CN102658122A - Catalyst for combustion of soot particles in diesel vehicle exhaust, and preparation method thereof - Google Patents
Catalyst for combustion of soot particles in diesel vehicle exhaust, and preparation method thereof Download PDFInfo
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Abstract
The invention provides a rare earth oxide and transition metal oxide-supported alkali metal catalyst for reducing the combustion temperature of soot particles in diesel vehicle exhaust, and a preparation method thereof. The preparation method is characterized in that non-noble metal salts are taken as raw materials, the sol-gel method is employed as the preparation technology, and the preparation process is easy to control. Soluble salts of rare earth Ce, transition metal Mn and alkali metal K are taken as precursors and the mass percents of Ce, Mn and K are adjusted to obtain the K/CeO2-MnO2 catalyst. In a bulk contact condition, the combustion temperature of the soot can be reduced from 575 DEG C in absent of a catalyst to 395 DEG C in present of the catalyst, thereby meeting the temperature range of the diesel vehicle exhaust. The catalyst is a catalyst which is capable of removing the soot in the diesel vehicle exhaust effectively.
Description
One, technical field
The invention belongs to the exhaust gas from diesel vehicle catalyst preparation technical field, be specifically related to a kind of Catalysts and its preparation method that can reduce the ignition temperature of carbon soot particles in the exhaust gas from diesel vehicle.
Two, background technology
Because the minimizing day by day of petroleum resources and the tendency of global warming are serious day by day; Diesel vehicle is because its low oil consumption; Low emission, high power, the characteristic of good endurance; On main equipments such as various power set, truck, locomotive and steamer, obtain increasingly extensive application, have vast potential for future development.But the NOx of diesel engine and particle (PM) discharge capacity is higher, and especially the discharge capacity of PM is about 70 times of gasoline cars, have in addition up to 100 times, brought serious harm for the earth and human beings'health.The combustion characteristic of diesel vehicle has determined carbon soot particles and nitrous oxides concentration height, is main control object.For the requirement of the Abgasgesetz that satisfies increasingly stringent, Europe, the U.S. and Japan are all the one preferred technique of grain catcher (DPF) as degree type diesel engine carbon black particulate burning purifying.In diesel engine exhaust system, trap being installed is a kind of cost-effective post-processing technology; It accumulates in the soot particulate in the diesel exhaust gas in the trap through means such as interception, depositions; After soot is accumulated to a certain degree; Be removed with means such as burnings again, thus the regeneration of realization trap.
The exploitation focus of trap regeneration mode is a catalytic combustion in recent years; It is the catalyst that incendivity is eliminated under delivery temperature that the initiation temperature of i.e. exploitation reduction soot particulate makes it; Cerium-based composite oxides can provide Lattice Oxygen to come the oxidation soot as activation oxygen species; And utilize and store oxygen characteristic additional and activation oxygen from air, become one type of new catalyst of primary study in recent years.To the doping vario-property of cerium base oxide, be the new way of an exploitation catalysis soot combustion catalyst, for reducing the carbon-smoke combustion temperature significantly, advancing the particle trap to realize that commercialization is significant.
Three, summary of the invention
The object of the present invention is to provide a kind of reduction carbon-smoke combustion temperature, improve the Catalysts and its preparation method of carbon-smoke combustion speed.Described catalyst preparation process is simple, can significantly reduce the temperature of carbon-smoke combustion.Its general formula is K
2O-CeO
2-MnO
2, wherein the mol ratio of Ce: Mn is 1: 3～7: 3, K: (Ce+Mn) be 1: 10-1: 1.
Described K
2O-CeO
2-MnO
2Catalyst adopts the sol-gel process preparation, and preparation process is following:
1), takes by weighing an amount of cerous nitrate Ce (NO according to the component and the mol ratio thereof of catalyst
3)
36H
2O, manganese nitrate Mn (NO
3)
2, potassium nitrate KNO
3Be mixed with solution,
2) in the mixed solution of step 1 gained, add complexing agent citric acid and pore creating material.Wherein the citric acid addition be the cation mole 1-3 doubly, the addition of pore creating material is the 5-15wt% of citric acid consumption, under 60-100 ℃ condition, forms thick colloid through stirring
3) with the colloid that obtains in the step 2 100-150 ℃ of drying in the baking oven of air atmosphere, 500-650 ℃ of following roasting promptly gets this catalyst.
