CN108435170A - A kind of oxidation catalyst and preparation method thereof of low temperature CO ignitions - Google Patents
A kind of oxidation catalyst and preparation method thereof of low temperature CO ignitions Download PDFInfo
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Abstract
The present invention relates to a kind of oxidation catalysts of low temperature CO ignitions, including carrier, coating is coated on carrier, the coated weight of coating is 80 ~ 180 grams per liters, load has precious metals pt and precious metals pd in coating, the load capacity of noble metal is 0.5 ~ 5.0 grams per liter, and wherein the mass ratio of precious metals pt and precious metals pd is 10 ~ 0.5：1, coating includes cerium-aluminium composite oxide, molecular sieve and auxiliary agent bismuth oxide.Preparation method of the present invention is simple, and step is easily operated, is particularly suitable for industrialization large-scale production, and the catalyst being prepared has low temperature CO light-off performances outstanding, high conversion rate, and thermal stability is good, and has good NO oxidabilities.
Description
Technical field
The present invention relates to a kind of oxidation catalysts and preparation method thereof of low temperature CO ignitions, belong to catalyst preparation technology
Field.
Background technology
In recent years, more serious by the atmosphere polluting problem caused by automotive emission.Investigation shows with China
The fast development of heating equipment increasingly improved with automotive industry, the type of China's atmosphere pollution turn from coal-smoke pollution
It is polluted to coal smoke and motor-vehicle tail-gas mixed type, and in most large size cities, tail gas pollution of motor-driven vehicle has become sky
The major source of gas pollution.Gasoline car is compared, diesel vehicle more has advantage in terms of fuel economy and carbon emission.With energy
Source problem increasingly becomes the key problem for restricting socio-economic development, the power high as a kind of efficiency, environment affinity is strong
Means, diesel vehicle get growing concern for and develop.Mainly there are carbon monoxide (CO), carbon in the pollutant of emission of diesel engine
Hydrogen compound (HC), oxynitrides (NOX) and particulate matter (PM), particulate matter mainly have dry carbon cigarette (soot), solubility to have
Machine object (SOF) and a small amount of sulfuric acid and sulfate composition.
HC (including various chain hydrocarbons and aromatic hydrocarbon) and CO in exhaust gas from diesel vehicle are since fuel oil imperfect combustion generates
, and each contaminant component content is varied from tail gas under different operating modes.Tail gas under the generally conventional combustion system of diesel engine
Middle HC and CO concentration is relatively low, but in novel combustion system, such as pre-mixing pression ingiter, can reduce the production of NOX and PM simultaneously
It gives birth to, will produce a considerable amount of HC and CO.
Diesel oxidation catalyst (DOC) is as the diesel engine vent gas post-processing technology being applied earliest, mainly
For eliminating the SOF in HC, CO and PM in tail gas.With the further upgrading of state motor vehicle tail-gas law, especially
It is HC, CO gas phase pollution processing capacity of light-duty diesel vehicle DOC, faces a severe challenge.DOC products currently on the market are generally deposited
It is bad in the low temperature light-off performance of low temperature ignition, especially CO, the problems such as initiation temperature T50 higher, and the row of light-duty diesel vehicle
Temperature degree is generally relatively low, therefore the low temperature ignition ability for promoting DOC is the hot spot of current this field research.
Invention content
The purpose of the present invention is to solve the above problem, provide a kind of oxidation catalyst for low temperature CO ignitions and
Preparation method, the catalyst low temperature CO light-off performances protrusion of preparation, high conversion rate, good thermal stability also have good
NO oxidabilities.
The present invention adopts the following technical scheme that：A kind of oxidation catalyst of low temperature CO ignitions, including carrier, the carrier
Upper to be coated with coating, the coated weight of the coating is 80~180 grams per liters, and being loaded in the coating has precious metals pt and noble metal
The load capacity of Pd, the precious metals pt and precious metals pd is 0.5~5.0 grams per liter, the wherein quality of precious metals pt and precious metals pd
Than being 10~0.5：1, the coating includes cerium-aluminium composite oxide, molecular sieve and auxiliary agent bismuth oxide.
Further, the mass ratio of the molecular sieve and cerium-aluminium composite oxide is 1：2~10.
Further, the mass ratio of cerium oxide and aluminium oxide is 1 in the cerium-aluminium composite oxide：3~39.
Further, the coated weight of bismuth oxide is 0.5~6.0 grams per liter in the coating.
Further, the molecular sieve is Hydrogen beta-molecular sieve.
