CN108993560A - A kind of water resistant, high temperature resistant methane oxidation catalyst and preparation method thereof - Google Patents

A kind of water resistant, high temperature resistant methane oxidation catalyst and preparation method thereof Download PDF

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Publication number
CN108993560A
CN108993560A CN201810824151.7A CN201810824151A CN108993560A CN 108993560 A CN108993560 A CN 108993560A CN 201810824151 A CN201810824151 A CN 201810824151A CN 108993560 A CN108993560 A CN 108993560A
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baco
preparation
methane oxidation
oxidation catalyst
pdo
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杜君臣
冯丰
王成雄
赵德鹏
黄卫强
杨冬霞
李红
张爱敏
赵云昆
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GUIYAN CATALYST CO Ltd KUNMING
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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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/20—Carbon compounds
    • B01J27/232—Carbonates
    • 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
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/864—Removing carbon monoxide or hydrocarbons
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • 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
    • B01D2257/702—Hydrocarbons
    • B01D2257/7022—Aliphatic hydrocarbons
    • B01D2257/7025—Methane
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/20—Capture or disposal of greenhouse gases of methane

Abstract

The invention discloses a kind of water resistant, high temperature resistant methane oxidation catalysts and preparation method thereof.Catalyst is by 0.5-5wt%PdO, 1-10wt%BaCO3, 85-98.5wt%Al2O3It forms, wherein Al2O3With BaCO3Molar ratio be 16.5~190.7；BaCO3/Al2O3Molar ratio with PdO is 7.8~81.4；BaCO3It is 1.25 with PdO molar ratio.Preparation method includes: that Ba presoma is impregnated in Al by (1)2O3On material, BaCO is formed after air roasting3/Al2O3Carrier；(2) Pd presoma is impregnated on carrier made from (1), a kind of PdO/BaCO is made after being air-dried and roasting3/Al2O3Water resistant, high temperature resistant methane oxidation catalyst.Methane oxidation catalyst prepared by the present invention shows excellent methyl hydride catalyzed activity and stability in aqueous atmosphere and hot environment, the catalyst is applicable not only to the exhaust aftertreatment of natural gas vehicle, gasoline car, it may also be used for using natural gas, coal gas, oil liquefied gas as the tail gas clean-up of the burner of fuel.