Catalyst provided by the invention is used for purification of diesel car discharge tail gas and pollutes, and can soot be transformed burning and be CO
2Temperature be reduced within the tail gas scope of diesel vehicle.In the presence of this catalyst; With the simulation exhaust gas from diesel vehicle is combustion atmosphere, can the ignition temperature of soot be reduced to 395 ℃ by 575 ℃, has satisfied the low temperature requirement of modern diesel engine truck exhaust basically; And burning velocity is fast nearly one times, and the particle trap can be regenerated rapidly.
The invention has the advantages that: adopting the nitrate of rare earth cerium and transient metal Mn and alkali metal K is raw material, and the Catalyst Production cost is low; The preparation of employing sol-gel process, technology is simple, and course of reaction is easy to control, easy realization of industrial production.
Four, description of drawings
Combustion curve when Fig. 1 is loose contact of catalyst-free and catalyst of the present invention simulation diesel vehicle exhaust carbon-smoke particle, the temperature when wherein Tm represents soot maximum combustion speed.
Five, the specific embodiment:
For clearer explanation the present invention, enumerate following examples, but it has no restriction to scope of the present invention.
Embodiment 1.
In the 200ml beaker, add 0.101g potassium nitrate KNO
3, 3.04g cerous nitrate Ce (NO
3)
36H
2O, 0.537g manganese nitrate Mn (NO
3)
2And the dissolving of 10ml deionized water and stirring, under stirring at room, add the 2.732g citric acid again, add 0.32g polyethylene glycol (molecular weight 400) after the dissolving again, after dropwising,, form thick colloid until water evaporates 75-80 ℃ of heated and stirred.Then the gained colloid was spent the night in air atmosphere 110 dryings in 24 hours, take out its porphyrize dry back, places 600 ℃ of roastings of Muffle furnace 4 hours, promptly gets composite oxide catalysts K after stove is cold
0.1/ Ce
0.7Mn
0.3O
2
With the above-mentioned catalyst that obtains, (Printex-U Degussa) in agate mortar with spoon gently scrapes mixing 2min by mass ratio, with the loose contact conditions of simulation catalyst and soot at 10: 1 with soot.At 10%O
2In the atmosphere of+Ar, air speed is 12000h
-1The time, carry out TPO experiment, with the heating rate of 5 ℃/min, burn down fully to soot from 200 ℃, write down CO with chromatogram
2Generation situation with CO.K
0.1/ Ce
0.7Mn
0.3O
2Tm be about 485 ℃, the CO of generation
2Selectivity be 95%.
As blank result, (Printex-U Degussa) is contained in the reactor, at 10%O to get the 5mg soot
2In the atmosphere of+Ar, air speed is 12000h
-1The time, carry out TPO experiment, with the heating rate of 5 ℃/min, burn down fully to soot from 200 ℃, write down CO with chromatogram
2Generation situation with CO.The Tm of soot is about 570 ℃, the CO of generation
2Selectivity be 20%.
Embodiment 2
In the 200ml beaker, add 0.202g potassium nitrate KNO
3, 3.04g cerous nitrate Ce (NO
3)
36H
2O, 0.537g manganese nitrate Mn (NO
3)
2And the dissolving of 10ml deionized water and stirring, under stirring at room, add the 2.732g citric acid again, add 0.32g polyethylene glycol (molecular weight 400) after the dissolving again, after dropwising,, form thick colloid until water evaporates 75-80 ℃ of heated and stirred.Then the gained colloid was spent the night in air atmosphere 110 dryings in 24 hours, take out its porphyrize dry back, places 600 ℃ of roastings of Muffle furnace 4 hours, promptly gets composite oxide catalysts K after stove is cold
0.2/ Ce
0.7Mn
0.3O
2
The same with embodiment 1, (Printex-U Degussa) gently scrapes with spoon in agate mortar by mass ratio 10: 1 and mixes 2min, with the loose contact conditions of simulation catalyst and soot with the above-mentioned catalyst that obtains and soot.At 10%O
2In the atmosphere of+Ar, air speed is 12000h
-1The time, carry out TPO experiment, with the heating rate of 5 ℃/min, burn down fully to soot from 200 ℃, write down CO with chromatogram
2Generation situation with CO.K
0.2/ Ce
0.7Mn
0.3O
2Tm be about 440 ℃, the CO of generation
2Selectivity be 97%.