Further, the carrier is cordierite honeycomb ceramic or iron-chromium-aluminum metal honeycomb, and the hole density of the carrier is
200~600 mesh/square feet.
The preparation method of the oxidation catalyst of low temperature CO ignitions, includes the following steps：
(1) equi-volume impregnating prepares cerium-aluminium composite oxide：It is 1 by the mass ratio of cerium oxide and aluminium oxide：3~39
Cerous nitrate and alumina powder are weighed respectively, cerous nitrate aqueous solution are prepared by the saturated extent of adsorption of aluminium oxide, by prepared nitre
Sour cerium aqueous solution is added dropwise in aluminium oxide and continues 3~12h of stirring, is then allowed to stand 5~18h of ageing, and in 100~160 DEG C of items
Drying under part obtains cerium-aluminium composite oxide after finally being roasted at 450~600 DEG C of temperature；
(2) preparation of coating slurry：It is 1 by molecular sieve and cerium-aluminium composite oxide mass ratio：2~10 is compound by cerium-aluminium
Oxide and molecular sieve are added into deionized water stirring and form slurries, the gross mass of cerium-aluminium composite oxide and molecular sieve with
The mass ratio of deionized water is 2：3~8, then ball-milling technology is used to handle slurries, the particle D90 for controlling slurries is 5~35 μm,
Obtain coating slurry；
(3) load of noble metal：It is that 0.5~5.0 grams per liter calculates precious metals pt and expensive by the load capacity of noble metal on carrier
Precursor solution containing precious metals pt, precious metals pd is pressed the quality of precious metals pt and precious metals pd by the requirement of metal Pd
Than 10~0.5：1 is added in the coating slurry of step (2), stirs evenly；
(4) in coating bismuth salt addition：It is the needs that 0.5~6.0 grams per liter calculates bismuth oxide according to the coated weight of bismuth oxide
Soluble bismuth salt is added in the coating slurry in step (3) amount；
(5) coating of carrier sizing liquor：Cordierite honeycomb ceramic or iron-chromium-aluminum metal honeycomb substrate are immersed in step (4)
In slurries in, taken out after impregnating 1~5min, blown the channel of carrier inside using compressed air logical, purge time is 0.5~
3min, it is then that carrier is 4~10 hours dry under the conditions of 100~160 DEG C, finally carrier is roasted under the conditions of 400~550 DEG C
It burns 1~3 hour, obtains the oxidation catalyst for low temperature CO ignitions.
It uses the aluminium oxide with porous structure, large specific surface area for coated substrate, further passes through incipient impregnation
Cerium-aluminium composite oxide is prepared in method.The Lattice Oxygen of cerium oxide can pass through overflow effect and ADSORPTION STATE at a lower temperature
CO react, therefore alumina doped cerium oxide can improve the oxidability of CO, and auxiliary agent bismuth oxide is added in coating,
The content of the oxide ion conduction rate and mobile oxonium ion of coating can be further promoted, and then promotes CO low temperature ignitions, noble metal
Solution is the mixed solution of Pt, Pd predecessor, and the Pt-Pd alloys of formation can improve the thermal stability of precious metals pt.
Preparation method of the present invention is simple, and step is easily operated, is particularly suitable for industrialization large-scale production, is prepared
Catalyst has low temperature CO light-off performances outstanding, high conversion rate, and thermal stability is good, and has good NO oxidabilities.
Specific implementation mode
The present invention is further explained below in conjunction with specific embodiment.
Embodiment one：
A kind of oxidation catalyst for low temperature CO ignitions, catalyst carrier is cordierite honeycomb ceramic, and volume is
1.39 liters, hole density is 400 mesh/square feet；Contain cerium-aluminium composite oxide, molecular sieve and the coating of 0.5 grams per liter in coating
The bismuth oxide of amount, coating coated weight are 110 grams per liters；The coated weight of noble metal used be 2.1 grams per liters, wherein precious metals pt with it is expensive
The mass ratio of metal Pd is 2：1.
Preparation method includes the following steps：
(1) equi-volume impregnating prepares cerium-aluminium composite oxide：Cerium-aluminium composite oxide uses incipient impregnation legal system
It is standby.The alumina powder that quality is 780 grams is weighed, 50.5 gram of six nitric hydrate cerium dissolving is weighed, it is full to be configured to aluminium oxide used
With the aqueous solution of adsorbance, then cerous nitrate aqueous solution is added dropwise in alumina powder and continue stir 5h；It is then allowed to stand, is aged
12h dries 10h at 130 DEG C, obtains cerium-aluminium composite oxide after 550 DEG C of roasting 2h of Muffle furnace, the cerium-aluminium being prepared later
In composite oxides, the mass ratio of cerium oxide and aluminium oxide is 1：39.
