富氧环境下碳烟还原NO_x的微观反应机理研究
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摘要
柴油机因热循环效率高、燃油经济性好、CO_2排放量低而倍受重视。但柴油机尾气中碳烟和NO_x造成的环境污染问题也日益突出。由于柴油机机内NO_x与碳烟控制存在所谓的trade-off关系,仅通过改进发动机降低NO_x和碳烟排放有一定的局限性。利用柴油机尾气中的碳烟还原NO_x为N_2、同时自身被氧化为CO_2,是较理想的同时去除NO_x和碳烟的后处理技术。而研究NO_x和碳烟微观反应机理,则有助于揭示催化剂催化NO_x和碳烟反应的本质,发现催化剂表面反应过程中促进和制约NO_x还原、碳烟燃烧的因素,对发展NO_x和碳烟互为氧化还原技术有指导意义。
本文将BaAl_2O_4用于催化NO_x和碳烟反应的研究,利用程序升温反应(TPR)技术评价了该催化剂在不同反应条件下催化同时去除碳烟和NO_x的活性。采用漫反射红外光谱和拉曼光谱,详细地研究了BaAl_2O_4催化碳烟和NO_x反应的微观机理。具体工作如下:
(1)制备了La_(0.8)K_(0.2)MnO_3和BaAl_2O_4催化剂,采用XRD、FT-IR、SEM等对制备的催化剂进行物理性能表征。利用TPR技术综合评价和比较了La_(0.8)K_(0.2)MnO_3和BaAl_2O_4的催化性能。结果表明,这两种催化剂催化碳烟和NO_x的反应均具有较高的活性,与非催化反应相比,碳烟的起燃温度和最大燃烧温度分别降低了175℃和240℃以上,NO_x转化为N_2的效率有了很大提高。
(2)分析了各种反应条件对催化同时去除碳烟和NO_x反应的影响。研究发现,反应气体的空速越低、碳烟和催化剂的质量比越高,越有利于催化反应进行;O_2的存在能促进碳烟和NO_x的催化反应,当模拟尾气中O_2含量由2%增加为5%时,碳烟的起燃温度和最大燃烧温度分别由330℃和405℃降低了大约30℃,在BaAl_2O_4催化作用下,NO_x转化为N_2和N_2O的效率分别由10.2%和3.5%升至12.1%和3.9%,在La_(0.8)K_(0.2)MnO_3催化作用下,由14.52%和6.63%降至11.02%和4.93%。
(3)采用漫反射红外光谱,用NH3作为探针分子,分析了BaAl_2O_4表面的酸性中心,发现BaAl_2O_4表面同时存在质子酸(Br?nsted酸)和非质子酸(Lewis酸)。分析了不同反应条件下NO、NO_2和O_2在BaAl_2O_4表面的动态行为以及它们之间的相互作用。研究表明,NO主要以线性和桥位亚硝酸盐的形态吸附在催化剂表面;除了形成亚硝酸盐外,NO_2在催化剂表面还直接形成了单齿硝酸盐、桥位硝酸盐和离子硝酸盐;生成的亚硝酸盐将继续与催化剂表面的吸附氧( O~-_(surf)和O 2 ?lattice)或O_2反应生成硝酸盐物种,其中O ? surf的氧化能力最强。研究发现,O_2除了将NO氧化为NO_2外,另外一个重要作用是将亚硝酸盐氧化为硝酸盐,O_2的浓度越高越有利于硝酸盐物种形成;高温也有利于形成硝酸盐物种,350℃时(碳烟和NO_x以较快速度反应),硝酸盐物种的形成与吸附时间关系不大。
(4)利用拉曼光谱(LRS)分析了碳烟与NO、NO_2及O_2的反应。发现碳烟用O_2或NO_x处理后,因与这些气体反应生成C(O)中间体,其非晶质碳渣和SP2碳结构被破坏。研究证明,高温有利于NO_x、O_2等与碳烟反应,相同温度下反应活性以NO+O_2 > O_2 > NO的顺序递减。
(5)采用漫反射红外光谱原位分析了碳烟和NO_x在催化剂BaAl_2O_4表面的详细反应过程。研究表明,催化剂表面的硝酸盐物种因具有较强的氧化能力,优先与碳烟的部分氧化产物(C(O))发生氧化还原反应,生成的最终产物CO_2、N_2和N_2O从催化剂表面脱附,催化剂获得再生;硝酸盐物种与C(O)中间体的反应在催化同时去除碳烟和NO_x的过程中起主要作用,是碳烟和NO_x反应的速控步骤,与程序升温反应结果及NO_x在催化剂表面动态行为的分析结果相符。研究发现,N_2O具有一定的氧化能力,高温下生成的N_2O还没有来得及被红外光谱检测到,就已和C(O)反应了。催化剂表面生成硝酸盐物种浓度的多少直接关系到NO_x转化为N_2的效率,这与催化剂吸附NO_x后生成硝酸盐物种的能力有关。
(6)利用密度泛函理论(DFT)构建并优化了BaAl_2O_4、C(O)中间体、NO_x在催化剂表面反应的中间产物及反应气体分子模型,利用推广的休克尔分子轨道法(EHMO)计算了各模型的分子轨道。结合分子轨道理论,比较分析了最高占据分子轨道和最低未占分子轨道的能级。结果表明催化剂表面O~-_(surf)的活性比O~(2-)_(lattice)强,其表面的亚硝酸盐物种被吸附氧( O~-_(surf)、O~(2-)_(lattice))或O_2氧化为硝酸盐物种。
