CN104307561A - Oxidative catalyst used for purifying diesel vehicle exhaust, and manufacturing method thereof - Google Patents
Oxidative catalyst used for purifying diesel vehicle exhaust, and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to an oxidative catalyst used for purifying diesel vehicle exhaust, and a preparation method thereof. The catalyst is composed of a substrate and a catalyst coating covered on the substrate. The catalyst coating is composed of a bottom layer and a top layer. The bottom layer is made from high temperature-resistant and anti-aging perovskite and the top layer is made from activated aluminium oxide, a rare earth oxygen-storage material, a molecular sieve, a catalyst active component and a catalyst auxiliary agent. The catalyst is high temperature-resistant and anti-aging, has high conversion rate for CO, HC in the diesel vehicle exhaust and SOF in particles, and has relatively strong inhibiting effect for oxidation of SO2. The oxidative catalyst used for purifying the diesel vehicle exhaust is high temperature-resistant and anti-aging; the preparation method is simple in process; and the catalyst has high catalytic activity, low ignition temperature and low preparation cost.
Description
Technical field
The present invention relates to a kind of oxidation catalyst of waste gas purification, more specifically to the oxidation catalyst for purifying tail gas of diesel vehicles, the invention still further relates to the preparation method of this kind for the oxidation catalyst of purifying tail gas of diesel vehicles, this catalyst effectively can reduce the discharge of SOF in carbon monoxide in exhaust gas from diesel vehicle and hydrocarbon and particle, and to SO
2oxidation have stronger inhibitory action.
Background technology
Diesel vehicle due to fuel efficiency high, power performance stablize, be widely used in communications and transportation.And along with the continuous increase of diesel vehicle quantity, the air environmental pollution that diesel vehicle causes also more and more causes the extensive concern of people.Mainly contain carbon monoxide, hydrocarbon, nitrogen oxide and particle in the pollutant of emission of diesel engine, particle mainly contains dry carbon, SOF and a small amount of sulfuric acid and sulfate composition.
Carbon monoxide, hydrocarbon and SOF are oxidized into carbon dioxide and water by oxidation by oxidation catalyst, thus reach the object reducing pollutant emission.In use do not need regeneration, safeguard simple, therefore oxidation catalyst is the exhaust gas from diesel vehicle post-processing technology be most widely used at present.But because in domestic oil product, sulfur content is higher, containing more sulfur dioxide in tail gas, and sulfur dioxide can be oxidized to sulfur trioxide forms sulfate further, along with the growing amount of sulfur trioxide is more, in tail gas, the discharge capacity of sulfate particulate increases thereupon, not only counteract the environmental benefit that part minimizing SOF brings, and sulfate can make catalysqt deactivation, poisoning, oxidation catalyst reduces the conversion capability of catalyst to the carbon monoxide in exhaust gas from diesel vehicle, hydrocarbon and SOF, so should have certain sulfur resistance.
Chinese patent publication No. CN101879445A, date of publication on November 10th, 2010, name is called that a kind of catalytic combustion removes composite rear earth pyrochlore-type oxide catalyst of diesel vehicle soot and preparation method thereof, this application case discloses a kind of catalytic combustion and removes composite rear earth pyrochlore-type oxide catalyst of diesel vehicle soot and preparation method thereof, and composite metal oxide expression formula is A
2b
2-xm
xo
7, wherein A is La, B be Sn, M is Mn, Fe, Co, Ni or Cu.Its weak point is, sulfur resistance is poor.
Summary of the invention
The object of the invention is to the defect of the catalyst resistance to SO_2 difference in order to solve existing removal diesel exhaust and provide a kind of oxidation catalyst for purifying tail gas of diesel vehicles, this oxidation catalyst has good oxidability to carbon monoxide, hydrocarbon and SOF, especially higher catalytic activity can be obtained within the scope of discharged at lower temperature, also there is high-selectivity oxidation ability simultaneously, effectively can suppress the oxidation of sulfur dioxide, there is stronger sulfur resistive ability.
Another object of the present invention is to the preparation method of the oxidation catalyst being also provided for purifying tail gas of diesel vehicles.The diesel vehicle oxidation catalyst initiation temperature produced by the method is low, conversion ratio is high, good endurance, and the method manufacture craft process is simple, and cost of manufacture is low.
