CN108745364A - A kind of preparation method of perovskite catalyst for catalytic oxidation NO - Google Patents
A kind of preparation method of perovskite catalyst for catalytic oxidation NO Download PDFInfo
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- CN108745364A CN108745364A CN201810459688.8A CN201810459688A CN108745364A CN 108745364 A CN108745364 A CN 108745364A CN 201810459688 A CN201810459688 A CN 201810459688A CN 108745364 A CN108745364 A CN 108745364A
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- salt
- perovskite catalyst
- nitrate
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- perovskite
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- 239000003054 catalyst Substances 0.000 title claims abstract description 101
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 41
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 38
- 230000003647 oxidation Effects 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 150000003839 salts Chemical class 0.000 claims abstract description 91
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Inorganic materials [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 55
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 8
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 7
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 6
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 6
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 5
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 229910052802 copper Inorganic materials 0.000 claims abstract description 4
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 4
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 65
- 235000019441 ethanol Nutrition 0.000 claims description 27
- 239000004323 potassium nitrate Substances 0.000 claims description 25
- 235000010333 potassium nitrate Nutrition 0.000 claims description 25
- 239000004317 sodium nitrate Substances 0.000 claims description 24
- 235000010344 sodium nitrate Nutrition 0.000 claims description 24
- 229910052751 metal Inorganic materials 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 18
- 239000012266 salt solution Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 239000011833 salt mixture Substances 0.000 claims description 9
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 abstract description 26
- 229910052708 sodium Inorganic materials 0.000 abstract description 26
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 abstract description 21
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 abstract description 21
- 238000006555 catalytic reaction Methods 0.000 abstract description 11
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052788 barium Inorganic materials 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910052796 boron Inorganic materials 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 25
- 238000006243 chemical reaction Methods 0.000 description 22
- 230000000694 effects Effects 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 9
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical group [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 9
- 229910002766 BaCoO3 Inorganic materials 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 229910002254 LaCoO3 Inorganic materials 0.000 description 7
- 230000010718 Oxidation Activity Effects 0.000 description 7
- 239000000470 constituent Substances 0.000 description 7
- 238000011156 evaluation Methods 0.000 description 7
- 229910002618 GdFeO3 Inorganic materials 0.000 description 6
- 229910002328 LaMnO3 Inorganic materials 0.000 description 6
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical group [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 6
- 239000011575 calcium Substances 0.000 description 6
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical group [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 6
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical group [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 6
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical group [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 6
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical group [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 6
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 6
- 239000011572 manganese Substances 0.000 description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000005169 Debye-Scherrer Methods 0.000 description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 3
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical group [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical group [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical group [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 235000011056 potassium acetate Nutrition 0.000 description 3
- 239000001632 sodium acetate Substances 0.000 description 3
- 235000017281 sodium acetate Nutrition 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910019016 NaNO3—KNO3 Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- RLDDBOUYRSPFAE-UHFFFAOYSA-N [Ti+4].[N+](=O)([O-])[O-].[Na+].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] Chemical compound [Ti+4].[N+](=O)([O-])[O-].[Na+].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] RLDDBOUYRSPFAE-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 210000002268 wool Anatomy 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
-
- 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
-
- 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
- B01J23/78—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 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
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
The present invention relates to a kind of preparation methods of the perovskite catalyst for catalytic oxidation NO, belong to catalyst technical field.The present invention uses molte-salt synthesis, in NaNO3And KNO3Melt the perovskite catalyst ABO that roasting in salt system prepares nanometer regular morphology3, wherein A is La, Ce, Nd, Gd, Ca, Sr or Ba, and B is transition metal element Co, Fe, Ni, Cu or Mn.Perovskite catalyst ABO3Can be efficiently nitrogen dioxide, perovskite catalyst ABO by nitric oxide catalysis oxidation within the scope of lower temperature and wider temperature3In introduce micro K, Na component, strengthen perovskite catalyst ABO3NO is oxidized to NO2Oxidation susceptibility, improve catalytic oxidation performance.
