CN100588460C - Double layer noble metal active component catalyst and preparing method thereof - Google Patents
Double layer noble metal active component catalyst and preparing method thereof Download PDFInfo
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- CN100588460C CN100588460C CN200810057679A CN200810057679A CN100588460C CN 100588460 C CN100588460 C CN 100588460C CN 200810057679 A CN200810057679 A CN 200810057679A CN 200810057679 A CN200810057679 A CN 200810057679A CN 100588460 C CN100588460 C CN 100588460C
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Abstract
The invention provides a dual-layer noble metal active component catalyst, wherein the active component is distributed in lamination, and a dual-layer coating method is adopted to separate the activecomponents of noble metal and lead the active components to stay on different layers to play individual functions fully. Not only the resistance to aging at high temperature of catalyst can be satisfied but also the catalytic reduction ability of nitrogen oxide under lean-burn condition can be improved and the ignition temperature of the catalyst can be reduced, thus greatly improving the utilization of active component.
Description
Technical field
The present invention relates to a kind of noble metal catalyst, specifically, relate to a kind of double layer noble metal active component catalyst and preparation method thereof, described catalyst contains noble metal active component first coating and noble metal active component second coating.
Background technology
Three-way catalyst is meant and can the CO in the motor vehicle exhaust gases, HC and NOx be changed into non-harmful steam H by catalytic oxidation and catalytic reduction reaction
2O, nitrogen N
2With carbon dioxide CO
2Deng.Along with further adding of Abgasgesetz is tight, three-way catalyst is proposed harsher requirement, for reducing engine at the cold-start phase pollutant discharge amount, require catalyst to be installed in from the nearer position of engine exhaust port, catalyst need have better resistance to elevated temperatures; For improving the engine fuel economy, require exploitation lean-burn type three-way catalyst, three-way catalyst only could carry out catalytic purification effectively to three kinds of major pollutants (HC, CO and Nox) of exhaust contaminant simultaneously when theoretical air-fuel ratio, during lean-burn in the exhaust oxygen excessive, to oxidize away most reducing agents (HC and CO) in the catalyst surface excess of oxygen, thereby suppress catalyst the NOx catalytic reduction.Therefore, three-way catalyst requires to have following feature: high-temperature aging resisting performance preferably; Low initiation temperature; Catalytic reduction ability to nitrogen oxide under the lean burn conditions is strong.
Precious metals pd, Pt, Rh are widely used in three-way catalyst as active constituent.The Pd catalyst has good active to the oxidation of HC in three kinds of noble metals, and high-temperature resistance is also stronger, is better than Pt and Rh, but anti-poisoning capability is relatively poor, especially to SO
2Poison relatively more responsive with plumbous Pb.Noble Metal Rhodium Rh is higher to the reducing activity of nitrogen oxide NOx, but at high temperature easy and Pd generation alloy reduces its catalytic activity greatly.
Summary of the invention
The purpose of this invention is to provide a kind of double layer noble metal active component catalyst, active constituent distributes at the catalyst higher slice, brings into play different effects, thereby improves the utilization rate of active constituent greatly.
Another object of the present invention provides a kind of preparation method of double layer noble metal active component catalyst.
In order to realize the object of the invention, a kind of double layer noble metal active component catalyst of the present invention, its active constituent is layer distributed, adopts the preparation of double-coating coating method, and its preparation process comprises the steps:
1) activated alumina, cerium zirconium sosoloid and nitric acid are mixed, add water then and carry out ground and mixed, controlling total solid content is 30～60%, makes alumina slurry C0;
2) then carrier is immersed slurry C 0 after, take out, blow most residual slurry, dry and roasting, make semi-finished product G0;
3) getting concentration is 20～30% palladium salting liquid P0, and above-mentioned catalyst semi-finished product G0 be impregnated among the palladium salting liquid P0, takes out, and blows off raffinate, and catalyst semi-finished product G1 is made in roasting;
4) catalyst semi-finished product G1 is immersed in the slurry C 0 again, take out, blow most residual slurry, semi-finished product G2 is made in oven dry and roasting;
5) getting concentration is 20～30%, and the solution P1 of the solution P1 of Pt: Rh=5～10: 1 impregnated in above-mentioned catalyst semi-finished product G2 among the active constituent solution P1, takes out, and blows off raffinate, and roasting forms.
