CN108212152A - A kind of oxide carried type NO of low temperature cerium zirconiumxCatalyst and its application - Google Patents
A kind of oxide carried type NO of low temperature cerium zirconiumxCatalyst and its application Download PDFInfo
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- CN108212152A CN108212152A CN201611195873.8A CN201611195873A CN108212152A CN 108212152 A CN108212152 A CN 108212152A CN 201611195873 A CN201611195873 A CN 201611195873A CN 108212152 A CN108212152 A CN 108212152A
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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
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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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
- B01J23/38—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
- B01J23/63—Platinum group metals with rare earths or actinides
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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
Abstract
The oxide carried type NO of low temperature cerium zirconium disclosed by the inventionxCatalyst and its application, its chemical formula of catalyst are Pt/BaO/CexZr(1‑x)O2.It is assembled, and impregnate Ba and Pt step by step on carrier by cerium zirconium elements different in catalyst, significantly improves its low temperature active, so as to obtain the NO in lean-combustion engine (light-duty gasoline engine and diesel engine) tail gasxThere is the catalyst of preferable low temperature active in processing, so as to the low temperature active widened the active temperature windows of catalyst, improved catalyst.
Description
Technical field
The present invention relates to a kind of oxide carried type NOxStorage and reduction catalyst and its application, particularly a kind of low temperature cerium
Zirconium oxide support type NOxCatalyst and its application, the oxide carried type NO of cerium zirconium that specially a kind of low temperature active improvesxStorage
Deposit reducing catalyst and its application.
Background technology
Lean-combustion engine (light-duty gasoline engine and diesel engine) is because of its higher fuel economy and low CO2It discharges and receives
Extensive concern.But a large amount of NO in tail gasxThe environmental problems such as photochemical fog, acid rain, and serious prestige can not only be caused
Coerce the health of the mankind.Therefore, lean-combustion engine NO how is removedxTail gas is the hot spot in current environmental catalysis field.NOx
Storage reduction (NSR) technology becomes most practical prospect because without additional reducing agent, facility is added without building reducing agent
NOxOne of post-processing technology.
According to lean-combustion engine operating condition, during lean burn to homogeneous theory air-fuel ratio combustion is layered, air-fuel
Compare consecutive variations.Therefore, triple effect catalytic converter can not purify the NO in discharge gasx.This is because three way catalytic converter
Device will carry out NO using the HC in exhaust or COxThe reason of reduction reaction.In lean burn, remained in discharge gas very much
Oxygen, it is impossible to carry out NOxReduction reaction.In routine techniques, in order to make NOxType of attracting deposit catalyst obtains efficient function, temperature
It preferably must be held in the range of 250-500 DEG C.
NSR technologies are the transient operations that catalyst is periodically switched between lean-burn and dense combustion wherein.In lean-burn item
Under part, NO is oxidized to NO2, stored in the form of nitrate；Under the conditions of dense combustion, nitrate decomposes release NOx, then gone back
Former agent is converted into N2.When lean-burn-dense combustion time ratio is higher, the fuel economy of engine is then higher.NSR catalyst generally includes
Three components：For storing NOxSubstance, generally alkali or alkaline earth metal；Noble metal, usually as the oxidation and reduction of NO
Active site；The carrier of high-specific surface area.Diesel exhaust gas wider range (150-550 DEG C), exhaust temperature during cold start-up
Spend it is minimum can be to 100 DEG C.Traditional Pt/BaO/Al2O3Optimum activity temperature window for 300-350 DEG C, be catalyzed in low temperature section
Activity is bad.
A kind of ceric oxide nanorod supported nitrogen oxide storage catalyst of the prior art and its preparation method and application,
It is disclosed in CN201510705645.X and a kind of novel ceric oxide nanorod loaded catalyst is prepared for hydrothermal synthesis method
(Pt/BaO/CeO2), there is preferable activity (200-400 DEG C) in middle-temperature section.But the catalyst there are still low temperature active not
The shortcomings that sufficient, is not suitable for being applied to exhaust temperature relatively low operating condition during diesel vehicle cold start-up.
Invention content
To solve the above problems, the oxide carried type NO of low temperature cerium zirconium disclosed by the inventionxCatalyst and its application, we
Case is assembled, and impregnate Ba and Pt step by step on carrier by cerium zirconium elements different in catalyst, makes its low temperature active bright
It is aobvious to improve, so as to obtain the NO in lean-combustion engine (light-duty gasoline engine and diesel engine) tail gasxThere is preferable low temperature to live in processing
Property catalyst, so as to widened the active temperature windows of catalyst, improve catalyst low temperature active.
