CN100448541C - High specific surface area alumina coating preparation method and coating prepared therefrom and metal carrier three-effect catalyzing device - Google Patents
High specific surface area alumina coating preparation method and coating prepared therefrom and metal carrier three-effect catalyzing device Download PDFInfo
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- CN100448541C CN100448541C CNB2006101650943A CN200610165094A CN100448541C CN 100448541 C CN100448541 C CN 100448541C CN B2006101650943 A CNB2006101650943 A CN B2006101650943A CN 200610165094 A CN200610165094 A CN 200610165094A CN 100448541 C CN100448541 C CN 100448541C
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Abstract
The specific high surface area of alumind coating features in the paste preparation by grinding alumind and batching for pastes with 0.2-1% organic alcohol agglomerate surface activator, with even blending for use, coating said alumind to carrier surface, through drying, baking and aging treatment to make the coating. It also provides the alumind coating and metal carrier three functions catalysts. The coating is in crust, big in specific surface area, stable and reliable in performance.
Description
Technical field
The present invention relates to the aluminum oxide coating technology of preparing, the coating that particularly relates to a kind of high-specific surface area aluminum oxide coating preparation method and prepare, and the metal carrier triple-effect catalytic unit that adopts this method to produce with aluminum oxide coating with this method.
Background technology
Catalyst all need in order to enlarge the contact area of catalyst and catalytic specie as far as possible, require its carrier to have bigger specific area attached to carrying out catalytic action on certain catalyst carrier mostly.
Alundum (Al is that aluminum oxide coating layer has bigger specific area characteristic, is one of mounting medium the most frequently used in the catalyst preparation technology, utilizes the aluminium oxide of different phases, can prepare the catalyst coat of different structure and composition.Aluminium oxide commonly used mainly contains two kinds on α type and γ type, and the aluminium oxide that wherein is used for the motor-vehicle tail-gas process field mainly is the γ type.
Catalyst need carry out high-temperature roasting usually in preparation process, aluminum oxide coating after high-temperature roasting, sintering phenomenon appears easily, this situation generally can cause the specific area of aluminum oxide coating sharply to descend, thereby influence the catalytic effect of catalyst, limited the application of alundum (Al dramatically as catalyst carrier.
If can make aluminum oxide coating through after the high-temperature roasting, still can keep its original specific area to greatest extent, then will improve the application performance of aluminum oxide coating greatly as catalyst carrier, also can improve the serviceability of catalyst simultaneously.The improvement of this performance for existing with the aluminum oxide coating be catalyst carrier the field particularly the triple-effect catalytic unit in the automotive field produce active influence.
Summary of the invention
One object of the present invention is to provide a kind of method for preparing aluminum oxide coating, to solve in the practical application aluminum oxide coating after high-temperature roasting, sintering phenomenon takes place and reduce the specific area characteristic of coating.
Another object of the present invention is to provide a kind of aluminum oxide coating that utilizes method for preparing, though the aluminum oxide coating that utilizes this method preparation is still kept the characteristics of high-specific surface area through sintering processes.
Another object of the present invention is to provide a kind of metal carrier triple-effect catalytic unit with aluminum oxide coating that utilizes said method and utilize this method preparation, and this catalyst converter has overcome the defective that easily causes sintering phenomenon in traditional triple-effect catalytic unit field after the aluminum oxide coating roasting and reduce its specific area.
Technical scheme of the present invention is:
A kind of method for preparing the high-specific surface area aluminum oxide coating is characterized in that: described preparation method comprises the steps:
A, preparation slurry:, be ground to grain fineness after mixing less than 20 microns by weight with 240 parts of alundum (Al powders, 20 parts of glacial acetic acids, 8 parts of barium monoxide, 210 parts of pure water; Add 5～10 parts of lanthanum nitrates, 3～5 parts of cobalt nitrates, 0.8～1.2 part of strontium nitrate, grind and disperse; It is 4.5～7 that adding alkali lye is adjusted to pH value; Press 0.2～1% of slurry total amount and add the organic alcohols copolymer surfactants, stir;
B, preparation coating: aforementioned alundum (Al slurry is coated on carrier surface, and drying, roast and burin-in process.
