核壳结构纳米催化剂的设计与制备及甲烷选择性氧化制合成气研究
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摘要
天然气转化与利用是当今石油化工及替代能源十分重要的研究领域,其中将甲烷转化为合成气成为关键步骤,并为其转化为具附加值的产品或者在燃料电池及电厂方面应用奠定了基础。同传统的甲烷水蒸汽重整相比,甲烷选择性氧化(POM)制取合成气由于其高效节能的优势引起了广泛的研究兴趣。
纳米材料因其独特的“表面效应”而在多相催化领域受到青睐。然而,纳米粒子在较高温度下不稳定,容易聚集,从而失去了本身固有的优势。因此,将纳米粒子包裹上一层多孔且稳定的壳层,既能提高纳米材料的热稳定性,又能改变它的表面电荷密度、反应性和多功能性。这类核壳结构材料由于其独特的结构和物理化学性质引起了广泛的关注。
本文立足于核壳结构纳米催化剂的设计与开发,并将其用于甲烷选择性氧化制取合成气的研究。通过精细调变形貌、结构、尺寸和元素组成,结合其在催化反应中的催化活性和相关的表征分析,我们对核壳结构纳米催化剂的特点及其在POM反应中的性能表现,获得如下认识：
1.不同尺寸与形貌的CuO、NiO纳米粒子,分别借助于超声或搅拌的手段,能够以溶胶-凝胶的方法将其包裹上一层微孔/介孔SiO2材料。所包裹的氧化物纳米材料,最终可通过H2原位还原的方法,转变为零价的活性组分。
2.核壳结构材料制备过程中,表面活性剂(PVP、CTAB)的添加与否,对壳层孔结构产生很大的影响。未添加表面活性剂,所得到的核壳结构形貌大小不是很均一,微孔居多。而加入表面活性剂PVP后,能够得到相对均一、形貌结构明显的核壳结构,且壳层具有较多的介孔。CTAB的加入,使得SiO：壳层具有更发达的孔结构,比表面积大。
3.核壳结构纳米催化剂的性能取决于Ni核尺寸的大小,研究发现,在POM反应中,在6-45nm尺寸范围,核粒子越小活性越高。建立了催化剂活性与Ni核粒子尺寸之间的构-效关系,同时,高温稳定的核壳结构纳米催化剂又为高温反应下纳米粒子尺寸与活性的关联提供了有效的策略。此外,积碳与核尺寸大小也有关联,小尺寸的Ni粒子能够较好地抑制表面积碳。
4.POM反应的催化活性强烈依赖于Co-Ni双组分的比例,当Co/Ni摩尔比为1：2时,具有最高的转化率和选择性。此外,Co的引入能够大大抑制积碳,在一定程度上增加了催化剂的稳定性。
5.SiO2壳层孔结构的改变,对催化活性有一定的影响。在使用PVP扩孔时,对甲烷转化率影响微小,而对H2的选择性影响较大,这表明壳层结构会影响分子的扩散。当采用CTAB扩孔时,疏松的壳层结构会减弱核壳间的相互作用,致使催化活性有所下降。
6.对Ni基核壳结构催化剂掺杂其他元素(如La、Ce、Cu等)可以调变催化剂的性能。研究表明,在甲烷转化率及H2和CO的选择性方面,La的掺杂明显优于其他元素；Ce和Cu的添加没有显著的促进作用,而Ba和Fe的掺杂对催化活性是不利的,尤其是Fe的掺杂,大大降低了催化活性。通过相关的表征手段和催化活性考察,可以发现,La掺杂的催化剂具有高效、稳定、抗积碳的特点。
7.核壳结构纳米催化剂在POM反应中高的催化活性源自：一方面为纳米尺寸效应,即Si02壳层能够有效隔离纳米粒子,防止其在高温反应下的聚集或烧结,更好地发挥纳米粒子的特性。另一方面,特殊的核壳结构,存在着一定的核壳间相互作用,以及含有空腔纳米反应器的限阈效应。
Natural gas conversion and utilization is very important in the fields of petrochemical and alternative energy resources. The conversion of methane to synthesis gas (syngas) will be a key step for value-added products, fuel cell, and power plant applications. Compared with the conventional steam reforming of methane, the partial oxidation of methane (POM) to syngas attracted extensive attentions due to its efficient energy-saving advantage.
The application of nanoparticles (NPs) in heterogeneous catalysis is highly desirable due to the intrinsic "surface effects". Unfortunately, NPs are unstable and aggregate easily especially at elevated temperatures. Enwrapping a nano-material in a stable and porous shell can enhance the thermal stability of the core material and in addition, may cause a change in electron charge, reactivity and functionality of enwrapped material. Core-shell structured materials have attracted great attentions because of the unique structural feature and physicochemical properties.
