CN108607611A - A kind of Cu-Ce-Zr mixed metal oxide catalysts - Google Patents
A kind of Cu-Ce-Zr mixed metal oxide catalysts Download PDFInfo
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- CN108607611A CN108607611A CN201810354497.5A CN201810354497A CN108607611A CN 108607611 A CN108607611 A CN 108607611A CN 201810354497 A CN201810354497 A CN 201810354497A CN 108607611 A CN108607611 A CN 108607611A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2213—At least two complexing oxygen atoms present in an at least bidentate or bridging ligand
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/60—Simultaneously removing sulfur oxides and nitrogen oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/62—Carbon oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0213—Complexes without C-metal linkages
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0238—Complexes comprising multidentate ligands, i.e. more than 2 ionic or coordinative bonds from the central metal to the ligand, the latter having at least two donor atoms, e.g. N, O, S, P
- B01J2531/0241—Rigid ligands, e.g. extended sp2-carbon frameworks or geminal di- or trisubstitution
Abstract
The present invention relates to a kind of Cu Ce Zr mixed metal oxide catalysts, the aperture of the catalyst is 3~12nm, and specific surface area is 10~40m2/ g, is prepared using following methods：Zirconium source and organic ligand are weighed, them is made to be dissolved completely in solvent, obtains mixed solution；Mixed solution is transferred in the stainless steel cauldron with polytetrafluoroethyllining lining and is reacted, reaction product is obtained；By reaction product washing, filtering, the drying of gained, solid Zr Base Metal organic framework catalysts are obtained；The sources Cu and the sources Ce are supported on solid Zr Base Metal organic framework catalysts by equi-volume impregnating, stands, is dry, then calcined to get.Compared with prior art, catalyst of the present invention uses metallo-organic framework, material structure controllable, not only with high hydrothermal stability but also with prodigious specific surface area, be conducive to the load of Cu and Ce, CO can not only be catalyzed, and high stability can also be kept.
Description
Technical field
The present invention relates to metal organic framework catalysis material fields, and in particular to a kind of Cu-Ce-Zr mixed-metal oxides
Catalyst.
Background technology
Automobile exhaust pollution becomes one of the main source of atmosphere pollution, and CO is then the major pollutants in vehicle exhaust
One of.And the various volatile organic matters come out due to construction material, house decorative material and life and office appliance etc.
Also it in the physical and mental health for endangering the mankind at every moment, is weighed very much so CO the and VOCs catalyst of exploitation efficient stable has
The meaning wanted.The structure of existing metal oxide catalyst material is uncontrollable, does not have high hydrothermal stability and specific surface
Product is catalyzed CO, high stability, prospects for commercial application cannot be kept bad.
Invention content
The purpose of the present invention is exactly to solve the above-mentioned problems and provides a kind of Cu-Ce-Zr mixed-metal oxides catalysis
Agent.
The purpose of the present invention is achieved through the following technical solutions：
The aperture of a kind of Cu-Ce-Zr mixed metal oxide catalysts, the catalyst is 3~12nm, specific surface area 10
~40m2/ g, is prepared using following methods：
(1) zirconium source and organic ligand are weighed, them is made to be dissolved completely in solvent, obtains mixed solution；
(2) mixed solution is transferred in the stainless steel cauldron with polytetrafluoroethyllining lining and is reacted, obtain reaction production
Object；
(3) by the washing of the reaction product of gained, filtering, drying, solid Zr Base Metal organic framework catalysts are obtained；
(4) sources Cu and the sources Ce are supported on solid Zr Base Metal organic framework catalysts by equi-volume impregnating, it is quiet
It sets, dry, then calcined to get to Cu-Ce-Zr mixed metal oxide catalysts.
Preferably, the zirconium source is one kind in zirconium chloride, zirconium sulfate or zirconium acetate.
Preferably, the organic ligand be selected from trimesic acid, terephthalic acid (TPA), 2,5-Dihydroxyterephthalic acid,
One or more of phthalic acid, succinic acid, trimellitic acid, 1,2,3,4- butane tetracarboxylic acid, oxalic acid or succinic acid.
