CN102658164A - NOx storage-reduction catalyst using nanosized composite oxide as carrier, and method for producing same - Google Patents
NOx storage-reduction catalyst using nanosized composite oxide as carrier, and method for producing same Download PDFInfo
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- CN102658164A CN102658164A CN2011104065340A CN201110406534A CN102658164A CN 102658164 A CN102658164 A CN 102658164A CN 2011104065340 A CN2011104065340 A CN 2011104065340A CN 201110406534 A CN201110406534 A CN 201110406534A CN 102658164 A CN102658164 A CN 102658164A
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Abstract
The invention discloses a NOx storage-reduction catalyst using a nanosized composite oxide as a carrier and a method for producing the same. The NOx storage-reduction catalyst is characterized by using a nanosized composite oxide as a carrier, which carries nanoscale catalytic active components of Pt, Ba, Co and Ag, the nanosized composite oxide being a coprecipitate of Al2O3, ZrO2 and CeO2, or ZrxCe1-xO2, or nano-Al2O3-centered Al2O3-ZrO2 and Al2O3-CeO2 obtained by coating Al2O3 with ZrO2 or CeO2. Compared with the prior art of catalyst preparation technology, the NOx storage-reduction catalyst using a nanosized composite oxide as a carrier provided by the invention enables an improvement in anti-sintering capability of metal/nanosized compound catalysts and a stability of catalytic performance, and is simple in technology, low in cost and convenient in practical production operation. The efficient catalytic reaction performance of the catalyst produced by the method of the invention can be maintained after a stable operation of 1000 hours under a high temperature of 800 DEG C.
Description
Technical field
The invention belongs to the motor vehicle tail-gas purifying field, be specifically related to the NO that a kind of nano composite oxide is a carrier
XStorage and reduction catalyst and preparation method.
Background technology
Huge in current energy demand, resource is near exhausted, under the situation of environment severe exacerbation, internal-combustion engines vehicle be the big power consumer be again the major source of pollutant of environment, so reduce motor vehicle fuel consumption, reducing tail gas pollution is an important topic of current scientific research.
The lean-combustion engine technology has the efficiency of combustion height, and the advantage that noxious emission is few is to reduce motor vehicle fuel consumption, reduces the major technique of tail gas pollution, and is widelyd popularize.But, because oxygen content significantly increases in the motor-vehicle tail-gas that the lean-combustion engine technology is produced, the result who is caused is that CO and HC content descend, and NO
XContent raise.Thereby, NO in the oxygen enrichment tail gas
XElimination become the problem that must solve.NO
XStorage and reduction (NO
XStorage-Reduction, NSR) catalysis technique is to solve NO in the lean-combustion engine oxygen enrichment tail gas
XThe most promising a kind of technological approaches of reduction.
Correlation technique and application study are all very active in indivedual developed countries; Mainly concentrate on the system integration and the optimal control of engine and tai-gas clean-up catalyst; The relation of catalyst composition, structure and performance, and auxiliary agent or carrier The properties etc. are wherein improving catalyst n O
XExploration reduces the use amount of Pt on the basis of storage capacity, the anti-agglutinatting property of raising catalyst can be development of practical NO
XThe core content of storage-reducing catalyst.In China, about the also starting gradually of basic research work of NSR catalyst, but the systematicness of research and the degree of depth and international most advanced level still have obvious gap.Under the situation that the technological system integration of present correlation engine technology and tail gas clean-up and optimal control reach its maturity, how further to improve the NO of catalyst
XStorage capacity, to keep enough catalytic stability and market acceptable cost in the life-span at vehicle complete vehicle be to limit the major obstacle of this technical application.
At present, typical Pt-Ba/Al
2O
3Catalyst is NO under the actual motion condition
XTherefore the general less than 10% of the utilization rate of storage material Ba, improves catalyst n O
XThe directly the most effective means of storage capacity are to improve NO
XThe utilization rate of storage material.
