CN107715858A - A kind of preparation method of high temperature resistant to sulfur Ce base SCR catalysts - Google Patents

A kind of preparation method of high temperature resistant to sulfur Ce base SCR catalysts Download PDF

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Publication number
CN107715858A
CN107715858A CN201710946222.6A CN201710946222A CN107715858A CN 107715858 A CN107715858 A CN 107715858A CN 201710946222 A CN201710946222 A CN 201710946222A CN 107715858 A CN107715858 A CN 107715858A
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catalyst
preparation
sulfur
scr
high energy
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何洪
朱红太
尹孟奇
宋丽云
邱文革
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BEIJING FANGXINLIHUA TECHNOLOGY Co Ltd
Beijing University of Technology
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BEIJING FANGXINLIHUA TECHNOLOGY Co Ltd
Beijing University of Technology
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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
    • B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
    • 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
    • B01D2251/00—Reactants
    • B01D2251/20—Reductants
    • B01D2251/206—Ammonium compounds
    • B01D2251/2062—Ammonia
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0283—Flue gases

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biomedical Technology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Catalysts (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)

Abstract

A kind of preparation method of high temperature resistant to sulfur Ce base SCR catalysts, belongs to catalyst preparation technical field.It is characterised in that it includes following steps：(1) quantitative Ce presomas and TiO are weighed respectively2Carrier, which is put into ball grinder, carries out high energy milling 0.1~6h, CeO2Content is 1~45wt%；(2) powder after high energy milling is placed in Muffle furnace, atmosphere is air, and temperature is 250~500 DEG C of 2~6h of roasting, you can obtains Ce base SCR denitrations.The present invention has the features such as raw material is cheap and easy to get, and preparation condition is easily controlled, and preparation process is green, and gained catalyst has higher NH3SCR reactivities and preferable sulfur resistive water repelling property.