Preferably, the solvent is one in ethyl alcohol, n,N-Dimethylformamide, n,N-dimethylacetamide or ethylene glycol
Kind is several.
Preferably, step (2) stainless steel cauldron reacts 20~24 hours at 120 DEG C.
Preferably, step (4) calcination temperature is 700 DEG C, calcination time 2h.
Preferably, the sources Cu and the sources Ce are respectively CuO and CeO2, load capacity be respectively catalyst 6wt.% and
20wt.%.
Preferably, the catalyst carries out activation process, and when activation process carries out 2-4h, Ring at 400~900 DEG C
Border is pure H2, pure Ar or 30%O2With 70%Ar.
When Cu series catalysts are used for the reaction, good catalytic activity is shown, but its catalytic performance and the gold that is added
It is closely related to belong to oxide.CeO2Material has fabulous storage oxygen oxygen release ability and improves the performance of catalyst thermal stability, with
When active component CuO effects, by synergy, the activity of catalyst is substantially increased.The present invention is by adding ZrO2With CeO2
Solid solution is formed, CeO can be further improved2Oxygen storage capacity, and CeO can be delayed2The formation of crystal grain, by CuO-CeO2-ZrO2
Catalyst system has good CO catalytic oxidation effects applied in the selective oxidation reaction of CO.
The method have the characteristics that：
(1) catalyst uses metallo-organic framework, and material structure is controllable, not only has high hydrothermally stable
Property but also have prodigious specific surface area, be conducive to the load of Cu and Ce.
(2) Cu-Ce-Zr mixed metal oxide catalysts of the present invention can not only be catalyzed CO, and can also keep high steady
It is qualitative.In addition, the catalyst is also used as CO oxidations in hydrogen-rich atmosphere, volatile organic contaminant, contains sulfur dioxide gas
In the reactions such as the NO_x elimination of atmosphere.
(3) preparation process and equipment are simple, reproducible, there is good prospects for commercial application.
Description of the drawings
Fig. 1 is Cu-Ce-Zr mixed metal oxide catalyst X-ray diffractograms；
Fig. 2 is the N of Cu-Ce-Zr mixed metal oxide catalysts2Adsorption-desorption figure；
Fig. 3 is the graph of pore diameter distribution of Cu-Ce-Zr mixed metal oxide catalysts；
Fig. 4 is the TEM figures of Cu-Ce-Zr mixed metal oxide catalysts；
Fig. 5 is the CO oxidation activities of Cu-Ce-Zr mixed metal oxide catalysts with reaction temperature change curve.
Specific implementation mode
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
Metal Zr source zirconium chlorides and organic ligand terephthalic acid (TPA) are weighed by a certain percentage, are made it completely dissolved in N, N- bis-
In methylformamide solvent；Solution is transferred in the stainless steel cauldron with polytetrafluoroethyllining lining and is reacted at 120 DEG C
24 hours；By products therefrom washing, filtering, drying, solid Zr Base Metal organic framework catalysts are obtained；Pass through incipient impregnation
Method adds the sources Cu and the sources Ce, wherein CuO and CeO2Load capacity be respectively 6wt.% and 20wt.%, stand, it is dry.By solid
Zr Base Metal organic backbones loaded Cu, Ce mix products calcine 2h at 700 DEG C and obtain Cu-Ce-Zr mixed-metal oxides
Catalyst.Its XRD, N2Adsorption-desorption, graph of pore diameter distribution, TEM results such as Fig. 1, shown in 2,3,4.
The activity rating of catalyst carries out in fixed bed continuously flows differential reactor, and reactor is the glass of internal diameter 4mm
Glass U-tube, loaded catalyst 100mg, unstripped gas composition：1%CO (volume ratio), 20%O2, 79%He, gas flow rate is
CO after 30ml/min, reaction 20min in product gas passes through the GC-2060 gas chromatographs equipped with thermal conductivity cell detector and divides online
Analysis, reactivity indicate that catalytic activity result is shown in Fig. 5 by the conversion ratio of CO.Active testing shows to prepare using this method
Cu-Ce-Zr mixed metal oxide catalysts 140 DEG C can by CO complete oxidations, have preferable CO catalysis oxidations effect
Fruit, conversion ratio 100%, catalyst is using still there is preferable activity after 48h.
