CN100398198C - Diesel vehicle exhaust carbon-smoke combustion and Nox storage-reduction dual-functional catalyst and its preparing method - Google Patents
Diesel vehicle exhaust carbon-smoke combustion and Nox storage-reduction dual-functional catalyst and its preparing method Download PDFInfo
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- CN100398198C CN100398198C CNB200510128436XA CN200510128436A CN100398198C CN 100398198 C CN100398198 C CN 100398198C CN B200510128436X A CNB200510128436X A CN B200510128436XA CN 200510128436 A CN200510128436 A CN 200510128436A CN 100398198 C CN100398198 C CN 100398198C
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Abstract
The present invention relates to a bifunctional catalyst capable of making soot in the tail gas of diesel vehicles to be burnt and NOx to be stored and reduced and a preparation method thereof. The catalyst uses Mg-Al hydrotalcite composite oxide for loading Pt and K as a basis and copper as an auxiliary active component (an assistant), and is synthesized with the coprecipitation method. With simulating the tail gas of the diesel vehicles as an atmosphere, the existing catalyst can simultaneously realize double functions of making the soot in the tail gas of the diesel vehicles to be burnt and the NOx to be stored and reduced, namely that when the NOx is stored and reduced, the catalyst can make the soot to be burnt at the burning temperature reaching the deflating temperature range of the diesel vehicles so as to simultaneously eliminate two pollutants of soot granules and the NOx in the tail gas of the diesel vehicles. Thus, the useful bifunctional catalyst can simultaneously eliminate two pollutants of the soot granules and the NOx in the tail gas of the diesel vehicles.
Description
(1) technical field under
The invention belongs to the technical field of exhaust gas from diesel vehicle catalyst, particularly a class can make bavin take out the bifunctional catalyst of carbon-smoke combustion and NOx storage-reduction in the tail gas, and above-mentioned Preparation of catalysts method.
(2) background technology
Diesel-powered car is because the low oil consumption, low emission, the high power characteristic that have, and the occupation rate in the European market has reached 40%, Germany even up to 50%.Europe has adopted diesel engine to reduce CO as carrying out " Kyoto Protocol "
2The prerequisite of discharging.In the automobile market of China, there is the Nanjing IVECO to use diesel in the homemade light bus, light card of part and pick up are just replaced by Diesel engine.What be with historically new significance is that FAW-Volkswagen released first natural aspiration diesel-powered car Jetta SDI in the whole nation in 2003, released another turbo-charging diesel car Bora TDI in February, 2004, released the A6TDI of Audi (2.5L) diesel-powered car July again.On January 22nd, 2005, the report of Development Research Center of the State Council's issue claimed, diesel-powered car is good in the market prospects of China, its efficient, economic, energy-conservation automotive industrial policy and environmental requirement that meets country.
Diesel engine truck exhaust has following feature: (1) diesel engine is at the burning down of high air-fuel ratio condition (20-50), O in the exhaust
2The concentration height, particle (PM) concentration of emission height, HC/NOx is than low.(2) diesel engine delivery temperature when steady-state operation is low, and temperature rises during acceleration; Delivery temperature but can reach more than 600 ℃ under the operating mode of running at high speed about 150-400 ℃ under the driving cycle in avenue.(3) the diesel combustion characteristics determined PM and NOx concentration height in the exhaust, be the major control object, and the two is a pair of paradox, suppress the generation of NOx, the trend that increases PM is just arranged.Therefore the three-way catalyst (TWC) that is used for gasoline car can not be suitable at all.
Particle shows as soot (soot) and goes up absorption some dissolved organic matters (SOF) mostly less than 2.5 μ m, and human and biological respiratory system is had bigger harm; NOx then is the arch-criminal of acid rain and photochemical fog.For the EuroV standard that satisfies Europe implementation in 2008, Tier 2 standards that the U.S. carries out, remove when must consider them.
