介孔材料的定向设计合成及其催化应用
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摘要
由于具有高的比表面积、规则有序的孔道排列、可调的孔径大小、较窄的孔径分布以及大的孔容等一系列特性,近年来介孔材料已经引起了各方面的广泛关注,并且已经成为纳米结构材料和催化领域中最为活跃的研究领域之一。本论文针对目前介孔材料研究领域内的三个前沿方向,即:硅基介孔材料的定向控制合成、非硅基多元介孔材料的合成、以及介孔材料的功能化,相应地开展了一系列研究,并探索了所合成的非硅基介孔材料的一些催化应用。主要研究内容如下:
在硅基介孔材料的定向控制合成方面(论文第2章),首先研究了温度对于MSU介孔材料合成过程的调控作用,关于在低于冰点的低温条件下进行MSU介孔材料的合成,目前尚未见有文献报道;在高于表面活性剂浊点温度的高温下进行MSU介孔材料的合成则被学术界认为是不可能的。我们的研究在国际上首次成功地在远低于冰点温度和远高于浊点温度条件下合成出了MSU介孔材料,从而将MSU介孔材料的合成温度范围拓展到了-25~140℃的范围。并且通过调节合成温度,实现了对所合成MSU的孔径、孔容、比表面积、孔道结构、以及微观形貌等织构性能的定向控制。发现在高温下所合成的MSU介孔材料具有多级孔分布,探讨了其可能的形成机理。接着研究了添加小分子添加剂环己烷对于MSU介孔材料合成过程的调控作用。发现通过调节环己烷在合成体系中的含量,也可以达到定向控制MSU的孔道和形貌等织构特征的目的。相对于温度控制的定向合成,在环己烷存在的情况下,高温下出现二级孔道的现象得到了较好的抑制。随着合成体系中环己烷添加量的增加,所合成出的介孔材料从蠕虫状结构向层状结构转变,同时,其形貌也由原来的实心球形转变成了空心囊泡,即实现了从MSU-1向MSU-V的转变。这种结果未见有文献报道。最后研究了合成温度对于MCM-41孔道结构和形貌的影响。研究结果表明,在低至-10℃的温度下仍然可以合成出具有完好孔道结构的MCM-41介孔材料。相对于较高温度下的合成,低温条件下所合成的MCM-41具有更小的颗粒度和更加连续的形貌。提出了合成温度影响MCM-41微观形貌的可能机理。
在非硅基介孔材料的合成与应用(论文的第3~7章)方面,在第3章中,以AEO9为表面活性剂模板,利用凝胶-溶胶路线成功地合成出了具有孔径分布均一和比表面大等特点的Ti-O-Co二元复合非硅基介孔材料Meso-Ti-Co。对Meso-Ti-Co进行了详细的表征,证实其具有介孔材料的完整的特征,Co物种完全进入孔壁骨架内部。考查了Meso-Ti-Co的合成工艺,给出了最佳工艺条件。通过自行设计的装置,考查了各介孔材料的催化氧化环己烷的催化性能。结果表明使用介孔催化剂转化率和选择性均要高于其他同类别催化剂,环己烷的转化率可以达到7.97%,环己醇和环己酮的选择性达到93.69%。催化剂的重复性非常好。
在第4章中,采用MSU介孔材料作为硬模板,通过纳米复制的方法成功地合成出了Ti-O-Co二元介孔材料。得到的Ti-O-Co二元介孔材料孔道结构同模板相似,表征显示Co已经进入骨架。将该系列材料进行光催化氧化降解甲基橙染料实验,发现无论是在紫外灯下还是太阳光下,介孔Ti-O-Co二元复合材料具有比普通二氧化钛高得多的活性。
在第5章中,开发了一种合成Ti-Ag介孔材料的新方法,即高分子网络模板法。该方法以三乙醇胺为碱催化剂催化甘油聚合生成聚甘油高分子网络以及TBOT的水解,自身即可形成介观结构。Ag离子与三乙醇胺的配位,降低了三乙醇胺的碱度,通过改变Ag离子的含量,可以调节聚甘油高分子网络的聚合度和交联度。通过超分子组装,得到一系列不同Ag/Ti比的Ti-Ag氧化物介孔材料。对其进行表征,结果显示,Ti-Ag氧化物介孔材料具有良好的孔隙性和高比表面积。Ag/Ti比较低时,Ag嵌入到了组成介孔孔壁的锐钛矿TiO2晶格中;Ag/Ti比较高时,部分Ag以金属簇的形式嵌于孔壁中。以具代表性的革兰氏阳性细菌和阴性细菌,真菌为实验菌种,利用该材料进行光催化杀菌,发现该材料是高效、广谱、MIC很小的抗菌剂。Ti-Ag氧化物介孔材料良好的光催化杀菌性能得益于其介孔结构以及锐钛矿TiO2与Ag金属簇之间的协同光催化作用。
在第6章中,基于第5章所开发的高分子网络模板法,进一步合成了含有其它过渡金属的Ti-M氧化物多元非硅基介孔材料。检测结果显示M组分进入了骨架,所有产物都具有介孔孔道结构,比表面积大,孔壁由锐钛矿纳米晶粒构成。分别取相应的Ti-M氧化物介孔材料进行催化氧化反应,发现这些材料用于光催化氧化环己烷反应,可以达到2.8%的转化率,比前人研究的最好结果增加了近10倍;当将该系列材料用于乳酸脱水和氧化制备丙酮酸和丙烯酸的时候,也比普通的负载型催化剂要高得多,并且由于M金属组分处于骨架中,其在反应前后不会流失,催化剂的催化性能重复性非常好。
在第7章中,成功合成了两种典型的具有磁性的壳-核纳米的硅基多孔材料。一种是具有微孔孔道的钛硅分子筛TS-1磁性材料,通过其对磁核的包覆,合成出来了壳核磁性纳米MTS颗粒。在该体系中得到的MTS颗粒与普通TS-1相比,颗粒要小很多,是典型的纳米颗粒,氮气吸附试验结果表明产物仍具有发达的微孔体系。将MTS应用到苯酚催化氧化制备苯二酚的反应中,其催化性能相对于纯的TS分子筛要高一些,重复性也非常好。同时,反应后的MTS可以很好的利用磁场回收,这对于成本高,价格贵的TS分子筛而言具有非常重要的意义。第二种是具有介孔孔道的硅基MSU介孔磁性材料MMSU,在证实其具有较好的磁性的同时,该材料仍然具有极高的比表面积和均一的介孔分布。
