CN107511147A - A kind of high stability catalyst for catalytic oxidation and preparation method - Google Patents

A kind of high stability catalyst for catalytic oxidation and preparation method Download PDF

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CN107511147A
CN107511147A CN201710563827.7A CN201710563827A CN107511147A CN 107511147 A CN107511147 A CN 107511147A CN 201710563827 A CN201710563827 A CN 201710563827A CN 107511147 A CN107511147 A CN 107511147A
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catalyst
palladium
nitrate
preparation
high stability
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郭耘
赵振阳
黄昶
王丽
龚学庆
郭杨龙
卢冠忠
王筠松
詹望成
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East China University of Science and Technology
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    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
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    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
    • F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
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Abstract

The present invention relates to a kind of high stability catalyst for catalytic oxidation and preparation method.The chemical composition of the catalyst is PdOx‑AmBnCyDzOδ, wherein A bits element is Rare Earth Lanthanum（La）, neodymium（Nd）, praseodymium（Pr）, erbium（Er）In one kind, B bits element is sodium（Na）, potassium（K）, strontium（Sr）, calcium（Ca）, magnesium（Mg）And barium（Ba）In one kind, C bits element is transition metal iron（Fe）, cobalt（Co）, nickel（Ni）, manganese（Mn）, copper（Cu）, aluminium（Al）In one kind, D positions are transition metal iron（Fe）, cobalt（Co）, nickel（Ni）, manganese（Mn）, copper（Cu）, aluminium（Al）In one kind；Pd/ (A+B) mol ratio is 0.002 0.10.The catalyst is prepared using epitaxial growth method, for CO catalysis oxidations, CH4The catalytic oxidation such as catalysis burning, the catalysis burning of volatile organic matter has excellent activity and stability, through 900 1200 oAfter the h of C high-temperature roastings 100, the activity of catalyst still keeps constant.This method has the advantages that preparation condition is simple, it is cheap to prepare cost.

Description

A kind of high stability catalyst for catalytic oxidation and preparation method
Technical field
The present invention relates to a kind of high stable catalyst and preparation method for catalysis oxidation, belong to the system of catalyst Standby and its application field, the perovskite structure specifically prepared with rare earth, alkali metal, alkaline-earth metal, transition metal, The composite oxides of perovskite-like structure, spinel structure or mixed structure are carrier, and unformed nano palladium oxide is work Property component catalysis oxidation catalyst, catalysis burning, the catalysis of volatile organic matter of catalysis oxidation, methane available for CO Burning etc..
Background technology
The problems such as energy shortage at present and environmental degradation, is increasingly subject to people's attention.Catalysis oxidation（Burning）Technology is the energy Efficiently utilize one of effective ways eliminated with organic pollution.Exploitation high activity, the catalyst for catalytic oxidation of high stability are The key of the technology.
Catalyst for catalysis oxidation has a lot, can be divided into noble metal catalyst and metal according to the difference of active component Oxide catalyst.How to improve the stability of noble metal catalyst and the activity of metal oxide catalyst is current catalysis oxygen Change（Burning）In difficult point.Wherein noble metal catalyst, such as Pd, have an excellent catalytic oxidation activity, but its heat endurance compared with It is low, easy high temperature sintering and loss；In metal oxide catalyst, copper, cobalt, the oxide and composite oxides of manganese and chromium have High heat endurance, but its catalytic oxidation activity is low compared to noble metal.
Such as：In oxide catalyst, mesoporous LaCoO3Higher activity is shown, perovskite is prepared by using hard template method LaCoO3Catalyst, substantially increase its specific surface area（96.7 m2 g-1）, its initiation temperature（T10）When with conversion ratio being half （T50）Temperature be respectively 335 and 470oC（Yangang. Wang et al. Journal of Nanoscience and Nanotechnology 8 (2008) 5652-5658.）.Carrier loaded Co is used as by the use of mesoporous SBA -153O4Catalyst, its methane Combustion activity is better than the cobalt or Mn catalyst of normal silicon oxides either alumina load, methyl hydride combustion T90Temperature is 576oC （G. Laugel et al. Catalysis Today 138 (2008) 38-42.）.Although the activity of transition metal oxide Greater advance is achieved, but is still had a long way to go compared with noble metal active.
