CN105664912A - Cerium-tin-zirconium composite oxide catalyst, and preparation method and use thereof - Google Patents

Cerium-tin-zirconium composite oxide catalyst, and preparation method and use thereof Download PDF

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CN105664912A
CN105664912A CN201511025305.9A CN201511025305A CN105664912A CN 105664912 A CN105664912 A CN 105664912A CN 201511025305 A CN201511025305 A CN 201511025305A CN 105664912 A CN105664912 A CN 105664912A
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zirconium
cerium
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catalyst
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贺泓
丁世鹏
刘福东
石晓燕
连志华
牛璨
谢利娟
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Research Center for Eco Environmental Sciences of CAS
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01D53/90—Injecting reactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/206—Rare earth metals
    • B01D2255/2065—Cerium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20715—Zirconium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/209—Other metals
    • B01D2255/2094—Tin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/40—Nitrogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/40—Nitrogen compounds
    • B01D2257/404—Nitrogen oxides other than dinitrogen oxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts

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Abstract

The invention relates to a cerium-tin-zirconium composite oxide catalyst, and a preparation method and a use thereof. The chemical composition of the catalyst is CeSnaZr2Ox, and a is 0 (exclusive) to 2.0. The addition of Sn promotes mutual synergism among Sn, Ce and Zr, changes the adsorption performance of reactants to the catalyst and makes the redox process of the catalyst be easily completed, so the NOx removal efficiency is improved. The CeSnaZr2Ox catalyst has the advantages of substantially improved activity, obvious widening of the temperature window, and excellent NH3-SCR activity at a temperature range of 200-450DEG C.

