CN104014339A - Anode aluminum oxide loaded core-shell type catalyst - Google Patents
Anode aluminum oxide loaded core-shell type catalyst Download PDFInfo
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- CN104014339A CN104014339A CN201410247395.5A CN201410247395A CN104014339A CN 104014339 A CN104014339 A CN 104014339A CN 201410247395 A CN201410247395 A CN 201410247395A CN 104014339 A CN104014339 A CN 104014339A
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Abstract
The invention discloses an anode aluminum oxide loaded core-shell type catalyst. The catalyst comprises an anode aluminum oxide nano tube array carrier and a core-shell structure unit Pd@CeO2, wherein the anode aluminum oxide nano tube array carrier has a regular pore structure; the mass percent of Pd is 0.05%-2% and the mass percent of CeO2 is 0.5%-10%. The catalyst is obtained by the steps of: synthesizing the Pd@CeO2 core-shell structure unit by a chemical self-assembling method; absorbing and adsorbing the Pd@CeO2 structure unit on the surface of anode aluminum oxide from a solution and roasting to obtain the anode aluminum oxide loaded core-shell type catalyst. The prepared catalyst has the characteristics of high activity and good stability in a catalytic combustion reaction of organic gas including methane, toluene and the like.
Description
Technical field
The present invention relates to a kind of hud typed catalyst of anodised aluminium load for the combustion reaction of organic gas compound for catalysis, belong to environmentally conscious materials, environment and energy catalysis and environmental protection technical field.
Background technology
Organic gas compound, especially methane and VOCs(Volatile Organic Compounds), be important industrial chemicals and energy fuel on the one hand, be also the important gas pollutant of a class on the other hand.Catalyst combustion reaction is with respect to conventional combustion method, have that initiation temperature is low, burning completely and the feature such as secondary pollution is few, no matter in organic gas burning energy supply field, or be all the method that has most application prospect eliminating aspect organic exhaust gas discharge.Wherein, the research and development of effective catalyst and utilization are the primary study objects in catalytic combustion field always.
At present, with CeO
2, SiO
2, TiO
2, ZrO
2deng indifferent oxide, as shell, protect core metal component, " core@shell " structured catalysis material of composition causes people's concern gradually in catalytic combustion field.Oxide shell can stop carbon deposit as protective layer, prevents the reunion of active component, improves the stable of kernel.Meanwhile, rely on cooperative effect unique between nucleocapsid component, in the inside of its sealing, will form a microenvironment, carry out adsorbing separation, bringing into play the effect of double-function catalyzing, can improve process activity and selectivity.Particularly metal@cerium is catalyst based, because the features such as its catalytic activity is high, oxygen storage capacity is strong are widely studied.Patent CN102527382 has reported kind metal-supported cerium-based core-shell structure catalyst and preparation method thereof, and coprecipitation and hydro-thermal method are combined and prepared a series of M@CeO
2(M=Ag, Cu, Pd) catalyst, but prepared kernel metal simple-substance particle is larger, and size is 15 ~ 25 nm.Cargnello etc. (Science, 2012,337:713-717) by the method for self assembly, synthesized Pd@CeO
2nucleocapsid structure, and loaded on
al
2o
3upper for methyl hydride catalyzed reaction, result confirms that reactant molecule can react effectively on Pd nano particle, the catalytic performance super common impregnated load type catalyst far away of catalyst, and with Pd CeO
2the distribution of construction unit on carrier is relevant.But these catalyst are still faced with some challenges, as the structural instability of catalyst, easily inactivation and activity still need further raising etc.Existing document shows, the size of metallic particles and carrier granular in catalyst, and interface interaction is between the two having a strong impact on the performance of catalyst.Simultaneously, the structure and composition of carrier has a great impact catalytic reaction, for example, in range scale tens to several thousand nanometer range, the size of catalyst pores and topological structure can have influence on flowing of reactant, the time of contact of the distribution of active sites and reactant and catalyst (Chemical Engineering Journal, 2005,109:11-36).When the special activity when catalyst is very high, the diffusion process between reactive component and catalyst is the important factor in order of organic gas catalytic combustion operating characteristics.But the structural design of existing metal load type catalyst and synthetic aspect still exist between activity, stability and reaction practical application and are related to phase disconnection problem at present, and this has seriously restricted improvement and the application of catalyst performance.
