CN101785994A - Nanocrystalline Ce-Ti composite oxide catalyst used for selective catalytic reduction of nitric oxide by utilizing ammonia - Google Patents
Nanocrystalline Ce-Ti composite oxide catalyst used for selective catalytic reduction of nitric oxide by utilizing ammonia Download PDFInfo
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- CN101785994A CN101785994A CN 201010119695 CN201010119695A CN101785994A CN 101785994 A CN101785994 A CN 101785994A CN 201010119695 CN201010119695 CN 201010119695 CN 201010119695 A CN201010119695 A CN 201010119695A CN 101785994 A CN101785994 A CN 101785994A
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Abstract
The invention relates to a preparation method of a nanocrystalline Ce-Ti composite oxide catalyst used for the selective catalytic reduction of nitric oxide by utilizing ammonia and an application thereof. The preparation method of the catalyst is the homogeneous precipitation method, namely, the required cerium salt and titanium salt are prepared to mixed solution, and the molar ratio of cerium and titanium is 0.1-1.0; the solution is continuously stirred for 6-10h at the temperature of 90-95 DEG C by taking excessive urea as the precipitator and then is pumped, filtered, washed and dried; and finally, the catalyst is obtained by roasting the processed solution for 4-6h in the air at the temperature of 400-500 DEG C. In the invention, the nanocrystalline Ce-Ti composite oxide catalyst is prepared by taking non-toxic and harmless raw materials and adopting the simple and easy method, which has the characteristics of high catalytic activity, good N2 selection, wide temperature window, good adaptability of high airspeed condition, good SO2 intoxication resistance and the like. The catalyst is applicable to various tail gas sources including fixed combustion devices in an engine of a diesel vehicle, a coal-fired power plant and the like.
Description
Technical field
The present invention is applied to the environmental catalysis technical field, relates to a kind of nanocrystalline Ce titanium compound oxide catalyst that is used for fixing catalytic purification of nitroxide in source flue gas and the exhaust gas from diesel vehicle.
Background technology
Nitrogen oxide (NO
x) be a kind of important atmosphere pollution, can cause direct harm to health, can also cause great environmental problem such as photochemical fog, acid rain.Therefore, NO
xEmission control technique becomes a research focus of current field of environment protection.
NO in the stationary source flue gas
xBe NO in the atmosphere
xAn important source.The gas denitrifying technology that is most widely used in the world is with NH
3Be reducing agent, selective reduction NO under the effect of catalyst
xGenerate N
2, i.e. NH
3-SCR technology.This The Application of Technology key is the catalyst of exploitation efficient stable.At present, the NH of industrial applications
3-SCR catalyst is many with TiO
2Be carrier loaded a certain amount of V
2O
5(be V
2O
5/ TiO
2), perhaps add WO on this basis
3Or MoO
3Carrying out modification etc. component (is V
2O
5-WO
3/ TiO
2And V
2O
5-MoO
3/ TiO
2).But this catalyst system remains in some problems, such as: contain the noxious material vanadium, in use, enter into environment and have very big bio-toxicity if come off; Its serviceability temperature mostly is 350～430 ℃, has the narrower shortcoming of operating temperature window.In addition,, just can reduce catalyst amount, save denitrification apparatus and take up an area of the space, reduce investment and operating cost if can improve the use air speed of catalyst.Therefore, new high activity, wide temperature window, adaptation high-speed environment, the nontoxic non-vanadium catalyst system of exploitation is used for fixing NO in the flue gas of source
xElimination, have very important economic implications and environmental benefit.
The gasoline car of the three-way catalyst of relative maturation with the technology that is equipped with is compared, with NO
xWith PM be that the tail gas pollution of feature becomes the bottleneck that the restriction diesel vehicle is applied.Up to now, the NO that does not also have a kind of maturation
xPurification techniques is widely used in diesel car tail gas refining, and NH
3-SCR is regarded as being hopeful most to be applied to this technology.
