CN101745405A - Perovskite type composite oxide catalyst for purifying tail gas of internal combustion engine - Google Patents
Perovskite type composite oxide catalyst for purifying tail gas of internal combustion engine Download PDFInfo
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Abstract
The invention discloses a rare earth perovskite type oxide catalyst and a preparation method thereof. The general formula of the catalyst is La1-xCuxBO3, wherein x is within 0.05 to 0.5, and B is Fe, Co, Ni, Cr and Mn or the combination thereof. Nitrates of elements that La, Cu and B stand for are dissolved into water to form mixed solution, ammonia water is added after citric acid is added and dissolved, the mixed solution is then heated into wet gel, the wet gel is dried into dried gel, the dried gel is heated for spontaneous combustion, and obtained ash powder is roasted into the rare earth perovskite type oxide catalyst. The elements La and Cu in the catalyst are located at the position A of the perovskite type structure, and the elements Fe, Co, Ni, Cr or Mn are located at the position B. The oxide catalyst has ideal purifying effect for NO, CO and HC in tail gas of an internal combustion engine.
Description
Technical field
The present invention relates to catalyst, relate in particular to oxynitrides in the exhaust gases of internal combustion engines (NO), carbon monoxide (CO) and hydrocarbon (HC) are converted into N
2And CO
2Three-way catalyst.
Background technology
Along with the development of coal-fired industry (for example coal fired power generation) and the increase of vehicle guaranteeding organic quantity, the oxynitrides of discharging (NO accounts for more than 90%), carbon monoxide (CO) and hydrocarbon (HC) are on the rise.This three classes gas not only contaminated environment influences human normal life, also can directly be detrimental to health.Therefore, develop a kind of three-way catalyst (Three Way Catalyst) that can effectively eliminate above-mentioned three class pernicious gases simultaneously, become one of research focus of many environment and chemist.At present, the three-way catalyst that has obtained using all is to adopt noble metal as active component basically, though catalytic performance is better, the noble metal reserves are few, cost an arm and a leg, and is difficult to generally promote.
Early 1970s, Libby has carried out system research to the perofskite type oxide that contains rare earth and cobalt, thinks to replace noble metal with the oxide of perovskite structure, might be used for the catalyst of purifying automobile tail gas.Then people such as Voorhoeve has carried out deep research to the RE perovskite type structure.The chemical general formula of perovskite type rare earth complex oxide can be expressed as ABO
3, A is lanthanide series normally, is positioned at cubical center, can with 12 O coordinations; B is the little metallic element of ratio of ionic radii A, is positioned at cubical drift angle, can with 6 O coordinations.This structure has can control oxygen vacancies and content thereof, the characteristics such as activity of oxygen in lattice, thereby helps improving the redox property of catalyst, and Heat stability is good.So the development of RE perovskite type catalyst is paid much attention to.
A kind of application mode of perovskite type rare earth complex oxide is that it is carried precious metal element as carrier, perhaps precious metal element is mixed in the B position, become the perovskite type rare earth complex oxide that contains precious metal element, as Chinese invention patent Shen Qing Publication specification CN1237480A, CN1665590A, CN1665589A, CN1669645A, CN1674985A, the disclosed catalyst of CN101027126A, CN101356005A.All cost is too high owing to use noble metal for reason as described above, these catalyst.
Chinese invention patent Shen Qing Publication specification CN1235065A thinks that its catalysis genetic horizon is perovskite-type rare-earth composite oxides such as LaCu
0.6Mn
0.4O
3, La
1.4Ba
0.6CuO
3, can make CO minimizing 12.5～45.45% in the tail gas, HC reduces 10～53.33%.
The disclosed catalyst A of CN1714931A
1-xA
xB
1-yB
yO
3(A=La, A=Ce, Ca, Sr, Ba, K, Cs; B, B=Co, Mn, Fe, Ni, Cr, Zn, Cu, V, Ti, Y, Zr, Rh, Ru, Pt, Au, Pd, Ag; X=0-1; Y=0-1) can be applicable to catalytic decomposition NOx under the excess oxygen, 70～85%, 450 ℃ of conversion ratios 87% of 30～50%, 350 ℃ of conversion ratios of 250 ℃ of conversion ratios.
