介孔过渡金属氧化物及多孔负载型氧化物催化活化甲烷的研究
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摘要
随着世界经济的飞速发展,石油和煤等能源、资源已经面临着日益短缺的问题,以甲烷为主要成分的C1资源已经成为人们争相开发和利用的资源,这也是世界各国改善环境和维持可持续发展的最佳选择。然而,甲烷是自然界中最稳定的碳氢分子,其转化研究已经历经百年,除已实现工业化的间接转化法外,直接转化法进展缓慢,已研究过的催化剂多达数千种以上,所使用的元素几乎包括了除零族元素以外的全部元素,但仍有诸多难以逾越的障碍。深入系统的研究和探索甲烷转化新途径,揭示甲烷转化的内在规律,对解决目前人类面临的能源、资源和环境等问题有着极为重要的理论和实用意义。
介孔过渡金属氧化物除具有过渡金属氧化物的组成和通常的物理化学性质外,由于介孔的存在,它们还呈现出大孔径,大比表面积,丰富的表面结构,纳米粒子属性和微型反应器的功能。此外,它们的孔道结构和组成是可调节的,具有可设计的特性。与已知的甲烷转化催化剂相比,确有许多无以伦比之处。因此,可以毫无怀疑的认为,稳定的介孔过渡金属氧化物材料为寻找能够在温和条件下打开甲烷分子中的C-H键,建立C-C、C-O等新键的新型高效催化剂提供了一个难得的机会。基于此,本文以介孔过渡金属氧化物为催化剂,开展了一系列催化活化甲烷转化的研究工作,主要内容如下：
(1)以离子液体和苯醚为媒介、乙酰丙酮铁为铁源、离子液体并参与形貌控制制备出新颖的介孔α-Fe203材料,通过扫描电镜(SEM)表征发现其具有花瓣状结构,每个纳米棒长约567nm,宽约52nm；进一步通过透射电镜(TEM)可以在棒体上观察到有明显的介孔孔道,孔径为3.2nm；N2吸附脱附曲线(BET)分析得该新颖介孔材料的比表面为55.1m2·g-1。同时将其用于催化活化甲烷,实验结果发现在3atm,CH4/02=3,GHSV=4800ml/g.h条件下,130℃的低温下就可以打破甲烷分子中的C-H键,生成含C-O键产物。这比文献上报道的纳米α-Fe203活化甲烷的最低温度降低了220℃,比目前报道的甲烷热转化的最低活化温度低70C。经研究证明此介孔α-Fe203材料中存在三种活性氧,其中对应于可在130℃时活化甲烷的是表面吸附氧。
(2)通过改进的硬模板法批量制备了介孔氧化物Co304及其掺杂5%其它过渡金属和稀土金属Ce氧化物材料,并将其用于活化甲烷,发现纯的介孔Co3O4可以在145℃时活化甲烷,在以5%Cr-Co3O4为催化剂时甲烷的最低活化温度也为130℃,这比目前文献中以Co3O4为活性组分的材料活化甲烷的最低温度要低71℃,在低温下CO的选择性高于90%,并有长寿命,其有望成为低温下甲烷重整制合成气的催化剂。通过XPS测试发现该系列催化剂上含有两种活性氧即表面吸附氧和晶格氧,该系列催化剂中表面吸附氧的含量大于介孔α-Fe2O3,这也是该系列催化剂在低温下较α-Fe2O3具有长寿命的催化活性的原因。
(3)利用改进并放大的硬模板法批量制备了介孔NiO及其掺杂过渡金属和稀土金属Ce氧化物系列催化剂并将其用于甲烷的活化,结果证明纯介孔NiO可以在210℃的低温下活化甲烷,以5%Fe-NiO的材料为催化剂时,发现其也可以在130℃的低温下活化甲烷,这比文献中报道的以NiO为活性的催化剂活化甲烷最低温度要低191℃,该系列催化剂在反应温度升高到250℃时,CO2的选择性始终高于80%,可见,该系列材料有可能发展为一种低温下催化燃烧甲烷的优秀催化剂。
(4)通过改进的酸碱自调节法制备了介孔TiO2以及负载过渡和稀土金属Ce氧化物系列材料,并将其用于催化活化甲烷,实验结果显示介孔TiO2催化剂可以在210℃活化甲烷,比块体TiO2对甲烷的活化温度低290℃。当以5%Ce-TiO2为催化剂时甲烷的活化温度可以低至140℃,这也比文献报道的最好的同类TiO2催化剂活化甲烷的最低温度降低了360℃,同时比目前报道的甲烷热转化的最低温度降低了60℃。掺杂少量铁系(Fe、Co和Ni)可以使甲烷的活化温度降低到160℃和180℃。XPS测试结果证实该类催化剂低温催化活性应归因于表面吸附氧,高温时主要是晶格氧起催化氧化作用。
