氮氧化物低温选择性催化还原锰基催化剂研究
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摘要
氮氧化物（NOx）污染所引起的酸雨、光化学烟雾等环境问题日益受到人们的重视。静态污染源尾气处理主要采用氨选择性催化还原技术（NH3-SCR），其使用的主要催化剂为V2O5-WO3(MO3)/TiO2。但现行SCR法还存在系列问题，包括催化剂活性温度范围高而窄（300~400℃），易受飞灰、水及SO2的影响，易生成N2O、催化剂寿命较短、容易堵塞失活等。低温SCR法（80~200℃）是近年来发展起来的新技术，其脱氮装置可置于脱硫装置之后，从而避免灰飞对催化剂的污染、磨损、堵塞，减轻SO2引起的毒化、失活，具有易与现有的烟道设备匹配、延长催化剂使用寿命、经济高效能耗低等优点。因此，低温SCR催化剂的设计与开发成为其重点研究方向。本论文发展并详细考察了三类Mn基催化剂的低温SCR性能及其抗水耐硫性能。同时，利用BET、XRD、TPR/TPD、FT-IR、XPS、SEM/TEM等对催化剂物性及结构进行了表征，对催化剂构效关系和反应动力学进行了深入探讨。
研究了系列Mn-Zr复合氧化物催化剂低温SCR性能，比较了柠檬酸法，共沉淀法，固相合成法对Mn-Zr复合氧化物催化剂性能结构的影响。结果表明，采用柠檬酸法制备的催化剂活性最高，低温SCR性能优越，当Mn/(Mn+Zr)摩尔比为0.5，450oC焙烧下，催化剂具有最佳的低温活性，在30000h-1空速下，在100~200oC温度范围内可获得近100%的脱硝效率。水对催化剂活性表现为可逆抑制效应，说明催化剂具有较好的抗水性能。但是SO2对催化剂的毒化作用为不可逆。催化过程中，催化剂表面生成了难于分解的硫酸锰铵盐，因而无法实现400oC加热再生，但通过水洗溶解可除去硫酸锰铵盐，且使催化剂活性得到恢复。系统表征结果表明，采用柠檬酸法制备的催化剂在合适的Mn/(Mn+Zr)摩尔比时，具有较高的比表面积，MnOx部分嵌入ZrO2晶格形成固溶体，余下部分在催化剂表面高度分散，并具有良好的氧化还原性能。此外，催化剂对NH3具有良好的吸附性能，及高表面氧含量的对SCR反应也有促进作用。对Mn-Zr催化剂的动力学研究表明，其反应级数对于NO、O2、NH3分别为0.6、0.5及0级。
采用溶剂热法制备了一系列Mn-TiO2催化剂，并与浸渍法进行比较，同时考察不同锰源的影响。采用溶剂热法，以乙酸锰为锰源，可以获得具有高脱硝性能的Mn-TiO2催化剂。当Mn/Ti摩尔比为0.2，经500oC焙烧后催化剂具有最佳活性，在空速为30,000h-1，反应温度为120oC时，催化剂可以获得近100%的脱硝效率。水对催化剂表现出可逆的抑制效应而硫对催化剂的作用表现为逐步毒化失活且活性不可恢复。系统结构表征表明，以乙酸锰为锰源，采用溶剂热法合成的催化剂具有较高的比表面，TiO2为高分散纳米级别，Mn活性组分以无定型状态分散在催化剂表面，从而具有较好的氧化还原性能。对催化剂的反应动力学的研究表明，其反应级数对于NO、O2、NH3分别为1、0.5及0级。反应的表观活化能为24.2kJ·mol-1，低于文献报道的同类催化剂。
采用柠檬酸法制备了Fe-Co复合氧化物，发现当Fe/Co比为4时，催化剂具有较好的活性，在200~300oC范围内NOx转化率接近100%，通过添加Mn，制备成Mn-Fe-Co三组分复合氧化物后催化剂具有较高的低温活性。当Fe/Co摩尔比为4，Mn添加量为0.3（Mn/(Fe+Co)摩尔比）时，催化剂在80oC即可达到100%的NOx转化率，高于之前报道的Fe-Mn体系，表明三组分催化剂具有更好的催化活性。系统表征结果表明，制备的Fe4Co1Ox催化剂为Fe2O3晶相和CoFe2O4尖晶石结构复合氧化物晶相，添加适量Mn后Fe2O3晶相消失，除CoFe2O4晶相外，多余的Fe和添加的Mn均以高分散形式存在于催化剂中。Mn的加入同时也促进了催化剂的氧化还原性能。
Selective catalytic reduction (SCR) of NOx(x=1,2) by ammonia is one of the majortechnologies for reducing nitrogen oxides emitted from stationary sources such as powerstations, industrial heaters, and cogeneration and has been successfully commercialized.Vanadium-based catalysts such as V2O5/TiO2(anatase) mixed with WO3or MoO3are typicalcommercial catalysts for this process; however, they are only active within a narrowtemperature window of300~400oC, and are susceptible to deactivation by dust deposition orSO2poisoning. Thus, there has been a very strong incentive to develop highly efficientdenitration catalysts for low-temperature SCR processes in which these catalysts would beplaced downstream of the desulfurizer and electrostatic precipitator in the power generationsystem. In this dissertation, three kinds of Mn-based catalysts were investigated for thelow-temperature SCR and systematically characterized and the structure-activity relationshipwere discussed and the catalytic kinetics were also studied.