Sulfur poisoning and high temperature sintering that two key reasons that influence catalyst stability are catalyst.The main cause of catalyst sulfur poisoning is SO
3With NO
XThe storage material reaction has formed stable sulfate, thereby has suppressed catalyst to NO
XAbsorption store.But, it is to be noted high temperature (＞650 ℃) thus handle and sulfate to be decomposed fully make fouled catalyst obtain regeneration, therefore, it is the anti-sintering problem of active component that the sulfur poisoning problem of solution catalyst largely can be returned root.Reducing and Pt and NO of the specific area that high temperature sintering caused of catalyst
XGrowing up of storage material particle can reduce NO
XThe utilization rate of storage material, and make catalyst that irreversibly inactivation take place.For guaranteeing that the NSR catalyst has enough NO in the whole life cycle of automobile
XDetergent power must contain a large amount of Pt to compensate the loss of the Pt metal surface area that causes because of sintering in the catalyst, these measures have further increased the catalyst cost.Therefore, the high temperature sintering resistant performance that improves catalyst not only directly influences life of catalyst, for the cost that reduces the NSR catalysis technique positive effect is arranged also, is the key point of development of practical NSR catalyst.
Summary of the invention
The nano composite oxide that the objective of the invention is to provide for the deficiency that solves above-mentioned prior art a kind of high temperature sintering resistant performance that improves catalyst, reduces the use cost of precious metals pt is the NO of carrier
XStorage and reduction catalyst and preparation method.
To achieve these goals, a kind of nano composite oxide that the present invention designed is the NO of carrier
XStorage and reduction catalyst is characterized in that: with the nano composite oxide is carrier, the Pt of loaded with nano yardstick, Ba, Co, Ag catalytic activity component on the carrier.
Described nano composite oxide is Al
2O
3, ZrO
2, CeO
2Coprecipitate or Zr
xCe
1-xO
2Or with nanometer Al
2O
3ZrO for " core "
2Or CeO
2Coat Al
2O
3Al
2O
3-ZrO
2And Al
2O
3-CeO
2
Described nano composite oxide is of a size of 5nm～40nm.
Described Ba species are to be BaO or BaCO
3
The weight ratio of nano composite oxide and Pt, Ba, Co, Ag catalytic activity component is respectively in 100 parts nano composite oxide: Pt content is 0.1 part～1.5 parts; Ba content is 1.0 parts～15.0 parts; Co content is 0.5 part～15 parts; Ag content is 0.5 part～2.5 parts.
A kind of nano composite oxide provided by the invention is the NO of carrier
XThe preparation method of storage and reduction catalyst is characterized in that may further comprise the steps:
Step 1, different oxides are carried out co-precipitation, dry then, roasting method prepares composite oxides; Thereby the nano composite oxide of preparation required size; Process the nano composite oxide slurries again;
Step 2, on the described nano composite oxide of step 1 supporting Pt, Ba species; Be that 0.1 part～1.5 parts nitrate or chloride solution is according to required consumption earlier promptly with Pt content; Quantitative joins in the nano composite oxide slurries, and slurry temperature remains on 35 ℃～55 ℃, and adding Ba content after 0.5～3 hour is 1.0 parts～15.0 parts barium acetates or barium nitrate or brium carbonate solution; 0.5 add concentration after～3 hours again and be 5.0%～20.0% methyl amine solution; After the ageing 6～48 hours,, obtain catalyst matrix through dry, roasting;
Step 3, Co oxide and Ag metal are introduced in the described catalyst matrix of step 2 simultaneously, be about to catalyst matrix and be distributed in the aqueous solution, stir; Be that 0.5 part～15 parts nitrate or chloride or acetate solution is according to needed content earlier with Co content; Quantitative joins in the catalyst matrix slurries, and slurry temperature remains on 35 ℃～55 ℃, and adding Ag content is 0.5 part～2.5 parts liquor argenti nitratis ophthalmicus after 0.5～3 hour; 0.5 add concentration after～3 hours again and be 5.0%～20.0% methyl amine or solution; After drying, roasting, obtain finished product, i.e. NO
XStorage and reduction catalyst.
In step 2, said baking temperature is 80 ℃～200 ℃, and be 2h～48h drying time; Sintering temperature is 600 ℃～1000 ℃, and roasting time is 2h～48h.In step 2, said baking temperature is preferably 120 ℃～180 ℃, is preferably 12h～24h drying time; Sintering temperature is preferably 750 ℃～850 ℃, and roasting time is preferably 6h～10h.
In step 3, said baking temperature is 80 ℃～200 ℃, and be 2h～48h drying time; Sintering temperature is 600 ℃～1000 ℃, and roasting time is 2h～48h.In step 3, said baking temperature is preferably 120 ℃～180 ℃, is preferably 12h～24h drying time; Sintering temperature is preferably 750 ℃～850 ℃, the preferred 6h～10h of roasting time.
