CN1721066A - Catalyst for lowering combustion temperature of soot in diesel exhaust gas and preparation method thereof - Google Patents
Catalyst for lowering combustion temperature of soot in diesel exhaust gas and preparation method thereof Download PDFInfo
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- CN1721066A CN1721066A CN 200510043564 CN200510043564A CN1721066A CN 1721066 A CN1721066 A CN 1721066A CN 200510043564 CN200510043564 CN 200510043564 CN 200510043564 A CN200510043564 A CN 200510043564A CN 1721066 A CN1721066 A CN 1721066A
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Abstract
The present invention relates catalyst to reduce burning temperature of carbon smoke particle in exhaust gas from diesel truck. Use LaNiO3 or La2NiO4base perovskite type composite oxide with B position atom of Ni as base, with assistant active constituent of kalium, cobalt, rare earth or palladium. It is prepared with sol-gal process or solution combustion method. It can reduce the burning temperature from 550Deg to 250~400Deg and satisfy low temperature require in the main; the burning speed enhances almost one times and very useful.
Description
(1) technical field under
The present invention relates to the catalyst of combustion temperature of soot in a kind of tail gas that can reduce emission of diesel engine and go up the Preparation of catalysts method.The technical field that belongs to catalytic combustion.
(2) background technology
Diesel-powered car is owing to have low oil consumption, low emission, high power characteristic, 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 2003, FAW-Volkswagen released first naturally aspirated Diesel car Jetta SDI in the whole nation, release another turbo-charging diesel car Bora TDI in February, 2004, releases the A6 TDI of Audi (2.5L) 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.But the major pollutants carbon soot particles and the nitrogen oxide of diesel engine emissions are higher.The former mostly is the particle less than 2.5 microns greatly, and human respiratory system and biology are had bigger harm; The latter is the arch-criminal of acid rain and photochemical fog, is the focus of studying in the world therefore.The research of relevant elimination NOx has more report both at home and abroad, but the research of elimination carbon soot particles is then less.The problem that solves soot mainly concentrates on particulate filter collects carbon soot particles and its oxidation (burning) is CO
2This be from twentieth century since the mid-90 developed country such as America and Europe at the emphasis of diesel exhaust gas field of purification research and development, also be that Euro V standard, U.S. execution Tier 2 standards are carried out in Europe in 2008, be hopeful the carbon soot particles purification techniques of extensive use most.At present, carbon soot particles is oxidized to CO
2Main direction be catalytic combustion, and activity of such catalysts not only will satisfy diesel engine vent gas 150-400 ℃ low temperature, but also can reach the high temperature more than 600 ℃ when running at high speed, and therefore also requires catalyst at the high-temperature hydrothermal stability more than 600 ℃.
(3) summary of the invention
The object of the present invention is to provide a kind of catalyst, can reduce diesel vehicle soot particle burning temperature, existing low-temperature burning activity has high-temperature stability again; In addition, this catalyst has the catalytic performance height, the characteristics that diesel vehicle soot particle initiation temperature is low, burning velocity is fast.
Another object of the present invention is to provide above-mentioned Preparation of catalysts method.
The present invention realizes by following measure:
The catalyst of combustion temperature of soot in the reduction exhaust gas from diesel vehicle of the present invention, active ingredient contains perofskite type oxide LaNiO
3Or perovskite-like type oxide La
2NiO
4One or both.
Catalyst of the present invention in order to improve catalytic effect, also is added with one or more of auxiliary activity component of potassium, cobalt, cerium or palladium.Wherein, potassium, cerium are used for replacing respectively lanthanum; Cobalt, palladium are used for replacing respectively nickel.
Catalyst of the present invention can also be added with auxiliary activity component of potassium, cobalt, cerium and palladium simultaneously, is used for part and replaces lanthanum and nickel.Wherein, the optimal proportion of above-mentioned replacement is: the mol ratio of lanthanum, cerium, potassium is 0.5: 0.3: 0.2; The mol ratio of nickel, cobalt, palladium is 0.8: 0.15: 0.05.
