铈铁基复合氧化物的制备及其催化碳烟燃烧性能研究
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摘要
柴油机凭借其良好的动力性、经济性、耐久性和低二氧化碳排放量等优点而日益受到重视。然而柴油机排放的碳烟对环境造成的污染也日益严重,它不仅对视觉和嗅觉产生不良影响,而且碳烟上常常粘附S02及致癌物质,对环境和人体的危害非常大。
由于碳烟的热氧化温度高达600℃以上,而柴油车的正常排气温度为150～450℃,无法直接氧化而除去。使用与碳烟低温燃烧催化剂相结合的过滤器收集碳烟颗粒,同时使碳烟颗粒被催化氧化为CO2而除去,是减少碳烟污染最直接有效的方法。在过滤器中使用的催化剂要求具有良好的催化活性和热稳定性。
本研究首先采用水热合成法和简单混合法制备了系列Ce1-xFexO2 (x=0,0.1,0.2, 0.3,0.4,0.5,0.6,0.7,0.8,0.9和1)复合氧化物碳烟燃烧催化剂,利用XRD、BET、Raman和H2-TPR等技术对催化剂进行了表征,采用程序升温氧化反应(TPO)技术评价了它们的碳烟燃烧催化活性,探讨了催化剂的表面状态和体相结构与催化性能的相关性,找出影响催化剂活性的关键因素。结果表明,部分Fe3+进入Ce02晶格中形成了铈铁固溶体,大量游离的Fe2O3高度分散在催化剂表面。固溶体形成而导致的氧空位能吸附活性氧,而表面高度分散的氧化铁既具有良好的氧化还原性能,且可以促进反应气氛中氧在催化剂表面的活化,还能促进Ce02晶格氧的活化,提高Ce02晶格氧的溢出速率,二者协同作用才能使催化剂显示出最好的催化活性。在系列Ce1-xFexO2复合氧化物中,Ce0.8Fe0.2O2和Ce0.4Fe0.6O2两个样品显示了最好的碳烟燃烧催化活性,其催化碳烟的起燃温度(Τi)和峰顶温度(Τp)较低,分别为262和314℃及255和314℃。历经长时间高温老化后,其催化活性均有所降低,其Τi和Τp分别增加为292和392℃及291和382℃。
基于Ce1-XFeX02复合氧化物虽然具有较好的催化活性,但是其热稳定性有待进一步提高,本论文还研究了采用水热合成法制备的锆掺杂的Ce0.5Fe0.5-xZrxO2(X=0,0.05, 0.10,0.15,0.20,0.25,0.30,0.35,0.40,0.45)复合氧化物碳烟燃烧催化剂。其XRD、BET、Raman和H2-TPR等表征和TPO活性评价结果表明,Ce1-xFexO2复合氧化物中掺杂Zr02不仅能提高固溶体的形成量,从而进一步提高碳烟燃烧催化活性,而且还能提高材料的抗烧结能力,稳定材料的结构,可以抑制材料晶粒的增长和固溶体的消失。较Ce1-xFexO2二元复合氧化物而言,Ce0.5Fe0.5-xZrxO2三元复合氧化物显示了更高的催化活性和热稳定性,其中活性最好的Ce0.5Fe0.30Zr0.20O2样品,其催化碳烟的Τi和Τp降低为251℃和310℃,△Τ仅为59℃。长时间高温老化后,其仍表现出较高的催化活性,Τi和Τp分别为273和361℃。
考虑到制备方法对催化剂结构和性能的影响很大,本研究最终以筛选出的活性最好的Ce0.5Fe0.30Zr0.20O2复合氧化物为研究目标,考虑了水热合成法、机械混合法、浸渍法、模板法、溶胶凝胶法及共沉淀法等六种不同制备方法对其碳烟燃烧催化活性的影响,结果显示,采用水热合成法制备的催化剂具有最好的催化活性和热稳定性。
Nowadays, diesel engines have been paid more and more attention due to the strong power, high economy, good durability and low carbon dioxide emission. However, the soot emissions from diesel engins also lead to serious environmental problems. The small size of diesel soot particles may be linked to a number of health problems by its ability to penetrate the body through the respiratory system.