The diesel engine truck exhaust post-processing technology mainly contains at present: (1) eliminates the oxidation catalyst (DOC) that does not fire SOF in HC, CO and the particle, and is inoperative to dried soot and NOx; (2) only eliminate the particle trap of particle; (3) only eliminate poor combustion deNOx technology and the catalyst of NOx; (4) eliminate the technology of soot and NOx simultaneously, as composite oxide catalysts catalyzed conversion soot and NOx simultaneously, promptly soot is oxidized to CO by NOx
2NOx is reduced to N simultaneously
2, but under the situation of a large amount of oxygen enrichments of diesel engine, NOx is reduced to N with soot
2Efficient too low.According to this deficiency, the invention provides a kind of catalyst, can under reducing atmosphere, be reduced to N with NOx storing under the oxygen atmosphere excessively
2The more important thing is and in the NOx storage-reduction, carbon soot particles can also be burnt.Thereby realize the difunctional of carbon-smoke combustion and NOx storage-reduction, simultaneously big pollutant carbon soot particles of two in the exhaust gas from diesel vehicle and NOx are removed simultaneously.
(3) summary of the invention
The object of the present invention is to provide a kind of catalyst, can realize carbon-smoke combustion and NO
xStorage-reduction difunctional is promptly at NO
xIn the time of storage and reduction, catalyst can also fall carbon-smoke combustion.
Another object of the present invention is to provide above-mentioned Preparation of catalysts method.
The present invention realizes by following measure:
The bifunctional catalyst of diesel vehicle exhaust carbon-smoke combustion of the present invention and NOx storage-reduction, its special feature is: loaded on the Mg-Al hydrotalcite composite oxides by active component K and Pt.
Catalyst of the present invention, the load capacity of described K are 3-7wt.%, and the load capacity of described Pt is 0.5-1wt.%, and the mol ratio of Mg and Al is 4～1.5: 1.
Catalyst of the present invention, in order further to improve its catalytic effect, load has auxiliary activity component Cu on the Mg-Al hydrotalcite composite oxides.The load capacity of described Cu is 0-3wt.%.
The Preparation of catalysts method of the invention described above may further comprise the steps:
Prepare the mixing salt solution of Mg, Al according to a certain percentage, Mg
2+, Al
3+The total concentration of ion is 1.5mol/l;
The sodium carbonate of preparing under the room temperature and the mixed ammonium/alkali solutions of NaOH, (CO
3 2-): (OH
-) mol ratio be 1: 2;
Mixing salt solution and mixed ammonium/alkali solutions drip to respectively and fill temperature is in 65 ℃ the container of deionized water, high degree of agitation keeps pH value about 10, after dripping off simultaneously, the gained slurries are worn out half an hour down at 65 ℃, suction filtration washs half an hour, suction filtration again with the filter cake making beating then, repeatedly several times, at last filter cake is placed under 120 ℃ of conditions, to evaporate in the baking oven and spends the night, the filter cake behind the evaporate to dryness is placed in the muffle furnace at different roasting temperatures, the magnalium hydrotalcite composite oxides;
Adopt the equivalent impregnation method, an amount of sylvite is loaded on the baked Mg-Al composite oxide, 120 ℃ of oven dry are spent the night, 600 ℃ of roasting 4h; Flood chloroplatinic acid or other platinum salt then, 120 ℃ of oven dry are spent the night, and 600 ℃ of roasting 4h are again at 5vol.%H
2/ N
2Under the atmosphere, 400 ℃ of reductase 12 h obtain catalyst of the present invention.
In the catalyst of the invention described above, if contain auxiliary activity component Cu, its preparation method can be, Cu, Mg, Al are made the mixing salt solution that total concentration is 1.5mol/l, is prepared into the magnalium hydrotalcite composite oxides of copper doped, floods potassium and platinum again.Also can synthesize the magnalium hydrotalcite composite oxides earlier, again with load copper, and then load potassium and platinum.