Summary of the invention
The problem facing for above-mentioned organic gas catalyst for catalytic combustion, the object of the invention is in order to solve conventional load type noble metal catalyst poor stability, the shortcomings such as the not high and mass-transfer performance of activity is poor, provide that a kind of long-range is unordered, short distance presents regular ordered structure for organic gas catalytic combustion class integral catalyzer and preparation method thereof.
Select nucleocapsid structure Pd@CeO
2as active component, porous anodic aluminium oxide prepared by electrochemistry anodic oxidation (AAO) is as carrier.Because AAO pore size homogeneous, and queueing discipline is orderly, has good orientation, can supported catalyst in each nano-pore, and utilize its confinement effect can effectively reduce the impact of sintering of catalyst inactivation.And reactive component can enter from the one end in hole, reaction and diffusion in hole, flow out from the other end in hole.In concept, each nano-pore can be as an independent nanometer microreactor, reactive component diffusion length is within it short, time of contact more homogeneous and easy-regulating more, as shown in schematic diagram 1.
In order to realize above-mentioned technical purpose, technical solution of the present invention is:
The hud typed catalyst of anodised aluminium load, described catalyst comprises anodised aluminium nano-tube array carrier and nucleocapsid structure unit Pd@CeO
2.The weight of catalyst of take is 100%, and the mass percent of noble metal active component Pd is 0.05% ~ 2%, CeO
2mass percent be 0.5% ~ 20%,, surplus is anodised aluminium nano-tube array carrier.CeO
2mass percent be preferably 5% ~ 10%.
The preparation method of the hud typed catalyst of described anodised aluminium load comprises the steps:
(1) using anodised aluminium nano-tube array as carrier, this carrier is carried out to roasting pretreatment;
(2) by the synthetic Pd@CeO of Chemical self-assembly method
2nucleocapsid structure unit;
(3) anodized aluminum support after roasting is added and contain Pd@CeO
2in the solution of nucleocapsid structure unit, normal temperature stirred overnight, 40 ℃ revolve steaming except desolventizing, obtain pressed powder, are placed in 120 ℃ of dried overnight, and roasting in Muffle furnace, obtains the hud typed catalyst of anodised aluminium load.
Described Pd@CeO
2the preparation method of nucleocapsid structure unit comprises following steps:
(1) at ambient temperature, the mol ratio stirring and dissolving that ammonium ceric nitrate and Decanol are pressed to 1:5 ~ 1:3 is in 30 ~ 60 ml methyl alcohol, methanol solution of sodium methylate 15 ~ 25 ml that the mass fraction that dropwise adds fresh configuration under stirring is 28% ~ 31%, continue again to stir after 1 ~ 3 hour, revolve and steam except desolventizing.Add 10 ~ 30 ml carrene lysate again, revolve and steam except desolventizing, and repeat twice, cross filtering precipitation, revolve and steam desolventizing, obtain grease product certain herbaceous plants with big flowers base cerium oxide.
(2) presoma that contains precious metals pd is dissolved in 5 ~ 10 ml distilled water, add again 15 ~ 30 ml carrene and four n-octyl bromination ammoniums (TOABr) (0.119mmol) as stabilizing agent and phase transfer reagent, stir 20 ~ 50 minutes, in separatory funnel, stratification is removed after inorganic phase, add 15 ~ 30 ml acetone and 11-sulfydryl hendecanoic acid (MUA) to stir, the mol ratio of Pd and MUA is: 1:2 ~ 3:1.Then methanol solution 10 ml that add reducing agent canopy sodium hydride, aluminum hydride reason or citric acid one of to receive, stir reduction 1 hour, the mol ratio of reducing agent and Pd is 3:1 ~ 10:1, filter and use twice of 15 ~ 30 ml acetone repeated washing sediment, finally use methanol solution (THF) the dissolution precipitation thing of 10 ~ 30 ml acidifyings, filter and collect black MUA-Pd solution.