Description

A kind of preparation method of high temperature resistant to sulfur Ce base SCR catalysts
Technical field
The present invention relates to a kind of preparation method of high temperature resistant to sulfur Ce base SCR catalysts and its in ammine selectivity catalytic reduction Application in reaction of nitrogen oxides, belong to the preparing technical field of SCR catalyst.
Background technology
In recent years, China's most area haze pollution takes place frequently, nitrogen oxides (NOx) it is cause atmosphere pollution main One of pollution sources.The current NO in ChinaxDischarge from the many-side such as automobile, boiler combustion, industrial production.The statistical number of 2016 According to showing, power plant turns into NOxThe largest source of pollution of discharge, account for the 39.6% of total emission volumn.Therefore, power-plant flue gas denitration skill The research of art causes the extensive concern of people.SCR gas denitrifying technologies are most widely used in power-plant flue gas denitration, mesh Before, most thermal power plant has all been mounted with SCR denitration device, and the core of the device is SCR catalyst, and it, which is mainly formed, is V2O5-WO3/TiO2Or V2O5-MoO3/TiO2.The type catalyst has higher SCR reactivities, for the NO in the whole worldxDischarge Control is made that huge contribution.But it there is also two defects：First, V2O5It is spent catalyst with larger toxicity Processing bring difficulty；2nd, running temperature window is about 300~400 DEG C, and temperature window is narrower.
Ce(4f15d16s2) element electron orbit it is more special, an electronics is only existed on 5d tracks, Ce elements are special Electronic configuration be advantageous to the transfer of electronics.CeO2Can according in external environment oxygen content number, in good time occur oxidation also Former reaction cycle, in Ce2O3And CeO2Between mutually change, form protoxide CeO2-xStable cubic fluorite structure is still kept, Therefore, CeO2Easily occurs Lacking oxygen defect in lattice, these Lacking oxygen defects are to CeO2Physicochemical property have significant shadow Ring.Ce bases SCR catalyst is without vanadium catalyst, will not cause secondary pollution to environment.It is resistance to that catalyst shows preferable sulfur resistive Water-based energy, stable, catalyst life is reliable so that gas cleaning flow is more reasonable, while energy consumption reduces, operating cost And one-time investment is greatly lowered.Therefore, Ce bases SCR catalyst receives much attention.Xu etc. prepares Ce/TiO using infusion process2 Catalyst, when the load capacity of Ce in sample is 5wt%, SCR reaction velocities are 5 × 104h-1When, in 275~400 DEG C of temperature ranges Interior, NO conversion ratios reach 90% (Xu W Q, et al, Catal Commun.2008,9,1453-1457).Wu etc. have studied with The different TiO of pattern2For carrier when, active component CeO2Form, the physico-chemical property and NH of catalyst3The change of-SCR activity Deng.With CeO2The increase of load capacity, CeOxSpecies are presented by unformed phase to little crystal grain CeO2, then to big crystal grain CeO2 Variation tendency, in unformed shape and the CeO of little crystal grain2In, Ce3+Ion concentration is higher, substantial amounts of surface defect and oxygen be present Room, show excellent redox performances (Wang H Q, et al, Catal Lett.2013,143,1312-1318). The researchs such as Cheng find CeO2It is scattered in bar-shaped Rutile Type TiO2On also show good SCR activity, 275~425 In DEG C temperature range, (air speed is 5 × 10 to NO high conversion rates in 90%4h-1)(Cheng K,et al,Catal Sci Technol.2016,6,4478-4490).Guo etc. result of study shows CeO2/TiO2Catalyst activity reduces and carrier TiO2 Particle diameter increase, specific surface area declines, factor relevant (Guo R T, the et al, Catal such as chemical absorption of surface oxygen species are reduced Commun.2015,59,136-139).Wang etc. has inquired into Alkali-Metal Na, K plasmas cause CeO2/TiO2Catalyst activity drops The reason for low, research show that the presence of alkali metal can reduce the surface acidity of catalyst, promote CeO2Component is turned by unformed shape Crystalline state is turned to, causes the reduction of redox performances, reduces catalyst to NH3The absorption of molecule, it is suppressed that the shape of reactive intermediate Into causing the reduction of catalyst SCR activity.When alkali metal ion concentration reaches a certain amount of, such as Na/Ti>When 0.25, catalyst loses (Wang H Q, et al, Catal Sci Technol.2013,3,715-722) living.Such as patent (application publication number： CN201610117933.8 a kind of preparation method of doping type cerium titanium catalyst) is disclosed, in the doping type cerium titanium catalyst The doping of cerium species enters titanium dioxide intracell, generates more Ce- -Ti type Lacking oxygens, improves catalyst by NO The efficiency of reaction intermediate nitro class species is oxidized to, so as to improve the denitration efficiency of cerium titanium catalyst.Such as patent (Shen Please publication No.：CN102240541A) disclose a kind of preparation of cerium and titanium compound oxide catalyst for denitrating flue gas and make With method, this catalyst is in 25000h-1Under air speed, its denitration efficiency is up to 99.2% at 225 DEG C.But most research The sulfur resistance of Ce base catalysis materials is not directed to, such material whether is can be used for the denitration of industrial smoke and is under suspicion.
