CN105797745A - Method for preparing automobile exhaust ternary catalyst by impregnation method - Google Patents
Method for preparing automobile exhaust ternary catalyst by impregnation method Download PDFInfo
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- CN105797745A CN105797745A CN201610268260.6A CN201610268260A CN105797745A CN 105797745 A CN105797745 A CN 105797745A CN 201610268260 A CN201610268260 A CN 201610268260A CN 105797745 A CN105797745 A CN 105797745A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
The invention relates to an automobile exhaust catalyst, in particular to a method for preparing an automobile exhaust ternary catalyst by an impregnation method. The method comprises the following steps that a nitrate solution of zirconium, cerium, iron and manganese is mixed into a salvolatile solution for reaction according to the mass fraction; after precipitate generation, precipitates are filtered and washed, and are then dried and roasted to obtain oxide composite powder; the composite powder is prepared into slurry by deionized water, and then, a pretreated cordierite carrier is soaked into the slurry; next, the carrier is soaked into a palladium chloride ammonia solution, and then, the carrier is taken out to be soaked into a potassium borohydride solution for reaction, and is then washed by the deionized water; then, the carrier is soaked into a solution prepared from palladium chloride, ammonia water, EEDTA (ethylenediaminetetraacetic acid), hydrazine hydrate and the deionized water for reaction, and then, the carrier is taken out for washing and drying. The method has the advantages that the activity of the catalyst is improved by adding manganese and iron; palladium plating is also performed on the carrier; a plating layer is uniform and compact; the chemical stability is good; the hardness is high; the lubricating property is good; the abrasion resistance and anti-scratch capability is high.
Description
Technical field
The present invention relates to auto-exhaust catalyst, the method that specifically infusion process prepares ternary catalyst for automobile tail gas.
Background technology
Along with the increase of automobile pollution, CO, HC, NO that automobile discharges in airXMore and more.At present, motor vehicle exhaust emission has been taken strict control emission measure by many countries.Therefore the process of vehicle exhaust is increasingly becoming important problem.In the prior art, be realize by installing catalytic cleaner additional the control of motor vehicle exhaust emission, and catalytic cleaner it is crucial that catalyst.Catalyst generally adopts three-decker to be namely made up of active component, washcoat and carrier.From RE perovskite oxide (PTO) for since tail gas catalyzed, having produced Lacking oxygen owing to its A, B position can replace, noble metal catalyst is had bigger price advantage by such catalyst simultaneously so that such catalyst becomes the focus of research.But, the PTO catalytic performance of existing one-component is not good, poor stability, it is impossible to meets increasingly serious motor vehicle exhaust emission and pollutes.
Summary of the invention
For above-mentioned technical problem, the present invention provides a kind of method that stable performance, lower-cost infusion process prepare ternary catalyst for automobile tail gas.
The technical solution used in the present invention is: infusion process prepares the method for ternary catalyst for automobile tail gas, and it comprises the following steps:
(1) being mixed by the nitrate solution of zirconium, cerium, ferrum and manganese by mass fraction, the pH value regulating solution is 2, is then added in sal volatile and reacts, and generates filtration after precipitating, washing, then dry, roasting, it is thus achieved that oxide composite end；
(2) above-mentioned composite powder deionized water is configured to slurry, more pretreated cordierite carrier is immersed in slurry, then take out, and blow away slurry unnecessary in duct, then carry out drying, roasting；
(3) then carrier is immersed in Palladous chloride. ammonia solution, then take out dry, roasting, cooling；
(4) again carrier is immersed in solution of potassium borohydride and react, then use deionized water wash；
(5) then carrier is immersed reaction in the solution by the preparation of Palladous chloride., ammonia, EDTA, hydrazine hydrate and deionized water, then take out washing, dry.
As preferably, in described composite powder, zirconium oxide accounts for 4 8wt%, and cerium oxide accounts for 15 20wt%, and ferrum oxide accounts for 2 3wt%, and manganese oxide accounts for 2 3wt%, and surplus is aluminium oxide.
As preferably, step (1) adopts deionized water and 95% washing with alcohol.
As preferably, step (1) adopting 120 DEG C of dry 4h, 650 DEG C of roasting 2h.