Because of their high specific surface area, large pore volume, ordered pore array, adjustable and narrowly pore size distribution, mesoporous materials have been paid much attentions in the fields of both the material and catalysis science for the past decade. Significantly large progresses were already attained on the studies of mesoporous materials, with numerous papers being published in various kinds of journals all over the world. A few aspects of this kind of materials, such as, the directionally controlled synthesis of mesoporous silica, the synthesis of non-silica mesoporous materials and the functionalization of mesoporous materials, however, are still waiting for further exploration. These topics constitute, in fact, the difficulties and focuses currently in the filed of mesoporous materials and are what the present dissertation was concerned about. Besides, some catalytic applications of the non-silica mesoporous materials synthesized in this dissertation were also addressed.
The first part of the dissertation, i.e., the chapter 2, dealt mainly with the directionally controlled synthesis of mesoporous silica.
Temperature is one of the most important influencing factors for the synthesis of mesoporous materials. MSU-type mesoporous materials are usually synthesized at a temperature ranging of above the ice point of water and below the cloud point of surfactant. No report on the synthesis of MSU at a temperature below the ice point of water could be found in literatures, and it was even believed that a MSU mesostructure could not be generated when the temperature was higher than the cloud point of the surfactant. In this dissertation, it was found, however, that the applicable range of temperature for the synthesis of MSU could be extended largely to that from far below the ice point of water (-25 oC) to much higher than the cloud point (140 oC). The textural properties of the MSU synthesized had been regulated by changing the synthesizing temperature. The MSU synthesized at a temperature higher than the cloud point of surfactant was identified to possess a multimodal mesoporous structure. A possible mechanism had been proposed for the above variation of mesoporous structure with the temperature.
The effect of addition of small molecular additive, cyclohexane, to the batch for the synthesis of MSU was, for the first time, investigated systematically. The addition of cyclohexane had been proved to be cable of another approach, besides changing the synthesizing temperature, to regulate the textural properties of MSU. It was observed that, with the increase of the amount of cyclohexane, the MSU synthesized suffered from a transformation from a wormlike mesostructure to a lamellar one, while its morphology changed from solid balls to hollow vesicles, being an indicative of a transformation of MSU-1 to MSU-V. For the temperature higher than the cloud point of surfactant, the MSU synthesized in the presence of cyclohexane displayed a monomodal mesoporous structure, being in contrast to a multimodal one synthesized in the absence of cyclohexane.