Wherein, the weight proportion of activated alumina, cerium zirconium sosoloid and nitric acid is in the step 1): 20～50: 5～10: 0.3～1.Described water is deionized water.
The time of described ground and mixed is 3～12hrs.
Step 2) carrier described in is metal or ceramic honeycomb carrier, and carrier must carry out preliminary treatment through processes such as cleaning, oxidation or dryings before use.
The time that carrier immerses in the slurry C 0 is 3～15s.
Bake out temperature is 80～120 ℃, and the time is 1～3h; Sintering temperature is 500～750 ℃, and the time is 1～4h.
The salt of palladium described in the step 3) is palladium nitrate or palladium.
The time of catalyst semi-finished product G0 dipping is 5～25 minutes.
Sintering temperature is 300～500 ℃, and the time is 1～3hrs.
The time of immersing slurry C 0 in the step 4) is 3～15s.
Bake out temperature is 80～120 ℃, and the time is 1～3h; Sintering temperature is 500～750 ℃, and the time is 1～4h.
The time of catalyst semi-finished product G2 dipping is 5～25 minutes in the step 5), and sintering temperature is 300～500 ℃, and the time is 1～3hrs.
Blowing off raffinate can adopt the compressed air of 0.15～0.25MPa to carry out; Blowing off residual slurry can adopt the compressed air of 0.25～0.45MPa to carry out.
In order to realize another purpose of the present invention, the preparation method of a kind of double layer noble metal active component catalyst of the present invention comprises the steps:
1) activated alumina, cerium zirconium sosoloid and nitric acid are mixed, add water then and carry out ground and mixed, controlling total solid content is 30～60%, makes alumina slurry C0;
2) then carrier is immersed slurry C 0 after, take out, blow most residual slurry, dry and roasting, make semi-finished product G0;
3) getting concentration is 20～30% palladium salting liquid P0, and above-mentioned catalyst semi-finished product G0 be impregnated among the palladium salting liquid P0, takes out, and blows off raffinate, and catalyst semi-finished product G1 is made in roasting;
4) catalyst semi-finished product G1 is immersed in the slurry C 0 again, take out, blow most residual slurry, semi-finished product G2 is made in oven dry and roasting;
5) getting concentration is 20～30%, and the solution P1 of Pt: Rh=5～10: 1 impregnated in above-mentioned catalyst semi-finished product G2 among the active constituent solution P1, takes out, and blows off raffinate, and roasting forms.
Specifically, the preparation method of double layer noble metal active component catalyst of the present invention comprises the steps:
1) 20～50 parts of activated aluminas, 5～10 parts of cerium zirconium sosoloids, 0.3～1 part in nitric acid and deionized water are carried out ground and mixed 3～12hrs, make alumina slurry C0, the total solid content of control slurry is 30～60%;
(2) will immerse in the slurry C 0 behind 3～15s through the metal of pre-treatment or ceramic honeycomb carrier, take out, with the compressed air of 0.25～0.45MPa, blow most residual slurry, 80～120C is dried 1～3h, and 500～750 ℃ of roasting 1～4h make semi-finished product G0 in the calcining kiln;
(3) getting concentration is 20～30% palladium salting liquid P0, above-mentioned catalyst semi-finished product G0 be impregnated among the palladium salting liquid P0 5～25 minutes, take out, blow off raffinate with the compressed air of 0.15～0.25MPa, 300～500 ℃ of roasting 1～3hrs make catalyst semi-finished product G1;
(4) catalyst semi-finished product G1 is immersed again in the slurry C 0 behind 3～15s, take out, compressed air with 0.25～0.45MPa, blow most residual slurry, put into 80～120 ℃ of oven dry of net belt type continuous drying kiln, 1～3h, 500～750 ℃ of roasting 1～4h in the calcining kiln make semi-finished product (having uploaded coating) G2;
(5) getting concentration is 20～30%, the solution P1 of Pt: Rh=5～10: 1, above-mentioned catalyst semi-finished product G2 be impregnated among the active constituent solution P1 5～25 minutes, take out, compressed air with 0.15～0.25MPa blows off raffinate, and 300～500 ℃ of roasting 1～3hrs make the double-deck catalyst that applies.