(2) deionized water 900g is weighed, cerium-aluminium composite oxide 500g is sequentially added, molecular sieve 150g stirs evenly shape
At coating slurry, ball milling slurries to serous granule degree D90About 20 μm, gained slurries are persistently stirred；
(3) in slurries whipping process, will be equivalent to the platinum nitrate aqueous solution of 1.4 grams per liter coated weight Pt, be equivalent to 0.7 gram/
The palladium nitrate solution for rising coated weight Pd is added in coating paste, stirs 2h；
(4) then, the bismuth nitrate that will be equivalent to 0.5 grams per liter coated weight bismuth oxide is added in slurry, stirs 1h, is formed
Final slurry.
(5) it is taken out after cordierite honeycomb ceramic carrier being impregnated 2min in this final slurry, it then will with compressed air
Extra slurries are blown down inside carrier surface and duct, purge time 2min, are subsequently placed in baking oven at 120 DEG C dry 8h,
550 DEG C of roasting 2h are to get to catalyst A in Muffle furnace.
Embodiment two：
Specific preparation method and example 1 are essentially identical, the difference is that, in cerium-aluminium composite oxide used, cerium oxide
Mass ratio with aluminium oxide is 1：19, obtain catalyst B.
Embodiment three：
Specific preparation method and example 1 are essentially identical, the difference is that, in cerium-aluminium composite oxide used, cerium oxide
Mass ratio with aluminium oxide is 1：9, obtain catalyst C.
Example IV：
Specific preparation method and example 1 are essentially identical, the difference is that, in cerium-aluminium composite oxide used, cerium oxide
Mass ratio with aluminium oxide is 1：3, obtain catalyst D.
Embodiment five：
Specific preparation method and example 1 are essentially identical, the difference is that, the coated weight of added auxiliary agent bismuth oxide is
1.0 grams per liters obtain catalyst E.
Embodiment six：
Specific preparation method and example 1 are essentially identical, the difference is that, the coated weight of added auxiliary agent bismuth oxide is
3.0 grams per liters obtain catalyst F.
Embodiment seven：
Specific preparation method and example 1 are essentially identical, the difference is that, the coated weight of added auxiliary agent bismuth oxide is
6.0 grams per liters obtain catalyst G.
Embodiment eight：
A kind of oxidation catalyst for low temperature CO ignitions, catalyst carrier is cordierite honeycomb ceramic, and volume is
1.39 liters, hole density is 400 mesh/square feet；Contain cerium-aluminium composite oxide and molecular sieve in coating, coating coated weight is
80 grams per liters；The coated weight of noble metal used is 0.5 grams per liter, and the mass ratio of wherein Pt and Pd are 0.5：1.
Preparation method includes the following steps：
(1) equi-volume impregnating prepares cerium-aluminium composite oxide：Cerium-aluminium composite oxide uses incipient impregnation legal system
It is standby.The alumina powder that quality is 780 grams is weighed, 50.5 gram of six nitric hydrate cerium dissolving is weighed, it is full to be configured to aluminium oxide used
With the aqueous solution of adsorbance, then cerous nitrate aqueous solution is added dropwise in alumina powder and continue stir 5h；It is then allowed to stand, is aged
12 hours, 10h is dried at 130 DEG C later, cerium-aluminium composite oxide is obtained after 550 DEG C of roasting 2h of Muffle furnace, is prepared
In cerium-aluminium composite oxide, the mass ratio of cerium oxide and aluminium oxide is 1：39.
(2) 900 grams of deionized water, 591 grams of cerium-aluminium composite oxide are weighed, 59.1 grams of molecular sieve stirs evenly to form painting
Layer slurries, ball milling slurries to serous granule degree D90 are about 5 μm, and gained slurries are stirred；
(3) in slurries whipping process, it will be equivalent to the platinum nitrate aqueous solution of 0.167 grams per liter coated weight Pt, be equivalent to
The palladium nitrate solution of 0.333 grams per liter coated weight Pd is added in coating paste, stirs 2h；
(4) then, the bismuth nitrate that will be equivalent to 0.5 grams per liter coated weight bismuth oxide is added in slurry, stirs 1h, is formed
Final slurry.