(3) MUA-M solution is slowly joined in the THF solution of certain herbaceous plants with big flowers base cerium oxide of 10 ml, separately the n-dodecane acid solution being dissolved in 10ml THF is added, the mol ratio of dodecanoic acid and certain herbaceous plants with big flowers base cerium oxide is 1:1 ~ 1:3, more slowly drips HF hydrolyzate (1.2 ml H
2o
10 ml HF), dripping mixing time is 2 ~ 12 hours, makes and contains M@CeO
2the solution of nucleocapsid structure unit.
Described anodized aluminum support pre-calcination temperature is 300 ~ 900 ℃, and preferably 700 ~ 900 ℃, roasting time is 3 ~ 24 hours, preferably 6 ~ 12 hours.The dried catalyst of described load, its sintering temperature is 300 ~ 900 ℃, preferably 500 ~ 700 ℃, roasting time is 3 ~ 24 hours, preferably 6 ~ 12 hours.
Described anodised aluminium nano-tube array carrier has regular pore structure, and its preparation method is prior art, and those skilled in the art can obtain above-mentioned carrier according to disclosed various preparation methods in prior art.Illustrative methods includes but not limited to the methods and apparatus disclosed in patent CN 1222943, CN 1609283, CN 101603191, CN 101831682 and ZL 201320008947.8 etc.
Described noble metal active component presoma is Pd (acac)
2, Pd (Ac)
2, Pd (NO
3)
2, K
2pdCl
4, in palladium bichloride one of.Above-mentioned noble metal active component presoma can be used alone, but also also mix together.
By the hud typed catalyst of anodised aluminium load of the present invention, for organic gas catalyst combustion reactions such as low-concentration methane and toluene, can be by most or all methane or toluene in system compared with (methane: 90% conversion temperature is lower than 450 ℃ under temperate condition, toluene: 90% conversion temperature is lower than 250 ℃) be carbon dioxide and water, there is no the accessory substances such as formic acid, carbon monoxide and methyl formate, conversion ratio can be up to 100%.
Compared with prior art, the present invention has following beneficial effect:
The hud typed catalyst of anodised aluminium load of the present invention, compares with support type graininess noble metal catalyst, and the diffusional resistance of this catalyst under identical purification efficiency is little, and catalytic efficiency is high, is assembled in the energy consumption causing after cleaning equipment low.With cellular integrated catalyst, compare, this catalyst does not need to introduce coating, and due to the confinement effect of regular nano-pore structure to noble metal granule, and shell CeO
2protective effect to noble metal core, carrier and active component bond strength are large, and catalyst stability is good.
The service condition of the hud typed catalyst of described anodised aluminium load is simple, easy to operate, can be effective to the organic gas catalyst combustion reactions such as methane and toluene, and just can catalytic oxidation methane compared with under temperate condition and the organic gas molecule such as toluene be carbon dioxide and water, there is no the accessory substances such as formic acid, carbon monoxide and methyl formate, conversion ratio can be up to 100%, and catalyst amount is few.
Accompanying drawing explanation
Fig. 1 is the hud typed catalyst schematic diagram of anodised aluminium load.
The specific embodiment
For the present invention is described better, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1
The hud typed catalyst of anodised aluminium load, described catalyst is by anodised aluminium nano-tube array carrier and nucleocapsid structure unit Pd@CeO
2.Anodised aluminium caliber is ~ 100 nm, and at 900 ℃, preroast is 6 hours.The percentage by weight that the weight of catalyst of take is 100%, Pd is 1%, CeO
2percentage by weight be 9%.Described nucleocapsid structure unit Pd@CeO
2preparation process is: described Pd@CeO
2the preparation method of nucleocapsid structure unit comprises following steps: (1) at ambient temperature, the mol ratio stirring and dissolving that ammonium ceric nitrate and Decanol are pressed to 1:4 is in 50 ml methyl alcohol, in the situation that stirring, methanol solution of sodium methylate 20 ml that the mass fraction that dropwise adds fresh configuration is 31%, continue again to stir after 1 hour, revolve and steam except desolventizing.Add 15 ml carrene lysate again, revolve and steam except desolventizing, and repeat twice, cross filtering precipitation, revolve and steam desolventizing, obtain grease product certain herbaceous plants with big flowers base cerium oxide.(2) 25.8 mg tetrachloro-palladium potassium chlorates are dissolved in 5 ml distilled water, add again 15 ml carrene and four n-octyl bromination ammoniums (TOABr) (0.119mmol) as stabilizing agent and phase transfer reagent, stir 30 minutes, in separatory funnel, stratification is removed after inorganic phase, add 15 ml acetone and 11-sulfydryl hendecanoic acid (MUA) to stir, the mol ratio of Pd and MUA is: 1:1.Then methanol solution 10 ml that add reducing agent canopy sodium hydride, stir reduction 1 hour, the mol ratio of reducing agent and Pd is 10:1, filter and use twice of 15 ml acetone repeated washing sediment, finally use methanol solution (THF) the dissolution precipitation thing of 15 ml acidifyings, filter and collect black MUA-Pd solution.(3) MUA-Pd solution is slowly joined in the THF solution of the certain herbaceous plants with big flowers base cerium oxide that 10 ml contain 0.0756 g, separately the n-dodecane acid solution being dissolved in 10 ml THF is added, the mol ratio of dodecanoic acid and certain herbaceous plants with big flowers base cerium oxide is 1:1, more slowly drips HF hydrolyzate (1.2 ml H
2o
10 ml HF), dripping mixing time is 2 hours, makes and contains Pd@CeO
2the solution of nucleocapsid structure unit.
