CN102389792A - Three-dimensional ordered macroporous LaMnO3 supported high-dispensability MnOx catalyst and preparation method and use thereof - Google Patents
Three-dimensional ordered macroporous LaMnO3 supported high-dispensability MnOx catalyst and preparation method and use thereof Download PDFInfo
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- CN102389792A CN102389792A CN2011103004960A CN201110300496A CN102389792A CN 102389792 A CN102389792 A CN 102389792A CN 2011103004960 A CN2011103004960 A CN 2011103004960A CN 201110300496 A CN201110300496 A CN 201110300496A CN 102389792 A CN102389792 A CN 102389792A
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Abstract
The invention discloses a three-dimensional ordered macroporous (3DOM) LaMnO3 supported high-dispensability MnOx catalyst and a preparation method and use thereof, which belong to the technical field of functional material. The MnOx is loaded on the three-dimensional ordered macroporous LaMnO3, and the MnOx loading capacity is 6.8 weight percent based on MnO2. The preparation method comprises: adding a precursor (manganese nitrate) to be loaded of a metal oxide in the 3DOM LaMnO3 carrier in an added amount when preparing the 3DOM LaMnO3 carrier, wherein the ratio of MnOx to 3DOM LaMnO3 is set to be 6.8 weight percent:1, and the MnOx loading capacity is based on MnO2 so that the MnOX can be loaded when the 3DOM LaMnO3 carrier is prepared. The preparation process of the three-dimensional ordered LaMnO3 supported high-dispensability MnOx catalyst prepared by the method is simple, the particle form and hole size of the product are controllable, and the application prospect in the field of catalytic oxidization of volatile toluene and the like is bright.
Description
Technical field
The present invention relates to a kind of three-dimensional ordered macroporous LaMnO
3The high dispersive MnO of load
xEfficient toluene oxidation Catalysts and its preparation method relates in particular to and adopts glue crystal template method in-situ preparing toluene oxidation to be had the three-dimensional ordered macroporous LaMnO of high catalytic activity
3The high dispersive MnO of load
xCatalyst belongs to technical field of function materials.
Background technology
The volatile organic matter that contains in the industrial waste gas (VOC) is one of main source that causes atmosphere pollution, and is therefore extremely urgent to the research of efficient elimination VOC.Catalytic oxidation is a kind of effective means.Perofskite type oxide (ABO
3) be one type of composite oxides with fault of construction (anion or cation vacancy), the VOC oxidation reaction is demonstrated good catalytic performance, belong to complete oxidation type catalysis material.With ABO
3Process three-dimensional ordered macroporous (3DOM) material, both can improve the material specific area, thereby allowing material to get into from all directions again reduces the material diffusional resistance in the hole, reach more high efficiency for the diffusion of material provides optimum flow rate, and the manganese oxide (MnO of highly dispersed state
x) itself also have good catalytic activity, therefore, 3DOM ABO
3The MnO of load
xCatalyst will demonstrate better physical and chemical performance for the VOC oxidation reaction, have a extensive future as numerous areas such as carrier, catalyst and parting materials.
The general at present glue crystal template method that adopts of 3DOM perofskite type oxide prepares, and existing bibliographical information is crossed employing glue crystal template legal system and is equipped with perofskite type oxide.For example: employing polymethyl methacrylate (PMMA) microballoons such as Kim are hard template; With lanthanum acetate; Manganese acetate and calcium acetate are source metal, are solvent with EGME and ethanol, and the gained predecessor has been made the La with 3DOM structure after 600 ℃ of roastings in air atmosphere
0.7Ca
0.3MnO
3(Y.N.Kim, et al., Solid State Communications, 2003,128:339-343).Employing polystyrene (PS) microballoons such as Sadakane are hard template, and with lanthanum nitrate, strontium nitrate and ferric nitrate are source metal, are solvent with ethylene glycol and methyl alcohol, the gained predecessor have been obtained to have the La of 3DOM structure in air atmosphere after 700 ℃ of roastings
1-xSr
xFeO
3(x=0～0.4) (M.Sadakane, et al., Chemistry of Materials, 2005,17:3546-3551).Employings such as Xu are hard template through the PMMA microballoon of modification, and with lanthanum nitrate, cobalt nitrate and potassium nitrate are source metal, are solvent with ethylene glycol and methyl alcohol, and the gained predecessor has been made the La with 3DOM structure after 700 ℃ of roastings in air atmosphere
1-xK
xCoO
3(x=0～0.3) (J.F.Xu, et al., Journal of Catalysis, 2011,282:1-12).