Description
Technical field
The present invention relates to a kind of preparation methods of the perovskite catalyst for catalytic oxidation NO, belong to catalyst technology neck
Domain.
Background technology
In purifying vehicle exhaust technical aspect, NO is NO by catalysis oxidation2Committed step is served not only as, and with important
Meaning：In LNT (the Lean-burn NOX Trap) stages, NO is oxidized to the NO being stored more easily2；In SCR (Selective
Catalytic Reduction) stage, NO：NO2Ratio be 1:1 catalytic efficiency is optimal；NO in particle trapper DPF2Presence
The initiation temperature of soot can be significantly reduced.The catalyst of catalytic oxidation NO is commonly used mainly using Pt as activated centre
It is supported on A12O3On equal carriers, wherein the load capacity of noble metal is 2% 3%.The higher operating costs of this catalyst, and your gold
Belonging to can occur to reunite and catalytic performance is made to decline in high-temperature catalytic reaction.
Compared with the noble metal catalysts such as Pt, Ru, Pd, perovskite material has cheap, stable structure, catalytic activity
The features such as thermodynamic property is stablized under good and high temperature has good development potentiality in tail gas catalytic purification field.But by
, specific surface area bad in the characteristic of its low temperature ignition is low and complicated component is difficult to deficiency prepared by batch, limits perovskite
The performance of material advantage and actual application.
Invention content
The problem of existing for the above-mentioned prior art and deficiency, the present invention provide a kind of perovskite for catalytic oxidation NO
The chemical general formula of the preparation method of catalyst, perovskite catalyst of the present invention is ABO3, wherein A is La, Ce, Nd, Gd, Ca, Sr
Or Ba, B are transition metal element Co, Fe, Ni, Cu or Mn.Double-perovskite catalyst can at a lower temperature and wider temperature
Spend range in efficiently by nitric oxide catalysis oxidation be nitrogen dioxide, at low cost, the conversion to nitric oxide catalysis oxidation
Rate can reach 80% or more, more adapt to the catalysis oxidation of NO under high temperature.
A kind of preparation method of perovskite catalyst for catalytic oxidation NO, is as follows：
（1）A salt and B salt are added in absolute ethyl alcohol and is ground to dissolving and obtains ethyl alcohol metal salt solution, wherein A salt be La, Ce,
The nitrate of Nd, Gd, Ca, Sr or Ba, B are the nitrate of transition metal element Co, Fe, Ni, Cu or Mn；
（2）In step（1）Gained ethyl alcohol metal salt solution, potassium nitrate and sodium nitrate are uniformly mixed, and drying and volatilizing ethyl alcohol is mixed
Close salt；
（3）Step（2）Gained salt-mixture is at the uniform velocity warming up to 400 ~ 800 DEG C with the heating rate of 2 ~ 10 DEG C/min and roasts 3 ~ 10h,
Then room temperature is at the uniform velocity cooled to the rate of temperature fall of 2 ~ 3 DEG C/min；
（4）By step（3）Gained product of roasting, which is adopted, to be washed with deionized 2 ~ 3 times, and double-perovskite catalyst is then drying to obtain
ABO3；
Further, the integral molar quantity of the A salt and B salt and the ratio of potassium nitrate and the integral molar quantity of sodium nitrate are 1:(20~60)；
Further, the molar ratio of the A salt and B salt is 1:1；
Further, the molar ratio of the potassium nitrate and sodium nitrate is 1:(1~1.5)；
The step（4）Middle deionized water is deionized water at room temperature.
