CN101664690A - Catalyst and preparation method and application thereof - Google Patents

Catalyst and preparation method and application thereof Download PDF

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CN101664690A
CN101664690A CN200810119338A CN200810119338A CN101664690A CN 101664690 A CN101664690 A CN 101664690A CN 200810119338 A CN200810119338 A CN 200810119338A CN 200810119338 A CN200810119338 A CN 200810119338A CN 101664690 A CN101664690 A CN 101664690A
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catalyst
molecular sieve
aqueous solution
metal oxide
temperature
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CN101664690B (en
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王虹
李翠清
宋永吉
王军利
迟姚玲
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Beijing Institute of Petrochemical Technology
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    • 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
    • Y02C20/10—Capture or disposal of greenhouse gases of nitrous oxide (N2O)

Abstract

The invention relates to a catalyst and a preparation method and application thereof. The catalyst contains a composite metal oxide and a molecular sieve carrier, wherein the composite metal oxide hasa spinel structure and/or a perovskite-like structure, and the molecular general formula of the composite metal oxide is Co3-xMxO4 or La2-yMyBO4. The molecular sieve carrier is an HZSM-5, HZSM-18 orRPSA molecular sieve with an MFI structure or an HY molecular sieve with a Y structure. The preparation method comprises the following steps: dissolving a corresponding metal salt and a correspondingorganic complexing agent into water respectively; putting the carrier into the aqueous solution for soaking; drying the mixture at a temperature of between 30 and 90 DEG C to obtain a catalyst precursor; and calcinating the catalyst precursor at a temperature of between 400 and 1,000 DEG C for 2 to 10 hours to obtain the catalyst. The catalyst has high activity and good stability; the decomposition temperature of N2O is low; after strengthening experiments for 100 hours, the catalyst still has high activity; and the analysis result of a scanning electron microscope shows that the surface shapeof the catalyst is basically not changed.

Description

A kind of Catalysts and its preparation method and purposes
Technical field
The present invention relates to a kind of a kind of catalyst that in air pollution control technique, uses, be specifically related to a kind of decomposing N that is used for 2The catalyst of O.
The invention still further relates to this Preparation of catalysts method and purposes.
Background technology
N 2O is a kind of important atmosphere pollution, and it is not only a kind of greenhouse gases, and ozone layer is had destruction.N 2The greenhouse effects of O are respectively CO 2310 times, CH 421 times (Ram í rez JP, KapteijnF,
Figure A20081011933800031
Ffel K, et al.Formation and control of N 2O in nitric acid production.Where do we stand today? [J] .Appl.Catal.B, 2003,44:1).N 2Combustion process that derives from ocean, soil, agricultural, various fossil fuels and the chemical industry of O.Nitric plant and employing nitric acid oxidation process are N as the organic synthesis factory that produces adipic acid and glyoxal 2The maximum emission source of O.Along with the continuous enhancing of people's environmental consciousness, N 2The improvement of O has caused the great attention of global various industrial production enterprise and environmental protection organization.
Have bibliographical information to adopt coprecipitation method to prepare cobalt cerium O composite metallic oxide catalyst, wherein cobalt is with Co 3O 4Form exists, and catalysis is at 10%O 2, 3%H 2O (percentage by volume) and 0.1%N is arranged 2Decomposing N during the O coexistence 2O's is active high, N in the time of 330 ℃ 2O just can decompose (Xue Li fully, Zhang Changbin, He Hong. nitrous oxide catalytic decomposition performance study on the cobalt cerium O composite metallic oxide catalyst. Chinese rare-earth journal, 2006,24 (special editions): 10 and Li Xue, Changbin Zhang, Hong He, Yasutake Teraoka.Catalytic decomposition ofN 2O over CeO 2Promoted Co 3O 4Spinel catalyst.Applied Catalysis B:Environmental, 2007,75:157-164).
