CN108940280A - A kind of gasoline car three-way catalyst and preparation method thereof - Google Patents
A kind of gasoline car three-way catalyst and preparation method thereof Download PDFInfo
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- CN108940280A CN108940280A CN201810782151.5A CN201810782151A CN108940280A CN 108940280 A CN108940280 A CN 108940280A CN 201810782151 A CN201810782151 A CN 201810782151A CN 108940280 A CN108940280 A CN 108940280A
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/8643—Removing mixtures of carbon monoxide or hydrocarbons and nitrogen oxides
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Abstract
The present invention relates to a kind of gasoline car three-way catalysts and preparation method thereof, belong to the preparation technical field of gasoline car catalyst.Catalyst is using cordierite honeycomb ceramic as catalyst carrier, coating of the surface applied in two coats of catalyst carrier containing precious metals pd and Rh, including primer coating and outer coating, wherein primer coating includes Pd-Sr/La-Al2O3Powder and Pd/Ce-Zr solid solution powder are made into slurries after mixing, auxiliary agent and binder is added, and are coated in catalyst carrier, form primer coating；Outer coating includes Rh/Zr-Nb-Al2O3Powder and Pd/Ce-Zr solid solution powder are mixed by being modified to mixing zirconium aluminium oxide and load a small amount of acidic oxide on zirconium aluminium oxide, can increase aluminium oxide surface acid site, be conducive to reduction-state Rh generation, oxidation state Rh is inhibited to generate.The present invention improves existing TWC catalyst ignition and endurance quality, improves hydrocarbon, CO and NOXLow temperature light-off performance, and the endurance quality of catalyst is more preferable.
Description
Technical field
The present invention relates to a kind of gasoline car three-way catalysts and preparation method thereof, belong to the technology of preparing of gasoline car catalyst
Field.
Background technique
Automobile exhaust pollution has become one of main source of atmosphere pollution.Most oxynitrides in city
(NOX), CO and hydrocarbon (HC) be all to be generated by vehicle exhaust.NOX, CO, HC, PM not only to human body cause damage and
And destroy the environment of human survival in certain condition.
Gasoline car three-way catalyst (TWC) is used for oxidation and NO to CO, HC in tail-gas from gasoline automobilesXReduction, coating
It is mainly made of aluminium oxide, Ce-Zr solid solution, auxiliary agent and active noble metal constituent, noble metal is gasoline car three-way catalyst
Key component.For gasoline car TWC catalyst, be exactly using TWC catalyst reduce gasoline tail gas in HC, CO and
NOXDeng chemical reaction activation energy, so that HC, CO in tail gas is carried out oxidation reaction at a lower temperature, be converted into CO2With
H2O, NOXReduction reaction is carried out at a lower temperature, is converted into N2.Gasoline car three-way catalyst usually with ceramic honey comb or
Honeycomb is carrier, loads oxide coating and active metal component thereon, common noble metal component is Pt, Pd, Rh,
Ir, Ru etc., it is Pd and Rh that tail-gas from gasoline automobiles, which post-processes widely used noble metal, at present.
As discharge standard is gradually stringent, emission limit is lower and lower, higher and higher to the life requirement of catalyst, right
HC, CO and NOXInitiation temperature require it is lower and lower, so developing the gasoline car three that a kind of light-off performance is good, endurance quality is good
Imitating catalyst becomes inevitable requirement.
Summary of the invention
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, provide a kind of gasoline car three
Imitate catalyst and preparation method thereof.Preparation method of the invention is simple, HC and CO initiation temperature is low and endurance quality is preferable.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of gasoline car three-way catalyst and its system
Preparation Method, which is characterized in that the preparation method has the feature that
A kind of gasoline car three-way catalyst, catalyst using cordierite honeycomb ceramic as catalyst carrier, catalyst carrier
Surface is coated with two layers of coating slurry containing precious metals pd and Rh, including primer coating and outer coating；
Wherein, primer coating includes Pd-Sr/La-Al2O3Powder and Pd/Ce-Zr solid solution powder are matched after mixing and are slurried
Auxiliary agent and binder is added in liquid, is coated in catalyst carrier, forms primer coating；Outer coating includes Rh/Zr-Nb-Al2O3
Powder and Pd/Ce-Zr solid solution powder, are made into slurries after mixing, are coated on primer coating, form outer coating.
The auxiliary agent is one of simple substance Sr, Ba or La and its compound or a variety of, and the binder is aluminium glue or zirconium
Glue.