Noble metal has obtained widely applying because it has high activity, if precious metals palladium catalyst is in CO catalysis oxygen Change, the catalysis of methane is burnt, being catalyzed in burning etc. for volatile organic matter shows excellent performance.In commercial Application, In order to reduce the cost of catalyst, it need to improve the stability of catalyst on the premise of activity is kept, urged frequently with load type palladium Agent.
For Pd catalyst, the size of Pd particles seriously affects the activity of catalyst, and researcher has found that the particle diameter of palladium is got over Small, catalyst activity is higher.The active activity of the PdO catalyst of smaller particle is active higher by two than bulky grain PdO catalyst The individual order of magnitude, their TOF are respectively 0.02 and 1.3 s-1（R.F. Hicks et al. Journal of Catalysis 122 (1990) 280-294.）.
Patent CN201310159743 discloses a kind of palladium-based catalyst and its preparation for being used to be catalyzed burning, is with your gold Belong to palladium as catalyst, boehmite is that mesoporous aluminas prepared by silicon source is carrier.The wherein ratio surface of meso-porous alumina Product is 200-400 m2 g-1, the content of active component palladium is the 0.1%-1% of overall catalyst weight.
Patent CN201510274648 discloses a kind of loaded palladium catalyst and preparation method for being used to be catalyzed burning.This is urged Agent is using precious metal palladium as active component, and auxiliary agent is rare earth oxide, and alkali and alkaline earth metal ions, carrier is tin oxide, its Middle palladium content is the 0.1%-5% of overall catalyst weight, and the content of alkali metal or alkaline-earth metal is 3%-10%.
Patent CN201110388703 discloses a kind of catalyst of low concentration reactant catalysis burning and preparation method thereof. Active component of the catalyst using the one or more combination in precious metals pd, Pt, Ru, Ir, Rh as catalyst, with Mg, La, At least one of Fe, Mn, Ni, Co, Cr, Ca metal oxide is as the common carrier of metal oxide；Utilize infusion process, homogeneous heavy Any one method in shallow lake method, coprecipitation thermal decomposition method, prepare containing altogether carrier catalyst precarsor, by filtering, Washing, dry, be calcined, be molded, be calcined again and form catalyst after reducing.
The content of the invention
The purpose of the present invention is to prepare a kind of high stability for catalysis oxidation, the nano oxidized palladium chtalyst of high activity Agent, can be compared with the complete oxidation that CO, methane etc. are realized under low temperature, and through 900-1200oAfter the h of C high-temperature roastings 100, activity is protected Hold constant.
Compared with the prior art, it is characteristic of the invention that：
（1）PdOxParticle is small, and decentralization is high, enhances the catalytic oxidation activity of catalyst.
（2）Prepared unformed nano Pd particle OxParticle has a high high-temp stability, PdO under high temperaturexWhat can be stablized deposits There is high heat endurance, through 900-1200oAfter C high temperature ageings, activity keeps constant, and noble metal is not lost in.
（3）Prepared catalyst after high-temperature roasting with perovskite structure, perovskite-like structure, spinel structure or The form of mixed structure is present.
（4）Catalyst is prepared using epitaxial growth method, goes out unformed PdO in catalyst surface growth in situxNanometer Grain, preparation method is simple, reproducible.