Transition metal oxide MO
x(M=Mn, Co, Cr, Ni, Fe, V, Cu) contains multiple oxidation state metal ion and lattice defect (oxygen room), helps VOC and O
2Absorption and activation, make said material in the complete oxidation of VOC, show good catalytic activity, wherein with CoO
x, MnO
xAnd CrO
xCatalytic activity be best.With MO
xSupport on the carrier of high-specific surface area, also can further improve its catalytic activity.It is 27000h that reports such as Wyrwalski are worked as air speed
-1When being lower than 290 ℃ with reaction temperature, toluene is at 4.0wt%Co
3O
4/ ZrO
2Conversion ratio on the catalyst reach 100% (F.Wyrwalski, et al., Catalysis Today, 2007,119:332-337).
With an amount of transition metal oxide MO
xNano particle supports the 3DOMABO with high specific surface area
3On the carrier, then can further improve its catalytic performance.MO
xAnd LaMO
3(the M ion in Co) contains multiple oxidation state, has stronger redox ability, in addition MO for M=Cr, Mn
xIn M ion and LaMO
3In the M ion between possibly have synergy, help promoting the oxidation-reduction process of catalyst, thereby help the raising of catalytic activity.Galenda etc. have prepared Fe
2O
3/ La
0.8Sr
0.2Co
0.8Fe
0.2O
3-δCatalyst also is used for the methanol steam reforming reaction, observe preferably catalytic activity (A.Galenda, et al., Journal of Molecular Catalysis A:Chemical, 2008,282:52-61).Transition metal oxide carried MO
xMethod to high specific surface carrier generally adopts equi-volume impregnating, and promptly first synthetic vectors is supported on carrier with metal nitrate or acetate again, forms support type MO through calcination
xCatalyst.As far as we know, also there is not bibliographical information to cross MnO at present
x/ 3DOM LaMnO
3The in-situ preparation method of catalyst and the application study in catalysis elimination toluene thereof.
Summary of the invention
The three-dimensional ordered macroporous LaMnO that the purpose of this invention is to provide a kind of efficient toluene oxidation
3The high dispersive MnO of load
xCatalysts and its preparation method relates in particular to and adopts glue crystal template method in-situ preparing toluene oxidation to be had the three-dimensional ordered macroporous LaMnO of high catalytic activity
3The high dispersive MnO of load
xThe method of catalyst, MnO
xBe manganese oxide, promptly at preparation 3DOM LaMnO
3The addition that to wherein treat the presoma (manganese nitrate) of the metal oxide of load during carrier adds in the lump, is set at 6.8wt%MnO
x/ 3DOM LaMnO
3, MnO
xLoad capacity with MnO
2Meter is so that at preparation 3DOM LaMnO
3Also realized MnO in the time of carrier
xLoading process.
A kind of six side's phase perofskite type oxide LaMnO with three-dimensional ordered macroporous structure
3
Three-dimensional ordered macroporous LaMnO
3The high dispersive MnO of load
xCatalyst is characterized in that, MnO
xLoad on three-dimensional ordered macroporous LaMnO
3On, MnO
xLoad capacity with MnO
2Count 6.8wt%.