Anodized aluminum support after 0.8 gram of roasting is added and contains Pd@CeO
2in the solution of nucleocapsid structure unit, normal temperature stirred overnight, 40 ℃ revolve and steam except desolventizing, obtain pressed powder, are placed in 120 ℃ of dried overnight, and in Muffle furnace, roasting 6 hours at 700 ℃, obtains the hud typed catalyst of anodised aluminium load.
Embodiment 2:
The hud typed catalyst of anodised aluminium load, described catalyst is by anodised aluminium nano-tube array carrier and nucleocapsid structure unit Pd@CeO
2.Anodised aluminium caliber is ~ 100 nm, and at 900 ℃, preroast is 6 hours.The percentage by weight that the weight of catalyst of take is 100%, Pd is 0.28 %, CeO
2percentage by weight be 2.52%.Described nucleocapsid structure unit Pd@CeO
2preparation process is: described Pd@CeO
2the preparation method of nucleocapsid structure unit comprises following steps: (1) at ambient temperature, the mol ratio stirring and dissolving that ammonium ceric nitrate and Decanol are pressed to 1:4 is in 50 ml methyl alcohol, in the situation that stirring, methanol solution of sodium methylate 20 ml that the mass fraction that dropwise adds fresh configuration is 31%, continue again to stir after 1 hour, revolve and steam except desolventizing.Add 15 ml carrene lysate again, revolve and steam except desolventizing, and repeat twice, cross filtering precipitation, revolve and steam desolventizing, obtain grease product certain herbaceous plants with big flowers base cerium oxide.(2) 14.0 mg palladium bichlorides are dissolved in 5 ml distilled water, add again 15 ml carrene and four n-octyl bromination ammoniums (0.119mmol) as stabilizing agent and phase transfer reagent, stir 30 minutes, in separatory funnel, stratification is removed after inorganic phase, add 15 ml acetone and 11-sulfydryl hendecanoic acid (MUA) to stir, the mol ratio of Pd and MUA is: 1:1.Then methanol solution 10 ml that add reducing agent canopy sodium hydride, stir reduction 1 hour, the mol ratio of reducing agent and Pd is 10: 1, filter and use twice of 15 ml acetone repeated washing sediment, finally use methanol solution (THF) the dissolution precipitation thing of 15 ml acidifyings, filter and collect black MUA-Pd solution.(3) MUA-Pd solution is slowly joined in the THF solution of the certain herbaceous plants with big flowers base cerium oxide that 10 ml contain 0.0756 g, separately the n-dodecane acid solution being dissolved in 10 ml THF is added, the mol ratio of dodecanoic acid and certain herbaceous plants with big flowers base cerium oxide is 1:1, more slowly drips HF hydrolyzate (1.2 ml H
2o
10 ml HF), dripping mixing time is 2 hours, makes and contains Pd@CeO
2the solution of nucleocapsid structure unit.