Oven dry is slowly oven dry 1.5～3 hours in the temperature environment below 120 ℃ among the described step b.
The load capacity that described alundum (Al slurries apply is 12%～20%.
Described roasting comprises: preroast is 1～3 hour under the temperature environment prior to 250～350 ℃; Constant temperature calcining 1～3 hour under 500～700 ℃ temperature environment again; Quick aging 4 hours under 1000 ℃ temperature environment then.
A kind of aluminum oxide coating is characterized in that: described aluminum oxide coating is for adopting aforesaid method preparation.
A kind of metal carrier triple-effect catalytic unit comprises the metallic carrier of triple-effect catalytic unit itself, and it is characterized in that: described metallic carrier is provided with foregoing aluminum oxide coating.
Be impregnated with load capacity on the described aluminum oxide coating and be the blending constituent of 1%～10% palladium, platinum, rhodium, its weight ratio is a palladium: platinum: rhodium=10: 2: 1, and through 500～700 ℃ of roastings.
Technique effect of the present invention is as follows:
The technical scheme that preparation method of the present invention adopted is by in the alundum (Al material of routine, special surfactant---organic alcohols copolymer surfactants mixes, this surfactant can form nano level mixed structure with alundum (Al, this mixed structure is through after the high-temperature roasting, wherein surfactant will break away from from the alundum (Al structure, thereby can guarantee the regularity of aluminum oxide coating on nanostructured, the aluminum oxide coating of this regular nanostructured is compared with traditional preparation method's gained, not only specific area obviously increases, can improve the distribution of the catalyst activity composition that is attached to coating surface, increase the reaction surface of catalytic reaction, make the reaction probability of catalyst and reacting gas increase, thus the corresponding task performance that improves catalyst; And the coating of this regular texture is when the attached catalyst active component, the even distribution that can keep active component, the defective that contact action is inhomogeneous, catalytic effect is not good when having overcome the configuration of surface that the aluminum oxide coating of conventional method preparation can't formation rule, the active component skewness that adheres to, catalytic reaction.
The aluminum oxide coating that preparation method of the present invention is prepared detects through adopting the BET method, the coating material before and after its burin-in process, and its specific area is as shown in the table.
| State | Fresh sample | Aging back sample |
| Specific area m 2/g | 220 | 180 |
Wherein, fresh sample is the product of producing according to normal process without burin-in process.
Utilize the aluminum oxide coating triple-effect catalytic unit of preparation method's preparation of the present invention, the good characteristic that has above-mentioned coating fully, it does the ignition temperature characterisitic respectively under the condition that simulates real real machine car discharging waste gas is formed and purifying rate detects, and detects data shown in following table 1,2:
1) detection of initiation temperature
| The sample initiation temperature | CO | HC | NOx |
| Fresh sample ℃ | 196.5 | 218 | 240 |
| Aged samples ℃ | 200 | 215 | 244 |
2) detection of purifying rate
| The sample initiation temperature | CO | HC | NOx |
| Fresh sample % | 99 | 98.5 | 100 |
| Aged samples % | 95.8 | 96 | 100 |
The contrast testing result, the aluminum oxide coating layer that adopts this method to prepare, through the high temperature quick aging, its specific area still can keep higher specific surface area, and decline scope is 18.18%, and from catalytic activity, aging front and back remain unchanged substantially.This shows that the aluminum oxide coating and the triple effect metallic carrier catalyst converter thereof that utilize the present invention to prepare through after the quick aging, still have higher specific surface area and catalytic activity.