Description

A kind of water resistant, high temperature resistant methane oxidation catalyst and preparation method thereof
Technical field
The invention belongs to catalysis material preparation technical fields, and in particular to a kind of water resistant, high temperature resistant methane oxidation catalyst and Preparation method.
Background technique
In face of the urgent need of increasingly serious atmosphere polluting problem and Energy restructuring, selection environmental protection, low-carbon can Generative fuel has become inexorable trend.Unique bridge of the natural gas as connection traditional fossil energy and renewable energy, by In rich reserves, technology maturation, cheap, at most potential alternative energy source.
The main component of natural gas is methane.It is unavoidable during being utilized using natural gas as the natural gas resource of fuel Ground can discharge certain density methane residual gas.Methane is as the second largest greenhouse gases, the potentiality that heats of unit volume 21 times of carbon dioxide, residence time in an atmosphere are generally 10 years.Therefore methane compares titanium dioxide to the greenhouse effects of atmosphere Carbon is more serious, needs to carry out strict control.The one kind for eliminating methane residual gas during natural gas resource utilizes has efficacious prescriptions Method is by methane oxidation by catalytic oxidation technologies into carbon dioxide and water.
Methane has the positive tetrahedron structure of high degree of symmetry, and c h bond bond energy is up to 439kJ/mol, logical in reaction process Often it is difficult to be activated, so Catalytic methane oxidation technology is always the research hotspot in environmental catalysis field.It can be used for methane oxidation Catalyst mainly have noble metal catalyst (mainly having support type Pt, Pd, Au catalyst) and metal oxide catalyst (main There are transition metal oxide, perofskite type oxide, spinel oxides, pyrochlore-type oxide, hexa-aluminate catalyzer) Two major classes.Metal oxide catalyst has certain advantage compared with noble metal catalyst in price, but it is active and steady There are also a certain distance for qualitative and noble metal catalyst, are only used for the high-temperature oxydation reaction of methane at present.Noble metal catalyst It is the highest methane oxidation material of activity, there is very high low-temperature catalytic oxidation activity and good anti-toxicity energy.And expensive In metallic catalyst, with PdO/Al2O3Catalyst being most widely used in the processing of methane residual gas, and most apply valence Value.
Document Catal.Commun.56 (2014) 157-163 is prepared for PdO/ θ-Al using infusion process2O3、PdO/δ- Al2O3、PdO/η-Al2O3、PdO/γ-Al2O3、PdO/κ-Al2O3The PdO/Al of serial difference crystal phase alumina load2O3Catalysis Agent.The study found that PdO/Al of the series in different crystal phases2O3In catalyst, aoxidized by catalyst methane made from carrier of θ phase Active highest, stability are best.But it is all during the reaction, due to the strong adsorption of PdO particle grown up with steam PdO/Al2O3There is deactivation phenomenoms for catalyst.CN 102974343A disclose it is a kind of with 2%PdO for active phase, with Ce, γ-the Al of Zr, Y, La modification2O3For the lean burn natural gas tailstock gas disposal catalyst of carrier.In 40000h- 11000ppmCH43000ppmCO 1000ppmNO 6.5%O210%CO2Simulate the CH under lean-combustion engine exhaust gas composition4 Activity of conversion sequence is Zr-Al2O3>Y-Al2O3>Ce-Al2O3>La-Al2O3.Subsequent inventor be respectively adopted Zr-Y, Zr-La, γ-the Al of Zr-Ce modification2O3The catalyst of identical PdO content is prepared for for carrier, under the same conditions to catalyst performance into Test is gone.As the result is shown: CH4Active sequence Zr-Y-Al2O3>Zr-Ce-Al2O3>Zr/Al2O3>Zr-La-Al2O3.This explanation Al2O3The modification of material influences catalyst performance significant.But the performance advantage of these materials is under reaction atmosphere anhydrous condition Displaying, cannot show the practical application performance of catalyst completely.
It is well known that remaining in methane gas during being utilized using natural gas as the natural gas resource of fuel and usually containing 5 ~15% steam.Reaction kinetics research show that moisture content is to PdO/Al2O3The catalytic activity and stability of catalyst have There is sizable adverse effect.It can disappear being present in steam (steam under hot conditions) environment therefore, it is necessary to develop Except the methane oxidation catalyst of methane residual gas.
Summary of the invention
The invention discloses a kind of water resistant, high temperature resistant methane oxidation catalysts and preparation method thereof, to overcome the prior art special It is not the problem of methyl hydride catalyzed activity is not high and catalyst unstability in aqueous atmosphere and hot environment.