The present invention relates to a kind of method that simple two step prepares Ce base SCR catalysts, the Ce bases SCR prepared using the method Catalyst has good sulfur resistance.The raw material of stoichiometry is weighed first, through high energy milling physical mixed, then, by institute Obtain mixture and carry out calcination process at a certain temperature, you can obtain final catalyst.So far, document and patent report be there is no Such Ce bases catalyst of road is used in SCR reactions.
The content of the invention
The present invention prepares high temperature resistant to sulfur Ce base SCR catalysts, catalyst tool by a kind of simple preparation method There is excellent NH3- SCR reactivities and sulfur resistive water repelling property.Raw material is cheap and easy to get used in catalyst preparation, technique letter It is single, there is potential application prospect in industrial smoke denitration field.
The preparation method of described a kind of high temperature resistant to sulfur Ce base SCR catalysts, it is characterised in that comprise the following steps：
(1) quantitative Ce presomas and TiO are weighed respectively2Carrier, which is put into ball grinder, carries out high energy milling；
(2) powder after high energy milling is placed in Muffle furnace, atmosphere is air, temperature be 250~500 DEG C of roastings 2~ 6h, you can obtain Ce base SCR denitrations.
A kind of preparation method of described high temperature resistant to sulfur Ce base SCR catalysts, it is characterised in that described Ce presomas Can be the salts containing cerium such as cerium oxalate, cerous sulfate, cerous acetate, cerous carbonate, cerous phosphate, cerous nitrate and ceria.
A kind of preparation method of described high temperature resistant to sulfur Ce base SCR catalysts, it is characterised in that the TiO2Carrier is The TiO of nano-sized anatase phase structure2Powder, TiO2Content is 92.0~99.5wt%.
A kind of preparation method of described high temperature resistant to sulfur Ce base SCR catalysts, it is characterised in that Ce base SCR catalysts Middle CeO2Content is 1~45wt%.
The preparation method of described a kind of high temperature resistant to sulfur Ce base SCR catalysts, it is characterised in that the high energy milling time is 0.1~6h, the rotating speed of ball mill is 50~500r/min.
Preparation process of the present invention is simple, and preparation condition is easily controllable, experimental raw environmental sound, is a kind of environment-friendly The SCR catalyst of type, and it is raw materials used cheap and easy to get, there is preferable economy compared with similar catalyst.
According to a kind of preparation method of high temperature resistant to sulfur Ce base SCR catalysts described in above technical scheme, preparation is urged Agent can be used for NH3- SCR denitration is reacted.In test condition：1000ppm NH3, 1000ppm NO, 175ppm SO2, 6% O2, 6%H2O, N2For Balance Air, 30000h-1It is that NO conversion ratios can maintain in the range of 280~550 DEG C in temperature under air speed More than 90%.
Brief description of the drawings
Fig. 1 is the XRD spectra of 1#, the 2# in embodiment 2 in embodiment 1 and the 3# catalyst samples in embodiment 3.
Fig. 2 comments for 1#, the 2# in embodiment 2 in embodiment 1 and the 3# catalyst samples in embodiment 3 SCR activity Valency result.
Fig. 3 is the sulfur resistive water resistant life test result of the 4# catalyst samples in 1# and embodiment 4 in embodiment 1.
Fig. 4 is SCR activity evaluation result of the 1# catalyst samples under different air speeds in embodiment 1.
Embodiment
The present invention is explained with reference to embodiment, but the present invention is not limited to following examples.
Embodiment 1：
Accurately weigh cerium oxalate 24.63g, TiO224g is put into ball grinder, is then added a certain number of a diameter of 10mm Ceramic Balls, ratio of grinding media to material 12:1, it is put into planetary ball mill, the rotating speed of ball mill is 500r/min, high energy milling 1h.Powder after high energy milling is placed in Muffle furnace, in air atmosphere, 250 DEG C of roastings 2h, 500 DEG C of roasting 2h.Then, It is 20~40 mesh by powder tabletting sieving, obtains 1# catalyst samples.
Embodiment 2：
The 1# catalyst samples in 10ml embodiments 1 are taken, are in reaction condition by the catalyst sample：1000ppm NH3, 1000ppm NO, 1500ppm SO2, 6%O2, N2For Balance Air, air speed 3000h-1, it is 300 DEG C of constant lower reactions in temperature 40h, obtain 2# catalyst samples.
