CN101249460A - Multipollutant catalytic removedcomposite oxides in poor/rich burn type motorcycle tail gas - Google Patents
Multipollutant catalytic removedcomposite oxides in poor/rich burn type motorcycle tail gas Download PDFInfo
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Abstract
The invention relates to a method of removing various pollutants discharged from vehicle tail gas by composite oxides as the catalyst, which is characterized in that adjusting ionic constituent, performing isomorphous replacement, selecting the appropriate crystal structure, loading with high specific surface carrier, etc. to vary physical chemical properties of the composite oxides so as to satisfy the requirements that various engines (gasoline engine and diesel engine) performs catalytic treatment on various pollutants (nitrogen oxide, carbon monoxide, hydrocarbon compound, carbon-containing granular substance and oxygen-containing organic substance). The prepared composite oxides catalyst has high oxygen and electron transfer capacity, good mechanical and thermal stability, strong resistance to water intoxication, low cost, and wide potential application; which can be used for treating multiple pollutants in the vehicle tail gas.
Description
Technical field
The present invention relates to the application of composite oxides aspect catalytic purification of motor vehicle tail gas, belong to the environmental catalysis field.It is catalyst that this technology adopts a series of composite oxides such as perovskite, spinelle, white tungsten stone, pyrochlore, tungsten bronze, heteropoly acid; reduced the discharging of pollutants such as nitrogen oxide, carbon monoxide, hydrocarbons, carbon-bearing particulate matter, oxygen-bearing organic matter, itrogenous organic substance in the motor-vehicle tail-gas significantly; thereby satisfied the requirement of associated drain rule, reached the purpose of protection environment.
Technical background
Composite oxides are different from the mixture of simple oxide, are a kind of multi-component oxides with definite superstructure.These composite oxides mostly are non-stoichiometry, its electricity, magnetic, light, superconduction, catalytic performance uniqueness wherein have practical significance and comprise composite oxides such as Ca-Ti ore type, spinel-type, white tungsten stone type, pyrochlore-type, tungsten bronze type and heteropoly acid what catalytic field caused extensive interest.Non-chemically the composite oxides of dosage exist the obvious defects structure: cation defect (oxygen excess), anion defect (oxygen room), and can further regulate this structural defective by the multiple cation valence of isomorphous replacement generation.These defect sturctures are considered to have the excellent transmission oxygen and the ability of electronics in redox reaction, thereby can consider to adopt composite oxides that carbon monoxide, hydrocarbon, carbon-bearing particulate matter, oxygen-bearing organic matter in the motor-vehicle tail-gas etc. are realized oxidation; Simultaneously nitrogen oxide is reduced; Obtain products such as innoxious carbon dioxide, water and nitrogen.
Oxygen according to engine fires than it being divided into rich burn type and fuel-lean type.Gasoline engine belongs to rich combustion (oxygen deprivation) type more, oxygen content is relatively low in its discharging tail gas, and reduction components (carbon monoxide, hydrocarbon) content height, adopt traditional three-way catalyst (alundum (Al load platinum, rhodium noble metal) can realize the purification of tail gas under this situation, but higher cost has limited the practical application of noble metal catalyst.In recent years, poor combustion (oxygen enrichment) the type gasoline engine that adopts for the utilization ratio that improves fuel has obtained paying close attention to and promoting, carbon monoxide in its tail gas and hydrocarbon have obtained sufficient oxidation under excess oxygen, thereby content is lower, but higher oxygen concentration also will cause traditional three-way catalyst to lose efficacy.Diesel engine also is to work under the condition of poor combustion (oxygen enrichment), and contains a large amount of carbon-bearing particulate matters in the tail gas.As seen, the purification of motor-vehicle tail-gas is faced with the comparatively complicated tail gas composition that various operating modes produce, and is difficult to obtain fine solution by the load of a kind of simple oxidation thing.And the diversity of composite oxides (different ion forms, different crystalline structure) and adjustable sex change (isomorphous replacement) are more suitable at the removing of different atmosphere exhaust pollutants it, and cost is lower.And active catalytic components can promptly obtain sufficient dispersion in composite oxides, and it is well fixing to have got back, the inactivation of having avoided factors such as loss, volatilization, sintering to cause.Porous, inorganic thing supported silver, noble metal, transition-metal catalyst (Chinese patent that the inventor once applied for, the patent No. 216040) lays particular emphasis on removing of nitrogen oxide under the excess oxygen, its active component is the mixing of one or more metals and metal simple oxide, and (0-20%) carries out catalysis treatment to multiple pollutants such as tail gas nitrogen oxide, carbon monoxide, hydrocarbon, carbon-bearing particulate matter, oxygen-bearing organic matter, itrogenous organic substances in the oxygen concentration scope of broad and the composite oxides that the present invention relates to form specific superstructure, physicochemical property uniqueness are used for.