A kind of preparation method of gasoline car three-way catalyst, includes the following steps:
Bottom preparation and coating:
(1) material weighs: by weight 0.17~0.6:0.3~0.75:0.01~0.1:0.01~0.05:0.01~
0.05 weighs La-Al respectively2O3, Ce-Zr solid solution, Ba (AC)2、Sr(NO3)3·6H2O, aluminium glue；
(2) noble metal weighs: quality=Pd concentration of the Pd/28.316/ total powder weight of coated weight * bottom, wherein Pd
Concentration: 5~150g/ft3, coated weight is 100~150g/L；
(3) precious metals pd-Sr/La-Al2O3The preparation of powder: 1/2~2/3 of Pd amount in step (2) is taken, by Sr
(NO3)3·6H2O is dissolved in Pd (NO3)2In solution, and ethanol solution dilution is added, stirs 5~10h, incipient wetness impregnation is in La-AL2O3
On, it is aged 12~36h；
(4) preparation of Pd/Ce-Zr solid solution powder: weighing 1/3~1/2 of Pd amount in step (2), by Pd (NO3)2Solution
It is diluted with ethanol solution, stirs 5~10h, incipient wetness impregnation is aged 12~36h on Ce-Zr solid solution；
(5)Pd-Sr/La-Al2O3The processing of powder and Pd/Ce-Zr solid solution powder: by powder material in step (3) and (4)
Material drying, roasting, 100~150 DEG C of drying temperature, 5~15h of drying time, 450~550 DEG C of maturing temperature, calcining time 1~
5h；
(6) preparation of slurries: by treated in step (5) Pd-Sr/La-Al2O3Powder and Pd/Ce-Zr solid solution powder
Body is added in deionized water, and load weighted Ba (AC) is added2And aluminium glue, it is in its solidfied material content between 35%~40%,
It is uniformly mixed；
(7) ball milling of slurries: slurries pass through ball mill grinding, and the final granularity D90 of slurries is 7~25 μm；
(8) determination of solid content: taking slurries 10g in step (7), 550~600 DEG C of 20~30min of roasting, surveys solidfied material and contains
Amount；
(9) slurry coating coat: with quantitatively coating special plane by coating slurry be coated in carrier on, coated weight be 80~
200g/L；
(10) catalyst is dried: the catalyst flash baking after coating, until catalyst quality no longer changes, drying temperature
It is 100~150 DEG C；
(11) catalyst roasts: the catalyst after drying being put into Muffle furnace, 1~5h is roasted at 450~550 DEG C, is protected
It is cooled to room temperature after temperature；
Outer layer preparation and coating:
(12) material weighs: claiming respectively by weight 0.35~0.7:0.2~0.6:0.01~0.1:0.01~0.05
Take Zr-Al2O3, Ce-Zr solid solution, C6H4NbO12And aluminium glue；
(13)Zr-Al2O3Modified preparation: by load weighted C in step (12)6H4NbO12Incipient wetness impregnation is in Zr-Al2O3
On, modified Zr-Nb-Al is made in drying, roasting2O3Powder；
(14) noble metal weighs: amount=Pd concentration of the Pd/28.316/ total powder weight of coated weight * outer layer, and the amount of Rh=
The concentration of the Rh/28.316/ total powder weight of coated weight * outer layer, wherein the concentration of Pd: 1~30g/ft3, the concentration of Rh: 1~60g/
ft3, coated weight is 70~100g/L；
(15) noble metal Rh/Zr-Nb-Al2O3The preparation of powder: by weighed Rh (NO3)3Solution ethanol solution is dilute
It releases, stirs 5~10h, incipient wetness impregnation is in Zr-Nb-Al2O3On, it is aged 12~36h；
(16) preparation of Pd/Ce-Zr solid solution powder: Pd (NO in step (14)3)2Solution is diluted with ethanol solution, stirring
5~10h, incipient wetness impregnation are aged 12~36h on Ce-Zr solid solution；
(17)Rh/Zr-Nb-Al2O3The processing of powder and Pd/Ce-Zr solid solution powder: by powder in step (15) and (16)
Body drying, roasting, 100~150 DEG C of drying temperature, 5~15h of drying time, 450~550 DEG C of maturing temperature, calcining time 1~
5h；
(18) preparation of slurries: the Rh/Zr-Nb-Al that will be handled well in step (17)2O3Powder and Pd/Ce-Zr solid solution
Powder is added in deionized water, and load weighted aluminium glue is added, and is in its solidfied material content between 28%~35%, and mixing is equal
It is even；
(19) ball milling of slurries: slurries pass through ball mill grinding, and the final granularity of slurries to D90 is 7~25 μm；
(20) determination of solid content: taking step (19) slurries 10g, 550~600 DEG C of 20~30min of roasting, surveys solidfied material and contains
Amount；
(21) slurry coating coat: with quantitatively coating special plane by coating slurry be coated in carrier on, coated weight be 70~
100g/L；
(22) catalyst is dried: the catalyst flash baking after coating, until catalyst quality no longer changes, drying temperature
It is 100~150 DEG C；
(23) catalyst roasts: drying rear catalyst being put into Muffle furnace, 450~550 DEG C of 1~5h of roasting, heat preservation knot
It is cooled to room temperature after beam.
La-Al in the step (1)2O3The mass content of middle La is 1%~4%.
The quality of precious metal palladium in the step (2) occupies the 85%~98% of Pd total amount.
The quality of precious metal palladium in the step (3) occupies the 40%~66% of Pd total amount.
The quality of precious metal palladium in the step (4) occupies the 25%~50% of Pd total amount.
Ce mass content is 25%~60% in Ce-Zr solid solution in the step (1) and (12), Zr- in step (12)
Al2O3Zr mass content be 5%~60%.
Aluminium glue solidfied material mass content in the step (1) and (12) is 10%.
Compared with the prior art, the present invention has the following advantages:
(1) improved for existing TWC catalyst ignition and endurance quality, the load matrix and noble metal of noble metal
Load process have larger difference, the low temperature light-off performance of hydrocarbon, CO and NOx can be improved in improved catalyst,
And the endurance quality of catalyst is more preferable.
(2) auxiliary agent and precious metals pd solution are impregnated on aluminium oxide, are conducive to inhibit precious metals pd particle at high temperature
Increase, precious metals pd catalytic activity is effectively guaranteed, while a part of precious metals pd being impregnated on Ce-Zr solid solution, dries
Dry, roasting forms Pd/Ce-Zr solid solution powder, promotes the storage of OSC, discharges the rate of oxygen.