Novel Mn-Zr mixed-oxide catalysts have been prepared by citric acid method for thelow-temperature SCR of NOxwith ammonia in the presence of excess oxygen compared tothe co-precipitation method and solid state reaction method. It was found that anMn(0.5)-ZrOx-450catalyst prepared by citric acid method showed the highest activity, givingalmost100%NOxconversion at100oC with a gas hourly space velocity of30,000h-1. Thecatalyst showed a certain level of sulfur tolerance and water resistance. The effect of H2Ocould be quickly eliminated after its removal, whereas deactivation by SO2proved to beirreversible. The formation of (NH4)2Mn2(SO4)3on the catalyst surface results in deactivationand the catalyst can be recovered by water washing but not thermal regeneration because(NH4)2Mn2(SO4)3is hard to decomposition but can dissolved in water. The characterizationresults suggested that an Mn-Zr solid solution was formed in the Mn(0.5)-ZrOx-450(CA)catalyst, with highly dispersed MnOx. An appropriate NH3adsorption ability was beneficialfor the low-temperature SCR. The kinetic study results show that the reaction order for NO,NH3and O2respectively is0.6,0and0.5.
Mn-TiO2catalysts have been prepared by the solvothermal method for the low-temperature SCR of NOxwith ammonia in the presence of excess oxygen with comparison to wetimpregnation method and the effect of Mn resource was also investigated. It was found thatthe Mn-TiO2catalyst prepared by solvothermal method using Mn(CHCOO)2as Mn precursorshowed the highest activity, giving almost100%NOxconversion at120oC with a gas hourlyspace velocity of30,000h1. The catalyst showed a certain level of sulfur tolerance and waterresistance. The effect of H2O could be quickly eliminated after its removal, whereasdeactivation by SO2proved to be irreversible. The characterization results showed that a highdispersity of Mn on nano TiO2particles and good reducibility and high surface area isbenefited for the low temperature SCR. The kinetic study results showed that the reactionorder for NO, NH3and O2respectively is1,0and0.5and the active energy is24.2kJ·mol-1which is lower than similar catalysts in the literatures.
