丙烷及乙苯氧化脱氢反应的新型催化剂研究
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摘要
本论文围绕丙烷、乙苯的氧化脱氢中新型催化材料的制备及其表征开展三部分工作。首先是高比表面的SiC的制备及其作为载体在丙烷氧化脱氢中应用；其次是模板法合成高比表面的CeO2和掺杂的CeO2作为催化剂在乙苯氧化脱氢中应用；最后为CeO2负载的纳米金催化剂在乙苯氧化脱氢中应用。具体内容如下：
一、高比表面SiC的合成及其在丙烷氧化脱氢催化材料中应用研究
丙烯是最早采用的化工原料,也是生产化工产品的重要烯烃之一。目前,丙烯绝大部分来源于石脑油等蒸气裂解乙烯的联产以及石油的催化裂化,石化资源的严重短缺使得该工艺难以满足日益增长的需求；而通过丙烷直接脱氢制取丙烷又存在在热力学受限、操作温度高、催化剂易失活的缺点。如果在丙烷脱氢原料中引入少量氧气(氧化脱氢),不仅能降低反应温度,而且催化剂不易失活,因此丙烷氧化脱氢近年来得到了极大关注。目前,在丙烷氧化脱氢催化研究中,催化剂载体主要为SiO2、Al2O3等传统材料。在高温高空速条件下,由于载体导热能力差,反应释放的热量极易在催化剂表面引发“热点效应”,即催化剂床层局部温度远高于平均温度。由于丙烷氧化脱氢的产物丙烯化学性质活泼,极易发生深度氧化,因而导致目标产物选择性降低。SiC材料具有极高的导热能力和优良的机械强度,广泛地应用于催化、电子等研究领域。目前,有报道指出使用SiC载体负载VPO催化剂在丁烷选择氧化制取马来酸酐反应中,较传统SiO2能显著降低热点效应而获得高选择性。此外,SiC材料在处理汽车尾气的三效催化反应、CH4部分氧化等多相放热反应中也有广泛应用。
在众多SiC材料合成方法中,溶胶-凝胶法具有操作简单,原料价廉的优点,因此被广泛采用。然而该方法制备的SiC比表面偏低(低于100 m2·g-1),因而不适合作为载体负载钒氧化物应用于丙烷氧化脱氢反应。本文在上述传统的溶胶-凝胶法制备SiC材料中做了改进,即在硅胶水解前,加入了一定比例的有机硅。N2吸脱附结果表明：有机硅的加入能显著提高SiC比表面,且引入有机硅的憎水碳链越长,硅胶干燥过程中体积坍缩程度越小,最后制得的SiC孔径越小,比表面越高。由此,通过C1、C4、C6、C8等不同碳链长度有机硅的系统调变,可以制得孔径在8-30 nm,比表面为150-360 m2·g-1的SiC。XRD和HRTEM表明制得的SiC为面心立方结构(β-SiC)。使用NH4VO3-甲醇浸渍法,将V2O5分散到SiC后,在600℃、C3H8/O2/N2=1/1/4(总流量：30 mL·min-1,催化剂50mg)条件下评估催化剂活性。结果表明：催化活性随V2O5的负载量增大而迅速增大,而相应的丙烯选择性则逐渐降低；在V2O5负载量为1.5 wt%时,丙烯选择性为62.1%,收率为20.2%；而在同等V2O5负载量下的SiO2和Al2O3催化剂的丙烯选择性较低,分别为51.0%,47.8%。实验中采用双热电偶测试了热点效应,结果显示：SiC负载的催化剂床层比设定温度偏差为16℃,而SiO2、Al2O3则分别55、78℃。此结果证实了SiC的高导热能力能显著地降低热点效应而缓解丙烯深度氧化。此外,通过XPS、H2-TPR表征结果发现,SiC表面的一层SiO2薄膜对分散V2O5起着至关重要的作用。
二、高比表面CeO2基催化剂在乙苯氧化脱氢中催化研究
苯乙烯是一种重要的基本有机化工原料,广泛应用于塑料、树脂和橡胶的合成,也是仅次于乙烯、丙烯、氯乙烯的第四位全球需求量最大的烯烃。目前,全球苯乙烯年生产能力在2500万吨以上,其中90%以上采用乙苯催化脱氢法生产。该工艺催化剂为K2O修饰的Fe2O3,由于乙苯直接脱氢是吸热反应,操作温度很高(650℃左右)。此外为了缓解催化剂积碳失活,原料中需要引入大量的水蒸气,因此该工艺存在能耗高、平衡转化率低等缺陷。乙苯氧化脱氢制取苯乙烯在热力学上具有很大的优势,且催化剂不易失活,能耗较低。目前在乙苯氧化脱氢研究领域,纳米碳管、碳纤维等碳质材料表现出极高的苯乙烯收率(-50%),但是由于碳材料质轻易燃,且难以成型,因此极不适于实际应用。CeO2是稀土氧化中在催化研究中使用最广泛的氧化物,以CeO2为基础的氧化物广泛地应用与处理汽车尾气的三效催化剂、CO氧化、CO2活性、NOx消除等反应。CeO2的诸多催化应用归结于其优良的储氧能力：贫氧环境下释放晶格氧,而富氧环境下储存晶格氧,即Ce4+和Ce3+能实现快速切换。在金属氧化物催化氧化脱氢反应中,晶格氧的移动、补充速率越快,则氧化脱氢速率越快。因此,近年来CeO2为基础的催化剂在氧化脱氢反应中催化应用受到了人们极大的关注。
