CN107597104A - Oxide carried Pt catalyst of core shell structure and its preparation method and application - Google Patents
Oxide carried Pt catalyst of core shell structure and its preparation method and application Download PDFInfo
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Abstract
Oxide carried Pt catalyst of core shell structure and its preparation method and application belongs to environmental catalysis and technical field of air pollution control.The catalyst is with the SiO with core shell structure2@TiO2For carrier, Pt is active constituent.It is characterized in spherical SiO2For kernel, SiO2Core surface coats TiO2, SiO2@TiO2The generation of core shell structure considerably improves hydrogen selective on Pt catalyst and reduces NOxPerformance, make the catalyst that there is good low-temperature denitration performance.Preparation technology of the present invention is simple, and NO under low temperature can be achievedxEfficient removal, have broad application prospects.
Description
Technical field
The present invention relates to a kind of oxide carried Pt catalyst of core shell structure, preparation method and using the catalyst in richness
Selective Catalytic Reduction of NO under the conditions of oxygenx.Suitable for the stationary source flue gas such as the moving sources such as diesel vehicle and Industrial Boiler, smeltery
Middle NOxElimination, belong to environmental catalysis and technical field of air pollution control.
Background technology
With the growth of energy-consuming and the quick increase of vehicle guaranteeding organic quantity, a large amount of Fossil fuel consumptions cause to be discharged into
NO in airxSwift and violent increase, NOxCan not only caused by the ecological environment problem such as acid rain, haze, also seriously endanger people's
Health.Therefore, how NO is effectively eliminatedxDischarge be current Air Pollution Control and environmental catalysis area research focus.
NH3SCR technology (NH3- SCR) discharge NO in thermal power plantxControl in be used widely.But ammonia
When making reducing agent, traditional vanadium tungsten titanium catalyst is in high-temperature region (300-400 DEG C) due to temperature window, it is impossible to effectively removes machine
Motor-car and the NO of Industrial Boiler dischargex；In addition, leakage of ammonia etc. also limit NH3- SCR application.In recent years, hydrogen selective
Reduce NOx(H2- SCR) cause the highest attention of researcher.When hydrogen makees reducing agent, NOxReduction temperature substantially reduce, and
Excess hydrogen will produce water with oxygen combustion, will not produce secondary pollution.
NO is reduced currently used for hydrogen selectivexCatalyst be mostly noble metal, the problem of existing is that temperature window is narrow, NOx
Conversion ratio have much room for improvement, and noble metal is expensive.Therefore, low precious metal content and the H with high activity are developed2-
SCR denitration, lean-burn gasoline motor car and emission of diesel engine NO can not only be metxElimination, moreover it is possible to applied to Industrial Boiler etc.
Fixed source emission NOxLow-temperature catalyzed removing, have great importance and application prospect.
The present invention is prepared for a kind of at low temperature to NOxThe catalytic eliminating core shell structure oxide with excellent properties bear
Carry Pt catalyst.
The content of the invention
It is an object of the invention to provide a kind of preparation method simply and to hydrogen selective catalytic reduction NOxWith high activity
The oxide carried Pt catalyst of core shell structure and preparation method thereof.In view of the interaction between active component and carrier to urging
The catalytic performance of agent has a significant effect, and the present invention is by synthesizing the SiO with core shell structure2@TiO2Oxide, pass through SiO2
With TiO2Between interaction and core shell structure carrier and precious metals pt between cooperative effect, develop it is a kind of to hydrogen select
Selecting property Reduction of NOxDenitrating catalyst with excellent activity.
The purpose of the present invention is achieved through the following technical solutions：
Catalyst composition is expressed as Pt/SiO2@TiO2, wherein spherical SiO2For kernel, SiO2Core surface coats TiO2, its
Middle shell TiO2With kernel SiO2Mol ratio between 0.1~0.2, Pt quality and SiO2@TiO2The ratio of quality is 0.5
~1%.