Embodiment 3：
The 1# catalyst samples in 10ml embodiments 1 are taken, are in reaction condition by the catalyst sample：1000ppm NH3, 1000ppm NO, 1500ppm SO2, 6%O2, N2For Balance Air, air speed 3000h-1, it is 300 DEG C of constant lower reactions in temperature 60h, obtain 3# catalyst samples.
Embodiment 4：
Accurately weigh cerium oxalate 8.21g, TiO218g is put into ball grinder, then adds a certain number of a diameter of 10mm Ceramic Balls, ratio of grinding media to material 12:1, it is put into planetary ball mill, the rotating speed of ball mill is 500r/min, high energy milling 1h.Will Powder after high energy milling is placed in Muffle furnace, in air atmosphere, 250 DEG C of roastings 2h, 500 DEG C of roasting 2h.Then, by the powder Body tabletting sieving is 20~40 mesh, obtains 4# catalyst samples.
Embodiment 5：
Accurately weigh cerous sulfate 11.58g, TiO214g is put into ball grinder, is then added a certain number of a diameter of 10mm Ceramic Balls, ratio of grinding media to material 12:1, it is put into planetary ball mill, the rotating speed of ball mill is 500r/min, high energy milling 1h.Powder after high energy milling is placed in Muffle furnace, in air atmosphere, 250 DEG C of roastings 2h, 500 DEG C of roasting 2h.Then, It is 20~40 mesh by powder tabletting sieving, obtains 5# catalyst samples.
Test case 1：
X-ray powder diffraction is utilized respectively to be catalyzed the 1# in embodiment 1, the 2# in embodiment 2 and the 3# in embodiment 3 Agent sample carries out phase structure analysis.Test result (Fig. 1) shows：1#, 2#, 3# catalyst sample contain Anatase structure TiO2Characteristic diffraction peak, show through high energy milling and be calcined and reaction some time after TiO2Still keep its original crystalline phase knot Structure.Meanwhile 1#, 2#, 3# catalyst sample also contain more sharp cubic fluorite structure C eO2Characteristic diffraction peak, show CeO in catalyst2Crystallinity it is higher.From 2#, 3# catalyst sample spectrogram it can also be seen that as catalyst sample reacts The growth of time, the TiO of catalyst sample2And CeO2Characteristic diffraction peak intensity gradually weaken, crystallinity gradually reduces, crystal grain Size is gradually reduced.The characteristic diffraction peak about sulfate species is not found from 2#, 3# catalyst sample spectrogram, shows sulphur Hydrochlorate species may with unformed state exist or formed sulfate species very little so that it cannot it was observed that.
Test case 2：
The 3# catalyst samples to the 1# in embodiment 1, the 2# in embodiment 2 and in embodiment 3 carry out SCR activity respectively Test, test condition are：1000ppm NH3, 1000ppm NO, 175ppm SO2, 6%O2, 6%H2O, N2For Balance Air, air speed For 30000h-1, reaction temperature is 160~550 DEG C.Test result (Fig. 2) shows：1# catalyst samples have higher NH3- SCR reactivities, it is that NO conversion ratios can maintain more than 90% in the range of 280~550 DEG C in temperature.
Test case 3：
The 5# catalyst samples progress sulfur resistive to the 1# in embodiment 1, the 4# in embodiment 4 and in embodiment 5 resists respectively Water life test, test condition are：1000ppm NH3, 1000ppm NO, 175ppm SO2, 6%O2, 6%H2O, N2For balance Gas, air speed 30000h-1, reaction temperature is 300 DEG C constant.Test result (Fig. 3) shows：When being passed through 175ppm to reaction system SO2Afterwards, the NO conversion ratios of 1#, 4# and 5# catalyst sample have is lifted by a small margin, by 6% H2After O introduces reaction system, 4# The NO conversion ratios decline of catalyst sample is the most obvious, and the NO conversion ratios of 43%, 5# catalyst samples are down to after 14h in 14h After be down to 62%, and the NO conversion ratios of 1# catalyst samples after 14h is reacted still more than 70%.As cut-out SO2Afterwards, 1#, 4# Recover respectively to 82%, 57% and 71% with the NO conversion ratios of 5# catalyst samples, then by H2After O cut-outs, 1#, 4# and 5# catalysis The NO conversion ratios of agent sample recover to 88%, 65% and 73%.It can be found that 1# catalyst samples have preferable sulfur resistive water resistant Performance.
Test case 4：
SCR activity test is carried out to the 1# catalyst samples in embodiment 1, test condition is：1000ppmNH3, 1000ppm NO, 175ppm SO2, 6%O2, 6%H2O, N2For Balance Air, (air speed is respectively 10000h-1, 30000h-1, 50000h-1, 70000h-1, 90000h-1), reaction temperature is 160~550 DEG C.Test result (Fig. 4) shows：1# catalyst samples NH3- SCR reactivities have declined with the increase of air speed, when air speed is less than 30000h-1When, catalyst reaches at 320 DEG C To NO conversion ratios maximum about 100%, and when air speed is higher than 30000h-1When, catalyst reaches NO conversion ratios maximum at 360 DEG C Value, is down to less than 85%.Therefore, it is 30000h to control air speed-1, good denitration effect can be obtained.