In the present thesis, we focused on the design and development of novel core-shell structured nanocatalysts and its application in POM. It was found that the catalytic performance can be modified by tuning the morphology, structure, size, and element composition of catalyst. Together with the characterization of catalysts and evaluation of catalytic performance, the major conclusions can be derived as follows:
1. NPs with different size and morphology can be encapsulated with a layer of microporous/mesoporous SiO2by a modified sol-gel method. The metal oxide cores can be in-situ reduced in hydrogen to generate metal cores for catalysis.
2. The application of certain surfactants (PVP and CTAB) in encapsulation has a significant impact on the property of the shell material, especially for the porosity of SiO2shell. The relatively homogeneous core-shell morphology with a higher fraction of mesopores can be obtained by adoption of PVP. In the case of CTAB, a higher porosity of SiO2shell can be achieved, with a larger specific surface area of catalyst.
3. The catalytic performance of a core-shell catalyst was mainly determined by the size of Ni cores in the POM reaction. And the smaller the size is; the higher activity will be. The structure-performance relationship has been established in the present study. An effective correlation between the core particle size and catalytic activity can also be obtained due to the high stability of core-shell structured catalysts at elevated temperatures. In addition, it was found that less carbon deposition occurred on the smaller sized Ni cores.
4. The catalytic activity of POM is strongly dependent on the proportion of Co in the binary Co-Ni cores. The best conversion and selectivity can be obtained over the core-shell catalyst with a molar ratio of Co/Ni=1:2. Co addition to Ni can also greatly suppress carbon deposition, and thus enhance catalyst stability.
5. The porosity of SiO2shell showed a certain impact on the catalytic activity. The shell structure of different porosity can play a role in molecule diffusion. When the PVP was adopted in catalyst preparation, the methane conversion changed slightly, while the H2selectivity was increased obviously. When the CTAB was applied in catalyst preparation, a much looser shell structure was generated, which weakens the core-shell interaction and further affects the catalytic activity.
6. The Ni-based core-shell catalysts doped with the elements such as La, Ce, Ba, and Cu, etc showed different catalytic behaviors. It was found that the La-doped catalyst outperformed the counterparts. The core-shell catalyst doped with Ce and Cu did not notably enhance the activity. While dopping of Ba and Fe to the Ni-based catalyst showed unfavorable effect, especially for Fe doping. The results of characterization and evaluation suggested that La doping caused less coking as well as anti-sintering of Ni NPs in the POM reaction.
7. The superior catalytic activities of the core-shell structured catalysts for POM are thought to be the consequence of the following factors:on one hand, the nano-sized core particles are effectively isolated by the silica shells which prevent aggregation or sintering of core NPs at high reaction temperatures of POM. On the other hand, the core-shell structured catalysts involve a strong core-shell interaction, and also provide the confined enviroment of a microcapsular-like reactor in which the enrichment of reactants would occur.
纳米材料因其独特的“表面效应”而在多相催化领域受到青睐。然而,纳米粒子在较高温度下不稳定,容易聚集,从而失去了本身固有的优势。因此,将纳米粒子包裹上一层多孔且稳定的壳层,既能提高纳米材料的热稳定性,又能改变它的表面电荷密度、反应性和多功能性。这类核壳结构材料由于其独特的结构和物理化学性质引起了广泛的关注。
本文立足于核壳结构纳米催化剂的设计与开发,并将其用于甲烷选择性氧化制取合成气的研究。通过精细调变形貌、结构、尺寸和元素组成,结合其在催化反应中的催化活性和相关的表征分析,我们对核壳结构纳米催化剂的特点及其在POM反应中的性能表现,获得如下认识：
1.不同尺寸与形貌的CuO、NiO纳米粒子,分别借助于超声或搅拌的手段,能够以溶胶-凝胶的方法将其包裹上一层微孔/介孔SiO2材料。所包裹的氧化物纳米材料,最终可通过H2原位还原的方法,转变为零价的活性组分。
2.核壳结构材料制备过程中,表面活性剂(PVP、CTAB)的添加与否,对壳层孔结构产生很大的影响。未添加表面活性剂,所得到的核壳结构形貌大小不是很均一,微孔居多。而加入表面活性剂PVP后,能够得到相对均一、形貌结构明显的核壳结构,且壳层具有较多的介孔。CTAB的加入,使得SiO：壳层具有更发达的孔结构,比表面积大。
3.核壳结构纳米催化剂的性能取决于Ni核尺寸的大小,研究发现,在POM反应中,在6-45nm尺寸范围,核粒子越小活性越高。建立了催化剂活性与Ni核粒子尺寸之间的构-效关系,同时,高温稳定的核壳结构纳米催化剂又为高温反应下纳米粒子尺寸与活性的关联提供了有效的策略。此外,积碳与核尺寸大小也有关联,小尺寸的Ni粒子能够较好地抑制表面积碳。
4.POM反应的催化活性强烈依赖于Co-Ni双组分的比例,当Co/Ni摩尔比为1：2时,具有最高的转化率和选择性。此外,Co的引入能够大大抑制积碳,在一定程度上增加了催化剂的稳定性。
5.SiO2壳层孔结构的改变,对催化活性有一定的影响。在使用PVP扩孔时,对甲烷转化率影响微小,而对H2的选择性影响较大,这表明壳层结构会影响分子的扩散。当采用CTAB扩孔时,疏松的壳层结构会减弱核壳间的相互作用,致使催化活性有所下降。
6.对Ni基核壳结构催化剂掺杂其他元素(如La、Ce、Cu等)可以调变催化剂的性能。研究表明,在甲烷转化率及H2和CO的选择性方面,La的掺杂明显优于其他元素；Ce和Cu的添加没有显著的促进作用,而Ba和Fe的掺杂对催化活性是不利的,尤其是Fe的掺杂,大大降低了催化活性。通过相关的表征手段和催化活性考察,可以发现,La掺杂的催化剂具有高效、稳定、抗积碳的特点。