Diesel engines have attracted much attention due to their high efficiency, economy and low CO_2 emissions. Correspondingly, with the main emissions of NO_x and soot, the related problems of environmental pollution are serious day by day. In cylinder, there exist trade-off effects for NO_x and soot control. Therefore, soot and NO_x cannot be reduced efficiently by improving combustion alone. Simultaneous removal of soot and NO_x is the optimal diesel engine after-treatment technique, in which NO_x is reduced into N_2 by soot, in return, soot is oxidized into CO_2 at the same time. To investigate the essence of the redox and find the crtical factors that promote and restrict the reaction, will be of great interesting in developing the technique for simultaneous removal of soot and NO_x.
In this study, the catalytic activity of BaAl_2O_4 in simultaneous removal of soot and NO_x was evaluated by Temperature Programmed Reaction (TPR) technique under various reaction conditions. Then, the micro mechanism for the catalytic reaction of soot with NO_x on the surface of BaAl_2O_4 was investigated by DRIFTS (Diffuse Reflectance Infrared Fourier Transform Spectroscopy) and LRS (Laser Raman Spectroscopy). The detailed research is summarized as following:
(1) La_(0.8)K_(0.2)MnO_3 and BaAl_2O_4 were prepared and characterized by XRD, FT-IR and SEM. The catalytical activity of La_(0.8)K_(0.2)MnO_3 and BaAl_2O_4 was evaluated systematically by TPR. These two catalysts all exhibit high catalytic activity in simultaneous removal of soot and NO_x, for exampe, Tig and Tm of soot decrease by more than 175℃and 240℃respectively, and the conversion of NO_x into N_2 is improved markedly.
(2) The reaction of soot with NO_x was studied under various conditions. It is found that low GHSV (Gas Hourly Space Velocity) and high mass ratio of soot to catalyst are benefitial to the redox. Oxygen may promote the catalytic reaction of soot with NO_x. Both Tig and Tm of soot is decreased by ca. 30℃by increasing O_2 content from 2% to 5%. It is interesting that O_2 ehances the maximum conversion efficiencies of NO_x into N_2 and N_2O with the catalysis of BaAl_2O_4, however, the conversion efficiencies were depressed by changing BaAl_2O_4 to La_(0.8)K_(0.2)MnO_3.