The present invention adopts the following technical scheme: Ba salting liquid is impregnated into Al by method that is isometric or excessively impregnating2O3 On powder and it is prepared into BaCO3/Al2O3Carrier, then Pd precursor water solution is impregnated by method that is isometric or excessively impregnating To BaCO3/Al2O3PdO/BaCO is prepared on carrier3/Al2O3A kind of water resistant, high temperature resistant methane oxidation catalyst.
A kind of water resistant, high temperature resistant methane oxidation catalyst, by 0.5-5wt%PdO, 1-10wt%BaCO3、85- 98.5wt%Al2O3It forms, wherein Al2O3With BaCO3Molar ratio be 16.5~190.7；BaCO3/Al2O3With the molar ratio of PdO It is 7.8~81.4；BaCO3It is 1.25 with PdO molar ratio.
A kind of water resistant, high temperature resistant methane oxidation catalyst preparation method, comprising the following steps:
(1)BaCO3/Al2O3The preparation of carrier: Ba precursor water solution is made in soluble Ba salt by metering, with isometric Or excessive infusion process, Ba precursor water solution is slowly added into Al2O31~2h is stood in powder at room temperature, is put into baking oven It is dried overnight at 100~120 DEG C, in 600 DEG C of Muffle kiln roasting 6h；
(2)PdO/BaCO3/Al2O3The preparation of catalyst: with isometric or excessive infusion process, by prepared precious metals pd Aqueous solution moves in (1) resulting vehicle, stands the 1~2h or ultrasound 30min under 80% power in ultrasonic cleaning machine at room temperature, and 90 DEG C water bath method, is put into baking oven and is dried overnight at 80~100 DEG C, in 600 DEG C of Muffle kiln roasting 4h.
The solubility Ba salt is barium nitrate or barium acetate.
The Al2O3For 100~400m of specific surface area2/ g, hole hold the γ phase and/or θ phase active oxygen of 0.20~0.60ml/g Change aluminium.
The precious metals pd presoma is four ammino palladium of palladium nitrate, palladium acetylacetonate or dinitroso.
The heating rate of Muffle furnace is 1~5 DEG C/min in the step (1) and step (2).
Water resistant, high temperature resistant methane oxidation catalyst provided by the invention and preparation method thereof first uses dipping-air roasting Method has synthesized BaCO3/Al2O3Carrier, then PdO/BaCO is prepared for infusion process3/Al2O3Catalyst.It is obtained prepared by the present invention Catalyst have high catalytic activity and good stability, for methane residual gas handle, removal efficiency with higher.
Detailed description of the invention
Fig. 1 is the phase structure phenogram of comparative example, embodiment 1, embodiment 2.
Specific embodiment
Below with reference to comparative example and embodiment, the present invention is further illustrated, but does not limit the invention.
Comparative example
(1) 19.7gAl is weighed2O3(specific surface area 195m2/ g, Kong Rongwei 0.78ml/g) it is roasted in 600 DEG C of Muffle furnace Burn 6h；
(2) Pd (NO that catalyst quality score is 1.5wt% will be accounted for3)2Aqueous solution moves in (1) in resulting vehicle, super Ultrasound 30min under 80% power, 90 DEG C of water bath methods are put into baking oven, are dried overnight at 100 DEG C, at 600 DEG C in sound washer Muffle kiln roasting 4h.
Embodiment 1
(1) 0.78g Ba (CH is weighed3COO)2It is configured to Ba precursor water solution, is added to 19.1gAl2O3(specific surface area For 195m2/ g, Kong Rongwei 0.78ml/g) in dipping, stand 2h at room temperature, be put into baking oven and be dried overnight at 120 DEG C, 600 DEG C Muffle kiln roasting 6h；
(2) Pd (NO that catalyst quality score is 1.5wt% will be accounted for3)2Aqueous solution moves in (1) in resulting vehicle, super Ultrasound 30min under 80% power, 90 DEG C of water bath methods are put into baking oven, are dried overnight at 100 DEG C, at 600 DEG C in sound washer Muffle kiln roasting 4h.
Embodiment 2
(1) 1.03g Ba (CH is weighed3COO)2It is configured to Ba precursor water solution, is added to 18.8gAl2O3(specific surface area For 195m2/ g, Kong Rongwei 0.78ml/g) in dipping, stand 2h at room temperature, be put into baking oven and be dried overnight at 120 DEG C, 600 DEG C Muffle kiln roasting 6h；
(2) Pd (NO that catalyst quality score is 2.0wt% will be accounted for3)2Aqueous solution moves in (1) in resulting vehicle, super Ultrasound 30min under 80% power, 90 DEG C of water bath methods are put into baking oven, are dried overnight at 100 DEG C, at 600 DEG C in sound washer Muffle kiln roasting 4h.
Comparative example, embodiment 1, the phase structure characterization of embodiment 2.
From fig. 1, it can be seen that providing the PdO/BaCO of preparation method synthesis using the present invention3/Al2O3Ba species in catalyst Phase structure is BaCO3。
Embodiment 3
(1) 1.30g Ba (CH is weighed3COO)2It is configured to Ba precursor water solution, is added to 18.7gAl2O3(specific surface area For 195m2/ g, Kong Rongwei 0.78ml/g) in dipping, stand 2h at room temperature, be put into baking oven and be dried overnight at 120 DEG C, 600 DEG C Muffle kiln roasting 6h；
(2) Pd (NO that catalyst quality score is 2.5wt% will be accounted for3)2Aqueous solution moves in (1) in resulting vehicle, super Ultrasound 30min under 80% power, 90 DEG C of water bath methods are put into baking oven, are dried overnight at 100 DEG C, at 600 DEG C in sound washer Muffle kiln roasting 4h.