Report the Co that alkali metal K modifies in addition 3O 4Catalyst is at 0.5%N 2O, 2%O 2, 2.5%H 2Decomposing N under the O condition 2The activity of O, N 2The temperature that O decomposes fully is about 380 ℃ of (Kimihiro Asano, Chie Ohnishi, Shinji Iwamoto, Yasushi Shioya, Masashi Inoue.Potassium-diped Co 3O 4Catalyst fordirect decomposition of N 2O.Applied Catalysis B:Environmental, 2008,78:242-249).
N 2The O decomposition reaction is a strong exothermal reaction, and reaction bed temperature raises significantly in course of reaction, and reaction bed temperature may reach 500-700 ℃.Though the catalyst of above-mentioned bibliographical information is better active, the sintering temperature of catalyst is on the low side, has only 400 ℃; N in the gas of Shi Yonging in addition 2The content of O has only 0.1-0.5%, N in the industrial waste gas 2The concentration of O is as N in the industrial waste gas of producing adipic acid factory 2The concentration of O can reach more than 40%.Also there is a big difference apart from commercial Application to this shows it.
Patent documentation CN1440309A describes N in a kind of decomposition gas 2O catalyst, this catalyst comprise that 0.1-10mol% loads on the Co on the cerium oxide carrier 3-xM xO 4, wherein M is Fe and Al, x=0-2, catalyst and N 2O contacts under 500～1000 ℃ temperature and reacts.The embodiment of this patent shows, N 2O is at CoO 4/ CeO 2Or Co 2AlO 4/ CeO 2Decomposition temperature is higher on the catalyst, and decomposition temperature is more than 800 ℃ fully.
Patent documentation CN1324265A and CN1116411A mention N in a kind of Cu of containing catalyst decomposes one gas 2O.It is M that this catalyst comprises a kind of general formula xAl 2O 4Compound, M is the mixture of Cu or Cu and Zn and/or Mg, x is 0.8～1.5.
Patent documentation CN1214850C discloses N in a kind of decomposition gas 2O catalyst and technology, this catalyst are one or more years of iron zeolites, and the kind of zeolite is: MFI, BEA, FER, MOR and/or MEL; Carrying the iron zeolite is MFI, and zeolite is Fe-ZSM5, and iron is carried on the zeolite by ion-exchange.
Though the activity that has in the prior art in sum is better but sintering temperature is on the low side, also there is a big difference apart from commercial Application, the decomposition temperature that has is higher, and the decomposition efficiency that has is low, and the combination of carrier of the present invention and active component still is not reported.
Summary of the invention
The objective of the invention is in order to overcome the above-mentioned shortcoming that oneself has a technology with not enough and provide a kind of catalyst, this catalyst activity height, good stability, N 2The decomposition temperature of O is low, uses this catalyst decomposing N 2O can make N in the industrial waste gas 2O concentration reduces, and reduces atmosphere pollution, the protection environment.
The present invention also provides this Preparation of catalysts method and purposes.
The present invention achieves the above object by the following technical programs:
A kind of catalyst contains composite metal oxide and molecular sieve carrier,
Described composite metal oxide has spinel structure and/or perovskite-like structure, and general molecular formula is Co 3-xM xO 4Or La 2-yM yBO 4, M is one or both and the two or more combination that is selected from rare earth metal, transition metal, alkali metal or the alkaline-earth metal, B is one or more the combination that is selected from the transition metal, x=0～2.8, y=0～1.8.
Described molecular sieve carrier is molecular sieve with MFI structure, in the Y structure molecular screen one or more.Molecular sieve with MFI structure is HZSM-5, RPSA and HZSM-18, and the molecular sieve with Y structure is the HY molecular sieve.
Described rare earth metal is La, Ce, Pr or Nd; Transition metal is Fe, Ni, Cu, Zn, Mn, Cr, V or Zr; Alkali metal is Na, K, Rb or Cs; Alkaline-earth metal is Mg, Ca, Sr or Ba.
The Preparation of catalysts method may further comprise the steps:
A) with corresponding metal salt and organic complexing agent, be dissolved in the water respectively, be mixed with mixed aqueous solution, obtain the aqueous solution of metalline and organic complexing agent,
B) molecular sieve carrier is inserted in (a) aqueous solution and flood, and dry under 30～90 ℃ of temperature, obtain catalyst precursor, then catalyst precursor is placed 400～1000 ℃ of following roastings 2～10 hours, promptly obtain described catalyst.