Description

A kind of cerium stannum zirconium mixed oxide catalyst, preparation method and its usage
Technical field
The present invention relates to a kind of catalyst, be specifically related to a kind of for the cerium stannum zirconium mixed oxide catalyst of catalytic cleaning nitrogen oxide, preparation method and its usage.
Background technology
NH3-SCR technology, namely with NH3For reducing agent Selective Catalytic Reduction of NO, it is widely used in moving source or stationary source tail-gas the removal of NO. Business-like SCR catalyst is V at present2O5-WO3(MoO3)/TiO2, but this system yet suffers from problems with, for instance low temperature active is poor, and heat stability is low, active component V during high temperature2O5Readily volatilized and there is bio-toxicity etc. Therefore developing practicality and high efficiency, environment-friendly catalyst is for removing diesel vehicle or the NO of coal-burning power plant's dischargexProtection China atmospheric environment is had very important significance. Study more SCR catalyst at present and mainly have molecular sieve (ZSM-5, HBEA, SSZ-34 and SAPO-34), oxide (Ce, Fe, Cu) and material with carbon element.
CeO2Start from the eighties in 20th century as catalyst for tail-gas from gasoline automobiles, can occur when lean fuel-rich operating mode alternate runRedox reaction, i.e. CeO under fuel-rich operating mode2Discharge oxygen, under lean combustion operating mode, absorb and store oxygen. In recent years, containing CeO2Catalyst is as NH3The auxiliary agent of-SCR catalyst or carrier cause people to pay close attention to greatly. Research finds to CeO2The cerium Zirconium oxide stability that doping Zr is formed is apparently higher than CeO2, there is certain NH simultaneously3-SCR activity. But the temperature window of this oxide is narrower, and low temperature active is poor, in order to by NO in its practical application exhaust gas from diesel vehiclexEfficient removal, it is necessary to carry out further optimizing and modified to it.
CN103240079A discloses a kind of for the cerium zirconium tungsten composite oxide catalysts of ammine selectivity catalytic reduction nitrous oxides, preparation method and its usage. Described catalyst is the composite oxide of metal of cerium, zirconium and three kinds of metal compositions of tungsten. This invention adopts nontoxic raw material, is prepared by simple method and adapts to high-speed reaction condition, and has catalysis superior activity, N2Generate the cerium zirconium tungsten composite oxide catalysts of the features such as high, the operation temperature window width of selectivity, it is adaptable to exhaust gas from diesel vehicle be representative moving source and be representative with coal-fired plant flue gas stationary source catalytic purification of nitroxide device.
CN101522298A discloses the catalyst that a kind of thermostability is good, can effectively purify nitrogen oxides. In the invention, the content of cerium oxide is the content of 10～30 weight % and tungsten oxide is 5～14 weight %. The thermostability of the metal composite oxide of tungstenic, zirconium and cerium is good, can effectively purify nitrogen oxides in the presence of ammonia. Therefore, the content containing metal composite oxide containing tungsten oxide, zirconium oxide and cerium oxide and described cerium oxide be 10～30 weight %, described tungsten oxide the catalyst that content is 5～14 weight % can be used for the purification of nitrogen oxides.
WO in above-mentioned cerium tungsten Zr catalyst3Price higher, be unfavorable for reduce commercial production cost.
Summary of the invention
For the problem of prior art, an object of the present invention is in that with cheap SnO2Replace expensive WO3, the cerium stannum Zr catalyst with greater activity is obtained with relatively low cost.
A kind of cerium stannum zirconium mixed oxide catalyst, it has following chemical composition: CeSnaZr2Ox, a is 0～2.0 and does not include 0.
In above-mentioned catalyst, the numerical value of x can be 0 obtain according to quantivalence sum.
In above-mentioned catalyst, the mol ratio of Ce and Zr is 1:2, the mol ratio of Sn and Ce is a, for instance 0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9,1.0,1.1,1.2,1.3,1.4,1.5,1.6,1.7,1.8,1.9 or 2.0, it is preferable that 2.0.
The present invention is to CeZrOxMiddle interpolation acidic oxide SnO2, remove NO to improving catalystxReactivity. The present invention utilizes the synergism between the oxide of cerium stannum zirconium, and have selected the mol ratio of suitable Ce and Zr and the mol ratio of Sn and Ce to catalyst there is the catalytic reaction activity of excellence, and temperature window wide ranges.
In described cerium zirconium stannum composite oxide catalysts, described composite oxide catalysts includes cerium (Ce), zirconium (Zr) and three kinds of metal components of stannum (Sn), described Ce, Zr and Sn oxide in composite oxide catalysts, form solid solution.
Described catalyst is composite oxide catalysts, and it need not can reach corresponding dispersion and catalytic effect by carrier.
The two of the purpose of the present invention are in that the preparation method providing a kind of cerium stannum zirconium mixed oxide catalyst as above, and described method is sluggish precipitation, comprises the following steps:
Cerium source and zirconium source are dissolved completely in water, are then slow added into Xi Yuan and excessive precipitant, so that cerium, zirconium and stannum precipitation are completely, separate and wash the precipitated product obtained to neutral, then dry, roasting, obtain cerium stannum zirconium mixed oxide catalyst.
The present invention is by first by soluble in water to cerium source and zirconium source, then adding Xi Yuan and precipitant, so that cerium, zirconium and stannum precipitation are completely. The method is adopted to make the cerium stannum zirconium mixed oxide catalyst obtained have the catalysis activity of excellence.
Preferably, described cerium source is the mixture of any one or at least two in cerous chlorate, cerous nitrate, ammonium ceric nitrate or cerous sulfate, the mixture of described mixture such as cerous chlorate and cerous nitrate, the mixture of ammonium ceric nitrate and cerous sulfate, the mixture of cerous chlorate, cerous nitrate and ammonium ceric nitrate, the mixture of cerous sulfate, cerous chlorate, cerous nitrate and ammonium ceric nitrate, it is preferable that cerous nitrate.
Preferably, described zirconium source is the mixture of any one or at least two in protochloride zirconium, zirconium nitrate or Disulfatozirconic acid., the mixture of described mixture such as protochloride zirconium and zirconium nitrate, the mixture of protochloride zirconium and Disulfatozirconic acid., the mixture of zirconium nitrate and Disulfatozirconic acid., the mixture of protochloride zirconium, zirconium nitrate and Disulfatozirconic acid., it is preferable that zirconium nitrate.
Preferably, described Xi Yuan is SnCl4、Sn(NO3)4Or SnSO4In the mixture of any one or at least two.
Preferably, described precipitant is carbamide.
In sluggish precipitation, making precipitant with carbamide, precipitation cerium source, zirconium source or Xi Yuan, due to the problem that carbamide there may exist not exclusively hydrolysis, it is therefore desirable to add excess urea. Carbamide is hydrolyzed, it it is the process of a slow releasing hydroxide ion and carbanion, the slowly hydrolysis of carbamide makes the reactant concentration around cerium ion in solution, zirconium ion or tin ion that too big change will not occur, relative to other precipitant such as ammonia and ammonium hydrogen carbonate etc., it is more beneficial for oxide precursor granule and precipitates equably.