(3) it by being modified to mixing zirconium aluminium oxide, mixes and loads a small amount of acidic oxide, Ke Yizeng on zirconium aluminium oxide
Oxygenation aluminium surface acid site is conducive to reduction-state Rh generation, oxidation state Rh is inhibited to generate.
Specific embodiment
It below will the invention will be further described according to specific embodiment.Three examples are all made of diameter and are below
The cylindrical cordierite honeycomb ceramic carrier of 80mm, a height of 60mm, volume 0.301L, vehicle weight 97g, precious metals pd
Concentration is 0.1405g (noble metal)/g (liquid), and the concentration of noble metal Rh is 0.1099g (noble metal)/g (liquid).
Embodiment one
Gasoline car three-way catalyst and preparation method thereof, includes the following steps:
Bottom preparation and coating
(1) material weighs: by weight 0.44:0.44:0.05:0.03:0.04 weighing La-Al respectively2O3, 45%Ce
Ce-Zr solid solution, the Ba (AC) of content2、Sr(NO3)3·6H2O, aluminium glue；
(2) noble metal weighs: taking above-mentioned powder 200g in proportion, the concentration of Pd is 36g/ft3, coated weight 120g/
L, according to the concentration of Pd, coated weight and the total powder re-computation of bottom and the amount for weighing noble metal, the amount of Pd is 15.08g；
(3) precious metals pd-Sr/La-Al2O3The preparation of powder: weigh precious metals pd in step (2) 2/3rds are
10.05g, by Sr (NO3)3·6H2O is dissolved in precious metals pd (NO3)2In solution and add ethanol solution (ethyl alcohol in mass ratio: water=1:
1) it is diluted to La-Al2O3The 95% of powder water absorption rate stirs 6h, and incipient wetness impregnation is in La-Al2O3On, it is aged 15h；
(4) precious metals pd/Ce-Zr solid solution powder preparation: the one third for weighing step (2) precious metals pd is
5.03g, by Pd (NO3)2Solution is diluted to the suction of Ce-Zr solid solution powder with ethanol solution (in mass ratio ethyl alcohol: water=1:1)
The 95% of water rate, stirs 5h, and incipient wetness impregnation is aged 12h on Ce-Zr solid solution；
(5)Pd-Sr/La-AL2O3The processing of powder and Pd/Ce-Zr solid solution powder: by the powder in step (3) and (4)
Material drying, roasting, 100 DEG C of drying temperature, drying time 15h, 450 DEG C of maturing temperature, calcining time 5h；
(6) preparation of slurries: by calcined material, that is, Pd-Sr/La-Al in step (5)2O3Powder and Pd/Ce-Zr solid solution
Powder is added in 250mL deionized water, 5% of Ba element wt in step (1) is added, with Ba (AC)2Form addition, adds simultaneously
Enter aluminium glue in step (1), adjusting its solidfied material content is 38%, is uniformly mixed；
(7) ball milling of slurries: slurries pass through ball mill grinding, and the final granularity of slurries to D90 is 10 μm；
(8) determination of solid content: step (7) slurries 10g, 550 DEG C of roasting 30min is taken to measure solidfied material content 32%；
(9) slurry coating coats: being coated with quantitatively coating special plane, catalyst carrier is placed at application chamber, is pressed
According to coated weight be 120g/L and the solid content that measures to calculate the wet weight gain of target be 112.8g, the slurries calculated are added to slurry
In disk, quantitative coating is carried out, coating slurry is coated on carrier；
(10) catalyst is dried: the catalyst flash baking after coating, until catalyst quality no longer changes, drying temperature
It is 110 DEG C；
(11) catalyst roasts: drying rear catalyst being put into Muffle furnace, 550 DEG C of roasting 2h are cooling after heat preservation
To room temperature；
Outer layer preparation and coating
(12) material weighs: by weight 0.62:0.31:0.05:0.02 weighing Zr-Al respectively2O3, 40%Ce content
Ce-Zr solid solution, C6H4NbO12, aluminium glue；
(13) noble metal weighs: precious metals pd is according to 4g/ft3, Rh is according to 6g/ft3It calculates, coated weight 80g/L, always
Powder by 200g calculate, calculated separately again according to the concentration of Pd, Rh, coated weight and the total powder of outer layer and weigh noble metal Pd and
Rh amount, the amount of Pd are 2.513g, and the amount of Rh is 4.819g；
(14)Zr-Al2O3Modified preparation: by step (12) C6H4NbO12Incipient wetness impregnation is in Zr-Al2O3On, drying, roasting
Modified Zr-Nb-Al is made2O3Powder；
(15) noble metal Rh/Zr-Nb-Al2O3The preparation of powder: by weighed Rh (NO3)3Solution is with ethyl alcohol (according to quality
Than ethyl alcohol: water=1:1) it is diluted to Zr-Nb-Al2O3The 95% of powder water absorption rate stirs 6h, and incipient wetness impregnation is in Zr-Nb-Al2O3
On, it is aged 12h；
(16) precious metals pd/Ce-Zr solid solution powder preparation: by weighed Pd (NO3)2Solution with ethanol solution (according to
Quality is than ethyl alcohol: water=1:1) be diluted to Ce-Zr solid solution powder water absorption rate 95%, stir 5h, incipient wetness impregnation is in Ce-Zr
On solid solution, it is aged 12h；
(17)Rh/Zr-Nb-Al2O3The processing of powder and Pd/Ce-Zr solid solution powder: by powder in step (15) and (16)
The drying of body material, roasting, 100 DEG C of drying temperature, drying time 15h, 550 DEG C of maturing temperature, calcining time 1h；
(18) preparation of slurries: by calcined material, that is, Rh/Zr-Nb-Al in step (15) and (16)2O3Powder and Pd/Ce-
Zr solid solution powder is added in 430mL deionized water, and aluminium glue in step (12) is added, and adjusting its solidfied material content is 30%, mixes
It closes uniform；
(19) ball milling of slurries: slurries pass through ball mill grinding, and the final granularity of slurries to D90 is 9 μm of iu
(20) determination of solid content: weighing slurries in step (19), weighs slurries 10g, and 550 DEG C of roasting 30min measure solidification
Object content is 26%；
(21) slurry coating coats: being coated with quantitatively coating special plane, catalyst carrier is placed at application chamber, is pressed
According to coated weight be 80g/L requirement and the wet weight gain of solid content calculating target measured is 92.6g, and the slurries calculated are added to slurry
In charging tray, quantitative coating is carried out, coating slurry is coated on carrier；
(22) catalyst is dried: the catalyst coated passes through 110 DEG C of flash bakings, and the water evaporation in coating is fallen；
(23) catalyst roasts: drying rear catalyst being put into Muffle furnace, 550 DEG C of roasting 2h are cooling after heat preservation
To room temperature.