With the catalyst weight is benchmark, and the load capacity that described composite metal oxide is carried on described molecular sieve carrier is 0.1-90%, and the preferred negative carrying capacity is 0.1-50%.
Described organic complexing agent is a kind of in oxalic acid, citric acid or the acetic acid, and described slaine is nitrate or acetate.
Catalyst of the present invention also can contain other component, binder component for example, and described binding agent is aluminium oxide, Ludox for example.
Described catalyst is used for flue gas or industrial waste gas N 2The decomposition of O.This catalyst can be used for the N of any concentration in the decomposition gas 2O, the O in the gas 2, NOx, CO 2The existence that reaches gas components such as CO does not influence the use of described catalyst.Because N 2The O decomposition reaction is a strong exothermal reaction, is the temperature rise of control beds, uses N in the gas of described catalyst treatment 2The concentration of O is preferably less than 20v%.
The technology of the present invention compared with the prior art, this catalyst combines composite metal oxide and molecular sieve carrier, is used for decomposing N 2The catalyst of O, it is active high, and good stability is used for N 2O directly decomposes, N 2The decomposition temperature of O is low, and decomposition temperature is not higher than 650 ℃ fully, and catalyst is tested through 100 hours reinforcement, and catalyst still keeps high activity.
The specific embodiment
By the following examples technical scheme of the present invention is described in further detail.
In each embodiment, all adopt following experimental facilities and analytical method.
Adopt fixed-bed micro-reactor to estimate catalyst provided by the invention at N 2Catalytic activity in the O decomposition reaction.Reactor adopts the quartz ampoule of internal diameter 8mm, the temperature reaction of automatic temperature control instrument control program, and programming rate is 5 ℃/min.The catalyst particles granularity is 20～40 orders, takes by weighing the sample of 0.4g, is filled in the constant temperature zone of reaction tube, prepares reacting gas on request in advance, and gas composition is the N of 12v% 2O, the O of 16.8v% 2, all the other are N 2, gas flow is 80ml/min, reaction end gas adopts gas-chromatography and the online detection of NOx analyzer.Use remaining N in Paropak Q chromatographic column and the TCD detector detection reaction tail gas 2O, the NO that forms in the NOx analyzer detection reaction.Use T 10And T 95Expression N 2The O conversion ratio is 10% and the reaction temperature of 95% o'clock correspondence, T 10Be N 2The O temperature of initial decomposition, T 95Be N 2The complete decomposition temperature of O.N 2The quality of O decomposition temperature reflection catalyst activity, its decomposition temperature is low more, and catalyst activity is good more.
Adopt the crystal structure of Japanese XRD-7000 type X-ray diffractometer test sample.Experiment condition is CuK αTarget, voltage 40KV, electric current 30mA, 4 °/min of sweep speed, 5 ° 80 ° of sweep limits.
In following examples, the activity of such catalysts appreciation condition is not described, all adopt above-mentioned experiment condition.
Embodiment 1
Take by weighing cobalt nitrate (Co (NO 3) 26H 2O) 402.87g and citric acid (C 6H 8O 7H 2O) 291.26g, be dissolved in the water respectively, be mixed with mixed aqueous solution, obtain the aqueous solution of metalline and organic complexing agent, molecular sieve carrier HZSM-51000g inserts in the aqueous solution and floods, and constantly stirs, dry under 70 ℃ of temperature, make its uniform load on molecular sieve carrier, obtain catalyst precursor, again presoma promptly being obtained load capacity of the present invention in 6 hours 800 ℃ of roastings is 10% Co 3O 4/ HZSM-5 catalyst, the XRD analysis result shows that composite metal oxide has spinel structure.
This catalyst is used for N 2The decomposition of O, gas composition is: the N of 0.65v% 2O, the O of 0.88v% 2, all the other are N 2Condition under, N 2The decomposition temperature T of O 10Be 330 ℃, T 95It is 460 ℃.