(5)为了进一步深入理解孔及其孔结构在催化转化甲烷中的作用,本文还利用浸渍法制备了无孔的石英砂、介孔分子筛KIT-6、微孔分子筛HZSM-5负载过渡金属氧化物及稀土金属Ln(Ln=La、Ce和Gd)的催化剂,并分别研究了它们对甲烷的催化活化行为。发现无孔的石英砂活化甲烷生成含C-O键产物的温度最高,为670℃；KIT-6分子筛上含C-O键的产物生成温度为550℃,纯的HZSM-5载体在350℃活化甲烷,生成含C-O键的产物(CO和CO2),微孔HZSM-5负载的稀土改性材料显示出优异的催化活性。微孔的HZSM-5负载双金属Ln和Zn的材料上最低在270℃活化甲烷生成含C-O键产物,介孔分子筛负载5%的Fe材料却可以在200℃时活化甲烷,这说明介孔分子筛负载的氧化物活化甲烷能力大于微孔分子筛负载的氧化物活化甲烷的活性,这证明了适宜的孔大小和结构因负载稀土改性的金属氧化物后可以创造出优异催化活性,负载了金属氧化物微孔分子筛催化剂的活性低于介孔分子筛负载氧化物的活性,是因为微孔分子筛催化剂中适宜的孔及其结构因负载而减少的缘故。这三类载体及负载金属氧化物材料活化甲烷生成C-C键产物的能力与生成C-O键产物能力有些不同。微孔HZSM-5负载金属氧化物材料活化甲烷生成C-C键产物的能力最强,可以在550℃时活化甲烷生成C-C键产物。有利于芳构化产物的生成。特别是在无氧、乙烯存在条件下该类催化剂可以显著降低甲烷的活化温度,使得甲烷在450℃的低温下生成芳烃,甲烷的最高转化率可以达到37.3%,这比文献上报道的获得相近甲烷转化率时的反应温度降低了150℃。
上述研究结果充分说明在过渡金属氧化物中的孔及其结构和组成对催化甲烷转化有非常重要的作用,能显著的提高低温催化活性。介孔过渡金属氧化物是一类很有希望的低温高效催化转化甲烷的材料。对其深入系统的研究不仅能深刻地揭示出甲烷催化转化的内在本质,丰富催化化学的基础理论知识,而且还可能开发出低耗高效清洁催化转化甲烷的实用技术。
At current usage, worldwide reserves of petroleum and coal are projected to only last for a few decades. This situation is a serious problem on a global level.Developin g efficient strategies for the selective activation and transformation of methane as the most abundant feedstock for organic chemicals to value-added chemicals or liquid fuels would provide a promising alternative for easing up the coal and oil-demanding situation during the high-growth process of the economic and the rapid development of science and technology. However, the bonds to be broken are thermodynamically strong and kinetically inert. Construction of the more sophisticated value-added architectures via C-H bond activation in methane is a highly difficult task.
Although methane conversion has been investigated for one hundred years, only indirect conversion method has realized in industrial scale. The development of direct conversion of methane to useful chemicals by activating C-H bonds still remains a difficult task despite thousands of Catalysts and almost all elements except group zero elements in periodical table used in the past decades.The investigation for new ways of methane conversion and the inherent laws of methane conversion is very important to solve the energy, resources and environmental problems in the sustainable development of humane society.