The invention provides a kind of preparation method of the oxide carried Pt catalyst of core shell structure, it is characterised in that：The party
Method comprises the following steps successively：
(1) ethanol, ammoniacal liquor and deionized water are stirred to obtain mixed solution, and positive silicic acid is then added into mixed solution
Tetra-ethyl ester, 50-70 DEG C is heated to, water-bath backflow 2-4h.Room temperature is cooled to, reaction solution is then subjected to centrifugal filtration, at 120 DEG C
Under the conditions of dry 12~24 hours, obtain spherical SiO2；
(2) ethanol and butyl titanate ultrasonic mixing are obtained into mixed solution, by spherical SiO obtained by step (1)2Add mixed
Close in solution, ultrasonic 30min, is designated as mixed liquor A after stirring；Ethanol and deionized water are stirred, are designated as solution B；
(3) step (2) resulting solution B is added drop-wise in mixed liquor A, continues stirring reaction 8-12h after being added dropwise, will be molten
Liquid centrifuges, and is dried under the conditions of 120 DEG C 12~24 hours, then roasting 4~8 is small under the conditions of 500 DEG C in Muffle furnace
When, the SiO of obtained core shell structure2@TiO2；
(4) SiO for taking step (3) to obtain2@TiO2, it is ground to powdered, addition 0.01-0.02mol/L chloroplatinic acids or nitre
Sour platinum solution, then stir 2~4 hours, until mixture is in muddy；
(5) the muddy solid obtained by step (4) is dried 12~24 hours under the conditions of 120 DEG C, is subsequently placed in Muffle
Calcined 4~8 hours under the conditions of 450~550 DEG C in stove, Pt/SiO is made2@TiO2Catalyst.
Present invention also offers be used for hydrogen selective reduction NO using the oxide carried Pt catalyst of above-mentioned core shell structurex
Method, it is characterised in that the application process comprises the following steps：
(1) the oxide carried Pt catalyst of core shell structure is loaded among fixed bed reactors, reaction temperature control exists
75~250 DEG C of scopes；
(2) using hydrogen as reducing agent, control total gas flow rate in 200~400ml/min, air speed 43,000~86,
000h-1。
The present invention compared with prior art, has advantages below and high-lighting effect：Using the SiO with core shell structure2@
TiO2As active constituent Pt carrier, acted on by the concerted catalysis between Pt and core shell structure oxide, substantially increase and urge
Agent reduces NO to hydrogen selectivexPerformance, although noble-metal-supported amount is low, there is the catalyst excellent low temperature to take off
Nitre performance.
Brief description of the drawings
Fig. 1 is 0.5%Pt/SiO2The scanning electron microscope (SEM) photograph of catalyst
Fig. 2 is 0.5%Pt/SiO2@TiO2(Ti:Si=1:5) scanning electron microscope (SEM) photograph of catalyst
Specific embodiment
Technical scheme is described further with reference to embodiment：The quality hundred of ammoniacal liquor in example below
It is 25% to divide specific concentration.
Embodiment 1：0.5%Pt/SiO2@TiO2(Ti:Si=1:5) preparation of catalyst
A) 145mL ethanol is taken, 95mL ammoniacal liquor and 20mL deionized waters are stirred to obtain mixed solution, then molten to mixing
50mmol tetraethyl orthosilicates are added in liquid, 50 DEG C is heated to, water-bath backflow 2h, is cooled to room temperature, then carries out reaction solution
Centrifugal filtration, dried 24 hours under the conditions of 120 DEG C, obtain spherical SiO2；
B) 250mL ethanol and 10mmol butyl titanate ultrasonic mixings are obtained into mixed solution, will be spherical obtained by step (a)
SiO2Add in mixed solution, ultrasonic 30min, is designated as mixed liquor A after stirring；50mL ethanol and 250mL deionized waters are stirred
Mixing, is designated as solution B.
C) step (b) resulting solution B is added drop-wise in mixed liquor A, continues stirring reaction 12h after being added dropwise.By solution
Centrifuge, dry 12 hours under the conditions of 120 DEG C, be then calcined 6 hours under the conditions of 500 DEG C in Muffle furnace, core is made
The SiO of shell structure2@TiO2。
D) SiO for taking step (c) to obtain2@TiO2, be ground to it is powdered, add 4.87mL 0.02mol/L chloroplatinic acids it is molten
Liquid, then stir 2 hours, until mixture is in muddy.