Embodiment two:
Gasoline car three-way catalyst and preparation method thereof, includes the following steps:
Bottom preparation and coating
(1) material weighs: by weight 0.4:0.4:0.1:0.05:0.05 weighing La-Al respectively2O3, 45%Ce content
Ce-Zr solid solution, Ba (AC)2、Sr(NO3)3·6H2O, aluminium glue；
(2) noble metal weighs: taking above-mentioned powder 200g in proportion, precious metals pd total amount is 135g/ft3, coated weight
For 140g/L, according to the concentration of Pd, coated weight and corresponding powder re-computation and the amount for weighing noble metal, the amount of Pd is
48.475g；
(3) precious metals pd-Sr/La-Al2O3The preparation of powder: weigh above-mentioned precious metals pd solution 2/3rds are
32.317g, by Sr (NO3)3·6H2O is dissolved in precious metals pd (NO3)2In solution and add ethanol solution (ethyl alcohol in mass ratio: water=
1:1) it is diluted to La-Al2O3The 95% of powder water absorption rate stirs 10h, and incipient wetness impregnation is in La-Al2O3On, it is aged 36h；
(4) precious metals pd/Ce-Zr solid solution powder preparation: the one third for weighing above-mentioned precious metals pd solution is
16.158g, by Pd (NO3)2Solution is diluted to Ce-Zr solid solution powder with ethanol solution (second alcohol and water=1:1 in mass ratio)
The 95% of water absorption rate, stirs 10h, and incipient wetness impregnation is aged 36h on Ce-Zr solid solution；(5)Pd-Sr/La-Al2O3Powder and
The processing of Pd/Ce-Zr solid solution powder: powder body material drying, roasting in step (3) and (4), are dried by 150 DEG C of drying temperature
Time 5h, 550 DEG C of maturing temperature, calcining time 1h；
(6) preparation of slurries: by step (5) calcined material, that is, Pd-Sr/La-Al2O3Powder and Pd/Ce-Zr solid solution powder
Body is added in 236mL deionized water, weight 10%Ba element in step (1) is added, with Ba (AC)2Form addition, is added simultaneously
Aluminium glue in step (1), adjusting its solidfied material content is 38%, is uniformly mixed；(7) ball milling of slurries: slurries are ground by ball mill
Mill, the final granularity of slurries to D90 are 12 μm；
(8) determination of solid content: step (7) slurries 10g, 600 DEG C of roasting 20min is taken to measure solidfied material content 33%；
(9) slurry coating coats: being coated with quantitatively coating special plane, catalyst carrier is placed at application chamber, is pressed
According to coated weight be 140g/L requirement and the wet weight gain of solid content calculating target measured is 127.6g, and the slurries calculated are added to
In slurry disk, quantitative coating is carried out, coating slurry is coated on carrier；
(10) catalyst is dried: the catalyst flash baking coated, until catalyst quality no longer changes, drying temperature
It is 150 DEG C；
(11) catalyst roasts: drying rear catalyst being put into Muffle furnace, 550 DEG C of roasting 1h are cooling after heat preservation
To room temperature；
Outer layer preparation and coating
(12) material weighs: by weight 0.58:0.3:0.08:0.04 weighing Zr-Al respectively2O3, 40%Ce content
Ce-Zr solid solution, C6H4NbO12, aluminium glue；
(13) noble metal weighs: precious metals pd is according to 15g/ft3, Rh is according to 22g/ft3It calculates, coated weight 85g/L,
Total powder is calculated by 200g, is calculated separately again according to the concentration of Pd, Rh, coated weight and the total powder of outer layer and is weighed the Pd of noble metal
And Rh amount, the amount of Pd are 8.871g, the amount of Rh is 16.634g；
(14)Zr-Al2O3Modified preparation: by step (12) C6H4NbO12Incipient wetness impregnation is in Zr-Al2O3On, drying, roasting
Modified Zr-Nb-Al is made2O3Powder；
(15) noble metal Rh/Zr-Nb-Al2O3The preparation of powder: by weighed Rh (NO3)3Solution (presses matter with ethanol solution
Amount is than ethyl alcohol: water=1:1) it is diluted to Zr-Nb-Al2O3The 95% of powder water absorption rate stirs 10h, and incipient wetness impregnation is in Zr-Nb-
Al2O3On, it is aged 36h；
(16) precious metals pd/Ce-Zr solid solution powder preparation: by weighed Pd (NO3)2Solution (presses matter with ethanol solution
Measure than second alcohol and water=1:1) be diluted to Ce-Zr solid solution powder water absorption rate 95%, stir 10h, incipient wetness impregnation is in Ce-Zr
On solid solution, it is aged 36h；
(17)Rh/Zr-Nb-Al2O3The processing of powder and Pd/Ce-Zr solid solution powder: by powder in step (15) and (16)
The drying of body material, roasting, 150 DEG C of drying temperature, drying time 5h, 550 DEG C of maturing temperature, calcining time 1h；
(18) preparation of slurries: by calcined material, that is, Rh/Zr-Nb-Al in step (17)2O3Powder and Pd/Ce-Zr solid solution
Body powder is added in 395mL deionized water, and aluminium glue in step (12) is added, and adjusting its solidfied material content is 30%, is uniformly mixed；
(19) ball milling of slurries: slurries pass through ball mill grinding, and the final granularity of slurries to D90 is 12 μm；