This catalyst is carried out the reinforcing life experiment, and experiment condition is: NO 2, 133ppm, CO 2, 2.02%, N 2O, 12%O 2, 16.8%, CO, 686ppm, NO, 215ppm, all the other are N 2, gas flow 320ml/min, 560 ± 5 ℃ of reaction temperatures, 100 hours reaction time, N 2The conversion ratio of O is higher than 98.5%, and the catalyst sample before and after the reaction is not seen notable difference with SEM (SEM) observation catalyst pattern.
Embodiment 2
Take by weighing cobalt nitrate 181.55g and lanthanum nitrate (La (NO 3) 36H 2O) 540.26g and citric acid 393.76g, be dissolved in the water respectively, be mixed with mixed aqueous solution, obtain the aqueous solution of metalline and organic complexing agent, molecular sieve carrier HZSM-51000g inserts in the aqueous solution and floods, and constantly stirs, and is dry under 50 ℃ of temperature, obtain catalyst precursor, again presoma promptly being obtained load capacity of the present invention in 8 hours 500 ℃ of roastings is 20% La 2CoO 4/ HZSM-5 catalyst.The XRD analysis result shows that composite metal oxide has perovskite-like structure.
This catalyst is used for N 2The decomposition of O, N 2The decomposition temperature T of O 10Be 320 ℃, T 95It is 472 ℃.
Embodiment 3
Take by weighing cobalt nitrate 516.00g and cerous nitrate (Ce (NO 3) 36H 2O) 769.90g and citric acid 746.09g, be dissolved in the water respectively, be mixed with mixed aqueous solution, obtain the aqueous solution of metalline and organic complexing agent, molecular sieve carrier RPSA 1000g inserts in the aqueous solution and floods, and constantly stirs, and is dry under 70 ℃ of temperature, obtain catalyst precursor, more above-mentioned presoma promptly being obtained load capacity of the present invention in 5 hours 600 ℃ of roastings is 30% Co 1.5Ce 1.5O 4/ RPSA catalyst.The XRD analysis result shows that composite metal oxide has spinel structure.
This catalyst is used for N 2The decomposition of O, N 2The decomposition temperature T of O 10Be 340 ℃, T 95It is 440 ℃.
Embodiment 4
Take by weighing cobalt nitrate 717.14g, strontium nitrate (Sr (NO 3) 2) 86.91g, ferric nitrate (Fe (NO 3) 29H 2O) 497.74g and lanthanum nitrate 889.19g and citric acid 1296.14g, be dissolved in the water respectively, be mixed with mixed aqueous solution, obtain the aqueous solution of metalline and organic complexing agent, molecular sieve carrier HY 1000g inserts in the aqueous solution and floods, and constantly stirs, dry under 30 ℃ of temperature, the slaine of composite metal oxide is loaded on the molecular sieve carrier, obtain catalyst precursor, again 700 ℃ of roastings of above-mentioned presoma promptly being obtained load capacity of the present invention in 5 hours is 40%Co 1.2Sr 0.2Fe 0.6LaO 4/ HY catalyst.XRD analysis detects spinel structure and perovskite-like structure.
This catalyst is used for N 2The decomposition of O, N 2The decomposition temperature T of O 10Be 430 ℃, T 95It is 630 ℃.
Embodiment 5
Take by weighing cobalt nitrate 2366.48g, barium nitrate (Ba (NO 3) 2) 386.38g and 50% manganese nitrate solution 529.13g and citric acid 2332.98g, be dissolved in the water respectively, be mixed with mixed aqueous solution, obtain the aqueous solution of metalline and organic complexing agent, molecular sieve carrier RPSA 1000g inserts in the aqueous solution and floods, and constantly stirs, and is dry under 90 ℃ of temperature, obtain catalyst precursor, more above-mentioned presoma promptly being obtained load capacity of the present invention in 2 hours 1000 ℃ of roastings is 50% Co 2.2Ba 0.4Mn 0.4O 4/ RPSA catalyst.The XRD analysis result shows that composite metal oxide has spinel structure.