The molten salt system of the present invention chooses NaNO3-KNO3Two end number mixing salt system, under standard pressure, NaNO3Fusing point be
308 DEG C, KNO3Fusing point be 344 DEG C, in NaNO3With KNO3Lowest total of the melting point proportioning composition molar fraction NaNO3/(NaNO3
+KNO3) be 47% when lowest total of the melting point be 225 DEG C, i.e., temperature be 225 DEG C when initially form fused salt eutectic, NaNO3-
KNO3Two end number mixing salt system does not dissolve in absolute ethyl alcohol, other metal mixed salt is not interfered to be uniformly mixed in absolute ethyl alcohol；?
Under high-temperature molten salt state, the partial oxidation oxic gas that makes the solid phase synthesis of double-perovskite catalyst be decomposed in fused salt eutectic
It is carried out in atmosphere, is conducive to the formation of metal oxide, after solid phase synthesis, NaNO3-KNO3Two end number mixing salt system group
It is point soluble easily in water, the fuse salt system component of most double-perovskite catalyst can be quickly disposed, is catalyzed in double-perovskite
Agent ABO3It is middle to introduce micro K and Na components, micro K and Na components and double-perovskite catalyst ABO3Collective effect can strengthen double calcium
Titanium ore catalyst ABO3NO is oxidized to NO2Oxidation susceptibility.
Double-perovskite catalyst can be used for catalytic oxidation NO, can be high at a lower temperature and within the scope of wider temperature
Nitric oxide catalysis oxidation is nitrogen dioxide by effect ground, has good thermal stability, and higher catalysis can be kept to live for a long time
Property, hence it is evident that improve the removal efficiency of nitrogen oxides in vehicle exhaust.
The beneficial effects of the invention are as follows：
（1）The method of the present invention, as mixed melting salt, is roasted in mixed melting salt up to double calcium using potassium nitrate and sodium nitrate
Titanium ore catalyst ABO3, preparation method is simple, easily operated, is suitble to heavy industrialization application；
（2）Double-perovskite catalyst of the present invention is double-perovskite type structure, and stable structure is not easy phase transformation, thus with excellent
Thermal stability, long lifespan can keep higher catalytic activity for a long time；
（3）Double-perovskite catalyst of the present invention can be used for catalytic oxidation NO, can at a lower temperature and wider temperature model
It is efficiently nitrogen dioxide by nitric oxide catalysis oxidation to enclose interior, has good thermal stability, can keep higher for a long time
Catalytic activity, hence it is evident that improve the removal efficiency of nitrogen oxides in vehicle exhaust；
（4）Micro K and Na components are introduced in double-perovskite catalyst of the present invention, micro K and Na components are catalyzed with double-perovskite
Agent ABO3Collective effect can strengthen double-perovskite catalyst ABO3NO is oxidized to NO2Oxidation susceptibility.
Description of the drawings
Fig. 1 is 1 LaMnO of embodiment3The XRD spectrum of perovskite catalyst；
Fig. 2 is conversion ratio-temperature variation curve of 1 ~ 2 double-perovskite catalyst oxidization of nitric oxide of embodiment.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1：The present embodiment double-perovskite catalyst is LaMnO3；
A kind of preparation method of perovskite catalyst for catalytic oxidation NO, is as follows：
（1）By A salt（A salt is lanthanum nitrate）With B salt（B salt is manganese nitrate）It is added in absolute ethyl alcohol and is ground to dissolving and obtains ethyl alcohol
Metal salt solution, wherein A salt（Lanthanum nitrate）With B salt（Manganese nitrate）Molar ratio be 1:1；
（2）In step（1）Gained ethyl alcohol metal salt solution, potassium nitrate and sodium nitrate are uniformly mixed, and drying and volatilizing ethyl alcohol is mixed
