CN102343265A - Nano-silver catalyst used for CO oxidation at normal temperature and preparation method thereof - Google Patents
Nano-silver catalyst used for CO oxidation at normal temperature and preparation method thereof Download PDFInfo
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- CN102343265A CN102343265A CN201110208943XA CN201110208943A CN102343265A CN 102343265 A CN102343265 A CN 102343265A CN 201110208943X A CN201110208943X A CN 201110208943XA CN 201110208943 A CN201110208943 A CN 201110208943A CN 102343265 A CN102343265 A CN 102343265A
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Abstract
The invention discloses a nano-silver catalyst used for CO oxidation at room temperature and a preparation method thereof. The catalyst comprises silver as a catalytic active component and SiO2 as a carrier. The catalyst is prepared by two steps of: preparing the SiO2 carrier by adopting a template method; and then preparing an Ag/SiO2 catalyst by adopting an impregnation method by taking SiO2 as the carrier. The SiO2 prepared in the invention has high specific surface area, and the catalyst has better stability, can be used for catalyzing CO to be completely converted at room temperature, has the activity basically unchanged after being used for 48h, and has a wide industrial application prospect.
Description
Technical field
The present invention relates to a kind of loaded nano silver catalyst that can make the CO oxidation at normal temperatures and preparation method thereof, specifically relating to silver is active component, SiO
2Be the catalyst of carrier, this catalyst is catalysis CO oxidation reaction at normal temperatures, and has good stability.Belong to inorganic nano catalysis material field.
Background technology
Along with development of modern industry, environmental pollution is on the rise, and preventing the pollution of the environment becomes the key subjects that are related to national economy.
Get into 21st century; The automobile industry fast development; Automobile exhaust pollution has become one of main source of atmosphere pollution; CO then is one of major pollutants in the vehicle exhaust, and vcehicular tunnel and the CO in the underground motor vehicle passage that causes severe contamination because of motor-vehicle tail-gas purified, and the normal temperature CO catalyst of exploitation efficient stable has very important significance.
Silver-colored in noble metal Au, Pt, cheapnesss such as Pd have commercial application prospect preferably.But not very desirable for CO oxidation, purification effect at present.Frey, K etc. utilize coprecipitation to prepare Ag/TiO
2Catalyst reaches 50% (Frey, K at the conversion ratio of 60 ℃ of following CO; Iablokov, V; Melaet, G; Guczi, L; Kruse, N.Catal.Lett.2008,124,74-79).Xu, R etc. utilize hydro-thermal method and the synthetic MnO of infusion process
2Carrier and Ag/MnO
2Catalyst reaches 90% (Xu, R at the conversion ratio of 126 ℃ of following CO; Wang, X; Wang, D.S; Zhou, K.B; Li, Y.D.J.Catal.2006,237,426-430.).Yu, LB etc. utilize one-step method to synthesize Ag/SiO
2Catalyst reaches 90% (Yu, L.B at the conversion ratio of 137 ℃ of following CO; Shi, Y.Y; Zhao, Z; Yin, H.B; Wei, Y.C; Liu, J; Kang, W.B; Jiang, T.S; Wang, A.L.Catal.Commun.2011,12,616-620).Dai, YM etc. utilize the heat chemistry evaporation precipitation method and infusion process synthesizing carbon nanotubes carrier and Ag/C catalyst, reach 100% (Dai, Y.M at the conversion ratio of 70 ℃ of following CO; Pan, T.C; Liu, W.J; Jehng, J.M.Appl.Catal.B2011,103,221-225).At present, Liu, HY etc. utilize a step template to synthesize Ag/SiO
2Catalyst reaches 100% (Liu, H.Y. at the conversion ratio of room temperature CO; Ma, D; Blackley, R.A.; Zhou, W.Z.; Bao, X.H.Chem.Commun.2008,2677-2679.).Because there is the active specy skewness in the one-step method synthetic catalyst when enlarging preparation, in commercial Application its limitation is arranged.