The disclosed catalyst La of CN1879961A
1-xAg
xMnO
3, constitute perovskite ABO by lanthanum element, silver element
3A position in the structure; Manganese element constitutes the B position; 0.05≤X≤0.4 wherein.Under 400～550 ℃, CO transforms 63～68%, and HC transforms 48～55%, and NO transforms 14～19%.
CN1973962A thinks, A
1-xA '
xB
1-yB '
yO
3(A represents La, and A ' comprises Zr, Ce, Sr, Ca, Ba, Pr; B and B ' represent transition metal Fe, Co, Ni, Mn, Cu and Ti; 0≤x≤0.9; 0≤y≤1.0) RE perovskite type catalyst can be used for before the purifying nitrogen oxides of lean-burn tail gas process, is nitrogen dioxide with nitric oxide pre-oxidation, improves the removal efficient of nitrogen oxide thus.
CN101484241A thinks, with perovskite type composite oxide catalyst ABO
3-x(A=La, Sr, Se, Ba, Ca and combination thereof, B=Fe, Go, Ni, Cr, Mn, Mg and combination thereof) supports in the porous silica carrier and can be used for purifying NO, as LaFeO
3Handling the temperature that the NO conversion ratio reaches at 50% o'clock is 319 ℃, 400～600 ℃ of following conversion ratios 98.4～99.9%.
Perovskite type rare earth complex oxide also is used for reducing the ignition temperature of tail gas carbon soot particles, the LaNiO that provides as CN1721066A
3Or La
2NiO
4, can be with the ignition temperature of soot by being reduced to 250-400 ℃ more than 550 ℃.The disclosed catalyst RTO of CN1898019A
3(R is selected from La, Sr, and Ba, one or more elements of Ca and Li, T is selected from Mn, Fe, Co, Cu, Zn, Ga, Zr, Mo, Mg, one or more elements of Al and Si), the disclosed catalyst La of CN101036888A
1-xK
xCoO
3(0.0≤X≤0.6) can to a certain degree remove particle and the NO in the tail gas.
Can see from bibliographical information so far, the RE perovskite type catalyst that contains noble metal can purify NO, CO and HC simultaneously, has the three-effect catalysis effect, the RE perovskite type catalyst that does not contain noble metal all has the suspicion of attending to one thing and lose sight of another to the purification of NO, CO and HC, wherein the part catalyst is higher but too low to the conversion ratio of NO to the conversion ratio of CO and HC, and another part is higher to the conversion ratio of NO, and the conversion ratio of CO and HC but is unwilling to mention.
Summary of the invention
The object of the present invention is to provide a kind of Rare Earth Perovskite-Type Oxide Catalysts and preparation method thereof, this catalyst has desirable clean-up effect simultaneously to the NO in the exhaust gases of internal combustion engines, CO and HC.
Catalyst general formula of the present invention is La
1-xCu
xBO
3, x=0.05～0.5 wherein, B=Fe, Co, Ni, Cr, Mn or their combination.
Preferred scheme is in the above-mentioned general formula: x=0.1～0.5 is more preferably x=0.1～0.3; The B element is B=Ni preferably
1-yM
y, 0＜y in the formula＜1, y=0.1～0.5 preferably, M=Fe, Co, Cr or Mn, preferably M=Fe or Mn.
The preparation method of Rare Earth Perovskite-Type Oxide Catalysts of the present invention comprises the steps:
A. by described mol ratio that the nitrate of the element of La, Cu and B representative is water-soluble, be made into the mixed solution that total concentration is 0.1～0.5mol/L;
B. 0.5～1 times citric acid by the molal quantity summation of the element of La, Cu and B representative joins in the mixed solution, after the stirring and dissolving, adds ammoniacal liquor and regulates mixed solution pH value to 7.5～10;
C. mixed solution is heated to 50～80 ℃ and stirs down until becoming wet gel, wet gel is at 100～150 ℃ of xerogel that formed in dry 5～15 hours down, and heating makes the xerogel spontaneous combustion, with the ashes grind into powder that obtains;
D. powder became Rare Earth Perovskite-Type Oxide Catalysts in 1～5 hour 600～900 ℃ of following roastings.
In step C, preferably 105～120 ℃ of the baking temperatures of wet gel.Among the step D, preferably 700～800 ℃ of sintering temperatures are more preferably 740～760 ℃.