Catalyst of the present invention is based on the Mg-Al hydrotalcite composite oxides of supporting Pt and K, and auxiliary activity composition (auxiliary agent) is a copper.This catalyst is synthetic with coprecipitation.In the presence of this catalyst, be combustion atmosphere with the simulation exhaust gas from diesel vehicle, can realize the difunctional of carbon-smoke combustion and NOx storage-reduction in the exhaust gas from diesel vehicle simultaneously, promptly catalyst is at NO
xIn the time of storage and reduction, carbon-smoke combustion can also be fallen, ignition temperature has reached in the temperature range of diesel engine truck exhaust; Thereby can eliminate the big pollutant of two in the exhaust gas from diesel vehicle simultaneously: carbon soot particles and NOx.Be a kind of two big pollutant carbon soot particles in the exhaust gas from diesel vehicle and bifunctional catalyst of NOx eliminated useful the time.
Preparation method of the present invention, it is simple to have method, and easy operating is suitable for the characteristics of suitability for industrialized production.
(4) description of drawings
The TG-DTA curve that Fig. 1 burns under air atmosphere for simulation pure carbon cigarette.
Fig. 2 is the catalyst activity that NO is reduced under different temperatures of embodiment 2.Among the figure, abscissa is a reaction temperature, and ordinate is the conversion ratio of NO, and reaction condition is 1000ppm NO, 1000ppm C
3H
6, 0.1vol% O
2, balance gas is Ar, air speed is 20000h
-1
Fig. 3 is the catalyst activity that NO is reduced under different temperatures of embodiment 2.Among the figure, abscissa is a reaction temperature, and ordinate is the conversion ratio of NO, and reaction condition is 1000ppm NO, and 1000ppm CO, balance gas are Ar, air speed 20000h
-1
(5) specific embodiment
In order to be illustrated more clearly in the present invention, enumerate following examples, but it there is not any restriction to scope of the present invention.
Embodiment 1:
According to magnalium copper mol ratio is 65: 33: 2, preparation Mg (NO
3)
2.6H
2O, Al (NO
3)
3.9H
2O and Cu (NO
3)
2.6H
2The mixing salt solution of O, Mg
2+, Al
3+And Cu
2+The total concentration of ion is 1.5mol/l, the mixed ammonium/alkali solutions (CO of configuration sodium carbonate and NaOH under the room temperature
3 2-): (OH
-)=1: 2, two solution drip to (65 ℃ of water temperatures, water yield 200ml) in the 500ml beaker that fills a certain amount of deionized water with certain speed of dripping respectively, and high degree of agitation is adjusted two drips of solution speed simultaneously, and the pH value of slurries is remained on about 10.After dripping off, with the gained slurries 65 ℃ of down aging half an hour, suction filtration then, with filter cake making beating washing half an hour, suction filtration again, repeatedly several times.At last filter cake is placed under 120 ℃ of conditions, to evaporate in the baking oven and spends the night, the filter cake behind the evaporate to dryness is placed in the muffle furnace at 600 ℃ of different roasting temperatures.
Adopt the equivalent impregnation method, will be equivalent to the K of 3.5wt.%K content
2CO
3Load on the Mg-Al composite oxide of 600 ℃ of baked doping steel, 120 ℃ of oven dry are spent the night, 600 ℃ of roasting 4h.
Adopt the equivalent impregnation method, on the 1wt.%Pt Mg-Al composite oxide that mixes of the copper of potassium that loaded to 600 ℃ of baked loads, 120 ℃ of oven dry are spent the night, and 600 ℃ of roasting 4h are again at 5vol.%H
2/ N
2Under the atmosphere, 400 ℃ of reductase 12 h obtain catalyst.The predecessor of Pt is the ammonium salt of chloroplatinic acid or platinum.