The oxide carried type NO of low temperature cerium zirconium disclosed by the inventionxCatalyst, chemical formula Pt/BaO/CexZr(1-x)O2。
In the present solution, the Lacking oxygen based on cerium base NSR catalyst surfaces is in NOxStorage reduction reaction in play the role of it is very important,
Lacking oxygen activates oxygen and then forms active oxygen, promotes the oxidation of NO with NOxAdsorption storage, and then improve catalyst it is anti-
It should activity；Meanwhile ZrO2Doping can improve CeO2The concentration of upper oxygen vacancies improves storage put oxygen performance (OSC)；Pass through Ce/Zr
The modulation of ratio can adjust oxygen vacancies is formed in cerium zirconium sosoloid difficulty or ease and concentration.So as to this programme, with cerium zirconium composite oxygen
Compound obtains the more excellent NO of low temperature active for carrierxStorage and reduction catalyst, the catalyst have good in low-temperature zone
Catalytic performance, meet job requirement during diesel vehicle cold start-up.
The oxide carried type NO of low temperature cerium zirconium disclosed by the inventionxA kind of improvement of catalyst, Pt/BaO/CexZr(1-x)O2
The value range of middle x is 0-1.This programme is made up of suitable Ce/Zr elements and is configured, and it is empty can to adjust oxygen in cerium zirconium sosoloid
The difficulty or ease and concentration that cave is formed.So as to which cerium zirconium compound oxide be made to obtain the more excellent NO of low temperature active for carrierxStorage
Reducing catalyst, the catalyst have good catalytic performance in low-temperature zone (special 100-150 DEG C of section range), meet diesel oil
Job requirement during vehicle cold start-up.
The oxide carried type NO of low temperature cerium zirconium disclosed by the inventionxA kind of improvement of catalyst, Pt/BaO/CexZr(1-x)O2
The value of middle x is following any：0、0.1、0.3、0.5、0.7、0.9、1.
The oxide carried type NO of low temperature cerium zirconium disclosed by the inventionxA kind of improvement of catalyst, Pt/BaO/CexZr(1-x)O2
The value 0.1 of middle x.This programme has good low-temperature catalyzed performance, at 150 to 400 DEG C by selecting specific technical solution
Within the temperature range of, reaction velocity be up to 360,000h-1, when lean-burn-ratio of dense combustion time is 90s-6s, can realize more than 96%
NOxPurification efficiency.Under same reaction conditions, compared with prior art conventional catalyst, particularly Pt/BaO/CeO2Nanometer rods
Catalyst is compared, the NO of this programme at 100 DEG C~150 DEG CxConversion ratio improves~40%.
The oxide carried type NO of low temperature cerium zirconium disclosed by the inventionxA kind of improvement of catalyst, catalyst are as follows by including
It is prepared by the method for step：CexZr(1-x)O2The preparation of nano material carrier；Based on nano material carrier, BaO/CexZr(1-x)
O2The preparation of composite oxides；Based on composite oxides, Pt/BaO/CexZr(1-x)O2The preparation of catalyst.
The oxide carried type NO of low temperature cerium zirconium disclosed by the inventionxA kind of improvement of catalyst, CexZr(1-x)O2Nano material
During the preparation of carrier, with any (such as Ce in the hydrate of cerous nitrate, ammonium ceric nitrate, cerous chlorate, cerous sulfate or more cerium salt
(NO3)3·6H2O) as Ce sources, with Zr (NO3)4·5H2O is as Zr sources.
The oxide carried type NO of low temperature cerium zirconium disclosed by the inventionxA kind of improvement of catalyst, CexZr(1-x)O2Nano material
During the preparation of carrier, Ce sources and the molar ratio (0 of the Ce and Zr in Zr sources:1)-(1:0).
The oxide carried type NO of low temperature cerium zirconium disclosed by the inventionxA kind of improvement of catalyst, CexZr(1-x)O2Nano material
During the preparation of carrier, the molar ratio of Ce sources and the Ce and Zr in Zr sources are following any：0:1、1:9、3:7、5:5、7:3、9:1、1:
0。
The oxide carried type NO of low temperature cerium zirconium disclosed by the inventionxA kind of improvement of catalyst, CexZr(1-x)O2Nano material
During the preparation of carrier, the molar ratio of Ce sources and the Ce and Zr in Zr sources are 1:9.