The control of the textural properties of MCM-41 had been achieved by changing the synthesizing temperature. It was found that MCM-41 could be synthesized at a temperature as low as -10 oC. The textural properties of MCM-41 changed continuously with temperature, and the crystal size of the MCM-41 synthesized at a low temperature had a much smaller particle size and smooth surface than at a high temperature. To interpret the change of the textural properties with temperature, a possible mechanism had been proposed.
The second part of this dissertation, involving chapters 3~7, were concerned about the synthesis of non-silica mesoporous materials and their and catalytic applications and the.
In chapter 3, mesoporous Ti-Co oxides were synthesized via the sol-gel route, being a supramolecular assembly of the surfactant AEO9. The mesoporous Ti-Co oxides synthesized were identified to possess a high specific surface area, narrowly distributed pore size and a pore wall consisting of the Co-incorporated anatase crystals. The mesoporous Ti-Co oxides had been employed, for the first time, as the catalysts for the oxidation of cyclohexane and a considerable high performance were achieved. An as high as 8.0 % conversion of cyclohexane at a 93.7 % selectivity to KA oil (cyclohexanol and cyclohexanone) had been obtained under the optimal conditions.
In chapter 4, mesoporous Ti-Co oxides were synthesized via a replication route, using MSU as the hard template. The mesoporous Ti-Co oxides synthesized were identified to possess a similar mesostructure with the hard template. The pore wall of the mesostructure comprised of the Co-incorporated anatase crystals. When employed as the photocatalysts for the degradation of dye, the mesoporous Ti-Co oxides presented a much higher activity than the pure TiO2, under whether UV or sunlight irradiation.
In chapter 5, mesoporous Ti-Ag oxides were synthesized via a supramolecular assembly of polyglycerol, using TBOT and AgNO3 as inorganic sources and glycerol and triethanolamine as organic sources. The template polyglycerol was in situ generated, being catalyzed by the triethanolamine. Because of the coordination with Ag+ ion, the alkalinity of triethanolamine was reduced, and thus, the degrees of the polymerization and crosslinking of polyglycerol could be regulated by changing the molar ratio of Ag/Ti. Through this way, a series of mesoporous Ti-Ag oxides with various Ag/Ti molar ratios had been synthesized. The characterizations to the mesoporous Ti-Ag oxides mesoporous showed that these materials possessed a considerably high BET specific surface area and porosity, with their pore walls consisting of Ag-containing anatase crystals. It was found that, at a lower Ag/Ti molar ratio, the Ag+ ions were incorporated into the framework of the anatase, while at a higher Ag/Ti molar ratio, a part of the Ag+ ions segregate as Ag clusters from the framework of anatase, covering partially the surfaces of the anatase crystals. The mesoporous Ti-Ag oxides synthesized had been employed as the photocatalysts in the antibacterial experiments, using several typical bacteria. It was shown that these mesoporous materials possessed a broad-spectrum antibacterial performance, with a high efficiency and low MIC, which is benefited from the mesostructures and the concerted photocatalysis between the anatase crystals and Ag clusters.
In chapter 6, numerous mesoporous Ti-M oxides were synthesized using the method developed in chapter 5. All the Ti-M oxides were identified to posses a mesostructure, with a high BET specific surface area, uniform mesopores and narrow pore size distribution. It suggests that the novel method developed in chapter 5 is of appreciable universality. The catalytic performances of the mesoporous Ti-O-M oxides synthesized had been evaluated by a few reactions, such as, the photocatalytic oxidation of cyclohexane, the dehydration of lactic acid to acrylic acid and the oxidative dehydrogenation of lactic acid to pyruvic acid. For the photocatalytic oxidation of cyclohexane, an as high as 2.8 % conversion of cyclohexane, being ten times of the best result ever reported in literatures. For the dehydration of lactic acid to acrylic acid and the oxidative dehydrogenation of lactic acid to pyruvic acid, much higher performances were obtained over the mesoporous Ti-M oxide catalysts than over the supported M/Ti oxide catalysts. It was also found that the mesoporous Ti-M oxide catalysts displayed a considerable stability during the above reaction, with almost no leaching of the active metal component M, due to the incorporation of the component M into the framework of the anatase crystals.