The non-catalytic ignition temperature of soot oxidation generally exceeds 600℃, while the normal temperature of typical diesel exhaust temperatures is 150～450℃. The soot can not be removed by direct oxidation. The combination of diesel particulate filter (DPF) and oxidation catalysts appears to be the most plausible after-treatment technique to eliminate soot particles. The catalysts used in a catalytic DPF should display good activity in the temperature range of diesel exhaust, and good thermal stability under practical working conditions.
In this paper, a series of Ce1-xFexO2(x=0,0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9 and 1) mixed oxides with different Ce/Fe molar ratios were prepared via hydrothermal method. The prepared catalysts were characterized by X-ray diffraction (XRD), BET specific surface area (BET), Raman spectroscopy (Raman) and H2 temperature-programmed reduction (H2-TPR) techniques. The performances of the catalysts in the soot oxidation were evaluated by temperature-programmed oxidation (TPO). We also investigated the correlation of catalysts surface states and bulk structures with catalytic properties, and find out the key factors affecting catalytic activity. The results showed that the strong synergetic effect between the Ce-Fe solid solutions and some highly dispersed Fe2O3, made the catalysts more active. The oxygen vacancies from the formation of Ce-Fe olid solutions can absorbe and activate oxygen, while the well dispersed surface Fe2O3 not only had a good reduction behaviour, but also can promote the activation of CeO2 lattice oxygen to improve the release rate of the lattice oxygen in CeO2. Among the series of Ce1-xFexO2 mixed oxides, the Ce0.8Fe0.2O2 and Ce0.4Fe0.6O2 two samples showed the best catalytic activity for soot combustion, and had the lowest Ti(262℃and 255℃, respectively, ignition temperature of soot oxidation) and Tp (both 314℃, temperature of maximum evolution of C02). Even after aging for long periods at high temperature, the Ti and Tp values for Ce0.8Fe0.2O2 and Ce0.4Fe0.6O2 samples were still relatively low. The Ti were 292 and 291℃, and Tp were 392 and 382℃, respectively.
Ce1-xFexO2 mixed oxides had good catalytic activity, but their thermal stability should be further improved. So, in this paper, a series of zirconium doped Ce0.5Fe0.5-xZrxO2(X=0, 0.05,0.10,0.15,0.20,0.25,0.30,0.35,0.40 and 0.45) mixed oxides were also prepared via hydrothermal method. The characterization of XRD, BET, Raman and H2-TPR, and the TPO results showed that introduction of ZrO2 into the Ce1-xFexO2 mixed oxides can promote the formation of solid solutions to improve the catalytic activity for soot combustion. Moreover, it also results in the ability to improve thermal stability of the materials. Remarkably, ZrO2 can inhibit the growth of CeO2 crystallite size and the disappearance of solid solutions. Totally, Ce0.5Fe0.5-xZrxO2 ternary mixed oxides showed higher catalytic activity than Ce1-xFexO2 binary mixed oxides. Among the series of Ce0.5Fe0.5-xZrxO2 mixed oxides, the Ce0.5Fe0.30Zr0.20O2 catalyst showed the best catalytic activity for soot combustion, and had the lowest Ti (251℃) and Tp (310℃). Even after aging for long periods at high temperature, the Ti and Tp values for Ce0.5Fe0.30Zr0.20O2 sample were still relatively low. The Ti was 273℃, and Tp was 361℃, indicating high thermal stability.