As preferably, the immersion time in step (2) is 2min, adopts 130 DEG C of dry 3h, 600 DEG C of roasting 1h.
As preferably, in step (3), the concentration of Palladous chloride. ammonia solution is 1g/L, and the immersion time is 3h, adopts 120 DEG C of dry 4h, 500 DEG C of roasting 2h.
As preferably, the response time in step (4) is 20-30min.
As preferably, the response time in step (5) is 20-30min, with deionized water wash to neutral after taking-up, and then 100 DEG C of dry 4h.
As can be known from the above technical solutions, the present invention adds manganese, ferrum makes the activity of catalyst improve；The present invention also carries out plating palladium on carrier, and not only coating is uniform, fine and close, and chemical stability is good, and hardness is high, and lubricity is good, resistance to wears and anti-scuffing function is strong.
Detailed description of the invention
The present invention is described more detail below, and illustrative examples and explanation in this present invention are used for explaining the present invention, but not as a limitation of the invention.
Infusion process prepares the method for ternary catalyst for automobile tail gas, and it comprises the following steps:
First press mass fraction to be mixed by the nitrate solution of zirconium, cerium, ferrum and manganese, the pH value regulating solution is 2, it is then added in sal volatile and reacts, filter after generating precipitation, wash, then dry, roasting, acquisition oxide composite end, wherein zirconium oxide accounts for 4 8wt%, and cerium oxide accounts for 15 20wt%, and ferrum oxide accounts for 2 3wt%, manganese oxide accounts for 2 3wt%, and surplus is aluminium oxide；Adopt deionized water and 95% washing with alcohol during washing, and adopt 120 DEG C of dry 4h, 650 DEG C of roasting 2h.
Acquisition oxide composite is last, it is configured to slurry with deionized water, again pretreated cordierite carrier is immersed in slurry, take out after about 1min, and blow away slurry unnecessary in duct, immersing 1min in slurry after drying again, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h, so can obtain the impregnating slurry layer of even compact on carrier.
After slurry coats, carrier is immersed in the Palladous chloride. ammonia solution of 1g/L, magnetic agitation 4h, make absorption palladium ion on carrier, then take out, blow down redundant solution, dry, adopt 120 DEG C of dry 4h, 500 DEG C of roasting 2h, cooling；Carrier is immersed reaction 20-30min in solution of potassium borohydride again, makes the palladium ion of absorption on carrier be reduced to simple substance palladium, then use deionized water wash；Then the carrier after reduction is immersed reaction 20-30min in the solution by the preparation of Palladous chloride., ammonia, EDTA, hydrazine hydrate and deionized water, then take out with deionized water wash to neutral, finally dry, 100 DEG C of dry 4h, thus obtaining the catalyst being coated with simple substance palladium.
Embodiment 1
By mass fraction, the nitrate solution of zirconium, cerium, ferrum and manganese is mixed, the pH value regulating solution is 2, is then added in sal volatile and reacts, and filters after generating precipitation, again with deionized water and 95% washing with alcohol precipitate, then 120 DEG C of dry 4h, 650 DEG C of roasting 2h, obtain oxide composite end, and wherein zirconium oxide accounts for 4wt%, cerium oxide accounts for 15wt%, ferrum oxide accounts for 2wt%, and manganese oxide accounts for 2wt%, and surplus is aluminium oxide；Followed by deionized water, composite powder is configured to slurry, then pretreated cordierite carrier is immersed in slurry, take out after about 1min, and blow away slurry unnecessary in duct, immerse 1min in slurry after drying again, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h；After slurry coats, carrier is immersed in the Palladous chloride. ammonia solution of 1g/L, magnetic agitation 4h, then take out, blow down redundant solution, dry, adopt 120 DEG C of dry 4h, 500 DEG C of roasting 2h, cooling；Carrier is immersed reaction 20min in solution of potassium borohydride again, then uses deionized water wash；Then carrier is immersed reaction 20min in the solution by the preparation of Palladous chloride., ammonia, EDTA, hydrazine hydrate and deionized water, then takes out with deionized water wash to neutral, finally dry, 100 DEG C of dry 4h, it is thus achieved that palladium load capacity is the catalyst of 1g/L；This catalyst is tested, and the conversion ratio of CO, HC and NO is reached 98.5% by it, and initiation temperature is between 150 170 DEG C.