The technology path of catalyst preparation of the present invention is：
The chemical composition of the catalyst of the present invention is PdOx-AmBnCyDzOδ, with unformed nano particle PdOxFor active component, Perovskite structure, perovskite-like structure, the composite oxides of spinel structure or mixed structure are carrier, pass through epitaxial growth It is prepared by method.Mixed solution is formed after the element of A, B, C and D position is dissolved in into water first, by the addition of complexing agent, heated stirring Gel is formed, is then carbonized in an oven, wherein A bits element is Rare Earth Lanthanum（La）, neodymium（Nd）, praseodymium（Pr）, erbium（Er）In one Kind, B bits element is sodium（Na）, potassium（K）, strontium（Sr）, calcium（Ca）, magnesium（Mg）And barium（Ba）In one kind, C bits element for transition gold Belong to iron（Fe）, cobalt（Co）, nickel（Ni）, manganese（Mn）, copper（Cu）, aluminium（Al）In one kind, D positions are transition metal iron（Fe）, cobalt （Co）, nickel（Ni）, manganese（Mn）, copper（Cu）, aluminium（Al）In one kind.Palladium presoma is impregnated afterwards on sample in the carbonized, It is calcined in atmosphere, it is A palladium ion is entered compositionmBnCyDzOδComposite oxides interstitial void in formed gap solid solution Body, continue to improve sintering temperature, using epitaxial growth, palladium ion is separated out the PdO for forming nano particle from interstitial voidx。 PdO can be not only effectively controlled by the method for this epitaxial growthxGranular size, and make PdOxStable growth In complex oxide surface.
Catalyst preparation route of the present invention is：
The soluble-salt of aluminium and rare earth is dissolved in deionized water by required stoichiometric proportion mixed solution is made, while by one Quantitative complexing agent is dissolved in deionized water, above two solution is mixed, stirring, controls solution ph between 0.5-2.0, Heating water bath, stirring are transferred to 60-90 to geloIn 100-160 after C oven dryingsoBe carbonized 8-15 h under C.Precious metals pd Introducing have two methods：（1）Soluble palladium salt forms mixed solution, remaining preparation method with rare earth and transition metal soluble salt It is identical；（2）Sample after gained carbonization is carrier, using soluble palladium salt, is introduced by infusion process, remaining preparation method phase Together.
Finally by sample 400o2-5 h are calcined under C, finally in 500-1200o1-10 is calcined at a temperature of C in air H, obtain catalyst.
Embodiment
The following examples further will be described to the present invention, but not limited the scope of the invention.
Embodiment 1：
3.75 g Al (NO are weighed respectively3)3•9H2O, 4.62 g C6H8O7•H2O and 0.73 g C6H14O6It is dissolved in 30 mL In deionized water, for heating stirring to being completely dissolved, solution final ph is 0.9.Mixed solution is 85oHeating is stirred in C water-bath Mix to gel, then through 120oIn the carbonized 500 after C dryingso3 h are calcined under C and obtain carrier γ-Al2O3, afterwards with Palladium nitrate incipient impregnation, Pd weight content is 2%, and dipping terminates rear 60oC dries 12 h, finally 1000o3 are calcined under C H obtains required catalyst.
Using homemade fixed-bed quartz reactor to catalyst in CH4Catalytic oxidation activity is tested.Urged before test 20 dry vol.% O of agent2/N2Gaseous mixture is 400o0.5 h is pre-processed under C.Each active testing uses 40-60 mesh The mg of catalyst 200.Reactor feed gas is 1 dry vol.% CH4And 20 vol.% O2, Balance Air N2, air speed 15, 000 ml g−1 h−1.Active testing is carried out after reaction reaches stable.
Activity evaluation shows, prepared PdOx/Al2O3CH on catalyst4Complete conversion temperature is 500oC。
Embodiment 2：
Weigh the γ-Al of 2.00 g business2O3For carrier, palladium nitrate solution incipient impregnation is on carrier, after the completion of dipping The h of drying at room temperature 12, then 1000o3 h are calcined under C and obtain required catalyst.The evaluation method of catalyst is the same as implementation Example 1.
Activity evaluation shows, prepared PdOx/Al2O3CH on catalyst4Complete conversion temperature is 480oC.Catalysis Agent is through 1000oAfter the h of C agings 100, CH4Complete conversion temperature is 560oC, noble metal are lost in 50%.