Anodized aluminum support after 2.9 grams of roastings is added and contains Pd@CeO
2in the solution of nucleocapsid structure unit, normal temperature stirred overnight, 40 ℃ revolve and steam except desolventizing, obtain pressed powder, are placed in 120 ℃ of dried overnight, and in Muffle furnace, roasting 6 hours at 600 ℃, obtains the hud typed catalyst of anodised aluminium load.
Embodiment 3:
Get respectively catalyst described in 200 mg embodiment 1-2, be positioned over and in tubular fixed-bed reactor, carry out toluene and methane catalytic combustion reaction experiment.Toluene catalytically combustion reaction experiment condition: oxygen 20%, nitrogen 80%, toluene gas, by bubbling, is blown into reaction system by nitrogen, and controlling Reactor inlet toluene concentration is 300 ppm, and air speed is 30000 ml g
-1h
-1, reaction temperature is 50 ~ 300 ℃, by charging, discharging toluene concentration, calculates toluene conversion.Methane catalytic combustion reaction experiment condition: air speed is 30000 ml g
-1h
-1, its proportioning is CH
4: O
2: N
2=1:20:79.Under normal pressure, reaction atmosphere, continuously by reaction bed, carries out the activity rating of catalyst within the scope of 200 ~ 600 ℃, by charging, discharging methane concentration, calculates methane conversion.Activity rating result is as shown in table 1, and under the reaction temperature of listed 95% conversion ratio of table 1, and embodiment synthesized catalyst can stable operation more than 50 hours.
Table 1 catalyst activity evaluation result
| ? | Embodiment 1 | Embodiment 2 |
| Toluene (>) 95% conversion ratio reaction temperature | 225 ℃ | 250 ℃ |
| Methane (>) 95% conversion ratio reaction temperature | 425℃ | 475 ℃ |
Claims (7)
1. the hud typed catalyst of anodised aluminium load, is characterized in that, described catalyst comprises anodised aluminium nano-tube array carrier and nucleocapsid structure unit Pd CeO
2.
2. the hud typed catalyst of anodised aluminium load as claimed in claim 1, is characterized in that, described anodised aluminium nano-tube array carrier has regular pore passage structure.
3. the hud typed catalyst of anodised aluminium load as claimed in claim 1, is characterized in that, the weight of catalyst of take is 100%, and the mass percent of noble metal active component Pd is 0.05% ~ 2%, CeO
2mass percent be 0.5% ~ 20%, surplus is anodised aluminium nano-tube array carrier.
4. the preparation method of the hud typed catalyst of anodised aluminium load described in claim 1, is characterized in that, comprises the steps:
(1) using anodised aluminium nano-tube array as carrier, this carrier is carried out to roasting pretreatment;
(2) by the synthetic Pd@CeO of Chemical self-assembly method
2nucleocapsid structure unit;
(3) mode to flood, by Pd@CeO
2the absorption of nucleocapsid structure unit is distributed on carrier anodised aluminium, and the carrier after then dipping being absorbed revolves steaming evaporate to dryness, and roasting in Muffle furnace, obtains the hud typed catalyst of anodised aluminium load.
5. preparation method as claimed in claim 4, is characterized in that, described anodized aluminum support, and its pre-calcination temperature is 300 ~ 900 ℃, roasting time is 3 ~ 24 hours.
