CN104624205A - Method for regenerating three-way catalyst Pd/Na2O/K2O/C - Google Patents
Method for regenerating three-way catalyst Pd/Na2O/K2O/C Download PDFInfo
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- CN104624205A CN104624205A CN201510086738.9A CN201510086738A CN104624205A CN 104624205 A CN104624205 A CN 104624205A CN 201510086738 A CN201510086738 A CN 201510086738A CN 104624205 A CN104624205 A CN 104624205A
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- catalyst
- regeneration
- way catalyst
- regenerating
- microwave
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- 239000003054 catalyst Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 22
- 230000001172 regenerating effect Effects 0.000 title claims abstract description 7
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 title abstract 2
- 238000011069 regeneration method Methods 0.000 claims abstract description 20
- 230000008929 regeneration Effects 0.000 claims abstract description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000009418 renovation Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000011084 recovery Methods 0.000 claims description 5
- 230000003213 activating effect Effects 0.000 claims description 3
- 238000007605 air drying Methods 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 231100000572 poisoning Toxicity 0.000 claims description 3
- 230000000607 poisoning effect Effects 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 15
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 12
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 230000002779 inactivation Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 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
- B01J23/90—Regeneration or reactivation
- B01J23/96—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides of the noble metals
-
- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/58—Platinum group metals with alkali- or alkaline earth metals
-
- 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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
- B01J38/12—Treating with free oxygen-containing gas
-
- 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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
-
- 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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/60—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using acids
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
The invention relates to a method for integrally regenerating a catalyst. The method disclosed by the invention is mainly used for regenerating similar three-way catalysts, namely Pd/Na2O/K2O/C and the like, outstandingly optimizing the regeneration treatment process by combining a microwave regeneration method with a low-temperature plasma regeneration method and regenerating the treated catalyst through a H2O2 solution, so that the catalyst is further enhanced in property, more stable in service life, good in repeatability and suitable for wide popularization and application in industry.
Description
Technical field
The invention belongs to catalyst regeneration field, be specifically related to a kind of comprehensive renovation process of three-way catalyst, especially Pd/Na
2o/K
2the renovation process of O/C three-way catalyst.
Background technology
Along with growing with each passing day of city automobile owning amount, the pollution that the waste gas of motor vehicle emission causes air is more and more serious.Therefore the automobile exhaust pollution limiting and administer as mobile pollution source has become current urgent task, and especially in non-row's warm period, automobile exhaust pollution thing share rate reaches more than 70%.Vehicle exhaust major pollutants are hydrocarbon (HC), carbon monoxide (CO), nitrogen oxide (NOx) and carbon dioxide (CO
2) etc.Automobile emission is administered and is divided into improvement and machine in machine to administer two large classes outward.(initiatively administering) is administered mainly by regulating engine combustion performance or use " to clean " discharge performance that fuel etc. improves engine, the generation of decreasing pollution thing from source in machine.But only can not reach emission request (unless electric vehicle) completely, even if clean fuel automobile (as LPG or CNG car) still discharges certain exhaust pollutant by administering in machine.Machine is administered outward (passive improvement) refers to and carries out (catalysis) purified treatment to pollutant engine exhaust port is outer, and tail gas is purified before entering air.Three-way catalyst (TWC) is the current main and effective method for the process of motor-vehicle tail-gas external purification.Three-way catalyst has developed into forth generation product, i.e. single palladium three-way catalyst.Pd/Na
2o/K
2o/ γ-Al
2o
3be a kind of single palladium three-way catalyst completely newly, alkali (soil) metal can improve three-way catalyst high-temperature behavior effectively, and has unique adsorption selection active to nitrogen oxide.
Regeneration recovery method at present for three phase catalyst mainly contains wet method and pyrogenic process, but the performance of the rate of recovery of these two kinds of methods and reconstituted product all can not be satisfactory.
Summary of the invention
The invention provides a kind of comprehensive renovation process of catalyst, be mainly used in Pd/Na
2o/K
2the three-way catalyst that O/C etc. are similar, method is simple to operate, and cost is low, excellent performance after catalyst regeneration, reproducible.