Embodiment 3：
3.24 g La (NO are weighed respectively3)3•nH2O, 3.75 g Al (NO3)3•9H2O, 4.73 g C6H8O7•H2O and 0.74 G C6H14O6It is dissolved in 30 mL deionized waters（The mol ratio of complexing agent and metal is 1.3）, heating stirring to being completely dissolved, Solution final ph is 1.2.Mixed solution is 85oHeating stirring is to gel in C water-bath, then through 130oC is carbonized, will On the sample of palladium nitrate solution dipping in the carbonized, Pd weight content is 1.5%, last first 500oC roasting temperatures 1 H, then 1000o3 h are calcined under C and obtain required catalyst.The evaluation method of catalyst is the same as embodiment 1.
Activity evaluation shows, prepared PdOx/LaAlO3CH on catalyst4Complete conversion temperature is 400oC.Urge Agent is through 1000oAfter the h of C agings 100, activity is kept, and noble metal is not lost in.
Embodiment 4：
3.24 g La (NO are weighed respectively3)3•nH2O, 3.37 g Al (NO3)3•9H2O and 4.79 g C6H8O7•H2O dissolves In 30 mL deionized waters（The mol ratio of complexing agent and metal is 1.2）, heating stirring is to being completely dissolved, solution final ph For 1.2.Mixed solution is 85oHeating stirring is to gel in C water-bath, then through 130oC is carbonized, and palladium nitrate solution is soaked On the sample of stain in the carbonized, Pd weight content is 1.5%, last first 500oThe h of C roasting temperatures 1, then 1000o3 h are calcined under C and obtain required catalyst.The evaluation method of catalyst is the same as embodiment 1.
Activity evaluation shows, prepared PdOx/LaAlO3CH on catalyst4Complete conversion temperature is 480oC。
Embodiment 5：
By the La (NO in embodiment 33)3•nH2O, change the Nd (NO of equimolar amounts into3)3•6H2O, remaining each portion is the same as embodiment 3.Urge The evaluation method of agent is the same as embodiment 1.
Activity evaluation shows, prepared PdOx/NdAlO3+δCH on catalyst4Complete conversion temperature is 500oC。
Embodiment 6：
By the La (NO of 3.24 g in embodiment 33)3•nH2O changes 2.60 g La (NO into3)3•nH2O and 0.65 g Pr (NO3)3, remaining each portion is the same as embodiment 3.The evaluation method of catalyst is the same as embodiment 1.
Activity evaluation shows, prepared PdOx/LaPrAlO3+δCH on catalyst4Complete conversion temperature is 440oC。
Embodiment 7：
By the Al (NO of 3.75 g in embodiment 33)3•9H2O changes 1.88 g Al (NO into3)3•9H2O and 1.46 g Co (NO3)2·6H2O, remaining each portion is the same as embodiment 3.The evaluation method of catalyst is the same as embodiment 1
Activity evaluation shows, prepared PdOx/LaAl0.5Co0.5O3+δCH on catalyst4Complete conversion temperature is 420oC。
Embodiment 8：
By the Al (NO of 3.75 g in embodiment 33)3•9H2O changes 1.88 g Al (NO into3)3•9H2O and 2.02 g Fe (NO3)2·9H2O, remaining each portion is the same as embodiment 3.The evaluation method of catalyst is the same as embodiment 1
Activity evaluation shows, prepared PdOx/LaAl0.5Fe0.5O3+δCH on catalyst4Complete conversion temperature is 470oC.Catalyst is through 1000oAfter the h of C agings 100, CH4Complete conversion temperature is 510oC, noble metal are lost in 20%.
Embodiment 9：
Change palladium nitrate solution in embodiment 3 into palladium solution, remaining each portion is the same as embodiment 3.The evaluation method of catalyst is same Embodiment 1.
Activity evaluation shows, prepared PdOx/LaAlO3+δCH on catalyst4Complete conversion temperature is 400oC。
Embodiment 10：
3.24 g La (NO are weighed respectively3)3•nH2O, 3.75 g Al (NO3)3•9H2O, 4.73 g C6H8O7•H2O and 0.74 G C6H14O6It is dissolved in 30 mL deionized waters（The mol ratio of complexing agent and metal is 1.3）, heating stirring to being completely dissolved, Solution final ph is 1.2.Mixed solution is 85oHeating stirring is to gel in C water-bath, then through 130oC is carbonized, will On the sample of palladium nitrate solution dipping in the carbonized, Pd weight content is 1.5%, last first 500oC roasting temperatures 1 H, then 1000o3 h are calcined under C and obtain required catalyst.