Claims (3)

1. a kind of preparation method of high temperature resistant to sulfur Ce base SCR catalysts, it is characterised in that comprise the following steps：
(1) quantitative Ce presomas and TiO are weighed respectively2It is put into ball grinder and carries out high energy milling；The high energy milling time is 0.1 ~6h, the rotating speed of ball mill is 50~500r/min；
(2) powder after high energy milling is placed in Muffle furnace, atmosphere is air, and temperature is 250~500 DEG C of 2~6h of roasting, is obtained To Ce base SCR denitrations；CeO in Ce base SCR catalysts2Content is 1~45wt%, and remaining is TiO2。
2. according to the method for claim 1, it is characterised in that the Ce presomas described in step (1) be cerium oxalate, cerous sulfate, Cerous acetate, cerous carbonate, cerous phosphate, cerous nitrate or ceria.
3. Ce base SCR catalysts prepared by any one of claim 1 or 2 methods described are in ammine selectivity catalytic reduction nitrous oxides Applied in reaction.
CN201710946222.6A 2017-10-12 2017-10-12 A kind of preparation method of high temperature resistant to sulfur Ce base SCR catalysts Pending CN107715858A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108816216A (en) * 2018-06-29 2018-11-16 凯龙高科技股份有限公司 A kind of high temperature modification SCR catalyst and its preparation method and application
CN109225260A (en) * 2018-08-01 2019-01-18 北京工业大学 A kind of regeneration method for sulfur poisoning Ce base SCR denitration
CN114289041A (en) * 2021-12-09 2022-04-08 安徽欣创节能环保科技股份有限公司 Preparation process of improved sulfur-resistant sintering flue gas decarburization catalyst

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CN106179301A (en) * 2016-07-01 2016-12-07 北京工业大学 A kind of preparation method of cerium-titanium composite oxide low-temperature SCR catalyst
CN106622207A (en) * 2017-01-06 2017-05-10 北京工业大学 Preparation method of cerium-based sulfate catalyst for SCR (selective catalytic reduction) reaction

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108816216A (en) * 2018-06-29 2018-11-16 凯龙高科技股份有限公司 A kind of high temperature modification SCR catalyst and its preparation method and application
CN109225260A (en) * 2018-08-01 2019-01-18 北京工业大学 A kind of regeneration method for sulfur poisoning Ce base SCR denitration
CN109225260B (en) * 2018-08-01 2021-11-05 北京工业大学 Regeneration method of Ce-based SCR denitration catalyst for sulfur poisoning
CN114289041A (en) * 2021-12-09 2022-04-08 安徽欣创节能环保科技股份有限公司 Preparation process of improved sulfur-resistant sintering flue gas decarburization catalyst
CN114289041B (en) * 2021-12-09 2023-09-29 安徽欣创节能环保科技股份有限公司 Preparation process of improved sulfur-resistant sintering flue gas decarburization catalyst

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Application publication date: 20180223