The present invention adopts precious metals pd is loaded on the ground floor of catalyst, and Pt and Rh are carried on the second layer of catalyst, active constituent is distributed at the catalyst higher slice, bring into play different effects, both can satisfy the high-temperature aging resisting performance of catalyst, can improve under the lean burn conditions catalytic reduction ability again, reduce the initiation temperature of catalyst, thereby improve the utilization rate of active constituent greatly nitrogen oxide.
The specific embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
The double layer noble metal active component catalyst of present embodiment is made by following steps:
(1) takes by weighing activated alumina 40kg, cerium zirconium sosoloid 7kg, nitric acid 1kg and deionized water 52kg, put into ball grinder ball milling 5h, make alumina slurry C0.
(2) will clean, the metal beehive carrier after the oxidation (
35 * 100 * 100 metallic carriers) be dipped in 10s in the above-mentioned slurry, take out the back and blow most residual slurry with 0.4MPa compressed air, the control content of metal is 50g/ft
3, put into 105 ℃ of oven dry of net belt type continuous drying kiln 3h; 500 ℃ of roasting 1h make semi-finished product G0 in the calcining kiln.
(3) getting concentration is 25% palladium nitrate solution P0, and above-mentioned catalyst semi-finished product be impregnated in wherein 5 minutes, takes out, and blows off raffinate with the compressed air of 0.25MPa.500 ℃ of roasting 2hrs naturally cool to room temperature in the calcining kiln, make catalyst semi-finished product G1.
(4) catalyst semi-finished product G1 is immersed in the slurry C 0 behind the 15s again, take out, the compressed air with 0.45MPa blows most residual slurry, puts into 105 ℃ of oven dry of net belt type continuous drying kiln 3h; 500 ℃ of roasting 1h make semi-finished product G2 in the calcining kiln.
(5) get concentration be 30% active constituent (Pt/Rh=5: 1) nitrate solution P1, above-mentioned catalyst semi-finished product G2 be impregnated in wherein 5 minutes, take out, blow off raffinate with the compressed air of 0.25MPa, the control content of metal is 30g/ft
3, 500 ℃ of roasting 2hrs naturally cool to room temperature in the calcining kiln, make the double-deck catalyst that applies, and are designated as A.
Comparative Examples 1
In order to compare with three-way catalyst of the present invention, adopt known method to prepare the identical three-way catalyst of component proportioning, concrete steps are as follows:
(1) takes by weighing activated alumina 40kg, cerium zirconium sosoloid 7kg, nitric acid 1kg and deionized water 52kg, put into ball grinder ball milling 5h, make alumina slurry.
(2) metal beehive carrier that preliminary treatment is good (
35 * 100 * 100 metallic carriers) be dipped in 10s in the above-mentioned slurry, take out the back and blow most residual slurry, put into 105 ℃ of oven dry of net belt type continuous drying kiln 3h with 0.4MPa compressed air; 500 ℃ of roasting 1h make semi-finished product in the calcining kiln.