(20) determination of solid content: taking step (19) slurries 10g, 600 DEG C of roasting 20min, and measuring solidfied material content is 25%；
(21) slurry coating coats: being coated with quantitatively coating special plane, catalyst carrier is placed at application chamber, is pressed
According to coated weight be 85g/L requirement and the wet weight gain of solid content calculating target measured is 102.3g, and the slurries calculated are added to
In slurry disk, quantitative coating is carried out, coating slurry is coated on carrier；
(22) catalyst is dried: the catalyst coated passes through 150 DEG C of flash bakings, and the water evaporation in coating is fallen；
(23) catalyst roasts: drying rear catalyst being put into Muffle furnace, 550 DEG C of roasting 1h are cooling after heat preservation
To room temperature.
Embodiment three:
Gasoline car three-way catalyst and preparation method thereof, includes the following steps:
Bottom preparation and coating
(1) material weighs: by weight 0.25:0.64:0.05:0.03:0.03 weighing La-Al respectively2O3, 45%Ce
Ce-Zr solid solution, the Ba (AC) of content2、Sr(NO3)3·6H2O, aluminium glue；
(2) noble metal weighs: taking above-mentioned powder 200g in proportion, precious metals pd total amount is 26g/ft3, coated weight is
120g/L, according to the concentration of Pd, coated weight and total powder re-computation and the amount for weighing noble metal, the amount of Pd is 10.892g；
(3) precious metals pd-Sr/La-Al2O3The preparation of powder: weighing 2/3rds of above-mentioned precious metals pd is 7.261g,
By Sr (NO3)3·6H2O is dissolved in precious metals pd (NO3)2In solution and add ethanol solution (in mass ratio ethyl alcohol: water=1:1) dilution
To La-Al2O3The 95% of powder water absorption rate stirs 6h, and incipient wetness impregnation is in La-Al2O3On, it is aged 12h；
(4) precious metals pd/Ce-Zr solid solution powder preparation: the one third for weighing above-mentioned precious metals pd solution is
3.63g, by Pd (NO3)2Solution is diluted to the suction of Ce-Zr solid solution powder with ethanol solution (in mass ratio ethyl alcohol: water=1:1)
The 95% of water rate, stirs 6h, and incipient wetness impregnation is aged 12h on Ce-Zr solid solution；(5)Pd-Sr/La-AL2O3Powder and Pd/
The processing of Ce-Zr solid solution powder: by powder body material drying, roasting in step (3) and (4), 100 DEG C of drying temperature, when drying
Between 8h, 550 DEG C of maturing temperature, calcining time 2h；
(6) preparation of slurries: by calcined material, that is, Pd-Sr/La-Al in step (5)2O3Powder and Pd/Ce-Zr solid solution
Powder is added in 272mL deionized water, weight 5%Ba element in step (1) is added, with Ba (AC)2Form addition, is added simultaneously
Aluminium glue in step (1), adjusting its solidfied material content is 38%, is uniformly mixed；
(7) ball milling of slurries: slurries pass through ball mill grinding, and the final granularity of slurries to D90 is 8 μm；
(8) determination of solid content: step (7) slurries 10g, 575 DEG C of roasting 25min is taken to measure solidfied material content 32%；
(9) slurry coating coats: being coated with quantitatively coating special plane, catalyst carrier is placed at application chamber, is pressed
According to coated weight be 120g/L requirement and the wet weight gain of solid content calculating target measured is 112.87g, and the slurries calculated are added
Into slurry disk, quantitative coating is carried out, coating slurry is coated on carrier；
(10) catalyst is dried: the catalyst coated passes through 100 DEG C of flash bakings, and the water evaporation in coating is fallen；
(11) catalyst roasts: drying rear catalyst being put into Muffle furnace, 550 DEG C of roasting 2h are cooling after heat preservation
To room temperature；
Outer layer preparation and coating
(12) material weighs: by weight 0.58:0.3:0.1:0.02 weighing Zr-Al respectively2O3, 40%Ce content
Ce-Zr solid solution, C6H4NbO12, aluminium glue；
(13) noble metal weighs: precious metals pd is according to 2g/ft3, Rh is according to 22g/ft3It calculates, coated weight 80g/L, always
Powder by 200g calculate, calculated separately again according to the concentration of Pd, Rh, coated weight and the total powder of outer layer and weigh noble metal Pd and
Rh amount, the amount of Pd are 1.256g, and the amount of Rh is 17.673g；
(14)Zr-Al2O3Modified preparation: by C6H4NbO12Incipient wetness impregnation is in Zr-Al2O3On, drying, roasting, which are made, to be modified
Zr-Nb-Al2O3Powder；
(15) noble metal Rh/Zr-Nb-Al2O3The preparation of powder: by weighed Rh (NO3)3Solution with ethyl alcohol (in mass ratio
Ethyl alcohol: water=1:1) it is diluted to Zr-Nb-Al2O3The 95% of powder water absorption rate stirs 8h, and incipient wetness impregnation is in Zr-Nb-Al2O3On,
It is aged 12h；
(16) precious metals pd/Ce-Zr solid solution powder preparation: by weighed Pd (NO3)2Solution (presses matter with ethanol solution