E) the muddy solid obtained by step (d) is dried 12 hours under the conditions of 120 DEG C, be subsequently placed in Muffle furnace
Calcined 4 hours under the conditions of 500 DEG C, 0.5%Pt/SiO is made2@TiO2(Ti:Si=1:5) catalyst.
Embodiment 2：0.5%Pt/SiO2@TiO2(Ti:Si=1:7.5) preparation of catalyst
A) 145mL ethanol is taken, 95mL ammoniacal liquor and 20mL deionized waters are stirred to obtain mixed solution, then molten to mixing
50mmol tetraethyl orthosilicates are added in liquid, 70 DEG C is heated to, water-bath backflow 4h, is cooled to room temperature, then carries out reaction solution
Centrifugal filtration, dried 12 hours under the conditions of 120 DEG C, obtain spherical SiO2；
B) 200mL ethanol and 6.67mmol butyl titanate ultrasonic mixings are obtained into mixed solution, by ball obtained by step (a)
Shape SiO2Add in mixed solution, ultrasonic 30min, is designated as mixed liquor A after stirring；50mL ethanol and 200mL deionized waters are stirred
Mixing is mixed, is designated as solution B；
C) step (b) resulting solution B is added drop-wise in mixed liquor A, continues stirring reaction 8h after being added dropwise.By solution from
The heart separates, and dries 24 hours under the conditions of 120 DEG C, is then calcined 4 hours under the conditions of 500 DEG C in Muffle furnace, and nucleocapsid is made
The SiO of structure2@TiO2；
D) SiO for taking step (c) to obtain2@TiO2, be ground to it is powdered, add 4.54mL 0.02mol/L chloroplatinic acids it is molten
Liquid, then stir 2 hours, until mixture is in muddy；
E) the muddy solid obtained by step (d) is dried 24 hours under the conditions of 120 DEG C, be subsequently placed in Muffle furnace
Calcined 8 hours under the conditions of 450 DEG C, 0.5%Pt/SiO is made2@TiO2(Ti:Si=1:7.5) catalyst.
Embodiment 3：0.5%Pt/SiO2@TiO2(Ti:Si=1:10) preparation of catalyst
A) 145mL ethanol is taken, 95mL ammoniacal liquor and 20mL deionized waters are stirred to obtain mixed solution, then molten to mixing
50mmol tetraethyl orthosilicates are added in liquid, 60 DEG C is heated to, water-bath backflow 3h, is cooled to room temperature, then carries out reaction solution
Centrifugal filtration, dried 12 hours under the conditions of 120 DEG C, obtain spherical SiO2；
B) 180mL ethanol and 5.0mmol butyl titanate ultrasonic mixings are obtained into mixed solution, by ball obtained by step (a)
Shape SiO2Add in mixed solution, ultrasonic 30min, is designated as mixed liquor A after stirring；50mL ethanol and 250mL deionized waters are stirred
Mixing is mixed, is designated as solution B；
C) step (b) resulting solution B is added drop-wise in mixed liquor A, continues stirring reaction 10h after being added dropwise.By solution
Centrifuge, dry 12 hours under the conditions of 120 DEG C, be then calcined 8 hours under the conditions of 500 DEG C in Muffle furnace, core is made
The SiO of shell structure2@TiO2；
D) SiO for taking step (c) to obtain2@TiO2, be ground to it is powdered, add 8.72mL 0.01mol/L platinum nitrates it is molten
Liquid, then stir 3 hours, until mixture is in muddy；
E) the muddy solid obtained by step (d) is dried 18 hours under the conditions of 120 DEG C, be subsequently placed in Muffle furnace
Calcined 6 hours under the conditions of 500 DEG C, 0.5%Pt/SiO is made2@TiO2(Ti:Si=1:10) catalyst.