Close salt；Wherein A salt（Lanthanum nitrate）With B salt（Manganese nitrate）Integral molar quantity and potassium nitrate and the ratio of integral molar quantity of sodium nitrate be 1:
30；The molar ratio of potassium nitrate and sodium nitrate is 1:1；
（3）Step（2）Gained salt-mixture is at the uniform velocity warming up to 700 DEG C with the heating rate of 2 DEG C/min and roasts 6h, then with 2 DEG C/
The rate of temperature fall of min is at the uniform velocity cooled to room temperature；
（4）It adopts and 2 steps is washed with deionized（3）Gained product of roasting, is then drying to obtain LaMnO3Double-perovskite is catalyzed
Agent；
The LaMnO of the present embodiment3The XRD spectrum of double-perovskite catalyst is as shown in Figure 1, from fig. 1, it can be seen that the LaMnO of pure phase3's
Spectrogram is the characteristic diffraction peak of perovskite structure occur at 23 °, 32 °, 40 °, 47 °, 52 °, 58 °, 68 ° and 78 ° in 2 θ, does not have
There is the appearance of dephasign peak, it was demonstrated that form single-phase rare earth double-perovskite complex metal；According to Debye Scherrer public affairs
Formula (Debye-Scherrer equation), can calculate the average grain size of nanotube sample, Debye Scherrer formula it is specific
Expression formula is：D=k λ/(β cos θ), wherein k are Scherrer constant, and numerical value 0.89, λ is the wavelength of incident X-rays, and β is diffraction maximum
Full width at half maximum (FWHM), θ is the angle of diffraction；LaMnO is calculated3The average grain size of double-perovskite catalyst is 14nm；
The LaMnO of the present embodiment3The NO catalytic oxidation activities evaluation experimental of double-perovskite catalyst is homemade columned anti-
It answers in device and carries out, wherein a diameter of 6 mm of columned reactor, length is 550 mm, by the LaMnO of 500mg3Double calcium titaniums
Mine catalyst is placed in reactor center position, and both ends are clogged with silica wool；Before carrying out catalysis reaction, by catalyst 10%
O2/N2（500mL/min）It is 300 DEG C of stable 1h that temperature is warming up under atmosphere, and it is 100 that temperature is then cooled under identical atmosphere
DEG C, after temperature stabilization, it is passed through total flow and contains 500 ppm NO, 10%O for 500 mL/min2N2Balance Air, air speed
(GHSV) it is 30000 h-1；Stablize 30 ~ 60min until NO concentration at the outlet no longer changes at being 150 DEG C in temperature；In identical gas
Under atmosphere, catalyst is risen into temperature as 450 DEG C with the heating rate of 10 DEG C/min, after initial concentration measures, temperature controller is adjusted and sets
Definite value makes reactor reach required test temperature, and Range of measuring temp is 150 DEG C ~ 400 DEG C, and a test is taken every 25 DEG C
Point is respectively kept for 15 minutes in each test point, exports NOX（NO,NO2）Concentration is by 42i-HL type high concentration nitrogen oxide analyzers
Analysis；LaMnO3Double-perovskite catalyst NO is oxidized to NO2Conversion ratio as shown in Fig. 2, as can be seen from Figure 2, LaMnO3Double calcium
The maximum conversion of titanium ore catalyst is 84%, and the temperature corresponding to maximum conversion is 308 DEG C.The double-perovskite catalyst pair
The catalytic oxidation performance of NO complies fully with thermodynamical equilibrium, i.e., NO is oxidized to NO under thermodynamical equilibrium2Conversion ratio reach maximum
After value, with the raising of temperature, conversion ratio continuously decreases, therefore there are maximum conversions；
The LaMnO of the present embodiment3Double-perovskite catalyst EDX elements contain spirogram it is found that La, Mn, O, K and Na elemental constituent
Quantitative atomic percentage is respectively 12.15%, 15.64%, 68.50%, 0.53% and 3.15%, LaMnO3Double-perovskite catalyst draws
Micro K and Na elements, micro K and Na components and double-perovskite catalyst LaMnO are entered3Collective effect can strengthen double-perovskite and urge
Agent LaMnO3NO is oxidized to NO2Oxidation susceptibility.
