CN105688933A - Technology for preparing three-way catalyst with ball milling method - Google Patents
Technology for preparing three-way catalyst with ball milling method Download PDFInfo
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- CN105688933A CN105688933A CN201610267751.9A CN201610267751A CN105688933A CN 105688933 A CN105688933 A CN 105688933A CN 201610267751 A CN201610267751 A CN 201610267751A CN 105688933 A CN105688933 A CN 105688933A
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- oxide
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- 238000000498 ball milling Methods 0.000 title claims abstract description 41
- 239000003054 catalyst Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 32
- 239000002002 slurry Substances 0.000 claims abstract description 25
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 22
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 17
- 239000002131 composite material Substances 0.000 claims abstract description 17
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 17
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 10
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 45
- 238000000227 grinding Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract 2
- 229910052742 iron Inorganic materials 0.000 abstract 1
- 229910052748 manganese Inorganic materials 0.000 abstract 1
- 239000011572 manganese Substances 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- 238000007747 plating Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- NDYYRETYXBJDGQ-UHFFFAOYSA-N [O-2].[Ce+3].[O-2].[Ce+3] Chemical compound [O-2].[Ce+3].[O-2].[Ce+3] NDYYRETYXBJDGQ-UHFFFAOYSA-N 0.000 description 2
- 238000003701 mechanical milling Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention relates to an automobile exhaust catalyst, in particular to a technology for preparing a three-way exhaust catalyst with a ball milling method.The technology includes the steps that zirconium oxide powder and cerium oxide powder are mixed by mass, ball milling is carried out, then aluminum oxide powder, iron oxide powder and manganese oxide powder are added, ball milling continues, and composite powder is obtained; the composite powder is prepared into slurry with deionized water, a pretreated cordierite carrier is immersed in the slurry and then taken out, the redundant slurry in pore channels is blown away, then the carrier is dried and roasted, and the catalyst is obtained.According to the technology, catalyst powder particles are refined by carrying out ball milling, and the grain size of the catalyst reaches the nanometer scale; meanwhile, the activity of the catalyst is improved by adding manganese and iron, and the obtained catalyst has a uniform and compact plating layer and is good in chemical stability.
Description
Technical field
The present invention relates to auto-exhaust catalyst, the technique that specifically ball-milling method prepares ternary tail-gas catalyst。
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 the technique that a kind of stable performance, lower-cost ball-milling method prepare ternary tail-gas catalyst。
The technical solution used in the present invention is: ball-milling method prepares the technique of ternary tail-gas catalyst, and it comprises the following steps:
(1) by mass fraction by zirconium oxide, cerium oxide powder mixing and ball milling, it is subsequently adding aluminium oxide, ferrum oxide, oxidation manganese powder continuation ball milling, obtains composite powder；
(2) above-mentioned composite powder deionized water is configured to slurry, more pretreated cordierite carrier is immersed in slurry；
(3) then take out, and blow away slurry unnecessary in duct, then carry out drying, roasting。
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, the mixing and ball milling time is 30 50h, and continuing Ball-milling Time is 20 40h。
As preferably, ball milling adopts the rotating speed of 180 220r/min, and ratio of grinding media to material is (9 10): 1。
As preferably, the immersion time in step (2) is 2min。。
As preferably, step (3) adopts 130 DEG C of dry 3h, 600 DEG C of roasting 1h。
As preferably, the pretreatment of described cordierite adopts the salpeter solution of 1mol/L to soak 1h, then cleans with deionized water, last 120 DEG C of dry 3h。
As can be known from the above technical solutions, the present invention makes catalyst fines grain refine by ball milling, and its crystallite dimension reaches nanoscale；Meanwhile, adding manganese, ferrum makes the activity of catalyst improve, it is thus achieved that catalyst not only coating uniform, fine and close, chemical stability is good。