Summary of the invention
The present invention provides a kind of nano-silver catalyst and preparation method of normal temperature CO oxidation support type.
Catalyst of the present invention is made up of catalytic active component and catalyst carrier two parts, and the activity of such catalysts component is Ag, and wherein the content of Ag in catalyst is 2-16wt%; Carrier is SiO
2
The carrier S iO of catalyst
2The preparation of employing template: take by weighing straight chain alkyl amine and be dissolved in the absolute ethyl alcohol, 20-50 ℃ of following vigorous stirring dissolved it fully in water-bath.Add silicon source, deionized water then successively, continue to stir 24-48h, the deionized water washing, suction filtration, 80-120 ℃ of dry 6-24h, 450-750 ℃ of roasting 3-8h prepares the SiO with meso-hole structure
2Carrier.The mole of reactant mixture consists of:
Silicon source: template: absolute ethyl alcohol: deionized water=1: 0.2965: 4-12: 12-36.
Described silicon source is methyl silicate or ethyl orthosilicate;
Described straight chain alkyl amine is lauryl amine, tetradecy lamine, cetylamine or octadecylamine;
Catalyst adopts immersion process for preparing under the condition of lucifuge, to carry out, and the preparation process is following: with SiO
2Carrier is dissolved in the water, under agitation adds silver nitrate, stirs 0.5-1h, leaves standstill, and Ag/SiO is prepared in oven dry
2Catalyst; The time of repose of catalyst is 6-24h; Bake out temperature is 80-120 ℃, and drying time is 6-24h;
In material mixed gas proportioning volume ratio is 1%CO, 0.5-20%O
2, 98.5-79%He, overall flow rate are 30-100ml/min, the active testing continued operation can be applied to catalysis CO low-temperature oxidation with nano-silver catalyst of the present invention.
Nano-silver catalyst of the present invention can not only be at room temperature catalysis CO complete oxidation, and can also keep stability preferably.In addition, this catalyst can also be used as CO selective oxidation, volatile organic contaminant, persistence organic pollutant oxidation, epoxidation of propylene, nitrogen oxide and SO
2Eliminate and wait in the reaction.
The invention has the beneficial effects as follows:
Technology and equipment are simple, and is with low cost, good reproducibility, prepared SiO
2Carrier has the meso-hole structure (aperture is 2-3nm) and the high-specific surface area (900-1100m of homogeneous
2/ g).The Ag/SiO of preparation
2Catalyst has the characteristics of room temperature catalysis CO complete oxidation, and better industrial application prospect is arranged.
The specific embodiment
Embodiment 1
SiO
2The preparation of carrier: the 1.25g lauryl amine joins in the 10ml absolute ethyl alcohol, 25 ℃ of stirrings in the water-bath, and lauryl amine dissolves fully, to forming clear solution.In solution, add 5ml ethyl orthosilicate and 10ml deionized water, constantly stirring reaction 24h.Spend deionised water, filter, 100 ℃ of dry 12h in baking oven, 450 ℃ of calcining 8h in the Muffle furnace can obtain SiO under air atmosphere
2Carrier.
Ag/SiO
2Preparation of catalysts: take by weighing 1gSiO
2Carrier is dissolved in the 5ml water, under agitation adds the 0.063g silver nitrate, continues to stir 1h, leaves standstill 12h, and 100 ℃ of dry 12h prepare 4wt%Ag/SiO in baking oven
2Catalyst.
The activity of such catalysts evaluation is carried out in fixed bed continuous-flow differential reactor, and reactor is the glass U type pipe of internal diameter 4mm, and loaded catalyst is 200mg, and unstripped gas is formed: 1%CO (volume ratio), 20%O
2, 79%He, gas flow rate are 30ml/min, the CO in the reaction 20min afterproduct gas is through being furnished with the GC-7890II gas chromatograph on-line analysis of thermal conductivity cell detector.Active testing shows, uses the 4wt%Ag/SiO of this method preparation
2Catalyst can be with the CO complete oxidation in room temperature, and activity was constant after catalyst used 48h.