To achieve these goals, the present invention is by the following technical solutions:
A kind of oxidation catalyst for purifying tail gas of diesel vehicles, this catalyst is made up of matrix and the catalyst coat be coated on matrix, coating is divided into bottom and upper strata, described catalyst floor coating is made up of perovskite, and upper strata coating is made up of activated alumina, rare earth oxygen storage material, molecular sieve, catalytic active component and catalyst promoter; In the coating of upper strata, the mass percent of each component is: catalyst aid 5-20%, rare earth oxygen storage material 30-60%, activated alumina 20-50%, molecular sieve 10-40% and catalytic active component 0.2-10%, and described perovskite is La
msr
(1-m)co
nni
(1-n)o
3, wherein m=0.6-0.9, n=0.6-0.9.In the technical program, diesel vehicle oxidation catalyst coating adds perovskite, rare earth oxygen storage material, high-specific surface area activated alumina material and molecular screen material, improve activity and the durability of diesel vehicle oxidation catalyst, reduce the use amount of active component, diesel vehicle oxidation catalyst provided by the invention is to carbon monoxide, hydrocarbon and SOF has good oxidability, especially higher catalytic activity can be obtained within the scope of discharged at lower temperature, also there is high-selectivity oxidation ability simultaneously, effectively can suppress the oxidation of sulfur dioxide, there is stronger sulfur resistive ability.
As preferably, described matrix is cordierite ceramic honeycomb carrier or mullite ceramic honeycomb substrate or silicon carbide ceramics honeycomb substrate or FeCrAl base high-temperature metal honeycomb substrate.
As preferably, described activated alumina is CeZr-Al
2o
3, La-Al
2o
3, SiO
2-Al
2o
3in one, or two or more mixture.
As preferably, described rare earth oxygen storage material is selected from by a kind of in La, Pr, Nd, Sr, Bi, Y, or two or more element carries out the Ce of modification
xzr
(1-x)o hydrogen-storing material, X=0.4-0.8; Described molecular sieve is the one in ZSM-5 molecular sieve, Cu-molecular sieve, β-molecular sieve, or two or more mixtures.
As preferably, described catalytic active component is the one in the oxide of Pd, Pt, Rh, or two or more hopcalite; Described catalyst promoter is three kinds in the oxide of Ce, Ba, Zr, La, Mn, Fe, Co, or more than three kinds hopcalites.
As preferably, described catalyst matrix is cordierite ceramic honeycomb carrier, and hole order number is 400 orders.
As preferably, the Ce of described modification
xzr
(1-x)o hydrogen-storing material, X=0.40 ~ 0.80.
As preferably, the catalyst coat of catalyst floor coating 60 ~ 100g/L, the catalyst coat of upper strata coating 60 ~ 100g/L.
For a preparation method for the oxidation catalyst of purifying tail gas of diesel vehicles, preparation method comprises the steps:
1) the choosing of matrix: the specification choosing matrix ceramic honeycomb is 20 × 20 × 30cm;
2) preparation of coating bottom slurries: get perovskite La
xsr
(1-x)co
yni
(1-y)o
3, add deionized water and regulate solid content to 50-60%, stirring ball-milling 10-20min, obtains the slurries that granularity is 5-10 μm, then adds deionized water adjustment solid content to 35-50%;
3) bottom coating: by step 2) gained coating is coated to step 1) on the matrix ceramic honeycomb chosen, obtain the ceramic monolith after bottom coating;
4) bottom dries roasting: step 3) gained metallic carrier toasts 1-3h to bone dry between 60-120 DEG C, then at 350-600 DEG C of roasting 2-5h, obtains catalyst semi-finished product;
5) preparation of coating upper strata slurries: get catalyst promoter, activated alumina, rare earth oxygen storage material, molecular sieve, adding deionized water after mixing regulates solid content to 50-60%, stirring ball-milling 10-20min obtains the slurries that granularity is 5-8 μm, then precious metal solution is added, stir, then add deionized water adjustment solid content to 35-50%;
6) upper strata coating: coating upper strata slurries are coated in step 4) on the catalyst semi-finished product that obtain, obtain the catalyst carrier of upper strata coating;
7) roasting is dried on upper strata: step 6) gained catalyst carrier toasts 1-3h to bone dry between 60-120 DEG C, then at 300-550 DEG C of roasting 2-5h, obtains finished catalyst.
As preferably, the hole density of matrix is 62-65 hole/cm
2.
The present invention compared with prior art, has following beneficial effect:
Catalyst coatings containing noble metal is applied directly on ceramic honeycomb matrix by double-deck coating method by the present invention, simplifies the preparation technology of diesel vehicle oxidation catalyst.