使用CTAB模板法,制备了一系列具有介孔结构的高比表面CeO2材料。N2吸脱附结果表明,焙烧温度越高,CeO2的比表面越低,XRD衍射峰宽化程度越高。作为催化剂应用于乙苯氧化脱氢(反应条件：450℃, EB/O2/N2=0.5/0.25/20,总流速：20.75 mL·min-1,催化剂50 mg),结果表明：高比表面的CeO2较低比表面的CeO2具有更高的催化活性(EB转化率：27.4%,苯乙烯选择性：87.0%)。H2-TPR谱图上发现高比表面的CeO2在200-450℃就表现出极强的还原峰,由此证实,比表面越高,晶格氧越活泼。在此结果基础上,在高比表面CeO2制备中掺入了10%的第二元金属离子(Al3+、Sn4+、Zr4+、Mn4+和Ni3+)以改善晶格氧活性。XRD结果表明,第二元金属离子的引入造成了CeO2晶格缺陷。催化实验结果表明,第二元金属离子的引入改变了CeO2的催化活性,其催化活性顺序依次为：Ce0.90Ni0.10Ox> Ce0.90Mn0.10ioOx> Ce0.90Sn0.10Ox> CeO2> Ce0.90Zr0.10Ox> Ce0.90Al0.10Ox。在此基础上,研究了不同Ni掺杂量的CeO2催化剂活性,结果表明：当Ni掺杂量为10%时,CeO2晶格缺陷程度最高。在乙苯氧化脱氢中(反应条件：500℃, EB/O2/N2=0.5/0.25/20,总流速：20.75 mL·min-1,催化剂50mg)达到了50%的苯乙烯得率。H2-TPR谱图结果表明：Ce0.90Ni0.10Ox较其他催化剂的低温还原峰的温度低,为284℃；同时H2-TOSC (500℃)结果表明：Ce0.90Ni0.10Ox在不同Ni掺杂量的CeO2催化剂中总储氧量最高,鉴于此,Ce0.90Ni0.10Ox快速的晶格氧迁移能力和较高的储氧量很好地解释了其在乙苯氧化脱氢中所表现出的极高的催化活性。
三、CeO2负载的纳米金催化乙苯氧化脱氢研究
金历来被认为是化学惰性的金属,相对于其他贵金属,金的催化潜力一直未能引起足够的重视。直至上世纪八十年代,Haruta等发现通过沉积-沉淀法制备Au/Fe2O3等催化剂能在CO低温氧化中表现出很高的催化活性,人们由此对金的催化开展了大量的工作。目前纳米金涉足多个催化领域,如氧化、加氢、异构化、多级串联反应等。尤其在选择氧化领域,纳米金被视为能够开展可持续、绿色化学的最佳催化剂。最近,科研工作者在醇、醛、胺等液相选择氧化反应中取得了一定的成果。相比之下,目前所报告的纳米金在烷烃、芳烃的选择氧化中的研究极少,其原因在于反应物和氧化产物的化学性质非常活泼,很容易在氧化气氛中发生催化燃烧。因此将纳米金应用于气相乙苯氧化脱氢反应不仅是对金在气相芳烃选择氧化领域中的一项重要补充,对开发新型乙苯氧化脱氢催化反应也有极其重要的现实意义。
通过不同制备方法,合成了一系列的金属氧化物等负载的贵金属催化剂,诸如Pt/CeO2、Ru/CeO2、Au/Al2O3、Au/Mn2O3、Au/CeO2等。催化结果表明：使用Au/CeO2催化剂的催化性能较其他贵金属(Pt、Ru)和载体(HAP、MnO2、Fe2O3、TiO2和Al2O3)高,其原因归结于其他贵金属和载体上较易引发反应物或产物的深度氧化。基于此结果,使用NaOH-DP法,在CeO2沉积了不同负载量的纳米金颗粒。XRD和HR-TEM结果表明在低于6.0 wt%的Au负载量下,金颗粒(-3.5 nm)能很好地分散在CeO2载体上。在同等4.0 wt%负载量下,如使用普通浸渍法和CO(NH2)2-DP法,Au颗粒尺寸将明显增至5-10 nm左右。作为催化剂应用于乙苯氧化脱氢反应(条件：450℃, EB/O2/N2=0.5/0.25/20,总流速：20.75 mL·min-1,催化剂50 mg),结果表明：负载金后,能显著地提高CeO2的催化活性,且随着金负载量的增大,EB转化率逐渐增加,最终在采用NaOH-DP法得到的6.0 wt%Au负载量Au/CeO2催化剂上得到了60.9%的苯乙烯收率。H2-TPR结果表明,Au/CeO2在80℃的低温即出现还原峰,表明负载Au后,能显著提高CeO2晶格氧的迁移能力。采用H2-TOSC实验测试了Au/CeO2催化剂的在450℃下化学储氧量,结果表明：在低于6.0wt%负载量下,Au负载量越高,其化学储氧量越高,且与催化活性呈现出很好的顺变关联。
The present dissertation, involving the synthesis and characterizations of novel catalysts for oxidative dehydrogenation (ODH) of propane and ethylbenzene (EB), consists of three parts. The first part (Chapter III) is the synthesis of mesostructured SiC materials with high surface area and the study for ODH of propane as catalytic support. The second part (Chapter IV) reports the synthesis of ceria-base catalysts and the catalysis study for ODH of ethylbenzene. The last part (Chapter V) discusses the catalysis study of ceria-supported nanogold catalysts for ODH of EB.