The present invention passes through in the preparation process, to adopt the combination of different components and different interpolation orders, thereby constructs and regulated and control the nanostructured of catalyst, makes that the nanostructured microscopic dimensions of catalyst is littler; Size Distribution is more concentrated; More easy-sintering is not assembled, thereby improves the NOx storage capacity of catalyst, and replaces the part precious metals pt with cheap transition metal and transition metal oxide on this basis; With the use amount of reduction Pt, and then the anti-agglutinatting property ability of raising catalyst.
Compared with prior art, a kind of nano composite oxide provided by the invention NO that is carrier
XStorage and reduction catalyst is to be carrier with the nano composite oxide, a kind of metal/nanometer compound type catalyst of the Pt of loaded with nano yardstick, Ba, Co, Ag catalytic active component on the carrier.Through preparation method of the present invention, make between the same type nano granular of catalyst surface by other nano particle good, also form the nanostructured that supports each other simultaneously between different nano particles, make it have extra stabilization property.Even mixing between the approaching different nano particles of particle diameter makes the Contact Boundary between the different nano particles with respect to traditional catalyst showed increased arranged, and this is for NO
XThis class of storage and reduction needs reaction intermediates (NO
X) (Pt, Ba, Co, Ag) constantly moves between the difference in functionality active component catalytic process, have outstanding advantage.Simultaneously, because the high-specific surface area of nano-complex, and the interval action of xenogenesis nano particle, make active component Ba species can remain suitable decentralization, significantly improved the utilization rate of Ba, improve the NO of catalyst
XStorage capacity, and then improved the catalytic performance of catalyst.Simultaneously, replaced expensive Pt metal Pt with relatively inexpensive metal A g and metal oxide Co oxide portion branch, reduced the NSR catalyst production cost, wherein, the effect of Co oxide is that catalytic oxidation NO generates NO
2, the effect of metal A g is a Reduction of NO
X, introduce the purpose that metal A g and metal oxide Co have realized reducing metal Pt content in the catalyst simultaneously.This nano composite oxide is the NO of carrier
XStorage and reduction catalyst has the efficient anti-sintering of low Pt.
Compare with existing catalyst preparation technology, a kind of nano composite oxide provided by the invention is the NO of carrier
XThe preparation method of storage and reduction catalyst through the nanostructured of regulation and control catalyst, has improved the anti-caking power of metal/nanometer complex catalyst, stablized catalytic performance, and technology is simple, and is with low cost, is convenient to the actual production operation.Catalyst through the present invention preparation after 1000 hours, still can be kept its catalytic perfomance efficiently 800 ℃ high temperatures operation.That the present invention makes is the efficient anti-sintering NO of low Pt of carrier with the nano composite oxide
XThe technical parameter of storage and reduction catalyst is following:
Nano composite oxide particle diameter 5nm～40nm
Metal or metal oxide particle diameter 5nm～20nm
The specific embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Embodiment 1:
The nano composite oxide that present embodiment provides is the NO of carrier
XStorage and reduction catalyst is with nano composite oxide Zr
xCe
1-xO
2Be carrier, the Pt of loaded with nano yardstick, Ba, Co, Ag catalytic activity component on the carrier.100 parts of Zr with weight ratio
xCe
1-xO
2Be nano composite oxide, the catalytic activity component of loaded with nano yardstick is: Pt content is 0.8 part nitrate; Ba content is 8.0 parts barium acetate; Co content is 10 parts nitrate; Ag content is 1.0 parts silver nitrate; 150 ℃ of baking temperatures, drying time 24h; 800 ℃ of sintering temperatures, roasting time 10h.
The nano composite oxide that present embodiment provides is the NO of carrier
XThe preparation method of storage and reduction catalyst is characterized in that may further comprise the steps:
Step 1, with ZrO
2, CeO
2Carry out co-precipitation, thus nano composite oxide Zr dry then, roasting preparation required size
xCe
1-xO
2
Step 2, at the described nano composite oxide Zr of step 1
xCe
1-xO
2Last supporting Pt, Ba species are that 0.8 part nitrate solution joins nano composite oxide Zr with Pt content earlier promptly
xCe
1-xO
2In the slurries, slurry temperature remains on 35 ℃～55 ℃, and adding Ba content is 8.0 parts barium acetate after 0.5～3 hour; 0.5 add concentration after～3 hours again and be 5.0%～20.0% methyl amine solution; After the ageing 6～48 hours,, obtain catalyst matrix through dry, roasting; Wherein baking temperature is 150 ℃, drying time 24h; 800 ℃ of sintering temperatures, roasting time 10h.