Embodiment 2
SiO of the present invention according to embodiment 1
2The preparation method adds the 3.6ml methyl silicate and replaces ethyl orthosilicate.The evaluation method of catalyst is with embodiment 1.Active testing shows, uses the 4wt%Ag/SiO of this method preparation
2Catalyst can be with the CO complete oxidation in room temperature, and activity was constant after catalyst used 48h.
Embodiment 3
SiO of the present invention according to embodiment 1
2The preparation method adopts the 1.8g octadecylamine to replace lauryl amine.The evaluation method of catalyst is with embodiment 1.Active testing shows, uses the 4wt%Ag/SiO of this method preparation
2Catalyst can be with the CO complete oxidation in room temperature, and activity was constant after catalyst used 48h.
Embodiment 4
SiO of the present invention according to embodiment 1
2The preparation method adopts the 1.43g tetradecy lamine to replace lauryl amine to join in the 5ml absolute ethyl alcohol, and the addition of water becomes 15ml.The water-bath temperature becomes 40 ℃, and the silver nitrate addition becomes 0.0315g.The evaluation method of catalyst is with embodiment 1.Active testing shows, uses the 2wt%Ag/SiO of this method preparation
2Catalyst can be with the CO complete oxidation in room temperature, and activity was constant after catalyst used 48h.
Embodiment 4
SiO of the present invention according to embodiment 1
2The preparing carriers method adopts the 1.6g cetylamine to replace lauryl amine to join in the 8ml absolute ethyl alcohol, and the addition of water becomes 12ml.The water-bath temperature becomes 50 ℃, after adding deionized water, stirs 48h, dry 24h under 120 ℃, and Muffle furnace is calcined 3h down for 750 ℃, and the silver nitrate addition becomes 0.2520g.According to the evaluation method of the catalyst of the present invention of embodiment 1, unstripped gas is formed: 1%CO (volume ratio), 0.5%O
2, 98.5%He, gas flow rate are 100ml/min.Active testing shows, uses the 16wt%Ag/SiO of this method preparation
2Catalyst can be with the CO complete oxidation in room temperature, and activity was constant after catalyst used 48h.
Embodiment 5
SiO of the present invention according to embodiment 1
2The preparing carriers method adopts the 1.25g lauryl amine to join in the 12ml absolute ethyl alcohol, and the addition of water becomes 8ml.After adding deionized water, stir 36h, dry 18h under 100 ℃, Muffle furnace is calcined 6h down for 650 ℃, and the silver nitrate addition becomes 0.1260g.According to the evaluation method of the catalyst of the present invention of embodiment 1, unstripped gas is formed: 1%CO (volume ratio), 10%O
2, 89%He, gas flow rate are 50ml/min.Active testing shows, uses the 8wt%Ag/SiO of this method preparation
2Catalyst can be with the CO complete oxidation in room temperature, and activity was constant after catalyst used 48h.
Embodiment 6
Ag/SiO of the present invention according to embodiment 1
2Method for preparing catalyst under agitation adds silver nitrate, continues to stir 0.5h, leaves standstill 24h, 120 ℃ of dry 6h.The evaluation method of catalyst is with embodiment 1.Active testing shows, uses the 4wt%Ag/SiO of this method preparation
2Catalyst can be with the CO complete oxidation in room temperature, and activity was constant after catalyst used 48h.