Sol-gel process, coprecipitation, solid reaction process, microemulsion method, citrate complexometry, spray drying process, freeze-drying etc. are used the preparation composite oxides.But these preparation methods exist problems such as complex process, cost be higher, seriously polluted, all are not suitable for large-scale industrial production.Adopt above method simultaneously, also the specific area of composite oxides can only be brought up to the level of 30 meters squared per gram.And the inventor once adopted mechanical milling method to prepare nanoscale composite oxides (Chinese patent, publication number CN1868967), and its specific area reaches as high as about 100 meters squared per gram.In addition, this method also helps the generation of crystal edge in the composite oxides, crystal angle, defect sturcture, thereby obtains excellent catalytic performance.The present invention is applicable to the serial composite oxides of the prepared in various methods that comprises mechanical lapping.
Summary of the invention
The present invention is directed to different tail gas atmosphere, select the composite oxides and their mixture of specific composition, crystalline structure to come the modulation catalytic performance, remove when reaching multiple discharging pollutants, what it was concrete thes contents are as follows:
1. the general general formula of composite oxide catalysts of the present invention is:
Ca-Ti ore type (ABO
3), spinel-type (routine AB
2O
4, trans BABO
4), scheelite type (ABO
4), heteropoly acid (AB
12O
40), pyrochlore-type (A
2B
2O
7), tungsten bronze type (A
xWO
3) and other general formula be A
xB
yO
zComposite oxides;
Wherein A is one or more in (La, Be, Mg, Ti, Ca, Ba, Cs, K, Sr, Ce, Zn, Pr, Hf, Ag, Au, Pd, Ru, Rh, Pt, Re, Cr, Rb, Nd, Bi, Zr, Pb, Y, Sb, Li, Fe, Co, Cu, Sm, Sn, Cd, Ni, In, Ga, Ge, Mn, P, Mo) plasma;
Wherein B is one or more in (Co, Fe, Ni, Mn, Cr, Ti, Cu, Mg, V, Nb, Ta, Mo, W, Zn, Zr, Ru, Ag, Au, Pd, Ru, Rh, Pt, Re, Al, W, Ga, Ge, B, C, Si, P, S, Cl, As, Br, In, Sn, Sb) plasma.
The present invention relates to one or more mixture of above-mentioned composite oxides, and comprise it is carried on inorganic porous, high surface area carrier, wherein carrier comprises various M
xO
y, zeolite, molecular sieve, sepiolite, active carbon, lamellar clay, and M is in (Al, Si, Ti, Zr, Co, Fe, Ni, Mn, Cr, Cu, Mg, V, Nb, Ta, Mo, W, Zn, W, Ga, Ge, In, Sn, Sb) plasma one or more.
The present invention not only relates to various composite oxide powers, also relates to (sphere, sheet, graininess, cylindrical, annular etc.) prepared therefrom preformed catalyst.Do not use any adhesive in the forming process or use in the adhesives such as Ludox, aluminium colloidal sol, inorganic acid, organic acid, inorganic base, water one or more.
Aforementioned catalyst can further be coated on ceramic honeycomb and metallic sieve stromal surface, make have porous channel, the integral catalyzer of low pressure drop, be used for the purification of motor-driven tail gas, wherein the hole density of honeycomb is the 50-800/ square inch, the catalyst component load capacity is 5-80%, and adhesive as previously mentioned.
2. preparation method
The requirement that the composite oxides of mentioning among the present invention use according to reality can adopt the serial of methods that comprises sol-gel process, coprecipitation, solid reaction process, microemulsion method, citrate complexometry, spray drying process, freeze-drying, mechanical milling method etc. to be prepared from.The composite oxides of mechanical milling method preparation wherein, specific area height, crystallite dimension are nanoscale, catalytic performance excellence.