Fe-Co mixed oxides were prepared by citric acid method and investigated for lowtemperature SCR. The Fe4Co1Ox(mole ratio of Fe/Co for4) gave the best activity. Nearly100%NOxconversion was achieved between200~300oC with a gas hourly space velocity of30,000h-1. The activity at low temperature (<200oC) can be improved by added Mn intoFe4Co1Oxand high low temperature activity can be obtained on Mn(0.3)-Fe4Co1Oxcatalystwith mole ratio of Mn/(Fe+CO) for0.3as100%NOxconversion can be obtain at80oC,which is also higher than Fe-Mn catalyst previous reported. The catalysts were examined byvarious characterization techniques and it was found that mixed crystal phases of Fe2O3andCoFe2O4spinel existed in Fe4Co1Oxwhile only CoFe2O4spinel crystal existed inMn(0.3)-Fe4Co1Ox. Highly dispersed Mn and Fe on the catalyst surface and good reducibilitycan be accounted for the high activity of Mn(0.3)-Fe4Co1Oxcatalyst.
研究了系列Mn-Zr复合氧化物催化剂低温SCR性能，比较了柠檬酸法，共沉淀法，固相合成法对Mn-Zr复合氧化物催化剂性能结构的影响。结果表明，采用柠檬酸法制备的催化剂活性最高，低温SCR性能优越，当Mn/(Mn+Zr)摩尔比为0.5，450oC焙烧下，催化剂具有最佳的低温活性，在30000h-1空速下，在100~200oC温度范围内可获得近100%的脱硝效率。水对催化剂活性表现为可逆抑制效应，说明催化剂具有较好的抗水性能。但是SO2对催化剂的毒化作用为不可逆。催化过程中，催化剂表面生成了难于分解的硫酸锰铵盐，因而无法实现400oC加热再生，但通过水洗溶解可除去硫酸锰铵盐，且使催化剂活性得到恢复。系统表征结果表明，采用柠檬酸法制备的催化剂在合适的Mn/(Mn+Zr)摩尔比时，具有较高的比表面积，MnOx部分嵌入ZrO2晶格形成固溶体，余下部分在催化剂表面高度分散，并具有良好的氧化还原性能。此外，催化剂对NH3具有良好的吸附性能，及高表面氧含量的对SCR反应也有促进作用。对Mn-Zr催化剂的动力学研究表明，其反应级数对于NO、O2、NH3分别为0.6、0.5及0级。
采用溶剂热法制备了一系列Mn-TiO2催化剂，并与浸渍法进行比较，同时考察不同锰源的影响。采用溶剂热法，以乙酸锰为锰源，可以获得具有高脱硝性能的Mn-TiO2催化剂。当Mn/Ti摩尔比为0.2，经500oC焙烧后催化剂具有最佳活性，在空速为30,000h-1，反应温度为120oC时，催化剂可以获得近100%的脱硝效率。水对催化剂表现出可逆的抑制效应而硫对催化剂的作用表现为逐步毒化失活且活性不可恢复。系统结构表征表明，以乙酸锰为锰源，采用溶剂热法合成的催化剂具有较高的比表面，TiO2为高分散纳米级别，Mn活性组分以无定型状态分散在催化剂表面，从而具有较好的氧化还原性能。对催化剂的反应动力学的研究表明，其反应级数对于NO、O2、NH3分别为1、0.5及0级。反应的表观活化能为24.2kJ·mol-1，低于文献报道的同类催化剂。
采用柠檬酸法制备了Fe-Co复合氧化物，发现当Fe/Co比为4时，催化剂具有较好的活性，在200~300oC范围内NOx转化率接近100%，通过添加Mn，制备成Mn-Fe-Co三组分复合氧化物后催化剂具有较高的低温活性。当Fe/Co摩尔比为4，Mn添加量为0.3（Mn/(Fe+Co)摩尔比）时，催化剂在80oC即可达到100%的NOx转化率，高于之前报道的Fe-Mn体系，表明三组分催化剂具有更好的催化活性。系统表征结果表明，制备的Fe4Co1Ox催化剂为Fe2O3晶相和CoFe2O4尖晶石结构复合氧化物晶相，添加适量Mn后Fe2O3晶相消失，除CoFe2O4晶相外，多余的Fe和添加的Mn均以高分散形式存在于催化剂中。Mn的加入同时也促进了催化剂的氧化还原性能。
Selective catalytic reduction (SCR) of NOx(x=1,2) by ammonia is one of the majortechnologies for reducing nitrogen oxides emitted from stationary sources such as powerstations, industrial heaters, and cogeneration and has been successfully commercialized.Vanadium-based catalysts such as V2O5/TiO2(anatase) mixed with WO3or MoO3are typicalcommercial catalysts for this process; however, they are only active within a narrowtemperature window of300~400oC, and are susceptible to deactivation by dust deposition orSO2poisoning. Thus, there has been a very strong incentive to develop highly efficientdenitration catalysts for low-temperature SCR processes in which these catalysts would beplaced downstream of the desulfurizer and electrostatic precipitator in the power generationsystem. In this dissertation, three kinds of Mn-based catalysts were investigated for thelow-temperature SCR and systematically characterized and the structure-activity relationshipwere discussed and the catalytic kinetics were also studied.
