CN1799689A - Close coupled catalyst - Google Patents

Close coupled catalyst Download PDF

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Publication number
CN1799689A
CN1799689A CN 200610020144 CN200610020144A CN1799689A CN 1799689 A CN1799689 A CN 1799689A CN 200610020144 CN200610020144 CN 200610020144 CN 200610020144 A CN200610020144 A CN 200610020144A CN 1799689 A CN1799689 A CN 1799689A
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catalyst
matrix
stable
carrier
designated
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CN1799689B (en
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史忠华
陈耀强
龚茂初
赵明
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Sichuan University
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Sichuan University
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Abstract

The invention relates to a close-coupled catalyst with high activity and thermal stability to purify the tail gas of cold start of motor. Said close-coupled catalyst comprises at least three kinds of alumina in different physical phased as catalyst carrier; the Pd as active component; at least one of rare-earth oxides as Y2O3, La2O3, Nd2O3 and Sm2O3; at least one of alkaline earth oxides as SrO, BaO and CaO; and ZrO2.

Description

Close coupled catalyst
One, technical field
The present invention relates to a kind of close coupled catalyst that is used for reducing effectively HC pollutant emission during the engine cold-start and preparation method thereof.
Two, background technology
In recent years, be used for the harmful substance HC of purifying automobile tail gas, the catalyst research of CO and NOx is very active.Along with the increasingly stringent of environmental emission rules, the HC discharging during the solution engine cold-start is very important.
Cold start-up is the brief moment that mean engine starts from environment temperature.The cold start-up process depends on the working method of environment temperature, engine type, engine control system and engine.Typical Cold Start is first two minutes after engine starts from environment temperature, and the FTP-75 method of testing thinks that then cold start-up is within after engine starts from environment temperature 505 seconds.The FTP-75 method of testing is the main test method of the clean-up effect of the present evaluation exhaust gas purifying catalyst that worldwide uses.In the three phases of FTP-75 test, 2/3rds of the HC that first HC that produces during 100 seconds discharging accounts in the generation of FTP-75 duration of test after the particularly cold start-up in cold start-up stage.Because the temperature from the tail gas of engine emission during the cold start-up is low, do not reach the initiation temperature of three-way catalyst, cause a large amount of HC directly to discharge.Usually use close coupled catalyst, usually be also referred to as " upstream catalyst " or " preheating catalyst ", reduce the HC discharge capacity during the cold start-up.Consider the following performance of close coupled catalyst from reducing the HC discharge capacity during the cold start-up and the long-time stability of catalyst effectively: (1) low temperature active, weigh with the initiation temperature of catalyst.Initiation temperature is that a certain specific components (as HC) transforms 50% temperature.Usually require 40 seconds or shorter time inner catalyst ignition after cold start-up; Corresponding, catalyst should reach 50% HC 250 ℃ or lower temperature and transform.Mainly realize by improving activity of such catalysts.(2) high-temperature stability, close coupled catalyst is the part of whole cleaning catalyst for tail gases of automobiles, it is than traditional " chassis catalyst " more close engine, this makes it can reach reaction temperature as early as possible, yet, after the engine steady operation, because close coupled catalyst has only one foot or six inches or directly touch the tail gas manifold apart from engine, so can directly be exposed to (sometimes above 1100 ℃) in the high-temperature tail gas.So close coupled catalyst not only will have lower initiation temperature, also must keep stable in the high temperature behind the engine steady operation, this can solve by the high-temperature stability that improves catalyst coat.(3) restriction of CO transforms, and the strong heat release of CO oxidation causes the sintering of catalyst, reduces the life-span of close coupled catalyst.Therefore, should be implemented in the restriction conversion of the CO on the close coupled catalyst by Preparation of catalysts.The three-way catalyst that a large amount of CO is offered the downstream makes it reach higher temperature as early as possible, to improve its efficient.
For reaching above-mentioned desired performance, Pd is owing to have the active component that excellent low temperature ignition performance is used as close coupled catalyst, Pt, Rh etc. also sometimes with Pd together as active component to improve the performance of catalyst.Cordierite honeycomb carrier or metal beehive carrier are as matrix, and heat-resistant inorganic oxide is (such as Al 2O 3) as the carrier of dispersed activity component, with the coating that consists of catalyst as the rare earth of auxiliary agent and stabilizing agent and alkaline-earth oxide etc.