Embodiment 3
In the 200ml beaker, add 0.303g potassium nitrate KNO
3, 3.04g cerous nitrate Ce (NO
3)
36H
2O, 0.537g manganese nitrate Mn (NO
3)
2And the dissolving of 10ml deionized water and stirring, under stirring at room, add the 2.732g citric acid again, add 0.32g polyethylene glycol (molecular weight 400) after the dissolving again, after dropwising,, form thick colloid until water evaporates 75-80 ℃ of heated and stirred.Then the gained colloid was spent the night in air atmosphere 110 dryings in 24 hours, take out its porphyrize dry back, places 600 ℃ of roastings of Muffle furnace 4 hours, promptly gets composite oxide catalysts K after stove is cold
0.3/ Ce
0.7Mn
0.3O
2
Press the combustion case that embodiment 1 the same method is measured soot, Tm is 420 ℃ under this catalyst, CO
2Selectivity is 97%.
Embodiment 4
In the 200ml beaker, add 0.404g potassium nitrate KNO
3, 3.04g cerous nitrate Ce (NO
3)
36H
2O, 0.537g manganese nitrate Mn (NO
3)
2And the dissolving of 10ml deionized water and stirring, under stirring at room, add the 2.732g citric acid again, add 0.32g polyethylene glycol (molecular weight 400) after the dissolving again, after dropwising,, form thick colloid until water evaporates 75-80 ℃ of heated and stirred.Then the gained colloid was spent the night in air atmosphere 110 dryings in 24 hours, take out its porphyrize dry back, places 600 ℃ of roastings of Muffle furnace 4 hours, promptly gets composite oxide catalysts K after stove is cold
0.4/ Ce
0.7Mn
0.3O
2
Press the combustion case that embodiment 1 the same method is measured soot, Tm is 395 ℃ under this catalyst, CO
2, selectivity is 98%.
Embodiment 5
In the 200ml beaker, add 0.505g potassium nitrate KNO
3, 3.04g cerous nitrate Ce (NO
3)
36H
2O, 0.537g manganese nitrate Mn (NO
3)
2And the dissolving of 10ml deionized water and stirring, under stirring at room, add the 2.732g citric acid again, add 0.32g polyethylene glycol (molecular weight 400) after the dissolving again, after dropwising,, form thick colloid until water evaporates 75-80 ℃ of heated and stirred.Then the gained colloid was spent the night in air atmosphere 110 dryings in 24 hours, take out its porphyrize dry back, places 600 ℃ of roastings of Muffle furnace 4 hours, promptly gets composite oxide catalysts K after stove is cold
0.5/ Ce
0.7Mn
0.3O
2
Press the combustion case that embodiment 1 the same method is measured soot, Tm is 410 ℃ under this catalyst, CO
2, selectivity is 96%.
Embodiment 6
In the 200ml beaker, add 0.707g potassium nitrate KNO
3, 3.04g cerous nitrate Ce (NO
3)
36H
2O, 0.537g manganese nitrate Mn (NO
3)
2And the dissolving of 10ml deionized water and stirring, under stirring at room, add the 2.732g citric acid again, add 0.32g polyethylene glycol (molecular weight 400) after the dissolving again, after dropwising,, form thick colloid until water evaporates 75-80 ℃ of heated and stirred.Then the gained colloid was spent the night in air atmosphere 110 dryings in 24 hours, take out its porphyrize dry back, places 600 ℃ of roastings of Muffle furnace 4 hours, promptly gets composite oxide catalysts K after stove is cold
0.7/ Ce
0.7Mn
0.3O
2
Press the combustion case that embodiment 1 the same method is measured soot, Tm is 425 ℃ under this catalyst, CO
2, selectivity is 95%.