In this study, we finally chose the Ce0.5Fe0.30Zr0.20O2 sample which has the best catalytic activity as the research object, and prepared it via hydrothermal, physical mixture, impregnation, template, citric acid sol-gel and co-precipitation methods. The results showed that catalysts preparation methods have a great influence on structure and properties of catalysts. The catalyst prepared by hydrothermal method displayed the best catalytic activity and thermal stability.
由于碳烟的热氧化温度高达600℃以上,而柴油车的正常排气温度为150～450℃,无法直接氧化而除去。使用与碳烟低温燃烧催化剂相结合的过滤器收集碳烟颗粒,同时使碳烟颗粒被催化氧化为CO2而除去,是减少碳烟污染最直接有效的方法。在过滤器中使用的催化剂要求具有良好的催化活性和热稳定性。
本研究首先采用水热合成法和简单混合法制备了系列Ce1-xFexO2 (x=0,0.1,0.2, 0.3,0.4,0.5,0.6,0.7,0.8,0.9和1)复合氧化物碳烟燃烧催化剂,利用XRD、BET、Raman和H2-TPR等技术对催化剂进行了表征,采用程序升温氧化反应(TPO)技术评价了它们的碳烟燃烧催化活性,探讨了催化剂的表面状态和体相结构与催化性能的相关性,找出影响催化剂活性的关键因素。结果表明,部分Fe3+进入Ce02晶格中形成了铈铁固溶体,大量游离的Fe2O3高度分散在催化剂表面。固溶体形成而导致的氧空位能吸附活性氧,而表面高度分散的氧化铁既具有良好的氧化还原性能,且可以促进反应气氛中氧在催化剂表面的活化,还能促进Ce02晶格氧的活化,提高Ce02晶格氧的溢出速率,二者协同作用才能使催化剂显示出最好的催化活性。在系列Ce1-xFexO2复合氧化物中,Ce0.8Fe0.2O2和Ce0.4Fe0.6O2两个样品显示了最好的碳烟燃烧催化活性,其催化碳烟的起燃温度(Τi)和峰顶温度(Τp)较低,分别为262和314℃及255和314℃。历经长时间高温老化后,其催化活性均有所降低,其Τi和Τp分别增加为292和392℃及291和382℃。
基于Ce1-XFeX02复合氧化物虽然具有较好的催化活性,但是其热稳定性有待进一步提高,本论文还研究了采用水热合成法制备的锆掺杂的Ce0.5Fe0.5-xZrxO2(X=0,0.05, 0.10,0.15,0.20,0.25,0.30,0.35,0.40,0.45)复合氧化物碳烟燃烧催化剂。其XRD、BET、Raman和H2-TPR等表征和TPO活性评价结果表明,Ce1-xFexO2复合氧化物中掺杂Zr02不仅能提高固溶体的形成量,从而进一步提高碳烟燃烧催化活性,而且还能提高材料的抗烧结能力,稳定材料的结构,可以抑制材料晶粒的增长和固溶体的消失。较Ce1-xFexO2二元复合氧化物而言,Ce0.5Fe0.5-xZrxO2三元复合氧化物显示了更高的催化活性和热稳定性,其中活性最好的Ce0.5Fe0.30Zr0.20O2样品,其催化碳烟的Τi和Τp降低为251℃和310℃,△Τ仅为59℃。长时间高温老化后,其仍表现出较高的催化活性,Τi和Τp分别为273和361℃。
考虑到制备方法对催化剂结构和性能的影响很大,本研究最终以筛选出的活性最好的Ce0.5Fe0.30Zr0.20O2复合氧化物为研究目标,考虑了水热合成法、机械混合法、浸渍法、模板法、溶胶凝胶法及共沉淀法等六种不同制备方法对其碳烟燃烧催化活性的影响,结果显示,采用水热合成法制备的催化剂具有最好的催化活性和热稳定性。
Nowadays, diesel engines have been paid more and more attention due to the strong power, high economy, good durability and low carbon dioxide emission. However, the soot emissions from diesel engins also lead to serious environmental problems. The small size of diesel soot particles may be linked to a number of health problems by its ability to penetrate the body through the respiratory system.