Catalyst of the present invention has perovskite structure, La element wherein and Cu element are positioned at the A position of perovskite structure, Fe, Co, Ni, Cr or Mn element are positioned at the B position, the advantage that possesses the perovskite structure Heat stability is good, in the common delivery temperature scope of internal combustion engine, CO, HC and NO in the tail gas had desirable clean-up effect simultaneously.
Description of drawings
Fig. 1 is La
0.8Cu
0.2Ni
0.8Mn
0.2O
3XRD figure.
Fig. 2 is La
0.8Cu
0.2Ni
0.8Mn
0.2O
3SEM figure.
The specific embodiment
Embodiment 1, La
0.8Cu
0.2Ni
0.8Mn
0.2O
3Activity of such catalysts
With mol ratio is 0.8: 0.2: 0.8: 0.2 La (NO
3)
36H
2O, Cu (NO
3)
23H
2O, Ni (NO
3)
26H
2O and Mn (NO
3)
24H
2O is water-soluble, be made into the mixed solution that the metal ion total concentration is 0.2mol/L, get citric acid by 0.6 times of metal ion molal quantity summation, join in the mixed solution, after the stirring and dissolving, it is about 8.5 that dropping ammonia is regulated mixed solution pH value, 70 ℃ of constant temperature, electronic stirring is until becoming wet gel, and 110 ℃ down after dry 12 hours, cooling, the xerogel that forms is being heated on the electric furnace about 350 ℃, and the xerogel spontaneous combustion obtains the grey black ashes, with the ashes grind into powder, 750 ℃ of following roastings 2 hours, become La
0.8Cu
0.2Ni
0.8Mn
0.2O
3Composite oxides.
Catalyst structure is confirmed: these composite oxides carry out X-ray diffraction (XRD) test and SEM test, and the XRD test is carried out on German Bruker-D8 type X-ray diffractometer.Adopt Cu Ka radiation source, pipe stream 40mA, pipe is pressed 40kV, and the XRD spectra that obtains is as shown in Figure 1.The SEM test is carried out on the Japanese JEOL Philips XS of company 30 type environmental scanning electron microscopes, and the SEM figure that obtains as shown in Figure 2.Fig. 1 and Fig. 2 show that these composite oxides have formed perovskite cube crystal structure and particle is less, even.Can know that by calculating the ionic radius (r) of component satisfies the tolerance limit factor (t): 0.75≤t≤1.0, wherein t=(r
A+ r
O)/1.414 (r
B+ r
O), can illustrate that La element and Cu element are positioned at the A position of perovskite structure, Ni element and Mn element are positioned at the B position of perovskite structure.
Activity of such catalysts is estimated: the simulated maneuver tail gas of use is formed and volumetric concentration is: NO0.1%, C
3H
60.1%, CO 1.0%, O
21.0%, use N
2As carrier gas, air speed is 40000h
-1, the catalyst useful load is 0.2g.Recording HC, CO and NO conversion ratio and be 50% temperature is: HC338 ℃, and 178 ℃ of CO, 303 ℃ of NO, conversion ratio under other temperature such as following table:
As seen, by above-mentioned La
0.8Cu
0.2Ni
0.8Mn
0.2O
3Catalyst purified treatment simulated maneuver tail gas has desirable clean-up effect simultaneously to CO, HC and NO under 400～500 ℃.
Embodiment 2, La
0.8Cu
0.2NiO
3Activity of such catalysts
With mol ratio 0.8: 0.2: 1 La (NO
3)
36H
2O, Cu (NO
3)
23H
2O and Ni (NO
3)
26H
2O is water-soluble, be made into the mixed solution that the metal ion total concentration is 0.2mol/L, get citric acid by 0.6 times of metal ion molal quantity summation, join in the mixed solution, after the stirring and dissolving, dropping ammonia is regulated about mixed solution pH value to 8.5,70 ℃ of constant temperature, electronic stirring is until becoming wet gel, and 110 ℃ down after dry 12 hours, cooling, the xerogel that forms is being heated on the electric furnace about 350 ℃, and the xerogel spontaneous combustion obtains the grey black ashes, with the ashes grind into powder, 750 ℃ of 2 times roastings 2 hours, become La
0.8Cu
0.2NiO
3Composite oxides.
