CN1220187A - Rare earth-noble metal catalyst for purifying motor vehicle exhaust and its preparing method - Google Patents
Rare earth-noble metal catalyst for purifying motor vehicle exhaust and its preparing method Download PDFInfo
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Abstract
The present invention discloses a catalyst for purifying exhaust of motor vehicle. Said catalyst is characterized by using iolite honeycomb ceramic as carrier, using noble metals of platinum, palladium and rhodium containing rare earth elements as active component coating and possessing rare-earth oxide-alumina composite coating so as to obtain effective exhaust-cleaning performance. Said invented catalyst possesses high rare earth oxide content and lower noble metal content, so that it is low in cost, long in service life, quick in cold starting, and can meet the requirements for people's practical application.
Description
The invention belongs to field of environment protection; relate to rare earth-noble metal catalyst of a kind of purifying exhausted gas of motor vehicle and preparation method thereof, more specifically to carbon monoxide, hydrocarbon and oxynitrides in a kind of purifying exhausted gas of motor vehicle simultaneously, be three-way catalyst of main active and preparation method thereof with rare earth oxide and small amount of precious metals.
Three unique catalytic converter (TWC) is widely used in the world as a kind of means of effective purifying exhausted gas of motor vehicle, but the exploration of the raw catelyst more excellent to performance, that cost is lower is still in the ascendant.Formed two developing direction at present: the one, the base metal three-way catalyst is as disclosed technology such as Chinese patent CN1046102A, CN1074629A and CN1129146A; It two is that transition metal adds small amount of precious metals, as Chinese patent CN1047225A and the disclosed technology of CN1119127A; And U.S.4,965,243 patent disclosures a kind of three-way catalyst of forming with rare earth cerium oxide or lanthana and noble metal.At present topmost in the world automobile catalyst factory also all adopts the prescription of noble metal system.At these is in the catalyst of active component with the noble metal, and the content of noble metal is all than higher, and general bullion content can reach more than every liter 1.0 gram.Because the resource of noble metal is very limited in the world, costs an arm and a leg, therefore, the disclosed technology of above-mentioned patent has been subjected to certain restriction when large-scale application.
The objective of the invention is to disclose a kind of is that carrier, the noble metal platinum to contain rare earth element, palladium, rhodium are the catalyst that active component coating and the purifying exhausted gas of motor vehicle with rare earth oxide-aluminium oxide composite coating are used with the cordierite honeycomb ceramic.Said catalyst has the noble metal of higher rare earth oxide of content and lower content, can not only guarantee the triple effect performance and the service life of catalyst, and cheap, and cold start-up is fast, can overcome the existing existing defective of catalyst, satisfy the needs of people's practical application.
Design of the present invention is such:
In order to reduce the cost of catalyst, improve catalytic performance, increasing kind and the content of rare earth oxide in catalyst is a valid approach.Therefore many rare earth oxides such as praseodymium oxide etc. also are compounds that valence state is variable, and many reactions are all had special catalysis, add praseodymium oxide etc. and also will will play a positive role to the performance of improving catalyst in catalyst.Simultaneously,, have only 1/2～1/3 of cordierite, and change very little with the rising of temperature because the specific heat of cerium oxide is less.Therefore, in the present invention introduces the rare earth oxide of varying number and kind the micropore of honeycomb ceramic carrier and in surface, duct, aluminum oxide coating layer and the active component layer when reducing the noble metal use amount, can not only reduce catalyst production cost effectively, and help reducing the specific heat of catalyst, improve cold starting performance.