Embodiment 2
By mass fraction, the nitrate solution of zirconium, cerium, ferrum and manganese is mixed, the pH value regulating solution is 2, is then added in sal volatile and reacts, and filters after generating precipitation, again with deionized water and 95% washing with alcohol precipitate, then 120 DEG C of dry 4h, 650 DEG C of roasting 2h, obtain oxide composite end, and wherein zirconium oxide accounts for 6wt%, cerium oxide accounts for 18wt%, ferrum oxide accounts for 2wt%, and manganese oxide accounts for 3wt%, and surplus is aluminium oxide；Followed by deionized water, composite powder is configured to slurry, then pretreated cordierite carrier is immersed in slurry, take out after about 1min, and blow away slurry unnecessary in duct, immerse 1min in slurry after drying again, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h；After slurry coats, carrier is immersed in the Palladous chloride. ammonia solution of 1g/L, magnetic agitation 4h, then take out, blow down redundant solution, dry, adopt 120 DEG C of dry 4h, 500 DEG C of roasting 2h, cooling；Carrier is immersed reaction 25min in solution of potassium borohydride again, then uses deionized water wash；Then carrier is immersed reaction 25min in the solution by the preparation of Palladous chloride., ammonia, EDTA, hydrazine hydrate and deionized water, then takes out with deionized water wash to neutral, finally dry, 100 DEG C of dry 4h, it is thus achieved that palladium load capacity is the catalyst of 2g/L；This catalyst is tested, and the conversion ratio of CO, HC and NO is reached 98.6% by it, and initiation temperature is between 130 150 DEG C.
Embodiment 3
By mass fraction, the nitrate solution of zirconium, cerium, ferrum and manganese is mixed, the pH value regulating solution is 2, is then added in sal volatile and reacts, and filters after generating precipitation, again with deionized water and 95% washing with alcohol precipitate, then 120 DEG C of dry 4h, 650 DEG C of roasting 2h, obtain oxide composite end, and wherein zirconium oxide accounts for 8wt%, cerium oxide accounts for 20wt%, ferrum oxide accounts for 3wt%, and manganese oxide accounts for 3wt%, and surplus is aluminium oxide；Followed by deionized water, composite powder is configured to slurry, then pretreated cordierite carrier is immersed in slurry, take out after about 1min, and blow away slurry unnecessary in duct, immerse 1min in slurry after drying again, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h；After slurry coats, carrier is immersed in the Palladous chloride. ammonia solution of 1g/L, magnetic agitation 4h, then take out, blow down redundant solution, dry, adopt 120 DEG C of dry 4h, 500 DEG C of roasting 2h, cooling；Carrier is immersed reaction 30min in solution of potassium borohydride again, then uses deionized water wash；Then carrier is immersed reaction 30min in the solution by the preparation of Palladous chloride., ammonia, EDTA, hydrazine hydrate and deionized water, then takes out with deionized water wash to neutral, finally dry, 100 DEG C of dry 4h, it is thus achieved that palladium load capacity is the catalyst of 2g/L；This catalyst is tested, and the conversion ratio of CO, HC and NO is reached 98.3% by it, and initiation temperature is between 140 160 DEG C.
The technical scheme above embodiment of the present invention provided is described in detail, principle and the embodiment of the embodiment of the present invention are set forth by specific case used herein, and the explanation of above example is only applicable to help to understand the principle of the embodiment of the present invention；Simultaneously for one of ordinary skill in the art, according to the embodiment of the present invention, all will change in detailed description of the invention and range of application, in sum, this specification content should not be construed as limitation of the present invention.
Claims (8)
1. the method that infusion process prepares ternary catalyst for automobile tail gas, it comprises the following steps:
(1) being mixed by the nitrate solution of zirconium, cerium, ferrum and manganese by mass fraction, the pH value regulating solution is 2, is then added in sal volatile and reacts, and generates filtration after precipitating, washing, then dry, roasting, it is thus achieved that oxide composite end；
(2) above-mentioned composite powder deionized water is configured to slurry, more pretreated cordierite carrier is immersed in slurry, then take out, and blow away slurry unnecessary in duct, then carry out drying, roasting；
(3) then carrier is immersed in Palladous chloride. ammonia solution, then take out dry, roasting, cooling；
(4) again carrier is immersed in solution of potassium borohydride and react, then use deionized water wash；
(5) then carrier is immersed reaction in the solution by the preparation of Palladous chloride., ammonia, EDTA, hydrazine hydrate and deionized water, then take out washing, dry.