The third part of the dissertation, i.e., the chapter 8, dealt mainly with the functionalization of mesoporous materials. Two kinds of magnetic core-shell mesostructured materials, namely MTS and MMSU, were prepared respectively by covering the nano-sized magnetic cores, cobalt ferrite, with a sol containing the TS-1 precursors or a sol conventionally used for the synthesis of MSU. The materials prepared were characterized by means of XRD, DRS UV-Vis, SEM, N2-physorption and magnetism determination. It was shown that the MMSU had a morphology of micro-ball with an average diameter of ca. 400 nm and the shell of the micro-ball consisted of the nano-sized MSU particles. The MTS had a morphology of elliptic micro-ball with an average of ca. 200-300 nm, and the shell of the elliptic micro-ball consisted of the nano-sized TS-1 crystals. Both the MMSU and MTS were determined to possess a high BET specific surface area, large pore volume and obvious magnetism. The MTS was also employed as the catalyst for the oxidation of phenol to dihydroxybenzene, and a slightly higher activity was observed over the MTS than over the conventional TS-1. After the reaction, the MTS could be readily recovered by a magnet.
在硅基介孔材料的定向控制合成方面(论文第2章),首先研究了温度对于MSU介孔材料合成过程的调控作用,关于在低于冰点的低温条件下进行MSU介孔材料的合成,目前尚未见有文献报道;在高于表面活性剂浊点温度的高温下进行MSU介孔材料的合成则被学术界认为是不可能的。我们的研究在国际上首次成功地在远低于冰点温度和远高于浊点温度条件下合成出了MSU介孔材料,从而将MSU介孔材料的合成温度范围拓展到了-25~140℃的范围。并且通过调节合成温度,实现了对所合成MSU的孔径、孔容、比表面积、孔道结构、以及微观形貌等织构性能的定向控制。发现在高温下所合成的MSU介孔材料具有多级孔分布,探讨了其可能的形成机理。接着研究了添加小分子添加剂环己烷对于MSU介孔材料合成过程的调控作用。发现通过调节环己烷在合成体系中的含量,也可以达到定向控制MSU的孔道和形貌等织构特征的目的。相对于温度控制的定向合成,在环己烷存在的情况下,高温下出现二级孔道的现象得到了较好的抑制。随着合成体系中环己烷添加量的增加,所合成出的介孔材料从蠕虫状结构向层状结构转变,同时,其形貌也由原来的实心球形转变成了空心囊泡,即实现了从MSU-1向MSU-V的转变。这种结果未见有文献报道。最后研究了合成温度对于MCM-41孔道结构和形貌的影响。研究结果表明,在低至-10℃的温度下仍然可以合成出具有完好孔道结构的MCM-41介孔材料。相对于较高温度下的合成,低温条件下所合成的MCM-41具有更小的颗粒度和更加连续的形貌。提出了合成温度影响MCM-41微观形貌的可能机理。
在非硅基介孔材料的合成与应用(论文的第3~7章)方面,在第3章中,以AEO9为表面活性剂模板,利用凝胶-溶胶路线成功地合成出了具有孔径分布均一和比表面大等特点的Ti-O-Co二元复合非硅基介孔材料Meso-Ti-Co。对Meso-Ti-Co进行了详细的表征,证实其具有介孔材料的完整的特征,Co物种完全进入孔壁骨架内部。考查了Meso-Ti-Co的合成工艺,给出了最佳工艺条件。通过自行设计的装置,考查了各介孔材料的催化氧化环己烷的催化性能。结果表明使用介孔催化剂转化率和选择性均要高于其他同类别催化剂,环己烷的转化率可以达到7.97%,环己醇和环己酮的选择性达到93.69%。催化剂的重复性非常好。
在第4章中,采用MSU介孔材料作为硬模板,通过纳米复制的方法成功地合成出了Ti-O-Co二元介孔材料。得到的Ti-O-Co二元介孔材料孔道结构同模板相似,表征显示Co已经进入骨架。将该系列材料进行光催化氧化降解甲基橙染料实验,发现无论是在紫外灯下还是太阳光下,介孔Ti-O-Co二元复合材料具有比普通二氧化钛高得多的活性。
在第5章中,开发了一种合成Ti-Ag介孔材料的新方法,即高分子网络模板法。该方法以三乙醇胺为碱催化剂催化甘油聚合生成聚甘油高分子网络以及TBOT的水解,自身即可形成介观结构。Ag离子与三乙醇胺的配位,降低了三乙醇胺的碱度,通过改变Ag离子的含量,可以调节聚甘油高分子网络的聚合度和交联度。通过超分子组装,得到一系列不同Ag/Ti比的Ti-Ag氧化物介孔材料。对其进行表征,结果显示,Ti-Ag氧化物介孔材料具有良好的孔隙性和高比表面积。Ag/Ti比较低时,Ag嵌入到了组成介孔孔壁的锐钛矿TiO2晶格中;Ag/Ti比较高时,部分Ag以金属簇的形式嵌于孔壁中。以具代表性的革兰氏阳性细菌和阴性细菌,真菌为实验菌种,利用该材料进行光催化杀菌,发现该材料是高效、广谱、MIC很小的抗菌剂。Ti-Ag氧化物介孔材料良好的光催化杀菌性能得益于其介孔结构以及锐钛矿TiO2与Ag金属簇之间的协同光催化作用。
在第6章中,基于第5章所开发的高分子网络模板法,进一步合成了含有其它过渡金属的Ti-M氧化物多元非硅基介孔材料。检测结果显示M组分进入了骨架,所有产物都具有介孔孔道结构,比表面积大,孔壁由锐钛矿纳米晶粒构成。分别取相应的Ti-M氧化物介孔材料进行催化氧化反应,发现这些材料用于光催化氧化环己烷反应,可以达到2.8%的转化率,比前人研究的最好结果增加了近10倍;当将该系列材料用于乳酸脱水和氧化制备丙酮酸和丙烯酸的时候,也比普通的负载型催化剂要高得多,并且由于M金属组分处于骨架中,其在反应前后不会流失,催化剂的催化性能重复性非常好。
在第7章中,成功合成了两种典型的具有磁性的壳-核纳米的硅基多孔材料。一种是具有微孔孔道的钛硅分子筛TS-1磁性材料,通过其对磁核的包覆,合成出来了壳核磁性纳米MTS颗粒。在该体系中得到的MTS颗粒与普通TS-1相比,颗粒要小很多,是典型的纳米颗粒,氮气吸附试验结果表明产物仍具有发达的微孔体系。将MTS应用到苯酚催化氧化制备苯二酚的反应中,其催化性能相对于纯的TS分子筛要高一些,重复性也非常好。同时,反应后的MTS可以很好的利用磁场回收,这对于成本高,价格贵的TS分子筛而言具有非常重要的意义。第二种是具有介孔孔道的硅基MSU介孔磁性材料MMSU,在证实其具有较好的磁性的同时,该材料仍然具有极高的比表面积和均一的介孔分布。
