CN109529859A - A kind of multi-functional mesoporous cerium based sosoloid catalyst for catalytic cleaning of car tail gas - Google Patents
A kind of multi-functional mesoporous cerium based sosoloid catalyst for catalytic cleaning of car tail gas Download PDFInfo
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- 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
- B01J23/83—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 rare earths or actinides
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- 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
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
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- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
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- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
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- B01D2258/00—Sources of waste gases
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- B01D2258/012—Diesel engines and lean burn gasoline engines
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Abstract
The present invention relates to a kind of mesoporous cerium based solid solution composite oxide material of Mobyneb, the chemical structural formula of the catalyst is Ce0.7Co0.3‑xFexO2‑ζ(0≤x≤0.3).Catalyst is using cerous nitrate, cobalt nitrate, ferric nitrate, cetab (CTAB) and dehydrated alcohol as raw material.The raw materials used cheap and easy to get, mild condition of the method for the present invention, process of preparing is simple, environmentally protective, has important scientific meaning and good application prospect.Cerium based sosoloid catalyst obtained has that large specific surface area, partial size be small, meso-hole structure of even particle distribution.Catalyst has multiple functions simultaneously, can be respectively used to the fields such as catalysis burning removal diesel vehicle soot particulate matter, catalytic oxidation NO, CO catalytic oxidation and low temperature NOx absorption.
Description
Technical field
The present invention relates to a kind of preparations of multi-functional mesoporous cerium base catalyst for catalytic cleaning of car tail gas, and its
Catalysis burning removal diesel vehicle soot particulate matter, NO, CO and low temperature NOx absorption etc. fields application, belong to rare earth material system
Standby and catalytic field.
Background technique
On December 23rd, 2016, Environmental Protection Department have issued " light-duty vehicle pollutant emission limit and measurement method (China
6th stage) " formal Press release (referred to as rear: " formal Press release "), indicate that " state six " discharge standard will be in the contribution
The year two thousand twenty executes from July 1.This is one of most stringent of compact car discharge standard in the whole world.It specifically mentions: implementing new in file
Standard, the main catalyst (increasing noble metal dosage etc.) improved in catalytic converter improve fuel injection manner, increase canister
Volume, improvement fuel system leakproofness, upgrading OBD system etc..Since state, China five and emission of diesel engine limit value are low, " state six "
Fuel neutrality principle will be used for the first time, and diesel vehicle upgrades difficulty and is higher than gasoline car.
It is well known that diesel vehicle due to the advantages such as its thermal efficiency height, good economy performance, CO2 emissions are low and it is extensive
Using, however diesel car bring facilitate while, also generate serious pollution.Chinese haze polluted day in recent years
Become serious, it has been investigated that, the PM in tail gas is the major reason to form haze.NOx is nitrogen oxides NO, NO2、N2O、
N2O2Deng general name, the nitrogen oxides being discharged in diesel exhaust gas is mainly NO and NO2.NO is a kind of gas of colorless and odorless, poison
Property is little, can generate NO in air2, and NO2It is a kind of rufous, there is intense irritation gas.It can be under strong sunlight
Photochemical reaction occurs for HC, forms secondary pollution, the regionality atmosphere such as acid rain and photochemical fog that some areas frequently occur
The NOx and HC of pollution problem and exhaust emissions of diesel engine are closely related.HC and CO content is lower in exhaust gas from diesel vehicle, and opposite
It is easy to purify, but CO is a kind of toxic gas, poisoning even death will be made one by sucking a small amount of gas.So controlling and reducing
Automotive emission is current urgent problem to be solved.
Currently, the catalyst of the catalytic cleaning of car tail gas used both at home and abroad mainly has noble metal catalyst, eutectic point
Catalyst and multicomponent composite oxide catalysts etc..Wherein, noble metal catalyst has good low temperature active, but holds
Easy sulphur (S) poisoning and deactivation, poor high temperature stability；And noble metal is expensive, and this also constrains the reality of noble metal catalyst
Using.The alkali metal salt catalyst high temperature of eutectic point can melt, and cause it with mobility, and then improve catalyst and soot
Contact condition between particle, promotes the catalysis oxidation of carbon soot particles, but base metal catalysts fusing point is low, alkaline strong feature
Also the disadvantages of bringing poor stability, corrosion ceramics DPF.And multicomponent composite oxide catalysts are with perovskite or perovskite-like
Type catalyst and spinel structure catalyst are representative, this type oxide has that high mechanical strength, thermal stability is good, price is low
Honest and clean, the advantages that catalytic activity is higher, but it is chiefly used in carbon soot particles combustion reaction, it is functional more single.