(5) it is taken out after impregnating cordierite honeycomb ceramic carrier 2 minutes in this final slurry, it then will with compressed air
Extra slurries are blown down inside carrier surface and duct, and purge time is 2 minutes, are subsequently placed in baking oven at 120 DEG C dry 8h,
550 DEG C of roasting 2h are to get to catalyst in Muffle furnace.
Embodiment nine：
A kind of oxidation catalyst for low temperature CO ignitions, catalyst carrier is cordierite honeycomb ceramic, and volume is
1.39 liters, hole density is 400 mesh/square feet；Contain cerium-aluminium composite oxide and molecular sieve in coating, coating coated weight is
180 grams per liters；The coated weight of noble metal used is 5.0 grams per liters, and the mass ratio of wherein Pt and Pd are 10：1.
Preparation method includes the following steps：
(1) equi-volume impregnating prepares cerium-aluminium composite oxide：Cerium-aluminium composite oxide uses incipient impregnation legal system
It is standby.The alumina powder that quality is 600 grams is weighed, 504.7 gram of six nitric hydrate cerium dissolving is weighed, it is full to be configured to aluminium oxide used
With the aqueous solution of adsorbance, then cerous nitrate aqueous solution is added dropwise in alumina powder and continue stir 5h；It is then allowed to stand, is aged
12h dries 10h at 130 DEG C, obtains cerium-aluminium composite oxide after 550 DEG C of roasting 2h of Muffle furnace, the cerium-aluminium being prepared later
In composite oxides, the mass ratio of cerium oxide and aluminium oxide is 1：3.
(2) 900 grams of deionized water, 433.3 grams of cerium-aluminium composite oxide are weighed, 216.7 grams of molecular sieve stirs evenly shape
At coating slurry, ball milling slurries to serous granule degree D90About 35 μm, gained slurries are stirred；
(3) in slurries whipping process, it will be equivalent to the platinum nitrate aqueous solution of 4.545 grams per liter coated weight Pt, be equivalent to
The palladium nitrate solution of 0.455 grams per liter coated weight Pd is added in coating paste, stirs 2h；
(4) then, the bismuth nitrate that will be equivalent to 6.0 grams per liter coated weight bismuth oxides is added in slurry, stirs 1h, is formed
Final slurry.
(5) it is taken out after cordierite honeycomb ceramic carrier being impregnated 2min in this final slurry, it then will with compressed air
Extra slurries are blown down inside carrier surface and duct, purge time 2min, are subsequently placed in baking oven at 120 DEG C dry 8h,
550 DEG C of roasting 2h are to get to catalyst in Muffle furnace.
Comparative example one：
Specific preparation method and example 1 are essentially identical, the difference is that, used coating material is pure alumina and molecule
Sieve, obtains catalyst H.
Comparative example two：
Specific preparation method and example 1 are essentially identical, the difference is that, used coating material is pure alumina and molecule
Sieve, and auxiliary agent bismuth oxide is not added, obtain catalyst I.
Performance evaluation is carried out to the catalyst A-I being prepared in implementation：
The catalyst sample being prepared is subjected to laboratory simulation distribution evaluation, distribution component list is as shown in table 1, simulation
Atmosphere air speed is 40000h-1.In sample evaluation procedure, electric furnace temperature programming is controlled by temperature controller, is analyzed by HC analyzers, CO
Instrument and NOx analyzers measure the concentration of the front and back gas each component of reaction, obtain the conversion ratio of sample under different temperatures, and thus obtain
To the T of sample50.The T of HC and CO50Temperature is lower, shows that the light-off performance of catalyst is better；React the NO generated2Concentration and nitrogen
Ratio (the NO of oxide total concentration2/ NOx) it is bigger, show that the NO oxidabilities of catalyst are stronger.Catalyst aging condition is gas
Atmosphere stove (750 DEG C, 20h, 10% vapor) hydrothermal aging.As a result as shown in table 2 and table 3.
1 diesel vehicle of table simulates distribution composition
| Gas | Content | Gas | Content |
| HC(C3H8) | 150ppm | O2 | 10% |
| NO | 200ppm | H2O | 10% |
| CO | 800ppm | N2 | Remaining nitrogen |
| CO2 | 6% |
The T of 2 fresh state catalyst of table50(HC、CO)
The T of 3 aging state catalyst of table50-aged(HC、CO)
As shown in Table 2, it is showed using the oxidation catalyst for CO low temperature ignitions that preparation method in the present invention obtains
CO light-off performances outstanding, the CO initiation temperatures (T of catalyst A-G are gone out50) it is significantly lower than comparative example H and I.In addition, catalyst
A-G equally has good NO oxidabilities.As seen from the results in Table 3, still have after catalyst A-G hydrothermal agings lower
HC, CO initiation temperature, this illustrates the catalyst good thermal stability that preparation method using the present invention obtains.