Because of their high specific surface area, large pore volume, ordered pore array, adjustable and narrowly pore size distribution, mesoporous materials have been paid much attentions in the fields of both the material and catalysis science for the past decade. Significantly large progresses were already attained on the studies of mesoporous materials, with numerous papers being published in various kinds of journals all over the world. A few aspects of this kind of materials, such as, the directionally controlled synthesis of mesoporous silica, the synthesis of non-silica mesoporous materials and the functionalization of mesoporous materials, however, are still waiting for further exploration. These topics constitute, in fact, the difficulties and focuses currently in the filed of mesoporous materials and are what the present dissertation was concerned about. Besides, some catalytic applications of the non-silica mesoporous materials synthesized in this dissertation were also addressed.
The first part of the dissertation, i.e., the chapter 2, dealt mainly with the directionally controlled synthesis of mesoporous silica.
Temperature is one of the most important influencing factors for the synthesis of mesoporous materials. MSU-type mesoporous materials are usually synthesized at a temperature ranging of above the ice point of water and below the cloud point of surfactant. No report on the synthesis of MSU at a temperature below the ice point of water could be found in literatures, and it was even believed that a MSU mesostructure could not be generated when the temperature was higher than the cloud point of the surfactant. In this dissertation, it was found, however, that the applicable range of temperature for the synthesis of MSU could be extended largely to that from far below the ice point of water (-25 oC) to much higher than the cloud point (140 oC). The textural properties of the MSU synthesized had been regulated by changing the synthesizing temperature. The MSU synthesized at a temperature higher than the cloud point of surfactant was identified to possess a multimodal mesoporous structure. A possible mechanism had been proposed for the above variation of mesoporous structure with the temperature.
The effect of addition of small molecular additive, cyclohexane, to the batch for the synthesis of MSU was, for the first time, investigated systematically. The addition of cyclohexane had been proved to be cable of another approach, besides changing the synthesizing temperature, to regulate the textural properties of MSU. It was observed that, with the increase of the amount of cyclohexane, the MSU synthesized suffered from a transformation from a wormlike mesostructure to a lamellar one, while its morphology changed from solid balls to hollow vesicles, being an indicative of a transformation of MSU-1 to MSU-V. For the temperature higher than the cloud point of surfactant, the MSU synthesized in the presence of cyclohexane displayed a monomodal mesoporous structure, being in contrast to a multimodal one synthesized in the absence of cyclohexane.