CeO2In there are easy Ce3+↔Ce4+It appraises at the current rate conversion, so that it is possessed good oxygen storage capacity, so extensive
For three-way catalyst (Three-Way Catalysts, TWC) hydrogen-storing material.But CeO2Thermal stability is lower, is undergoing
Easy-sintering after high temperature, and then lose its excellent oxygen storage capacity.It, usually will be other in order to improve its heat resistance and oxygen storage capacity
It is metal-doped into CeO2Lattice forms solid solution, oxide, and then shows desired physicochemical property: the specific surface area of increase, increases
The promotion of the Lacking oxygen and redox property that add.Simultaneously because CeO2It is with splendid electron transfer capacity so available
Make active component, also can be used as modified additive and carrier come using.And transition metal Co, Fe have excellent redox special
Property, its either high redox performance can be made full use of to realize low-temperature catalytic oxidation.
For these reasons, a kind of multi-functional mesoporous cerium base catalyst for catalytic cleaning of car tail gas is researched and developed
With important economy and practical significance.
Summary of the invention
The object of the present invention is to provide a kind of multi-functional mesoporous cerium based solid solution catalysis for catalytic cleaning of car tail gas
Agent.
A kind of preparation method of the multi-functional mesoporous cerium based sosoloid catalyst for catalytic cleaning of car tail gas of the present invention,
The following steps are included:
(1) suitable Ce (NO is weighed in proportion3)3·6H2O、Co(NO3)3·6H2O、Fe(NO3)3·9H2O is dissolved in deionized water
Middle stirring is made into mixed solution；(2) it weighs appropriate CTAB to be dissolved in deionized water, be stirred at 30 DEG C to being completely dissolved.With
Beaker is added dropwise as precipitating reagent in NaOH under lasting stirring, and demarcates pH ≈ 11 with pH meter；(3) it stands to after room temperature, with true
Empty pumping filter, is washed out, dries, calcines；(4) it is cooled to room temperature taking-up, sample obtained is that the mesoporous cerium base synthesized is answered
Close oxide catalyst.
The present invention compared with prior art, has following obvious substantive distinguishing features.
1. the catalyst that the present invention synthesizes is multi-functional mesoporous cerium sill.
2. the present invention is by a certain percentage while to be doped into two kinds of metals of Co, Fe in cerium based solid solution.
3. the cerium base catalyst that the present invention synthesizes has, large specific surface area, partial size be small, mesoporous knot of even particle distribution
Structure.
4. the present invention simultaneously have catalysis burning removal diesel vehicle soot particulate matter, catalytic oxidation NO, CO catalytic oxidation with
And the functions such as low temperature NOx absorption.
5. the method for the present invention is simple and easy, preparation condition is mild, and raw material is cheap and easy to get, and toxic reaction raw materials are not used,
It is a kind of environmental-friendly green syt catalyst.
Detailed description of the invention
Fig. 1 is Ce prepared by the present invention0.7Co0.3-xFexO2-ζThe pore size distribution curve figure of (x=0,0.15,0.3) catalyst
Spectrum；
Fig. 2 is Ce prepared by the present invention0.7Co0.3-xFexO2-ζ(x=0,0.15,0.3) catalyst is in O2Carbon soot particles under atmosphere
Object catalysis oxidation map；
Fig. 3 is Ce prepared by the present invention0.7Co0.3-xFexO2-ζ(x=0,0.15,0.3) catalyst is in NO+O2Soot under atmosphere
Grain object catalysis oxidation map；
Fig. 4 is Ce prepared by the present invention0.7Co0.3-xFexO2-ζThe NO of (x=0,0.15,0.3) catalyst aoxidizes map；
Fig. 5 is Ce prepared by the present invention0.7Co0.3-xFexO2-ζThe CO of (x=0,0.15,0.3) catalyst aoxidizes map.
Specific embodiment
The present invention is further explained in the light of specific embodiments, and the present invention includes but is not limited to following implementation
Example.
Embodiment one:
(1) Ce (NO is added in (7:1.5:1.5) in molar ratio in deionized water3)3·6H2O 、Co(NO3)3·6H2O、Fe
(NO3)3·9H2O stirs to form mixed solution, then weighs appropriate CTAB and is dissolved in deionized water, is stirred later to completely molten
Solution.
(2) continue to be slowly added to NaOH solution in the solution obtained under stirring to step (1), and demarcated with pH meter
pH≈11。
(3) it stands to room temperature, the solution that step (2) obtains is filtered with vacuum pump, is washed out, dries, calcining drop
It is taken out after to room temperature, obtained sample is a kind of mesoporous cerium-based composite oxides catalyst, referred to as CCF0.15.