Preferably, carbamide/(cerium+stannum+zirconium) mol ratio is 8～12, it is preferable that 10.
Preferably, described precipitation carries out under agitation, and described mixing time is 0.5～48h, such as 5h, 6h, 7h, 8h, 9h, 10h, 11h, 12h, 13h, 14h, 18h, 22h, 26h, 32h, 38h, 42h, 45h, preferably 1～24h, it is preferred that 4～15h, it is most preferred that 12h.
Preferably, the temperature of described precipitation is 60～100 DEG C, for instance 65 DEG C, 72 DEG C, 75 DEG C, 78 DEG C, 83 DEG C, 88 DEG C, 92 DEG C, 95 DEG C, 98 DEG C, it is preferable that 70～98 DEG C, it is preferred that 80～95 DEG C, it is most preferred that 90 DEG C.
Preferably, described washing adopts deionized water wash.
Preferably, the temperature of described drying is 80～120 DEG C, it is preferable that 100 DEG C.
Preferably, drying time is 1～36h, it is preferable that 2～24h, it is preferred that 4～12h, it is most preferred that 12h.
The temperature of described drying is such as 84 DEG C, 88 DEG C, 92 DEG C, 96 DEG C, 100 DEG C, 104 DEG C, 108 DEG C, 112 DEG C, 116 DEG C. The time of described drying is such as 2h, 4h, 8h, 12h, 16h, 20h, 24h, 28h, 30h, 34h.
Preferably, described roasting carries out in air atmosphere, and described sintering temperature is 400～800 DEG C, for instance 420 DEG C, 440 DEG C, 480 DEG C, 520 DEG C, 560 DEG C, 600 DEG C, 640 DEG C, 680 DEG C, 720 DEG C, 760 DEG C, 780 DEG C, preferably 400～600 DEG C, it is preferred that 500 DEG C.
Preferably, described roasting time is 1～24h, for instance 2h, 4h, 6h, 8h, 10h, 12h, 14h, 16h, 18h, 20h, 22h, it is preferable that 2～12h, it is preferred that 3h.
Described sluggish precipitation, its reaction pressure is not particularly limited, but generally adopts synthesis under normal pressure.
The preparation method of exemplary cerium stannum zirconium mixed oxide catalyst, comprises the following steps:
First cerous nitrate and zirconium nitrate are dissolved completely in deionized water, are then slow added into SnCl4And carbamide, wherein the mol ratio of carbamide and total metal ion is 10:1, and it is 250ml that the most backward solution mixed above adds deionized water to cumulative volume, and under 90 DEG C of water bath condition continuous stirring 12h. After above-mentioned mixed liquor is cooled to room temperature, with deionized water, gained precipitate is carried out abundant sucking filtration and washing to neutral, then put the precipitate in 100 DEG C of oven for drying overnight, finally at 500 DEG C of roasting 3h.
The three of the purpose of the present invention are in that to provide the purposes of a kind of cerium stannum zirconium mixed oxide catalyst as above, and it is used for catalytic oxidation of nitric oxide.
Compared with the prior art, there is advantages that
The interpolation of Sn has promoted the mutual synergism between Sn, Ce, Zr, changes the catalyst absorption property to reactant, makes catalyst redox process be more prone to, thus improve NO simultaneouslyxRemoval efficiency. Described CeSnaZr2OxCatalyst activity significantly improves, and temperature window is also substantially widened simultaneously, and described cerium stannum zirconium mixed oxide catalyst has the NH of excellence in 200 DEG C～450 DEG C temperature ranges3-SCR activity.
Additionally, described catalyst adopts urea homogeneous precipitation method to prepare, preparation process is simple, with low cost, it is easy to realize industrialization.
Detailed description of the invention
Technical scheme is further illustrated below by detailed description of the invention.
Embodiment 1
First cerous nitrate and zirconium nitrate are dissolved completely in deionized water, are then slow added into quantitative SnCl4And carbamide, wherein the mol ratio of carbamide and total metal ion is 10:1, and it is 250ml that the most backward solution mixed above adds deionized water to cumulative volume, and under 90 DEG C of water bath condition continuous stirring 12h. After above-mentioned mixed liquor is cooled to room temperature, with deionized water, gained precipitate is carried out abundant sucking filtration and washing to neutral, then put the precipitate in 100 DEG C of oven for drying overnight, finally at 500 DEG C of roasting 3h, obtaining cerium stannum zirconium mixed oxide catalyst, it has following chemical composition: CeSnaZr2Ox, a is 0.5.
Embodiment 2
Other conditions, with embodiment 1, consist of except adding control catalyst by raw material: CeSnaZr2Ox, a is 1.0.
Embodiment 3
Other conditions, with embodiment 1, consist of except adding control catalyst by raw material: CeSnaZr2Ox, a is 1.5.
Embodiment 4
Other conditions, with embodiment 1, consist of except adding control catalyst by raw material: CeSnaZr2Ox, a is 2.0.
Embodiment 5
All the other are identical with embodiment 2, except cerium source be cerous nitrate by, zirconium source is zirconium nitrate, and precipitation temperature is 80 DEG C, and mixing time is 48h, and drying temperature is 80 DEG C, and drying time is 36h, and sintering temperature is 400 DEG C, and roasting time is outside 24h.
Comparative example 1
All the other are with embodiment 1, and except being added without Xi Yuan, the catalyst obtained has following composition: Ce1Zr2Ox。
Comparative example 2
All the other are with embodiment 1, and except being added without zirconium source, the catalyst obtained has following composition: Ce1Sn2Ox。
Comparative example 3
All the other same embodiments, except by controlling raw material addition, controlling Ce and Zr mol ratio is 1.
The catalyst obtained is carried out performance test, specific as follows:
Test condition simulated flue gas consists of, and the concentration of each component is NH3=500ppm, NO=500ppm, O2=5%, N2For Balance Air, total flow=500mL/min, reaction velocity is 50,000h-1, reaction temperature 150～300 DEG C. NO and NH3And by-product N2O, NO2Infrared-gas pond is all utilized to measure. Test result is as shown in the table:
Prepared best CeSn2Zr2OxCatalyst (embodiment 4) is 50,000h in air speed-1, temperature when 150 DEG C to 300 DEG C, NOxPurification efficiency is above Ce1Zr2Ox(comparative example 1), Ce1Sn2Ox(comparative example 2) and CeSnZr2Ox(comparative example 3).
Comparative example 4
Adopt above-mentioned catalyst performance evaluation method that catalyst B disclosed in embodiment 2 optimum disclosed in CN103240079A is carried out performance test.
Comparative example 5
Adopt above-mentioned catalyst performance evaluation method that catalyst 9 disclosed in CN101522298A is carried out performance test.
Comparative example 6
Adopt above-mentioned catalyst performance evaluation method that the catalyst of CN102671654A disclosed embodiment 5 is carried out performance test.
Comparative example 7
Adopt above-mentioned catalyst performance evaluation method that the catalyst of CN103736479A disclosed embodiment 5 is carried out performance test.
Applicant states, the present invention illustrates the method detailed of the present invention by above-described embodiment, but the invention is not limited in above-mentioned method detailed, does not namely mean that the present invention has to rely on above-mentioned method detailed and could implement. 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 (10)