7.核壳结构纳米催化剂在POM反应中高的催化活性源自：一方面为纳米尺寸效应,即Si02壳层能够有效隔离纳米粒子,防止其在高温反应下的聚集或烧结,更好地发挥纳米粒子的特性。另一方面,特殊的核壳结构,存在着一定的核壳间相互作用,以及含有空腔纳米反应器的限阈效应。
Natural gas conversion and utilization is very important in the fields of petrochemical and alternative energy resources. The conversion of methane to synthesis gas (syngas) will be a key step for value-added products, fuel cell, and power plant applications. Compared with the conventional steam reforming of methane, the partial oxidation of methane (POM) to syngas attracted extensive attentions due to its efficient energy-saving advantage.
The application of nanoparticles (NPs) in heterogeneous catalysis is highly desirable due to the intrinsic "surface effects". Unfortunately, NPs are unstable and aggregate easily especially at elevated temperatures. Enwrapping a nano-material in a stable and porous shell can enhance the thermal stability of the core material and in addition, may cause a change in electron charge, reactivity and functionality of enwrapped material. Core-shell structured materials have attracted great attentions because of the unique structural feature and physicochemical properties.
In the present thesis, we focused on the design and development of novel core-shell structured nanocatalysts and its application in POM. It was found that the catalytic performance can be modified by tuning the morphology, structure, size, and element composition of catalyst. Together with the characterization of catalysts and evaluation of catalytic performance, the major conclusions can be derived as follows:
1. NPs with different size and morphology can be encapsulated with a layer of microporous/mesoporous SiO2by a modified sol-gel method. The metal oxide cores can be in-situ reduced in hydrogen to generate metal cores for catalysis.
2. The application of certain surfactants (PVP and CTAB) in encapsulation has a significant impact on the property of the shell material, especially for the porosity of SiO2shell. The relatively homogeneous core-shell morphology with a higher fraction of mesopores can be obtained by adoption of PVP. In the case of CTAB, a higher porosity of SiO2shell can be achieved, with a larger specific surface area of catalyst.
3. The catalytic performance of a core-shell catalyst was mainly determined by the size of Ni cores in the POM reaction. And the smaller the size is; the higher activity will be. The structure-performance relationship has been established in the present study. An effective correlation between the core particle size and catalytic activity can also be obtained due to the high stability of core-shell structured catalysts at elevated temperatures. In addition, it was found that less carbon deposition occurred on the smaller sized Ni cores.
4. The catalytic activity of POM is strongly dependent on the proportion of Co in the binary Co-Ni cores. The best conversion and selectivity can be obtained over the core-shell catalyst with a molar ratio of Co/Ni=1:2. Co addition to Ni can also greatly suppress carbon deposition, and thus enhance catalyst stability.
5. The porosity of SiO2shell showed a certain impact on the catalytic activity. The shell structure of different porosity can play a role in molecule diffusion. When the PVP was adopted in catalyst preparation, the methane conversion changed slightly, while the H2selectivity was increased obviously. When the CTAB was applied in catalyst preparation, a much looser shell structure was generated, which weakens the core-shell interaction and further affects the catalytic activity.
6. The Ni-based core-shell catalysts doped with the elements such as La, Ce, Ba, and Cu, etc showed different catalytic behaviors. It was found that the La-doped catalyst outperformed the counterparts. The core-shell catalyst doped with Ce and Cu did not notably enhance the activity. While dopping of Ba and Fe to the Ni-based catalyst showed unfavorable effect, especially for Fe doping. The results of characterization and evaluation suggested that La doping caused less coking as well as anti-sintering of Ni NPs in the POM reaction.
7. The superior catalytic activities of the core-shell structured catalysts for POM are thought to be the consequence of the following factors:on one hand, the nano-sized core particles are effectively isolated by the silica shells which prevent aggregation or sintering of core NPs at high reaction temperatures of POM. On the other hand, the core-shell structured catalysts involve a strong core-shell interaction, and also provide the confined enviroment of a microcapsular-like reactor in which the enrichment of reactants would occur.
引文
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