In US6254842, with γ-Al 2O 3(160m 2/ g) load P d (100g/ft 3), add La, Zr, Sr and Nd make auxiliary agent, have prepared close coupled catalyst take cordierite honeycomb bodies as matrix.Through 950 ℃ of 12 hours (10%H in air 2O) after aging, to HC, CO and NO xInitiation temperature be respectively 252 ℃, 228 ℃ and 213 ℃.
In US6602822, with γ-Al 2O 3Load P d has prepared the close coupled catalyst of different Pd load capacity and different coating thickness.Find that suitably reducing coating layer thickness can reduce initiation temperature.
In US5878567, advocate Pd or three metals (Pd, Pt and Rh) (100-300g/ft with high capacity 3) and add La, Ba, Zr, the auxiliary agents such as Ce prepare close coupled catalyst.
In CN1197686A, introduced a kind of pair of coating cooled activated catalyst.Ground floor comprises La-Al 2O 3The Pd of load, cerium/Zr mixed oxide, zirconia and zeolite ZSM-5.The second layer comprises La-Al 2O 3The Rh of load, the Y zeolite of cerium/Zr mixed oxide and dealuminzation.Adding zeolite is not adsorb HC before reaching initiation temperature at catalyst, makes it that desorption is transformed by catalyst after catalyst reaches initiation temperature.But up to the present, also there is not a kind of zeolite can bear the high temperature of tail gas behind the engine start, stability existing problems.
Because close coupled catalyst will be exposed to up in the tail gas more than 1000 ℃, the carrier as close coupled catalyst is γ-Al at present 2O 3Or La-Al 2O 3, all existing at high temperature particularly (has the H about 10% in the tail gas under the high temperature that steam exists 2O) volume contraction that phase transformation causes causes the loss of the specific area of catalyst, the sintering of active component and the decline of catalytic activity.In this respect, La-Al 2O 3Than γ-Al 2O 3Better, but problem still exists.Therefore, the high-temperature stability of improving catalyst carrier and catalyst coat needs.
Three, summary of the invention
The invention provides close coupled catalyst of a kind of high stable and preparation method thereof.Unlike the prior art be that the present invention adopts single γ-Al 2O 3Or the stable Al of La 2O 3As carrier, but adopt the Al of multiple different phases 2O 3As carrier.Its reason is the Al of same phase 2O 3Particle between have identical phase interface, when high temperature ageing, sintering takes place in identical phase interface easily.Cause the decline of specific area.And the Al of different phases 2O 3Particle between have not identical phase interface, different phase interfaces has better anti-caking power.The present invention is the Al that utilizes different phases 2O 3Between exist the anti-caking power of the excellence that different phase interfaces provides to improve the stability of catalyst carrier and catalyst coat.According to thinking of the present invention, can be used as the Al of the different phases of close coupled catalyst of the present invention 2O 3Carrier material is: γ-Al 2O 3, θ-Al 2O 3, δ-Al 2O 3, γ-Al that La is stable 2O 3(be designated as La-γ-Al 2O 3), θ-Al that La is stable 2O 3(be designated as La-θ-Al 2O 3), δ-Al that La is stable 2O 3(be designated as La-δ-Al 2O 3), Y, γ-Al that Zr is stable 2O 3(be designated as YSZ-γ-Al 2O 3) etc.At above-mentioned Al 2O 3In the aluminium oxide of existing different phases, the aluminium oxide that belongs to same phase is also arranged, such as γ-Al 2O 3, La-γ-Al 2O 3With YSZ-γ-Al 2O 3Belong to same phase, but γ-Al 2O 3No auxiliary agent, La-γ-Al 2O 3With YSZ-γ-Al 2O 3Institute's adding assistant difference, their grain size and pattern are different.Mix when using and have better anti-caking power than any independent use.In order to reach effect of the present invention, at the Al that uses different phases 2O 3When making carrier, in above-mentioned material, at least three kinds are used simultaneously, and every kind of Al 2O 3The highest 50% of the total use amount that is no more than of use amount, minimum use amount is not less than 10% of total use amount.In principle at the Al of above-mentioned different phases 2O 3But any combination in the carrier material all can produce good effect.The Al of the different phases that the present invention uses 2O 3Performance as described below:
γ-Al 2O 3: pure γ-Al 2O 3, BET surface area: 180m 2/ g.