Step 3, Co oxide and Ag metal are introduced in the described catalyst matrix of step 2 simultaneously, be about to catalyst matrix and be distributed in the aqueous solution, stir; Be that 10 parts nitrate joins in the catalyst matrix slurries with Co content earlier, slurry temperature remains on 35 ℃～55 ℃, adds Ag content after 0.5～3 hour and be 1.0 parts liquor argenti nitratis ophthalmicus; 0.5 add concentration after～3 hours again and be 5.0%～20.0% methyl amine or solution; After drying, roasting, obtain finished product, i.e. NO
XStorage and reduction catalyst.Wherein baking temperature is 150 ℃, drying time 24h; 800 ℃ of sintering temperatures, roasting time 10h.
In the above-described embodiments, in weight ratio be 100 parts nano composite oxide Zr
xCe
1-xO
2On, can be that Pt content is arranged is 0.1 part～1.5 parts nitrate in load; Ba content is 1.0 parts～15.0 parts barium acetate; Co content is 0.5 part～15 parts nitrate; Ag content is 0.5 part～2.5 parts silver nitrate.
Embodiment 2:
The nano composite oxide that present embodiment provides is the NO of carrier
XStorage and reduction catalyst is with nano composite oxide Al
2O
3-ZrO
2Be carrier, the Pt of loaded with nano yardstick, Ba, Co, Ag catalytic activity component on the carrier.100 parts of Al with weight ratio
2O
3-ZrO
2Be nano composite oxide, the catalytic activity component of loaded with nano yardstick is: Pt content is 0.1 part nitrate; Ba content is 8 parts barium acetate; Co content is 10 parts nitrate; Ag content is 2.0 parts silver nitrate; 150 ℃ of baking temperatures, drying time 24h; 800 ℃ of sintering temperatures, roasting time 10h.
The nano composite oxide that present embodiment provides is the NO of carrier
XThe preparation method of storage and reduction catalyst is characterized in that may further comprise the steps:
Step 1: choose nano composite oxide Al
2O
3-ZrO
2
Step 2, at the described nano composite oxide Al of step 1
2O
3-ZrO
2Last supporting Pt, Ba species are that 0.1 part nitrate solution joins nano composite oxide Al with Pt content earlier promptly
2O
3-ZrO
2In the slurries, slurry temperature remains on 35 ℃～55 ℃, and adding Ba content is 8.0 parts barium acetate after 0.5～3 hour; 0.5 add concentration after～3 hours again and be 5.0%～20.0% methyl amine solution; After the ageing 6～48 hours,, obtain catalyst matrix through dry, roasting; Wherein baking temperature is 120 ℃～180 ℃, and be 12h～24h drying time; Sintering temperature is 750 ℃～850 ℃, and roasting time is 6h～10h.
Step 3, Co oxide and Ag metal are introduced in the described catalyst matrix of step 2 simultaneously, be about to catalyst matrix and be distributed in the aqueous solution, stir; Be that 10 parts nitrate joins in the catalyst matrix slurries with Co content earlier, slurry temperature remains on 35 ℃～55 ℃, adds Ag content after 0.5～3 hour and be 2.0 parts liquor argenti nitratis ophthalmicus; 0.5 add concentration after～3 hours again and be 5.0%～20.0% methyl amine or solution; After drying, roasting, obtain finished product, i.e. NO
XStorage and reduction catalyst.Said baking temperature is 120 ℃～180 ℃, and be 12h～24h drying time; Sintering temperature is 750 ℃～850 ℃, and roasting time is 6h～10h.The parameter that can control especially is 150 ℃ of baking temperatures, drying time 24h; 800 ℃ of sintering temperatures, roasting time 10h.
The above is the specific embodiment of the present invention, should be pointed out that under the prerequisite based on the principle of the invention, and some variations or the improvement made by those of ordinary skills also are regarded as protection scope of the present invention.
Claims (10)
1. NO that nano composite oxide is a carrier
XStorage and reduction catalyst is characterized in that: with the nano composite oxide is carrier, the Pt of loaded with nano yardstick, Ba, Co, Ag catalytic activity component on the carrier.
2. nano composite oxide according to claim 1 is the NO of carrier
XStorage and reduction catalyst is characterized in that described nano composite oxide is Al
2O
3, ZrO
2, CeO
2Coprecipitate or Zr
xCe
1-xO
2Or with nanometer Al
2O
3ZrO for " core "
2Or CeO
2Coat Al
2O
3Al
2O
3-ZrO
2And Al
2O
3-CeO
2
3. nano composite oxide according to claim 1 and 2 is the NO of carrier
XStorage and reduction catalyst is characterized in that described nano composite oxide is of a size of 5nm～40nm.