Because diesel vehicle oxidation catalyst coating adds perovskite, rare earth oxygen storage material, high-specific surface area activated alumina material and molecular screen material, improve activity and the durability of diesel vehicle oxidation catalyst, reduce the use amount of active component, diesel vehicle oxidation catalyst provided by the invention has good oxidability to carbon monoxide, hydrocarbon and SOF, especially higher catalytic activity can be obtained within the scope of discharged at lower temperature, also there is high-selectivity oxidation ability simultaneously, effectively can suppress the oxidation of sulfur dioxide, there is stronger sulfur resistive ability.
Because diesel vehicle oxidation catalyst of the present invention has very high heat endurance, wider air-fuel ratio window and stronger sulfur resistive ability, therefore can meet the tail gas clean-up requirement that diesel vehicle produces when different operating mode work.
Detailed description of the invention
For making those skilled in the art know the present invention further, describe the present invention in detail by specific embodiment given below.Except as otherwise noted, the percentage adopted in the present invention is percetage by weight.
Embodiment 1
The matrix optional holes density of diesel vehicle oxidation catalyst is 62 holes/cm
2ceramic honeycomb carrier, specification is Φ 20 × 30/400; Catalyst coat bottom: perovskite accounts for 100% of catalyst coat bottom gross weight.Catalyst coat upper strata: the weight of activated alumina, rare earth oxygen storage material and molecular sieve accounts for 30%, 40% and 20% of catalyst coat upper strata gross weight respectively, and catalyst promoter accounts for 10% of catalyst upper strata total coating weight; Catalyst coat upper strata Pd, Pt content is respectively 20g/ft
3, 20g/ft
3, presoma is nitrate solution; Auxiliary component is the oxide of 4%Ce, 3%Ba and 3%Zr, and presoma is nitrate.
The preparation method of diesel vehicle oxidation catalyst:
1. bottom preparation: add perovskite La
0.9sr
0.1co
0.8ni
0.2o
3, Ce
0.6zr
0.4o and deionized water and stirring ball milling 10 minutes, making granularity about 5 μm of solid contents is the catalyst pulp of 45%, bottom coating is carried out to ceramic honeycomb matrix, coated catalyst matrix is placed in the drying machine of 80 DEG C and dries, time is 90 minutes, until coating bone dry, if do not have drying can extend drying time completely, then by drying, catalyst matrix is placed on temperature is completely roasting 3 hours under the condition of 550 DEG C, has namely obtained catalyst semi-finished product;
2. upper strata preparation: by auxiliary agent and deionized water stirring ball-milling 10 minutes in ball mill, then add CeZr-Al
2o
3, Ce
0.6zr
0.4o, ZSM-5 molecular sieve, add deionized water and regulate solid content to 50 %, stirring ball-milling 10 minutes, adds 20g/ft
3precious metals pd solution stirs, and adds 20g/ft again after leaving standstill 1h
3precious metals pt solution, add deionized water again and regulate solid content to 35%, upper strata coating is carried out to catalyst semi-finished product, coated catalyst matrix is placed in the drying machine of 80 DEG C and dries, time is 90 minutes, until coating bone dry, if do not have drying can extend drying time completely, then by drying, catalyst matrix is placed on temperature is completely roasting 3 hours under the condition of 500 DEG C, has namely obtained finished catalyst.
Embodiment 2
The matrix optional holes density of catalytic conversion agent is 62 holes/cm
2two S type or concentric ring type metal beehive carrier, specification is Φ 20 × 30/400; Catalyst coat bottom: catalyst coat bottom: perovskite accounts for 100% of catalyst coat bottom gross weight.Catalyst coat upper strata: the weight of activated alumina, rare earth oxygen storage material and molecular sieve accounts for 30%, 40% and 20% of catalyst coat upper strata gross weight respectively, and catalyst promoter accounts for 10% of catalyst upper strata total coating weight; Catalyst coat upper strata Pd, Pt content is respectively 15g/ft
3, 25g/ft
3, presoma is nitrate solution; Auxiliary component is the oxide of 4%Ce, 3%Ba and 3%Zr, and presoma is nitrate.The preparation method of diesel vehicle oxidation catalyst is identical with embodiment 1.