1. a cerium stannum zirconium mixed oxide catalyst, it has following chemical composition: CeSnaZr2Ox, a is 0～2.0 and does not include 0.
2. a preparation method for cerium stannum zirconium mixed oxide catalyst as claimed in claim 1, described method is sluggish precipitation, comprises the following steps:
Cerium source and zirconium source are dissolved completely in water, are then slow added into Xi Yuan and excessive precipitant, so that cerium, zirconium and stannum precipitation are completely, separate and wash the precipitated product obtained to neutral, then dry, roasting, obtain cerium stannum zirconium mixed oxide catalyst.
3. method as claimed in claim 2, it is characterised in that described cerium source is the mixture of any one or at least two in cerous chlorate, cerous nitrate, ammonium ceric nitrate or cerous sulfate, it is preferable that cerous nitrate;
Preferably, described zirconium source is the mixture of any one or at least two in protochloride zirconium, zirconium nitrate or Disulfatozirconic acid., it is preferable that zirconium nitrate.
4. method as claimed in claim 2 or claim 3, it is characterised in that described Xi Yuan is SnCl4、Sn(NO3)2Or SnSO4In the mixture of any one or at least two;
Preferably, described precipitant is carbamide.
5. the method as described in one of claim 2-4, it is characterised in that carbamide/(cerium+stannum+zirconium) mol ratio is 8～12, it is preferable that 10.
6. the method as described in one of claim 2-5, it is characterised in that described precipitation carries out under agitation, described mixing time is 0.5～48h, it is preferable that 1～24h, it is preferred that 4～15h, it is most preferred that 12h;
Preferably, the temperature of described precipitation is 60～100 DEG C, it is preferable that 70～98 DEG C, it is preferred that 80～95 DEG C, it is most preferred that 90 DEG C;
Preferably, described washing adopts deionized water wash.
7. the method as described in one of claim 2-6, it is characterised in that the temperature of described drying is 80～120 DEG C, it is preferable that 100 DEG C.
8. the method as described in one of claim 2-7, it is characterised in that drying time is 1～36h, it is preferable that 2～24h, it is preferred that 4～12h, it is most preferred that 12h.
9. the method as described in one of claim 2-8, it is characterised in that described roasting carries out in air atmosphere, described sintering temperature is 400～800 DEG C, it is preferable that 400～600 DEG C, it is preferred that 500 DEG C;
Preferably, described roasting time is 1～24h, it is preferable that 2～12h, it is preferred that 3h.
10. a purposes for cerium stannum zirconium mixed oxide catalyst as claimed in claim 1, it is used for catalytic oxidation of nitric oxide.
CN201511025305.9A 2015-12-31 2015-12-31 Cerium-tin-zirconium composite oxide catalyst, and preparation method and use thereof Pending CN105664912A (en)