Above-mentioned catalyst can be prepared by the following method:
A is according to the component and the weight ratio preparing metal mixed nitrate aqueous solution thereof of catalyst;
B adding mol ratio is 1.5 times a citric acid, forms citric acid metal salt complex colloidal sol;
C colloidal sol changes gel 70 ℃ of oven dry into after 24 hours, in 850 ℃ of roastings 18 hours in Muffle furnace, obtains this catalyst.
Above-mentioned catalyst can also be prepared by the following method:
A is according to the component and the weight ratio preparing metal mixed nitrate aqueous solution thereof of catalyst;
B adding mol ratio is 1.5 times a citric acid, forms citric acid metal salt complex colloidal sol;
C puts into the Muffle furnace that preheats under 350 ℃ with colloidal sol, burns, and obtains fluffy catalyst fines, in 850 ℃ of roastings 18 hours, obtains this catalyst again.
Catalyst of the present invention is used for purification of diesel car discharge tail gas and pollutes, and can be CO with the carbon-smoke combustion of collecting on the particle trap
2Temperature be reduced in the temperature range of exhaust gas from diesel vehicle.In the presence of this catalyst, with the simulation exhaust gas from diesel vehicle is combustion atmosphere, can be with the ignition temperature of soot by being reduced to 250 ℃-400 ℃ more than 550 ℃, basically satisfied the low temperature requirement of modern diesel engine truck exhaust, and burning velocity is fast nearly one times, make the particle trap need not other assisted heating device, can regenerate rapidly.Because the stability of perovskite structure itself, catalyst of the present invention has at the high-temperature hydrothermal stability more than 600 ℃.The activity characterization result also obtains after heat treatment more than 600 ℃ (roasting is 18 hours in 850 ℃ of air).
Preparation method of the present invention, it is simple to have method, and easy operating is suitable for suitability for industrialized production.
(4) description of drawings
Fig. 1 is the thermal analysis curve of pure carbon cigarette burning
Fig. 2 is the catalyst La of embodiment 10
0.8K
0.2Ni
0.8Co
0.2O
3The thermal analysis curve of catalysis carbon-smoke combustion
Among the figure, 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
f-T
i) represent carbon-smoke combustion speed.
Among Fig. 1 during catalyst-free, the pure carbon cigarette initiation temperature be that 564.2 ℃, burning velocity are 97 ℃.
Among Fig. 2 at La
0.8K
0.2Ni
0.8Co
0.2O
3Catalyst exists down, and the initiation temperature of soot is that 350 ℃, burning velocity are 56 ℃, and burning velocity has been compared soon nearly one times with the pure carbon cigarette.
(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
Take by weighing 0.025 mole lanthanum nitrate, 0.015 mole cerous nitrate, 0.01 mole potassium nitrate, 0.04 mole nickel nitrate, 0.0075 mole cobalt nitrate, 0.0025 mole palladium nitrate, add 50 ml deionized water, stirring and dissolving, add 0.075 mole of citric acid again, stirring makes it dissolving, gets a kind of liquid with viscosity.This liquid is put into baking oven at 70 ℃ slowly evaporate,, then it is transferred in the clean enamel tray until the gel that gets a kind of thickness, evenly spread out, add about 50 milliliters of absolute ethyl alcohols, after in air, lighting, gel generation self-propagating combustion produces extremely bulk pitchy powder at last.Collect the powder of gained, be transferred in the crucible, put into Muffle furnace, 850 ℃ of following roastings 18 hours.
Above-mentioned catalyst is mixed by mass ratio with carbon soot particles at 9: 1, grind the platinum crucible of putting into thermal analyzer in one hour at agate mortar, the programming rate with 10 ℃/min under the atmosphere of air is raised to 725 ℃ from 30 ℃.Write down weightless starting point with thermal analyzer, be the burning initial temperature of carbon soot particles, generally at 300 ℃-400 ℃.
Embodiment 2:
Take by weighing 0.025 mole lanthanum nitrate, 0.015 mole cerous nitrate, 0.01 mole potassium nitrate, 0.04 mole nickel nitrate, 0.0075 mole cobalt nitrate, 0.0025 mole palladium nitrate, add 50 ml deionized water, stirring and dissolving, add 0.075 mole of citric acid again, stirring makes it dissolving, gets a kind of liquid with viscosity.This liquid is put into baking oven at 70 ℃ slowly evaporate,, then it is transferred in the clean enamel tray until the gel that gets a kind of thickness, evenly spread out, add about 50 milliliters of absolute ethyl alcohols, after in air, lighting, gel generation self-propagating combustion produces extremely bulk pitchy powder at last.Collect the powder of gained, be transferred in the crucible, put into Muffle furnace, 850 ℃ of following roastings 18 hours.