(3) Adsorption of ammonia was studied in order to obtain informaion on the surface acidity (Lewis and Br?nsted) of BaAl_2O_4 by DRIFTS. It is found that Lewis and Br?nsted acid exist simultaneously on the the surface of BaAl_2O_4. The dynamic behavior of NO, NO_2 and O_2 on the surface of the sample as well as their interactions was analyzed under different reaction conditions. NO adsorption produces linear nitrites and bridged nitrites in the absence of O_2. NO_2 adsorption produces monodentate nitrates, bridged nitrates and ionic nitrates besides nitrites species. The produced nitrites will further react with O? surf, O~(2-)_(lattice) and O_2 to form nitrates, of which O ? surf owns the highest oxidative activity. Besides oxidizing NO into NO_2, O_2 oxidizes nitrites into nitrates, while this role is neglected by previous study. High oxygen content in the NO-containing flow and high temperature contribute to the formation of nitrates species.
(4) The reaction of soot with NO, NO_2 and O_2 was analyzed by LRS (Laser Raman Spectroscopy). It is found that amorphous material and SP2 structure of soot are destroyed after soot is pretreated with NO_x or O_2. High temperature favors the reaction of soot with NO_x and O_2, and the reaction activity is weakened in the order of NO+O_2> O_2 > NO at the same temperature.
(5) The reaction of soot and NO_x was analyzed in situ on the surface of BaAl_2O_4 by DRIFTS. The chemical configuration of NO_x in the redox is revealed. Nitrates species on the sample will react with C(O) preferentially due to their high oxidative ability, accompanied by the formation of CO_2, N_2 and N_2O. When these products desorb from the catalyst, the catalyst is regenerated. It is presumed that the reaction of nitrates with C(O) plays the main role in the redox and is regarded as the rate determing step. The presumption is consistent with the dynamic behavior of NO_x on BaAl_2O_4 during the TPR proceedure. The produced N_2O at high temperature will react with C(O) as an oxidant before it can be detected by DRIFTS easily. The conversion efficiency of NO_x into N_2 and N_2O directly depends on the quantity of nitrates on BaAl_2O_4, which is related to the performance of the catalyst in forming of nitrates.
(6) The molecule model of BaAl_2O_4, the intermediates of adsorbed NO_x, carbon-oxygen complexes and the reaction gases were constructed and optimized with DFT (Density Functional Theory) theory. The molecular orbital and the molecular orbital energy of the constructed model were calculated by EHMO (Extended Hückel Molecular Orbital) method. It is also revealed with frontier molecular orbital theory that nitrites will be oxidized into nitrates by O~-_(surf), O~(2-)_(lattice) or O_2, of which O~-_(surf) presents the highest oxidative activity by comparing the energy of HOMO (High Occupied Molecular Orbital) and LUMO (Low Unoccupied Molecular Orbital). The results of simulation calculation are in accordance with those of TPR and DRIFTS experiments.