Embodiment 2:
According to magnalium copper mol ratio is 64: 33: 3, preparation Mg (NO
3)
2.6H
2O, Al (NO
3)
3.9H
2O and Cu (NO
3)
2.6H
2The mixing salt solution of O, Mg
2+, Al
3+And Cu
2+The total concentration of ion is 1.5mol/l, the mixed ammonium/alkali solutions (CO of configuration sodium carbonate and NaOH under the room temperature
3 2-): (OH
-)=1: 2, two solution drip to (65 ℃ of water temperatures, water yield 200ml) in the 500ml beaker that fills a certain amount of deionized water with certain speed of dripping respectively, and high degree of agitation is adjusted two drips of solution speed simultaneously, and the pH value of slurries is remained on about 10.After dripping off, with the gained slurries 65 ℃ of down aging half an hour, suction filtration then, with filter cake making beating washing half an hour, suction filtration again, repeatedly several times.At last filter cake is placed under 120 ℃ of conditions, to evaporate in the baking oven and spends the night, the filter cake behind the evaporate to dryness is placed in the muffle furnace at 600 ℃ of different roasting temperatures, the Mg-Al composite oxide of copper doped.
Adopt the equivalent impregnation method, will be equivalent to the K of 4.5wt.%K content
2CO
3Load on the Mg-Al composite oxide of 600 ℃ of baked copper doped, 120 ℃ of oven dry are spent the night, 600 ℃ of roasting 4h.
Adopt the equivalent impregnation method, on the 1wt.%Pt Mg-Al composite oxide that mixes of the steel of potassium that loaded to 600 ℃ of baked loads, 120 ℃ of oven dry are spent the night, and 600 ℃ of roasting 4h are again at 5vol.%H
2/ N
2Under the atmosphere, 400 ℃ of reductase 12 h obtain catalyst.The predecessor of Pt is the ammonium salt of chloroplatinic acid or platinum.
Embodiment 3:
According to magnalium copper mol ratio is 64: 33: 3, preparation Mg (NO
3)
2.6H
2O, Al (NO
3)
3.9H
2O and Cu (NO
3)
2.6H
2The mixing salt solution of O, Mg
2+, Al
3+And Cu
2+The total concentration of Gao Zi is 1.5mol/l, the mixed ammonium/alkali solutions (CO of configuration sodium carbonate and NaOH under the room temperature
3 2-): (OH
-)=1: 2, two solution drip to (65 ℃ of water temperatures, water yield 200ml) in the 500ml beaker that fills a certain amount of deionized water with certain speed of dripping respectively, and high degree of agitation is adjusted two drips of solution speed simultaneously, and the pH value of slurries is remained on about 10.After dripping off, with the gained slurries 65 ℃ of down aging half an hour, suction filtration then, with filter cake making beating washing half an hour, suction filtration again, repeatedly several times.At last filter cake is placed under 120 ℃ of conditions, to evaporate in the baking oven and spends the night, the filter cake behind the evaporate to dryness is placed in the muffle furnace at 600 ℃ of different roasting temperatures, the Mg-Al composite oxide of copper doped.
Adopt the equivalent impregnation method, will be equivalent to the K of 6.5wt.%K content
2CO
3Load on the Mg-Al composite oxide of 600 ℃ of baked copper doped, 120 ℃ of oven dry are spent the night, 600 ℃ of roasting 4h.
Adopt the equivalent impregnation method, on the 1wt.%Pt Mg-Al composite oxide that mixes of the copper of potassium that loaded to 600 ℃ of baked loads, 120 ℃ of oven dry are spent the night, and 600 ℃ of roasting 4h are again at 5vol.%H
2/ N
2Under the atmosphere, 400 ℃ of reductase 12 h obtain catalyst.The predecessor of Pt is the ammonium salt of chloroplatinic acid or platinum.