1. Synthesis of SiC materials with high surface area and the catalysis study for ODH of propane as catalytic support
As one of major building blocks for modern petrochemical industry, propylene is widely used for the production of diverse products, ranging from rubbers to plastics. Nowadays, propylene are mostly produced by steam pyrolysis of naphtha (as coproduct of ethylene), and fluid catalytic cracking (FCC) in oil refining. As the oil gets scarcer and more expensive, the two convenient processes could not meet the tremendous demand of propylene. Meanwhile, the new process of the synthesis of propylene via the direct dehydrogenation (DH) of propane still presents some disadvantages, such as the thermodynamical limitations, high temperature, and easy deactivation. Alternatively, based on the introduction of oxygen into the feedstock, the process of ODH of propane could decrease the reaction temperature and simultaneously, prevent the deactivation and thus has spurred the interest as a promising route. Up to now, the catalytic supports applied for ODH of propane are mainly traditional metal oxides such as SiO2, Al2O3. It is noteworthy that, in the heterogeneously exothermic reaction, the support with a low thermal conductivity cannot disperse the reaction heat well, issuing in partial hot spots on the surface of the catalyst bed, wherein the temperature is far beyond the average level. On the other hand, owing to its highly reactive nature, the propylene molecular in the vicinity of the hot spots is liable to consecutive oxidation, which leads to low selectivity of the target product. SiC material possesses highly thermal conductivity and excellent mechanical strength, which enables it wide application in the fields of catalysis, electronics, etc. Recently, Ledoux et al. has reported that the SiC-supported VPO catalyst demonstrated superior catalytic performance to SiO2-supported catalyst for the selective oxidation of butane into maleic acid, due to its high thermal conductivity. Moreover, SiC material has been extensively used as catalytic supports in the TWC catalytic system, partial oxidation of CH4, and other heterogeneously exothermal reactions.
A wide range of methods have been reported for the synthesis of SiC materials and therein the sol-gel method presents the convenience and low cost and other several advantages, and therefore is widely used to fabricate the SiC materials. However, due to the low surface area (< 100 m2·g-1), the synthesized SiC material via sol-gel method is not suitable to load the vanadia catalyst for ODH of propane. In this paper, a given amount of alkyloxysilane is introduced into the precursor of the silica solution before the hydrolysis. The results of N2 adsorption-desorption indicated that the incorporation of alkyloxysilane can increase the surface area of SiC materials and the longer length of hydrophobic chain of alkyloxysilane was favorable for the higher surface area. Consequently, a series of mesostructuredβ-SiC with high surface area (151-350 m2·g-1) and tunable porosity (8-30 nm) were synthesized by adjusting the length of hydrophobic chain of alkyloxysilane (C1, C4, C6, and C8), which was confirmed by N2 adsorption-desorption, XRD, and HR-TEM techniques. Loaded with vanadia by wet impregnant method (NH4VO3-CH3OH), SiC was employed as catalyst support for ODH of propane to propylene (reaction temperature:600℃; C3H8/O2/N2=1/1/4; total gas velocity:30 mL·min-1; Catalyst weight:50 mg). The catalytic performances demonstrated the selectivity of propylene decreased with the increase of the loading amount of vanadia and the highest yield of propylene (20.2%) along with the selectivity of 62.1% was obtained when the loading amount was 1.5 wt%. However, as the counterparts, SiO2 and A12O3 gave low selectivity to propylene (51.0 and 47.8% respectively) under the identical reaction conditions. By employing two thermocouples, hot spot effect was tested and the results demonstrates the differential temperature for SiC-supported catalyst was 16℃, while the catalyst supported by SiO2 and A12O3 were 58 and 73℃respectively. The results above confirmed that, over the SiC-supported catalyst, high thermal conductivity could alleviate the hot spot effect and therefore prevent the deep oxidation of propylene. In addition, the results of XPS and H2-TPR characterizations revealed that the silica film on the surface of SiC material played a crucial role to disperse the vanadia species.
2. Synthesis of ceria base catalysts and the catalysis study for ODH of ethyl benzene
Styrene (ST) is an important monomer extensively used in the chemical industry for the manufacture of plastic, resin, and rubber, and ranks the forth place in the highest demand alkenes, only following ethylene, propylene, and vinychorine. Nowadays, the annual capacity of the styrene synthesis is above 25 Mt over the world. Therein,90% of styrene is commercially produced by means of the direct DH of EB over potassium-iron oxide as a catalyst at high temperature (ca.650℃) in presence of a lot of steam. Due to its highly endothermic nature, this conventional route suffers from several disadvantages such as intensive energy consumption and rapid coking. Alternatively, the ODH of EB has attracted considerable recent attention since it can be operated at lower temperatures and the EB conversion would not be equilibrium limited. Currently, among a range of catalysts reported for DH of EB, nanocarbon materials like carbon nanotubes and carbon nanofibers exhibit an excellent catalytic performance with a yield of ST of ca.50%. Nevertheless, the industrial application of the carbon-based catalysts has been till now prevented by their fine powder nature and intrinsically low resistance to combustion. As the most widely used oxide in the family of rare earth, Ceria (CeO2) is a key redox component in the catalyst formulations for many industrially important reactions, such as TWC catalysts for automobile exhaust treatment, CO2 activation, CO oxidation, and low temperature water-gas shift reaction. The success of ceria in various applications is largely attributed to its superior oxygen storage capacity, viz. releasing and storing the oxygen lattice species under the lean-O2 and rich-02 conditions respectively. In the reactions based on the oxidative dehydrogenation, high 02-supplying rate are favorable for the high catalytic performance and therefore ceria-based catalysts have been received tremendous attention in the ODH reactions.