Measure than ethyl alcohol: water=1:1) be diluted to Ce-Zr solid solution powder water absorption rate 95%, stir 8h, incipient wetness impregnation is solid in Ce-Zr
On solution, it is aged 12h；
(17)Rh/Zr-Nb-Al2O3The processing of powder and Pd/Ce-Zr solid solution powder: by powder in step (15) and (16)
The drying of body material, roasting, 100 DEG C of drying temperature, drying time 10h, 550 DEG C of maturing temperature, calcining time 2h；
(18) preparation of slurries: by calcined material, that is, Rh/Zr-Nb-Al in step (17)2O3Powder and Pd/Ce-Zr solid solution
Body powder is added in 430mL deionized water, and aluminium glue in step (12) is added, and adjusting its solidfied material content is 30%, is uniformly mixed；
(19) ball milling of slurries: slurries pass through ball mill grinding, and the final granularity of slurries to D90 is 12 μm；
(20) determination of solid content: slurries 10g in step (19) is taken, 575 DEG C of roasting 25min, measuring solidfied material content is
26%；
(21) slurry coating coats: being coated with quantitatively coating special plane, catalyst carrier is placed at application chamber, is pressed
According to coated weight be 80g/L requirement and the wet weight gain of solid content calculating target measured is 92.6g, and the slurries calculated are added to slurry
In charging tray, quantitative coating is carried out, coating slurry is coated on carrier；
(22) catalyst is dried: the catalyst coated passes through 100 DEG C of flash bakings, and the water evaporation in coating is fallen；
(23) catalyst roasts: drying rear catalyst being put into Muffle furnace, 550 DEG C of roasting 2h are cooling after heat preservation
To room temperature.
Comparative example
Bottom preparation and coating
(1) material weighs: by weight 0.28:0.64:0.05:0.03 weighing La-Al respectively2O3, 40%Ce content
Ce-Zr solid solution, Ba (AC)2, aluminium glue, be made into slurries, be milled to granularity D90 be 8 μm；
(2) noble metal weighs: calculating according to above-mentioned powder 200g, precious metals pd total amount is 28g/ft3, coated weight is
120g/L, according to the concentration of Pd, coated weight and total powder re-computation and the amount for weighing noble metal, the amount of Pd is 11.729g；
(3) precious metals pd solution the addition of precious metals pd: is added to 188g's containing powder (Ba and aluminium glue not wherein)
In slurries；
(4) addition of Ba and aluminium glue: weight 5%Ba element is added, with Ba (AC)2Form addition, while it is mixed that aluminium glue is added
It closes uniform；
(5) determination of solid content: taking step (4) to weigh slurries 10g, and 550~600 DEG C of 20~30min of roasting measure solidfied material
Content 34%；
(6) slurry coating coats: being coated with quantitatively coating special plane, catalyst carrier is placed at application chamber, is pressed
According to coated weight be 120g/L requirement and the wet weight gain of solid content calculating target measured is 106.2g, and the slurries calculated are added to
In slurry disk, quantitative coating is carried out, coating slurry is coated on carrier；
(7) catalyst is dried: the catalyst coated passes through 100 DEG C of flash bakings, and the water evaporation in coating is fallen；
(8) catalyst roasts: drying rear catalyst being put into Muffle furnace, 550 DEG C of roasting 2h are cooled to after heat preservation
Room temperature；
Outer layer preparation and coating
(9) material weighs: by weight 0.3:0.68:0.02 weighing La-Al respectively2O3, 20%Ce content Ce-Zr
Solid solution, aluminium glue, are made into slurries, and being milled to granularity D90 is 12 μm；
(10) noble metal weighs: Rh is according to 22g/ft3It calculates, is calculated according to above-mentioned powder 200g, coated weight 80g/
L, according to the concentration of Rh, coated weight and total powder re-computation and the amount for weighing noble metal Rh, the amount of Rh is 17.673g；
(11) addition of noble metal Rh: noble metal Rh solution is added in the slurries of the 196g containing powder；
(12) aluminium glue is added: aluminium glue is added, is uniformly mixed；
(13) determination of solid content: step (12) slurries 10g, 575 DEG C of roasting 25min is taken to measure solidfied material content 28%；
(14) slurry coating coats: being coated with quantitatively coating special plane, catalyst carrier is placed at application chamber, is pressed
According to coated weight be 80g/L requirement and the wet weight gain of solid content calculating target measured is 86g, and the slurries calculated are added to slurry
In disk, quantitative coating is carried out, coating slurry is coated on carrier；
(15) catalyst is dried: the catalyst coated passes through 100 DEG C of flash bakings, and the water evaporation in coating is fallen；
(16) catalyst roasts: drying rear catalyst being put into Muffle furnace, 550 DEG C of roasting 2h are cooling after heat preservation
To room temperature.