δ-Al 2O 3: pure δ-Al 2O 3, BET surface area: 120m 2/ g.
θ-Al 2O 3: pure θ-Al 2O 3, BET surface area: 80m 2/ g.
La-γ-Al 2O 3: γ-Al 2O 3, with 2-4% (weight) lanthanum stabilisation (by lanthana), BET surface area: 140m 2/ g.
La-θ-Al 2O 3: θ-Al 2O 3, with 2-4% (weight) lanthanum stabilisation (by lanthana), BET surface area: 75m 2/ g.
La-δ-Al 2O 3: δ-Al 2O 3, with 2-4% (weight) lanthanum stabilisation (by lanthana), BET surface area: 115m 2/ g.
YSZ-γ-Al 2O 3: γ-Al 2O 3, with the zirconium stabilisation (all by oxide) of yttrium and the 4-5% (weight) of 2-3% (weight),
BET surface area: 110m 2/ g.
Close coupled catalyst provided by the invention is with the Al of above-mentioned different phases 2O 3Be carrier, the Al of different phases 2O 3Vector contg is 70～90% (weight).Pd is an active component, and its content is 1～5% (weight).Co-catalyst is rare earth oxide and alkaline-earth oxide, rare earth oxide is at least a in the oxide of rare earth element y, La, Nd and Sm, and content is 2～15% (weight), and alkaline-earth oxide is at least a in the oxide of Ca, Sr, Ba, content is 3～15% (weight), ZrO 2Content is 2-5% (weight).The matrix of selecting for use is cordierite honeycomb ceramic matrix or metal beehive matrix, and hole density is more than 400cpsi (cells per square inch) reaches.The sample matrix is formed by the bulk substrate cutting, and makes the nearly cylinder of φ 12 * 25.
Close coupled catalyst provided by the invention prepares by following method:
1, active component Pd is carried on the Al of different phases 2O 3For on the carrier and carry out immobilization and process;
2, load there is the precursor of the carrier of active component and auxiliary agent grind in the lump and makes the coating liquid that solid weight content is 25-51%;
3, matrix is dipped in the coating liquid;
4, matrix takes out from coating solution with compressed air and blows down unnecessary coating solution in the matrix hole;
5, the matrix that will apply coating liquid carries out roasting after drying, and catalyst coat is solidificated on the matrix, promptly makes close coupled catalyst of the present invention.
In above-mentioned preparation method, load has the carrier of active component to be preferably under 100-150 ℃ the environmental condition dry 4-8 hour, again under 400-500 ℃ of condition roasting 2-4 hour afterwards.The matrix that scribbles coating liquid is preferably under 100-150 ℃ the environmental condition dry 3-5 hour, again under 400-550 ℃ of condition roasting 3-5 hour afterwards.
The inventor tests the performance of close coupled catalyst provided by the invention, and close coupled catalyst is behind 1050 ℃ of hydrothermal agings, and catalyst below 250 ℃, shows excellent ageing resistace to the initiation temperature of HC.
The present invention compared with prior art, maximum contribution is the Al of different phases 2O 3Greatly improved the ageing resistace of catalyst for carrier.Can satisfy better the emission request during the cold start-up.
Specification implementation part is described having in of the present invention more specifically, can understand other characteristics of the present invention, details and advantage by this part of reading specification more full and accurately.