2. the method that infusion process prepares ternary catalyst for automobile tail gas according to claim 1, it is characterised in that: in described composite powder, zirconium oxide accounts for 4 8wt%, and cerium oxide accounts for 15 20wt%, and ferrum oxide accounts for 2 3wt%, and manganese oxide accounts for 2 3wt%, and surplus is aluminium oxide.
3. the method that infusion process prepares ternary catalyst for automobile tail gas according to claim 1, it is characterised in that: step (1) adopts deionized water and 95% washing with alcohol.
4. the method that infusion process prepares ternary catalyst for automobile tail gas according to claim 1, it is characterised in that: step (1) adopts 120 DEG C of dry 4h, 650 DEG C of roasting 2h.
5. the method that infusion process prepares ternary catalyst for automobile tail gas according to claim 1, it is characterised in that: the immersion time in step (2) is 2min, adopts 130 DEG C of dry 3h, 600 DEG C of roasting 1h.
6. the method that infusion process prepares ternary catalyst for automobile tail gas according to claim 1, it is characterised in that: in step (3), the concentration of Palladous chloride. ammonia solution is 1g/L, and the immersion time is 3h, adopts 120 DEG C of dry 4h, 500 DEG C of roasting 2h.
7. the method that infusion process prepares ternary catalyst for automobile tail gas according to claim 1, it is characterised in that: the response time in step (4) is 20-30min.
8. the method that infusion process prepares ternary catalyst for automobile tail gas according to claim 1, it is characterised in that: the response time in step (5) is 20-30min, with deionized water wash to neutral after taking-up, then 100 DEG C of dry 4h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610268260.6A CN105797745A (en) | 2016-04-27 | 2016-04-27 | Method for preparing automobile exhaust ternary catalyst by impregnation method |
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| CN201610268260.6A CN105797745A (en) | 2016-04-27 | 2016-04-27 | Method for preparing automobile exhaust ternary catalyst by impregnation method |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003023A (en) * | 2006-01-19 | 2007-07-25 | 清华大学 | Method for preparing catalyst to purify automobile tail gas |
| WO2011092521A1 (en) * | 2010-02-01 | 2011-08-04 | Johnson Matthey Plc | Extruded scr filter |
| US20130004391A1 (en) * | 2010-04-14 | 2013-01-03 | Umicore Ag & Co. Kg | Reduction-catalyst-coated diesel particle filter having improved characteristics |
| CN104772162A (en) * | 2015-04-11 | 2015-07-15 | 桂林理工大学 | Zr-Ce-Mn-Fe/ZSM-5 composite oxide catalyst for NOx reduction by using low-temperature NH3 and preparation method thereof |
| CN105170148A (en) * | 2015-10-30 | 2015-12-23 | 苏州莲池环保科技发展有限公司 | Method for preparing three-way catalyst with efficient sulfur resisting characteristic |
-
2016
- 2016-04-27 CN CN201610268260.6A patent/CN105797745A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003023A (en) * | 2006-01-19 | 2007-07-25 | 清华大学 | Method for preparing catalyst to purify automobile tail gas |
| WO2011092521A1 (en) * | 2010-02-01 | 2011-08-04 | Johnson Matthey Plc | Extruded scr filter |
| US20130004391A1 (en) * | 2010-04-14 | 2013-01-03 | Umicore Ag & Co. Kg | Reduction-catalyst-coated diesel particle filter having improved characteristics |
| CN104772162A (en) * | 2015-04-11 | 2015-07-15 | 桂林理工大学 | Zr-Ce-Mn-Fe/ZSM-5 composite oxide catalyst for NOx reduction by using low-temperature NH3 and preparation method thereof |
| CN105170148A (en) * | 2015-10-30 | 2015-12-23 | 苏州莲池环保科技发展有限公司 | Method for preparing three-way catalyst with efficient sulfur resisting characteristic |
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Application publication date: 20160727 |