Embodiment 2：The present embodiment double-perovskite catalyst is LaCoO3；
A kind of preparation method of perovskite catalyst for catalytic oxidation NO, is as follows：
（1）By A salt（A salt is lanthanum nitrate）With B salt（B salt is cobalt nitrate）It is added in absolute ethyl alcohol and is ground to dissolving and obtains ethyl alcohol
Metal salt solution, wherein A salt（Lanthanum nitrate）With B salt（Cobalt nitrate）Molar ratio be 1:1；
（2）In step（1）Gained ethyl alcohol metal salt solution, potassium nitrate and sodium nitrate are uniformly mixed, and drying and volatilizing ethyl alcohol is mixed
Close salt；Wherein A salt（Lanthanum nitrate）With B salt（Cobalt nitrate）Integral molar quantity and potassium nitrate and the ratio of integral molar quantity of sodium nitrate be 1:
30；The molar ratio of potassium nitrate and sodium nitrate is 1:1.1；
（3）Step（2）Gained salt-mixture is at the uniform velocity warming up to 800 DEG C with the heating rate of 3 DEG C/min and roasts 4h, then with 2.5
DEG C/rate of temperature fall of min is at the uniform velocity cooled to room temperature；
（4）It adopts and 3 steps is washed with deionized（3）Gained product of roasting, is then drying to obtain LaCoO3Double-perovskite is catalyzed
Agent；
The LaCoO of the present embodiment3The NO catalytic oxidation activity evaluation experimentals of double-perovskite catalyst are same as Example 1,
LaCoO3The catalysis NO of double-perovskite catalyst is oxidized to NO2Conversion ratio as shown in Fig. 2, as can be seen from Figure 2, LaCoO3Double calcium titaniums
The maximum conversion of mine catalyst is 95%, and the temperature corresponding to maximum conversion is 300 DEG C；
From the LaCoO of the present embodiment3Double-perovskite catalyst EDX elements contain spirogram it is found that La, Co, O, K and Na elemental constituent
Quantitative atomic percentage be respectively 13.75%, 14.52%, 68.84%, 0.75% and 2.14%, LaCoO3Double-perovskite catalyst
Introduce micro K and Na elements, micro K and Na components and double-perovskite catalyst LaCoO3Collective effect can strengthen double-perovskite
Catalyst LaCoO3NO is oxidized to NO2Oxidation susceptibility.
Embodiment 3：The present embodiment double-perovskite catalyst is BaCoO3；
A kind of preparation method of perovskite catalyst for catalytic oxidation NO, is as follows：
（1）By A salt（A salt is barium nitrate）With B salt（B salt is cobalt nitrate）It is added in absolute ethyl alcohol and is ground to dissolving and obtains ethyl alcohol
Metal salt solution, wherein A salt（Barium nitrate）With B salt（Cobalt nitrate）Molar ratio be 1:1；
（2）In step（1）Gained ethyl alcohol metal salt solution, potassium nitrate and sodium nitrate are uniformly mixed, and drying and volatilizing ethyl alcohol is mixed
Close salt；Wherein A salt（Barium nitrate）With B salt（Cobalt nitrate）Integral molar quantity and potassium nitrate and the ratio of integral molar quantity of sodium nitrate be 1:
40；The molar ratio of potassium nitrate and sodium nitrate is 1:1.2；
（3）Step（2）Gained salt-mixture is at the uniform velocity warming up to 800 DEG C with the heating rate of 4 DEG C/min and roasts 4h, then with 3 DEG C/
The rate of temperature fall of min is at the uniform velocity cooled to room temperature；
（4）It adopts and 2 steps is washed with deionized（3）Gained product of roasting, is then drying to obtain BaCoO3Double-perovskite is catalyzed
Agent；
The BaCoO of the present embodiment3The NO catalytic oxidation activity evaluation experimentals of double-perovskite catalyst are same as Example 1, from
BaCoO3Double-perovskite catalyst NO is oxidized to NO2Conversion ratio it is found that BaCoO3The highest of double-perovskite catalyst converts
Rate is 82%, and the temperature corresponding to maximum conversion is 310 DEG C；
From the BaCoO of the present embodiment3Double-perovskite catalyst EDX elements contain spirogram it is found that Ba, Co, O, K and Na elemental constituent
Quantitative atomic percentage be respectively 10.50%, 16.12%, 67.87%, 1.20% and 4.31%, BaCoO3Double-perovskite catalyst
Introduce micro K and Na elements, micro K and Na components and double-perovskite catalyst BaCoO3Collective effect can strengthen double-perovskite
Catalyst BaCoO3NO is oxidized to NO2Oxidation susceptibility.