Above-mentioned catalyst is mixed by mass ratio with carbon soot particles at 9: 1, in measuring cup, shake up one hour, put into fixed bed reactors, at 1000ppm NO+10v%O
2Programming rate with 10 ℃/min under the atmosphere of+Ar is raised to 725 ℃ from 30 ℃.Write down CO with quadrupole mass spectrometer
2The generation situation, CO
2The starting point that generates is the burning initial temperature of carbon soot particles, generally at 250 ℃-350 ℃.
Embodiment 3:
Take by weighing 0.025 mole lanthanum nitrate, 0.015 mole cerous nitrate, 0.01 mole potassium nitrate, 0.04 mole nickel nitrate, 0.0075 mole cobalt nitrate, 0.0025 mole palladium nitrate, add 50 ml deionized water, stirring and dissolving, add 0.075 mole of citric acid again, stirring makes it dissolving, gets a kind of liquid with viscosity.This liquid is put into the Muffle furnace that is heated to 350 ℃, and solution burns, and obtains fluffy catalyst fines, again 850 ℃ of following roastings 18 hours.
Press the burning initial temperature of embodiment 1 measurement carbon soot particles, generally at 300 ℃-400 ℃.Press the burning initial temperature of embodiment 2 measurement carbon soot particles, generally at 250 ℃-350 ℃.
Embodiment 4:
Take by weighing 0.05 mole lanthanum nitrate, 0.05 mole nickel nitrate, add 50 ml deionized water, stirring and dissolving adds 0.075 mole of citric acid again, stirs to make it dissolving, gets a kind of liquid with viscosity.This liquid is put into baking oven at 70 ℃ slowly evaporate,, then it is transferred in the clean enamel tray until the gel that gets a kind of thickness, evenly spread out, add about 50 milliliters of absolute ethyl alcohols, after in air, lighting, gel generation self-propagating combustion produces extremely bulk pitchy powder at last.Collect the powder of gained, be transferred in the crucible, put into Muffle furnace, 850 ℃ of following roastings 18 hours.
Press the burning initial temperature of embodiment 1 measurement carbon soot particles, generally at 400 ℃.
Embodiment 5:
Take by weighing 0.05 mole lanthanum nitrate, 0.05 mole nickel nitrate, add 50 ml deionized water, stirring and dissolving adds 0.075 mole of citric acid again, stirs to make it dissolving, gets a kind of liquid with viscosity.This liquid is put into the Muffle furnace that is heated to 350 ℃, and solution burns, and obtains fluffy catalyst fines, again 850 ℃ of following roastings 18 hours.
Press the burning initial temperature of embodiment 1 measurement carbon soot particles, generally at 400 ℃.
Embodiment 6:
Take by weighing 0.1 mole lanthanum nitrate, 0.05 mole nickel nitrate, add 50 ml deionized water, stirring and dissolving adds 0.075 mole of citric acid again, stirs to make it dissolving, gets a kind of liquid with viscosity.This liquid is put into baking oven at 70 ℃ slowly evaporate,, then it is transferred in the clean enamel tray until the gel that gets a kind of thickness, evenly spread out, add about 50 milliliters of absolute ethyl alcohols, after in air, lighting, gel generation self-propagating combustion produces extremely bulk pitchy powder at last.Collect the powder of gained, be transferred in the crucible, put into Muffle furnace, 850 ℃ of following roastings 18 hours.
Press the burning initial temperature of embodiment 1 measurement carbon soot particles, generally at 400 ℃.
Embodiment 7:
Take by weighing 0.1 mole lanthanum nitrate, 0.05 mole nickel nitrate, add 50 ml deionized water, stirring and dissolving adds 0.075 mole of citric acid again, stirs to make it dissolving, gets a kind of liquid with viscosity.This liquid is put into the Muffle furnace that is heated to 350 ℃, and solution burns, and obtains fluffy catalyst fines, again 850 ℃ of following roastings 18 hours.