Four, the specific embodiment
Embodiment 1
Get the Al of the different phases of 112 grams 2O 3Powders A l 2 3Gram, wherein γ-Al 2O 3, La-γ-Al 2O 3, δ-Al 2O 3With La-θ-Al 2O 3Respectively account for 25% (weight).With the palladium nitrate solution dipping that contains Pd2.24 gram, 120 ℃ of dryings 4 hours, 550 ℃ of roasting 3h obtain containing the Pd aluminium oxide.To contain Pd aluminium oxide and strontium nitrate (containing the SrO5 gram), lanthanum nitrate (contains La 2O 37 grams), zirconium nitrate (contains ZrO 27 gram) Xiao Suan Nd (contain Nd 2O 34 the gram) and an amount of water polo wear into the coating solution that solid content is 40% (weight).The cordierite matrix of getting 400cpsi immerses coating liquid, and take out the back and blows down unnecessary coating liquid with compressed air, 120 ℃ of dryings 3 hours, 500 ℃ of roasting 4h obtain catalyst C1.Pd content is 2.24 grams per liters, 112 grams per liter Al 2O 3, 5 grams per liter SrO, 7 grams per liter La 2O 3, 8 grams per liter ZrO 2, 4 grams per liter Nd 2O 3
Embodiment 2
The preparation method is with embodiment 1, the Al that different is in different phases 2O 3In, θ-Al 2O 3, La-γ-Al 2O 3, YSZ-γ-Al 2O 3La-δ-Al 2O 3Respectively account for 25%.Obtain catalyst C2
Embodiment 3
The preparation method is with embodiment 1, the Al that different is in different phases 2O 3In, La-δ-Al 2O 3Account for 15%, YSZ-γ-Al 2O 3Account for 20%, La-γ-Al 2O 3Account for 45%, γ-Al 2O 3Account for 20%.Obtain catalyst C3
Embodiment 4
The preparation method is with embodiment 1, the Al that different is in different phases 2O 3In, γ-Al 2O 3Account for 30%, La-γ-Al 2O 3Account for 40%, La-θ-Al 2O 3Account for 30%.Obtain catalyst C4
Embodiment 5
The preparation method is with embodiment 1, the Al that different is in different phases 2O 3In, θ-Al 2O 3Account for 10%, La-γ-Al 2O 3Account for 10%, YSZ-γ-Al 2O 3Account for 15%, La-δ-Al 2O 3Account for 15%, γ-Al 2O 3Account for 10%, δ-Al 2O 3Account for 15% and La-θ-Al 2O 3Account for 25%.Obtain catalyst C5
Embodiment 6
The preparation method is with embodiment 1, and different is that lanthanum nitrate is changed to yttrium nitrate, and strontium nitrate is changed to barium nitrate; Pd content is 3.5 grams per liters.Obtain catalyst C6
Embodiment 7
The preparation method is with embodiment 1, and different is that lanthanum nitrate is changed to samaric nitrate, and strontium nitrate is changed to calcium nitrate; Pd content is 2.8 grams per liters.Obtain catalyst C7
Comparing embodiment 1
The preparation method is with embodiment 1, and different is only with γ-Al 2O 3Be carrier.Obtain catalyst C8
Comparing embodiment 2
The preparation method is with embodiment 1, and different is only with La-γ-Al 2O 3Be carrier.Obtain catalyst C9
Comparing embodiment 3
The preparation method is with embodiment 1, and different is only with La-θ-Al 2O 3Be carrier.Obtain catalyst C10.
Comparing embodiment 4
The preparation method is with embodiment 1, and different is only with θ-Al 2O 3Be carrier.Obtain catalyst C11.
Comparing embodiment 5
The preparation method is with embodiment 1, and different is only with δ-Al 2O 3Be carrier.Obtain catalyst C12.
Comparing embodiment 6
The preparation method is with embodiment 1, and different is only with La-δ-Al 2O 3Be carrier.Obtain catalyst C13.
Comparing embodiment 7
The preparation method is with embodiment 1, and different is only with YSZ-γ-Al 2O 3Be carrier.Obtain catalyst C14.
Catalyst ageing
The fresh catalyst that makes is placed tube furnace, and feeding contains 10%H 2The O air is in 1050 ℃ of aging 10h.
Test
Carry out the activity rating of catalyst at the cleaning catalyst for tail gases of automobiles simulating-estimating device, evaluating apparatus is fixed-bed flow reactor.Contain HC 550ppm (C in the simulated automotive tail gas 3H 8And C 3H 6Each half), 0.6% CO, the NOx of 600ppm and 10%H 2O, surplus N 2The air speed of reaction is controlled at 5.0 * 10 4h -1In course of reaction, the content of oxygen can change.