6. preparation method as claimed in claim 4, is characterized in that, the Pd@CeO that step (2) is described
2the preparation method of nucleocapsid structure unit comprises the following steps:
(1) at ambient temperature, the mol ratio stirring and dissolving that ammonium ceric nitrate and Decanol are pressed to 1:5 ~ 1:3 is in 30 ~ 60 ml methyl alcohol, methanol solution of sodium methylate 15 ~ 25 ml that the mass fraction that dropwise adds fresh configuration under stirring is 28 ~ 31%, then continue to stir after 1 ~ 3 hour, revolve and steam except desolventizing; Add 10 ~ 30 ml carrene lysate again, revolve and steam except desolventizing, and repeat twice, cross filtering precipitation, revolve and steam desolventizing, obtain grease product certain herbaceous plants with big flowers base cerium oxide;
(2) presoma that contains precious metals pd is dissolved in 5 ~ 10 ml distilled water, add again 15 ~ 30 ml carrene and four n-octyl bromination ammoniums as stabilizing agent and phase transfer reagent, stir 20 ~ 50 minutes, in separatory funnel, stratification is removed after inorganic phase, add 15 ~ 30 ml acetone and 11-sulfydryl hendecanoic acid to stir, the mol ratio of Pd and MUA is: 1:2 ~ 3:1; Then methanol solution 10 ml that add one of reducing agent canopy sodium hydride, aluminum hydride reason or natrium citricum, stir reduction 1 hour, the mol ratio of reducing agent and Pd is 3:1 ~ 10:1, filter and use twice of 15 ~ 30 ml acetone repeated washing sediment, finally use the dissolve with methanol solution sediment of 10 ~ 30 ml acidifyings, filter and collect black MUA-Pd solution;
(3) MUA-Pd solution is slowly joined in the THF solution of certain herbaceous plants with big flowers base cerium oxide of 10 ml, separately the n-dodecane acid solution being dissolved in 10 ml THF is added, the mol ratio of dodecanoic acid and certain herbaceous plants with big flowers base cerium oxide is 1:1 ~ 1:3, slowly drip again HF hydrolyzate, dripping mixing time is 2 ~ 12 hours, makes and contains Pd@CeO
2the solution of nucleocapsid structure unit.
7. the preparation method of the hud typed catalyst of anodised aluminium load described in claim 1, is characterized in that comprising the steps, the anodized aluminum support after 0.5 ~ 5 g roasting is added and contains Pd@CeO
2in the solution of nucleocapsid structure unit, normal temperature stirred overnight, 40 ℃ revolve steaming except desolventizing, obtain pressed powder, are placed in 120 ℃ of dried overnight.
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Cited By (6)
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| CN105200480A (en) * | 2015-10-30 | 2015-12-30 | 苏州莲池环保科技发展有限公司 | Preparation method of automobile exhaust catalyst |
| CN108465466A (en) * | 2018-03-20 | 2018-08-31 | 福州大学 | A kind of spheric catalyst and preparation method thereof of ceria package Pd |
| CN109364931A (en) * | 2018-11-05 | 2019-02-22 | 江南大学 | A kind of hydrogenation of carbon dioxide catalyst for methanol of core-shell structure and preparation method thereof |
| CN112642490A (en) * | 2019-10-12 | 2021-04-13 | 兰溪市向荣电子电器有限公司 | Preparation method of high-efficiency catalyst for hard anodizing of cast aluminum and die-cast aluminum |
| CN113368810A (en) * | 2021-07-14 | 2021-09-10 | 南京信息工程大学 | Core-shell VOCs adsorbent and preparation method thereof |
| CN115845839A (en) * | 2022-11-22 | 2023-03-28 | 东莞理工学院 | Catalyst for low-concentration methane combustion and preparation method thereof |
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Cited By (8)
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| CN105200480A (en) * | 2015-10-30 | 2015-12-30 | 苏州莲池环保科技发展有限公司 | Preparation method of automobile exhaust catalyst |
| CN108465466A (en) * | 2018-03-20 | 2018-08-31 | 福州大学 | A kind of spheric catalyst and preparation method thereof of ceria package Pd |
| CN108465466B (en) * | 2018-03-20 | 2020-08-07 | 福州大学 | Cerium dioxide-coated Pd spherical catalyst and preparation method thereof |
| CN109364931A (en) * | 2018-11-05 | 2019-02-22 | 江南大学 | A kind of hydrogenation of carbon dioxide catalyst for methanol of core-shell structure and preparation method thereof |
| CN112642490A (en) * | 2019-10-12 | 2021-04-13 | 兰溪市向荣电子电器有限公司 | Preparation method of high-efficiency catalyst for hard anodizing of cast aluminum and die-cast aluminum |
| CN113368810A (en) * | 2021-07-14 | 2021-09-10 | 南京信息工程大学 | Core-shell VOCs adsorbent and preparation method thereof |
| CN113368810B (en) * | 2021-07-14 | 2023-06-02 | 南京信息工程大学 | Core-shell VOCs adsorbent and preparation method thereof |
| CN115845839A (en) * | 2022-11-22 | 2023-03-28 | 东莞理工学院 | Catalyst for low-concentration methane combustion and preparation method thereof |
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