CN105664917A - Layered structure cerium based oxide catalyst, preparation method and application thereof - Google Patents
Layered structure cerium based oxide catalyst, preparation method and application thereof Download PDFInfo
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B01D53/34—Chemical or biological purification of waste gases
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J23/28—Molybdenum
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- B01D2257/404—Nitrogen oxides other than dinitrogen oxide
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Abstract
The invention discloses a cerium based oxide catalyst for catalytic purification of nitrogen oxides and a preparation method thereof. The catalyst is a layered structure CeOx/MoO3-TiO2 catalyst formed by step-by-step uniform precipitation based on controllable adjustment of a pH value in the preparation process. According to the invention, non-toxic and harmless raw materials are employed to prepare the cerium based oxide catalyst with the characteristics of excellent catalytic activity, high N2 generation selectivity, wide operation temperature window and the like through a simple and practicable method. The catalyst is suitable for nitrogen oxide catalytic purification devices adopting a diesel vehicle exhaust represented mobile source and a coal-fired power plant flue gas represented stationary source.
Description
Technical field
The present invention relates to a kind of catalyst, preparation method and application thereof, particularly a kind of for the cerium base oxide catalyst of catalytic cleaning nitrogen oxide, preparation method and application thereof.
Background technology
Nitrogen oxides (NOx, refer mainly to NO and NO2) it is one of main atmosphere pollution, it is possible to cause the great environmental problem such as gray haze, photochemical fog and acid rain, also can produce health directly endanger. Therefore, NO is effectively controlledxDischarge be the significant challenge that field of environment protection faces.
Increasingly strict along with environmental regulation and standard, NH3Selective Catalytic Reduction of NOx(i.e. NH3-SCR) technology is considered as have most at present the NO of application prospectxThe technology purified. Catalyst is the core of SCR response system, and the performance (including activity, selectivity, stability) etc. of catalyst directly affects denitration efficiency. Although traditional V2O5-WO3/TiO2Catalyst is used as business SCR catalyst existing decades in stationary source denitrating flue gas field, but is still limited by restriction in actual applications because having the shortcomings such as bio-toxicity, poor high temperature stability, operation temperature window be narrower. Therefore, develop catalyst stable, efficient, environmentally friendly and become NH3-SCR develops the new challenge faced.
Non-vanadio transition metal (such as Fe, Cu, Mn and Ce) oxide catalyst is considered as the potential succedaneum of catalytic component based on vanadium, but such catalyst is with NOxRemove in the actual application for target and still suffer from many problems: though Mn base oxide catalyst has the low-temperature SCR activity of excellence, but water resistant resistance to SO_2 is poor; Cu is catalyst based to be existed operation temperature window is narrower and N2The problems such as selectivity is poor; Fe base oxide catalyst activity when low temperature and high-speed is poor. Although the resistance to SO_2 of Ce base oxide catalyst and high temperature stability performance need to be improved further, but wherein high temperature section SCR activity and N2Selectivity is higher, and has abundant rare earth resources attribute, and what therefore Ce was catalyst based modifiies at solution NH3The practical application of-SCR catalyst has stronger researching value.
NH in early days3In the research of-SCR catalyst, Ce is often used as NH3The auxiliary agent of-SCR catalyst or carrier, along with going deep into of research, it has been found that because it has the advantages such as the oxidation-reduction characteristic of excellence, oxygen storage capability and surface acidity, CeO2Can also serve as NH3The active component of-SCR catalyst.Due to simple CeO2Reduction temperature is higher and high temperature easy-sintering, and is not suitable for being used alone as NH3-SCR catalyst.
Summary of the invention
For existing NH3The deficiency that-SCR catalyst exists, and a large amount of of LREE Ce overstock, the present invention provides a kind of by CeO firstxEvenly spread to metal oxide catalyst that molybdenum (Mo) titanium (Ti) complex oxide surface formed and preparation method thereof, can be used as with exhaust gas from diesel vehicle be representative moving source and be representative with coal-fired plant flue gas stationary source NOxCatalytic purification.