Gas before and after the reaction carries out quantitative analysis with the FGA4100 type five component exhaust analyzers that Foshan Buddhist branch environmental protection tests equipment Co., Ltd produces.
Because the purpose of close coupled catalyst is the HC discharging when being used to handle the gasoline car cold start-up, all mainly measure the initiation temperature (T of aging rear catalyst HC 50%).
During mensuration, earlier catalyst is activated 2h under 550 ℃ of tail gas states.Measurement result is as shown in table 1.
Initiation temperature (the T of HC after table 1 is aging 50%)
Catalyst Aged samples
C1 245
C2 240
C3 248
C4 240
C5 246
C6 235
C7 241
C8 278
C9 260
C10 288
C12 298
C13 300
C14 276
Can obviously find out from the result of table 1, use the Al of different phases 2O 3For the initiation temperature of HC after the catalyst ageing of carrier is starkly lower than single Al 2O 3Catalyst for carrier.Can be fine satisfy the HC low temperature ignition requirement during the cold start-up.

Claims (5)

1, a kind of stable close coupled catalyst comprises the Al by different phases 2O 3Carrier: γ-Al 2O 3, θ-Al 2O 3, δ-Al 2O 3, γ-Al that La is stable 2O 3(be designated as La-γ-Al 2O 3), θ-Al that La is stable 2O 3(be designated as La-θ-Al 2O 3), δ-Al that La is stable 2O 3(be designated as La-δ-Al 2O 3), Y, γ-Al that Zr is stable 2O 3(be designated as YSZ-γ-Al 2O 3) at least three kinds, auxiliary agent comprises, rare earth oxide, Y 2O 3, La 2O 3, Nd 2O 3And Sm 2O 3In at least a, alkaline-earth oxide, SrO, at least a and ZrO among BaO and the CaO 2, and the precious metals pd active component forms.
2, close coupled catalyst according to claim 1 is characterized in that the Al of said different phases 2O 3Carrier is γ-Al 2O 3, θ-Al 2O 3, δ-Al 2O 3, γ-Al that La is stable 2O 3(be designated as La-γ-Al 2O 3), θ-Al that La is stable 2O 3(be designated as La-θ-Al 2O 3), δ-Al that La is stable 2O 3(be designated as La-δ-Al 2O 3), Y, γ-Al that Zr is stable 2O 3(be designated as YSZ-γ-Al 2O 3) at least three kinds; The content of alumina support in catalyst of different phases is 70-90% (weight).Rare earth oxide is a rare earth element y, La, and at least a in the oxide of Nd and Sm, the content in catalyst is 2-15% (weight).The alkaline-earth oxide carrier can be Sr, at least a in the oxide of Ba and Ca, and the content in catalyst is 3-12% (weight).ZrO in catalyst 2Content be 2-7% (weight).
3, close coupled catalyst according to claim 1 is characterized in that the Al of said different phases 2O 3Any Al in the carrier 2O 3The highest Al that is no more than of use amount 2O 3Total use amount 50%, minimum use amount is not less than 10% of total use amount.
4, close coupled catalyst according to claim 1 is characterized in that close coupled catalyst is carried on the matrix, and matrix is cordierite honeycomb ceramic matrix or metal beehive matrix, and hole density is more than 400cpsi reaches.
5, according to the preparation method of the described close coupled catalyst of each claim in the claim 1 to 4, it is characterized in that comprising following processing step:
(1) active component Pd is carried on the Al of different phases 2O 3For on the carrier and carry out immobilization and process;
(2) load there is the precursor of the carrier of active component and auxiliary agent grind in the lump and makes the coating liquid that solid weight content is 25-51%;
(3) matrix is dipped in the coating liquid;
(4) matrix takes out from coating solution with compressed air and blows down unnecessary coating solution in the matrix hole;
(5) matrix that will apply coating liquid carries out roasting after drying, and catalyst coat is solidificated on the matrix.