Embodiment 4
(1) 1.55g Ba (CH is weighed3COO)2It is configured to Ba precursor water solution, is added to 18.2gAl2O3(specific surface area For 195m2/ g, Kong Rongwei 0.78ml/g) in dipping, stand 2h at room temperature, be put into baking oven and be dried overnight at 120 DEG C, 600 DEG C Muffle kiln roasting 6h；
(2) Pd (NO that catalyst quality score is 3.0wt% will be accounted for3)2Aqueous solution moves in (1) in resulting vehicle, super Ultrasound 30min under 80% power, 90 DEG C of water bath methods are put into baking oven, are dried overnight at 100 DEG C, at 600 DEG C in sound washer Muffle kiln roasting 4h.
Embodiment 5
(1) 1.81g Ba (CH is weighed3COO)2It is configured to Ba precursor water solution, is added to 17.9gAl2O3(specific surface area For 195m2/ g, Kong Rongwei 0.78ml/g) in dipping, stand 2h at room temperature, be put into baking oven and be dried overnight at 120 DEG C, 600 DEG C Muffle kiln roasting 6h；
(2) Pd (NO that catalyst quality score is 3.5wt% will be accounted for3)2Aqueous solution moves in (1) in resulting vehicle, super Ultrasound 30min under 80% power, 90 DEG C of water bath methods are put into baking oven, are dried overnight at 100 DEG C, at 600 DEG C in sound washer Muffle kiln roasting 4h.
Embodiment 6
(1) 2.07g Ba (CH is weighed3COO)2It is configured to Ba precursor water solution, is added to 17.6gAl2O3(specific surface area For 195m2/ g, Kong Rongwei 0.78ml/g) in dipping, stand 2h at room temperature, be put into baking oven and be dried overnight at 120 DEG C, 600 DEG C Muffle kiln roasting 6h；
(2) Pd (NO that catalyst quality score is 4.0wt% will be accounted for3)2Aqueous solution moves in (1) in resulting vehicle, super Ultrasound 30min under 80% power, 90 DEG C of water bath methods are put into baking oven, are dried overnight at 100 DEG C, at 600 DEG C in sound washer Muffle kiln roasting 4h.
Embodiment 7
(1) 2.33g Ba (CH is weighed3COO)2It is configured to Ba precursor water solution, is added to 17.3gAl2O3(specific surface area For 195m2/ g, Kong Rongwei 0.78ml/g) in dipping, stand 2h at room temperature, be put into baking oven and be dried overnight at 120 DEG C, 600 DEG C Muffle kiln roasting 6h；
(2) Pd (NO that catalyst quality score is 4.5wt% will be accounted for3)2Aqueous solution moves in (1) in resulting vehicle, super Ultrasound 30min under 80% power, 90 DEG C of water bath methods are put into baking oven, are dried overnight at 100 DEG C, at 600 DEG C in sound washer Muffle kiln roasting 4h.
Embodiment 8
(1) 2.59g Ba (CH is weighed3COO)2It is configured to Ba precursor water solution, is added to 17.0gAl2O3(specific surface area For 195m2/ g, Kong Rongwei 0.78ml/g) in dipping, stand 2h at room temperature, be put into baking oven and be dried overnight at 120 DEG C, 600 DEG C Muffle kiln roasting 6h；
(2) Pd (NO that catalyst quality score is 5.0wt% will be accounted for3)2Aqueous solution moves in (1) in resulting vehicle, super Ultrasound 30min under 80% power, 90 DEG C of water bath methods are put into baking oven, are dried overnight at 100 DEG C, at 600 DEG C in sound washer Muffle kiln roasting 4h.
Embodiment 9
(1) 0.52g Ba (CH is weighed3COO)2It is configured to Ba precursor water solution, is added to 19.4gAl2O3(specific surface area For 195m2/ g, Kong Rongwei 0.78ml/g) in dipping, stand 2h at room temperature, be put into baking oven and be dried overnight at 120 DEG C, 600 DEG C Muffle kiln roasting 6h；
(2) Pd (NO that catalyst quality score is 1.0wt% will be accounted for3)2Aqueous solution moves in (1) in resulting vehicle, super Ultrasound 30min under 80% power, 90 DEG C of water bath methods are put into baking oven, are dried overnight at 100 DEG C, at 600 DEG C in sound washer Muffle kiln roasting 4h.
Embodiment 10
(1) 0.26g Ba (CH is weighed3COO)2It is configured to Ba precursor water solution, is added to 19.7gAl2O3(specific surface area For 195m2/ g, Kong Rongwei 0.78ml/g) in dipping, stand 2h at room temperature, be put into baking oven and be dried overnight at 120 DEG C, 600 DEG C Muffle kiln roasting 6h；
(2) Pd (NO that catalyst quality score is 0.5wt% will be accounted for3)2Aqueous solution moves in (1) in resulting vehicle, super Ultrasound 30min under 80% power, 90 DEG C of water bath methods are put into baking oven, are dried overnight at 100 DEG C, at 600 DEG C in sound washer Muffle kiln roasting 4h.
The hydrothermal aging of the above catalyst sample.
Take the above catalyst preparation sample in part at 1000 DEG C, 10%H2Catalyst sample aging is carried out under the conditions of O, 10h.
The activity rating of the above catalyst sample.
The fresh and aged samples for taking the above catalyst form are as follows: methane in reaction gas volume: 1000ppm, oxygen: 10%, water: 10%, nitrogen: Balance Air, air speed 80000h-1Fixed bed reactors on carry out activity rating.
Activity evaluation such as table 1.
Table 1
As known from Table 1, compared to PdO/Al2O3Catalyst, PdO/BaCO3/Al2O3Catalyst activity and stability show It is very excellent.