It is detected and is found by XRD, transition metal enters CeO2Cerium based solid solution composite oxide material is formed in lattice,
And partial size is small, even particle distribution；By test, specific surface area 92.0m2/g；Fig. 1 is the pore size distribution curve figure of sample
Spectrum, it can be seen that the pore size distribution curve of this type belongs to mesoporous material (pore-size distribution is in 2-50 nm), wherein CCF0.15
Most probable diameter is 9nm.
Embodiment two
(1) Ce (NO is added in (7:3) in molar ratio in deionized water3)3·6H2O 、Co(NO3)3·6H2O stirs to form mixing
Then solution weighs appropriate CTAB and is dissolved in deionized water, stirred later to being completely dissolved.
(2) continue to be slowly added to NaOH solution in the solution obtained under stirring to step (1), and demarcated with pH meter
pH≈11。
(3) it stands to room temperature, the solution that step (2) obtains is filtered with vacuum pump, is washed out, dries, calcining drop
It is taken out after to room temperature, obtained sample is a kind of mesoporous cerium-based composite oxides catalyst, referred to as CCF0.
It is detected and is found by XRD, transition metal enters CeO2Cerium based solid solution composite oxide material is formed in lattice,
And partial size is small, even particle distribution；By test, specific surface area 66.0m2/g.Fig. 1 is the pore size distribution curve figure of sample
Spectrum, it can be seen that the pore size distribution curve of this type belongs to mesoporous material (pore-size distribution is in 2-50 nm), and the most probable of CCF0 is straight
Diameter is 6nm.
Embodiment three
(1) Ce (NO is added in (7:3) in molar ratio in deionized water3)3·6H2O 、Fe(NO3)3·9H2O stirs to form mixing
Then solution weighs appropriate CTAB and is dissolved in deionized water, stirred later to being completely dissolved.
(2) continue to be slowly added to NaOH solution in the solution obtained under stirring to step (1), and demarcated with pH meter
pH≈11。
(3) it stands to room temperature, the solution that step (2) obtains is filtered with vacuum pump, is washed out, dries, calcining drop
It is taken out after to room temperature, obtained sample is a kind of mesoporous cerium-based composite oxides catalyst, referred to as CCF0.3.
It is detected and is found by XRD, transition metal enters CeO2Cerium based solid solution composite oxide material is formed in lattice,
And partial size is small, even particle distribution；By test, specific surface area 116.3m2/ g, biggish specific surface area, which is more advantageous to, to be mentioned
High activity；Fig. 1 is the pore size distribution curve map of sample, it can be seen that the pore size distribution curve of this type belongs to mesoporous material
(pore-size distribution is in 2-50 nm), the most probable diameter of CCF0.3 are 5nm.
Example IV
It takes above-described embodiment one, two and three that mesoporous cerium base catalyst is made respectively, diesel engine truck exhaust atmosphere is simulated, with Germany
The soot particulate of the Printex-U carbon black diesel oil substitute machine discharge of Degussa company, is evaluated using temperature programmed oxidation technology
The soot catalytic combustion activity of catalyst.As shown in Fig. 2, in O2Under atmosphere, measured according to carbon-smoke combustion reaction conversion ratio curve
The initiation temperature of carbon-smoke combustion is generally 270~300 DEG C on catalyst, generates CO2Selectivity reach 100%, CO will not be generated
Cause secondary pollution.
As shown in figure 3, in NO+O2Under atmosphere, the initiation temperature of carbon-smoke combustion is reduced to 250~290 DEG C on catalyst, life
At CO2Selectivity equally reach 100%, the generation of no CO, while polluted gas NO can be eliminated.
The obtained catalyst activity of this method is good, and selectivity is high, has with its biggish specific surface area, lesser partial size
It closes.
Embodiment five
It takes above-described embodiment one, two and three that mesoporous cerium base catalyst is made for NO oxidation reaction respectively, catalyst tabletting is ground
The catalyst that 40-80 mesh is filtered out after broken is packed into the reaction tube that diameter is 6mm, and experiment carries out in fixed bed reactors,
Reaction temperature is 150-600 DEG C.
200 DEG C of pretreatment 2h, are switched to NO+O after being cooled to room temperature first under He atmosphere2Atmosphere, later will catalysis
Agent is warming up to 700 DEG C；As shown in figure 4, NO can be effectively oxidized to NO in the presence of mesoporous cerium base catalyst2Even if
100 DEG C of low temperature NO conversion ratios can also be more than 10%；When temperature is more than 200 DEG C, cerium base catalyst accelerates NO oxidation rate,
NO2Reach maximum production quantity at 300-330 DEG C, wherein the maximum NO conversion ratio of CCF0 has reached 70%, illustrates synthesized mesoporous
Cerium base catalyst has excellent NO oxidability.