Above-mentioned a kind of six side's phase perofskite type oxide LaMnO with three-dimensional ordered macroporous structure
3The preparation method is characterized in that, may further comprise the steps:
According to lanthanum nitrate hexahydrate: mass fraction is 50% Mn (NO
3)
2Mn (NO in the aqueous solution
3)
2Mol ratio is that 1: 1 ratio is dissolved in the PEG400 solution, and the used PEG400 of every 0.01mol lanthanum nitrate is 1mL, and the normal temperature lower magnetic force stirs 4h, forms homogeneous solution; Add methyl alcohol again, wherein every 0.03mol lanthanum nitrate hexahydrate adds 14mL methyl alcohol, continues to be stirred to evenly; Above-mentioned mixed liquor impouring is equipped with in the container of PMMA glue crystal template, makes PMMA glue crystal template thorough impregnation, flood about 5h; Behind suction filtration and the drying at room temperature 12h, the magnetic boat of packing into places tube furnace subsequently, earlier at N
2(20mL/min) rises to 500 ℃ and under this temperature, keep 3h with the speed of 1 ℃/min from room temperature under the atmosphere; Switch to air atmosphere (20mL/min) after waiting to reduce to 50 ℃; Rise to 750 ℃ and under this temperature, keep 4h with the speed of 1 ℃/min again, obtain having six side's phase perofskite type oxide LaMnO of 3DOM structure
3, the aperture is about 140nm.Toluene concentration be 1000ppm, toluene/oxygen mol ratio be 1/400 and air speed be under 20000mL/ (gh) condition, this catalyst T
50%(toluene conversion reaches 50% o'clock desired reaction temperature) and T
90%(toluene conversion reaches 90% o'clock desired reaction temperature) is respectively 241 ℃ and 262 ℃, and body phase LaMnO
3The T of catalyst
50%And T
90%Be respectively 267 ℃ and 298 ℃.
Above-mentioned a kind of three-dimensional ordered macroporous LaMnO
3The high dispersive MnO of load
xMethod for preparing catalyst is characterized in that, may further comprise the steps:
According to lanthanum nitrate hexahydrate: mass fraction is 50% Mn (NO
3)
2Mn (NO in the aqueous solution
3)
2Mol ratio is that 1: 1.166 ratio is dissolved in the PEG400 solution, and the used PEG400 of every 0.01mol lanthanum nitrate is 1mL, and the normal temperature lower magnetic force stirs 4h; Form uniform solution, add methyl alcohol again, wherein every 0.03mol lanthanum nitrate hexahydrate adds 15mL methyl alcohol; Continue to be stirred to evenly, above-mentioned mixed liquor impouring is equipped with in the container of polymethyl methacrylate (PMMA) glue crystal template, make PMMA glue crystal template thorough impregnation; Flood about 5h; Behind suction filtration and the drying at room temperature 12h, the magnetic boat of packing into places tube furnace subsequently, earlier at N
2(20mL/min) rises to 500 ℃ and under this temperature, keep 3h with the speed of 1 ℃/min from room temperature under the atmosphere; Switch to air atmosphere (20mL/min) after waiting to reduce to 50 ℃; Rise to 750 ℃ and under this temperature, keep 4h with the speed of 1 ℃/min again, obtain having the 6.8wt%MnO of 3DOM structure
x/ 3DOM LaMnO
3(MnO
xLoad capacity with MnO
2Meter), the aperture is about 145nm.Toluene concentration be 1000ppm, toluene/oxygen mol ratio be 1/400 and air speed be under 20000mL/ (gh) condition, have the 6.8wt%MnO of single-phase six side's perovskite crystal structures
x/ 3DOM LaMnO
3Catalyst, its T
50%And T
90%Be respectively 224 ℃ and 245 ℃.
Characteristics such as the present invention has low in raw material cost and is easy to get, and the preparation process is simple, and product particle morphology and hole dimension are controlled.