本文将BaAl_2O_4用于催化NO_x和碳烟反应的研究,利用程序升温反应(TPR)技术评价了该催化剂在不同反应条件下催化同时去除碳烟和NO_x的活性。采用漫反射红外光谱和拉曼光谱,详细地研究了BaAl_2O_4催化碳烟和NO_x反应的微观机理。具体工作如下:
(1)制备了La_(0.8)K_(0.2)MnO_3和BaAl_2O_4催化剂,采用XRD、FT-IR、SEM等对制备的催化剂进行物理性能表征。利用TPR技术综合评价和比较了La_(0.8)K_(0.2)MnO_3和BaAl_2O_4的催化性能。结果表明,这两种催化剂催化碳烟和NO_x的反应均具有较高的活性,与非催化反应相比,碳烟的起燃温度和最大燃烧温度分别降低了175℃和240℃以上,NO_x转化为N_2的效率有了很大提高。
(2)分析了各种反应条件对催化同时去除碳烟和NO_x反应的影响。研究发现,反应气体的空速越低、碳烟和催化剂的质量比越高,越有利于催化反应进行;O_2的存在能促进碳烟和NO_x的催化反应,当模拟尾气中O_2含量由2%增加为5%时,碳烟的起燃温度和最大燃烧温度分别由330℃和405℃降低了大约30℃,在BaAl_2O_4催化作用下,NO_x转化为N_2和N_2O的效率分别由10.2%和3.5%升至12.1%和3.9%,在La_(0.8)K_(0.2)MnO_3催化作用下,由14.52%和6.63%降至11.02%和4.93%。
(3)采用漫反射红外光谱,用NH3作为探针分子,分析了BaAl_2O_4表面的酸性中心,发现BaAl_2O_4表面同时存在质子酸(Br?nsted酸)和非质子酸(Lewis酸)。分析了不同反应条件下NO、NO_2和O_2在BaAl_2O_4表面的动态行为以及它们之间的相互作用。研究表明,NO主要以线性和桥位亚硝酸盐的形态吸附在催化剂表面;除了形成亚硝酸盐外,NO_2在催化剂表面还直接形成了单齿硝酸盐、桥位硝酸盐和离子硝酸盐;生成的亚硝酸盐将继续与催化剂表面的吸附氧( O~-_(surf)和O 2 ?lattice)或O_2反应生成硝酸盐物种,其中O ? surf的氧化能力最强。研究发现,O_2除了将NO氧化为NO_2外,另外一个重要作用是将亚硝酸盐氧化为硝酸盐,O_2的浓度越高越有利于硝酸盐物种形成;高温也有利于形成硝酸盐物种,350℃时(碳烟和NO_x以较快速度反应),硝酸盐物种的形成与吸附时间关系不大。
(4)利用拉曼光谱(LRS)分析了碳烟与NO、NO_2及O_2的反应。发现碳烟用O_2或NO_x处理后,因与这些气体反应生成C(O)中间体,其非晶质碳渣和SP2碳结构被破坏。研究证明,高温有利于NO_x、O_2等与碳烟反应,相同温度下反应活性以NO+O_2 > O_2 > NO的顺序递减。
(5)采用漫反射红外光谱原位分析了碳烟和NO_x在催化剂BaAl_2O_4表面的详细反应过程。研究表明,催化剂表面的硝酸盐物种因具有较强的氧化能力,优先与碳烟的部分氧化产物(C(O))发生氧化还原反应,生成的最终产物CO_2、N_2和N_2O从催化剂表面脱附,催化剂获得再生;硝酸盐物种与C(O)中间体的反应在催化同时去除碳烟和NO_x的过程中起主要作用,是碳烟和NO_x反应的速控步骤,与程序升温反应结果及NO_x在催化剂表面动态行为的分析结果相符。研究发现,N_2O具有一定的氧化能力,高温下生成的N_2O还没有来得及被红外光谱检测到,就已和C(O)反应了。催化剂表面生成硝酸盐物种浓度的多少直接关系到NO_x转化为N_2的效率,这与催化剂吸附NO_x后生成硝酸盐物种的能力有关。
(6)利用密度泛函理论(DFT)构建并优化了BaAl_2O_4、C(O)中间体、NO_x在催化剂表面反应的中间产物及反应气体分子模型,利用推广的休克尔分子轨道法(EHMO)计算了各模型的分子轨道。结合分子轨道理论,比较分析了最高占据分子轨道和最低未占分子轨道的能级。结果表明催化剂表面O~-_(surf)的活性比O~(2-)_(lattice)强,其表面的亚硝酸盐物种被吸附氧( O~-_(surf)、O~(2-)_(lattice))或O_2氧化为硝酸盐物种。
Diesel engines have attracted much attention due to their high efficiency, economy and low CO_2 emissions. Correspondingly, with the main emissions of NO_x and soot, the related problems of environmental pollution are serious day by day. In cylinder, there exist trade-off effects for NO_x and soot control. Therefore, soot and NO_x cannot be reduced efficiently by improving combustion alone. Simultaneous removal of soot and NO_x is the optimal diesel engine after-treatment technique, in which NO_x is reduced into N_2 by soot, in return, soot is oxidized into CO_2 at the same time. To investigate the essence of the redox and find the crtical factors that promote and restrict the reaction, will be of great interesting in developing the technique for simultaneous removal of soot and NO_x.