Embodiment 4：1%Pt/SiO2@TiO2(Ti:Si=1:10) preparation of catalyst
A) 145mL ethanol is taken, 95mL ammoniacal liquor and 20mL deionized waters are stirred to obtain mixed solution, then molten to mixing
50mmol tetraethyl orthosilicates are added in liquid, 50 DEG C is heated to, water-bath backflow 4h, is cooled to room temperature, then carries out reaction solution
Centrifugal filtration, dried 24 hours under the conditions of 120 DEG C, obtain spherical SiO2；
B) 180mL ethanol and 5.0mmol butyl titanate ultrasonic mixings are obtained into mixed solution, by ball obtained by step (a)
Shape SiO2Add in mixed solution, ultrasonic 30min, is designated as mixed liquor A after stirring；50mL ethanol and 250mL deionized waters are stirred
Mixing is mixed, is designated as solution B；
C) step (b) resulting solution B is added drop-wise in mixed liquor A, continues stirring reaction 8h after being added dropwise.By solution from
The heart separates, and dries 24 hours under the conditions of 120 DEG C, is then calcined 6 hours under the conditions of 500 DEG C in Muffle furnace, and nucleocapsid is made
The SiO of structure2@TiO2；
D) SiO for taking step (c) to obtain2@TiO2, be ground to it is powdered, add 8.72mL 0.02mol/L platinum nitrates it is molten
Liquid, then stir 2 hours, until mixture is in muddy；
E) the muddy solid obtained by step (d) is dried 24 hours under the conditions of 120 DEG C, be subsequently placed in Muffle furnace
Calcined 4 hours under the conditions of 550 DEG C, 1%Pt/SiO is made2@TiO2(Ti:Si=1:10) catalyst.
Embodiment 5 (reference)：0.5%Pt/SiO2The preparation of catalyst
A) 145mL ethanol is taken, 95mL ammoniacal liquor and 20mL deionized waters are stirred to obtain mixed solution, then molten to mixing
50mmol tetraethyl orthosilicates are added in liquid, are heated to 50 DEG C, water-bath backflow 2h.Room temperature is cooled to, then reaction solution will be entered
Row centrifugal filtration, dried 24 hours under the conditions of 120 DEG C, obtain spherical SiO2；
B) spherical SiO for taking step (a) to obtain2, be ground to it is powdered, add 7.69mL 0.01mol/L chloroplatinic acids it is molten
Liquid, then stir 2 hours, until mixture is in muddy；
C) the muddy solid obtained by step (b) is dried 12 hours under the conditions of 120 DEG C, be subsequently placed in Muffle furnace
Calcined 4 hours under the conditions of 500 DEG C, 0.5%Pt/SiO is made2Catalyst.
Embodiment 6：The preparation method of catalyst is same as Example 1, and 0.2g catalyst is loaded in into fixed bed reactors
Central, reaction gas composition is 0.2%NO, 1%H2, 5%O2, the flow velocity of reaction gas is 200ml/min, air speed 43,000h-1。
Activity rating temperature range is 75~250 DEG C, and under different temperatures, the conversion ratio of catalyst reduction nitrogen oxides is shown in Table 1.
Embodiment 7：The preparation method of catalyst is same as Example 2, and 0.2g catalyst is loaded in into fixed bed reactors
Central, reaction gas composition is 0.2%NO, 1%H2, 5%O2, the flow velocity of reaction gas is 200ml/min, air speed 43,000h-1。
Activity rating temperature range is 75~250 DEG C, and under different temperatures, the conversion ratio of catalyst reduction nitrogen oxides is shown in Table 1.
Embodiment 8：The preparation method of catalyst is same as Example 3, and 0.2g catalyst is loaded in into fixed bed reactors
Central, reaction gas composition is 0.2%NO, 1%H2, 5%O2, the flow velocity of reaction gas is 200ml/min, air speed 43,000h-1。
Activity rating temperature range is 75~250 DEG C, and under different temperatures, the conversion ratio of catalyst reduction nitrogen oxides is shown in Table 1.
Embodiment 9：The preparation method of catalyst is same as Example 4, and 0.2g catalyst is loaded in into fixed bed reactors
Central, reaction gas composition is 0.2%NO, 1%H2, 5%O2, the flow velocity of reaction gas is 200ml/min, air speed 43,000h-1。
Activity rating temperature range is 75~250 DEG C, and under different temperatures, the conversion ratio of catalyst reduction nitrogen oxides is shown in Table 1.
