CN105688933B - The technique that ball-milling method prepares three-way catalyst - Google Patents
The technique that ball-milling method prepares three-way catalyst Download PDFInfo
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- CN105688933B CN105688933B CN201610267751.9A CN201610267751A CN105688933B CN 105688933 B CN105688933 B CN 105688933B CN 201610267751 A CN201610267751 A CN 201610267751A CN 105688933 B CN105688933 B CN 105688933B
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- 238000000498 ball milling Methods 0.000 title claims abstract description 40
- 239000003054 catalyst Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 27
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002002 slurry Substances 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 16
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 16
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 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
- 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
- 238000002156 mixing Methods 0.000 claims abstract description 6
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 4
- 230000003647 oxidation Effects 0.000 claims abstract description 3
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 238000007654 immersion Methods 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 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 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- 238000003701 mechanical milling Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 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 present invention relates to auto-exhaust catalyst, the technique that specifically ball-milling method prepares ternary tail-gas catalyst, it is included zirconium oxide, cerium oxide powder mixing and ball milling by mass fraction, then adds aluminum oxide, iron oxide, oxidation manganese powder and continues ball milling, obtains composite powder；Above-mentioned composite powder is configured to slurry with deionized water, then pretreated cordierite carrier is immersed in slurry；Then take out, and blow away slurry unnecessary in duct, then dried, be calcined, obtain catalyst.The present invention refines catalyst fines particle by ball milling, and its crystallite dimension reaches nanoscale；Meanwhile addition manganese, iron make it that the activity of catalyst is improved, not only coating is uniform, fine and close for the catalyst of acquisition, and chemical stability is good.
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
With the increase of car ownership, CO, HC, NO that automobile discharges into airXIt is more and more.At present, many states
Family has taken strict control emission measure to motor vehicle exhaust emission.Therefore the processing of vehicle exhaust has become important
Problem.In the prior art, the control to motor vehicle exhaust emission is realized by installing catalytic cleaner additional, and catalytic cleaner
Key be catalyst.Catalyst generally use three-decker is made up of active component, washcoat and carrier.From rare earth calcium
Titanium ore oxide（PTO）Since tail gas catalyzed, because its A, B position can substitute and Lacking oxygen is produced, while such is urged
Agent has larger price advantage to noble metal catalyst so that such catalyst becomes the focus of research.It is but existing single
The PTO catalytic performances of component are bad, stability is poor, it is impossible to meet increasingly serious motor vehicle exhaust emission pollution.
The content of the invention
For above-mentioned technical problem, the present invention provides a kind of stable performance, lower-cost ball-milling method prepares ternary tail gas
The technique of catalyst.
The technical solution adopted by 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, aluminum oxide, iron oxide, oxidation manganese powder are then added
Continue ball milling, obtain composite powder；
（2）Above-mentioned composite powder is configured to slurry with deionized water, then pretreated cordierite carrier is immersed and starched
In material；
（3）Then take out, and blow away slurry unnecessary in duct, then dried, be calcined.
Preferably, in the composite powder, zirconium oxide accounts for 4-8wt%, and cerium oxide accounts for 15-20wt%, iron oxide accounts for 2-
3wt%, manganese oxide account for 2-3wt%, and surplus is aluminum oxide.
Preferably, the mixing and ball milling time is 30-50h, continuation Ball-milling Time is 20-40h.
Preferably, ball milling uses 180-220r/min rotating speed, ratio of grinding media to material is（9—10）:1.
Preferably, step（2）In the immersion time be 2min..
Preferably, step（3）Using 130 DEG C of dry 3h, 600 DEG C of roasting 1h.
Preferably, then the pretreatment of the cordierite uses deionized water using 1mol/L salpeter solution immersion 1h
Cleaning, last 120 DEG C dry 3h.