The 3DOM LaMnO of the present invention's preparation
3And 6.8wt%MnO
x/ 3DOM LaMnO
3Have the characteristics of loose structure and degree of crystallinity and MnO preferably
xBe highly dispersed state at carrier surface, have a good application prospect at catalytic field.
Utilize crystal structure, particle morphology and the pore structure of D8ADVANCE type X-ray diffractometer (XRD), ZEISS SUPRA 55 type SEM (SEM), JEOL-2010 type transmission electron microscope (TEM) and Tianjin, island GC-2010 gas-chromatography Instrument measuring gained target products such as (GC) and to the catalytic activity of toluene.The result shows, adopts prepared each sample of method of the present invention all to have 3DOM structure and degree of crystallinity preferably, MnO
xBe highly dispersed state at carrier surface, load MnO
xThe prepared catalyst activity in back is significantly increased.
Description of drawings
Fig. 1 is obtained LaMnO
3And 6.8wt%MnO
x/ 3DOM LaMnO
3The XRD spectra of sample, wherein curve (a) and (b) be respectively the XRD spectra of embodiment 1 and embodiment 2 samples;
Fig. 2 is prepared LaMnO
3And 6.8wt%MnO
x/ 3DOM LaMnO
3The SEM of sample and TEM photo, wherein figure (a) and the HRSEM photo that (c) is respectively embodiment 1 and embodiment 2 samples, figure (b) and (d) be respectively the TEM photo of embodiment 1 and embodiment 2 samples;
Fig. 3 is obtained LaMnO
3And 6.8wt%MnO
x/ 3DOM LaMnO
3Sample is to the catalytic activity curve of toluene oxidation, and the curve (a) and (b) are respectively body LaMnO mutually with (c) among the figure
3, embodiment 1 and embodiment 2 gained samples the catalytic activity curve.
The specific embodiment
Elaborate with embodiment below.For further explanation the present invention, the LaMnO that the present invention obtains toluene oxidation is had the 3DOM structure of excellent catalytic activity is described in conjunction with accompanying drawing
3And 6.8wt%MnO
x/ 3DOM LaMnO
3In order to represent contrast, adopt the body phase LaMnO of sol-gel process preparation
3Sample accompanying drawing is in the lump explained.
Embodiment 1: take by weighing 0.03mol La (NO
3)
36H
2O and 0.03mol mass fraction are 50% Mn (NO
3)
2The aqueous solution places the 50mL beaker, adds the 3mL PEG400, behind the magnetic agitation 4h, forms uniform solution, adds 14mL methyl alcohol again, continues to be stirred to evenly, above-mentioned mixed liquor impouring is equipped with in the 50mL beaker of 1g PMMA.For keeping the original orderly arrangement of PMMA, in this mixed liquor impouring process, do not stir.The at room temperature dry 12h of sample that suction filtration obtains behind the about 5h of mixed liquor dipping PMMA places tube furnace with the sample magnetic boat of packing into, subsequently earlier at N
2(20mL/min) rises to 500 ℃ and under this temperature, keep 3h with the speed of 1 ℃/min from room temperature under the atmosphere; Switch to air atmosphere (20mL/min) after waiting to reduce to 50 ℃; Rise to 750 ℃ and under this temperature, keep 4h with the speed of 1 ℃/min again, promptly obtain having six side's phase perofskite type oxide LaMnO of 3DOM structure
3, macropore diameter is about 140nm.Toluene concentration be 1000ppm, toluene/oxygen mol ratio be 1/400 and air speed be under 20000mL/ (gh) condition, 3DOM LaMnO
3The T of catalyst
50%And T
90%Be respectively 241 ℃ and 262 ℃.