4. nano composite oxide according to claim 1 and 2 is the NO of carrier
XStorage and reduction catalyst, it is characterized in that the weight ratio of nano composite oxide and Pt, Ba, Co, Ag catalytic activity component is respectively in 100 parts nano composite oxide: Pt content is 0.1 part～1.5 parts; Ba content is 1.0 parts～15.0 parts; Co content is 0.5 part～15 parts; Ag content is 0.5 part～2.5 parts.
5. nano composite oxide according to claim 3 is the NO of carrier
XStorage and reduction catalyst, it is characterized in that the weight ratio of nano composite oxide and Pt, Ba, Co, Ag catalytic activity component is respectively in 100 parts nano composite oxide: Pt content is 0.1 part～1.5 parts; Ba content is 1.0 parts～15.0 parts; Co content is 0.5 part～15 parts; Ag content is 0.5 part～2.5 parts.
6. NO that nano composite oxide is a carrier
XThe preparation method of storage and reduction catalyst is characterized in that may further comprise the steps:
Step 1, different oxides are carried out co-precipitation, dry then, roasting method prepares composite oxides; Thereby the nano composite oxide of preparation required size; Process the nano composite oxide slurries again;
Step 2, on the described nano composite oxide of step 1 supporting Pt, Ba species; Be that 0.1 part～1.5 parts nitrate or chloride solution is according to required consumption earlier promptly with Pt content; Quantitative joins in the nano composite oxide slurries, and slurry temperature remains on 35 ℃～55 ℃, and adding Ba content after 0.5～3 hour is 1.0 parts～15.0 parts barium acetates or barium nitrate or brium carbonate solution; 0.5 add concentration after～3 hours again and be 5.0%～20.0% methyl amine solution; After the ageing 6～48 hours,, obtain catalyst matrix through dry, roasting;
Step 3, Co oxide and Ag metal are introduced in the described catalyst matrix of step 2 simultaneously, be about to catalyst matrix and be distributed in the aqueous solution, stir; Be that 0.5 part～15 parts nitrate or chloride or acetate solution is according to needed content earlier with Co content; Quantitative joins in the catalyst matrix slurries, and slurry temperature remains on 35 ℃～55 ℃, and adding Ag content is 0.5 part～2.5 parts liquor argenti nitratis ophthalmicus after 0.5～3 hour; 0.5 add concentration after～3 hours again and be 5.0%～20.0% methyl amine or solution; After drying, roasting, obtain finished product, i.e. NO
XStorage and reduction catalyst.
7. described nano composite oxide according to claim 6 is the NO of carrier
XThe preparation method of storage and reduction catalyst is characterized in that at baking temperature described in the step 2 be 80 ℃～200 ℃, and be 2h～48h drying time; Sintering temperature is 600 ℃～1000 ℃, and roasting time is 2h～48h.
8. nano composite oxide according to claim 7 is the NO of carrier
XThe preparation method of storage and reduction catalyst is characterized in that being preferably 120 ℃～180 ℃ at baking temperature described in the step 2, drying time preferred 12h～24h; Preferred 750 ℃～850 ℃ of sintering temperature, roasting time is preferably 6h～10h.
9. nano composite oxide according to claim 6 is the NO of carrier
XThe preparation method of storage and reduction catalyst is characterized in that in step 3, and baking temperature is 80 ℃～200 ℃, and be 2h～48h drying time; Sintering temperature is 600 ℃～1000 ℃, and roasting time is 2h～48h.
10. nano composite oxide according to claim 9 is the NO of carrier
XThe preparation method of storage and reduction catalyst is characterized in that in step 3, preferred 120 ℃～180 ℃ of baking temperature, drying time preferred 12h～24h; Preferred 750 ℃～850 ℃ of sintering temperature, the preferred 6h～10h of roasting time.
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| CN2011104065340A CN102658164A (en) | 2011-12-08 | 2011-12-08 | NOx storage-reduction catalyst using nanosized composite oxide as carrier, and method for producing same |
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Cited By (1)
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| WO2008127671A2 (en) * | 2007-04-11 | 2008-10-23 | Exxonmobil Research And Engineering Company | Regenerable sulfur traps for on-board vehicle applications |
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Application publication date: 20120912 |