(3) compound concentration is noble metal (Pd/Pt/Rh=5: 2: 1) the solution P0 of 20-30%, and above-mentioned catalyst semi-finished product be impregnated in wherein 5 minutes, takes out, and blows off raffinate with the compressed air of 0.15-0.25MPa, and the control content of metal is 80g/ft
3500 ℃ of roasting 2hrs naturally cool to room temperature in the calcining kiln, make catalyst, are designated as B.
The catalyst activity that makes in embodiment 1 and the Comparative Examples 1 is detected, and the gained result is as shown in the table:
| Catalyst | CO T 50/℃ | NOx T 50/℃ | HC T 50/℃ |
| A | 214 | 217 | 231 |
| B | 218 | 233 | 240 |
Catalyst A, B after 10 hours, are detected its catalyst activity at 1100 ℃ of high temperature sinterings:
| Catalyst | CO T50/℃ | NOx T50/℃ | HC T50/℃ |
| A | 273 | 271 | 266 |
| B | 292 | 287 | 269 |
By the result of the foregoing description as can be known, this catalyst low-temperature activity is good, still can keep advantages of high catalytic activity and stability at 1100 ℃ of high temperature ageings after 10 hours, shows triple effect activity preferably.
Embodiment 2
The double layer noble metal active component catalyst of present embodiment is made by following steps:
(1) takes by weighing activated alumina 50kg, cerium zirconium sosoloid 5kg, nitric acid 0.5kg and deionized water 44.5kg, put into ball grinder ball milling 3h, make alumina slurry C0.
(2) will clean, dried ceramic honeycomb carrier (
35 * 100 * 100 ceramic monoliths) be dipped in 15s in the above-mentioned slurry, take out the back and blow most residual slurry with 0.45MPa compressed air, the control content of metal is 50g/ft
3, put into 80 ℃ of oven dry of net belt type continuous drying kiln 2h; 600 ℃ of roasting 3h make semi-finished product G0 in the calcining kiln.
(3) getting concentration is 30% palladium solution P0, and above-mentioned catalyst semi-finished product be impregnated in wherein 20 minutes, takes out, and blows off raffinate with the compressed air of 0.15MPa.300 ℃ of roasting 3hrs naturally cool to room temperature in the calcining kiln, make catalyst semi-finished product G1.
(4) catalyst semi-finished product G1 is immersed in the slurry C 0 behind the 10s again, take out, the compressed air with 0.25MPa blows most residual slurry, puts into 120 ℃ of oven dry of net belt type continuous drying kiln 1h; 750 ℃ of roasting 2h make semi-finished product G2 in the calcining kiln.
(5) get concentration be 20% active constituent (Pt/Rh=10: 1) nitrate solution P1, above-mentioned catalyst semi-finished product G2 be impregnated in wherein 20 minutes, take out, blow off raffinate with the compressed air of 0.20MPa, the control content of metal is 30g/ft
3, 400 ℃ of roasting 3hrs naturally cool to room temperature in the calcining kiln, make the double-deck catalyst that applies.
Embodiment 3
The double layer noble metal active component catalyst of present embodiment is made by following steps:
(1) takes by weighing activated alumina 20kg, cerium zirconium sosoloid 10kg, nitric acid 0.3kg and deionized water 69.7kg, put into ball grinder ball milling 12h, make alumina slurry C0.
(2) will clean, the metal beehive carrier after the oxidation (
35 * 100 * 100 metallic carriers) be dipped in 3s in the above-mentioned slurry, take out the back and blow most residual slurry with 0.25MPa compressed air, the control content of metal is 50g/ft
3, put into 120 ℃ of oven dry of net belt type continuous drying kiln 1h; 750 ℃ of roasting 4h make semi-finished product G0 in the calcining kiln.
(3) getting concentration is 20% palladium nitrate solution P0, and above-mentioned catalyst semi-finished product be impregnated in wherein 25 minutes, takes out, and blows off raffinate with the compressed air of 0.20MPa.450 ℃ of roasting 1hrs naturally cool to room temperature in the calcining kiln, make catalyst semi-finished product G1.