TiO
2And CeO
xAs cheap, nontoxic and efficiently catalysis material obtained paying close attention to widely and studying.TiO
2Mainly be used as various catalyst carriers and photochemical catalyst; CeO
xOwing to its very strong storage-release free oxygen ability and excellent redox property are widely used in the environmental catalysis field.Yet, at present with TiO
2And CeO
xIn conjunction with as NH
3The research of-SCR catalyst seldom.The clear 52-42463A of Japan Patent TOHKEMY discloses a kind of employing coprecipitation method, is the cerium-titanium composite oxide of precipitating reagent preparation with ammoniacal liquor, is used for NH
3-SCR reaction finds that the Ce/Ti mol ratio is the catalytic effect the best between 0.05～0.25.(W.Q.Xu, Y.B.Yu, C.B.Zhang, H.He, Selective catalytic reduction of NO by NH such as Xu
3Over a Ce/TiO
2Catalyst.Catalysis Communications, 9 (2008) 1453-1457.) adopt the Ce/TiO of immersion process for preparing
2Catalyst can realize in 250～375 ℃ of scopes that (air speed is 25000h to 95% above NO conversion ratio
-1); (X.Gao, Y.Jiang, Z.Y.Luo, K.F.Cen, The activity and characterization of CeO such as Gao
2-TiO
2Catalystsprepared by the sol-gel method for selective catalytic reduction of NO with NH
3.Journal ofHazardous Materials doi:10.1016/j.jhazmat.2009.09.112.) adopts the CeO of sol-gel process preparation
2-TiO
2Catalyst can realize in 300～400 ℃ of scopes that (air speed is 50000h for 98.6% NO conversion ratio
-1).More than the cerium titanium catalyst of three kinds of methods preparation have all that temperature window is narrower, low-temperature space is active lower and can not adapt to problem such as high-speed.
Summary of the invention
Existing catalyst system and catalyzing active temperature windows is narrow, low temperature active is poor in order to solve, to shortcomings such as reaction velocity sensitivities, the present invention provides a kind of new nanocrystalline Ce titanium compound oxide catalyst first, is applied to stationary source flue gas and diesel engine vent gas NH
3-SCR denitration.
The Preparation of catalysts method is a sluggish precipitation among the present invention, be about to required two kinds of pairing salt of metal oxide and be made into mixed solution, wherein cerium salt is at least a in cerous chlorate or cerous nitrate or ammonium ceric nitrate or the cerous sulfate, titanium salt is at least a in titanium sulfate or titanyl sulfate or titanium tetrachloride or the Titanium Nitrate, molar ratio computing with metallic element, the ratio of cerium and titanium is 0.1～1.0, with excessive urea (mol ratio of urea and metallic element is 15: 1～30: 1) as precipitating reagent, continuous stirring 6～10h under 90～95 ℃ of temperature conditions, carry out suction filtration and washing then, filter cake is put into baking oven spend the night, after Muffle furnace roasting 4～6h in 400～600 ℃ of air promptly makes the catalyst finished product in 80～120 ℃ of oven dry.The TEM measurement result shows, active phase CeO in the catalyst (the Ce/Ti mol ratio is 0.2) of roasting 5h in 400 ℃ of air
xParticle grain size mainly is distributed in below the 15nm, active phase CeO in the catalyst (the Ce/Ti mol ratio is 0.2) of roasting 5h in 500 ℃ of air
xParticle grain size mainly is distributed in 10～40nm scope.The catalyst (the Ce/Ti mol ratio is 0.2) of roasting 5h has then shown tangible sintering feature in 600 ℃ of air, causes CeO
xAgglomeration of particles has lost nanocrystalline characteristics, thereby makes catalytic activity reduce (seeing Table 1).
The present invention has following advantage:
(1) active temperature windows wide (especially low-temperature space active good) is particularly useful for the big applied environment of motor-vehicle tail-gas range of temperature; Aspect the stationary source denitrating flue gas, be expected to catalyst as low form SCR, be applied to after the flue gas desulfurization, to improve the service life of catalyst;
(2) insensitive to reaction velocity, be applicable to the characteristic of motor vehicle tail-gas purifying high-speed, can reduce the use amount of catalyst when being applied to the stationary source denitrating flue gas significantly, reduce cost, conserve space;
(3) adopt nontoxic component, reduce risk human body and environmental hazard;
(4) has anti-preferably SO
2Poisoning capability.