Novel Mn-Zr mixed-oxide catalysts have been prepared by citric acid method for thelow-temperature SCR of NOxwith ammonia in the presence of excess oxygen compared tothe co-precipitation method and solid state reaction method. It was found that anMn(0.5)-ZrOx-450catalyst prepared by citric acid method showed the highest activity, givingalmost100%NOxconversion at100oC with a gas hourly space velocity of30,000h-1. Thecatalyst showed a certain level of sulfur tolerance and water resistance. The effect of H2Ocould be quickly eliminated after its removal, whereas deactivation by SO2proved to beirreversible. The formation of (NH4)2Mn2(SO4)3on the catalyst surface results in deactivationand the catalyst can be recovered by water washing but not thermal regeneration because(NH4)2Mn2(SO4)3is hard to decomposition but can dissolved in water. The characterizationresults suggested that an Mn-Zr solid solution was formed in the Mn(0.5)-ZrOx-450(CA)catalyst, with highly dispersed MnOx. An appropriate NH3adsorption ability was beneficialfor the low-temperature SCR. The kinetic study results show that the reaction order for NO,NH3and O2respectively is0.6,0and0.5.
Mn-TiO2catalysts have been prepared by the solvothermal method for the low-temperature SCR of NOxwith ammonia in the presence of excess oxygen with comparison to wetimpregnation method and the effect of Mn resource was also investigated. It was found thatthe Mn-TiO2catalyst prepared by solvothermal method using Mn(CHCOO)2as Mn precursorshowed the highest activity, giving almost100%NOxconversion at120oC with a gas hourlyspace velocity of30,000h1. The catalyst showed a certain level of sulfur tolerance and waterresistance. The effect of H2O could be quickly eliminated after its removal, whereasdeactivation by SO2proved to be irreversible. The characterization results showed that a highdispersity of Mn on nano TiO2particles and good reducibility and high surface area isbenefited for the low temperature SCR. The kinetic study results showed that the reactionorder for NO, NH3and O2respectively is1,0and0.5and the active energy is24.2kJ·mol-1which is lower than similar catalysts in the literatures.
Fe-Co mixed oxides were prepared by citric acid method and investigated for lowtemperature SCR. The Fe4Co1Ox(mole ratio of Fe/Co for4) gave the best activity. Nearly100%NOxconversion was achieved between200~300oC with a gas hourly space velocity of30,000h-1. The activity at low temperature (<200oC) can be improved by added Mn intoFe4Co1Oxand high low temperature activity can be obtained on Mn(0.3)-Fe4Co1Oxcatalystwith mole ratio of Mn/(Fe+CO) for0.3as100%NOxconversion can be obtain at80oC,which is also higher than Fe-Mn catalyst previous reported. The catalysts were examined byvarious characterization techniques and it was found that mixed crystal phases of Fe2O3andCoFe2O4spinel existed in Fe4Co1Oxwhile only CoFe2O4spinel crystal existed inMn(0.3)-Fe4Co1Ox. Highly dispersed Mn and Fe on the catalyst surface and good reducibilitycan be accounted for the high activity of Mn(0.3)-Fe4Co1Oxcatalyst.
引文
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