The oxide carried type NO of low temperature cerium zirconium disclosed by the inventionxCatalyst NO in lean-combustion engine tail gasxIn processing
Using.
Compared with prior art, it is as follows the advantages of this programme：
1st, the doping of Zr significantly improves Pt/BaO/CeO2The low temperature NSR reactivities of catalyst.With Ce/Zr=1:9
CeZrOxPt/BaO/CeZrO for carrierxCatalyst has optimal NOxConversion ratio, reaction temperature have when being 150-400 DEG C
More than 96% NOxRemoval rate has widened reaction temperature window significantly.
2nd, 360,000h-1 are up in air speed, lean-burn-dense combustion time is under conditions of 90s-6s, has carried out 60 dynamics and followed
After ring experiment, Pt/BaO/Ce0.1Zr0.9O2Catalyst still has excellent NOxIt is stronger resistance to illustrate that the catalyst has for conversion ratio
Long property.
3、Pt/BaO/Ce0.1Zr0.9O2Catalyst surface trivalent cerium concentration is higher, i.e., containing abundant surface Lacking oxygen, carries
The high mobility of oxygen, promotes NOxAbsorbing and storing and release NOxReduction so that there is the catalyst excellent reaction to live
Property.
4th, the catalyst is suitable for exhaust temperature relatively low catalytic purification of nitroxide operating condition during diesel vehicle cold start-up.
Specific embodiment
With reference to embodiment, the present invention is furture elucidated, it should be understood that following specific embodiments are only used for
It is bright the present invention rather than limit the scope of the invention.
Embodiment
In the present embodiment, its chemical formula of catalyst is Pt/BaO/CexZr(1-x)O2。
It is distinguished with above-described embodiment, catalyst Pt/BaO/CexZr(1-x)O2The value range of middle x is 0-1.
It is distinguished with above-described embodiment, catalyst Pt/BaO/CexZr(1-x)O2The value of middle x is following any：0、
0.1、0.3、0.5、0.7、0.9、1。
It is distinguished with above-described embodiment, catalyst Pt/BaO/CexZr(1-x)O2The value 0.1 of middle x.
It is distinguished with above-described embodiment, catalyst is prepared by the method included the following steps：CexZr(1-x)O2Nanometer material
Expect the preparation of carrier；Based on nano material carrier, BaO/CexZr(1-x)O2The preparation of composite oxides；With composite oxides
Based on, Pt/BaO/CexZr(1-x)O2The preparation of catalyst.
It is distinguished with above-described embodiment, CexZr(1-x)O2During the preparation of nano material carrier, with Ce (NO3)3·6H2O makees
For Ce sources (Ce sources can also be cerous nitrate, ammonium ceric nitrate, cerous chlorate, cerous sulfate or more cerium salt hydrate in it is any),
With Zr (NO3)4·5H2O is as Zr sources.
It is distinguished with above-described embodiment, CexZr(1-x)O2During the preparation of nano material carrier, the Ce in Ce sources and Zr sources with
The molar ratio (0 of Zr:1)-(1:0).
It is distinguished with above-described embodiment, CexZr(1-x)O2During the preparation of nano material carrier, the Ce in Ce sources and Zr sources with
The molar ratio of Zr is following any：0:1、1:9、3:7、5:5、7:3、9:1、1:0.
It is distinguished with above-described embodiment, CexZr(1-x)O2During the preparation of nano material carrier, the Ce in Ce sources and Zr sources with
The molar ratio of Zr is 1:9.
Catalyst disclosed by the invention can be applied to the tail gas NO of lean-combustion enginexProcessing, especially suitable for including
Gasoline engine (including but not limited to light-duty gasoline engine) and diesel engine (including but not limited to light diesel engine) are not limited to, is particularly existed
Catalytic efficiency is higher during exhaust temperature relatively low low temperature section, significant effect.
Specifically by taking specific examples below as an example, illustrate the excellent part of the present invention program respectively：
With Ce (NO3)3·6H2O is as Ce sources, with Zr (NO3)4·5H2O is as Zr sources, and NaOH is as precipitating reagent, Ce and Zr
Molar ratio be respectively 0:1、1:9、3:7、5:5、7:3、9:1 and 1:0.First, cerous nitrate and zirconium nitrate are configured to solution, filled
After dividing stirring and dissolving, suitable NaOH solution (can also be KOH solution) is added in thereto, after stirring 1h, in 100 DEG C of baking ovens
Hydro-thermal reaction 12h.To reaction products therefrom filtered and washed, place it in 60 DEG C of oven dried overnights later, most after
4h is roasted in air atmosphere for 550 DEG C, it is spare.ZrO is made2、Ce0.1Zr0.9O2、Ce0.3Zr0.7O2、Ce0.5Zr0.5O2、
Ce0.7Zr0.3O2、Ce0.9Zr0.1O2And CeO2Nano material is respectively designated as Z, C1Z9, C3Z7, C5Z5, C7Z3, C9Z1 and C.