In the present work, a series of mesostructured ceria with high surface area has been prepared via template-assisted precipitation method. The results of N2 adsorption-desorption revealed that the surface area of ceria samples decrease with the increment of the calcination temperature, accompanied by the wider peak in the corresponding XRD patterns. In the reaction of ODH of EB to ST (reaction temperature:450℃; EB/O2/N2=0.5/0.25/20; 20.75 mL·mim-1; Catalyst weight:50 mg), the CeO2-500 sample with the highest surface area displayed the highest catalytic performance with the EB convention of 30% and ST selectivity of 82%. By analysis of the H2-TPR profiles, it is found the CeO2-500 sample presented a highly intense reduction peak at 200-450℃compared with other samples with low surface areas, which revealed that high surface are would favor the mobility of lattice oxygen species and consequently enhance the catalytic activity. As to the results above,10 wt% of the second metal species as dopant (Al3+, Sn4+, Zr4+, Mn4+, and Ni3+) were introduced into the ceria samples. The XRD patterns indicated the second metal species have been incorporated into the ceria lattice and leads to the lattice defeats. As catalysts for ODH of EB, the introduction of other metal ions haves changed the catalytic activity of the pristine ceria and the order of the catalytic activity was as follows:Ce0.90Ni0.10Ox> Ce0.90Mn0.10Ox> Ce0.90Sn0.10Ox> CeO2> Ce0.90Zr0.10Ox> Ce0.90Al0.10Ox (reaction temperature:500℃; EB/O2/N2=0.5/0.25/20; 20.75 mL·min-1; Catalyst weight:50 mg). To further investigate the effect of the amount of Ni on the catalytic performance, a series of Ni-doped ceria catalysts were studied for ODH of EB and the highest yield of ST (ca.50%) was obtained over Ce0.90Ni0.10Ox catalyst. The XRD patterns revealed that the Ce0.90Ni0.10Ox sample presented a highest lattice defeat, compared with other Ni-doped ceria catalysts, which is correlated with the corresponding reduction peak with the lowest temperature at ca.284℃in H2-TPR profiles, indicating the Ce0.90Ni0.10Ox possessed the considerable lattice oxygen mobility rate. Moreover, the H2-total oxygen storage experiments proved that the Ce0.90Ni0.10Ox catalyst possessed the highest oxygen storage capacity at 500℃, which could explained the highest catalytic performances in ODH of EB.
3. Catalysis study of ceria supported nanogold catalysts for ODH of ethylbenzene
Gold has been originally labeled as a chemically inert metal and long disregarded for catalytic applications. Compared with other noble metals such as Pt and Ru, the catalytic potential of gold has not been received considerable attention. Since Haruta discovered a remarkable activity of supported gold nanoparticles (NPs) in CO oxidation, catalysis by gold has become one of the most intensively studied topics in chemistry. Currently, gold could become a highly active and selective catalyst in many reactions including oxidation, hydrogenation, selective isomerization, and one-pot multistep reactions. Of particular interest to the current chemical community is the Au-catalyzed selective oxidation, which is believed to be essential for the development of new alternative and greener routes toward sustainability. Recently, several liquid phase aerobic oxidations, including the selective oxidation of alcohols, aldehydes, and amines have been developed. Despite significant research effort, there have been few studies on the selective oxidation of less reactive hydrocarbons in the gas phase over the supported Au nanoparticles probably due to the fact that both the reactants and products are prone to undesired combustion in the presence of molecular oxygen at high temperatures. In the context, the application of Au NPs into the ODH of EB in gas phase not only serves as a major supplement to the field of selective oxidative over Au catalyst in gas phase, but also presents a practical significance to develop a novel catalytic system for ODH of EB.
A range of noble catalysts including Pt/CeO2, Ru/CeO2, Au/Al2O3, Au/Mn2O3, and Au/CeO2 were prepared via different methods and investigated for ODH of EB. Compared with Au/CeO2 catalysts, the Pt and Ru based catalyst, as well as other metal oxides supported Au catalyst demonstrated low selectivity to ST, due to the direct and deep combustion. Moreover, according the results of XRD patterns and HR-TEM images of the Au/CeO2 catalysts prepared by different methods, NaOH-DP, rather than urea-DP and wet impregnant methods, could assure a good dispersion of Au nanoparticles over ceria at the same loading amount of Au. In the ODH of EB, the existence of Au NPs could improve the catalytic activity of the pristine ceria and highest yield of 60.9% was obtained over 6.0 wt%Au/CeO2 catalyst. The results of H2-TPR profiles and H2-TOSC experiments revealed that the 6.0 wt%Au/CeO2 presented the highest OSC and oxygen mobility, which proved the highest catalytic performances.