The specific embodiment
The present invention enumerate following examples in order more clearly to illustrate, but it there is not any restriction to scope of the present invention.
[embodiment 1-4]
Be cerium salt and titanium salt with six nitric hydrate ceriums and titanium sulfate respectively, preparation Ce/Ti mol ratio is 0.1 solution and mixes, in this solution, add excessive urea liquid (mol ratio of urea and metallic element is 23: 1), and under 90 ℃ of temperature conditions continuous stirring 8h, carry out suction filtration and washing then, filter cake is put into baking oven spend the night, after Muffle furnace roasting 5h in 500 ℃ of air makes powder catalyst in 100 ℃ of oven dry.With the catalyst compressing tablet that makes, grind, sieve, it is standby to get 60～80 orders, is called catalyst A.Other condition is constant, and changing the Ce/Ti mol ratio is 0.2,0.5,1.0, makes catalyst B, C, D respectively.
[embodiment 5-7]
Be cerium salt and titanium salt with seven hydration cerous chlorates and titanium sulfate respectively, preparation Ce/Ti mol ratio is 0.2 solution and mixes, in this solution, add excessive urea liquid (mol ratio of urea and metallic element is 23: 1), and under 90 ℃ of temperature conditions continuous stirring 8h, carry out suction filtration and washing then, filter cake is put into baking oven spend the night, after Muffle furnace roasting 5h in 500 ℃ of air makes powder catalyst in 100 ℃ of oven dry.With the catalyst compressing tablet that makes, grind, sieve, it is standby to get 60～80 orders, is called catalyst E.Other condition is constant, and changing cerium salt is four cerium sulfate hydrates, ammonium ceric nitrate, makes catalyst F, G respectively.
[embodiment 8-9]
Be cerium salt and titanium salt with six nitric hydrate ceriums and titanium sulfate respectively, preparation Ce/Ti mol ratio is 0.2 solution and mixes, in this solution, add excessive urea liquid (mol ratio of urea and metallic element is 23: 1), and under 90 ℃ of temperature conditions continuous stirring 8h, carry out suction filtration and washing then, filter cake is put into baking oven spend the night, after Muffle furnace roasting 5h in 400 ℃ of air makes powder catalyst in 100 ℃ of oven dry.With the catalyst compressing tablet that makes, grind, sieve, it is standby to get 60～80 orders, is called catalyst H.Other condition is constant, and changing sintering temperature is 600 ℃, makes catalyst I.
[embodiment 10]
Cerium and titanium compound oxide catalyst with embodiment 1-9 makes carries out NH on homemade micro fixed-bed reactor
3The investigation of Selective Catalytic Reduction of NO reactivity.The use amount of catalyst is 0.6ml, the consisting of of reaction mixture gas: [NO]=[NH
3]=500ppm, [O
2]=5%, N
2Make balance gas, air speed is 50,000h
-1, 200～400 ℃ of reaction temperatures.NO and NH
3And accessory substance N
2O, NO
2All utilize the infrared-gas pond to measure.Reaction result is as shown in table 1.
[embodiment 11]
Use catalyst B, on homemade micro fixed-bed reactor, investigate the influence of reaction velocity catalyst activity.The use amount of catalyst is respectively 0.6ml, 0.3ml, 0.2ml, the consisting of of reaction mixture gas: [NO]=[NH
3]=500ppm, [O
2]=5%, N
2Make balance gas, corresponding air speed is respectively 50,000h
-1, 100,000h
-1, 150,000h
-1, 200～400 ℃ of reaction temperatures.NO and NH
3And accessory substance N
2O, NO
2All utilize the infrared-gas pond to measure.Reaction result is as shown in table 2.
[embodiment 12]
Use catalyst B, on homemade micro fixed-bed reactor, investigate SO
2Influence to catalyst activity.The use amount of catalyst is 0.6ml, the consisting of of reaction mixture gas: [NO]=[NH
3]=500ppm, [O
2]=5%, [SO
2]=100ppm, N
2Make balance gas, air speed is 50,000h
-1, reaction temperature is 300 ℃.NO and NH
3And accessory substance N
2O, NO
2All utilize the infrared-gas pond to measure.In the 24h that investigates, the NO conversion ratio is stable to remain between 98～100%, obvious reduction trend do not occur.As seen, this catalyst has anti-preferably SO
2Poisoning capability.