In addition to with the composition of the transition metal oxides and the usual physical and chemical properties, mesoporous transition metal oxides possess a large aperture, large surface area, diverse surface structures, nanoparticle properties and function of micro-reactor. Moreover, their pore structure and composition can be tunable. By comparison with the known methane conversion catalyst, mesoporous transition metal oxide materials exhibit a lot of unusual characters and may provide a great deal of opportunity to find the excellent catalysts for breaking the C-H bonds to establish the new C-C, C-O. In this thesis, the research effort has focused on the preparation of mesoporous transition metal oxide and activation of methane by mesoporous transition metal oxide as catalyst. The main points of the thesis are as follows.
(1) A novel mesoporous α-Fe2O3material have been prepared by using the ionic liquid as the media, acetylacetone iron as the iron source and diphenyl ether as the morphology control reagent. It is found that the material has a flower-like structure by SEM, each nanorod of about567nm, the width of52nm. It is also characterized by TEM, and found there are mesopores in the the nanorod, the pore diameter is3.2nm. The BET showed that the novel material has a specific surface area of55.1m2·g-1. Carried out the catalytic activation of methane experiments, at3atm, CH4/O2=3, GHSV=4800ml/g-h, the results show the lowest temperature of breaking C-H bond of methane is130℃over this Mesoporous α-Fe2O3nanorods catalyst. The reason is mesoporous α-Fe2O3surface adsorption of oxygen and interstitial oxygen plays an important part in the methane activation
(2) Three-dimensional mesoporous CO3O4and doped with other transition metal and rare earth metal (Ce) material have been prepared by using improved hard template methods. Activation methane experiment were carried out over these CO3O4materials, and found mesoporous Co3O4catalyst can activate methane at145℃, compared to bulk Co3O4,the activation temperature is lower30℃, which is lower71℃than the lowest temperature in the literature. While using the mesoporous Co3O4doped with chromium(5%Cr-Co3O4) it can help break C-H bond of methane and build C-O bond at130℃, the selectivity of CO is higher than90%, and the catalyst has long life. It is promising that the material can be used as syngas catalyst.
(3) Mesoporous NiO and doped with other transition metal and rare earth metal (Ce) material have been prepared by using improved hard template methods. Activation methane experiment were carried out over these NiO materials, and found mesoporous NiO catalyst can activate methane at210℃, compared to bulk NiO, the activation temperature is lower70℃, While using the mesoporous NiO doped with iron (5%Fe-NiO) it can help break C-H bond of methane and build C-O bond at130℃, which is lower86℃than the lowest temperature in the literature. The selectivity of CO2is higher than90%at250℃, and the catalyst has long life. It is promising that the material can be used as methane combustion catalyst.
(4) Synthesis of the two-dimensional mesoporous TiO2and doped transition and rare earth metal oxide (Ce) catalysts have been completed by using acid-base self-regulating method. Activation methane experiment were carried out over these TiO2catalyst, we can found that the mesoporous TiO2can activate methane at210℃, compared to bulk TiO2,the activation temperature is lower290℃. The5%Ce-TiO2catalyst can activate methane at140℃, which is lower76℃than the lowest temperature in the literature. The XPS results confirmed the type of catalyst the reason is mainly chemical adsorbed oxygen from the catalytic oxidation at low react temperature, while and lattice oxygen plays an important part in high react temperature.
(5) In order to further understand the rule of pore and pore structure in the catalytic conversion of methane, we prepared non-porous quartz sand, and mesoporous molecular sieve KIT-6, microporous zeolite HZSM-5supported transition metal oxides and rare earth metal Ln (Ln=La and Ce, and Gd) catalyst by impregnation method, and studied the behavior of the catalytic activation respectively. According to the experiment results, the activation temperature in non-porous quartz sand supported is the highest (670℃). Methane activation temperature over KIT-6supported metal catalyst is550℃, while the HZSM-5supported transition metal oxides and rare earth metal can activate methane at350℃. At low temperature of723K, methane can be easily activated in the presence of ethylene in the feed, and converted to higher hydrocarbons (C2-C4) and aromatics (C6-C10), through its reaction over rare metals modified Zn/HZSM-5zeolite catalysts. Methane can get37.3%conversion over the above catalysts, the catalysts show a longer lifetime than usual metal supported HZSM-5zeolite catalysts without adding any rare earth metals.