Activity rating is carried out to catalyst prepared by embodiment three and comparative example, as a result as follows:
1, fresh state catalyst activity evaluation is investigated:
Test carries out in reacting furnace.Test method: NO, CO will be contained2、H2O、C3H6、C3H8, CO gaseous mixture be passed through height
In warm reacting furnace, wherein NO:820ppm, CO:1.5%, C3H8: 140ppm, C3H6: 280ppm, H2O:10%, CO2: 14%；It rises
Warm rate is 10 DEG C/min, is eventually raised to 500 DEG C.Test result is shown in Table 1
The fresh state catalyst activity evaluation result of table 1
As shown in Table 1, NO, C of catalyst prepared by embodiment three3H6Initiation temperature T50Respectively 217 DEG C and 218
DEG C, the initiation temperature T of CO50It is 254 DEG C, C3H8Initiation temperature T50It is 345 DEG C, T50It is below comparative catalyst.Wherein, T50
It is temperature to be achieved needed for reaching 50% conversion ratio, temperature more high-performance is poorer, and temperature more low performance is better.It can by table 1
To find out, the initiation temperature of catalyst prepared by preparation method of the present invention is lower, better catalytic activity.
2, heat ageing rear catalyst activity rating is investigated:
Pre-treatment: catalyst is placed in aging in tube furnace, oxidizing gas (1%O first2) and reducibility gas
(0.5%CO) is alternately passed through, and aging temperature is 1050 DEG C, ageing time 36h, then the NO in simulated automotive tail gas againX、CO
With the carry out activity investigation of HC.
Test is carried out in high temperature reaction stove.Test method: NO, CO will be contained2、H2O、C3H6、C3H8, CO gaseous mixture
It is passed through in high temperature reaction stove, wherein NO:820ppm, CO:1.5%, C3H8: 140ppm, C3H6: 280ppm, H2O:10%, CO2:
14%；Heating rate is 10 DEG C/min, is eventually raised to 500 DEG C.Test result is shown in Table 2.
2 aging catalyst Activity evaluation of table
From the data in table 2, it can be seen that NO, C of catalyst prepared by embodiment three3H6Initiation temperature T50Respectively 262 DEG C
With 279 DEG C or so, the initiation temperature T of CO50It is 284 DEG C, C3H8Initiation temperature T50It is 410 DEG C, and C in comparative example3H8Conversion ratio
Only 30%, these results indicate that the initiation temperature T of 3 indices of embodiment50It is below the catalyst of comparative example preparation.Its
In, T50It is temperature to be achieved needed for reaching 50% conversion ratio, temperature more high-performance is poorer, and temperature more low performance is better.Pass through
Table 2 is as can be seen that catalyst prepared by preparation method of the present invention initiation temperature after the high temperature ageing by the long period is more right
Ratio is low, better catalytic activity, and durability is good.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way.It is all according to the present invention
Essence any simple modification, change and equivalence change to the above embodiments, still fall within technical solution of the present invention
In protection scope.
Claims (9)
1. a kind of gasoline car three-way catalyst, which is characterized in that catalyst is using cordierite honeycomb ceramic as catalyst carrier, catalysis
The surface of agent carrier is coated with two layers of coating slurry containing precious metals pd and Rh, including primer coating and outer coating；
Wherein, primer coating includes Pd-Sr/La-Al2O3Powder and Pd/Ce-Zr solid solution powder, are made into slurries after mixing, add
Enter auxiliary agent and binder, be coated in catalyst carrier, forms primer coating；Outer coating includes Rh/Zr-Nb-Al2O3Powder
With Pd/Ce-Zr solid solution powder, slurries are made into after mixing, are coated on primer coating, outer coating is formed.
2. a kind of gasoline car three-way catalyst according to claim 1, which is characterized in that the auxiliary agent is simple substance Sr, Ba
Or one of La and its compound or a variety of, the binder are aluminium glue or zirconium glue.