Press the burning initial temperature of embodiment 1 measurement carbon soot particles, generally at 400 ℃.
Embodiment 8:
Take by weighing 0.03 mole lanthanum nitrate, 0.02 mole cerous nitrate, 0.04 mole nickel nitrate, 0.01 mole cobalt nitrate, add 50 ml deionized water, stirring and dissolving adds 0.075 mole of citric acid again, stirring makes it dissolving, gets a kind of liquid with viscosity.This liquid is put into baking oven at 70 ℃ slowly evaporate,, then it is transferred in the clean enamel tray until the gel that gets a kind of thickness, evenly spread out, add about 50 milliliters of absolute ethyl alcohols, after in air, lighting, gel generation self-propagating combustion produces extremely bulk pitchy powder at last.Collect the powder of gained, be transferred in the crucible, put into Muffle furnace, 850 ℃ of following roastings 18 hours.
Press the burning initial temperature of embodiment 1 measurement carbon soot particles, generally at 365 ℃
Embodiment 9:
Take by weighing 0.03 mole lanthanum nitrate, 0.02 mole cerous nitrate, 0.04 mole nickel nitrate, 0.01 mole cobalt nitrate, add 50 ml deionized water, stirring and dissolving adds 0.075 mole of citric acid again, stirring makes it dissolving, gets a kind of liquid with viscosity.This liquid is put into the Muffle furnace that is heated to 350 ℃, and solution burns, and obtains fluffy catalyst fines, again 850 ℃ of following roastings 18 hours.
Press the burning initial temperature of embodiment 1 measurement carbon soot particles, generally at 365 ℃
Take by weighing 0.04 mole lanthanum nitrate, 0.01 mole potassium nitrate, 0.04 mole nickel nitrate, 0.01 mole cobalt nitrate, add 50 ml deionized water, stirring and dissolving adds 0.075 mole of citric acid again, stirring makes it dissolving, gets a kind of liquid with viscosity.This liquid is put into baking oven at 70 ℃ slowly evaporate,, then it is transferred in the clean enamel tray until the gel that gets a kind of thickness, evenly spread out, add about 50 milliliters of absolute ethyl alcohols, after in air, lighting, gel generation self-propagating combustion produces extremely bulk pitchy powder at last.Collect the powder of gained, be transferred in the crucible, put into Muffle furnace, 850 ℃ of following roastings 18 hours.
Press the burning initial temperature of embodiment 1 measurement carbon soot particles, generally at 350 ℃.
Get above-mentioned catalyst, carbon-smoke combustion carried out heat analyze, the thermal analysis curve of its carbon-smoke combustion as shown in Figure 2, burning velocity is 56 ℃, compares with the burning velocity 97 ℃ (as Fig. 1) of catalyst-free, and is fast nearly 1 times.
Embodiment 11
Take by weighing 0.04 mole lanthanum nitrate, 0.01 mole potassium nitrate, 0.04 mole nickel nitrate, 0.01 mole cobalt nitrate, add 50 ml deionized water, stirring and dissolving adds 0.075 mole of citric acid again, stirring makes it dissolving, gets a kind of liquid with viscosity.This liquid is put into the Muffle furnace that is heated to 350 ℃, and solution burns, and obtains fluffy catalyst fines, again 850 ℃ of following roastings 18 hours.
Press the burning initial temperature of embodiment 1 measurement carbon soot particles, generally at 350 ℃.
Embodiment 12
Take by weighing 0.03 mole lanthanum nitrate, 0.02 mole cerous nitrate, 0.05 mole nickel nitrate, add 50 ml deionized water, stirring and dissolving adds 0.075 mole of citric acid again, stirs to make it dissolving, gets a kind of liquid with viscosity.This liquid is put into baking oven at 70 ℃ slowly evaporate,, then it is transferred in the clean enamel tray until the gel that gets a kind of thickness, evenly spread out, add about 50 milliliters of absolute ethyl alcohols, after in air, lighting, gel generation self-propagating combustion produces extremely bulk pitchy powder at last.Collect the powder of gained, be transferred in the crucible, put into Muffle furnace, 850 ℃ of following roastings 18 hours.
Press the burning initial temperature of embodiment 1 measurement carbon soot particles, generally at 365 ℃.