Embodiment 7
In the 200ml beaker, add 1.01g potassium nitrate KNO
3, 3.04g cerous nitrate Ce (NO
3)
36H
2O, 0.537g manganese nitrate Mn (NO
3)
2And the dissolving of 10ml deionized water and stirring, under stirring at room, add the 2.732g citric acid again, add 0.32g polyethylene glycol (molecular weight 400) after the dissolving again, after dropwising,, form thick colloid until water evaporates 75-80 ℃ of heated and stirred.Then the gained colloid was spent the night in air atmosphere 110 dryings in 24 hours, take out its porphyrize dry back, places 600 ℃ of roastings of Muffle furnace 4 hours, promptly gets composite oxide catalysts K after stove is cold
1.0/ Ce
0.7Mn
0.3O
2
Press the combustion case that embodiment 1 the same method is measured soot, Tm is 430 ℃ under this catalyst, CO
2, selectivity is 95%.
Embodiment 8
In the 200ml beaker, add 0.404g potassium nitrate KNO
3, 2.17g cerous nitrate Ce (NO
3)
36H
2O, 0.895g manganese nitrate Mn (NO
3)
2And the dissolving of 10ml deionized water and stirring, under stirring at room, add the 2.732g citric acid again, add 0.32g polyethylene glycol (molecular weight 400) after the dissolving again, after dropwising,, form thick colloid until water evaporates 75-80 ℃ of heated and stirred.Then the gained colloid was spent the night in air atmosphere 110 dryings in 24 hours, take out its porphyrize dry back, places 600 ℃ of roastings of Muffle furnace 4 hours, promptly gets composite oxide catalysts K after stove is cold
0.4/ Ce
0.5Mn
0.5O
2
Press the combustion case that embodiment 1 the same method is measured soot, Tm is 440 ℃ under this catalyst, CO
2, selectivity is 94%.
Embodiment 9
In the 200ml beaker, add 0.404g potassium nitrate KNO
3, 1.085g cerous nitrate Ce (NO
3)
36H
2O, 1.342g manganese nitrate Mn (NO
3)
2And the dissolving of 10ml deionized water and stirring, under stirring at room, add the 2.732g citric acid again, add 0.32g polyethylene glycol (molecular weight 400) after the dissolving again, after dropwising,, form thick colloid until water evaporates 75-80 ℃ of heated and stirred.Then the gained colloid was spent the night in air atmosphere 110 dryings in 24 hours, take out its porphyrize dry back, places 600 ℃ of roastings of Muffle furnace 4 hours, promptly gets composite oxide catalysts K after stove is cold
0.4/ Ce
0.25Mn
0.75O
2
Press the combustion case that embodiment 1 the same method is measured soot, Tm is 455 ℃ under this catalyst, CO
2, selectivity is 92%.
Embodiment 10
In the 200ml beaker, add 3.04g cerous nitrate Ce (NO
3)
36H
2O, 0.537g manganese nitrate Mn (NO
3)
2And the dissolving of 10ml deionized water and stirring, under stirring at room, add the 2.732g citric acid again, add 0.32g polyethylene glycol (molecular weight 400) after the dissolving again, after dropwising,, form thick colloid until water evaporates 75-80 ℃ of heated and stirred.Then the gained colloid was spent the night in air atmosphere 110 dryings in 24 hours, take out its porphyrize dry back, places 600 ℃ of roastings of Muffle furnace 4 hours, promptly gets composite oxide catalysts Ce after stove is cold
0.7Mn
0.3O
2
Press the combustion case that embodiment 1 the same method is measured soot, Tm is 530 ℃ under this catalyst, CO
2Selectivity is 91%.
Embodiment 11
In the 200ml beaker, add 0.404g potassium nitrate KNO
3, 4.34g cerous nitrate Ce (NO
3)
36H
2O and the dissolving of 10ml deionized water and stirring add the 2.732g citric acid again under stirring at room, add 0.32g polyethylene glycol (molecular weight 400) after the dissolving again, after dropwising, 75-80 ℃ of heated and stirred, form thick colloid until water evaporates.Then the gained colloid was spent the night in air atmosphere 110 dryings in 24 hours, take out its porphyrize dry back, places 600 ℃ of roastings of Muffle furnace 4 hours, promptly gets composite oxide catalysts K after stove is cold
0.4/ CeO
2
Press the combustion case that embodiment 1 the same method is measured soot, Tm is 435 ℃ under this catalyst, CO
2, selectivity is 93%.