Secondly, with the Ce preparedxZr1-xO2Nano material is carrier, and a certain amount of barium acetate is prepared solution, a certain amount of
Carrier be placed in above-mentioned solution, stir 1h after carry out decompression rotary evaporation, 60 DEG C of baking ovens are put in after moisture is evaporated and were dried
In 500 DEG C of Muffle kiln roasting 3h under air atmosphere, BaO/Ce is made in nightxZr1-xO2Composite oxides (in composite oxides,
The load capacity of barium monoxide is following any：5wt%, 5.1wt%, 5.2wt%, 5.3wt%, 5.4wt%, 5.5wt%,
5.6wt%, 5.7wt%, 5.8wt%, 5.9wt%, 6wt%, 6.1wt%, 6.2wt%, 6.3wt%, 6.4wt%,
6.5wt%, 6.6wt%, 6.7wt%, 6.8wt%, 6.9wt%, 7wt%, 7.1wt%, 7.2wt%, 7.3wt%,
7.4wt%, 7.5wt%, 7.6wt%, 7.7wt%, 7.8wt%, 7.9wt%, 8wt%, 8.1wt%, 8.2wt%,
8.3wt%, 8.4wt%, 8.5wt%, 8.6wt%, 8.7wt%, 8.8wt%, 8.9wt%, 9wt%, 9.1wt%,
9.2wt%, 9.3wt%, 9.4wt%, 9.5wt%, 9.6wt%, 9.7wt%, 9.8wt%, 9.9wt%, 10wt% and model
Enclose the interior other arbitrary values of 5-10wt%).
Finally, by a certain amount of PtCl4Prepare solution, a certain amount of above-mentioned obtained BaO/CexZr1-xO2Composite oxides are put
In wherein, decompression rotary evaporation is carried out after stirring 1h, 60 DEG C of baking oven drying are put in after moisture is evaporated overnight, under air atmosphere
In 500 DEG C of Muffle kiln roasting 3h, Pt/BaO/Ce is madexZr1-xO2Catalyst (in catalyst, to be following appoint by the load capacity of platinum
One：0.1wt%, 0.2wt%, 0.3wt%, 0.4wt%, 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt%,
1wt%, 1.1wt%, 1.2wt%, 1.3wt%, 1.4wt%, 1.5wt%, 1.6wt%, 1.7wt%, 1.8wt%,
The other arbitrary values of 0.1-2wt% in 1.9wt%, 2wt% and range), be respectively designated as PBZ, PBC1Z9, PBC3Z7,
PBC5Z5, PBC7Z3, PBC9Z1 and PBC by seven kinds of catalyst accordingly labeled as example 1- examples 7, while need special
Illustrate, there are the difference of the molar ratio of Ce and Zr, remaining features between the technical solution of the example 1-7 of the same system
All same.
In made most preferred catalysts (PBC1Z9, embodiment 2), within the temperature range of 150 to 400 DEG C, instead
Air speed is answered to be up to 360,000h-1, when lean-burn-ratio of dense combustion time is 90s-6s, can realize more than 96% NOxPurification efficiency.
With the Pt/BaO/CeO of same reaction conditions2Nanorods Catalyst is compared, the NO at 100 DEG C~150 DEG CxConversion ratio improves
About 40%.