一、高比表面SiC的合成及其在丙烷氧化脱氢催化材料中应用研究
丙烯是最早采用的化工原料,也是生产化工产品的重要烯烃之一。目前,丙烯绝大部分来源于石脑油等蒸气裂解乙烯的联产以及石油的催化裂化,石化资源的严重短缺使得该工艺难以满足日益增长的需求；而通过丙烷直接脱氢制取丙烷又存在在热力学受限、操作温度高、催化剂易失活的缺点。如果在丙烷脱氢原料中引入少量氧气(氧化脱氢),不仅能降低反应温度,而且催化剂不易失活,因此丙烷氧化脱氢近年来得到了极大关注。目前,在丙烷氧化脱氢催化研究中,催化剂载体主要为SiO2、Al2O3等传统材料。在高温高空速条件下,由于载体导热能力差,反应释放的热量极易在催化剂表面引发“热点效应”,即催化剂床层局部温度远高于平均温度。由于丙烷氧化脱氢的产物丙烯化学性质活泼,极易发生深度氧化,因而导致目标产物选择性降低。SiC材料具有极高的导热能力和优良的机械强度,广泛地应用于催化、电子等研究领域。目前,有报道指出使用SiC载体负载VPO催化剂在丁烷选择氧化制取马来酸酐反应中,较传统SiO2能显著降低热点效应而获得高选择性。此外,SiC材料在处理汽车尾气的三效催化反应、CH4部分氧化等多相放热反应中也有广泛应用。
在众多SiC材料合成方法中,溶胶-凝胶法具有操作简单,原料价廉的优点,因此被广泛采用。然而该方法制备的SiC比表面偏低(低于100 m2·g-1),因而不适合作为载体负载钒氧化物应用于丙烷氧化脱氢反应。本文在上述传统的溶胶-凝胶法制备SiC材料中做了改进,即在硅胶水解前,加入了一定比例的有机硅。N2吸脱附结果表明：有机硅的加入能显著提高SiC比表面,且引入有机硅的憎水碳链越长,硅胶干燥过程中体积坍缩程度越小,最后制得的SiC孔径越小,比表面越高。由此,通过C1、C4、C6、C8等不同碳链长度有机硅的系统调变,可以制得孔径在8-30 nm,比表面为150-360 m2·g-1的SiC。XRD和HRTEM表明制得的SiC为面心立方结构(β-SiC)。使用NH4VO3-甲醇浸渍法,将V2O5分散到SiC后,在600℃、C3H8/O2/N2=1/1/4(总流量：30 mL·min-1,催化剂50mg)条件下评估催化剂活性。结果表明：催化活性随V2O5的负载量增大而迅速增大,而相应的丙烯选择性则逐渐降低；在V2O5负载量为1.5 wt%时,丙烯选择性为62.1%,收率为20.2%；而在同等V2O5负载量下的SiO2和Al2O3催化剂的丙烯选择性较低,分别为51.0%,47.8%。实验中采用双热电偶测试了热点效应,结果显示：SiC负载的催化剂床层比设定温度偏差为16℃,而SiO2、Al2O3则分别55、78℃。此结果证实了SiC的高导热能力能显著地降低热点效应而缓解丙烯深度氧化。此外,通过XPS、H2-TPR表征结果发现,SiC表面的一层SiO2薄膜对分散V2O5起着至关重要的作用。
二、高比表面CeO2基催化剂在乙苯氧化脱氢中催化研究
苯乙烯是一种重要的基本有机化工原料,广泛应用于塑料、树脂和橡胶的合成,也是仅次于乙烯、丙烯、氯乙烯的第四位全球需求量最大的烯烃。目前,全球苯乙烯年生产能力在2500万吨以上,其中90%以上采用乙苯催化脱氢法生产。该工艺催化剂为K2O修饰的Fe2O3,由于乙苯直接脱氢是吸热反应,操作温度很高(650℃左右)。此外为了缓解催化剂积碳失活,原料中需要引入大量的水蒸气,因此该工艺存在能耗高、平衡转化率低等缺陷。乙苯氧化脱氢制取苯乙烯在热力学上具有很大的优势,且催化剂不易失活,能耗较低。目前在乙苯氧化脱氢研究领域,纳米碳管、碳纤维等碳质材料表现出极高的苯乙烯收率(-50%),但是由于碳材料质轻易燃,且难以成型,因此极不适于实际应用。CeO2是稀土氧化中在催化研究中使用最广泛的氧化物,以CeO2为基础的氧化物广泛地应用与处理汽车尾气的三效催化剂、CO氧化、CO2活性、NOx消除等反应。CeO2的诸多催化应用归结于其优良的储氧能力：贫氧环境下释放晶格氧,而富氧环境下储存晶格氧,即Ce4+和Ce3+能实现快速切换。在金属氧化物催化氧化脱氢反应中,晶格氧的移动、补充速率越快,则氧化脱氢速率越快。因此,近年来CeO2为基础的催化剂在氧化脱氢反应中催化应用受到了人们极大的关注。
使用CTAB模板法,制备了一系列具有介孔结构的高比表面CeO2材料。N2吸脱附结果表明,焙烧温度越高,CeO2的比表面越低,XRD衍射峰宽化程度越高。作为催化剂应用于乙苯氧化脱氢(反应条件：450℃, EB/O2/N2=0.5/0.25/20,总流速：20.75 mL·min-1,催化剂50 mg),结果表明：高比表面的CeO2较低比表面的CeO2具有更高的催化活性(EB转化率：27.4%,苯乙烯选择性：87.0%)。H2-TPR谱图上发现高比表面的CeO2在200-450℃就表现出极强的还原峰,由此证实,比表面越高,晶格氧越活泼。在此结果基础上,在高比表面CeO2制备中掺入了10%的第二元金属离子(Al3+、Sn4+、Zr4+、Mn4+和Ni3+)以改善晶格氧活性。