WO_3的引入对MnO_x-Fe_2O_3催化剂上NH_3-SCR反应中N_2选择性的促进作用
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摘要
采用溶胶-凝胶法制备了不同含量钨修饰的MnO_x-Fe_2O_3催化剂,重点考察WO_3的引入对NH_3-SCR反应中N2选择性的影响,通过XRD、BET、XPS、H2-TPR、Raman和In situ DRIFTS等手段对催化剂的物理化学性质进行表征。结果表明,钨的引入显著提高NH_3-SCR的N2选择性,当WO3质量分数为15%时,具有最佳的NH3-SCR催化性能,且在50-250℃条件下N_2O浓度始终低于0.003%。这主要是由于适量WO_3的引入,导致催化剂物相由α-Fe2O3向γ-Fe2O3转变,并与锰相互作用形成新的无定型Mn WO_4,获得较大的比表面积;使得Mn4+/(Mn~(3+)+Mn~(4+))比例减少但Fe~(2+)及表面化学吸附氧(Oα)含量增加,从而降低催化剂氧化性;增强催化剂表面的Lewis酸性位点的含量及强度,增强NH3的吸附,促进了SCR反应,同时抑制了NO_2深度氧化形成硝酸盐物种,降低硝酸盐物种还原产生的副产物N2O含量,从而显著提高WO3-MnO_x-Fe_2O_3催化剂在NH_3-SCR中的N2选择性。
A series of tungsten modified MnOx-Fe_2O_3 catalysts with different tungsten contents were prepared by sol-gel method. The influence of tungsten on N_2 selectivity of NH_3-SCR reaction was investigated particularly.Physical and chemical properties of the catalysts were characterized by means of XRD,BET,XPS,H_2-TPR,Raman and in situ DRIFTS. The results showed that N_2 selectivity of NH_3-SCR at high temperature was significantly improved by introducing tungsten. NH_3-SCR possessed the best catalytic performance when the tungsten content was 15%( mass ratio),as well as N2 O concentration was less than 0.003% within the range of50-250 ℃. The primary causes were the phase change from α-Fe_2O_3 to γ-Fe_2O_3 due to the introduction of appropriate amount of WO_3. Besides,the interaction between tungsten and manganese formed a newamorphous MnWO_4 and obtained a large specific surface area. In addition,the ratio of Mn~(4+)/( Mn~(3+)+Mn~(4+)) decreased while the content of Fe2+and surface chemical adsorption oxygen( Oα) increased,thus the oxidability of the catalyst was reduced. Meanwhile,tungsten doping enhanced the content and strength of Lewis acid sites on the surface of catalysts at high temperatures. Moreover,the adsorption of NH_3 was enhanced,thus,NH_3-SCR reaction was accelerated. The doping of WO_3 inhibited the deep oxidation of NO_2 to form nitrate species,reduced the content of by-product N2 O produced by nitrate species reduction,and significantly improved the NH_3-SCR activity and N2 selectivity of WO_3-MnO_x-Fe_2O_3 catalyst at experimental temperature.
A series of tungsten modified MnOx-Fe_2O_3 catalysts with different tungsten contents were prepared by sol-gel method. The influence of tungsten on N_2 selectivity of NH_3-SCR reaction was investigated particularly.Physical and chemical properties of the catalysts were characterized by means of XRD,BET,XPS,H_2-TPR,Raman and in situ DRIFTS. The results showed that N_2 selectivity of NH_3-SCR at high temperature was significantly improved by introducing tungsten. NH_3-SCR possessed the best catalytic performance when the tungsten content was 15%( mass ratio),as well as N2 O concentration was less than 0.003% within the range of50-250 ℃. The primary causes were the phase change from α-Fe_2O_3 to γ-Fe_2O_3 due to the introduction of appropriate amount of WO_3. Besides,the interaction between tungsten and manganese formed a newamorphous MnWO_4 and obtained a large specific surface area. In addition,the ratio of Mn~(4+)/( Mn~(3+)+Mn~(4+)) decreased while the content of Fe2+and surface chemical adsorption oxygen( Oα) increased,thus the oxidability of the catalyst was reduced. Meanwhile,tungsten doping enhanced the content and strength of Lewis acid sites on the surface of catalysts at high temperatures. Moreover,the adsorption of NH_3 was enhanced,thus,NH_3-SCR reaction was accelerated. The doping of WO_3 inhibited the deep oxidation of NO_2 to form nitrate species,reduced the content of by-product N2 O produced by nitrate species reduction,and significantly improved the NH_3-SCR activity and N2 selectivity of WO_3-MnO_x-Fe_2O_3 catalyst at experimental temperature.