3. motor-vehicle tail-gas is formed
(1) rich burn type gasoline locomotive tail gas:
Oxygen content: 0.5-5%; Amount of nitrogen oxides: 0-4,000ppm;
Carbon monoxide content: 0-14%; Carbon dioxide content: 4-18%;
THC content: 300-1000ppm; Hydrogen content: 0-6%;
(2) fuel-lean type gasoline locomotive and diesel locomotive tail gas:
Oxygen content: 5-20%; Amount of nitrogen oxides: 0-4,000ppm;
Carbon monoxide content: 0-4000ppm; THC content: 0-800ppm;
Carbon-bearing particulate matter: 0.1-4BSU;
(3) reaction atmosphere of catalyst activity evaluation:
O
2：0-20％；NO：0-3,000ppm；CO：0-5000ppm；C
3H
6：0-5,000ppm
Carbon granule: the 2-10% of catalyst weight; GHSV=10,000-100,000/h
4. the interpolation of reduction components
Composition according to tail gas, in order to reach best removal of nitrogen oxide effect, can consider to add a series of reduction components in tail gas, wherein hydrocarbons comprises: one or more of all kinds of alkane, alkene, alkadienes, alkynes, benzene,toluene,xylene, kerosene, gasoline, diesel oil etc.; Wherein oxygen-bearing organic matter comprises: one or more of all kinds of alcohol, ether, aldehyde, ketone, acid etc.; Comprise other reduction components such as ammonia, hydrogen, urea in addition.
The interpolation of above-mentioned (gaseous state or liquid state) reduction components can adopt the form of spraying to realize by the upstream of catalyst in exhaust pipe, also above-mentioned reduction components can be injected into combustion chambers of internal combustion engines, the remaining reduction components of utilization burning is come the nitrogen oxide in the catalytic reduction tail gas.
5. with the perovskite composite oxide purification of the main active component nitrogen oxide that is used under the oxygen deprivation condition rich combustion gasoline engine tail gas, carbon monoxide, hydrocarbon.
Be lower than at oxygen concentration under 5% the situation, consider that adopting perovskite composite oxide is major catalyst, it is formed as previously mentioned, this catalyst can use separately, or the isomorphous of passing through the B position replaces, or pass through the high surface area carrier load, or (spinel-type, scheelite type, pyrochlore-type, tungsten bronze type, heteropoly acid and other general formula are A with other crystal formation composite oxides
xB
yO
zComposite oxides) mix, to reach removing of nitrogen oxide in the tail gas, carbon monoxide, hydrocarbon.
6. with the spinelle type composite oxides purification that main active component is used for poor combustion gasoline engine and diesel engine vent gas nitrogen oxide under the excess oxygen, carbon monoxide, hydrocarbon.
Be higher than at oxygen concentration under 5% the situation, consider that adopting spinelle type composite oxides is major catalyst, it is formed as previously mentioned, this catalyst can use separately, or the isomorphous of passing through the B position replaces, or pass through the high surface area carrier load, or (Ca-Ti ore type, scheelite type, pyrochlore-type, tungsten bronze type, heteropoly acid and other general formula are A with other crystal formation composite oxides
xB
yO
zComposite oxides) mix, to reach removing of nitrogen oxide in the tail gas, carbon monoxide, hydrocarbon.
7. with the perovskite composite oxide purification that main active component is used for diesel engine vent gas carbon-bearing particulate matter under the excess oxygen.
Be higher than at oxygen concentration under 5% the situation, consider that adopting perovskite composite oxide is major catalyst, it is formed as previously mentioned, this catalyst can use separately, or the isomorphous of passing through the B position replaces, or pass through the high surface area carrier load, or (spinel-type, scheelite type, pyrochlore-type, tungsten bronze type, heteropoly acid and other general formula are A with other crystal formation composite oxides
xB
yO
zComposite oxides) mix, to reach removing of carbon-bearing particulate matter in the tail gas.
Based on technology provided by the invention there are following characteristics in the purification that composite oxides are used for pollutant of vehicle exhaust:
1. active cation is introduced in the composite oxides lattice, made it obtain good dispersion on the one hand, present advantages of high catalytic activity; Active component is fixed on the other hand, has avoided the generation of its loss, volatilization, sintering.