In conclusions, these results indicated the pore and porous structure in mesoporous transition metal oxides play a important role in the activate methane and can significantly improve the catalytic activity of mesoporous transition metal oxides under low temperature. Mesoporous transition metal oxides may be a promising catalytic material in the large-scale production of the fine chemicals.
介孔过渡金属氧化物除具有过渡金属氧化物的组成和通常的物理化学性质外,由于介孔的存在,它们还呈现出大孔径,大比表面积,丰富的表面结构,纳米粒子属性和微型反应器的功能。此外,它们的孔道结构和组成是可调节的,具有可设计的特性。与已知的甲烷转化催化剂相比,确有许多无以伦比之处。因此,可以毫无怀疑的认为,稳定的介孔过渡金属氧化物材料为寻找能够在温和条件下打开甲烷分子中的C-H键,建立C-C、C-O等新键的新型高效催化剂提供了一个难得的机会。基于此,本文以介孔过渡金属氧化物为催化剂,开展了一系列催化活化甲烷转化的研究工作,主要内容如下：
(1)以离子液体和苯醚为媒介、乙酰丙酮铁为铁源、离子液体并参与形貌控制制备出新颖的介孔α-Fe203材料,通过扫描电镜(SEM)表征发现其具有花瓣状结构,每个纳米棒长约567nm,宽约52nm；进一步通过透射电镜(TEM)可以在棒体上观察到有明显的介孔孔道,孔径为3.2nm；N2吸附脱附曲线(BET)分析得该新颖介孔材料的比表面为55.1m2·g-1。同时将其用于催化活化甲烷,实验结果发现在3atm,CH4/02=3,GHSV=4800ml/g.h条件下,130℃的低温下就可以打破甲烷分子中的C-H键,生成含C-O键产物。这比文献上报道的纳米α-Fe203活化甲烷的最低温度降低了220℃,比目前报道的甲烷热转化的最低活化温度低70C。经研究证明此介孔α-Fe203材料中存在三种活性氧,其中对应于可在130℃时活化甲烷的是表面吸附氧。
(2)通过改进的硬模板法批量制备了介孔氧化物Co304及其掺杂5%其它过渡金属和稀土金属Ce氧化物材料,并将其用于活化甲烷,发现纯的介孔Co3O4可以在145℃时活化甲烷,在以5%Cr-Co3O4为催化剂时甲烷的最低活化温度也为130℃,这比目前文献中以Co3O4为活性组分的材料活化甲烷的最低温度要低71℃,在低温下CO的选择性高于90%,并有长寿命,其有望成为低温下甲烷重整制合成气的催化剂。通过XPS测试发现该系列催化剂上含有两种活性氧即表面吸附氧和晶格氧,该系列催化剂中表面吸附氧的含量大于介孔α-Fe2O3,这也是该系列催化剂在低温下较α-Fe2O3具有长寿命的催化活性的原因。
(3)利用改进并放大的硬模板法批量制备了介孔NiO及其掺杂过渡金属和稀土金属Ce氧化物系列催化剂并将其用于甲烷的活化,结果证明纯介孔NiO可以在210℃的低温下活化甲烷,以5%Fe-NiO的材料为催化剂时,发现其也可以在130℃的低温下活化甲烷,这比文献中报道的以NiO为活性的催化剂活化甲烷最低温度要低191℃,该系列催化剂在反应温度升高到250℃时,CO2的选择性始终高于80%,可见,该系列材料有可能发展为一种低温下催化燃烧甲烷的优秀催化剂。
(4)通过改进的酸碱自调节法制备了介孔TiO2以及负载过渡和稀土金属Ce氧化物系列材料,并将其用于催化活化甲烷,实验结果显示介孔TiO2催化剂可以在210℃活化甲烷,比块体TiO2对甲烷的活化温度低290℃。当以5%Ce-TiO2为催化剂时甲烷的活化温度可以低至140℃,这也比文献报道的最好的同类TiO2催化剂活化甲烷的最低温度降低了360℃,同时比目前报道的甲烷热转化的最低温度降低了60℃。掺杂少量铁系(Fe、Co和Ni)可以使甲烷的活化温度降低到160℃和180℃。XPS测试结果证实该类催化剂低温催化活性应归因于表面吸附氧,高温时主要是晶格氧起催化氧化作用。
(5)为了进一步深入理解孔及其孔结构在催化转化甲烷中的作用,本文还利用浸渍法制备了无孔的石英砂、介孔分子筛KIT-6、微孔分子筛HZSM-5负载过渡金属氧化物及稀土金属Ln(Ln=La、Ce和Gd)的催化剂,并分别研究了它们对甲烷的催化活化行为。发现无孔的石英砂活化甲烷生成含C-O键产物的温度最高,为670℃；KIT-6分子筛上含C-O键的产物生成温度为550℃,纯的HZSM-5载体在350℃活化甲烷,生成含C-O键的产物(CO和CO2),微孔HZSM-5负载的稀土改性材料显示出优异的催化活性。微孔的HZSM-5负载双金属Ln和Zn的材料上最低在270℃活化甲烷生成含C-O键产物,介孔分子筛负载5%的Fe材料却可以在200℃时活化甲烷,这说明介孔分子筛负载的氧化物活化甲烷能力大于微孔分子筛负载的氧化物活化甲烷的活性,这证明了适宜的孔大小和结构因负载稀土改性的金属氧化物后可以创造出优异催化活性,负载了金属氧化物微孔分子筛催化剂的活性低于介孔分子筛负载氧化物的活性,是因为微孔分子筛催化剂中适宜的孔及其结构因负载而减少的缘故。这三类载体及负载金属氧化物材料活化甲烷生成C-C键产物的能力与生成C-O键产物能力有些不同。微孔HZSM-5负载金属氧化物材料活化甲烷生成C-C键产物的能力最强,可以在550℃时活化甲烷生成C-C键产物。有利于芳构化产物的生成。特别是在无氧、乙烯存在条件下该类催化剂可以显著降低甲烷的活化温度,使得甲烷在450℃的低温下生成芳烃,甲烷的最高转化率可以达到37.3%,这比文献上报道的获得相近甲烷转化率时的反应温度降低了150℃。