This catalyst is used for N 2The decomposition of O, N 2The decomposition temperature T of O 10Be 370 ℃, T 95It is 600 ℃.
Embodiment 6
Take by weighing cobalt nitrate 14.15g, potassium nitrate (KNO 3) 0.17g and citric acid 10.58g, be dissolved in the water respectively, be mixed with mixed aqueous solution, obtain the aqueous solution of metalline and organic complexing agent, molecular sieve carrier HZSM-54000g inserts in the aqueous solution and floods, and constantly stirs, and is dry under 60 ℃ of temperature, obtain catalyst precursor, more above-mentioned presoma promptly being obtained load capacity of the present invention in 4 hours 650 ℃ of roastings is 0.1% Co 2.9K 0.1O 4/ HZSM-5 catalyst, the XRD analysis result shows that composite metal oxide has spinel structure.
This catalyst is used for N 2The decomposition of O consists of 0.88v%N at reacting gas 2O, all the other are N 2Condition under, N 2The decomposition temperature T of O 10Be 410 ℃, T 95It is 650 ℃.
Embodiment 7
Take by weighing cobalt acetate (Co (CH 3COO) 24H 2O) 2368.44g, Schweinfurt green (Cu (CH 3COO) 2H 2O) 949.13g and acetic acid (CH 3COOH) 856.43g, be dissolved in the water respectively, be mixed with mixed aqueous solution, obtain the aqueous solution of metalline and organic complexing agent,, insert in the aqueous solution and flood carrier HZSM-5 molecular sieve 400g and HZSM-18 molecular sieve 100g, and constantly stir, dry under 70 ℃ of temperature, obtain catalyst precursor, more above-mentioned presoma promptly being obtained load capacity of the present invention in 6 hours 600 ℃ of roastings is 70% Co 2CuO 4/ (HZSM-5+HZSM-18) catalyst.The XRD analysis result shows that composite metal oxide has spinel structure.
This catalyst is used for N 2The decomposition of O, N 2The decomposition temperature T of O 10Be 390 ℃, T 95It is 570 ℃.
Embodiment 8
Take by weighing cobalt nitrate 1367.27g, magnesium nitrate (Mg (NO 3) 26H 2O) 1204.62g and cerous nitrate 2040.03g and oxalic acid ((COOH) 22H 2O) 1776.84g, be dissolved in the water respectively, be mixed with mixed aqueous solution, obtain the aqueous solution of metalline and organic complexing agent, molecular sieve carrier HZSM-5150g inserts in the aqueous solution and floods, and constantly stir, dry under 60 ℃ of temperature, obtain catalyst precursor, more above-mentioned presoma promptly being obtained load capacity of the present invention in 6 hours 600 ℃ of roastings is 90% CoMgCeO 4/ HZSM-5 catalyst.The XRD analysis result shows that composite metal oxide has spinel structure.
This catalyst is used for N 2The decomposition of O, N 2The decomposition temperature T of O 10Be 390 ℃, T 95It is 580 ℃.
Embodiment 9
Take by weighing cobalt nitrate 7.83g, lanthanum nitrate 104.86g and zinc nitrate (Zn (NO 3) 26H 2O) 40.02g and citric acid 84.92g, be dissolved in the water respectively, be mixed with mixed aqueous solution, obtain the aqueous solution of metalline and organic complexing agent, molecular sieve carrier HZSM-51000g inserts in the aqueous solution and floods, and constantly stir, dry under 70 ℃ of temperature, obtain catalyst precursor, more above-mentioned presoma promptly being obtained load capacity of the present invention in 10 hours 400 ℃ of roastings is 5% La 1.8ZnCo 0.2O 4/ HZSM-5 catalyst.The XRD analysis result shows that composite metal oxide has perovskite-like structure.
This catalyst is used for N 2The decomposition of O consists of 20v%N at reacting gas 2O, 15.8v%O 2Condition under, N 2The decomposition temperature T of O 10Be 360 ℃, T 95It is 550 ℃.