These composite oxides have also formed perovskite cube crystal structure, and La element and Cu element are positioned at the A position of perovskite structure, and the Ni element is positioned at the B position of perovskite structure.
It is active to press under the activity rating condition of embodiment 1 test, records HC, CO and NO conversion ratio and be 50% temperature to be: 283 ℃ of HC, and 267 ℃ of CO, 425 ℃ of NO, conversion ratio under other temperature such as following table:
As seen, by above-mentioned La
0.8Cu
0.2NiO
3Catalyst purified treatment simulated maneuver tail gas has desirable clean-up effect simultaneously to CO, HC and NO in the time of 450～500 ℃.
Embodiment 3, La
0.8Cu
0.2Ni
0.8Fe
0.2O
3Activity of such catalysts
With mol ratio is 0.8: 0.2: 0.8: 0.2 La (NO
3)
36H
2O, Cu (NO
3)
23H
2O, Ni (NO
3)
26H
2O and Fe (NO
3)
39H
2O is water-soluble, be made into the mixed solution that the metal ion total concentration is 0.2mol/L, get citric acid by 0.6 times of metal ion molal quantity summation, join in the mixed solution, after the stirring and dissolving, it is about 8.5 that dropping ammonia is regulated mixed solution pH value, 70 ℃ of electronic stirrings of constant temperature are until becoming wet gel, 110 ℃ drying is after 12 hours down, and cooling is being heated to the xerogel that forms about 350 ℃ on the electric furnace, the xerogel spontaneous combustion obtains the grey black ashes, with the ashes grind into powder,, become La 750 ℃ of following roastings 2 hours
0.8Cu
0.2Ni
0.8Fe
0.2O
3Composite oxides.
These composite oxides have also formed perovskite cube crystal structure, and La element and Cu element are positioned at the A position of perovskite structure, and Ni element and Fe element are positioned at the B position of perovskite structure.
It is active to press under the activity rating condition of embodiment 1 test, records HC, CO and NO conversion ratio and be 50% temperature to be: 306 ℃ of HC, and 227 ℃ of CO, 438 ℃ of NO, conversion ratio under other temperature such as following table:
As seen, by above-mentioned La
0.8Cu
0.2Ni
0.8Fe
0.2O
3Catalyst purified treatment simulated maneuver tail gas has desirable clean-up effect simultaneously to CO, HC and NO under 450～500 ℃.
Embodiment 4, La
0.7Cu
0.3Ni
0.8Mn
0.2O
3Activity of such catalysts
With mol ratio is 0.7: 0.3: 0.8: 0.2 La (NO
3)
36H
2O, Cu (NO
3)
23H
2O, Ni (NO
3)
26H
2O and Mn (NO
3)
24H
2O is water-soluble, be made into the mixed solution that the metal ion total concentration is 0.2mol/L, get citric acid by 0.6 times of metal ion molal quantity summation, join in the mixed solution, after the stirring and dissolving, it is about 8.5 that dropping ammonia is regulated mixed solution pH value, 70 ℃ of electronic stirrings of constant temperature are until becoming wet gel, 110 ℃ drying is after 12 hours down, and cooling is being heated to the xerogel that forms about 350 ℃ on the electric furnace, the xerogel spontaneous combustion obtains the grey black ashes, with the ashes grind into powder,, become La 750 ℃ of following roastings 2 hours
0.7Cu
0.3Ni
0.8Mn
0.2O
3Composite oxides.
These composite oxides have also formed perovskite cube crystal structure, and La element and Cu element are positioned at the A position of perovskite structure, and Ni element and Mn element are positioned at the B position of perovskite structure.
It is active to press under the activity rating condition of embodiment 1 test, records HC, CO and NO conversion ratio and be 50% temperature to be: 341 ℃ of HC, and 175 ℃ of CO, 324 ℃ of NO, conversion ratio under other temperature such as following table:
As seen, by above-mentioned La
0.7Cu
0.3Ni
0.8Mn
0.2O
3Catalyst purified treatment simulated maneuver tail gas has desirable clean-up effect simultaneously to CO, HC and NO under 400～500 ℃.