The said catalyst of the present invention is that cordierite honeycomb ceramic with Any shape is a carrier, and cell densities is advisable with every square centimeter 15～47 hole;
In the micropore of carrier, have one deck rare earth oxide-aluminium oxide composite coating, on composite coating, have one deck to contain the noble metal active component coating of rare earth oxide again with the surface, duct.The total consumption of rare earth oxide in catalyst is 10～150 grams per liter catalyst, the consumption of aluminium oxide in catalyst is 15～200 grams per liter catalyst, the percentage by weight of rare earth oxide can be greater than aluminium oxide, the consumption of noble metal is 0.01～1.5 grams per liter catalyst, and what preferably use is 0.1～0.5 grams per liter catalyst;
Said composite coating is made up of a rare earth oxide bottom and an aluminium oxide upper strata of having added rare earth oxide, and the composite coating amount is 50～200 grams per liter catalyst.Wherein, the coating amount of rare earth oxide bottom is 10～60 grams per liter catalyst; The coating amount on aluminium oxide upper strata is 15～200 grams per liter catalyst; The weight ratio of composite coating middle rare earth oxide and aluminium oxide is 0.05～2;
Said rare earth oxide is one or more in lanthanide rare earth oxide or the yittrium oxide;
For heat endurance and the oxygen storage capacity that improves catalyst, can also add in the aluminum oxide coating layer contain at least two kinds of elements in lanthanum, cerium, praseodymium, barium, magnesium, the zirconium oxide as additive, the addition of additive is 1～50% of an aluminum oxide coating layer gross weight, and preferred addition is 5～30%;
Said active component layer is made up of in one or more and lanthanide rare earth oxide or the yttrium oxide among precious metals pt, Pd or the Rh one or more, wherein: Pt: Pd: Rh=(0～3): 1: (0～6), active component middle rare earth oxide is (0.05～30) with the ratio of noble metal gross weight: 1, and what preferably use is 0.5～20: 1.Preferred use be in rare earth oxide cerium oxide, lanthana, praseodymium oxide, neodymia, samarium oxide or the yittrium oxide one or more
By above-mentioned disclosed technical scheme as seen, the content of noble metal is lower than the content of noble metal in the present commercial automobile catalyst widely in the said catalyst of the present invention, content of rare earth then improves significantly, and introduce catalyst with three levels, thereby not only cost reduces significantly, and catalytic performance also will improve greatly.
The said catalyst of the present invention also is preparation like this:
1. ceramic honey comb is a carrier after the degassing is handled, and adopts equi-volume impregnating to impregnated in one or more the aqueous solution in nitrate, acetate or the chloride that contains rare-earth elements of lanthanum, cerium or yttrium.The concentration of rare earths salt can be calculated according to the load capacity of required rare earth oxide and the water absorption rate of carrier.Soaked carrier under 80～150 ℃ temperature dry 2～6 hours, roasting is 2～8 hours in 350～700 ℃ air, obtains to have the catalyst carrier of rare earth oxide bottom;
2. with above-mentioned carrier with rare earth oxide bottom, under vacuum, adopt excessive dip coating, dip-coating aluminium oxide slurries, contain in nitrate, acetate, sulfate, chloride or the oxide of rare-earth elements of lanthanum, cerium, praseodymium, neodymium, samarium or yttrium one or more in the said aluminium oxide slurries, can also add in oxychlorination thing, nitrate or the hydroxide of zirconium, barium or magnesium one or more in these slurries, its addition (in oxide) is 2～10 (wt) (slurries).Adopt centrifugal shake-off or compressed air sweeping method remove behind the residue slurries duct in 80～150 ℃ dry 2～12 hours down, roasting is 2～8 hours in 350 ℃～900 ℃ air, acquisition has the catalyst carrier of composite coating;
With contain precious metals pt, Pd and (or) one or more the mixing salt solution dipping in nitrate, acetate, sulfate, chloride or the oxide of Rh and lanthanide series rare-earth elements or yttrium has the carrier of composite coating, drying is 2～10 hours under 80～150 ℃, roasting is 2～8 hours in 350 ℃～700 ℃ air, obtains to have the catalyst crude product of composite coating and active component coating;
With above-mentioned catalyst crude product at H
2Or under other reducing atmosphere, under 100～500 ℃ temperature, activate 1～4 hour, promptly make the said finished catalyst of the present invention.