3. a kind of preparation method of gasoline car three-way catalyst, which comprises the steps of:
Bottom preparation and coating:
(1) material weighs: distinguishing by weight 0.17 ~ 0.6: 0.3 ~ 0.75:0.01 ~ 0.1:0.01 ~ 0.05:0.01 ~ 0.05
Weigh La-Al2O3, Ce-Zr solid solution, Ba (AC)2、Sr(NO3)3·6H2O, aluminium glue；
(2) noble metal weighs: quality=Pd concentration of the Pd/28.316/ total powder weight of coated weight * bottom, wherein Pd's is dense
Degree: 5 ~ 150g/ft3, coated weight is 100 ~ 150g/L；
(3) precious metals pd-Sr/La-Al2O3The preparation of powder: taking 1/2 ~ 2/3 of Pd amount in step (2), by Sr (NO3)3·6H2O
It is dissolved in Pd (NO3)2In solution, and ethanol solution dilution is added, stirs 5 ~ 10h, incipient wetness impregnation is in La-AL2O3On, ageing 12 ~
36h；
(4) preparation of Pd/Ce-Zr solid solution powder: weighing 1/3 ~ 1/2 of Pd amount in step (2), by Pd (NO3)2Solution second
Alcoholic solution dilution, stirs 5 ~ 10h, and incipient wetness impregnation is aged 12 ~ 36h on Ce-Zr solid solution；
(5) Pd-Sr/La-Al2O3The processing of powder and Pd/Ce-Zr solid solution powder: powder body material in step (3) and (4) is dried
Dry, roasting, 100 ~ 150 DEG C of drying temperature, 5 ~ 15h of drying time, 450 ~ 550 DEG C of maturing temperature, 1 ~ 5h of calcining time；
(6) preparation of slurries: by treated in step (5) Pd-Sr/La-Al2O3Powder and Pd/Ce-Zr solid solution powder add
Enter in deionized water, load weighted Ba (AC) is added2And aluminium glue, it is in its solidfied material content between 35% ~ 40%, mixing is equal
It is even；
(7) ball milling of slurries: slurries pass through ball mill grinding, and the final granularity D90 of slurries is 7 ~ 25 μm；
(8) determination of solid content: taking slurries 10g in step (7), 550 ~ 600 DEG C of 20 ~ 30min of roasting, surveys solidfied material content；
(9) slurry coating coats: coating slurry being coated on carrier with quantitatively coating special plane, coated weight is 80 ~ 200g/L；
(10) catalyst is dried: the catalyst flash baking after coating, until catalyst quality no longer changes, drying temperature is
100~150℃；
(11) catalyst roasts: the catalyst after drying being put into Muffle furnace, 1 ~ 5h is roasted at 450 ~ 550 DEG C, heat preservation terminates
After be cooled to room temperature；
Outer layer preparation and coating:
(12) material weighs: weighing Zr- respectively by weight 0.35 ~ 0.7:0.2 ~ 0.6:0.01 ~ 0.1:0.01 ~ 0.05
Al2O3, Ce-Zr solid solution, C6H4NbO12And aluminium glue；
(13) Zr-Al2O3Modified preparation: by load weighted C in step (12)6H4NbO12Incipient wetness impregnation is in Zr-Al2O3On, it dries
Modified Zr-Nb-Al is made in dry, roasting2O3Powder；
(14) noble metal weighs: amount=Pd concentration of the Pd/28.316/ total powder weight of coated weight * outer layer, amount=Rh of Rh be dense
Spend/28.316/ total powder weight of coated weight * outer layer, wherein the concentration of Pd: 1 ~ 30g/ft3, the concentration of Rh: 1 ~ 60g/ft3, coating
Amount is 70 ~ 100g/L；
(15) noble metal Rh/Zr-Nb-Al2O3The preparation of powder: by the Rh (NO in step (14)3)3Solution ethanol solution is dilute
It releases, stirs 5 ~ 10h, incipient wetness impregnation is in Zr-Nb-Al2O3On, it is aged 12 ~ 36h；
(16) preparation of Pd/Ce-Zr solid solution powder: by Pd (NO in step (14)3)2Solution is diluted with ethanol solution, and stirring 5 ~
10h, incipient wetness impregnation are aged 12 ~ 36h on Ce-Zr solid solution；
(17) Rh/Zr-Nb-Al2O3The processing of powder and Pd/Ce-Zr solid solution powder: powder in step (15) and (16) is dried
Dry, roasting, 100 ~ 150 DEG C of drying temperature, 5 ~ 15h of drying time, 450 ~ 550 DEG C of maturing temperature, 1 ~ 5h of calcining time；
(18) preparation of slurries: the Rh/Zr-Nb-Al that will be handled well in step (17)2O3Powder and Pd/Ce-Zr solid solution powder
It is added in deionized water, load weighted aluminium glue is added, be in its solidfied material content between 28% ~ 35%, be uniformly mixed；
(19) ball milling of slurries: slurries pass through ball mill grinding, and the final granularity of slurries to D90 is 7 ~ 25 μm；
(20) determination of solid content: taking step (19) slurries 10g, 550 ~ 600 DEG C of 20 ~ 30min of roasting, surveys solidfied material content；
(21) slurry coating coats: coating slurry being coated on carrier with quantitatively coating special plane, coated weight is 70 ~ 100g/L；
(22) catalyst is dried: the catalyst flash baking after coating, until catalyst quality no longer changes, drying temperature is
100~150℃；
(23) catalyst roasts: drying rear catalyst being put into Muffle furnace, 450 ~ 550 DEG C of roasting 1 ~ 5h are cold after heat preservation
But to room temperature.
4. a kind of preparation method of gasoline car three-way catalyst according to claim 3, which is characterized in that the step
(1) La-Al in2O3The mass content of middle La is 1% ~ 4%.
5. a kind of preparation method of gasoline car three-way catalyst according to claim 3, which is characterized in that the step
(2) quality of the precious metal palladium in occupies the 85% ~ 98% of Pd total amount.
6. a kind of preparation method of gasoline car three-way catalyst according to claim 3, which is characterized in that the step
(3) quality of the precious metal palladium in occupies the 40% ~ 66% of Pd total amount.
7. a kind of preparation method of gasoline car three-way catalyst according to claim 3, which is characterized in that the step
(4) quality of the precious metal palladium in occupies the 25% ~ 50% of Pd total amount.
8. a kind of preparation method of gasoline car three-way catalyst according to claim 3, which is characterized in that step (1) and
(12) Ce mass content is 25% ~ 60% in Ce-Zr solid solution in, Zr-Al in step (12)2O3Zr mass content be 5% ~ 60%.
9. a kind of preparation method of gasoline car three-way catalyst according to claim 3, which is characterized in that step (1) and
(12) the aluminium glue solidfied material mass content in is 10%.
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