CN200610020144.9A 2006-01-13 2006-01-13 Close coupled catalyst Expired - Fee Related CN1799689B (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
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CN102133536A (en) * 2011-03-07 2011-07-27 兰嘉铭 Front multi-element catalyst and preparation method thereof
CN101249439B (en) * 2008-03-28 2012-09-26 无锡威孚环保催化剂有限公司 Catalyst assembly for processing organic halogenated alkane industrial waste gas and method of preparing the same
CN102740953A (en) * 2009-12-21 2012-10-17 约翰逊马西有限公司 NOx trap
CN104016841A (en) * 2013-03-01 2014-09-03 赢创工业集团股份有限公司 Process for preparing ketones from epoxides
WO2018213183A1 (en) * 2017-05-15 2018-11-22 Sabic Global Technologies, B.V. Mixed oxides catalysts for oxidative coupling of methane
WO2019082905A1 (en) * 2017-10-24 2019-05-02 Sumitomo Chemical Company, Limited Alumina material
CN110170141A (en) * 2019-06-26 2019-08-27 厦门一泰消防科技开发有限公司 A kind of multifunctional fire extinguishing agent and preparation method thereof
CN110560056A (en) * 2019-08-30 2019-12-13 无锡威孚环保催化剂有限公司 Universal small gasoline engine tail gas catalyst and preparation method thereof

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CN1052170C (en) * 1994-09-24 2000-05-10 华夏海南开发建设经营公司 Purifying catalyst for gas exhausted from internal combustion engine
US6044644A (en) * 1994-12-06 2000-04-04 Engelhard Corporation Close coupled catalyst
US5878567A (en) * 1996-01-22 1999-03-09 Ford Global Technologies, Inc. Closely coupled exhaust catalyst system and engine strategy associated therewith
US6087298A (en) * 1996-05-14 2000-07-11 Engelhard Corporation Exhaust gas treatment system
CN1047540C (en) * 1997-10-31 1999-12-22 北京绿创环保科技有限责任公司 Ternary composite metal oxide catalyst for treating automobile's waste gas, and method for preparing same
KR100527943B1 (en) * 2003-06-04 2005-11-09 현대자동차주식회사 Method for manufacturing double layer coated Pd only three way catalyst

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CN101249439B (en) * 2008-03-28 2012-09-26 无锡威孚环保催化剂有限公司 Catalyst assembly for processing organic halogenated alkane industrial waste gas and method of preparing the same
CN102740953B (en) * 2009-12-21 2015-11-25 约翰逊马西有限公司 NO xtrap
CN102740953A (en) * 2009-12-21 2012-10-17 约翰逊马西有限公司 NOx trap
CN102133536B (en) * 2011-03-07 2012-11-14 兰嘉铭 Front multi-element catalyst and preparation method thereof
CN102133536A (en) * 2011-03-07 2011-07-27 兰嘉铭 Front multi-element catalyst and preparation method thereof
CN104016841B (en) * 2013-03-01 2017-10-24 赢创德固赛有限公司 The method that ketone is prepared by epoxides
CN104016841A (en) * 2013-03-01 2014-09-03 赢创工业集团股份有限公司 Process for preparing ketones from epoxides
WO2018213183A1 (en) * 2017-05-15 2018-11-22 Sabic Global Technologies, B.V. Mixed oxides catalysts for oxidative coupling of methane
WO2019082905A1 (en) * 2017-10-24 2019-05-02 Sumitomo Chemical Company, Limited Alumina material
US11578000B2 (en) 2017-10-24 2023-02-14 Sumitomo Chemical Company, Limited Alumina material
CN110170141A (en) * 2019-06-26 2019-08-27 厦门一泰消防科技开发有限公司 A kind of multifunctional fire extinguishing agent and preparation method thereof
CN110560056A (en) * 2019-08-30 2019-12-13 无锡威孚环保催化剂有限公司 Universal small gasoline engine tail gas catalyst and preparation method thereof
CN110560056B (en) * 2019-08-30 2022-11-01 无锡威孚环保催化剂有限公司 Universal small gasoline engine tail gas catalyst and preparation method thereof

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