To achieve these goals, the present invention adopts following technical scheme: a kind of Pd/Na
2o/K
2the renovation process of O/C three-way catalyst, comprises the following steps:
(1) by poisoning Pd/Na
2o/K
2after O/C three-way catalyst is washed, be soaked in dilution heat of sulfuric acid, regenerate 2-5h under heating using microwave, regeneration temperature is at 40-50 DEG C, regeneration solid-to-liquid ratio (volume of the addition/dilute sulfuric acid of catalyst) is 15-25g/L, then air drying 15-24h;
(2) catalyst nitrogen step (1) obtained and the plasma of oxygen carry out activating and regenerating, regeneration condition is: adopt the pulse power, crest voltage is 5-8kV, and frequency is 100-200hz, recovery time is 1-2h, and temperature is 100-150 DEG C;
(3) catalyst step (2) obtained is the H of 15-20% in concentration
2o
2soak 1-5h in solution, then at 80-100 DEG C, drying obtains.
In a preferred embodiment of the present invention, the mass concentration of dilute sulfuric acid is 20-30%.
In a preferred embodiment of the present invention, heating using microwave adopts heating using microwave reacting furnace to realize.
Regeneration methods of the invention may be used for the three-way catalyst of various level of deactivation, also may be used for the three-way catalyst of other inactivations.
Beneficial effect of the present invention is: for Pd/Na
2o/K
2o/C three-way catalyst, the present invention, by long-term experimental study, finds to adopt micro wave regeneration to combine with the method that low temperature plasma regenerates, regeneration process can be made to obtain significant optimization, by the catalyst that processes again through H
2o
2regeneration of waste liquor, make again the performance of catalyst be improved further, service life is more stable, reproducible, is suitable for industrial wide popularization and application.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described:
Embodiment 1
By the Pd/Na of inactivation
2o/K
2o/C three-way catalyst is handled as follows:
(1) by poisoning Pd/Na
2o/K
2after O/C three-way catalyst is washed, being soaked into mass concentration is in 20% dilution heat of sulfuric acid, regenerates 3h under heating using microwave, and regeneration temperature is at 40 DEG C, and regeneration solid-to-liquid ratio is 20g/L, then air drying 15h;
(2) catalyst nitrogen step (1) obtained and the plasma of oxygen carry out activating and regenerating, and regeneration condition is: adopt the pulse power, crest voltage is 8kV, and frequency is 150hz, and the recovery time is 2h, and temperature is 100 DEG C;
(3) catalyst step (2) obtained is the H of 15% in concentration
2o
23h is soaked in solution, then dry at 80 DEG C, obtain dried three-way catalyst.
Laboratory simulation air distribution system measures Pd/Na
2o/K
2o/C three-way catalyst is active.Distribution consists of O
20.80%, C
3h
6750ppm, NO 1000ppm, CO 1.00%, with N
2make spirit, probe temperature is 400 DEG C, and air speed is 60000h
-1.Survey NOx content by Ministry of Coal Industry standard MT60-1995, remaining gas content measures on SP-3400 gas chromatograph.Do carrier gas with nitrogen, adopt the T-shaped packed column of Propack and 13X type molecular sieve packed column (TCD) separated island form O
2, CO and N
2content; Adopt and activate Al with KCl
2o
3what apply dissolves silicon wide bore capillary column (FID) separated island form hydrocarbon.Test result is as follows:
Table 1 Pd/Na
2o/K
2the performance test results of O/C three-way catalyst
As can be seen from above-mentioned performance test, the conversion ratio of the three-way catalyst after regeneration exceeds multiple percentage point than the conversion ratio of freshly prepd fresh catalyst, and service life stablizes.
Be understandable that, the illustrative embodiments that above embodiment is only used to principle of the present invention is described and adopts, but the present invention is not limited thereto.For those skilled in the art, without departing from the spirit and substance in the present invention, can make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (3)
1. a Pd/Na
2o/K
2the renovation process of O/C three-way catalyst, comprises the following steps:
(1) by poisoning Pd/Na
2o/K
2after O/C three-way catalyst is washed, be soaked in dilution heat of sulfuric acid, regenerate 2-5h under heating using microwave, regeneration temperature is at 40-50 DEG C, regeneration solid-to-liquid ratio (volume of the addition/dilute sulfuric acid of catalyst) is 15-25g/L, then air drying 15-24h;
(2) catalyst nitrogen step (1) obtained and the plasma of oxygen carry out activating and regenerating, regeneration condition is: adopt the pulse power, crest voltage is 5-8kV, and frequency is 100-200hz, recovery time is 1-2h, and temperature is 100-150 DEG C;
(3) catalyst step (2) obtained is the H of 15-20% in concentration
2o
2soak 1-5h in solution, then at 80-100 DEG C, drying obtains.