XRD结果表明,第二元金属离子的引入造成了CeO2晶格缺陷。催化实验结果表明,第二元金属离子的引入改变了CeO2的催化活性,其催化活性顺序依次为：Ce0.90Ni0.10Ox> Ce0.90Mn0.10ioOx> Ce0.90Sn0.10Ox> CeO2> Ce0.90Zr0.10Ox> Ce0.90Al0.10Ox。在此基础上,研究了不同Ni掺杂量的CeO2催化剂活性,结果表明：当Ni掺杂量为10%时,CeO2晶格缺陷程度最高。在乙苯氧化脱氢中(反应条件：500℃, EB/O2/N2=0.5/0.25/20,总流速：20.75 mL·min-1,催化剂50mg)达到了50%的苯乙烯得率。H2-TPR谱图结果表明：Ce0.90Ni0.10Ox较其他催化剂的低温还原峰的温度低,为284℃；同时H2-TOSC (500℃)结果表明：Ce0.90Ni0.10Ox在不同Ni掺杂量的CeO2催化剂中总储氧量最高,鉴于此,Ce0.90Ni0.10Ox快速的晶格氧迁移能力和较高的储氧量很好地解释了其在乙苯氧化脱氢中所表现出的极高的催化活性。
三、CeO2负载的纳米金催化乙苯氧化脱氢研究
金历来被认为是化学惰性的金属,相对于其他贵金属,金的催化潜力一直未能引起足够的重视。直至上世纪八十年代,Haruta等发现通过沉积-沉淀法制备Au/Fe2O3等催化剂能在CO低温氧化中表现出很高的催化活性,人们由此对金的催化开展了大量的工作。目前纳米金涉足多个催化领域,如氧化、加氢、异构化、多级串联反应等。尤其在选择氧化领域,纳米金被视为能够开展可持续、绿色化学的最佳催化剂。最近,科研工作者在醇、醛、胺等液相选择氧化反应中取得了一定的成果。相比之下,目前所报告的纳米金在烷烃、芳烃的选择氧化中的研究极少,其原因在于反应物和氧化产物的化学性质非常活泼,很容易在氧化气氛中发生催化燃烧。因此将纳米金应用于气相乙苯氧化脱氢反应不仅是对金在气相芳烃选择氧化领域中的一项重要补充,对开发新型乙苯氧化脱氢催化反应也有极其重要的现实意义。
通过不同制备方法,合成了一系列的金属氧化物等负载的贵金属催化剂,诸如Pt/CeO2、Ru/CeO2、Au/Al2O3、Au/Mn2O3、Au/CeO2等。催化结果表明：使用Au/CeO2催化剂的催化性能较其他贵金属(Pt、Ru)和载体(HAP、MnO2、Fe2O3、TiO2和Al2O3)高,其原因归结于其他贵金属和载体上较易引发反应物或产物的深度氧化。基于此结果,使用NaOH-DP法,在CeO2沉积了不同负载量的纳米金颗粒。XRD和HR-TEM结果表明在低于6.0 wt%的Au负载量下,金颗粒(-3.5 nm)能很好地分散在CeO2载体上。在同等4.0 wt%负载量下,如使用普通浸渍法和CO(NH2)2-DP法,Au颗粒尺寸将明显增至5-10 nm左右。作为催化剂应用于乙苯氧化脱氢反应(条件：450℃, EB/O2/N2=0.5/0.25/20,总流速：20.75 mL·min-1,催化剂50 mg),结果表明：负载金后,能显著地提高CeO2的催化活性,且随着金负载量的增大,EB转化率逐渐增加,最终在采用NaOH-DP法得到的6.0 wt%Au负载量Au/CeO2催化剂上得到了60.9%的苯乙烯收率。H2-TPR结果表明,Au/CeO2在80℃的低温即出现还原峰,表明负载Au后,能显著提高CeO2晶格氧的迁移能力。采用H2-TOSC实验测试了Au/CeO2催化剂的在450℃下化学储氧量,结果表明：在低于6.0wt%负载量下,Au负载量越高,其化学储氧量越高,且与催化活性呈现出很好的顺变关联。
The present dissertation, involving the synthesis and characterizations of novel catalysts for oxidative dehydrogenation (ODH) of propane and ethylbenzene (EB), consists of three parts. The first part (Chapter III) is the synthesis of mesostructured SiC materials with high surface area and the study for ODH of propane as catalytic support. The second part (Chapter IV) reports the synthesis of ceria-base catalysts and the catalysis study for ODH of ethylbenzene. The last part (Chapter V) discusses the catalysis study of ceria-supported nanogold catalysts for ODH of EB.