Claims (4)
1. nano-silver catalyst that is used for the CO normal temperature oxidation, the catalytic active component that it is characterized in that this catalyst is Ag, wherein the content of Ag in catalyst is 2-16wt%; Carrier is SiO
2
2. the preparation method of the said nano-silver catalyst of claim 1 is characterized in that,
The carrier S iO of catalyst
2The preparation of employing template, the preparation process is following: straight chain alkyl amine is dissolved in the absolute ethyl alcohol, and 20-50 ℃ of following vigorous stirring dissolved it fully in water-bath; Add silicon source, deionized water successively, continue to stir 24-48h, spend deionised water, oven dry, roasting again, prepare SiO with meso-hole structure
2Carrier; Bake out temperature is 80-120 ℃, and drying time is 6-24h; Sintering temperature is 450-750 ℃, and roasting time is 3-8h;
The mole of above-mentioned reactant mixture consists of:
Silicon source: straight chain alkyl amine: absolute ethyl alcohol: deionized water=1: 0.2965: 4-12: 12-36;
Described silicon source is methyl silicate or ethyl orthosilicate;
Described straight chain alkyl amine is lauryl amine, tetradecy lamine, cetylamine or octadecylamine;
Catalyst adopts immersion process for preparing under the condition of lucifuge, to carry out, and the preparation process is following: with SiO
2Carrier is dissolved in the water, under agitation adds silver nitrate, stirs 0.5-1h, leaves standstill, and Ag/SiO is prepared in oven dry
2Catalyst; The time of repose of catalyst is 6-24h; Bake out temperature is 80-120 ℃, and drying time is 6-24h;
3. the application of the said nano-silver catalyst of claim 1 is characterized in that, is 1%CO in material mixed gas proportioning volume ratio, 0.5-20%O
2, 98.5-79%He, overall flow rate are 30-100ml/min, the active testing continued operation is applied to catalysis CO low-temperature oxidation.
4. the application of the said nano-silver catalyst of claim 1 is characterized in that, said nano-silver catalyst is as CO selective oxidation, persistence organic pollutant oxidation, epoxidation of propylene, nitrogen oxide and SO
2The catalyst of eliminating.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437666A (en) * | 2014-12-18 | 2015-03-25 | 上海理工大学 | Al-SBA-15 support and Ag/Al-SBA-15 catalyst and preparation method of support and catalyst and application of catalyst in environmental pollution control |
| CN104492458A (en) * | 2014-12-18 | 2015-04-08 | 上海理工大学 | AgCu catalyst as well as preparation method and application thereof in preventing and controlling environmental pollution |
| CN113509903A (en) * | 2020-04-09 | 2021-10-19 | 石河子大学 | Photostimulation response type material and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101890349A (en) * | 2010-06-28 | 2010-11-24 | 大连理工大学 | Preparation method of mesoporous silicon oxide-based silver catalyst and application thereof in carbon monoxide oxidation |
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2011
- 2011-07-25 CN CN201110208943XA patent/CN102343265A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101890349A (en) * | 2010-06-28 | 2010-11-24 | 大连理工大学 | Preparation method of mesoporous silicon oxide-based silver catalyst and application thereof in carbon monoxide oxidation |
Non-Patent Citations (3)
| Title |
|---|
| 《中国科技论文在线》 20090531 闻梦等 "Ag/SiO2催化剂对CO低温催化氧化活性" 第1和2部分 1-4 第4卷, 第5期 * |
| HONGYANG LIU ET AL.: ""Highly active mesostructured silica hosted silver catalysts for CO oxidation using the one-pot synthesis approach"", 《CHEMICAL COMMUNICATIONS》 * |
| 闻梦等: ""Ag/SiO2催化剂对CO低温催化氧化活性"", 《中国科技论文在线》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437666A (en) * | 2014-12-18 | 2015-03-25 | 上海理工大学 | Al-SBA-15 support and Ag/Al-SBA-15 catalyst and preparation method of support and catalyst and application of catalyst in environmental pollution control |
| CN104492458A (en) * | 2014-12-18 | 2015-04-08 | 上海理工大学 | AgCu catalyst as well as preparation method and application thereof in preventing and controlling environmental pollution |
| CN113509903A (en) * | 2020-04-09 | 2021-10-19 | 石河子大学 | Photostimulation response type material and preparation method and application thereof |
| CN113509903B (en) * | 2020-04-09 | 2022-06-28 | 石河子大学 | Photostimulation response type material and preparation method and application thereof |
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Application publication date: 20120208 |