上述研究结果充分说明在过渡金属氧化物中的孔及其结构和组成对催化甲烷转化有非常重要的作用,能显著的提高低温催化活性。介孔过渡金属氧化物是一类很有希望的低温高效催化转化甲烷的材料。对其深入系统的研究不仅能深刻地揭示出甲烷催化转化的内在本质,丰富催化化学的基础理论知识,而且还可能开发出低耗高效清洁催化转化甲烷的实用技术。
At current usage, worldwide reserves of petroleum and coal are projected to only last for a few decades. This situation is a serious problem on a global level.Developin g efficient strategies for the selective activation and transformation of methane as the most abundant feedstock for organic chemicals to value-added chemicals or liquid fuels would provide a promising alternative for easing up the coal and oil-demanding situation during the high-growth process of the economic and the rapid development of science and technology. However, the bonds to be broken are thermodynamically strong and kinetically inert. Construction of the more sophisticated value-added architectures via C-H bond activation in methane is a highly difficult task.
Although methane conversion has been investigated for one hundred years, only indirect conversion method has realized in industrial scale. The development of direct conversion of methane to useful chemicals by activating C-H bonds still remains a difficult task despite thousands of Catalysts and almost all elements except group zero elements in periodical table used in the past decades.The investigation for new ways of methane conversion and the inherent laws of methane conversion is very important to solve the energy, resources and environmental problems in the sustainable development of humane society.
In addition to with the composition of the transition metal oxides and the usual physical and chemical properties, mesoporous transition metal oxides possess a large aperture, large surface area, diverse surface structures, nanoparticle properties and function of micro-reactor. Moreover, their pore structure and composition can be tunable. By comparison with the known methane conversion catalyst, mesoporous transition metal oxide materials exhibit a lot of unusual characters and may provide a great deal of opportunity to find the excellent catalysts for breaking the C-H bonds to establish the new C-C, C-O. In this thesis, the research effort has focused on the preparation of mesoporous transition metal oxide and activation of methane by mesoporous transition metal oxide as catalyst. The main points of the thesis are as follows.