The following examples will further be illustrated detail of the present invention, but not constitute the restriction to claim of the present invention.
Embodiment 1
With one be of a size of φ 100 * 100, hole count is 47 holes/cm
2Cordierite ceramic honeycomb be carrier, with this carrier place concentration be 705 grams per liters cerous nitrate solution dipping and 80 ℃ dry 2 hours down, then 350 ℃ of following roastings 2 hours, make to form a rare earth oxide bottom that accounts for total catalyst weight 10%;
It is that it is as follows that the weight percent of used slip is formed (in oxide) in 40% the alumina slurry that this carrier with rare earth oxide bottom is immersed a solid content:
Gama-alumina (adding) 75% with boehmite and active oxidation aluminium powder
Lanthana (adding) 8% with lanthanum nitrate
Barium monoxide (adding) 5% with barium nitrate
Magnesia (adding) 2% with magnesium nitrate
Cerium oxide (adding) 10% with cerous nitrate
Remove residue slurries in the duct with compressed air,,, obtain to have the carrier of rare earth-aluminium oxide composite coating then 700 ℃ of following roastings 2 hours in 120 ℃ of dryings 2 hours;
The carrier that will have above-mentioned rare earth-aluminium oxide composite coating immerses in the active component aqueous solution of metal ion 128.3 grams per liters that are made of chloroplatinic acid, palladium bichloride and cerous nitrate, and wherein, the weight ratio of each metal is:
Platinum: palladium: cerium=1: 3: 10
Soaked carrier 80 ℃ dry 2 hours down, 500 ℃ of following roastings 2 hours, then in nitrogen atmosphere in 450 ℃ of reduction 4 hours, can obtain the said catalyst of the present invention.The total load amount of gained catalyst noble metal is 1.0 grams per liters.
Embodiment 2
Adopt the preparation method identical with embodiment 1, but the amount of cerous nitrate increase twice in the activity component impregnation liquid, the total load amount of gained catalyst noble metal is 0.5 grams per liter.
Embodiment 3
Adopt the preparation method identical, but in alumina slurry, add the zirconia (with the zirconium oxychloride adding) of 5% (alumina slurry weight) with embodiment 1.
Embodiment 4
Adopt the preparation method identical with embodiment 1, but the amount of cerous nitrate increases twice in the activity component impregnation liquid, add in addition and the praseodymium nitrate of cerous nitrate identical weight again, the total load amount of gained catalyst noble metal is 0.2 grams per liter.
Comparative Examples 1
Adopt carrier and the preparation method identical with embodiment 1, but coated with rare earth oxide layer bottom no longer.The total load amount of gained catalyst noble metal is 1.0 grams per liters.
The present invention has carried out the test of catalytic performance to the catalyst of the foregoing description and Comparative Examples gained, and method of testing and test result are as described below:
(1) laboratory tests:
From the catalyst of above-mentioned preparation, take out the sample of φ 20 * 20 respectively, in the automobile exhausting of simulation, check and rate used analog gas composed as follows:
Carbon monoxide 2%
Hydrocarbon (C
3H
6) 1000ppm
Nitrogen oxide (NO) 1000ppm
Oxygen 1.4%
Steam 10%
Nitrogen 86.3% appraisal result is as shown in table 1.