Embodiment 3
The matrix optional holes density of catalytic conversion agent is 62 holes/cm
2two S type or concentric ring type metal beehive carrier, specification is Φ 20 × 30/400; Catalyst coat bottom: catalyst coat bottom: perovskite accounts for 100% of catalyst coat bottom gross weight.Catalyst coat upper strata: the weight of activated alumina, rare earth oxygen storage material and molecular sieve accounts for 30%, 40% and 20% of catalyst coat upper strata gross weight respectively, and catalyst promoter accounts for 10% of catalyst upper strata total coating weight; Catalyst coat upper strata Pd, Pt content is respectively 10g/ft
3, 30g/ft
3, presoma is nitrate solution; Auxiliary component is the oxide of 4%Ce, 3%Ba and 3%Zr, and presoma is nitrate.The preparation method of diesel vehicle oxidation catalyst is identical with embodiment 1.
Embodiment 4
The matrix optional holes density of catalytic conversion agent is 62 holes/cm
2two S type or concentric ring type metal beehive carrier, specification is Φ 20 × 30/400; Catalyst coat bottom: catalyst coat bottom: perovskite accounts for 100% of catalyst coat bottom gross weight.Catalyst coat upper strata: the weight of activated alumina, rare earth oxygen storage material and molecular sieve accounts for 30%, 40% and 20% of catalyst coat upper strata gross weight respectively, and catalyst promoter accounts for 10% of catalyst upper strata total coating weight; Catalyst coat upper strata Pd, Pt content is respectively 5g/ft
3, 35g/ft
3, presoma is nitrate solution; Auxiliary component is the oxide of 4%Ce, 3%Ba and 3%Zr, and presoma is nitrate.The preparation method of diesel vehicle oxidation catalyst is identical with embodiment 1.
As follows to the activity rating of catalyst obtained in above-described embodiment:
Waste gas evaluating apparatus carries out the activity rating of catalyst, and evaluating apparatus is fixed-bed flow reactor.Containing CO:1%, C in simulation exhaust gas from diesel vehicle
3h
8: 500ppm, NO:800ppm, CO
2: 7%, O
2: 4%, SO
2: 50ppm, N
2: balance.Unaged experiment condition: air speed 4 × 10
4h
-1, reaction temperature is 400 DEG C.Senile experiment condition: 1050 DEG C of roasting 5h, test air speed 4 × 10
4h
-1, reaction temperature is 400 DEG C.
Test experimental data as shown in Table 1 and Table 2:
Table 1 catalyst light-off temperature test result
| ? | CO T50 | CO T50 | HC T50 | HC T50 | SO 2T50 | SO 2T50 |
| ? | Before aging | After aging | Before aging | After aging | Before aging | After aging |
| Embodiment 1 | 172 | 176 | 253 | 258 | 363 | 380 |
| Embodiment 2 | 165 | 168 | 248 | 252 | 369 | 373 |
| Embodiment 3 | 161 | 163 | 248 | 251 | 356 | 370 |
| Embodiment 4 | 158 | 160 | 245 | 251 | 359 | 361 |
Under table 2 different temperatures, catalyst is to SO
2conversion ratio
| ? | Reaction temperature/DEG C | Reaction temperature/DEG C | Reaction temperature/DEG C | Reaction temperature/DEG C |
| ? | 250 | 300 | 350 | 400 |
| Embodiment 1 | 6.10% | 40.30% | 47.50% | 53.40% |
| Embodiment 2 | 4.70% | 36.40% | 45.40% | 52.80% |
| Embodiment 3 | 2.30% | 25.90% | 46.10% | 52.30% |
| Embodiment 4 | 3.60% | 26.30% | 46.30% | 51.10% |
Table 3 catalyst is to CO and HC oxidation conversion test result
| ? | CO | CO | HC | HC |
| ? | T50 | T90 | T50 | T90 |
| Embodiment 1 | 172 | 208 | 253 | 282 |
| Embodiment 2 | 165 | 200 | 248 | 281 |
| Embodiment 3 | 161 | 198 | 248 | 280 |
| Embodiment 4 | 158 | 197 | 245 | 281 |
Can be found by table 1, table 2, table 3, diesel vehicle oxidation catalyst initiation temperature of the present invention is low, high to the activity of conversion of CO and HC, and catalyst can suppress SO preferably simultaneously
2oxidation, decrease sulfate generate, reduce the discharge of particle, show that catalyst has stronger sulfur resistance.By aging front and back initiation temperature contrast experiment, show that catalyst is high temperature resistant ageing-resistant, there is stronger durability.Diesel vehicle oxidation catalyst manufacture craft of the present invention is simple, and cost of manufacture is low, can effectively meet diesel car tail gas refining requirement, has good application and development prospect.