(4) catalyst semi-finished product G1 is immersed in the slurry C 0 behind the 3s again, take out, the compressed air with 0.35MPa blows most residual slurry, puts into 80 ℃ of oven dry of net belt type continuous drying kiln 2h; 600 ℃ of roasting 4h make semi-finished product G2 in the calcining kiln.
(5) get concentration be 25% active constituent (Pt/Rh=6: 1) acetate solution P1, above-mentioned catalyst semi-finished product G2 be impregnated in wherein 25 minutes, take out, blow off raffinate with the compressed air of 0.15MPa, the control content of metal is 30g/ft
3, 300 ℃ of roasting 1hrs naturally cool to room temperature in the calcining kiln, make the double-deck catalyst that applies.
Though above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a double layer noble metal active component catalyst is characterized in that, its active constituent is layer distributed, adopts the preparation of double-coating coating method, and its preparation process comprises the steps:
1) activated alumina, cerium zirconium sosoloid and nitric acid are mixed, add water then and carry out ground and mixed, controlling total solid content is 30～60%, makes alumina slurry C0;
2) then carrier is immersed slurry C 0 after, take out, blow most residual slurry, dry and roasting, make semi-finished product G0;
3) getting concentration is 20～30% palladium salting liquid P0, and above-mentioned catalyst semi-finished product G0 be impregnated among the palladium salting liquid P0, takes out, and blows off raffinate, and catalyst semi-finished product G1 is made in roasting;
4) catalyst semi-finished product G1 is immersed in the slurry C 0 again, take out, blow most residual slurry, semi-finished product G2 is made in oven dry and roasting;
5) getting concentration is 20～30%, and the solution P1 of Pt: Rh=5～10: 1 impregnated in above-mentioned catalyst semi-finished product G2 among the active constituent solution P1, takes out, and blows off raffinate, and roasting forms.
2. double layer noble metal active component catalyst according to claim 1 is characterized in that the weight proportion of activated alumina in the step 1), cerium zirconium sosoloid and nitric acid is: 20～50: 5～10: 0.3～1.
3. double layer noble metal active component catalyst according to claim 1 and 2 is characterized in that, the time of catalyst semi-finished product G0 dipping is 5～25 minutes in the step 3).
4. double layer noble metal active component catalyst according to claim 3 is characterized in that, sintering temperature is 300～500 ℃ in the step 3), and the time is 1～3 hour.
5. according to claim 1 or 2 described double layer noble metal active component catalysts, it is characterized in that the time of immersing slurry C 0 in the step 4) is 3～15 seconds.
6. according to the described double layer noble metal active component catalyst of claim 5, it is characterized in that bake out temperature is 80～120 ℃ in the step 4), the time is 1～3 hour; Sintering temperature is 500～750 ℃, and the time is 1～4 hour.
7. according to claim 1 or 2 described double layer noble metal active component catalysts, it is characterized in that the time of catalyst semi-finished product G2 dipping is 5～25 minutes in the step 5),
8. double layer noble metal active component catalyst according to claim 7 is characterized in that, sintering temperature is 300～500 ℃ in the step 5), and the time is 1～3 hour.
9. a method for preparing any described double layer noble metal active component catalyst of claim 1-7 is characterized in that, comprises the steps:
1) activated alumina, cerium zirconium sosoloid and nitric acid are mixed, add water then and carry out ground and mixed, controlling total solid content is 30～60%, makes alumina slurry C0;
2) then carrier is immersed slurry C 0 after, take out, blow most residual slurry, dry and roasting, make semi-finished product G0;
3) getting concentration is 20～30% palladium salting liquid P0, and above-mentioned catalyst semi-finished product G0 be impregnated among the palladium salting liquid P0, takes out, and blows off raffinate, and catalyst semi-finished product G1 is made in roasting;
4) catalyst semi-finished product G1 is immersed in the slurry C 0 again, take out, blow most residual slurry, semi-finished product G2 is made in oven dry and roasting;
5) getting concentration is 20～30%, and the solution P1 of Pt: Rh=5～10: 1 impregnated in above-mentioned catalyst semi-finished product G2 among the active constituent solution P1, takes out, and blows off raffinate, and roasting forms.