1. Synthesis of SiC materials with high surface area and the catalysis study for ODH of propane as catalytic support
As one of major building blocks for modern petrochemical industry, propylene is widely used for the production of diverse products, ranging from rubbers to plastics. Nowadays, propylene are mostly produced by steam pyrolysis of naphtha (as coproduct of ethylene), and fluid catalytic cracking (FCC) in oil refining. As the oil gets scarcer and more expensive, the two convenient processes could not meet the tremendous demand of propylene. Meanwhile, the new process of the synthesis of propylene via the direct dehydrogenation (DH) of propane still presents some disadvantages, such as the thermodynamical limitations, high temperature, and easy deactivation. Alternatively, based on the introduction of oxygen into the feedstock, the process of ODH of propane could decrease the reaction temperature and simultaneously, prevent the deactivation and thus has spurred the interest as a promising route. Up to now, the catalytic supports applied for ODH of propane are mainly traditional metal oxides such as SiO2, Al2O3. It is noteworthy that, in the heterogeneously exothermic reaction, the support with a low thermal conductivity cannot disperse the reaction heat well, issuing in partial hot spots on the surface of the catalyst bed, wherein the temperature is far beyond the average level. On the other hand, owing to its highly reactive nature, the propylene molecular in the vicinity of the hot spots is liable to consecutive oxidation, which leads to low selectivity of the target product. SiC material possesses highly thermal conductivity and excellent mechanical strength, which enables it wide application in the fields of catalysis, electronics, etc. Recently, Ledoux et al. has reported that the SiC-supported VPO catalyst demonstrated superior catalytic performance to SiO2-supported catalyst for the selective oxidation of butane into maleic acid, due to its high thermal conductivity. Moreover, SiC material has been extensively used as catalytic supports in the TWC catalytic system, partial oxidation of CH4, and other heterogeneously exothermal reactions.
A wide range of methods have been reported for the synthesis of SiC materials and therein the sol-gel method presents the convenience and low cost and other several advantages, and therefore is widely used to fabricate the SiC materials. However, due to the low surface area (< 100 m2·g-1), the synthesized SiC material via sol-gel method is not suitable to load the vanadia catalyst for ODH of propane. In this paper, a given amount of alkyloxysilane is introduced into the precursor of the silica solution before the hydrolysis. The results of N2 adsorption-desorption indicated that the incorporation of alkyloxysilane can increase the surface area of SiC materials and the longer length of hydrophobic chain of alkyloxysilane was favorable for the higher surface area. Consequently, a series of mesostructuredβ-SiC with high surface area (151-350 m2·g-1) and tunable porosity (8-30 nm) were synthesized by adjusting the length of hydrophobic chain of alkyloxysilane (C1, C4, C6, and C8), which was confirmed by N2 adsorption-desorption, XRD, and HR-TEM techniques. Loaded with vanadia by wet impregnant method (NH4VO3-CH3OH), SiC was employed as catalyst support for ODH of propane to propylene (reaction temperature:600℃; C3H8/O2/N2=1/1/4; total gas velocity:30 mL·min-1; Catalyst weight:50 mg). The catalytic performances demonstrated the selectivity of propylene decreased with the increase of the loading amount of vanadia and the highest yield of propylene (20.2%) along with the selectivity of 62.1% was obtained when the loading amount was 1.5 wt%. However, as the counterparts, SiO2 and A12O3 gave low selectivity to propylene (51.0 and 47.8% respectively) under the identical reaction conditions. By employing two thermocouples, hot spot effect was tested and the results demonstrates the differential temperature for SiC-supported catalyst was 16℃, while the catalyst supported by SiO2 and A12O3 were 58 and 73℃respectively. The results above confirmed that, over the SiC-supported catalyst, high thermal conductivity could alleviate the hot spot effect and therefore prevent the deep oxidation of propylene. In addition, the results of XPS and H2-TPR characterizations revealed that the silica film on the surface of SiC material played a crucial role to disperse the vanadia species.
2. Synthesis of ceria base catalysts and the catalysis study for ODH of ethyl benzene
Styrene (ST) is an important monomer extensively used in the chemical industry for the manufacture of plastic, resin, and rubber, and ranks the forth place in the highest demand alkenes, only following ethylene, propylene, and vinychorine. Nowadays, the annual capacity of the styrene synthesis is above 25 Mt over the world. Therein,90% of styrene is commercially produced by means of the direct DH of EB over potassium-iron oxide as a catalyst at high temperature (ca.650℃) in presence of a lot of steam. Due to its highly endothermic nature, this conventional route suffers from several disadvantages such as intensive energy consumption and rapid coking. Alternatively, the ODH of EB has attracted considerable recent attention since it can be operated at lower temperatures and the EB conversion would not be equilibrium limited. Currently, among a range of catalysts reported for DH of EB, nanocarbon materials like carbon nanotubes and carbon nanofibers exhibit an excellent catalytic performance with a yield of ST of ca.50%. Nevertheless, the industrial application of the carbon-based catalysts has been till now prevented by their fine powder nature and intrinsically low resistance to combustion. As the most widely used oxide in the family of rare earth, Ceria (CeO2) is a key redox component in the catalyst formulations for many industrially important reactions, such as TWC catalysts for automobile exhaust treatment, CO2 activation, CO oxidation, and low temperature water-gas shift reaction. The success of ceria in various applications is largely attributed to its superior oxygen storage capacity, viz. releasing and storing the oxygen lattice species under the lean-O2 and rich-02 conditions respectively. In the reactions based on the oxidative dehydrogenation, high 02-supplying rate are favorable for the high catalytic performance and therefore ceria-based catalysts have been received tremendous attention in the ODH reactions.