Embodiment 4：The present embodiment double-perovskite catalyst is CeMnO3；
A kind of preparation method of perovskite catalyst for catalytic oxidation NO, is as follows：
（1）By A salt（A salt is cerous nitrate）With B salt（B salt is manganese nitrate）It is added in absolute ethyl alcohol and is ground to dissolving and obtains ethyl alcohol
Metal salt solution, wherein A salt（Cerous nitrate）With B salt（Manganese nitrate）Molar ratio be 1:1；
（2）In step（1）Gained ethyl alcohol metal salt solution, potassium nitrate and sodium nitrate are uniformly mixed, and drying and volatilizing ethyl alcohol is mixed
Close salt；Wherein A salt（Cerous nitrate）With B salt（Manganese nitrate）Integral molar quantity and potassium nitrate and the ratio of integral molar quantity of sodium nitrate be 1:
20；The molar ratio of potassium nitrate and sodium nitrate is 1:1.2；
（3）Step（2）Gained salt-mixture is at the uniform velocity warming up to 800 DEG C with the heating rate of 4 DEG C/min and roasts 4h, then with 3 DEG C/
The rate of temperature fall of min is at the uniform velocity cooled to room temperature；
（4）It adopts and 3 steps is washed with deionized（3）Gained product of roasting, is then drying to obtain CeMnO3Double-perovskite is catalyzed
Agent；
The CeMnO of the present embodiment3The NO catalytic oxidation activity evaluation experimentals of double-perovskite catalyst are same as Example 1, from
CeMnO3Double-perovskite catalyst NO is oxidized to NO2Conversion ratio it is found that BaCoO3The highest of double-perovskite catalyst converts
Rate is 85%, and the temperature corresponding to maximum conversion is 297 DEG C；
From the CeMnO of the present embodiment3Double-perovskite catalyst EDX elements contain spirogram it is found that Ce, Mn, O, K and Na elemental constituent
Quantitative atomic percentage be respectively 16.51%, 14.89%, 65.00%, 1.01% and 2.59%, CeMnO3Double-perovskite catalyst
Introduce micro K and Na elements, micro K and Na components and double-perovskite catalyst CeMnO3Collective effect can strengthen double-perovskite
Catalyst CeMnO3NO is oxidized to NO2Oxidation susceptibility.