Claims (7)
1. a kind of oxidation catalyst of low temperature CO ignitions, it is characterised in that：Including carrier, coating is coated on the carrier,
The coated weight of the coating is 80 ~ 180 grams per liters, and being loaded in the coating has precious metals pt and precious metals pd, the precious metals pt
Load capacity with precious metals pd is 0.5 ~ 5.0 grams per liter, and wherein the mass ratio of precious metals pt and precious metals pd is 10 ~ 0.5：1, institute
It includes cerium-aluminium composite oxide, molecular sieve and auxiliary agent bismuth oxide to state coating.
2. the oxidation catalyst of low temperature CO ignitions as described in claim 1, it is characterised in that：The molecular sieve with
The mass ratio of cerium-aluminium composite oxide is 1：2~10.
3. the oxidation catalyst of low temperature CO ignitions as described in claim 1, it is characterised in that：Cerium-the aluminium is compound
The mass ratio of cerium oxide and aluminium oxide is 1 in oxide：3~39.
4. the oxidation catalyst of low temperature CO ignitions as described in claim 1, it is characterised in that：Bismuth oxide in the coating
Coated weight is 0.5 ~ 6.0 grams per liter.
5. the oxidation catalyst of low temperature CO ignitions as described in claim 1, it is characterised in that：The molecular sieve is Hydrogen β
Molecular sieve.
6. the oxidation catalyst of low temperature CO ignitions as described in claim 1, it is characterised in that：The carrier is cordierite bee
The hole density of nest ceramics or iron-chromium-aluminum metal honeycomb, the carrier is 200 ~ 600 mesh/square feet.
7. the preparation method of the oxidation catalyst of low temperature CO ignitions described in claim 1, it is characterised in that：Including walking as follows
Suddenly：
（1）Equi-volume impregnating prepares cerium-aluminium composite oxide：It is 1 by the mass ratio of cerium oxide and aluminium oxide：3 ~ 39 claim respectively
Cerous nitrate and alumina powder are taken, cerous nitrate aqueous solution is prepared by the saturated extent of adsorption of aluminium oxide, by prepared cerous nitrate water
Solution is added dropwise in aluminium oxide and continues 3 ~ 12h of stirring, is then allowed to stand 5 ~ 18h of ageing, and dried under the conditions of 100 ~ 160 DEG C,
Cerium-aluminium composite oxide is obtained after finally being roasted at 450 ~ 600 DEG C of temperature；
（2）The preparation of coating slurry：It is 1 by molecular sieve and cerium-aluminium composite oxide mass ratio：2 ~ 10 by cerium-aluminum composite oxide
Object and molecular sieve are added into deionized water stirring and form slurries, the gross mass of cerium-aluminium composite oxide and molecular sieve and go from
The mass ratio of sub- water is 2：3 ~ 8, then ball-milling technology is used to handle slurries, the particle D90 for controlling slurries is 5 ~ 35 μm, is applied
Layer slurries；
（3）The load of noble metal：It is that 0.5 ~ 5.0 grams per liter calculates precious metals pt and noble metal by the load capacity of noble metal on carrier
The requirement of Pd, by the precursor solution containing precious metals pt, precious metals pd by precious metals pt and precious metals pd mass ratio 10 ~
0.5：1 is added to step（2）Coating slurry in, stir evenly；
（4）The addition of bismuth salt in coating：It is the requirement that 0.5 ~ 6.0 grams per liter calculates bismuth oxide according to the coated weight of bismuth oxide, it will
Step is added in soluble bismuth salt（3）In coating slurry in；
（5）The coating of carrier sizing liquor：Cordierite honeycomb ceramic or iron-chromium-aluminum metal honeycomb substrate are immersed in step（4）In
It in slurries, being taken out after impregnating 1 ~ 5min, is blown the channel of carrier inside using compressed air logical, purge time is 0.5 ~ 3min,
Then carrier under the conditions of 100 ~ 160 DEG C is dried to 4 ~ 10 h, carrier is finally roasted to 1 ~ 3 h under the conditions of 400 ~ 550 DEG C, is obtained
To the oxidation catalyst for low temperature CO ignitions.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113856678A (en) * | 2021-11-01 | 2021-12-31 | 中国科学院城市环境研究所 | Oxidation catalyst and preparation method and application thereof |
| CN114768795A (en) * | 2022-03-30 | 2022-07-22 | 安徽方信立华环保科技有限公司 | Preparation method of honeycomb catalyst for treating CO in sintering flue gas |
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