2. Zhi Bei composite oxide catalysts has a large amount of faults of construction, and especially oxygen room and oxygen excess play important catalytic action in comprising a series of redox reactions such as nitrogen oxide reduction, carbon monoxide oxidation, oxidizing hydrocarbon, carbon-bearing particulate matter burning.
3. by selection, high surface area carrier load, can obtain being applicable to from richness and fire (oxygen concentration is in the 0-20% scope) effective catalyst under the poor combustion situation crystalline structure, catalytic component.
4. aforementioned composite oxide catalysts is applicable to removing of multiple exhaust pollutant (comprising nitrogen oxide, carbon monoxide, hydrocarbon, carbon-bearing particulate matter, oxygen-bearing organic matter etc.).
5. the interpolation by hydrocarbon, oxygen-bearing organic matter can solve under some engine operating condition the problem of reduction components deficiency in the tail gas, realizes best purification of nitrogen oxides effect.
Description of drawings
Fig. 1 is the structural representation of perovskite and spinelle type composite oxides.The B position ion of perovskite and 6 oxygen coordinations form the regular octahedron structure, and A position ion and 12 oxygen coordinations are enclosed in BO
6In the octahedra supercage that forms.The B position ion of spinelle also forms the regular octahedron structure with 6 oxygen coordinations, but A position ion and 4 oxygen coordinations form positive tetrahedron, and by oxygen atom and BO
6Octahedron is connected.As seen, exist bigger architectural difference between each based composite oxide, thereby cause its catalytic performance different.
Fig. 2 is for adopting the LaFe of mechanical milling method preparation
0.97Pd
0.03O
3The X ray diffracting spectrum of perovskite composite oxide.Diffraction maximum that presents among the figure and LaFeO
3The JCPDS card of composite oxides fits like a glove, and shows that perovskite structure forms in product.
Fig. 3 is for adopting the ZnGa of solid reaction process preparation
2O
4The X ray diffracting spectrum of spinel complex oxide.Diffraction maximum that presents among the figure and ZnGa
2O
4The JCPDS card of composite oxides fits like a glove, and shows that spinel structure forms in product.
Fig. 4 is LaFe
0.97Pd
0.03O
3The temperature programmed reduction curve of perovskite composite oxide.As seen from the figure, (about 80 ℃) these composite oxides can be reduced under lower temperature, have hinted the low-temperature oxidation reducing property of this catalyst excellence.
Specific embodiment
Further specify characteristics of the present invention below by example, and unrestricted the present invention; Outstanding feature of the present invention and marked improvement never are limited to following example.
Example one:
Adopt mechanical milling method to prepare LaFe
0.97Pd
0.03O
3Perovskite type composite oxide catalyst, and at the removing of rich burn type gasoline engine pollutant, at 3000ppm NO, 3000ppm C
3H
6, 3000ppm CO, 2%O
2, air speed is 50, investigate under the condition of 000/h.Catalytic activity is as shown in Table 1: catalyst shows higher low temperature active, and 300 ℃ of transformation efficiency of the oxides of nitrogen can reach 66%.Further rising temperature to 500 ℃, the conversion ratio of nitrogen oxide, hydrocarbon, carbon monoxide all can reach more than 90%.
Table one
Example two:
Adopt solid reaction process to prepare ZnGa
2O
4Spinelle type composite oxides, and it is loaded on high specific surface gamma-alumina carrier, and at the removing of fuel-lean type gasoline engine or diesel engine pollutant, at 1000ppm NO, 3000ppm C
3H
6, 10%O
2, air speed is 30, investigate under the condition of 000/h.Catalytic activity is as shown in Table 2: under excess oxygen, the nitrogen oxide maximum conversion appears at about 500 ℃, can reach 42%.And hydrocarbon raises with temperature and improves rapidly, and reaches 84% in 600 ℃.
Table two
Example three:
Adopt sol-gel process to prepare La
0.9Sr
0.1CoO
3Perovskite composite oxide, and at the removing of carbon-bearing particulate matter in the diesel emission mixes the active carbon of catalyst weight 5%, at 5%O with composite oxides
2/ He atmosphere, heating rate are 5 ℃/minute, and air speed is 50, investigate the catalytic combustion of carbon granule under the condition of 000/h.The result shows that initiation temperature is 200 ℃; In the time of 400 ℃, the oxidized elimination of 33% carbon granule; And when temperature reached 500 ℃, the conversion ratio of carbon granule was up to 98%.