| Sample | Fresh | Aging (1050 ℃/10 hours) | ||||||||||
| Initiation temperature, T 50 | 400 ℃ of conversion ratios, % | Initiation temperature, T 50 | 400 ℃ of conversion ratios, % | |||||||||
| ?CO | ?HC | ?NO | ?CO | ?HC | ?NO | ?CO | ?HC | ?NO | ?CO | ?HC | ????NO | |
| Embodiment 1 | ?178 | ?178 | ?180 | ?96 | ?93 | ?93 | ?320 | ?331 | ?334 | ?93 | ?89 | ????80 |
| Embodiment 2 | ?180 | ?182 | ?190 | ?95 | ?94 | ?90 | ?330 | ?345 | ?366 | ?92 | ?86 | ????77 |
| Embodiment 3 | ?180 | ?183 | ?186 | ?95 | ?91 | ?91 | ?289 | ?296 | ?303 | ?92 | ?90 | ????83 |
| Embodiment 4 | ?181 | ?178 | ?190 | ?93 | ?92 | ?94 | ??/ | ??/ | ??/ | ??/ | ??/ | ????/ |
| Comparative Examples 1 | ?206 | ?208 | ?208 | ?92 | ?90 | ?80 | ?324 | ?346 | ?360 | ?91 | ?88 | ????78 |
Table 1
(2) preventing test: prepare 2 catalyst and be assembled into clarifier by embodiment 1 and embodiment 3, be installed on LX type Santana respectively on car, tail gas with PGA-5 (U.S. MPSI company) type divides the instrument tracking and testing, and method of testing is the idling operation method, and appraisal result is shown in table 2 and table 3.
Table 2
Table .3
| Distance travelled (ten thousand kilometers) | Purifying rate (%) | |||||
| Low speed (＜1000 Rpm) | (＞2000 Rpm) at a high speed | |||||
| ????CO | ????HC | ????NOx | ????CO | ????HC | ????NOx | |
| ????0 | ????92 | ????90 | ????89 | ????＞99 | ????97 | ????96 |
| ????2.6 | ????80 | ????82 | ????53 | ????91 | ????89 | ????54 |
| ????3.0 | ????84 | ????88 | ????30 | ????98 | ????91 | ????62 |
| ????4.8 | ????＞99 | ????94 | ????53 | ????85 | ????78 | ????48 |
| ????5.2 | ????＞99 | ????＞99 | ????32 | ????54 | ????93 | ????52 |
| ????6.6 | ????66 | ????61 | ????/ | ????80 | ????63 | ????/ |
| ????7.9 | ????40 | ????54 | ????/ | ????88 | ????58 | ????/ |
| ????8.5 | ????47 | ????41 | ????60 | ????96 | ????58 | ????32 |
| ????10.4 | ????44 | ????40 | ????53 | ????91 | ????46 | ????34 |
| ????11.4 | ????35 | ????33 | ????48 | ????87 | ????72 | ????36 |
| Distance travelled (ten thousand kilometers) | Purifying rate (%) | |||||
| Low speed (＜1000 Rpm) | (＞2000 Rpm) at a high speed | |||||
| ????CO | ????HC | ????NOx | ????CO | ????HC | ????NOx | |
| ????0 | ????88 | ????88 | ????61 | ????99 | ????96 | ????53 |
| ????0.3 | ????82 | ????81 | ????74 | ????98 | ????88 | ????34 |
| ????2.7 | ????85 | ????81 | ????44 | ????88 | ????78 | ????44 |
| ????3.6 | ????78 | ????85 | ????/ | ????81 | ????80 | ????/ |
| ????4.8 | ????84 | ????61 | ????35 | ????82 | ????76 | ????31 |
(3) bench test
Make each 2 catalyst and be assembled into clarifier by embodiment 3, carry out the initiation temperature and the air-fuel ratio characteristic contrast test of catalyst accelerated ageing front and back on Department of Automobile Engineering of Tsing-Hua University engine rig test device, experimental condition is as follows: initiation temperature test: 200～550 ℃ of catalyst inlet temperature
Air-fuel ratio A/F=14.55, air speed SV=40000h
-1Air-fuel ratio characteristic: 520 ℃ of catalyst inlet temperature
Air-fuel ratio A/F=13.8～15.2, air speed SV=40000h
-1Quick aging: 760 ℃ of catalyst inlet temperature, 60 seconds at the uniform velocity, 5 seconds oil-breaks, air speed SV=60000/h
62.5 hours time (being equivalent to drive a vehicle 50,000 kilometers) result of the test is as shown in table 4.
