降解有机废水处理中的应用研究. 徐甦，全文，www.cnki.net. 2004 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102941087A (en) * | 2012-10-25 | 2013-02-27 | 常州大学 | Composite silver-titanium catalyst preparation method |
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