Embodiment 2
According to the preparation method of the present invention of embodiment 1, change activation temperature, in 500 DEG C of reaction atmosphere O2(atmosphere group
At：30%O2, 70%Ar) in pre-process 2h.The evaluation method of catalyst is the same as embodiment 1.The Cu-Ce- prepared using this method
CO complete oxidations can be had preferable CO catalytic oxidation effects, conversion ratio by Zr mixed metal oxide catalysts at 170 DEG C
It is 100%, catalyst is using still there is preferable activity after 48h.
Embodiment 3
According to the preparation method of the present invention of embodiment 1, change activation temperature, in 600 DEG C of reaction atmosphere O2(atmosphere group
At：30%O2, 70%Ar) in pre-process 2h.The evaluation method of catalyst is the same as embodiment 1.The Cu-Ce- prepared using this method
CO complete oxidations can be had preferable CO catalytic oxidation effects, conversion ratio by Zr mixed metal oxide catalysts at 170 DEG C
It is 100%, catalyst is using still there is preferable activity after 48h.
Embodiment 4
According to the preparation method of the present invention of embodiment 1, change activation temperature, in 800 DEG C of reaction atmosphere O2(atmosphere group
At：30%O2, 70%Ar) in pre-process 2h.The evaluation method of catalyst is the same as embodiment 1.The Cu-Ce- prepared using this method
CO complete oxidations can be had preferable CO catalytic oxidation effects, conversion ratio by Zr mixed metal oxide catalysts at 160 DEG C
It is 100%, catalyst is using still there is preferable activity after 48h.
Embodiment 5
According to the preparation method of the present invention of embodiment 1, change activation temperature, in 900 DEG C of reaction atmosphere O2(atmosphere group
At：30%O2, 70%Ar) in pre-process 2h.The evaluation method of catalyst is the same as embodiment 1.The Cu-Ce- prepared using this method
CO complete oxidations can be had preferable CO catalytic oxidation effects, conversion ratio by Zr mixed metal oxide catalysts at 165 DEG C
It is 100%, catalyst is using still there is preferable activity after 48h.
Embodiment 6
According to the preparation method of the present invention of embodiment 1, change activation temperature, in 400 DEG C of reaction atmosphere O2(atmosphere group
At：30%O2, 70%Ar) in pre-process 2h.The evaluation method of catalyst is the same as embodiment 1.The Cu-Ce- prepared using this method
CO complete oxidations can be had preferable CO catalytic oxidation effects, conversion ratio by Zr mixed metal oxide catalysts at 205 DEG C
It is 100%, catalyst is using still there is preferable activity after 48h.
Embodiment 7
According to the preparation method of the present invention of embodiment 1, change activation temperature, in 300 DEG C of reaction atmosphere O2(atmosphere group
At：30%O2, 70%Ar) in pre-process 2h.The evaluation method of catalyst is the same as embodiment 1.The Cu-Ce- prepared using this method
CO complete oxidations can be had preferable CO catalytic oxidation effects, conversion ratio by Zr mixed metal oxide catalysts at 240 DEG C
It is 100%, catalyst is using still there is preferable activity after 48h.
Embodiment 8
According to the preparation method of the present invention of embodiment 1, changes reaction atmosphere, pre-processed in 700 DEG C of reaction atmosphere Ar
2h.The evaluation method of catalyst is the same as embodiment 1.Active testing shows.The Cu-Ce-Zr mixed metal oxygen prepared using this method
CO complete oxidations can be had preferable CO catalytic oxidation effects, conversion ratio 100%, catalyst by compound catalyst at 330 DEG C
Using still there is preferable activity after 48h.