Embodiment 2: take by weighing 0.03mol La (NO
3)
36H
2O and 0.035mol mass fraction are 50% Mn (NO
3)
2The aqueous solution places the 50mL beaker, adds the 3mL PEG400, behind the magnetic agitation 4h, forms homogeneous solution, adds 15mL methyl alcohol again, continues to be stirred to evenly.Above-mentioned mixed liquor impouring is equipped with in the 50mL beaker of 1g PMMA.For keeping the original orderly arrangement of PMMA, in this mixed liquor impouring process, do not stir.The at room temperature dry 12h of sample that suction filtration obtains behind the about 5h of liquid to be mixed dipping PMMA places tube furnace with the sample magnetic boat of packing into subsequently, and is first at N
2(20mL/min) rises to 500 ℃ and under this temperature, keep 3h with the speed of 1 ℃/min from room temperature under the atmosphere; Switch to air atmosphere (20mL/min) after waiting to reduce to 50 ℃; Rise to 750 ℃ and under this temperature, keep 4h with the speed of 1 ℃/min again, promptly obtain having the 6.8wt%MnO of 3DOM structure
X/ LaMnO
3, macropore diameter is about 145nm.Toluene concentration be 1000ppm, toluene/oxygen mol ratio be 1/400 and air speed be under 20000mL/ (g h) condition, have the 6.8wt%MnO of single-phase six side's perovskite type crystal structures
x/ LaMnO
3Catalyst, its T
50%And T
90%Be respectively 224 ℃ and 245 ℃.
The obtained LaMnO of the foregoing description
3And 6.8wt%MnO
x/ 3DOM LaMnO
3The XRD spectra of sample is seen Fig. 1, wherein curve (a) and (b) be respectively the XRD spectra of embodiment 1 and embodiment 2 samples; Prepared LaMnO
3And 6.8wt%MnO
x/ 3DOM LaMnO
3The SEM of sample and TEM photo are seen Fig. 2, wherein figure (a) and the HRSEM photo that (c) is respectively embodiment 1 and embodiment 2 samples, figure (b) and (d) be respectively the TEM photo of embodiment 1 and embodiment 2 samples; Obtained LaMnO
3And 6.8wt%MnO
x/ 3DOMLaMnO
3Sample is seen Fig. 3 to the catalytic activity curve of toluene oxidation, and the curve (a) and (b) are respectively body LaMnO mutually with (c) among the figure
3, embodiment 1 and embodiment 2 gained samples the catalytic activity curve.
Claims (6)
1. three-dimensional ordered macroporous LaMnO
3The high dispersive MnO of load
xCatalyst, MnO
xBe manganese oxide, it is characterized in that, MnO
xLoad on three-dimensional ordered macroporous LaMnO
3On, MnO
xLoad capacity with MnO
2Count 6.8wt%.
2. according to the three-dimensional ordered macroporous LaMnO of claim 1
3The high dispersive MnO of load
xThe Preparation of catalysts method, it is characterized in that may further comprise the steps: according to lanthanum nitrate hexahydrate: mass fraction is 50% Mn (NO
3)
2Mn (NO in the aqueous solution
3)
2Mol ratio is that 1: 1.166 ratio is dissolved in the PEG400 solution, and the used PEG400 of every 0.01mol lanthanum nitrate is 1mL, and the normal temperature lower magnetic force stirs 4h; Form uniform solution, add methyl alcohol again, wherein every 0.03mol lanthanum nitrate hexahydrate adds 15mL methyl alcohol; Continue to be stirred to evenly, above-mentioned mixed liquor impouring is equipped with in the container of polymethyl methacrylate (PMMA) glue crystal template, make PMMA glue crystal template thorough impregnation; Flood about 5h; Behind suction filtration and the drying at room temperature 12h, the magnetic boat of packing into places tube furnace subsequently, earlier at N
2Rise to 500 ℃ and under this temperature, keep 3h with the speed of 1 ℃/min from room temperature under the atmosphere, switch to air atmosphere after waiting to reduce to 50 ℃, rise to 750 ℃ and under this temperature, keep 4h with the speed of 1 ℃/min again, obtain having the 6.8wt%MnO of 3DOM structure
x/ 3DOM LaMnO
3, N wherein
2Atmosphere is 20mL/min, and air atmosphere is 20mL/min.