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。
Ball-milling method prepares the technique of ternary tail-gas catalyst, and it comprises the following steps:
First mass fraction is pressed by zirconium oxide, cerium oxide powder mixing and ball milling 30 50h, add aluminium oxide, ferrum oxide, manganese oxide continuation Ball-milling Time 20 40h, obtain composite powder, wherein zirconium oxide accounts for 4 8wt%, cerium oxide accounts for 15 20wt%, ferrum oxide accounts for 2 3wt%, and manganese oxide accounts for 2 3wt%, and surplus is aluminium oxide；Mechanical milling process adopts the rotating speed of 180 220r/min, (9 10): the ratio of grinding media to material of 1, so can obtain nano level composite powder。In mechanical milling process, owing to stress-induced isomer phase transformation can occur aluminium oxide ball milling, the α-Al of generation2O3Catalytic performance is unfavorable, so should participate in again grinding after ball milling zirconium oxide, cerium oxide and powder；And ferrum oxide, manganese oxide are as participated in grinding in early stage, it is difficult to obtain nano-scale particle。The present invention first avoid aluminium oxide and only ball milling zirconium oxide, cerium oxide to a certain extent, then add aluminium oxide, ferrum oxide and manganese oxide and continue ball milling, zirconium oxide can be made to be solidly soluted into completely in cerium oxide, reduce the lattice paprmeter of cerium oxide, can make highly dispersed in the solid solution of cerium oxide-cerium oxide simultaneously；Therefore, this ball-milling technology not only can obtain cerium oxide-cerium oxide solid solution, and has refined powder, and whole composite powder particle diameter can reach 60 90nm。
Acquisition nanometer grade composit powder 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 catalyst of even compact on carrier。The pretreatment of cordierite adopts the salpeter solution of 1mol/L to soak 1h, then cleans with deionized water, last 120 DEG C of dry 3h；It is greatly promoted the performance of catalyst。
Embodiment 1
By mass fraction by zirconium oxide, cerium oxide powder mixing, adopt the rotating speed of 180r/min, the ratio of grinding media to material ball milling 30h of 9:1, adding aluminium oxide, ferrum oxide, manganese oxide continuation Ball-milling Time 20h, obtain composite powder, 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, the salpeter solution that then cordierite adopts 1mol/L soaks 1h, then clean with deionized water, cool down after last 120 DEG C of dry 3h, be re-used as carrier and immerse in slurry, take out after about 1min, and blow away slurry unnecessary in duct, 1min in slurry is immersed again, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h, it is thus achieved that three-way catalyst after drying；This catalyst is tested, and the conversion ratio of CO, HC and NO is reached 97.8% by it, and initiation temperature is between 180 200 DEG C。
Embodiment 2
By mass fraction by zirconium oxide, cerium oxide powder mixing, adopt the rotating speed of 200r/min, the ratio of grinding media to material ball milling 40h of 10:1, adding aluminium oxide and continue Ball-milling Time 30h, obtain composite powder, 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, the salpeter solution that then cordierite adopts 1mol/L soaks 1h, then clean with deionized water, cool down after last 120 DEG C of dry 3h, be re-used as carrier and immerse in slurry, take out after about 1min, and blow away slurry unnecessary in duct, 1min in slurry is immersed again, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h, it is thus achieved that three-way catalyst after drying；This catalyst is tested, and the conversion ratio of CO, HC and NO is reached 98.3% by it, and initiation temperature is between 160 180 DEG C。
Embodiment 3
By mass fraction by zirconium oxide, cerium oxide powder mixing, adopt the rotating speed of 220r/min, the ratio of grinding media to material ball milling 50h of 10:1, adding aluminium oxide and continue Ball-milling Time 40h, obtain composite powder, 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, the salpeter solution that then cordierite adopts 1mol/L soaks 1h, then clean with deionized water, cool down after last 120 DEG C of dry 3h, be re-used as carrier and immerse in slurry, take out after about 1min, and blow away slurry unnecessary in duct, 1min in slurry is immersed again, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h, it is thus achieved that three-way catalyst after drying；This catalyst is tested, and the conversion ratio of CO, HC and NO is reached 98% by it, and initiation temperature is between 170 190 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 (7)