Embodiment 9
According to the preparation method of the present invention of embodiment 1, change reaction atmosphere, in 700 DEG C of reaction atmosphere H2Middle pretreatment
2h.The evaluation method of catalyst is the same as embodiment 1.Active testing shows.The Cu-Ce-Zr mixed metal oxygen prepared using this method
Compound catalyst can be by CO complete oxidations at 370 DEG C, and catalyst is using still there is preferable activity after 48h.
Embodiment 10
According to the preparation method of the present invention of embodiment 1, change soak time, in 700 DEG C of reaction atmosphere O2(atmosphere group
At：30%O2, 70%Ar) in pre-process 1h.The evaluation method of catalyst is the same as embodiment 1.Active testing shows.Use this method
The Cu-Ce-Zr mixed metal oxide catalysts of preparation can still have CO complete oxidations, catalyst using after 48h at 150 DEG C
Preferably activity.
Embodiment 11
According to the preparation method of the present invention of embodiment 1, change soak time, in 700 DEG C of reaction atmosphere O2(atmosphere group
At：30%O2, 70%Ar) in pre-process 3h.The evaluation method of catalyst is the same as embodiment 1.Active testing shows.Use this method
The Cu-Ce-Zr mixed metal oxide catalysts of preparation can still have CO complete oxidations, catalyst using after 48h at 155 DEG C
Preferably activity.
Embodiment 12
According to the preparation method of the present invention of embodiment 1, change soak time, in 700 DEG C of reaction atmosphere O2(atmosphere group
At：30%O2, 70%Ar) in pre-process 4h.The evaluation method of catalyst is the same as embodiment 1.Active testing shows.Use this method
The Cu-Ce-Zr mixed metal oxide catalysts of preparation can still have CO complete oxidations, catalyst using after 48h at 145 DEG C
Preferably activity.
Embodiment 13
According to the preparation method of the present invention of embodiment 1, it is applied to volatile organic contaminant oxidation of formaldehyde, unstripped gas composition
Become：1000ppm formaldehyde, 20%O2, Ar balances, gas flow rate 50ml/min.Active testing shows to prepare using this method
Cu-Ce-Zr mixed metal oxide catalysts at 210 DEG C formaldehyde completely eliminate.
Embodiment 14
According to the preparation method of the present invention of embodiment 1, it is applied to volatile organic contaminant oxidation of formaldehyde, unstripped gas composition
Become：1000ppm toluene, 20%O2, Ar balances, gas flow rate 50ml/min.Active testing shows to prepare using this method
Cu-Ce-Zr mixed metal oxide catalysts at 320 DEG C toluene completely eliminate.
1 Cu-Ce-Zr mixed metal oxide catalyst performance indicators of table
The catalytic performance of 2 Cu-Ce-Zr mixed metal oxide catalysts of table
Claims (8)
1. a kind of Cu-Ce-Zr mixed metal oxide catalysts, which is characterized in that the aperture of the catalyst is 3~12nm, than
Surface area is 10~40m2/ g, is prepared using following methods：
(1) zirconium source and organic ligand are weighed, them is made to be dissolved completely in solvent, obtains mixed solution；
(2) mixed solution is transferred in the stainless steel cauldron with polytetrafluoroethyllining lining and is reacted, obtain reaction product；
(3) by the washing of the reaction product of gained, filtering, drying, solid Zr Base Metal organic framework catalysts are obtained；
(4) sources Cu and the sources Ce are supported on solid Zr Base Metal organic framework catalysts by equi-volume impregnating, stand, is dry
It is dry, then calcined to get to Cu-Ce-Zr mixed metal oxide catalysts.
2. a kind of Cu-Ce-Zr mixed metal oxide catalysts according to claim 1, which is characterized in that the zirconium source
For one kind in zirconium chloride, zirconium sulfate or zirconium acetate.
3. a kind of Cu-Ce-Zr mixed metal oxide catalysts according to claim 1, which is characterized in that described organic
Ligand is selected from trimesic acid, terephthalic acid (TPA), 2,5- dihydric para-phthalic acids, M-phthalic acid, succinic acid, inclined benzene front three
One or more of acid, 1,2,3,4- butane tetracarboxylic acid, oxalic acid or succinic acid.