Embodiment 5：The present embodiment double-perovskite catalyst is NdMnO3；
The preparation method of perovskite catalyst for catalytic oxidation NO, is as follows：
（1）By A salt（A salt is neodymium nitrate）With B salt（B salt is manganese nitrate）It is added in absolute ethyl alcohol and is ground to dissolving and obtains ethyl alcohol
Metal salt solution, wherein A salt（Neodymium nitrate）With B salt（Manganese nitrate）Molar ratio be 1:1；
（2）In step（1）Gained ethyl alcohol metal salt solution, potassium acetate and sodium acetate are uniformly mixed, and drying and volatilizing ethyl alcohol is mixed
Close salt；Wherein A salt（Neodymium nitrate）With B salt（Manganese nitrate）The ratio of integral molar quantity and the integral molar quantity with potassium nitrate and sodium nitrate be
1:35；The molar ratio of potassium nitrate and sodium nitrate is 1:1.2；
（3）Step（2）Gained salt-mixture is at the uniform velocity warming up to 400 DEG C with the heating rate of 2 DEG C/min and roasts 10h, then with 3
DEG C/rate of temperature fall of min is at the uniform velocity cooled to room temperature；
（4）It adopts and 2 steps is washed with deionized（3）Gained product of roasting, is then drying to obtain NdMnO3Double-perovskite is catalyzed
Agent；
The NdMnO of the present embodiment3The NO catalytic oxidation activity evaluation experimentals of perovskite catalyst are same as Example 1, NdMnO3
The maximum conversion of the catalytic performance of perovskite catalyst is 87%, and the temperature corresponding to maximum conversion is 315 DEG C；
From the NdMnO of the present embodiment3Double-perovskite catalyst EDX elements contain spirogram it is found that Nd, Mn, O, K and Na elemental constituent
Quantitative atomic percentage be respectively 18.23%, 16.59%, 60.87%, 0.56% and 3.75%, NdMnO3Double-perovskite catalyst
Introduce micro K and Na elements, micro K and Na components and double-perovskite catalyst n dMnO3Collective effect can strengthen double-perovskite
Catalyst n dMnO3NO is oxidized to NO2Oxidation susceptibility.
Embodiment 6：The present embodiment double-perovskite catalyst is GdFeO3；
A kind of preparation method of perovskite catalyst for catalytic oxidation NO, is as follows：
（1）By A salt（A salt is gadolinium nitrate）With B salt（B salt is ferric nitrate）It is added in absolute ethyl alcohol and is ground to dissolving and obtains ethyl alcohol
Metal salt solution, wherein A salt（Gadolinium nitrate）With B salt（Ferric nitrate）Molar ratio be 1:1；
（2）In step（1）Gained ethyl alcohol metal salt solution, potassium acetate and sodium acetate are uniformly mixed, and drying and volatilizing ethyl alcohol is mixed
Close salt；Wherein A salt（Gadolinium nitrate）With B salt（Ferric nitrate）The ratio of integral molar quantity and the integral molar quantity with potassium nitrate and sodium nitrate be
1:40；The molar ratio of potassium nitrate and sodium nitrate is 1:1.3；
（3）Step（2）Gained salt-mixture is at the uniform velocity warming up to 400 DEG C with the heating rate of 5 DEG C/min and roasts 10h, then with 2
DEG C/rate of temperature fall of min is at the uniform velocity cooled to room temperature；
（4）It adopts and 3 steps is washed with deionized（3）Gained product of roasting, is then drying to obtain GdFeO3Double-perovskite is catalyzed
Agent；
The GdFeO of the present embodiment3The NO catalytic oxidation activity evaluation experimentals of perovskite catalyst are same as Example 1, GdFeO3
The maximum conversion of the catalytic performance of perovskite catalyst is 84%, and the temperature corresponding to maximum conversion is 320 DEG C；
From the GdFeO of the present embodiment3Double-perovskite catalyst EDX elements contain spirogram it is found that Gd, Fe, O, K and Na elemental constituent
Quantitative atomic percentage be respectively 11.36%, 13.95%, 68.70%, 1.34% and 4.65%, GdFeO3Double-perovskite catalyst
Introduce micro K and Na elements, micro K and Na components and double-perovskite catalyst GdFeO3Collective effect can strengthen double-perovskite
Catalyst GdFeO3NO is oxidized to NO2Oxidation susceptibility.