Table 4
| Air-fuel ratio | Purifying rate % | |||||
| Fresh | After aging | |||||
| ????CO | ????HC | ????NOx | ????CO | ????HC | ????NOx | |
| ????13.8 | ????5 | ????15 | ????52 | ????6 | ????14 | ????19 |
| ????14 | ????12 | ????22 | ????60 | ????8 | ????22 | ????28 |
| ????14.2 | ????20 | ????37 | ????74 | ????20 | ????38 | ????43 | ||
| ????14.4 | ????52 | ????62 | ????90 | ????54 | ????62 | ????60 | ||
| ????14.55 | ????84 | ????96 | ????95 | ????88 | ????87 | ????75 | ||
| ????14.6 | ????89 | ????97 | ????61 | ????92 | ????86 | ????60 | ||
| ????14.8 | ????93 | ????96 | ????21 | ????95 | ????85 | ????20 | ||
| ????15.0 | ????94 | ????94 | ????7 | ????94 | ????84 | ????7 | ||
| ????15.2 | ????93 | ????92 | ????8 | ????94 | ????80 | ????9 | ||
| Initiation temperature | ????319 | ????321 | ????321 | ????375 | ????390 | ????406 | ||
| Purifying rate in the time of 550 ℃ | ????95 | ????87 | ????96 | ????95 | ????87 | ????68 | ||
Above result of the test shows, although the said catalyst of the present invention has reduced the consumption of noble metal, but still has good triple effect performance, and its life-span can be satisfied the instructions for use more than 50,000 kilometers fully.
Claims (7)
1. the rare earth-noble metal catalyst of a purifying exhausted gas of motor vehicle, be carrier with the cordierite honeycomb ceramic, be active component with noble metal platinum, palladium, rhodium, it is characterized in that: in the micropore of carrier and on the surface in duct, have one deck rare earth oxide-aluminium oxide composite coating, on composite coating, there is one deck to contain the noble metal active component coating of rare earth oxide again, wherein:
Said composite coating is made up of a rare earth oxide bottom and an aluminium oxide upper strata of having added rare earth oxide;
Said rare earth oxide is one or more in lanthanide rare earth oxide or the yittrium oxide.
2. catalyst as claimed in claim 1, it is characterized in that: the total consumption of rare earth oxide in catalyst is (10～150) grams per liter catalyst, the consumption of aluminium oxide in catalyst is (15～200) grams per liter catalyst, the percentage by weight of rare earth oxide can be greater than aluminium oxide, and the consumption of noble metal is (0.01～1.5) grams per liter catalyst.
3. as the described catalyst of claim 1-2, it is characterized in that: the composite coating amount is 50～200 grams per liter catalyst, and wherein, the coating amount of rare earth oxide bottom is 10～60 grams per liter catalyst; The coating amount on aluminium oxide upper strata is 15～200 grams per liter catalyst; The weight ratio of composite coating middle rare earth oxide and aluminium oxide is 0.05～2, and active component layer middle rare earth oxide is (0.05～30) with the ratio of noble metal gross weight: 1.
4. catalyst as claimed in claim 1, it is characterized in that: can add in the aluminum oxide coating layer contain at least two kinds of elements in lanthanum, cerium, praseodymium, barium, magnesium, the zirconium oxide as additive, the addition of additive is 1～50% of an aluminum oxide coating layer gross weight;
5. catalyst as claimed in claim 1 is characterized in that:
(1) in the active component layer the preferred rare earth that adds be cerium oxide, lanthana, praseodymium oxide, neodymia,
In samarium oxide or the yittrium oxide one or more;
(2) consumption of the preferred noble metal that uses is (0.1～0.5) grams per liter catalyst;
(3) the preferred active component middle rare earth oxide that uses is (5～20) with the ratio of noble metal gross weight:
1；
(4) the preferred addition of the auxiliary agent that adds in the aluminum oxide coating layer is 5～30%;
(5) the preferred rare earth that adopts is a cerium oxide in the rare earth oxide bottom;
(6) in the aluminum oxide coating layer the preferred rare earth that adopts be a kind of in cerium oxide, lanthana and the praseodymium oxide or
More than one.