Claims (8)

1. a kind of methane oxidation catalyst, it is characterised in that: by 0.5-5wt%PdO, 1-10wt%BaCO3, 85-98.5wt% Al2O3It forms, wherein Al2O3With BaCO3Molar ratio be 16.5~190.7；BaCO3/Al2O3With the molar ratio of PdO be 7.8~ 81.4；BaCO3It is 1.25 with PdO molar ratio.
2. a kind of preparation method of methane oxidation catalyst, it is characterised in that include the following steps:
(1)BaCO3/Al2O3The preparation of carrier: Ba precursor water solution is made in soluble Ba salt by metering, with isometric or mistake Infusion process is measured, Ba precursor water solution is slowly added into Al2O31~2h is stood in powder at room temperature, is put into 100 in baking oven It is dried overnight at~120 DEG C, in 600 DEG C of Muffle kiln roasting 6h；
(2)PdO/BaCO3/Al2O3The preparation of catalyst: with isometric or excessive infusion process, by prepared precious metals pd forerunner Body aqueous solution moves in (1) resulting vehicle, stands the 1~2h or ultrasound 30min under 80% power in ultrasonic cleaning machine at room temperature, 90 DEG C of water bath methods, are put into baking oven and are dried overnight at 80~100 DEG C, in 600 DEG C of Muffle kiln roasting 4h.
3. the preparation method of methane oxidation catalyst as claimed in claim 2, it is characterised in that solubility Ba in the step (1) Salt is barium nitrate or barium acetate.
4. the preparation method of methane oxidation catalyst as claimed in claim 2, it is characterised in that Al in the step (1)2O3For than 100~400m of surface area2/ g, hole hold the γ phase or/and θ phase activated alumina of 0.20~0.60ml/g.
5. the preparation method of methane oxidation catalyst as claimed in claim 2, it is characterised in that the step (1) and step (2) The heating rate of middle Muffle furnace is 1~5 DEG C/min.
6. the preparation method of methane oxidation catalyst as claimed in claim 2, it is characterised in that precious metals pd in the step (2) Presoma is four ammino palladium of palladium nitrate, palladium acetylacetonate or dinitroso.
7. methane oxidation catalyst described in claim 1 is applied to be resistant to aqueous atmosphere and hot environment.
8. methane oxidation catalyst described in claim 1 is applied to natural gas vehicle, the exhaust aftertreatment of gasoline car or with natural Gas, coal gas, oil liquefied gas be fuel burner tail gas clean-up.
CN201810824151.7A 2018-07-25 2018-07-25 A kind of water resistant, high temperature resistant methane oxidation catalyst and preparation method thereof Pending CN108993560A (en)

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CN111921554A (en) * 2020-07-27 2020-11-13 中广核研究院有限公司 Pd-based catalyst for catalytic oxidation of methane under water-containing condition and preparation method thereof
CN111921554B (en) * 2020-07-27 2022-12-30 中广核研究院有限公司 Pd-based catalyst for catalytic oxidation of methane under water-containing condition and preparation method thereof
CN113042039A (en) * 2021-03-24 2021-06-29 中国科学院生态环境研究中心 Palladium-based catalyst, and preparation method and application thereof

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Application publication date: 20181214