10. the preparation method of double layer noble metal active component catalyst according to claim 9 is characterized in that, comprises the steps:
1) 20～50 parts of activated aluminas, 5～10 parts of cerium zirconium sosoloids, 0.3～1 part in nitric acid and deionized water were carried out ground and mixed 3～12 hours, make alumina slurry C0, the total solid content of control slurry is 30～60%;
(2) will immerse in the slurry C 0 behind 3～15s through the metal of pre-treatment or ceramic honeycomb carrier, take out, with the compressed air of 0.25～0.45MPa, blow most residual slurry, 80～120 ℃ of oven dry 1～3 hour, 500～750 ℃ of roastings are 1～4 hour in the calcining kiln, make semi-finished product G0;
(3) getting concentration is 20～30% palladium salting liquid P0, above-mentioned catalyst semi-finished product G0 be impregnated among the palladium salting liquid P0 5～25 minutes, take out, blow off raffinate with the compressed air of 0.15～0.25MPa, catalyst semi-finished product G1 is made in 300～500 ℃ of roastings 1～3 hour;
(4) catalyst semi-finished product G1 is immersed in the slurry C 0 after 3～15 seconds again, take out, with the compressed air of 0.25～0.45MPa, blow most residual slurry, put into 80～120 ℃ in net belt type continuous drying kiln oven dry 1～3 hour, 500～750 ℃ of roastings are 1～4 hour in the calcining kiln, make semi-finished product G2;
(5) getting concentration is 20～30%, the solution P1 of Pt: Rh=5～10: 1 impregnated among the active constituent solution P1 5～25 minutes with above-mentioned catalyst semi-finished product G2, takes out, compressed air with 0.15～0.25MPa blows off raffinate, 300～500 ℃ of roastings 1～3 hour.
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| JP6106458B2 (en) * | 2013-02-26 | 2017-03-29 | 本田技研工業株式会社 | Exhaust gas catalytic device |
| CN104001507B (en) * | 2013-06-09 | 2016-12-28 | 杭州尹力环保科技有限公司 | A kind of dehydrogenation catalyst and preparation method thereof |
| JP6572675B2 (en) * | 2015-08-18 | 2019-09-11 | 株式会社デンソー | Exhaust gas purification catalyst |
| EP3281699A1 (en) * | 2016-08-11 | 2018-02-14 | Umicore AG & Co. KG | Particle filter with scr active coating |
| CN108404975B (en) * | 2018-04-27 | 2021-03-23 | 中自环保科技股份有限公司 | Oxidation type catalytic system with good low-temperature ignition performance and preparation process thereof |
| CN109248714B (en) * | 2018-10-12 | 2021-09-21 | 南京德普瑞克催化器有限公司 | Manufacturing process of low-reaction-temperature and low-degradation wire mesh catalyst |
| JP7195995B2 (en) * | 2019-03-27 | 2022-12-26 | 株式会社キャタラー | Exhaust gas purification catalyst |
| CN110404536A (en) * | 2019-08-08 | 2019-11-05 | 无锡威孚环保催化剂有限公司 | The preparation method of the three-way catalyst of bilayer coating |
| CN111939928B (en) * | 2020-08-18 | 2022-10-04 | 无锡威孚环保催化剂有限公司 | Three-way catalyst for enhancing durability of tail gas purification and preparation method thereof |
| CN111939905B (en) * | 2020-08-26 | 2021-05-07 | 湖南第一师范学院 | Preparation method of catalyst for automobile exhaust, product and application thereof |
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