Embodiment 13
Take by weighing 0.03 mole lanthanum nitrate, 0.02 mole cerous nitrate, 0.05 mole nickel nitrate, add 50 ml deionized water, stirring and dissolving adds 0.075 mole of citric acid again, stirs to make it dissolving, gets a kind of liquid with viscosity.This liquid is put into the Muffle furnace that is heated to 350 ℃, and solution burns, and obtains fluffy catalyst fines, again 850 ℃ of following roastings 18 hours.
Press the burning initial temperature of embodiment 1 measurement carbon soot particles, generally at 365 ℃.
Embodiment 14
Take by weighing 0.09 mole lanthanum nitrate, 0.01 mole potassium nitrate, 0.04 mole nickel nitrate, 0.01 mole cobalt nitrate, add 50 ml deionized water, stirring and dissolving adds 0.075 mole of citric acid again, stirring makes it dissolving, gets a kind of liquid with viscosity.This liquid is put into baking oven at 70 ℃ slowly evaporate,, then it is transferred in the clean enamel tray until the gel that gets a kind of thickness, evenly spread out, add about 50 milliliters of absolute ethyl alcohols, after in air, lighting, gel generation self-propagating combustion produces extremely bulk pitchy powder at last.Collect the powder of gained, be transferred in the crucible, put into Muffle furnace, 850 ℃ of following roastings 18 hours.
Press the burning initial temperature of embodiment 1 measurement carbon soot particles, generally at 350 ℃.
Embodiment 15
Take by weighing 0.09 mole lanthanum nitrate, 0.01 mole potassium nitrate, 0.04 mole nickel nitrate, 0.01 mole cobalt nitrate, add 50 ml deionized water, stirring and dissolving adds 0.075 mole of citric acid again, stirring makes it dissolving, gets a kind of liquid with viscosity.This liquid is put into the Muffle furnace that is heated to 350 ℃, and solution burns, and obtains fluffy catalyst fines, again 850 ℃ of following roastings 18 hours.
Press the burning initial temperature of embodiment 1 measurement carbon soot particles, generally at 350 ℃.
Claims (6)
1. catalyst that reduces combustion temperature of soot in the exhaust gas from diesel vehicle is characterized in that:
Active ingredient contains perofskite type oxide LaNiO
3Or perovskite-like type oxide La
2NiO
4One or both.
2. catalyst according to claim 1 is characterized in that: contain one or more of auxiliary activity component of potassium, cobalt, cerium or palladium.
3. catalyst according to claim 1 is characterized in that: contain auxiliary activity component of potassium, cobalt, cerium and palladium.
4. catalyst according to claim 3 is characterized in that: the mol ratio of lanthanum, cerium, potassium is 0.5: 0.3: 0.2; The mol ratio of nickel, cobalt, palladium is 0.8: 0.15: 0.05.
5. a claim 1,2 or 3 described Preparation of catalysts methods is characterized in that: may further comprise the steps,
A is according to the component and the weight ratio preparing metal mixed nitrate aqueous solution thereof of catalyst;
B adding mol ratio is 1.5 times a citric acid, forms citric acid metal salt complex colloidal sol;
C colloidal sol changes gel 70 ℃ of oven dry into after 24 hours, in 850 ℃ of roastings 18 hours in Muffle furnace, obtains this catalyst.
6. a claim 1,2 or 3 described Preparation of catalysts methods is characterized in that: may further comprise the steps,
A is according to the component and the weight ratio preparing metal mixed nitrate aqueous solution thereof of catalyst;
B adding mol ratio is 1.5 times a citric acid, forms citric acid metal salt complex colloidal sol;
C puts into the Muffle furnace that preheats under 350 ℃ with colloidal sol, burns, and obtains fluffy catalyst fines, in 850 ℃ of roastings 18 hours, obtains this catalyst again.
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| CN101199932B (en) * | 2006-12-13 | 2010-12-22 | 中国石油化工股份有限公司 | Iron-based catalyst for ft synthesis and preparation thereof |
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| CN101822979B (en) * | 2009-03-04 | 2013-05-29 | 中国科学院大连化学物理研究所 | Catalyst capable of reducing soot particle combustion temperature and preparation method thereof |
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