Catalyst is tested in CO catalytic oxidation activities using homemade fixed-bed quartz reactor.It is catalyzed before test 20 dry vol.% O of agent2/N2Gaseous mixture is 400o0.5 h is pre-processed under C.Each active testing uses 40-60 purposes The mg of catalyst 200.Reactor feed gas is dry 1 vol.% CO and 20 vol.% O2, Balance Air N2, air speed 15,000 ml g−1 h−1.Active testing is carried out after reaction reaches stable.
Activity evaluation shows, prepared PdOx/LaAlO3+δCO initiation temperature is 120 on catalystoC, completely Conversion temperature is 170oC.Catalyst is through 1000oAfter the h of C agings 100, activity is kept, and noble metal is not lost in.

Claims (8)

1. a kind of high stability catalyst for catalysis oxidation, the chemical composition of the catalyst is PdOx-AmBnCyDzOδ, its In：The active component of catalyst is unformed PdOx, wherein 0< x ≤ 1；Carrier is AmBnCyDzOδOxide, wherein A positions Element is Rare Earth Lanthanum（La）, neodymium（Nd）, praseodymium（Pr）, erbium（Er）In one kind, B bits element is sodium（Na）, potassium（K）, strontium（Sr）, calcium （Ca）, magnesium（Mg）And barium（Ba）In one kind, C bits element is transition metal iron（Fe）, cobalt（Co）, nickel（Ni）, manganese（Mn）, copper （Cu）, aluminium（Al）In one kind, D positions are transition metal iron（Fe）, cobalt（Co）, nickel（Ni）, manganese（Mn）, copper（Cu）, aluminium（Al）In One kind.
2. a kind of high stability catalyst for catalysis oxidation according to claim 1, it is characterised in that the catalyst has There are high catalytic oxidation activity and heat endurance, the catalysis burning of catalysis oxidation, methane available for CO, volatile organic matter Catalysis burning etc., its initiation temperature to methane is less than 280oC, CO initiation temperature are less than 120oC。
3. a kind of high stability catalyst for catalysis oxidation according to claim 1, it is characterised in that the catalyst passes through 900-1200 oAfter C high temperature ageings, activity keeps constant, and noble metal is not lost in.
4. a kind of high stability catalyst for catalysis oxidation according to claim 1, it is characterised in that the catalyst passes through 900-1200 oAfter C high temperature ageings, exist with perovskite structure, perovskite-like structure, spinel structure or jointly.
5. a kind of high stability catalyst for catalysis oxidation according to claim 1, it is characterised in that the catalyst is adopted Prepared with epitaxial growth method, go out unformed nano palladium oxide particle, its particle diameter distribution in composite oxide carrier in-situ preparation In 0.5 ~ 10 nm, detailed process is：（1）Mixed solution is made in rare earth, transition metal dissolution in deionized water；（2）By one Quantitative complexing agent, which is dissolved in deionized water, is made certain density mixed solution；（3）Under water bath condition, by step（1）With （2）Obtained mixed solution mixing, control ph is between 0.5-2.0, and control temperature is in 50-90oBetween C, stir to gel Shape；（4）By obtained gel in 60-90o4-8 h are dried in C baking ovens, after being completely dried, oven temperature is brought rapidly up 100- 160 oC makes its 8-15 h that are carbonized；（5）The introducing of precious metals pd has two methods：（1）In it is solvable with rare earth and transition metal Salt forms mixed solution, and remaining preparation method is identical；Or with（4）Sample after gained carbonization is carrier, using soluble palladium Salt, introduced by infusion process, remaining preparation method is identical；（6）Gained sample is in 300-400o2-5 h, Ran Hou are calcined under C 500-1200 o1-10 h are calcined at a temperature of C in air, obtain the high stability catalyst for catalysis oxidation.