4. a kind of Cu-Ce-Zr mixed metal oxide catalysts according to claim 1, which is characterized in that the solvent
For one or more of ethyl alcohol, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide or ethylene glycol.
5. a kind of Cu-Ce-Zr mixed metal oxide catalysts according to claim 1, which is characterized in that step (2)
Stainless steel cauldron reacts 20~24 hours at 120 DEG C.
6. a kind of Cu-Ce-Zr mixed metal oxide catalysts according to claim 1, which is characterized in that step (4)
Calcination temperature is 700 DEG C, calcination time 2h.
7. a kind of Cu-Ce-Zr mixed metal oxide catalysts according to claim 1, which is characterized in that the sources Cu
It is respectively CuO and CeO2 with the sources Ce, load capacity is respectively the 6wt.% and 20wt.% of catalyst.
8. a kind of Cu-Ce-Zr mixed metal oxide catalysts according to claim 1, which is characterized in that the catalysis
Agent carries out activation process, and when activation process carries out 2-4h at 400~900 DEG C, and gaseous environment is pure H2, pure Ar or 30%O2With
70%Ar.
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Cited By (6)
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| CN109289911A (en) * | 2018-10-11 | 2019-02-01 | 中国科学院大学 | A kind of catalyst handling nitrogenous volatile organic contaminant and method |
| CN110951088A (en) * | 2019-12-13 | 2020-04-03 | 安徽大学 | Zirconium-based metal organic framework material, preparation and application as chromium removal agent |
| CN111085214A (en) * | 2019-12-31 | 2020-05-01 | 华东理工大学 | Cu-Co-Ce ternary metal oxide catalyst and preparation method and application thereof |
| CN111185181A (en) * | 2020-01-08 | 2020-05-22 | 北京机械设备研究所 | Acetic acid catalytic oxidation amorphous catalyst, preparation method and catalytic oxidation process |
| CN111185234A (en) * | 2020-01-08 | 2020-05-22 | 北京机械设备研究所 | Acetic acid catalytic oxidation supported catalyst, preparation method and catalytic oxidation process |
| CN113304603A (en) * | 2021-04-27 | 2021-08-27 | 广州紫科环保科技股份有限公司 | Porous MOFs metal oxide and application thereof in purifying atmosphere |
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|---|---|---|---|---|
| CN109289911A (en) * | 2018-10-11 | 2019-02-01 | 中国科学院大学 | A kind of catalyst handling nitrogenous volatile organic contaminant and method |
| CN109289911B (en) * | 2018-10-11 | 2021-06-08 | 中国科学院大学 | Catalyst and method for treating nitrogen-containing volatile organic pollutants |
| CN110951088A (en) * | 2019-12-13 | 2020-04-03 | 安徽大学 | Zirconium-based metal organic framework material, preparation and application as chromium removal agent |
| CN111085214A (en) * | 2019-12-31 | 2020-05-01 | 华东理工大学 | Cu-Co-Ce ternary metal oxide catalyst and preparation method and application thereof |
| CN111185181A (en) * | 2020-01-08 | 2020-05-22 | 北京机械设备研究所 | Acetic acid catalytic oxidation amorphous catalyst, preparation method and catalytic oxidation process |
| CN111185234A (en) * | 2020-01-08 | 2020-05-22 | 北京机械设备研究所 | Acetic acid catalytic oxidation supported catalyst, preparation method and catalytic oxidation process |
| CN111185181B (en) * | 2020-01-08 | 2023-02-03 | 北京机械设备研究所 | Acetic acid catalytic oxidation amorphous catalyst, preparation method and catalytic oxidation process |
| CN111185234B (en) * | 2020-01-08 | 2023-02-21 | 北京机械设备研究所 | Acetic acid catalytic oxidation supported catalyst, preparation method and catalytic oxidation process |
| CN113304603A (en) * | 2021-04-27 | 2021-08-27 | 广州紫科环保科技股份有限公司 | Porous MOFs metal oxide and application thereof in purifying atmosphere |
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