2. renovation process according to claim 1, is characterized in that, the mass concentration of dilute sulfuric acid is 20-30%.
3. renovation process according to claim 1, is characterized in that, heating using microwave adopts heating using microwave reacting furnace to realize.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610393467.6A CN106000421B (en) | 2015-02-25 | 2015-02-25 | A kind of regeneration method of three-way catalyst |
| CN201510086738.9A CN104624205B (en) | 2015-02-25 | 2015-02-25 | A kind of Pd/Na2o/K2the renovation process of O/C three-way catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510086738.9A CN104624205B (en) | 2015-02-25 | 2015-02-25 | A kind of Pd/Na2o/K2the renovation process of O/C three-way catalyst |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610393467.6A Division CN106000421B (en) | 2015-02-25 | 2015-02-25 | A kind of regeneration method of three-way catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104624205A true CN104624205A (en) | 2015-05-20 |
| CN104624205B CN104624205B (en) | 2016-12-07 |
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|---|---|---|---|
| CN201610393467.6A Active CN106000421B (en) | 2015-02-25 | 2015-02-25 | A kind of regeneration method of three-way catalyst |
| CN201510086738.9A Expired - Fee Related CN104624205B (en) | 2015-02-25 | 2015-02-25 | A kind of Pd/Na2o/K2the renovation process of O/C three-way catalyst |
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| CN201610393467.6A Active CN106000421B (en) | 2015-02-25 | 2015-02-25 | A kind of regeneration method of three-way catalyst |
Country Status (1)
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107486253A (en) * | 2017-08-30 | 2017-12-19 | 大连民族大学 | A kind of dielectric barrier discharge plasma makes the Ag/Al of inactivation2O3Catalyst original position regeneration method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0187007A2 (en) * | 1984-12-14 | 1986-07-09 | Engelhard Corporation | Porous mullite |
| CN102614874A (en) * | 2011-01-28 | 2012-08-01 | 比亚迪股份有限公司 | Preparation method of alumina slurry, automobile exhaust purification catalyst containing the alumina slurry and preparation method of the automobile exhaust purification catalyst containing the alumina slurry |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4682363B2 (en) * | 2006-08-25 | 2011-05-11 | 独立行政法人産業技術総合研究所 | Method and apparatus for regenerating noble metal supported catalyst |
| CN103736393B (en) * | 2014-01-16 | 2016-04-20 | 昆明理工大学 | A kind of low temperature plasma removes the method for nitrogen oxide |
| CN104190479B (en) * | 2014-08-01 | 2016-06-29 | 中国华能集团清洁能源技术研究院有限公司 | A kind of renovation process of microwave-assisted denitrating catalyst |
| CN104190477A (en) * | 2014-09-09 | 2014-12-10 | 华电高科（高碑店）环保技术有限公司 | Method for regenerating titanium-based vanadium-series SCR (Selective Catalytic Reduction) denitration catalyst |
| CN104324764B (en) * | 2014-09-22 | 2016-05-18 | 攀枝花市正源科技有限责任公司 | Stop up reclaiming method and the regeneration SCR catalyst carrier of the SCR catalyst of inactivation |
| CN104289258A (en) * | 2014-10-08 | 2015-01-21 | 於承志 | Acid pickling regenerating liquid for denitration catalyst and regenerating method |
-
2015
- 2015-02-25 CN CN201610393467.6A patent/CN106000421B/en active Active
- 2015-02-25 CN CN201510086738.9A patent/CN104624205B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0187007A2 (en) * | 1984-12-14 | 1986-07-09 | Engelhard Corporation | Porous mullite |
| CN102614874A (en) * | 2011-01-28 | 2012-08-01 | 比亚迪股份有限公司 | Preparation method of alumina slurry, automobile exhaust purification catalyst containing the alumina slurry and preparation method of the automobile exhaust purification catalyst containing the alumina slurry |
Non-Patent Citations (1)
| Title |
|---|
| 冯长根 等: "Pd/Na2O/K2O/γ-2Al2O3三元催化活性分析与评价", 《工业催化》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107486253A (en) * | 2017-08-30 | 2017-12-19 | 大连民族大学 | A kind of dielectric barrier discharge plasma makes the Ag/Al of inactivation2O3Catalyst original position regeneration method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106000421B (en) | 2018-07-27 |
| CN104624205B (en) | 2016-12-07 |
| CN106000421A (en) | 2016-10-12 |
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