Embodiment 10
Take by weighing cobalt nitrate 365.69g, lanthanum nitrate 60.46g and 50% manganese nitrate solution 249.84g and citric acid 440.63g, be dissolved in the water respectively, be mixed with mixed aqueous solution, obtain the aqueous solution of metalline and organic complexing agent, molecular sieve carrier HZSM-181000g inserts in the aqueous solution and floods, and constantly stir, dry under 70 ℃ of temperature, obtain catalyst precursor, more above-mentioned presoma promptly being obtained load capacity of the present invention in 4 hours 600 ℃ of roastings is 15% La 10.2MnCo 1.8O 4/ HZSM-18 catalyst.The XRD analysis result shows that composite metal oxide has spinel structure.
This catalyst is used for N 2The decomposition of O, N 2The decomposition temperature T of O 10Be 395 ℃, T 95It is 580 ℃.
Embodiment 11
Take by weighing copper nitrate 66.22g, lanthanum nitrate 273.38g and citric acid 173.01g, be dissolved in the water respectively, be mixed with mixed aqueous solution, obtain the aqueous solution of metalline and organic complexing agent, molecular sieve carrier HZSM-51000g inserts in the aqueous solution and floods, and constantly stir, dry under 70 ℃ of temperature, obtain catalyst precursor, more above-mentioned presoma promptly being obtained load capacity of the present invention in 8 hours 500 ℃ of roastings is 10% La 2CuO 4/ RPSA catalyst.The XRD analysis result shows that composite metal oxide has perovskite-like structure.
This catalyst is used for N 2The decomposition of O, N 2The decomposition temperature T of O 10Be 350 ℃, T 95It is 510 ℃.

Claims (8)

1, a kind of catalyst contains composite metal oxide and molecular sieve carrier, and composite metal oxide loads on the molecular sieve carrier, it is characterized in that:
Described composite metal oxide has spinel structure and/or perovskite-like structure, and general molecular formula is Co 3-xM xO 4Or La 2-yM yBO 4, M is one or both or the two or more combination that is selected from rare earth metal, transition metal, alkali metal or the alkaline-earth metal, B is one or more the combination that is selected from the transition metal, x=0～2.8, y=0～1.8.
2, according to the described catalyst of claim 1, it is characterized in that: described molecular sieve carrier is molecular sieve with MFI structure, in the Y structure molecular screen one or more.
3, catalyst according to claim 2 is characterized in that: the molecular sieve of the described MFI of having structure is HZSM-5, RPSA and HZSM-18, and the molecular sieve of described Y structure is the HY molecular sieve.
4, catalyst according to claim 1 is characterized in that: described rare earth metal is La, Ce, Pr or Nd; Transition metal is Fe, Ni, Cu, Zn, Mn, Cr, V or Zr; Alkali metal is Na, K, Rb or Cs; Alkaline-earth metal is Mg, Ca, Sr or Ba.
5, catalyst according to claim 1 is characterized in that: be benchmark with the catalyst weight, composite metal oxide is 0.1～90% in the load capacity of molecular sieve carrier, and the preferred negative carrying capacity is 0.1～50%.
6, a kind of method for preparing the described catalyst of claim 1, it is characterized in that: this method may further comprise the steps:
A) with corresponding metal salt and organic complexing agent, be dissolved in the water respectively, be mixed with mixed aqueous solution, obtain the aqueous solution of metalline and organic complexing agent,
B) molecular sieve carrier is inserted in (a) aqueous solution and flood, and dry under 30～90 ℃ of temperature, obtain catalyst precursor, then catalyst precursor is placed 400～1000 ℃ of following roastings 2～10 hours, promptly obtain catalyst of the present invention.
7, the described method for preparing catalyst of claim 1～5 is characterized in that: described organic complexing agent is a kind of in oxalic acid, citric acid or the acetic acid, and described slaine is nitrate or acetate.
8, the described catalyst of claim 1 is used for flue gas or industrial waste gas N 2The decomposition of O.
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