低温等离子体催化氧化甲烷合成甲醇的应用基础研究
摘要
随着世界性石油资源的日益短缺,开发以天然气或甲烷水合物(可燃冰)为原料替代石油资源,并原位转化为有机含氧化合物成为重要的研究课题。低温等离子体技术可在温和反应条件下实现甲烷的活化,若将其与催化技术相结合,有望形成一种既具强活化能力、又具高选择性的等离子体-催化协同活化新技术。本文主要开展了等离子体-催化协同作用于甲烷／空气选择性氧化合成甲醇的应用基础研究。
首先,利用介质阻挡放电等离子体实现常温常压条件下甲烷直接转化合成甲醇。考察了电源输入功率、放电频率、放电间隙、气体停留时间、气体组分对甲烷转化率及甲醇产率的影响,并对参数进行优化；同时,考察了放电体系添加惰性气体Ar或N2对反应的影响,研究表明惰性气体的加入有利于提高放电强度和放电效率,获得更高的甲烷转化率及甲醇产率；通过等离子体发射光谱原位诊断证实甲烷选择性氧化合成甲醇主要通过自由基反应得以实现。
其次,将催化剂引入等离子体反应体系,构建后置式及内置式等离子体-催化反应体系。针对后置式体系筛选出单组分催化剂Fe2O3/CP,当催化温度仅为150℃时,甲醇选择性达到10.66%,较单纯等离子体提高了35.1%。当添加助剂CuO构成复合催化剂,在相同催化温度下可将甲醇选择性提高至11.33%；对于内置式反应体系,放电区域填充Fe2O3-CuO/γ-Al2O3催化剂既有助于增强电场强度,又可造成催化剂表面局部反应分子和活性自由基的富集,提高反应效率。研究表明,催化剂在后置式体系中具有更好的抗积碳性能以及反应稳定性。通过对不同体系各类瞬时基团物质及稳态物质的分析探索了甲醇合成的主要途径。
最后,研究了两种Ar等离子体预处理方法对Fe2O3-CuO/γ-Al2O3催化剂性能的影响,对比发现催化剂焙烧前等离子体改性能有效提高活性组分的分散性,加强金属氧化物与载体间的相互作用,显著提高催化剂的抗积碳性能。
With the lack of petroleum resources in the world, the development of natural gas and methane hydrate (flammable ice) utilization as the feedstock, instead of crude oil, for the in-situ production of oxygenates has been extensively studied. Cold plasma offers a unique way to excite stable methane molecule under mild conditions. High conversion and selectivity are expected to be obtained by exploiting the inherent synergetic potential of plasma through combination with heterogeneous catalysts. In our study, methane-air partial oxidation to methanol (MPOM) was investigated using plasma-catalysis hybrid system.
Firstly, MPOM through a dielectric barrier discharge (DBD) plasma reaction was performed at ambient temperature and atmospheric pressure. The effects of input power, discharge frequency, discharge gap distance, residence time, and CH4/air ratio on CH4 conversion and CH3OH yield were studied, and those parameters were optimized. Moreover, the discharge intensity and the reaction efficiency were greatly enhanced with the addition of inert gases such as argon and nitrogen. It was found from optical emission spectrometry that free radical reactions were of importance for initiating methanol synthesis.
Secondly, combination of heterogeneous catalysts with non-thermal plasma was operated in two configurations:post-plasma catalysis (PPC) or in-plasma catalysis (IPC). In the former case, Fe2O3-based catalyst showed the best catalytic activity and high stability in the reaction. The CH3OH selectivity of 10.66%was obtained over Fe2O3/CP at the rather low catalyst temperature (150℃), which was 35.1% higher than that of non-catalytic system. Addition of the CuO promoter to Fe2O3/CP facilitated selective methane oxidation. At the same catalyst temperature, the CH3OH selectivity achieved with the Fe2O3-CuO/CP catalyst was at 11.33%. For the IPC configuration, the average electric field in a packed-bed reactor would be enhanced compared with the non-packed plasma reactor. Furthermore, the reaction efficiency over the Fe2O3-CuO/γ-Al2O3 catalyst was improved due to the enrichment of reactants and radicals on the catalyst surface. However, the alumina based catalyst exhibited superior anti-deactivation ability and reaction stability in the PPC process compared to the IPC process. In addition, the main pathways to methanol synthesis in the different processes were investigated based on the behavior of both short-and long-lived species.