Embodiment 7：The present embodiment double-perovskite catalyst is CeNiO3；
A kind of preparation method of perovskite catalyst for catalytic oxidation NO, is as follows：
（1）By A salt（A salt is cerous nitrate）With B salt（B salt is nickel nitrate）It is added in absolute ethyl alcohol and is ground to dissolving and obtains ethyl alcohol
Metal salt solution, wherein A salt（Cerous nitrate）With B salt（Nickel nitrate）Molar ratio be 1:1；
（2）In step（1）Gained ethyl alcohol metal salt solution, potassium acetate and sodium acetate are uniformly mixed, and drying and volatilizing ethyl alcohol is mixed
Close salt；Wherein A salt（Cerous nitrate）With B salt（Nickel nitrate）The ratio of integral molar quantity and the integral molar quantity with potassium nitrate and sodium nitrate be
1:50；The molar ratio of potassium nitrate and sodium nitrate is 1:1.4；
（3）Step（2）Gained salt-mixture is at the uniform velocity warming up to 500 DEG C with the heating rate of 2 DEG C/min and roasts 10h, then with 3
DEG C/rate of temperature fall of min is at the uniform velocity cooled to room temperature；
（4）It adopts and 2 steps is washed with deionized（3）Gained product of roasting, is then drying to obtain CeNiO3Perovskite catalyst；
The CeNiO of the present embodiment3The NO catalytic oxidation activity evaluation experimentals of perovskite catalyst are same as Example 1, CeNiO3
The maximum conversion of the catalytic performance of perovskite catalyst is 83%, and the temperature corresponding to maximum conversion is 323 DEG C；
From the CeNiO of the present embodiment3Double-perovskite catalyst EDX elements contain spirogram it is found that Ce, Ni, O, K and Na elemental constituent
Quantitative atomic percentage be respectively 14.88%, 13.52%, 65.07%, 0.86% and 5.67%, CeNiO3Double-perovskite catalyst
Introduce micro K and Na elements, micro K and Na components and double-perovskite catalyst CeNiO3Collective effect can strengthen double-perovskite
Catalyst CeNiO3NO is oxidized to NO2Oxidation susceptibility.
The specific implementation mode of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula can also be made without departing from the purpose of the present invention within the knowledge of a person skilled in the art
Go out various change.
Claims (4)
1. a kind of preparation method of perovskite catalyst for catalytic oxidation NO, which is characterized in that be as follows：
（1）A salt and B salt are added in absolute ethyl alcohol and is ground to dissolving and obtains ethyl alcohol metal salt solution, wherein A salt be La, Ce,
The nitrate of Nd, Gd, Ca, Sr or Ba, B are the nitrate of transition metal element Co, Fe, Ni, Cu or Mn；
（2）In step（1）Gained ethyl alcohol metal salt solution, potassium nitrate and sodium nitrate are uniformly mixed, and drying and volatilizing ethyl alcohol is mixed
Close salt；
（3）Step（2）Gained salt-mixture is at the uniform velocity warming up to 400 ~ 800 DEG C with the heating rate of 2 ~ 10 DEG C/min and roasts 3 ~ 10h,
Then room temperature is at the uniform velocity cooled to the rate of temperature fall of 2 ~ 3 DEG C/min；
（4）By step（3）Gained product of roasting, which is adopted, to be washed with deionized 2 ~ 3 times, and double-perovskite catalyst is then drying to obtain
ABO3。
2. being used for the preparation method of the perovskite catalyst of catalytic oxidation NO according to claim 1, it is characterised in that：A salt
Integral molar quantity and the ratio of potassium nitrate and the integral molar quantity of sodium nitrate with B salt are 1:(20~60).
3. being used for the preparation method of the perovskite catalyst of catalytic oxidation NO according to claim 1, it is characterised in that：A salt
Molar ratio with B salt is 1:1.
4. being used for the preparation method of the perovskite catalyst of catalytic oxidation NO according to claim 1, it is characterised in that：Nitric acid
The molar ratio of potassium and sodium nitrate is 1:(1~1.5).
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| CN115487803A (en) * | 2022-09-16 | 2022-12-20 | 南京工业大学 | Hollow porous perovskite-containing cerium-manganese composite oxide and preparation and application thereof |
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