Embodiment 4:
According to the magnalium mol ratio is 67: 33, preparation Mg (NO
3)
2.6H
2O and Al (NO
3)
3.9H
2The mixing salt solution of O, Mg
2+And Al
3+The total concentration of ion is 1.5mol/l, the mixed ammonium/alkali solutions (CO of configuration sodium carbonate and NaOH under the room temperature
3 2-): (OH
-)=1: 2, two solution drip to (65 ℃ of water temperatures, water yield 200ml) in the 500ml beaker that fills a certain amount of deionized water with certain speed of dripping respectively, and high degree of agitation is adjusted two drips of solution speed simultaneously, and the pH value of slurries is remained on about 10.After dripping off, with the gained slurries 65 ℃ of down aging half an hour, suction filtration then, with filter cake making beating washing half an hour, suction filtration again, repeatedly several times.At last filter cake is placed under 120 ℃ of conditions, to evaporate in the baking oven and spends the night, the filter cake behind the evaporate to dryness is placed in the muffle furnace at 600 ℃ of different roasting temperatures.
Adopt the equivalent impregnation method, will be equivalent to the K of 4.5wt.%K content
2CO
3Load on 600 ℃ of baked Mg-Al composite oxides, 120 ℃ of oven dry are spent the night, 600 ℃ of roasting 4h.
Adopt the equivalent impregnation method, 0.5wt.%Pt has been loaded to 600 ℃ of baked loads on the Mg-Al composite oxide of potassium, 120 ℃ of oven dry are spent the night, and 600 ℃ of roasting 4h are again at 5vol.%H
2/ N
2Under the atmosphere, 400 ℃ of reductase 12 h obtain catalyst.The predecessor of Pt is the ammonium salt of chloroplatinic acid or platinum.
Test case 1:
At simulation diesel vehicle oxidisability tail gas, 1000ppm NO, 5vol%O
2, balance gas is under the atmosphere of Ar, promptly when NOx stored, the results are shown in Table 1 for the catalytic combustion of soot.Wherein, T
iRepresent the initiation temperature of soot, T
MaxTemperature when representing the peak firing rate of soot, T
fThe temperature of representing carbon-smoke combustion to finish, Δ T (T
rT
i) represent carbon-smoke combustion speed.The NOx memory space of the embodiment 2 that employing TG records is about 15mg/g.
At simulation diesel vehicle reproducibility tail gas, 100ppm C
3H
6, balance gas is under the atmosphere of Ar, promptly when NOx reduces, has stored the catalyst of a certain amount of NOx, and the catalytic action of carbon-smoke combustion is descended to some extent, improves about 10-50 ℃ than the initiation temperature in the table 1.
Table 1 result of TG-DTA simulated air atmosphere catalysis carbon-smoke combustion
Test case 2:
Pt/K/Cu/MgAlO catalyst with embodiment 2 is that example is carried out following reproducibility test.
NO stable state reduction experiment is carried out at the quartz ampoule fixed bed reactors.0.3g 40-60 purpose Pt/K/Cu/MgAlO catalyst (embodiment 2), at 1000ppm NO, 1000ppm C
3H
6, 0.1vol%O
2, balance gas is Ar, air speed is 20000h
-1The time, the conversion ratio of NO is seen Fig. 2,300 ℃, the conversion ratio of NO almost reaches 100%.At 1000ppm NO, 1000ppm CO, balance gas are Ar, and air speed is 20000h
-1The time, the conversion ratio of NO is seen Fig. 3,150 ℃, the conversion ratio of NO almost reaches 100%.
Test case 3:
Pt/K/MgAlO catalyst with embodiment 4 is that example is carried out following reproducibility test.
NO stable state reduction experiment is carried out at the quartz ampoule fixed bed reactors.0.3g 40-60 purpose Pt/K/MgAlO catalyst agent (embodiment 4), at 1000ppm NO, 1000ppm C
3H
6, 0.1vol%O
2, balance gas is Ar, air speed is 20000h
-1The time, the conversion ratio of NO is in the time of 300 ℃, and the conversion ratio of NO almost reaches 100%.At 1000ppm NO, 1000ppm CO, balance gas are Ar, and air speed is 20000h
-1The time, the conversion ratio of NO is in the time of 150 ℃, and the conversion ratio of NO almost reaches 100%.