Embodiment 5, La
0.9Cu
0.1Ni
0.8Mn
0.2O
3Activity of such catalysts
With mol ratio is 0.9: 0.1: 0.8: 0.2 La (NO
3)
36H
2O, Cu (NO
3)
23H
2O, Ni (NO
3)
26H
2O and Mn (NO
3)
24H
2O is water-soluble, be made into the mixed solution that the metal ion total concentration is 0.2mol/L, 0.6 times by metal ion molal quantity summation takes by weighing citric acid, join in the mixed solution, after the stirring and dissolving, it is about 8.5 that dropping ammonia is regulated mixed solution pH value, 70 ℃ of electronic stirrings of constant temperature are until becoming wet gel, 110 ℃ drying is after 12 hours down, and cooling is being heated to the xerogel that forms about 350 ℃ on the electric furnace, the xerogel spontaneous combustion obtains the grey black ashes, with the ashes grind into powder,, become La 750 ℃ of following roastings 2 hours
0.9Cu
0.1Ni
0.8Mn
0.2O
3Composite oxides.
These composite oxides have also formed perovskite cube crystal structure, and La element and Cu element are positioned at the A position of perovskite structure, and Ni element and Mn element are positioned at the B position of perovskite structure.
It is active to press under the activity rating condition of embodiment 1 test, records HC, CO and NO conversion ratio and be 50% temperature to be: 335 ℃ of HC, and 194 ℃ of CO, 329 ℃ of NO, conversion ratio under other temperature such as following table:
As seen, by above-mentioned La
0.9Cu
0.1Ni
0.8Mn
0.2O
3Catalyst purified treatment simulated maneuver tail gas has desirable clean-up effect simultaneously to CO, HC and NO under 450～500 ℃.
Claims (10)
1. the perovskite type rare earth complex oxide catalyst of purification of exhaust gases of internal combustion engines has the perovskite type rare earth complex oxide structure, it is characterized in that, this catalyst general formula is La
1-xCu
xBO
3, x=0.05～0.5 wherein, B=Fe, Co, Ni, Cr, Mn or their combination.
2. according to the described perovskite type rare earth complex oxide catalyst of claim 1, it is characterized in that described general formula La
1-xCu
xBO
3In, x=0.1～0.5.
3. according to the described perovskite type rare earth complex oxide catalyst of claim 2, it is characterized in that described general formula La
1-xCu
xBO
3In, x=0.1～0.3.
4. according to the described perovskite type rare earth complex oxide catalyst of the arbitrary claim of claim 1～3, it is characterized in that described general formula La
1-xCu
xBO
3In, B=Ni
1-yM
y, 0＜y＜1 wherein, M=Fe, Co, Cr or Mn.
5. according to the described perovskite type rare earth complex oxide catalyst of claim 4, it is characterized in that, at described B=Ni
1-yM
yIn the formula, y=0.1～0.5.
6. according to the described perovskite type rare earth complex oxide catalyst of claim 4, it is characterized in that, at described B=Ni
1-yM
yIn the formula, M=Fe or Mn.
7. the described perovskite type rare earth complex oxide Preparation of catalysts of the arbitrary claim of claim 1～6 method is characterized in that, comprises the steps:
A. by described mol ratio that the nitrate of the element of La, Cu and B representative is water-soluble, be made into the mixed solution that total concentration is 0.1～0.5mol/L;
B. 0.5～1 times citric acid by the molal quantity summation of the element of La, Cu and B representative joins in the mixed solution, and after the stirring and dissolving, dropping ammonia is regulated mixed solution pH to 7.5～10;
C. mixed solution is heated to 50～80 ℃ and stirs down until becoming wet gel, wet gel is at 100～150 ℃ of xerogel that formed in dry 5～15 hours down, and heating makes the xerogel spontaneous combustion, with the ashes grind into powder that obtains;
D. powder became the perovskite type rare earth complex oxide catalyst in 1～5 hour 600～900 ℃ of following roastings.
8. according to the described preparation method of claim 7, it is characterized in that among the step C, the baking temperature of wet gel is 105～120 ℃.
9. according to the described preparation method of claim 7, it is characterized in that among the step D, sintering temperature is 700～800 ℃.
10. according to the described preparation method of claim 9, it is characterized in that among the step D, sintering temperature is 740～760 ℃.
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