In order to achieve the above object, present invention employs following technical scheme:
A kind of cerium base oxide catalyst, described catalyst is metal oxide catalyst CeOx/MoO3-TiO2, described catalyst is by CeOxEvenly spread to zirconium titanium composite oxides MoO3-TiO2Surface is formed.
Described CeOxFor Ce3+And Ce4+Mixed oxide, 3/2 < x < 2.
Above-mentioned catalyst adopts substep sluggish precipitation to prepare, and it comprises the steps:
(1) mixed solution in preparation cerium source, molybdenum source and titanium source, stirs under normal temperature condition;
(2) in solution, slow release precipitator is added;
(3) solution temperature is increased to 65～95 DEG C, and maintenance stirring precipitation 2～24h;
(4) precipitate in solution is easily separated and washs;
(5) undertaken drying and roasting by gained solid content, obtain described CeOx/MoO3-TiO2Catalyst.
In step (1), described cerium source at least one in cerous nitrate, ammonium ceric nitrate, cerous chlorate or cerous sulfate.
In step (1), described molybdenum source at least one in ammonium molybdate or molybdic acid.
In step (1), described titanium source at least one in titanium sulfate, titanium tetrachloride or butyl titanate.
In step (2), described slow release precipitator at least one in ammonium carbonate, ammonium hydrogen carbonate or carbamide.
In step (2), described slow release precipitator consumption is 8～20 times of the integral molar quantity in cerium source, molybdenum source and titanium source.
In step (3), described solution temperature preferably 80～90 DEG C.
In step (3), described stirring sedimentation time preferably 6～12h.
In step (5), described drying temperature is 80～120 DEG C, it is preferable that 90～110 DEG C.
In step (5), described roasting carries out in air atmosphere, and described sintering temperature is 400～800 DEG C, it is preferable that 500 DEG C; Described roasting time is 1～24h, it is preferable that 4～6h.
The application of above-mentioned cerium base oxide catalyst, is applied to nitrogen oxides in catalytic purification gas by described catalyst.
This catalyst can carry out slurrying according to actual needs, is then applied on various honeycomb ceramic carrier, and the catalyst preparing into molding uses, it is also possible to use after extruded.
Compared with prior art, present invention have the advantage that
(1) the operation temperature window width of described cerium base oxide catalyst, it is adaptable to the applied environment that motor-vehicle tail-gas range of temperature is big; In stationary source denitrating flue gas, can be used as the alternative catalysts of catalytic component based on vanadium;
(2) even if described cerium base oxide catalyst still can show the catalytic performance of excellence at high-speed environment, it is the very efficient SCR catalyst of one;
(3) described cerium base oxide catalyst has very excellent N2Generate selectivity;
(4) described cerium base oxide catalyst has extraordinary water resistant and thermal stability;
(5) preparation process of described cerium base oxide catalyst makes cerium oxide may be uniformly dispersed in molybdenum titanium composite oxide surface, so that it possesses the catalytic performance of above-mentioned excellence.
Detailed description of the invention
For the present invention is better described, it is simple to understand technical scheme, the typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1
It is 2:1 according to Ce:Mo mol ratio, preparation cerous nitrate and ammonium molybdate mixed solution, it is subsequently adding carbamide, controlling the pH value of mixed solution after all dissolving is 3.1, is then heated to 80～90 DEG C and continuous stirring 12h, pH are increased to 7.2, then it is filtered and washs, gained solid content is put in baking oven and dry 12h in 100～110 DEG C, prepare powder catalyst through Muffle furnace roasting 5h in 500 DEG C of air after, be called catalyst A.
Embodiment 2
According to cerium, molybdenum, titanium mol ratio be 2:1:10, titanium sulfate is dissolved in deionized water, being subsequently adding cerous nitrate and ammonium molybdate, and add carbamide as precipitant, controlling the pH value of mixed solution after all dissolving is 1.2, it is then heated to 80～90 DEG C and continuous stirring 12h, it is 7.3 that pH raises, and is then filtered and washs, and is put into by gained solid content in baking oven and dries 12h in 100～110 DEG C, prepare powder catalyst through Muffle furnace roasting 5h in 500 DEG C of air after, be called catalyst B.