6. Preparation of catalysts method as claimed in claim 1 is characterized in that in turn including the following steps:
1. honeycomb ceramic carrier impregnated in nitrate, the acetic acid of rare-earth elements of lanthanum, cerium or yttrium after the degassing is handled
In the aqueous solution of one or more in salt or the chloride, soaked carrier is 80～150
℃ temperature under dry 2～6 hours, roasting is 2～8 hours in 350～700 ℃ air,
Acquisition has the catalyst carrier of rare earth oxide bottom;
2. with above-mentioned carrier with rare earth oxide bottom, under vacuum with rare-earth elements of lanthanum, cerium, praseodymium, neodymium,
In the nitrate of samarium or yttrium, acetate, sulfate, chloride or the oxide a kind of or a kind of with
Go up the mixed serum dip-coating with aluminium oxide, the method that the catalyst carrier usefulness after the dip-coating is known is removed the hole
Descended dry 2～12 hours at 80～150 ℃ behind the residue slurries in the road, 350 ℃～900
℃ air in roasting 2～8 hours, obtain to have the catalyst carrier of composite coating;
With contain precious metals pt, Pd and (or) Rh and rare-earth element cerium, lanthanum, praseodymium, neodymium, samarium or iridium
The mixing of one or more in nitrate, acetate, sulfate, chloride or the oxide
Salt solution impregnation has the carrier of composite coating, and drying is 2～10 hours under 80～150 ℃,
Roasting is 2～8 hours in 350 ℃～700 ℃ air, obtains the catalyst crude product;
With the catalyst crude product under H2 or reproducibility automobile exhaust atmosphere, under 100～500 ℃ temperature
Activate 1～4 hour, promptly make the said finished catalyst of the present invention.
7. preparation method as claimed in claim 6, it is characterized in that adding in the aluminium oxide mixed serum in oxychlorination thing, nitrate or the hydroxide of zirconium, barium or magnesium one or more, its addition (in oxide) is 2～10% (wt) (slurries).
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|---|---|---|---|
| CN98122041A CN1101727C (en) | 1998-11-27 | 1998-11-27 | Rare earth-noble metal catalyst for purifying motor vehicle exhaust and its preparing method |
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| CN98122041A CN1101727C (en) | 1998-11-27 | 1998-11-27 | Rare earth-noble metal catalyst for purifying motor vehicle exhaust and its preparing method |
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| CN1101727C CN1101727C (en) | 2003-02-19 |
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| CN103191735A (en) * | 2013-03-29 | 2013-07-10 | 无锡威孚环保催化剂有限公司 | Preparation method of lean-burn type natural gas vehicle catalyst |
| CN103191735B (en) * | 2013-03-29 | 2015-05-20 | 无锡威孚环保催化剂有限公司 | Preparation method of lean-burn type natural gas vehicle catalyst |
| CN104556032A (en) * | 2013-10-16 | 2015-04-29 | 海尔集团公司 | CO purifier and gas heater with same |
| CN104556032B (en) * | 2013-10-16 | 2018-11-23 | 海尔集团公司 | CO clarifier and gas heater equipped with the CO clarifier |
| CN104307517A (en) * | 2014-09-11 | 2015-01-28 | 北京振金鑫达环保科技有限公司 | Ternary catalyst |
| CN106110886A (en) * | 2016-08-25 | 2016-11-16 | 深圳沃海森科技有限公司 | Idle call rare earth filter |
| CN108554425A (en) * | 2017-12-29 | 2018-09-21 | 佛山科学技术学院 | A kind of exhaust gas purifying catalyst |
| CN109675557A (en) * | 2019-01-09 | 2019-04-26 | 无锡威孚环保催化剂有限公司 | Noble metal catalyst and preparation method thereof with high thermal stability |
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