Embodiment 12
In the 200ml beaker, add 0.404g potassium nitrate KNO
3, 1.79g manganese nitrate Mn (NO
3)
2, and the dissolving of 10ml deionized water and stirring, under stirring at room, add the 2.732g citric acid again, add 0.32g polyethylene glycol (molecular weight 400) after the dissolving again, after dropwising,, form thick colloid until water evaporates 75-80 ℃ of heated and stirred.Then the gained colloid was spent the night in air atmosphere 110 dryings in 24 hours, take out its porphyrize dry back, places 600 ℃ of roastings of Muffle furnace 4 hours, promptly gets composite oxide catalysts K after stove is cold
0.4/ CeO
2
Press the combustion case that embodiment 1 the same method is measured soot, Tm is 460 ℃ under this catalyst, CO
2Selectivity is 91%.
Above-mentioned test experiments result is as shown in table 1:
| Catalyst | Tm(℃) | ?CO 2The selectivity (%) that generates |
| Catalyst-free | 575 | ?/ |
| K 0.1/Ce 0.7Mn 0.3O 2 | 485 | ?94 |
| K 0.2/Ce 0.7Mn 0.3O 2 | 440 | ?95 |
| K 0.3/Ce 0.7Mn 0.3O 2 | 420 | ?97 |
| K 0.4/Ce 0.7Mn 0.3O 2 | 395 | ?98 |
| K 0.5/Ce 0.7Mn 0.3O 2 | 410 | ?96 |
| K 0.7/Ce 0.7Mn 0.3O 2 | 425 | ?95 |
| K 1.0/Ce 0.7Mn 0.3O 2 | 430 | ?95 |
| K 0.4/Ce 0.5Mn 0.5O 2 | 440 | ?94 |
| K 0.4/Ce 0.25Mn 0.75O 2 | 455 | ?92 |
| Ce 0.7Mn 0.3O 2 | 530 | ?91 |
| K 0.4/CeO 2 | 435 | ?93 |
| K 0.4/MnO x | 460 | ?90 |
Claims (5)
1. the catalyst of catalyzed carbon smoke particle burning, it is characterized in that: the composition general formula of this catalyst is K/CeO
2-MnO
2
2. catalyst according to claim 1 is characterized in that: the existence form of K is an oxide, carbonate or nitrate, and the existence form of Ce is CeO
2, the existence form of Mn is MnO
2
3. catalyst according to claim 1, the mol ratio of Ce: Mn are 1: 3～7: 3, K: mol ratio (Ce+Mn) is 1: 10-1: 1.
4. according to the said catalyst K-CeO of claim 1
2-MnO
2The preparation of employing sol-gel process is characterized in that its preparation method is following:
1) according to the composition and the content thereof of catalyst, take by weighing proper C e, the salt of the solubility of Mn and K is mixed with solution;
2) in the mixed solution of step 1 gained, add complexing agent citric acid and pore creating material.Wherein the addition of complexing agent be the cation mole 1-3 doubly, the addition of pore creating material is the 5-15wt% of complexing agent consumption; Under 60-100 ℃ condition, form thick colloid through stirring;
3) with the colloid that obtains in the step 2 100-150 ℃ of drying in the baking oven of air atmosphere, 500-650 ℃ of following roasting promptly gets this catalyst.
5. Preparation of catalysts method according to claim 3 is characterized in that: selected pore creating material is polyethylene glycol or methylcellulose, and the cerium salt of used solubility is cerous nitrate (Ce (NO
3)
3), ammonium ceric nitrate (Ce (NH
4)
2(NO
3)
6) or cerium chloride (CeCl
3); Used manganese salt is manganese nitrate (Mn (NO
3)
2) or manganese acetate Mn (Ac)
2); The K salt that uses is nitric acid (KNO
3), potassium acetate KAc or potassium chloride (KCl).
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| CN103464145A (en) * | 2013-09-11 | 2013-12-25 | 东华大学 | Preparation method of catalyst for simultaneously removing NO and fine particles in coal-fired flue gas |
| CN105498742A (en) * | 2015-09-15 | 2016-04-20 | 昆明理工大学 | Potassium-based soot combustion catalyst and preparation method thereof |
| CN105797706A (en) * | 2014-12-29 | 2016-07-27 | 北京有色金属研究总院 | Cerium-lanthanum solid solution catalyst for purifying diesel vehicle exhaust particles and preparation method thereof |
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Application publication date: 20120912 |