The non-catalytic ignition temperature of soot oxidation generally exceeds 600℃, while the normal temperature of typical diesel exhaust temperatures is 150～450℃. The soot can not be removed by direct oxidation. The combination of diesel particulate filter (DPF) and oxidation catalysts appears to be the most plausible after-treatment technique to eliminate soot particles. The catalysts used in a catalytic DPF should display good activity in the temperature range of diesel exhaust, and good thermal stability under practical working conditions.
In this paper, a series of Ce1-xFexO2(x=0,0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9 and 1) mixed oxides with different Ce/Fe molar ratios were prepared via hydrothermal method. The prepared catalysts were characterized by X-ray diffraction (XRD), BET specific surface area (BET), Raman spectroscopy (Raman) and H2 temperature-programmed reduction (H2-TPR) techniques. The performances of the catalysts in the soot oxidation were evaluated by temperature-programmed oxidation (TPO). We also investigated the correlation of catalysts surface states and bulk structures with catalytic properties, and find out the key factors affecting catalytic activity. The results showed that the strong synergetic effect between the Ce-Fe solid solutions and some highly dispersed Fe2O3, made the catalysts more active. The oxygen vacancies from the formation of Ce-Fe olid solutions can absorbe and activate oxygen, while the well dispersed surface Fe2O3 not only had a good reduction behaviour, but also can promote the activation of CeO2 lattice oxygen to improve the release rate of the lattice oxygen in CeO2. Among the series of Ce1-xFexO2 mixed oxides, the Ce0.8Fe0.2O2 and Ce0.4Fe0.6O2 two samples showed the best catalytic activity for soot combustion, and had the lowest Ti(262℃and 255℃, respectively, ignition temperature of soot oxidation) and Tp (both 314℃, temperature of maximum evolution of C02). Even after aging for long periods at high temperature, the Ti and Tp values for Ce0.8Fe0.2O2 and Ce0.4Fe0.6O2 samples were still relatively low. The Ti were 292 and 291℃, and Tp were 392 and 382℃, respectively.
Ce1-xFexO2 mixed oxides had good catalytic activity, but their thermal stability should be further improved. So, in this paper, a series of zirconium doped Ce0.5Fe0.5-xZrxO2(X=0, 0.05,0.10,0.15,0.20,0.25,0.30,0.35,0.40 and 0.45) mixed oxides were also prepared via hydrothermal method. The characterization of XRD, BET, Raman and H2-TPR, and the TPO results showed that introduction of ZrO2 into the Ce1-xFexO2 mixed oxides can promote the formation of solid solutions to improve the catalytic activity for soot combustion. Moreover, it also results in the ability to improve thermal stability of the materials. Remarkably, ZrO2 can inhibit the growth of CeO2 crystallite size and the disappearance of solid solutions. Totally, Ce0.5Fe0.5-xZrxO2 ternary mixed oxides showed higher catalytic activity than Ce1-xFexO2 binary mixed oxides. Among the series of Ce0.5Fe0.5-xZrxO2 mixed oxides, the Ce0.5Fe0.30Zr0.20O2 catalyst showed the best catalytic activity for soot combustion, and had the lowest Ti (251℃) and Tp (310℃). Even after aging for long periods at high temperature, the Ti and Tp values for Ce0.5Fe0.30Zr0.20O2 sample were still relatively low. The Ti was 273℃, and Tp was 361℃, indicating high thermal stability.
In this study, we finally chose the Ce0.5Fe0.30Zr0.20O2 sample which has the best catalytic activity as the research object, and prepared it via hydrothermal, physical mixture, impregnation, template, citric acid sol-gel and co-precipitation methods. The results showed that catalysts preparation methods have a great influence on structure and properties of catalysts. The catalyst prepared by hydrothermal method displayed the best catalytic activity and thermal stability.
引文
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