In this study, the catalytic activity of BaAl_2O_4 in simultaneous removal of soot and NO_x was evaluated by Temperature Programmed Reaction (TPR) technique under various reaction conditions. Then, the micro mechanism for the catalytic reaction of soot with NO_x on the surface of BaAl_2O_4 was investigated by DRIFTS (Diffuse Reflectance Infrared Fourier Transform Spectroscopy) and LRS (Laser Raman Spectroscopy). The detailed research is summarized as following:
(1) La_(0.8)K_(0.2)MnO_3 and BaAl_2O_4 were prepared and characterized by XRD, FT-IR and SEM. The catalytical activity of La_(0.8)K_(0.2)MnO_3 and BaAl_2O_4 was evaluated systematically by TPR. These two catalysts all exhibit high catalytic activity in simultaneous removal of soot and NO_x, for exampe, Tig and Tm of soot decrease by more than 175℃and 240℃respectively, and the conversion of NO_x into N_2 is improved markedly.
(2) The reaction of soot with NO_x was studied under various conditions. It is found that low GHSV (Gas Hourly Space Velocity) and high mass ratio of soot to catalyst are benefitial to the redox. Oxygen may promote the catalytic reaction of soot with NO_x. Both Tig and Tm of soot is decreased by ca. 30℃by increasing O_2 content from 2% to 5%. It is interesting that O_2 ehances the maximum conversion efficiencies of NO_x into N_2 and N_2O with the catalysis of BaAl_2O_4, however, the conversion efficiencies were depressed by changing BaAl_2O_4 to La_(0.8)K_(0.2)MnO_3.
(3) Adsorption of ammonia was studied in order to obtain informaion on the surface acidity (Lewis and Br?nsted) of BaAl_2O_4 by DRIFTS. It is found that Lewis and Br?nsted acid exist simultaneously on the the surface of BaAl_2O_4. The dynamic behavior of NO, NO_2 and O_2 on the surface of the sample as well as their interactions was analyzed under different reaction conditions. NO adsorption produces linear nitrites and bridged nitrites in the absence of O_2. NO_2 adsorption produces monodentate nitrates, bridged nitrates and ionic nitrates besides nitrites species. The produced nitrites will further react with O? surf, O~(2-)_(lattice) and O_2 to form nitrates, of which O ? surf owns the highest oxidative activity. Besides oxidizing NO into NO_2, O_2 oxidizes nitrites into nitrates, while this role is neglected by previous study. High oxygen content in the NO-containing flow and high temperature contribute to the formation of nitrates species.
(4) The reaction of soot with NO, NO_2 and O_2 was analyzed by LRS (Laser Raman Spectroscopy). It is found that amorphous material and SP2 structure of soot are destroyed after soot is pretreated with NO_x or O_2. High temperature favors the reaction of soot with NO_x and O_2, and the reaction activity is weakened in the order of NO+O_2> O_2 > NO at the same temperature.
(5) The reaction of soot and NO_x was analyzed in situ on the surface of BaAl_2O_4 by DRIFTS. The chemical configuration of NO_x in the redox is revealed. Nitrates species on the sample will react with C(O) preferentially due to their high oxidative ability, accompanied by the formation of CO_2, N_2 and N_2O. When these products desorb from the catalyst, the catalyst is regenerated. It is presumed that the reaction of nitrates with C(O) plays the main role in the redox and is regarded as the rate determing step. The presumption is consistent with the dynamic behavior of NO_x on BaAl_2O_4 during the TPR proceedure. The produced N_2O at high temperature will react with C(O) as an oxidant before it can be detected by DRIFTS easily. The conversion efficiency of NO_x into N_2 and N_2O directly depends on the quantity of nitrates on BaAl_2O_4, which is related to the performance of the catalyst in forming of nitrates.
(6) The molecule model of BaAl_2O_4, the intermediates of adsorbed NO_x, carbon-oxygen complexes and the reaction gases were constructed and optimized with DFT (Density Functional Theory) theory. The molecular orbital and the molecular orbital energy of the constructed model were calculated by EHMO (Extended Hückel Molecular Orbital) method. It is also revealed with frontier molecular orbital theory that nitrites will be oxidized into nitrates by O~-_(surf), O~(2-)_(lattice) or O_2, of which O~-_(surf) presents the highest oxidative activity by comparing the energy of HOMO (High Occupied Molecular Orbital) and LUMO (Low Unoccupied Molecular Orbital). The results of simulation calculation are in accordance with those of TPR and DRIFTS experiments.
引文
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