Embodiment 3
Other condition such as embodiment 2 is constant, change cerium, molybdenum, titanium mol ratio be 2:1:2, obtain catalyst C.
Embodiment 4
Other condition such as embodiment 2 is constant, change cerium, molybdenum, titanium mol ratio be 2:1:4, obtain catalyst D.
Embodiment 5
Other condition such as embodiment 2 is constant, change cerium, molybdenum, titanium mol ratio be 2:1:20, obtain catalyst E.
Embodiment 6
Other condition such as embodiment 2 is constant, and the change continuous stirring time is 1h, pH rising is 1.6, obtains catalyst F.
Embodiment 7
Other condition such as embodiment 2 is constant, and the change continuous stirring time is 2h, pH rising is 4.9, obtains catalyst G.
Embodiment 8
Other condition such as embodiment 2 is constant, and the change continuous stirring time is 4h, pH rising is 6.3, obtains catalyst H.
Embodiment 9
Prepared catalyst B, F, G, H are carried out x-ray photoelectron power spectrum (XPS) test, obtains mole relative amount situation (table 1) of each sample surface cerium, molybdenum, titanium.
The different surface cerium of sample of table 1, molybdenum, titanium atom mole relative amount
| Sample | F | G | H | B |
| Ce (%) | 0 | 2.7 | 13.1 | 17.2 |
| Mo (%) | 14.8 | 14.0 | 11.8 | 11.6 |
| Ti (%) | 85.2 | 83.3 | 75.1 | 71.2 |
Table 1 can clearly be presented below as rule: along with the increase of mixing time, pH raises, and molybdenum titanium compound species are first begin to precipitation, and now deposited phenomenon does not occur cerium species, so the sample F surface cerium atom content obtained is 0; Along with mixing time extends, pH continues to raise, and cerium species, when pH rises to 4.9, start precipitation occur, so a small amount of cerium atom is contained on the sample G surface obtained, relative amount is 2.7%; Along with mixing time continues to extend, pH continues to raise, and cerium species continue precipitation, so the relative amount of the sample H surface cerium atom obtained increases to 13.1%; Along with mixing time continues to extend, pH continues to raise, and cerium species, when pH rises to 7.3, occur in that more precipitation, so the relative amount of the sample B surface cerium atom obtained increases to 17.2%, the relative amount of surface molybdenum atom and titanium atom is down to 11.6% and 71.2% respectively simultaneously. Therefore, the generation process that can obtain catalyst is by the adjustment to pH, molybdenum titanium species preferential precipitation goes out solution, then cerium species uniformly, high degree of dispersion be deposited in molybdenum titanium species surface, namely obtain cerium oxide after fired and be highly dispersed at molybdenum titanium composite oxide surface, there is the catalyst of hierarchy.
Application examples 1
Prepared sample A, B, C, D, E, F, G, H are carried out tabletting, grind, sieve, takes 40～60 order granules on fixed bed reactors, carry out NH3Selective Catalytic Reduction of NOx(NH3-SCR) investigation of reactivity.
The consumption that makes of catalyst is 0.12mL, consisting of of reaction mixture gas: [NO]=[NH3]=500ppm, [O2]=5%, N2Making Balance Air, total gas flow rate is 200mL/min, and air speed is 100,000h-1, reaction temperature 150～450 DEG C. NO and NH3And by-product N2O、NO2NicoletAntarisIGS infrared gas analyser is all utilized to measure.NOxConversion ratio and N2Generate selectivity respectively as shown in table 2 and table 3.
The NO of the different sample of table 2xConversion ratio
As shown in Table 2, catalyst A, B, C, D, E are gradually increased along with Ti content, its low-temperature zone NOxDownward trend after transformation efficiency appearance first rising, Ti:Mo mol ratio is the middle low temperature NO of the catalyst B of 10xConversion ratio is maximum, it was shown that cerium, molybdenum, titanium the catalyst B that mol ratio is 2:1:10 have excellence catalytic performance; Catalyst F, G, H, B are along with the increase of surface cerium content, and it is lower than the NO in 350 DEG C of temperature rangesxTransformation efficiency substantially increases, it was shown that cerium oxide is the main active component of this catalyst.