3. the described three-dimensional ordered macroporous LaMnO of claim 1
3The high dispersive MnO of load
xCatalyst applications in the catalysis toluene oxidation.
4. six side's phase perofskite type oxide LaMnO with three-dimensional ordered macroporous structure
3
5. according to a kind of six side's phase perofskite type oxide LaMnO of claim 4 with three-dimensional ordered macroporous structure
3The preparation method is characterized in that, may further comprise the steps: according to lanthanum nitrate hexahydrate: mass fraction is 50% Mn (NO
3)
2Mn (NO in the aqueous solution
3)
2Mol ratio is that 1: 1 ratio is dissolved in the PEG400 solution, and the used PEG400 of every 0.01mol lanthanum nitrate is 1mL, and the normal temperature lower magnetic force stirs 4h, forms homogeneous solution; Add methyl alcohol again, wherein every 0.03mol lanthanum nitrate hexahydrate adds 14mL methyl alcohol, continues to be stirred to evenly; Above-mentioned mixed liquor impouring is equipped with in the container of PMMA glue crystal template, makes PMMA glue crystal template thorough impregnation, flood about 5h; Behind suction filtration and the drying at room temperature 12h, the magnetic boat of packing into places tube furnace subsequently, earlier at N
2Rise to 500 ℃ and under this temperature, keep 3h with the speed of 1 ℃/min from room temperature under the atmosphere; Switch to air atmosphere after waiting to reduce to 50 ℃; Rise to 750 ℃ and under this temperature, keep 4h with the speed of 1 ℃/min again, obtain having six side's phase perofskite type oxide LaMnO of 3DOM structure
3, N wherein
2Flow is 20mL/min, and air mass flow is 20mL/min.
6. a kind of six side's phase perofskite type oxide LaMnO of claim 4 with three-dimensional ordered macroporous structure
3Be applied to the catalysis toluene oxidation.
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| CN109908951B (en) * | 2019-04-12 | 2020-09-22 | 中国环境科学研究院 | Multi-stage micro-mesoporous low-temperature catalyst and preparation method thereof |
| CN109908952B (en) * | 2019-04-12 | 2020-10-16 | 中国环境科学研究院 | Catalytic coating of volatile organic compound and preparation method thereof |
| CN110639519A (en) * | 2019-10-09 | 2020-01-03 | 北京工业大学 | Three-dimensional ordered mesoporous cerium dioxide loaded Pt-MnO for efficiently catalyzing and oxidizing toluenexCatalyst and process for preparing same |
| CN110639519B (en) * | 2019-10-09 | 2022-07-05 | 北京工业大学 | Three-dimensional ordered mesoporous cerium dioxide loaded Pt-MnO for efficiently catalyzing and oxidizing toluenexCatalyst and process for preparing same |
| CN111905719A (en) * | 2020-08-13 | 2020-11-10 | 清华大学 | Novel manganese-based catalyst and preparation method thereof |
| CN111905719B (en) * | 2020-08-13 | 2021-07-27 | 清华大学 | Manganese-based catalyst and preparation method thereof |
| CN112337461A (en) * | 2020-10-26 | 2021-02-09 | 苏州大学 | Composite material of strontium-doped ordered mesoporous lanthanum manganate-loaded noble metal palladium, preparation method thereof and application thereof in catalytic oxidation of toluene |
| CN112337461B (en) * | 2020-10-26 | 2023-11-03 | 苏州大学 | Composite material of strontium doped ordered mesoporous lanthanum manganate loaded with noble metal palladium, preparation method thereof and application thereof in catalytic oxidation of toluene |
| CN116020445A (en) * | 2022-12-22 | 2023-04-28 | 南昌大学 | La with cation defect x MnO 3±δ Catalyst, preparation method and application |
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