1. ball-milling method prepares the technique of ternary tail-gas catalyst, and it comprises the following steps:
(1) by mass fraction by zirconium oxide, cerium oxide powder mixing and ball milling, it is subsequently adding aluminium oxide, ferrum oxide, oxidation manganese powder continuation ball milling, obtains composite powder；
(2) above-mentioned composite powder deionized water is configured to slurry, more pretreated cordierite carrier is immersed in slurry；
(3) then take out, and blow away slurry unnecessary in duct, then carry out drying, roasting。
2. the technique that ball-milling method prepares ternary tail-gas catalyst 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 technique that ball-milling method prepares ternary tail-gas catalyst according to claim 1, it is characterised in that: the mixing and ball milling time is 30 50h, and continuing Ball-milling Time is 20 40h。
4. the technique that ball-milling method prepares ternary tail-gas catalyst according to claim 1, it is characterised in that: ball milling adopts the rotating speed of 180 220r/min, and ratio of grinding media to material is (9 10): 1。
5. the technique that ball-milling method prepares ternary tail-gas catalyst according to claim 1, it is characterised in that: the immersion time in step (2) is 2min。
6. the technique that ball-milling method prepares ternary tail-gas catalyst according to claim 1, it is characterised in that: step (3) adopts 130 DEG C of dry 3h, 600 DEG C of roasting 1h。
7. the technique that ball-milling method prepares ternary tail-gas catalyst according to claim 1, it is characterised in that: the pretreatment of described cordierite adopts the salpeter solution of 1mol/L to soak 1h, then cleans with deionized water, last 120 DEG C of dry 3h。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610267751.9A CN105688933B (en) | 2016-04-27 | 2016-04-27 | The technique that ball-milling method prepares three-way catalyst |
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| CN201610267751.9A CN105688933B (en) | 2016-04-27 | 2016-04-27 | The technique that ball-milling method prepares three-way catalyst |
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| Publication Number | Publication Date |
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| CN105688933A true CN105688933A (en) | 2016-06-22 |
| CN105688933B CN105688933B (en) | 2018-03-20 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108311157A (en) * | 2018-02-07 | 2018-07-24 | 天津爱蓝天环保科技有限公司 | A kind of nanometer catalyst and preparation method thereof |
| CN109847863A (en) * | 2018-12-31 | 2019-06-07 | 柳州申通汽车科技有限公司 | The technique that ball-milling method prepares three-way catalyst |
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|---|---|---|---|---|
| CN101003023A (en) * | 2006-01-19 | 2007-07-25 | 清华大学 | Method for preparing catalyst to purify automobile tail gas |
| CN101721997A (en) * | 2009-11-10 | 2010-06-09 | 华东理工大学 | Integral type metal carrier three-way catalyst and preparation method thereof |
| 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 |
| CN104338528A (en) * | 2013-07-30 | 2015-02-11 | 江苏瑞丰科技实业有限公司 | Preparation of room temperature formaldehyde catalyst |
-
2016
- 2016-04-27 CN CN201610267751.9A patent/CN105688933B/en active Active
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 |
| CN101721997A (en) * | 2009-11-10 | 2010-06-09 | 华东理工大学 | Integral type metal carrier three-way catalyst and preparation method thereof |
| 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 |
| CN104338528A (en) * | 2013-07-30 | 2015-02-11 | 江苏瑞丰科技实业有限公司 | Preparation of room temperature formaldehyde catalyst |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108311157A (en) * | 2018-02-07 | 2018-07-24 | 天津爱蓝天环保科技有限公司 | A kind of nanometer catalyst and preparation method thereof |
| CN109847863A (en) * | 2018-12-31 | 2019-06-07 | 柳州申通汽车科技有限公司 | The technique that ball-milling method prepares three-way catalyst |
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| CN105688933B (en) | 2018-03-20 |
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