As can be known from the above technical solutions, the present invention refines catalyst fines particle by ball milling, and its crystallite dimension reaches
Nanoscale；Meanwhile addition manganese, iron make it that the activity of catalyst is improved, not only coating is uniform, fine and close for the catalyst of acquisition,
Chemical stability is good.
Embodiment
The present invention is described more detail below, illustrative examples of the invention and explanation are used for explaining the present invention herein,
It is 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：
Zirconium oxide, cerium oxide powder 30-50h of mixing and ball milling are added into aluminum oxide, iron oxide, oxygen by mass fraction first
Change manganese and continue 20-40h of Ball-milling Time, obtain composite powder, wherein zirconium oxide accounts for 4-8wt%, and cerium oxide accounts for 15-20wt%, oxygen
Change iron and account for 2-3wt%, manganese oxide accounts for 2-3wt%, and surplus is aluminum oxide；Turned in mechanical milling process using 180-220r/min
Speed,（9—10）:1 ratio of grinding media to material, it can so obtain nano level composite powder.In mechanical milling process, due to aluminum oxide ball milling meeting
Stress-induced isomer phase transformation, the α-Al of generation occurs2O3It is unfavorable to catalytic performance, so should be in ball milling zirconium oxide, oxygen
Participate in grinding again after changing cerium and powder；And iron oxide, manganese oxide such as participate in grinding in early stage, it is difficult to which nano-scale particle must be obtained.This
Aluminum oxide is first avoided in invention and only ball milling zirconium oxide, cerium oxide to a certain extent, then add aluminum oxide, iron oxide and manganese oxide
Continue ball milling, zirconium oxide can be made to be dissolved into completely in cerium oxide, reduce the lattice constant of cerium oxide, while highly dispersed can be made to exist
In the solid solution of cerium oxide-cerium oxide；Therefore, this ball-milling technology can not only obtain cerium oxide-oxidation cerium solid solution, and refine
Powder, whole composite powder particle diameter can reach 60-90nm.
It is last to obtain nanometer grade composit powder, is configured to slurry with deionized water, then pretreated cordierite carrier is soaked
Enter in slurry, taken out after about 1min, and blow away slurry unnecessary in duct, immerse 1min in slurry after drying again, then 130 DEG C
3h, 600 DEG C of roasting 1h are dried, the catalyst of even compact can be so obtained on carrier.The pretreatment of cordierite uses 1mol/
L salpeter solution immersion 1h, is then cleaned, last 120 DEG C dry 3h with deionized water；Greatly promote the performance of catalyst.
Embodiment 1
Zirconium oxide, cerium oxide powder are mixed by mass fraction, using 180r/min rotating speed, 9:1 ratio of grinding media to material ball milling
30h, adding aluminum oxide, iron oxide, manganese oxide and continue Ball-milling Time 20h, obtain composite powder, wherein zirconium oxide accounts for 4wt%,
Cerium oxide accounts for 15wt%, and iron oxide accounts for 2wt%, and manganese oxide accounts for 2wt%, and surplus is aluminum oxide；Then with deionized water by composite powder
Slurry is configured to, cordierite is then soaked into 1h using 1mol/L salpeter solution, then cleaned with deionized water, last 120
Cooled down after DEG C drying 3h, be re-used as carrier and immerse in slurry, take out, and blow away slurry unnecessary in duct, dry after about 1min
Immerse 1min in slurry again afterwards, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h, obtain three-way catalyst；The catalyst is carried out
Test, its conversion ratio to CO, HC and NO reach 97.8%, and initiation temperature is between 180-200 DEG C.