Embodiment six
It takes above-described embodiment one, two and three that mesoporous cerium base catalyst is made for CO oxidation reaction respectively, catalyst tabletting is ground
The catalyst that 40-80 mesh is filtered out after broken is packed into the reaction tube that diameter is 6mm, and experiment carries out in fixed bed reactors,
Reaction temperature is 100-500 DEG C.
200 DEG C of pretreatment 2h, are switched to CO+O after being cooled to room temperature first under He atmosphere2Atmosphere carries out journey later
Sequence temperature reaction；COx after reaction in tail gas is detected with gas chromatograph, as shown in figure 5, catalyst has good middle low temperature
CO oxidability reaches 50% in the CO conversion ratio of 150 DEG C or so CCF0 and CCF0.15.
Embodiment seven
It takes above-described embodiment one, two and three that mesoporous cerium base catalyst is made respectively and aoxidizes diffusing reflection in situ for the NO at 100 DEG C
Reaction is first handled sample before carrying out sample measurement, and 500 DEG C of pretreatment 1h, are down in room temperature process under He atmosphere,
Specific temperature acquisition background spectrum；It is switched to NO+O later2Atmosphere acquires the sample spectra of relevant temperature.
By diffusing reflection in situ react find, the species of catalyst CCF0 and CCF0.15 adsorption be mainly it is some not
With the NO3-N and NO2-N species of form；As temperature increases, synthesized mesoporous cerium base catalyst is shown quickly
NOx absorbing and storing rate and very big adsorbance, in general, the NOx species of absorption can be with nitrate and nitrous acid
The form of salt is stored in catalyst, then can directly be reacted with adjacent carbon soot particles, or resolve into oxidation
The stronger NO of property2Promote soot catalysis burning.
Claims (5)
1. a kind of preparation method of the multi-functional mesoporous cerium based sosoloid catalyst for catalytic cleaning of car tail gas, feature exist
In the following steps are included:
(1) Ce (NO is added by a certain percentage in deionized water3)3·6H2O 、Co(NO3)3·6H2O、Fe(NO3)3·9H2O is stirred
It mixes to form mixed solution, then weighs a certain amount of CTAB and be dissolved in deionized water, stirred later to being completely dissolved；
(2) continuing under stirring, be slowly added to NaOH solution in the solution that obtains to step (1), control solution ph is 10 ~
11；
(3) it stands to room temperature, the solution that step (2) obtains is filtered with vacuum pump, is washed out, dries, calcining and be down to room
It is taken out after temperature, obtained sample is a kind of multi-functional mesoporous cerium based sosoloid catalyst for catalytic cleaning of car tail gas.
2. a kind of multi-functional mesoporous cerium based sosoloid catalyst for catalytic cleaning of car tail gas according to claim 1
Preparation method, it is characterised in that: the concentration of NaOH is 1.0 ~ 1.5 mol/l.
3. a kind of multi-functional mesoporous cerium based sosoloid catalyst for catalytic cleaning of car tail gas according to claim 1
Preparation method, it is characterised in that: in the step (2), when washing precipitated product, successively washed using deionized water, ethyl alcohol
Precipitated product removes impurity；It is dry to precipitated product after washing at 150-200 DEG C in drying precipitated product
At least 2 h.
4. a kind of multi-functional mesoporous cerium based sosoloid catalyst for catalytic cleaning of car tail gas according to claim 1
Preparation method, it is characterised in that: CTAB is 1 ~ 2 with metal ion molar ratio.
5. a kind of multi-functional mesoporous cerium based sosoloid catalyst for catalytic cleaning of car tail gas according to claim 1
Preparation method, it is characterised in that: while there is catalysis burning removal diesel vehicle soot particulate matter, catalytic oxidation NO, catalysis oxidation
The multifunctionalities such as CO and low temperature NOx absorption.
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Cited By (2)
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| CN114904507A (en) * | 2022-06-15 | 2022-08-16 | 济南大学 | Multifunctional praseodymium oxide nanorod catalyst for catalytic purification of diesel vehicle exhaust |
| CN116550319A (en) * | 2023-06-20 | 2023-08-08 | 南昌大学 | Catalyst for eliminating soot particle combustion and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114904507A (en) * | 2022-06-15 | 2022-08-16 | 济南大学 | Multifunctional praseodymium oxide nanorod catalyst for catalytic purification of diesel vehicle exhaust |
| CN116550319A (en) * | 2023-06-20 | 2023-08-08 | 南昌大学 | Catalyst for eliminating soot particle combustion and preparation method and application thereof |
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