Table 1 catalyst activity evaluation result
Table 2 reaction velocity is to the influence of catalyst B activity
Claims (5)
1. nanocrystalline Ce titanium compound oxide catalyst that is used for ammine selectivity catalytic reduction nitrous oxides, it is characterized in that this catalyst is that cerium salt and titanium salt mixed solution obtain by Preparation by Uniform Precipitation, wherein the mol ratio of Ce elements and titanium elements is 0.1～1.0.
2. Preparation of catalysts method according to claim 1 is characterized in that used cerium salt is at least a in cerous chlorate or cerous nitrate or ammonium ceric nitrate or the cerous sulfate, and titanium salt is at least a in titanium tetrachloride or titanium sulfate or titanyl sulfate or the Titanium Nitrate.
3. Preparation of catalysts method according to claim 1, it is characterized in that with excessive urea as precipitating reagent, the mol ratio of urea and metallic element is 20: 1～30: 1, continuous stirring 6～10h under 90～95 ℃ of temperature conditions, carry out suction filtration and washing then, the gained filter cake is put into baking oven in 80～120 ℃ of oven dry, then through Muffle furnace roasting 4～6h in 400～500 ℃ of air.
4. catalyst according to claim 1 is characterized in that active phase CeO
xParticle grain size mainly is distributed in below the 40nm.
5. catalyst according to claim 1 is characterized in that being applied to stationary source denitrating flue gas and exhaust gas from diesel vehicle purification of nitrogen oxides.
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| CN102240541A (en) * | 2011-05-23 | 2011-11-16 | 济南大学 | Amorphous composite oxide denitration catalyst and preparation method and use thereof |
| CN102302930A (en) * | 2011-07-05 | 2012-01-04 | 中国科学院生态环境研究中心 | Transition metal doped cerium and titanium compound oxide catalyst for selective catalytic reduction of nitric oxide by ammonia |
| WO2012071971A1 (en) * | 2010-12-01 | 2012-06-07 | 中国科学院生态环境研究中心 | Ce-based composite oxide catalyst, preparation method and application thereof |
| CN103157491A (en) * | 2011-12-12 | 2013-06-19 | 中国科学院生态环境研究中心 | Mesoporous metal oxide-supported palladium catalyst used for catalytic oxidation of volatile organic compounds |
| CN103170326A (en) * | 2013-04-03 | 2013-06-26 | 中国科学院生态环境研究中心 | Vanadium-cerium oxide catalyst as well as preparation method and purpose thereof |
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| US9498770B2 (en) | 2010-12-01 | 2016-11-22 | Research Center For Eco-Environmental Sciences, Chinese Academy Of Sciences | Ce-based composite oxide catalyst, preparation method and application thereof |
| CN102240541B (en) * | 2011-05-23 | 2013-04-17 | 济南大学 | Amorphous composite oxide denitration catalyst and preparation method and use thereof |
| CN102240541A (en) * | 2011-05-23 | 2011-11-16 | 济南大学 | Amorphous composite oxide denitration catalyst and preparation method and use thereof |
| CN102302930B (en) * | 2011-07-05 | 2015-05-20 | 中国科学院生态环境研究中心 | Transition metal doped cerium and titanium compound oxide catalyst for selective catalytic reduction of nitric oxide by ammonia |
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| CN103846083A (en) * | 2014-03-24 | 2014-06-11 | 南京理工大学 | Tungsten titanium composite oxide supported cerium oxide catalyst, preparation method as well as application of catalyst |
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| CN105126819A (en) * | 2015-09-01 | 2015-12-09 | 中国石油大学(北京) | Composite oxide catalyst for eliminating NH3, NO and soot particles at same time and preparation method and purpose of composite oxide catalyst |
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| CN110465284A (en) * | 2018-05-10 | 2019-11-19 | 国家能源投资集团有限责任公司 | Rare earth based denitration catalyst and its preparation method and application |
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Application publication date: 20100728 |