引文
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[4] BYRNE J W,CHEN J M,SPERONELLO B K. Selective catalytic reduction of NOxusing zeolitic catalysts for high temperature applications[J]. Catal Today,1992,13:33-42.
[5] WING C W,NOBE K. Reduction of NO with NH3on Al2O3-and TiO2-supported metal oxide[J]. Ind Eng Chem Prod Res Dev,1986,25:179-186.
[6] ZHANG C A,CHEN T H,LIU H B,CHEN D,XU B,QING C S. Low temperature SCR reaction over nano-structured Fe-Mn oxides:Characterization,performance,and kinetic study[J]. Appl Sur Sci,2018,457:1116-1125.
[7] CHEN X H,ZHENG Y Y,ZHANG Y B. MnO2-Fe2O3catalysts supported on polyphenylene sulfide filter felt by a redox method for the lowtemperature NO reduction w ith NH3[J]. Catal Commun,2018,105:16-19.
[8] WANG Z,SHEN G L,LI J Q,LIU H D,WANG Q,CHEN Y F. Catalytic removal of benzene over CeO2-Mn Oxcomposite oxides prepared by hydrothermal method[J]. Appl Catal B:Environ,2013,138-139:253-259.
[9] ZHANG D S,ZHANG L,SHI L Y,FANG C. In situ supported MnO(x)-CeO(x)on carbon nanotubes for the low-temperature selective catalytic reduction of NO w ith NH3[J]. Nanoscale,2013,5(3):1127-1136.
[10] LIU F D,HE H,ZHANG C B,FENG Z C,ZHENG L R,XIE Y M,HU T D. Selective catalytic reduction of NO with NH3over iron titanate catalyst:Catalytic performance and characterization[J]. Appl Catal B:Environ,2010,96(3/4):408-420.
[11] YAO X J,ZHANG L,LI L L,LIU L C,CAO Y,DONG X,GAO F,DENG Y,TANG C J,CHEN Z,DONG L,CHEN Y. Investigation of the structure,acidity,and catalytic performance of CuO/Ti0.95Ce0.05O2catalyst for the selective catalytic reduction of NO by NH3at low temperature[J]. Appl Catal B:Environ,2014,150/151:315-329.
[12] YAO X J,KONG T T,YU S H,LI L L,YANG F M,DONG L. Influence of different supports on the physicochemical properties and denitration performance of the supported Mn-based catalysts for NH3-SCR at low temperature[J]. Appl Sur Sci,2017,402:208-217.
[13] SINGOREDJO L,KORVER R,KAPTEQN F,MOUHJN J. Alumina supported manganese oxides for the low temperature selective catalytic reduction of nitric oxide w ith ammonia[J]. Appl Catal B:Environ,1992,1:297-316.
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[15] LIN Q C,LI J H,MA L,HAO J M. Selective catalytic reduction of NO with NH3over Mn-Fe/USY under lean burn conditions[J]. Catal Today,2010,151(3/4):251-256.
[16] LIU F D,HE H,ZHANG C B. Novel iron titanate catalyst for the selective catalytic reduction of NO with NH3in the medium temperature range[J]. Chem Commun,2008,17:2043-2045.
[17] XIONG Z B,LU C M,GUO D X,ZHANG X L,HAN K H. Selective catalytic reduction of NOxw ith NH3over iron-cerium mixed oxide catalyst:Catalytic performance and characterization[J]. J Chem Technol Biot,2013,88(7):1258-1265.
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[19] APOSTOLESCU N,GEIGERAK B,HIZBULLAH K,JANC MT,KURETI S,REICHERT D,SCHOTT F,WEISWEILER W. Selective catalytic reduction of nitrogen oxides by ammonia on iron oxide catalysts[J]. Appl Catal B:Environ,2006,62(1/2):104-114.