In the present work, a series of mesostructured ceria with high surface area has been prepared via template-assisted precipitation method. The results of N2 adsorption-desorption revealed that the surface area of ceria samples decrease with the increment of the calcination temperature, accompanied by the wider peak in the corresponding XRD patterns. In the reaction of ODH of EB to ST (reaction temperature:450℃; EB/O2/N2=0.5/0.25/20; 20.75 mL·mim-1; Catalyst weight:50 mg), the CeO2-500 sample with the highest surface area displayed the highest catalytic performance with the EB convention of 30% and ST selectivity of 82%. By analysis of the H2-TPR profiles, it is found the CeO2-500 sample presented a highly intense reduction peak at 200-450℃compared with other samples with low surface areas, which revealed that high surface are would favor the mobility of lattice oxygen species and consequently enhance the catalytic activity. As to the results above,10 wt% of the second metal species as dopant (Al3+, Sn4+, Zr4+, Mn4+, and Ni3+) were introduced into the ceria samples. The XRD patterns indicated the second metal species have been incorporated into the ceria lattice and leads to the lattice defeats. As catalysts for ODH of EB, the introduction of other metal ions haves changed the catalytic activity of the pristine ceria and the order of the catalytic activity was as follows:Ce0.90Ni0.10Ox> Ce0.90Mn0.10Ox> Ce0.90Sn0.10Ox> CeO2> Ce0.90Zr0.10Ox> Ce0.90Al0.10Ox (reaction temperature:500℃; EB/O2/N2=0.5/0.25/20; 20.75 mL·min-1; Catalyst weight:50 mg). To further investigate the effect of the amount of Ni on the catalytic performance, a series of Ni-doped ceria catalysts were studied for ODH of EB and the highest yield of ST (ca.50%) was obtained over Ce0.90Ni0.10Ox catalyst. The XRD patterns revealed that the Ce0.90Ni0.10Ox sample presented a highest lattice defeat, compared with other Ni-doped ceria catalysts, which is correlated with the corresponding reduction peak with the lowest temperature at ca.284℃in H2-TPR profiles, indicating the Ce0.90Ni0.10Ox possessed the considerable lattice oxygen mobility rate. Moreover, the H2-total oxygen storage experiments proved that the Ce0.90Ni0.10Ox catalyst possessed the highest oxygen storage capacity at 500℃, which could explained the highest catalytic performances in ODH of EB.
3. Catalysis study of ceria supported nanogold catalysts for ODH of ethylbenzene
Gold has been originally labeled as a chemically inert metal and long disregarded for catalytic applications. Compared with other noble metals such as Pt and Ru, the catalytic potential of gold has not been received considerable attention. Since Haruta discovered a remarkable activity of supported gold nanoparticles (NPs) in CO oxidation, catalysis by gold has become one of the most intensively studied topics in chemistry. Currently, gold could become a highly active and selective catalyst in many reactions including oxidation, hydrogenation, selective isomerization, and one-pot multistep reactions. Of particular interest to the current chemical community is the Au-catalyzed selective oxidation, which is believed to be essential for the development of new alternative and greener routes toward sustainability. Recently, several liquid phase aerobic oxidations, including the selective oxidation of alcohols, aldehydes, and amines have been developed. Despite significant research effort, there have been few studies on the selective oxidation of less reactive hydrocarbons in the gas phase over the supported Au nanoparticles probably due to the fact that both the reactants and products are prone to undesired combustion in the presence of molecular oxygen at high temperatures. In the context, the application of Au NPs into the ODH of EB in gas phase not only serves as a major supplement to the field of selective oxidative over Au catalyst in gas phase, but also presents a practical significance to develop a novel catalytic system for ODH of EB.
A range of noble catalysts including Pt/CeO2, Ru/CeO2, Au/Al2O3, Au/Mn2O3, and Au/CeO2 were prepared via different methods and investigated for ODH of EB. Compared with Au/CeO2 catalysts, the Pt and Ru based catalyst, as well as other metal oxides supported Au catalyst demonstrated low selectivity to ST, due to the direct and deep combustion. Moreover, according the results of XRD patterns and HR-TEM images of the Au/CeO2 catalysts prepared by different methods, NaOH-DP, rather than urea-DP and wet impregnant methods, could assure a good dispersion of Au nanoparticles over ceria at the same loading amount of Au. In the ODH of EB, the existence of Au NPs could improve the catalytic activity of the pristine ceria and highest yield of 60.9% was obtained over 6.0 wt%Au/CeO2 catalyst. The results of H2-TPR profiles and H2-TOSC experiments revealed that the 6.0 wt%Au/CeO2 presented the highest OSC and oxygen mobility, which proved the highest catalytic performances.
引文
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