Finally, the Fe203-Cu0/y-Al203 catalyst was modified by Ar plasma treatment using two methods. Modification of catalyst before calcination was preferred because it could improve the dispersion of active species and enhance the metal-support interaction, which led to high catalytic activity and excellent resistance to carbon formation.
首先,利用介质阻挡放电等离子体实现常温常压条件下甲烷直接转化合成甲醇。考察了电源输入功率、放电频率、放电间隙、气体停留时间、气体组分对甲烷转化率及甲醇产率的影响,并对参数进行优化；同时,考察了放电体系添加惰性气体Ar或N2对反应的影响,研究表明惰性气体的加入有利于提高放电强度和放电效率,获得更高的甲烷转化率及甲醇产率；通过等离子体发射光谱原位诊断证实甲烷选择性氧化合成甲醇主要通过自由基反应得以实现。
其次,将催化剂引入等离子体反应体系,构建后置式及内置式等离子体-催化反应体系。针对后置式体系筛选出单组分催化剂Fe2O3/CP,当催化温度仅为150℃时,甲醇选择性达到10.66%,较单纯等离子体提高了35.1%。当添加助剂CuO构成复合催化剂,在相同催化温度下可将甲醇选择性提高至11.33%；对于内置式反应体系,放电区域填充Fe2O3-CuO/γ-Al2O3催化剂既有助于增强电场强度,又可造成催化剂表面局部反应分子和活性自由基的富集,提高反应效率。研究表明,催化剂在后置式体系中具有更好的抗积碳性能以及反应稳定性。通过对不同体系各类瞬时基团物质及稳态物质的分析探索了甲醇合成的主要途径。
最后,研究了两种Ar等离子体预处理方法对Fe2O3-CuO/γ-Al2O3催化剂性能的影响,对比发现催化剂焙烧前等离子体改性能有效提高活性组分的分散性,加强金属氧化物与载体间的相互作用,显著提高催化剂的抗积碳性能。
With the lack of petroleum resources in the world, the development of natural gas and methane hydrate (flammable ice) utilization as the feedstock, instead of crude oil, for the in-situ production of oxygenates has been extensively studied. Cold plasma offers a unique way to excite stable methane molecule under mild conditions. High conversion and selectivity are expected to be obtained by exploiting the inherent synergetic potential of plasma through combination with heterogeneous catalysts. In our study, methane-air partial oxidation to methanol (MPOM) was investigated using plasma-catalysis hybrid system.
Firstly, MPOM through a dielectric barrier discharge (DBD) plasma reaction was performed at ambient temperature and atmospheric pressure. The effects of input power, discharge frequency, discharge gap distance, residence time, and CH4/air ratio on CH4 conversion and CH3OH yield were studied, and those parameters were optimized. Moreover, the discharge intensity and the reaction efficiency were greatly enhanced with the addition of inert gases such as argon and nitrogen. It was found from optical emission spectrometry that free radical reactions were of importance for initiating methanol synthesis.
Secondly, combination of heterogeneous catalysts with non-thermal plasma was operated in two configurations:post-plasma catalysis (PPC) or in-plasma catalysis (IPC). In the former case, Fe2O3-based catalyst showed the best catalytic activity and high stability in the reaction. The CH3OH selectivity of 10.66%was obtained over Fe2O3/CP at the rather low catalyst temperature (150℃), which was 35.1% higher than that of non-catalytic system. Addition of the CuO promoter to Fe2O3/CP facilitated selective methane oxidation. At the same catalyst temperature, the CH3OH selectivity achieved with the Fe2O3-CuO/CP catalyst was at 11.33%. For the IPC configuration, the average electric field in a packed-bed reactor would be enhanced compared with the non-packed plasma reactor. Furthermore, the reaction efficiency over the Fe2O3-CuO/γ-Al2O3 catalyst was improved due to the enrichment of reactants and radicals on the catalyst surface. However, the alumina based catalyst exhibited superior anti-deactivation ability and reaction stability in the PPC process compared to the IPC process. In addition, the main pathways to methanol synthesis in the different processes were investigated based on the behavior of both short-and long-lived species.
Finally, the Fe203-Cu0/y-Al203 catalyst was modified by Ar plasma treatment using two methods. Modification of catalyst before calcination was preferred because it could improve the dispersion of active species and enhance the metal-support interaction, which led to high catalytic activity and excellent resistance to carbon formation.
引文
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