[20] AI-ZENG M,GRNERT W. Selective catalytic reduction of NO by ammonia over Fe-ZSM-5 catalysts[J]. Chem Commun,1999:71-72.
[21] SUN W B,LI X Y,ZHAO Q,MU J C,CHEN J H. Fe-Mn mixed oxide catalysts synthesized by one-step urea-precipitation method for the selective catalytic reduction of NOxw ith NH3at low temperatures[J]. Catal Lett,2017,148(1):227-234.
[22] CHEN Z H,WANG F R,LI H,YANG Q,WANG L F,LI X H. Low-temperature selective catalytic reduction of NOxw ith NH3over Fe-Mn mixed-oxide catalysts containing Fe3Mn3O8phase[J]. Ind Eng Chem Res,2011,51(1):202-212.
[23] PARK H,SHIN B,LEE H. Catalytic activity and surface characteristics of WO3-doped MnOx-TiO2catalysts for low-temperature selective catalytic reduction of NOxw ith NH3[J]. J Korean Inst Met Mater,2016,54(10):787-792.
[24] WANG X M,LI X Y,ZHAO Q D,SUN W B,TADE M,LIU S M. Improved activity of W-modified Mn Ox-TiO2catalysts for the selective catalytic reduction of NO w ith NH3[J]. Chem Eng J,2016,288:216-222.
[25] SHI J,ZHANG Z H,CHEN MX,ZHANG Z X,SHANG GUAN W F. Promotion effect of tungsten and iron co-addition on the catalytic performance of MnOx/TiO2for NH3-SCR of NOx[J]. Fuel,2017,210:783-789.
[26] SHIN B,LEE H,PARK H. Catalytic activity and surface characteristics of WO3-doped MnOx-TiO2catalysts for low-temperature selective catalytic reduction of NOxw ith NH3[J]. Korean J Met Mater,2016,54:787-792.
[27] CHOUNG J W,NAMI S,HAMS W. Effect of promoters including tungsten and barium on the thermal stability of V2O5/sulfated TiO2catalyst for NO reduction by NH3[J]. Catal Today,2006,111(3/4):242-247.
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[29] SHAN W P,LIU F D,HE H,SHI X Y,ZHANG C B. Novel cerium-tungsten mixed oxide catalyst for the selective catalytic reduction of NO(x)w ith NH3[J]. Chem Commun,2011,47(28):8046-8048.
[30] SHAN W P,GENG Y,CHEN X L,HUANG N,LIU F D,YANG S J. A highly efficient CeWOxcatalyst for the selective catalytic reduction of NOxw ith NH3[J]. Catal Sci Technol,2016,6(4):1195-1200.
[31] HEINZ W,ULRIKE G,PAUL R M,BRIAN B B. Immunocytochemical characterization and spatial distribution of midget bipolar cells in the macaque monkey retina[J]. Vision Res,1994,34:561-579.
[32]王琪莹,刘自力,邹汉波,赵朝晖,韦星船.表面活性剂改性对Zn/Ti-PILCs吸附剂脱硫性能的影响[J].燃料化学学报,2011,39(3):203-206.(WANG Qi-ying,LIU Zi-li,ZOU Han-bo,ZHAO Chao-hui,WEI Xing-chuan. Effect of surfactant modification on desulfurization performance of Zn/Ti-PILCs adsorbent[J]. J Fuel Chem Technol,2011,39(3):203-206.)
[33] LEE J,KWAK S Y. Mn-doped maghemite(γ-Fe2O3)from metal-organic framework accompanying redox reaction in a bimetallic system:The structural phase transitions and catalytic activity tow ard NOxremoval[J]. ACS Omega,2018,3:2634-2640.
[34]张信莉,王栋,彭建升,路春美,徐丽婷.煅烧温度对Mn改性γ-Fe2O3催化剂结构及低温SCR脱硝活性的影响[J].燃料化学学报,2015,43(2):244-250.(ZHANG Xin-li,WANG Dong,PENG Jian-sheng,LU Chun-mei,XU Li-ting. Effect of calcination temperature on structure of Mn Modifiedγ-Fe2O3catalyst and denitration activity of low temperature SCR[J]. J Fuel Chem Technol,2015,43(2):244-250.)
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