Claims (10)
1. the oxidation catalyst for purifying tail gas of diesel vehicles, this catalyst is made up of matrix and the catalyst coat be coated on matrix, coating is divided into bottom and upper strata, it is characterized in that, described catalyst floor coating is made up of perovskite, and upper strata coating is made up of activated alumina, rare earth oxygen storage material, molecular sieve, catalytic active component and catalyst promoter; In the coating of upper strata, the mass percent of each component is: catalyst aid 5-20%, rare earth oxygen storage material 30-60%, activated alumina 20-50%, molecular sieve 10-40% and catalytic active component 0.2-10%, and described perovskite is La
msr
(1-m)co
nni
(1-n)o
3, wherein m=0.6-0.9, n=0.6-0.9.
2. a kind of oxidation catalyst for purifying tail gas of diesel vehicles according to claim 1, it is characterized in that, described matrix is cordierite ceramic honeycomb carrier or mullite ceramic honeycomb substrate or silicon carbide ceramics honeycomb substrate or FeCrAl base high-temperature metal honeycomb substrate.
3. a kind of oxidation catalyst for purifying tail gas of diesel vehicles according to claim 1, is characterized in that, described activated alumina is CeZr-Al
2o
3, La-Al
2o
3, SiO
2-Al
2o
3in one, or two or more mixture.
4. a kind of oxidation catalyst for purifying tail gas of diesel vehicles according to claim 1, is characterized in that, described rare earth oxygen storage material is selected from by a kind of in La, Pr, Nd, Sr, Bi, Y, or two or more element carries out the Ce of modification
xzr
(1-x)o hydrogen-storing material, X=0.4-0.8; Described molecular sieve is the one in ZSM-5 molecular sieve, Cu-molecular sieve, β-molecular sieve, or two or more mixtures.
5. a kind of oxidation catalyst for purifying tail gas of diesel vehicles according to claim 1, is characterized in that, described catalytic active component is the one in the oxide of Pd, Pt, Rh, or two or more hopcalite; Described catalyst promoter is three kinds in the oxide of Ce, Ba, Zr, La, Mn, Fe, Co, or more than three kinds hopcalites.
6. a kind of oxidation catalyst for purifying tail gas of diesel vehicles according to claim 1 and 2, is characterized in that, described catalyst matrix is cordierite ceramic honeycomb carrier, and hole order number is 400 orders.
7. a kind of oxidation catalyst for purifying tail gas of diesel vehicles according to claim 1 or 4, is characterized in that, the Ce of described modification
xzr
(1-x)o hydrogen-storing material, X=0.40 ~ 0.80.
8. a kind of oxidation catalyst for purifying tail gas of diesel vehicles according to claim 1, is characterized in that, the catalyst coat of catalyst floor coating 60 ~ 100g/L, the catalyst coat of upper strata coating 60 ~ 100g/L.
9., as claimed in claim 1 for a preparation method for the oxidation catalyst of purifying tail gas of diesel vehicles, it is characterized in that, preparation method comprises the steps:
1) the choosing of matrix: the specification choosing matrix ceramic honeycomb is 20 × 20 × 30cm;
2) preparation of coating bottom slurries: get perovskite La
xsr
(1-x)co
yni
(1-y)o
3, add deionized water and regulate solid content to 50-60%, stirring ball-milling 10-20min, obtains the slurries that granularity is 5-10 μm, then adds deionized water adjustment solid content to 35-50%;
3) bottom coating: by step 2) gained coating is coated to step 1) on the matrix ceramic honeycomb chosen, obtain the ceramic monolith after bottom coating;
4) bottom dries roasting: step 3) gained metallic carrier toasts 1-3h to bone dry between 60-120 DEG C, then at 350-600 DEG C of roasting 2-5h, obtains catalyst semi-finished product;
5) preparation of coating upper strata slurries: get catalyst promoter, activated alumina, rare earth oxygen storage material, molecular sieve, adding deionized water after mixing regulates solid content to 50-60%, stirring ball-milling 10-20min obtains the slurries that granularity is 5-8 μm, then precious metal solution is added, stir, then add deionized water adjustment solid content to 35-50%;
6) upper strata coating: coating upper strata slurries are coated in step 4) on the catalyst semi-finished product that obtain, obtain the catalyst carrier of upper strata coating;
7) roasting is dried on upper strata: step 6) gained catalyst carrier toasts 1-3h to bone dry between 60-120 DEG C, then at 300-550 DEG C of roasting 2-5h, obtains finished catalyst.
10. the preparation method of a kind of oxidation catalyst for purifying tail gas of diesel vehicles according to claim 9, is characterized in that, the hole density of matrix is 62-65 hole/cm
2.
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