Claims (3)
1. the bifunctional catalyst of diesel vehicle exhaust carbon-smoke combustion and NOx storage-reduction is characterized in that: loaded on the Mg-Al hydrotalcite composite oxides by active component K and Pt; The load capacity of described K is 3-7wt%, and the load capacity of described Pt is 0.5-1wt%, and the mol ratio of Mg and Al is 1.5～4: 1.
2. catalyst according to claim 1 is characterized in that: load capacity is arranged is greater than 0 and less than the auxiliary activity component Cu of 3wt% in load on the Mg-Al hydrotalcite composite oxides.
3. the described Preparation of catalysts method of claim 1 is characterized in that: may further comprise the steps, prepare the mixing salt solution of Mg, Al according to a certain percentage, Mg
2+, Al
3+The total concentration of ion is 1.5mol/L; The sodium carbonate of preparing under the room temperature and the mixed ammonium/alkali solutions of NaOH, (CO
3 2-): (OH
-) mol ratio be 1: 2;
Mixing salt solution and mixed ammonium/alkali solutions drip to respectively and fill temperature is in 65 ℃ the container of deionized water, high degree of agitation keeps the pH value 10, after dripping off simultaneously, the gained slurries are worn out half an hour down at 65 ℃, suction filtration washs half an hour, suction filtration again with the filter cake making beating then, repeatedly several times, at last filter cake is placed under 120 ℃ of conditions, to evaporate in the baking oven and spends the night, the filter cake behind the evaporate to dryness is placed in the Muffle furnace roasting temperature at 600 ℃, Mg-Al hydrotalcite composite oxides;
Adopt the equivalent impregnation method, an amount of sylvite is loaded on the baked Mg-Al hydrotalcite composite oxides, 120 ℃ of oven dry are spent the night, 600 ℃ of roasting 4h; Flood chloroplatinic acid or platinum salt then, 120 ℃ of oven dry are spent the night, and 600 ℃ of roasting 4h are again at 5vol%H
2/ N
2Under the atmosphere, 400 ℃ of reductase 12 h obtain described catalyst.
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| EP2153894A1 (en) * | 2008-08-05 | 2010-02-17 | Sued-Chemie AG | Catalyst for the reduction of nitrogen oxides in exhaust gas |
| CN101623639B (en) * | 2009-08-11 | 2011-09-14 | 清华大学 | Barium-transition metal-cerium base oxide catalyst for eliminating carbon smoke |
| KR101011830B1 (en) * | 2009-09-30 | 2011-01-31 | 상명대학교 산학협력단 | Mixed metal oxide catalyst for decomposition of nitrogen oxide |
| CN102188971B (en) * | 2011-03-31 | 2013-07-17 | 济南大学 | Quadruple effect catalyst of diesel tail gas and preparation method and application of quadruple effect catalyst |
| CN106362744A (en) * | 2016-08-29 | 2017-02-01 | 环境保护部华南环境科学研究所 | Desulfurization and denitrification catalyst with magnesium aluminum hydrotalcite as carriers and preparing method and application thereof |
| CN106378138A (en) * | 2016-08-29 | 2017-02-08 | 环境保护部华南环境科学研究所 | Catalyst for cooperative control of multiple pollutants in waste incineration flue gas and preparation method and application of catalyst |
| CN110087771A (en) * | 2016-12-19 | 2019-08-02 | Scg化学有限公司 | NOx storage and reducing catalyst and preparation method thereof |
| CN110075833A (en) * | 2019-05-24 | 2019-08-02 | 北京市劳动保护科学研究所 | It is a kind of to remove NO simultaneouslyxWith the catalyst of carbon soot particles and preparation method thereof |
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