Take Pt/BaO/CexZr1-xO2Catalyst series, quality 100mg, 40-120 mesh are put into catalyst activity evaluation dress
It puts, activity rating carries out in fixed bed reactors.Test condition is：Lean-burn (90s) NO=500ppm, O2=8%, N2It is flat
Weigh gas；Dense combustion (6s) H2=3%, N2For Balance Air；Lean-burn-dense combustion cycle number：60, total flow=300mL/min, reaction
Air speed is 360,000h-1.Test result is as follows shown in table one：
Table one
Take Pt/BaO/CexZr1-xO2Catalyst series, quality 100mg, 40-120 mesh are put into catalyst activity evaluation dress
It puts, activity rating carries out in fixed bed reactors.Test condition is：Lean-burn (90s) NO=500ppm, O2=8%, N2It is flat
Weigh gas；Dense combustion (5s) H2=3%, N2For Balance Air；Lean-burn-dense combustion cycle number：60, total flow=300mL/min, reaction
Air speed is 360,000h-1.Test result is as follows shown in table two：
Table two
Take Pt/BaO/CexZr1-xO2Catalyst series, quality 100mg, 40-120 mesh are put into catalyst activity evaluation dress
It puts, activity rating carries out in fixed bed reactors.Test condition is：Lean-burn (90s) NO=500ppm, O2=8%, N2It is flat
Weigh gas；Dense combustion (4s) H2=3%, N2For Balance Air；Lean-burn-dense combustion cycle number：60, total flow=300mL/min, reaction
Air speed is 360,000h-1.Test result is as follows shown in table three：
Table three
This place embodiment is in place of the claimed non-limit of technical scope midrange and in embodiment technology
The new technical solution formed is replaced on an equal basis to single or multiple technical characteristics in scheme, equally all the present invention claims
In the range of protection；Simultaneously the present invention program it is all enumerate or unrequited embodiment in, in the same embodiment each
Parameter is merely representative of an example (i.e. a kind of feasible scheme) for its technical solution, and between parameters and is not present stringent
Cooperation and qualified relation, wherein each parameter can be replaced mutually when stating and asking without prejudice to axiom and the present invention, special declaration
Except.
The technical means disclosed in the embodiments of the present invention is not limited to the technical means disclosed in the above technical means, and is further included
By more than technical characteristic arbitrarily the formed technical solution of combination.The above is the specific embodiment of the present invention, should be referred to
Go out, for those skilled in the art, without departing from the principle of the present invention, can also make several
Improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (10)
1. a kind of oxide carried type NO of low temperature cerium zirconiumxCatalyst, chemical formula Pt/BaO/CexZr(1-x)O2。
2. the oxide carried type NO of low temperature cerium zirconium according to claim 1xCatalyst, which is characterized in that the Pt/BaO/
CexZr (1-x)O2The value range of middle x is 0-1.
3. the oxide carried type NO of low temperature cerium zirconium according to claim 2xCatalyst, which is characterized in that the Pt/BaO/
CexZr (1-x)O2The value of middle x is following any：0、0.1、0.3、0.5、0.7、0.9、1.
4. the oxide carried type NO of low temperature cerium zirconium according to claim 3xCatalyst, which is characterized in that the Pt/BaO/
CexZr (1-x)O2The value 0.1 of middle x.
5. according to any oxide carried type NO of low temperature cerium zirconium of claim 1-4xCatalyst, which is characterized in that described to urge
Agent is prepared by the method included the following steps：CexZr(1-x)O2The preparation of nano material carrier；Using nano material carrier as base
Plinth, BaO/CexZr(1-x)O2The preparation of composite oxides；Based on composite oxides, Pt/BaO/CexZr(1-x)O2Catalyst
It prepares.
6. the oxide carried type NO of low temperature cerium zirconium according to claim 5xCatalyst, which is characterized in that the CexZr(1-x)
O2During the preparation of nano material carrier, in the hydrate of cerous nitrate, ammonium ceric nitrate, cerous chlorate, cerous sulfate or more cerium salt
It is any as Ce sources, with Zr (NO3)4·5H2O is as Zr sources.
7. the oxide carried type NO of low temperature cerium zirconium according to claim 6xCatalyst, which is characterized in that the CexZr(1-x)
O2During the preparation of nano material carrier, Ce sources and the molar ratio (0 of the Ce and Zr in Zr sources:1)-(1:0).
8. the oxide carried type NO of low temperature cerium zirconium according to claim 7xCatalyst, which is characterized in that the CexZr(1-x)
O2During the preparation of nano material carrier, the molar ratio of Ce sources and the Ce and Zr in Zr sources are following any：0:1、1:9、3:7、5:5、
7:3、9:1、1:0。
9. the oxide carried type NO of low temperature cerium zirconium according to claim 8xCatalyst, which is characterized in that the CexZr(1-x)
O2During the preparation of nano material carrier, the molar ratio of Ce sources and the Ce and Zr in Zr sources are 1:9.
10. a kind of oxide carried type NO of low temperature cerium zirconiumxCatalyst NO in lean-combustion engine tail gasxApplication in processing.
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Application publication date: 20180629 |