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CN107649116A (en) * 2017-11-02 2018-02-02 北京化工大学 Cerium tin composite oxides denitrating catalyst and its preparation method and application
CN110947377A (en) * 2019-12-31 2020-04-03 中国科学院生态环境研究中心 Cerium-tin-based composite oxide catalyst for catalytic purification of nitrogen oxides, preparation method and application thereof
CN117899848A (en) * 2023-12-28 2024-04-19 江门市科恒实业股份有限公司 Oxygen storage material and preparation method thereof

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CN104368329A (en) * 2014-09-19 2015-02-25 中国科学院生态环境研究中心 Cerium-niobium-zirconium composite oxide catalyst, preparation method and uses thereof
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CN107649116A (en) * 2017-11-02 2018-02-02 北京化工大学 Cerium tin composite oxides denitrating catalyst and its preparation method and application
CN110947377A (en) * 2019-12-31 2020-04-03 中国科学院生态环境研究中心 Cerium-tin-based composite oxide catalyst for catalytic purification of nitrogen oxides, preparation method and application thereof
CN110947377B (en) * 2019-12-31 2021-06-11 中国科学院生态环境研究中心 Cerium-tin-based composite oxide catalyst for catalytic purification of nitrogen oxides, preparation method and application thereof
WO2021134957A1 (en) * 2019-12-31 2021-07-08 中国科学院生态环境研究中心 Cerium-tin-based composite oxide catalyst for catalyzing purification of nitrogen oxide, preparation method and application thereof
CN117899848A (en) * 2023-12-28 2024-04-19 江门市科恒实业股份有限公司 Oxygen storage material and preparation method thereof
CN117899848B (en) * 2023-12-28 2024-08-23 江门市科恒实业股份有限公司 Oxygen storage material and preparation method thereof

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