The N of the different sample of table 32Generate selectivity
It addition, the N of catalyst provided by the invention2It is all non-normally low that O generates concentration, therefore has very excellent N2Generate selectivity (table 3).
Application examples 2
Prepared sample B is carried out tabletting, grind, sieves, takes 40～60 order granules on fixed bed reactors, investigate addition 5%H in reaction atmosphere2The O impact on catalyst activity.
Consisting of of reaction mixture gas: [NO]=[NH3]=500ppm, [O2]=5%, [H2O]=5%, N2Making Balance Air, total gas flow rate is 200mL/min, and air speed is 100,000h-1, reaction temperature 150～450 DEG C. NO and NH3And by-product N2O、NO2NicoletAntarisIGS infrared gas analyser is all utilized to measure. NOxConversion ratio is as shown in table 4.
Containing 5%H in table 4 reaction atmosphere2The NO of catalyst sample B during OxConversion ratio
As shown in Table 4, H in reaction atmosphere2The addition of O, it is possible to significantly reduce the low temperature NO of catalyst B provided by the inventionxConversion ratio, but high temperature NO can be promoted to a certain extentxConversion ratio. Even if containing 5%H in reaction atmosphere2During O, catalyst B still can realize the NO of more than 80% in 250～450 DEG C of temperature rangesxConversion ratio.
Application examples 3
Prepared sample B is carried out tabletting, grind, sieves, takes 4060 order granules on fixed bed reactors, investigate the reaction velocity impact on catalyst activity.
Consisting of of reaction mixture gas: [NO]=[NH3]=500ppm, [O2]=5%, N2Making Balance Air, total gas flow rate is 200mL/min, reaction temperature 150～450 DEG C. The consumption that makes of catalyst is 0.24mL, and corresponding reaction velocity is 50,000h-1. NO and NH3And by-product N2O、NO2NicoletAntarisIGS infrared gas analyser is all utilized to measure. NOxConversion ratio is as shown in table 5.
Table 5 reaction velocity is 50,000h-1Time catalyst sample B NOxConversion ratio
The NO of catalyst sample B in contrast table 5 and table 2xConversion ratio, it is possible to find that reducing reaction velocity can improve the catalysis activity of catalyst.
Time actually used, catalyst is placed in exhaust pipe way, reducing agent and tail gas mixing is sprayed in the upstream of catalyst, reducing agent adopts ammonia or carbamide (can obtain ammonia after hydrolysis), reducing agent consumption is 0.8～1.2 times of nitrogen oxide in tail gas, can by NO in very wide temperature window under excess oxygenxIt is reduced to N2And H2O, is provided simultaneously with significantly high N2Generate selectivity and sulfur resistive water repelling property.
Described tail gas is preferably moving source gas containing nitrogen oxide, for instance exhaust gas from diesel vehicle, or stationary source gas containing nitrogen oxide, for instance coal-fired plant flue gas. Described gas is preferably exhaust gas from diesel vehicle, namely the present invention is especially suitable for the catalytic purification of nitrogen oxides in exhaust gas from diesel vehicle.
Applicant states, the present invention illustrates composition and the method in detail of the present invention by above-described embodiment, but the invention is not limited in above-mentioned detailed composing method, does not namely mean that the present invention has to rely on above-mentioned detailed composition and method could be implemented.The equivalence of each raw material of product of the present invention, it will be clearly understood that any improvement in the present invention, is replaced and the interpolation of auxiliary element, concrete way choice etc. by person of ordinary skill in the field, all falls within protection scope of the present invention and open scope.
Claims (9)
1. a cerium base oxide catalyst, it is characterised in that described catalyst is metal-oxide CeO x /MoO3-TiO2, described catalyst is by CeO x Evenly spread to zirconium titanium composite oxides MoO3-TiO2Surface is formed.
2. catalyst as claimed in claim 1, it is characterised in that described CeO x For Ce3+And Ce4+Mixed oxide, 3/2 < x < 2.