(1) A novel mesoporous α-Fe2O3material have been prepared by using the ionic liquid as the media, acetylacetone iron as the iron source and diphenyl ether as the morphology control reagent. It is found that the material has a flower-like structure by SEM, each nanorod of about567nm, the width of52nm. It is also characterized by TEM, and found there are mesopores in the the nanorod, the pore diameter is3.2nm. The BET showed that the novel material has a specific surface area of55.1m2·g-1. Carried out the catalytic activation of methane experiments, at3atm, CH4/O2=3, GHSV=4800ml/g-h, the results show the lowest temperature of breaking C-H bond of methane is130℃over this Mesoporous α-Fe2O3nanorods catalyst. The reason is mesoporous α-Fe2O3surface adsorption of oxygen and interstitial oxygen plays an important part in the methane activation
(2) Three-dimensional mesoporous CO3O4and doped with other transition metal and rare earth metal (Ce) material have been prepared by using improved hard template methods. Activation methane experiment were carried out over these CO3O4materials, and found mesoporous Co3O4catalyst can activate methane at145℃, compared to bulk Co3O4,the activation temperature is lower30℃, which is lower71℃than the lowest temperature in the literature. While using the mesoporous Co3O4doped with chromium(5%Cr-Co3O4) it can help break C-H bond of methane and build C-O bond at130℃, the selectivity of CO is higher than90%, and the catalyst has long life. It is promising that the material can be used as syngas catalyst.
(3) Mesoporous NiO and doped with other transition metal and rare earth metal (Ce) material have been prepared by using improved hard template methods. Activation methane experiment were carried out over these NiO materials, and found mesoporous NiO catalyst can activate methane at210℃, compared to bulk NiO, the activation temperature is lower70℃, While using the mesoporous NiO doped with iron (5%Fe-NiO) it can help break C-H bond of methane and build C-O bond at130℃, which is lower86℃than the lowest temperature in the literature. The selectivity of CO2is higher than90%at250℃, and the catalyst has long life. It is promising that the material can be used as methane combustion catalyst.
(4) Synthesis of the two-dimensional mesoporous TiO2and doped transition and rare earth metal oxide (Ce) catalysts have been completed by using acid-base self-regulating method. Activation methane experiment were carried out over these TiO2catalyst, we can found that the mesoporous TiO2can activate methane at210℃, compared to bulk TiO2,the activation temperature is lower290℃. The5%Ce-TiO2catalyst can activate methane at140℃, which is lower76℃than the lowest temperature in the literature. The XPS results confirmed the type of catalyst the reason is mainly chemical adsorbed oxygen from the catalytic oxidation at low react temperature, while and lattice oxygen plays an important part in high react temperature.
(5) In order to further understand the rule of pore and pore structure in the catalytic conversion of methane, we prepared non-porous quartz sand, and mesoporous molecular sieve KIT-6, microporous zeolite HZSM-5supported transition metal oxides and rare earth metal Ln (Ln=La and Ce, and Gd) catalyst by impregnation method, and studied the behavior of the catalytic activation respectively. According to the experiment results, the activation temperature in non-porous quartz sand supported is the highest (670℃). Methane activation temperature over KIT-6supported metal catalyst is550℃, while the HZSM-5supported transition metal oxides and rare earth metal can activate methane at350℃. At low temperature of723K, methane can be easily activated in the presence of ethylene in the feed, and converted to higher hydrocarbons (C2-C4) and aromatics (C6-C10), through its reaction over rare metals modified Zn/HZSM-5zeolite catalysts. Methane can get37.3%conversion over the above catalysts, the catalysts show a longer lifetime than usual metal supported HZSM-5zeolite catalysts without adding any rare earth metals.
In conclusions, these results indicated the pore and porous structure in mesoporous transition metal oxides play a important role in the activate methane and can significantly improve the catalytic activity of mesoporous transition metal oxides under low temperature. Mesoporous transition metal oxides may be a promising catalytic material in the large-scale production of the fine chemicals.
引文
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