The oxide carried Pt catalyst of the core shell structure of table 1 and reference catalyst Activity evaluation
Claims (3)
1. the oxide carried Pt catalyst of core shell structure, it is characterised in that：It is expressed as Pt/SiO2@TiO2, wherein spherical SiO2For
Kernel, SiO2Core surface coats TiO2, wherein shell TiO2With kernel SiO2Mol ratio between 0.1~0.2, Pt matter
Amount and SiO2@TiO2The ratio of quality is 0.5%~1%.
2. prepare the method for the oxide carried Pt catalyst of core shell structure as claimed in claim 1, it is characterised in that this method
Comprise the following steps successively：
(1) ethanol, ammoniacal liquor and deionized water are stirred to obtain mixed solution, and positive silicic acid tetrem is then added into mixed solution
Ester, 50~70 DEG C are heated to, 2~4h of water-bath backflow；Room temperature is cooled to, reaction solution is then subjected to centrifugal filtration, in 120 DEG C of bars
Dried 12~24 hours under part, obtain spherical SiO2；
(2) ethanol and butyl titanate ultrasonic mixing are obtained into mixed solution, by spherical SiO obtained by step (1)2It is molten to add mixing
In liquid, ultrasonic 30min, is designated as mixed liquor A after stirring；Ethanol and deionized water are stirred, are designated as solution B；
(3) step (2) resulting solution B is added drop-wise in mixed liquor A, continues 8~12h of stirring reaction after being added dropwise, by solution
Centrifuge, dry 12~24 hours under the conditions of 120 DEG C, be then calcined 4~8 hours under the conditions of 500 DEG C in Muffle furnace,
The SiO of core shell structure is made2@TiO2；
(4) SiO for taking step (3) to obtain2@TiO2, it is ground to powdered, addition 0.01-0.02mol/L chloroplatinic acids or platinum nitrate
Solution, then stir 2~4 hours, until mixture is in muddy；
(5) the muddy solid obtained by step (4) is dried 12~24 hours under the conditions of 120 DEG C, be subsequently placed in Muffle furnace
Calcined 4~8 hours under the conditions of 450~550 DEG C, Pt/SiO is made2@TiO2Catalyst.
3. Pt/SiO described in claim 12@TiO2Catalyst is used for hydrogen selective reduction NOxMethod, it is characterised in that bag
Include following steps：
(1) by Pt/SiO2@TiO2Catalyst is loaded among fixed bed reactors, and reaction temperature is controlled in 75~250 DEG C of scopes；
(2) using hydrogen as reducing agent, control total gas flow rate is in 200~400ml/min, air speed 43,000~86,000h-1。
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| CN110975883A (en) * | 2019-12-05 | 2020-04-10 | 东北石油大学 | Preparation method of bifunctional core-shell catalyst for preparing aviation kerosene through carbon dioxide hydrogenation |
| CN115555044A (en) * | 2022-10-10 | 2023-01-03 | 无锡威孚环保催化剂有限公司 | Preparation method of catalyst for NOx pollutants of hydrogen internal combustion engine |
| CN115779927A (en) * | 2022-12-08 | 2023-03-14 | 万华化学集团股份有限公司 | Cobalt-aluminum shell-core composite oxide supported monatomic iridium catalyst and preparation method and application thereof |
| CN116672901A (en) * | 2023-08-04 | 2023-09-01 | 西安金沃泰环保科技有限公司 | Nanofiltration material for acid-containing waste gas and preparation method thereof |
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| CN115779927A (en) * | 2022-12-08 | 2023-03-14 | 万华化学集团股份有限公司 | Cobalt-aluminum shell-core composite oxide supported monatomic iridium catalyst and preparation method and application thereof |
| CN115779927B (en) * | 2022-12-08 | 2024-05-03 | 万华化学集团股份有限公司 | Cobalt-aluminum shell-core composite oxide loaded monoatomic iridium catalyst and preparation method and application thereof |
| CN116672901A (en) * | 2023-08-04 | 2023-09-01 | 西安金沃泰环保科技有限公司 | Nanofiltration material for acid-containing waste gas and preparation method thereof |
| CN116672901B (en) * | 2023-08-04 | 2023-10-27 | 西安金沃泰环保科技有限公司 | Nanofiltration material for acid-containing waste gas and preparation method thereof |
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