Description of drawings
The specific embodiment
1, prepare raw material:
Aluminium oxide, barium monoxide, contain lanthanum cerium zirconium sosoloid, organic alcohols copolymer surfactants, lanthanum nitrate, strontium nitrate, cobalt nitrate.Wherein aluminium oxide is that specific area is 200～250m
2The commodity of/g, SASOL company in South Africa is on sale; Contain the lanthanum cerium zirconium sosoloid: the Rare Earth Company commercial goods is ground in Beijing; The organic alcohols copolymer surfactants, present embodiment adopts the diethylene glycol copolymer; It is pure that above-mentioned all kinds of chemical material quality is analysis.
2, preparation process:
2.1, pulp preparation
Accurately take by weighing 240 parts of alumina powders, 20 parts of glacial acetic acids, 8 parts of barium monoxide, 210 parts of pure water according to weight ratio, mix and be placed in the high-speed grinder, be ground to grain fineness at a high speed and after 20 microns, add 5～10 parts of lanthanum nitrates, 3～5 parts of cobalt nitrates, 0.8～1.2 part of strontium nitrate, take out after 1 hour through grinding dispersion, add 25% alkali lye and adjust the pH value of gained slurry between 4.5～7, press 0.2～1% of slurry total amount again and add the organic alcohols copolymer surfactants, the back that stirs is standby.
2.2, the preparation of coating: with the alumina slurry that regulates, the method that the pool is soaked in employing is coated on carrier surface, be lower than the slowly oven dry through 1.5～3 hours under 120 ℃ of conditions then, preroast after 1～3 hour under 250～350 ℃ of conditions again, be warmed up to 500～700 ℃, constant temperature calcining 1～3 hour got final product 1000 ℃ of quick agings then in 4 hours.
Adopt the BET method to detect, the pulverulent material of aging front and back, its specific area is as shown in the table.
| State | Fresh sample | Aging back sample |
| Specific area m 2/g | 220 | 180 |
If the preparation metal carrier triple-effect catalytic unit applies metal beehive carrier with method with the alumina slurry that regulates, load capacity is controlled at 12%～20% scope, and subsequent heat treatment condition method is the same; With the metallic honeycomb substrate that is coated with aluminum oxide coating of heat treatment gained, dipping Pd: Pt: Rh=10: 2: 1 noble metal, control its load capacity in 1%～10% scope, after 500～700 ℃ of roastings, be the metal carrier triple-effect catalytic unit finished product.
Prepared catalyst converter is done ignition temperature characterisitic and purifying rate respectively and is detected under the condition that simulates real real machine car discharging waste gas is formed.Data are as shown in the table:
1) detection of initiation temperature
| The sample initiation temperature | CO | HC | NOx |
| Fresh sample ℃ | 196.5 | 218 | 240 |
| Aged samples ℃ | 200 | 215 | 244 |
2) detection of purifying rate
| The sample initiation temperature | CO | HC | NOx |
| Fresh sample % | 99 | 98.5 | 100 |
| Aged samples % | 95.8 | 96 | 100 |
Wherein, fresh sample is the product of producing according to normal process without burin-in process.
The contrast testing result as can be seen, adopts the aluminum oxide coating of the metal carrier triple-effect catalytic unit of this method preparation, and through the high temperature quick aging, its specific area still can keep higher specific surface area, and decline scope is 18.18%; From catalytic activity, aging front and back catalytic activity remains unchanged substantially.
Claims (7)
1, a kind of method for preparing the high-specific surface area aluminum oxide coating, it is characterized in that: described preparation method comprises the steps:
A, preparation slurry:, be ground to grain fineness after mixing less than 20 microns by weight with 240 parts of alundum (Al powders, 20 parts of glacial acetic acids, 8 parts of barium monoxide, 210 parts of pure water; Add 5～10 parts of lanthanum nitrates, 3～5 parts of cobalt nitrates, 0.8～1.2 part of strontium nitrate, grind and disperse; It is 4.5～7 that adding alkali lye is adjusted to pH value; Press 0.2～1% of slurry total amount and add the organic alcohols copolymer surfactants, stir;
B, preparation coating: aforementioned alundum (Al slurry is coated on carrier surface, and drying, roast and burin-in process.