3. the preparation method of catalyst as claimed in claim 1 or 2, it is characterised in that it comprises the steps:
(1) mixed solution in preparation cerium source, molybdenum source and titanium source, stirs under normal temperature condition;
(2) in solution, slow release precipitator is added;
(3) solution temperature is increased to 65 ~ 95oC, and maintenance stirring precipitation 2 ~ 24h;
(4) precipitate in solution is easily separated and washs;
(5) undertaken drying and roasting by gained solid content, obtain described CeO x /MoO3-TiO2Catalyst.
4. preparation method as claimed in claim 3, it is characterised in that in step (1), described cerium source at least one in cerous nitrate, ammonium ceric nitrate, cerous chlorate or cerous sulfate; Described molybdenum source at least one in ammonium molybdate or molybdic acid; Described titanium source at least one in titanium sulfate, titanium tetrachloride or butyl titanate.
5. preparation method as claimed in claim 3, it is characterised in that in step (2), described slow release precipitator at least one in ammonium carbonate, ammonium hydrogen carbonate or carbamide; Described slow release precipitator consumption is 8～20 times of the integral molar quantity in cerium source, molybdenum source and titanium source.
6. preparation method as claimed in claim 3, it is characterised in that in step (3), described solution temperature is 80 ~ 90oC; , the described stirring sedimentation time is 6 ~ 12h.
7. preparation method as claimed in claim 3, it is characterised in that in step (5), described drying temperature is 80～120oC。
8. preparation method as claimed in claim 3, it is characterised in that in step (5), described roasting carries out in air atmosphere, and described sintering temperature is 400～800oC; Described roasting time is 1～24h.
9. cerium base oxide catalyst application in nitrogen oxides in catalytic purification gas as claimed in claim 1.
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| CN107913695A (en) * | 2016-10-10 | 2018-04-17 | 中国石油天然气股份有限公司 | A kind of denitrating catalyst of preventing from heavy metal deposition and preparation method thereof |
| CN107913697A (en) * | 2016-10-10 | 2018-04-17 | 中国石油天然气股份有限公司 | A kind of wide temperature window denitrating catalyst and preparation method thereof |
| CN107913696A (en) * | 2016-10-10 | 2018-04-17 | 中国石油天然气股份有限公司 | A kind of denitrating catalyst of anti-oxidizing sulfur dioxide and preparation method thereof |
| CN109529812A (en) * | 2018-12-05 | 2019-03-29 | 北京工业大学 | A kind of SCR catalyst and preparation method suitable for high temperature high-humidity gas fume condition |
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| US20130202513A1 (en) * | 2010-12-01 | 2013-08-08 | Research Center For Eco-Environmental Sciences Chinese Academy of Sciences | Ce-BASED COMPOSITE OXIDE CATALYST, PREPARATION METHOD AND APPLICATION THEREOF |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107913695A (en) * | 2016-10-10 | 2018-04-17 | 中国石油天然气股份有限公司 | A kind of denitrating catalyst of preventing from heavy metal deposition and preparation method thereof |
| CN107913697A (en) * | 2016-10-10 | 2018-04-17 | 中国石油天然气股份有限公司 | A kind of wide temperature window denitrating catalyst and preparation method thereof |
| CN107913696A (en) * | 2016-10-10 | 2018-04-17 | 中国石油天然气股份有限公司 | A kind of denitrating catalyst of anti-oxidizing sulfur dioxide and preparation method thereof |
| CN107913696B (en) * | 2016-10-10 | 2020-01-03 | 中国石油天然气股份有限公司 | Denitration catalyst capable of resisting sulfur dioxide oxidation and preparation method thereof |
| CN107913695B (en) * | 2016-10-10 | 2020-01-03 | 中国石油天然气股份有限公司 | Heavy metal deposition-resistant denitration catalyst and preparation method thereof |
| CN107913697B (en) * | 2016-10-10 | 2020-01-07 | 中国石油天然气股份有限公司 | Denitration catalyst with wide temperature window and preparation method thereof |
| CN109529812A (en) * | 2018-12-05 | 2019-03-29 | 北京工业大学 | A kind of SCR catalyst and preparation method suitable for high temperature high-humidity gas fume condition |
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