Embodiment 2
Zirconium oxide, cerium oxide powder are mixed by mass fraction, using 200r/min rotating speed, 10:1 ratio of grinding media to material ball milling
40h, adding aluminum oxide and continue Ball-milling Time 30h, obtain composite powder, wherein zirconium oxide accounts for 6wt%, and cerium oxide accounts for 18wt%,
Iron oxide accounts for 2wt%, and manganese oxide accounts for 3wt%, and surplus is aluminum oxide；Then composite powder is configured to slurry with deionized water, so
Cordierite is soaked into 1h using 1mol/L salpeter solution afterwards, then cleaned with deionized water, it is cold after last 120 DEG C dry 3h
But, it is re-used as carrier to immerse in slurry, is taken out after about 1min, and blow away slurry unnecessary in duct, immerses slurry after drying again
Middle 1min, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h, obtain three-way catalyst；The catalyst is tested, its to CO,
HC and NO conversion ratio reaches 98.3%, and initiation temperature is between 160-180 DEG C.
Embodiment 3
Zirconium oxide, cerium oxide powder are mixed by mass fraction, using 220r/min rotating speed, 10:1 ratio of grinding media to material ball milling
50h, adding aluminum oxide and continue Ball-milling Time 40h, obtain composite powder, wherein zirconium oxide accounts for 8wt%, and cerium oxide accounts for 20wt%,
Iron oxide accounts for 3wt%, and manganese oxide accounts for 3wt%, and surplus is aluminum oxide；Then composite powder is configured to slurry with deionized water, so
Cordierite is soaked into 1h using 1mol/L salpeter solution afterwards, then cleaned with deionized water, it is cold after last 120 DEG C dry 3h
But, it is re-used as carrier to immerse in slurry, is taken out after about 1min, and blow away slurry unnecessary in duct, immerses slurry after drying again
Middle 1min, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h, obtain three-way catalyst；The catalyst is tested, its to CO,
HC and NO conversion ratio reaches 98%, and initiation temperature is between 170-190 DEG C.
The technical scheme provided above the embodiment of the present invention is described in detail, specific case used herein
The principle and embodiment of the embodiment of the present invention are set forth, the explanation of above example is only applicable to help and understands this
The principle of inventive embodiments；Meanwhile for those of ordinary skill in the art, according to the embodiment of the present invention, in specific embodiment party
There will be changes in formula and application, in summary, this specification content should not be construed as limiting the invention.
Claims (6)
1. ball-milling method prepares the technique of ternary tail-gas catalyst, it comprises the following steps：
（1）By mass fraction by zirconium oxide, cerium oxide powder mixing and ball milling, then add aluminum oxide, iron oxide, oxidation manganese powder and continue
Ball milling, obtain composite powder；
（2）Above-mentioned composite powder is configured to slurry with deionized water, then pretreated cordierite carrier is immersed in slurry；
（3）Then take out, and blow away slurry unnecessary in duct, then dried, be calcined；In the composite powder, zirconium oxide
4-8wt% is accounted for, cerium oxide accounts for 15-20wt%, and iron oxide accounts for 2-3wt%, and manganese oxide accounts for 2-3wt%, and surplus is aluminum oxide.
2. 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
For 30-50h, continuation Ball-milling Time is 20-40h.
3. the technique that ball-milling method prepares ternary tail-gas catalyst according to claim 1, it is characterised in that：Ball milling uses
180-220r/min rotating speed, ratio of grinding media to material are（9—10）:1.
4. the technique that ball-milling method prepares ternary tail-gas catalyst according to claim 1, it is characterised in that：Step（2）In
The immersion time is 2min.
5. the technique that ball-milling method prepares ternary tail-gas catalyst according to claim 1, it is characterised in that：Step（3）Using
130 DEG C of dry 3h, 600 DEG C of roasting 1h.
6. the technique that ball-milling method prepares ternary tail-gas catalyst according to claim 1, it is characterised in that：The cordierite
Then pretreatment is cleaned, last 120 DEG C dry 3h using 1mol/L salpeter solution immersion 1h with deionized water.
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| 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 |
| CN109847863B (en) * | 2018-12-31 | 2021-09-07 | 柳州申通汽车科技有限公司 | Process for preparing three-way catalyst by ball milling method |
Citations (5)
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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 |
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