6. the preparation method of the high stability catalyst of a kind of catalysis oxidation according to claim 5, it is characterised in that made Complexing agent is the one or more in citric acid, sorbierite, and the mol ratio of complexing agent and metal is 0.1-2.0；It is dilute The precursor salt of soil is nitrate, can make lanthanum nitrate, neodymium nitrate, nitric acid is general, one kind in erbium nitrate；Transition-metal Fe, Co, Ni, Mn, Cu and Al presoma are nitrate, one kind in acetate, sulfate, preferably nitrate；Alkali metal and alkaline earth gold The presoma for belonging to Na, K, Sr, Ca, Mg and Ba is nitrate, one kind in acetate, sulfate, preferably nitrate；Before middle palladium Drive body is one kind in palladium nitrate, chloric acid palladium, palladium, palladium acetylacetonate, preferably palladium nitrate.
7. the preparation method of catalyst according to claim 5, it is characterised in that through 600-1000oFormed and contained after C roastings Pd perovskite, the perovskite-like containing Pd, the spinel structure containing Pd, or form the mixed structure containing Pd.
8. the preparation method of catalyst according to claim 5, it is characterised in that through 600-1000oIt is being catalyzed after C roastings The epitaxial growth of agent surface goes out unformed nano palladium oxide particle.
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Cited By (9)

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CN110152660A (en) * 2019-05-29 2019-08-23 昆明理工大学 A kind of liquid nitrogen washing tail-gas high temperature catalytic combustion catalyst and its preparation method and application
CN110835295A (en) * 2019-11-12 2020-02-25 云南正邦科技有限公司 Method for preparing acetic acid by using microchannel reactor
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CN115779900A (en) * 2022-10-25 2023-03-14 中船动力(集团)有限公司 Tail gas CH for natural gas engine of ship 4 Purified oxidation catalyst, method for the production thereof and use thereof
CN116726948A (en) * 2023-06-13 2023-09-12 华东理工大学 Catalyst for low-temperature catalytic combustion elimination of light alkane and preparation method and application thereof

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CN108654592A (en) * 2018-04-29 2018-10-16 华中科技大学 A kind of perovskite catalyst and preparation method thereof and home position testing method
CN111229219A (en) * 2018-11-29 2020-06-05 中国科学院大连化学物理研究所 Tail gas combustion catalyst and preparation and application thereof
CN110152660A (en) * 2019-05-29 2019-08-23 昆明理工大学 A kind of liquid nitrogen washing tail-gas high temperature catalytic combustion catalyst and its preparation method and application
CN110835295A (en) * 2019-11-12 2020-02-25 云南正邦科技有限公司 Method for preparing acetic acid by using microchannel reactor
WO2021159951A1 (en) * 2020-02-11 2021-08-19 中国石油化工股份有限公司 Catalyst and catalytic oxidation-deoxidation method for unsaturated hydrocarbon-containing gas
CN111282571A (en) * 2020-03-20 2020-06-16 北京工业大学 Preparation method and application of praseodymium-neodymium-palladium doped cerium-manganese composite catalyst
CN111282571B (en) * 2020-03-20 2022-06-21 北京工业大学 Preparation method and application of praseodymium-neodymium-palladium doped cerium-manganese composite catalyst
CN111589452A (en) * 2020-06-03 2020-08-28 潍柴动力股份有限公司 Tail gas combustion catalyst for solid oxide fuel cell system and preparation method thereof
WO2021244599A1 (en) * 2020-06-03 2021-12-09 潍柴动力股份有限公司 Tail gas combustion catalyst for solid oxide fuel cell system and preparation method therefor
CN111589452B (en) * 2020-06-03 2023-04-18 潍柴动力股份有限公司 Tail gas combustion catalyst for solid oxide fuel cell system and preparation method thereof
CN115779900A (en) * 2022-10-25 2023-03-14 中船动力(集团)有限公司 Tail gas CH for natural gas engine of ship 4 Purified oxidation catalyst, method for the production thereof and use thereof
CN116726948A (en) * 2023-06-13 2023-09-12 华东理工大学 Catalyst for low-temperature catalytic combustion elimination of light alkane and preparation method and application thereof

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