Claims (7)
1, the composite oxides of multiple pollutant catalytic eliminating in poor, the rich burn type motorcycle tail gas is characterized in that:
(1) adopt sol-gel process, coprecipitation, solid reaction process, microemulsion method, citrate complexometry, spray drying process, mechanical milling method etc. in interior a series of method, preparation has the multicomponent composite oxides of the different crystal forms of long-range order superstructure
(2) cation with catalytic activity can be distributed to the composite oxides lattice equably, and active component is fixed, and has avoided its loss, volatilization and sintering, guarantees its advantages of high catalytic activity,
(3) based on the dose chemistry of composite oxides, the defect sturcture that be rich on the surface (oxygen room, cation vacancy, boundary migration oxygen etc.), composite oxides have the unique transmission oxygen and the ability of electronics, at relevant oxidation/reduction reaction excellent performance,
(4) at the characteristics separately of petrol engine and diesel engine emissions, we are by to the selection of crystalline structure and catalytic component, the load of high specific surface carrier, can obtain being applicable to from richness firing removing of (the oxygen concentration scope is 0-20%) automotive emission produces under the poor combustion situation multiple pollutant.
2, according to claims 1, it is characterized in that related composite oxides contain series such as perovskite, spinelle, scheelite, heteropoly acid, pyrochlore, tungsten bronze.
3, according to claims 1, it is characterized in that removing pollutant and comprise nitrogen oxide, various hydrocarbons, carbon monoxide, carbon containing organic particulate matter, contain oxygen organic particulate matter, nitrogenous organic particulate matter.
4, according to claims 1, it is characterized in that with the perovskite composite oxide being the purification of the main active component nitrogen oxide that is used under the oxygen deprivation condition rich combustion gasoline engine tail gas, carbon monoxide, hydrocarbon.
5, according to claims 1, it is characterized in that with the spinelle type composite oxides being the purification that main active component is used for poor combustion gasoline engine and diesel engine vent gas nitrogen oxide under the excess oxygen, carbon monoxide, hydrocarbon.
6, according to claims 1, it is characterized in that with the perovskite composite oxide being the purification that main active component is used for diesel engine vent gas carbon-bearing particulate matter under the excess oxygen.
7, according to claims 1, it is characterized in that in order to reach best removal of nitrogen oxide effect, can consider to add a series of reduction components in tail gas, wherein hydrocarbons comprises: all kinds of alkane, alkene, alkadienes, alkynes, benzene,toluene,xylene, kerosene, gasoline, diesel oil etc.; Wherein oxygen-bearing organic matter comprises: all kinds of alcohol, ether, aldehyde, ketone, acid etc.; Comprise other reduction components such as ammonia, hydrogen, urea in addition.
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| CN103990496B (en) * | 2014-04-16 | 2016-09-14 | 浙江大学 | A kind of middle low temperature SCR denitration catalyst with anti-poisoning performance and preparation method thereof |
| CN107626328B (en) * | 2017-10-12 | 2020-06-09 | 浙江师范大学 | Catalyst for catalytic oxidation of halogenated hydrocarbon and preparation method thereof |
| CN107626328A (en) * | 2017-10-12 | 2018-01-26 | 浙江师范大学 | A kind of catalyst for catalysis oxidation halogenated hydrocarbons and preparation method thereof |
| CN108686671A (en) * | 2018-06-11 | 2018-10-23 | 福州大学 | A kind of preparation of low-temp methanol decomposition catalyst |
| CN112316934A (en) * | 2020-11-24 | 2021-02-05 | 南昌大学 | Pyrochlore composite oxide carbon smoke elimination catalyst and preparation method and application thereof |
| CN112316934B (en) * | 2020-11-24 | 2022-12-02 | 南昌大学 | Pyrochlore composite oxide carbon smoke elimination catalyst and preparation method and application thereof |
| CN114425366A (en) * | 2022-04-02 | 2022-05-03 | 广东联南环保科技有限公司 | Method for preparing lanthanum-manganese-copper composite oxide catalyst |
| CN114471537A (en) * | 2022-04-02 | 2022-05-13 | 广东联南环保科技有限公司 | Preparation method of lanthanum-manganese composite oxide catalyst |
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