2, a kind of method as claimed in claim 1 is characterized in that: oven dry is slowly oven dry 1.5～3 hours in the temperature environment below 120 ℃ among the described step b.
3, a kind of method as claimed in claim 2 is characterized in that: the load capacity that described alundum (Al slurries apply is 12%～20%.
4, a kind of method as claimed in claim 3, it is characterized in that: described roasting comprises: preroast is 1～3 hour under the temperature environment prior to 250～350 ℃; Constant temperature calcining 1～3 hour under 500～700 ℃ temperature environment again; Quick aging 4 hours under 1000 ℃ temperature environment then.
5, a kind of aluminum oxide coating is characterized in that: described aluminum oxide coating is for adopting the method for claim 1 preparation.
6, a kind of metal carrier triple-effect catalytic unit comprises the metallic carrier of triple-effect catalytic unit itself, and it is characterized in that: described metallic carrier is provided with aluminum oxide coating as claimed in claim 5.
7, a kind of metal carrier triple-effect catalytic unit as claimed in claim 6, it is characterized in that: the blending constituent that is impregnated with load capacity on the described aluminum oxide coating and is 1%～10% palladium, platinum, rhodium, its weight ratio is a palladium: platinum: rhodium=10: 2: 1, and through 500～700 ℃ of roastings.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006101650943A CN100448541C (en) | 2006-12-13 | 2006-12-13 | High specific surface area alumina coating preparation method and coating prepared therefrom and metal carrier three-effect catalyzing device |
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| CNB2006101650943A CN100448541C (en) | 2006-12-13 | 2006-12-13 | High specific surface area alumina coating preparation method and coating prepared therefrom and metal carrier three-effect catalyzing device |
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| CN1970152A CN1970152A (en) | 2007-05-30 |
| CN100448541C true CN100448541C (en) | 2009-01-07 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110479252A (en) * | 2019-08-23 | 2019-11-22 | 西安交通大学 | A kind of preparation method for the catalyst coating multistage γ-aluminum oxide coating |
| CN110672653B (en) * | 2019-10-24 | 2022-12-02 | 浙江达峰汽车技术有限公司 | Method for simulating aging of automobile exhaust purification catalyst |
| CN112892546B (en) * | 2019-12-03 | 2022-04-29 | 中国科学院大连化学物理研究所 | Honeycomb metal, preparation method and application of honeycomb metal as catalyst carrier |
| CN114618513B (en) * | 2020-12-10 | 2023-07-25 | 中国科学院大连化学物理研究所 | Integral metal honeycomb ozone decomposition catalyst, preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045549C (en) * | 1993-11-26 | 1999-10-13 | 中国科学技术大学 | Three-effect catalyst and preparing method containing copper and lanthanum-oxides, platinum and rhodium |
| CN1171682C (en) * | 2002-02-07 | 2004-10-20 | 中国石油化工股份有限公司 | Coating method of automobile tail gas purifying catalyst |
| CN1179792C (en) * | 2002-04-26 | 2004-12-15 | 中国石油化工股份有限公司 | Method of loading automobile tail gas purifying catalyst onto honeycomb carrier |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045549C (en) * | 1993-11-26 | 1999-10-13 | 中国科学技术大学 | Three-effect catalyst and preparing method containing copper and lanthanum-oxides, platinum and rhodium |
| CN1171682C (en) * | 2002-02-07 | 2004-10-20 | 中国石油化工股份有限公司 | Coating method of automobile tail gas purifying catalyst |
| CN1179792C (en) * | 2002-04-26 | 2004-12-15 | 中国石油化工股份有限公司 | Method of loading automobile tail gas purifying catalyst onto honeycomb carrier |
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