The control of the textural properties of MCM-41 had been achieved by changing the synthesizing temperature. It was found that MCM-41 could be synthesized at a temperature as low as -10 oC. The textural properties of MCM-41 changed continuously with temperature, and the crystal size of the MCM-41 synthesized at a low temperature had a much smaller particle size and smooth surface than at a high temperature. To interpret the change of the textural properties with temperature, a possible mechanism had been proposed.
The second part of this dissertation, involving chapters 3~7, were concerned about the synthesis of non-silica mesoporous materials and their and catalytic applications and the.
In chapter 3, mesoporous Ti-Co oxides were synthesized via the sol-gel route, being a supramolecular assembly of the surfactant AEO9. The mesoporous Ti-Co oxides synthesized were identified to possess a high specific surface area, narrowly distributed pore size and a pore wall consisting of the Co-incorporated anatase crystals. The mesoporous Ti-Co oxides had been employed, for the first time, as the catalysts for the oxidation of cyclohexane and a considerable high performance were achieved. An as high as 8.0 % conversion of cyclohexane at a 93.7 % selectivity to KA oil (cyclohexanol and cyclohexanone) had been obtained under the optimal conditions.
In chapter 4, mesoporous Ti-Co oxides were synthesized via a replication route, using MSU as the hard template. The mesoporous Ti-Co oxides synthesized were identified to possess a similar mesostructure with the hard template. The pore wall of the mesostructure comprised of the Co-incorporated anatase crystals. When employed as the photocatalysts for the degradation of dye, the mesoporous Ti-Co oxides presented a much higher activity than the pure TiO2, under whether UV or sunlight irradiation.
In chapter 5, mesoporous Ti-Ag oxides were synthesized via a supramolecular assembly of polyglycerol, using TBOT and AgNO3 as inorganic sources and glycerol and triethanolamine as organic sources. The template polyglycerol was in situ generated, being catalyzed by the triethanolamine. Because of the coordination with Ag+ ion, the alkalinity of triethanolamine was reduced, and thus, the degrees of the polymerization and crosslinking of polyglycerol could be regulated by changing the molar ratio of Ag/Ti. Through this way, a series of mesoporous Ti-Ag oxides with various Ag/Ti molar ratios had been synthesized. The characterizations to the mesoporous Ti-Ag oxides mesoporous showed that these materials possessed a considerably high BET specific surface area and porosity, with their pore walls consisting of Ag-containing anatase crystals. It was found that, at a lower Ag/Ti molar ratio, the Ag+ ions were incorporated into the framework of the anatase, while at a higher Ag/Ti molar ratio, a part of the Ag+ ions segregate as Ag clusters from the framework of anatase, covering partially the surfaces of the anatase crystals. The mesoporous Ti-Ag oxides synthesized had been employed as the photocatalysts in the antibacterial experiments, using several typical bacteria. It was shown that these mesoporous materials possessed a broad-spectrum antibacterial performance, with a high efficiency and low MIC, which is benefited from the mesostructures and the concerted photocatalysis between the anatase crystals and Ag clusters.
In chapter 6, numerous mesoporous Ti-M oxides were synthesized using the method developed in chapter 5. All the Ti-M oxides were identified to posses a mesostructure, with a high BET specific surface area, uniform mesopores and narrow pore size distribution. It suggests that the novel method developed in chapter 5 is of appreciable universality. The catalytic performances of the mesoporous Ti-O-M oxides synthesized had been evaluated by a few reactions, such as, the photocatalytic oxidation of cyclohexane, the dehydration of lactic acid to acrylic acid and the oxidative dehydrogenation of lactic acid to pyruvic acid. For the photocatalytic oxidation of cyclohexane, an as high as 2.8 % conversion of cyclohexane, being ten times of the best result ever reported in literatures. For the dehydration of lactic acid to acrylic acid and the oxidative dehydrogenation of lactic acid to pyruvic acid, much higher performances were obtained over the mesoporous Ti-M oxide catalysts than over the supported M/Ti oxide catalysts. It was also found that the mesoporous Ti-M oxide catalysts displayed a considerable stability during the above reaction, with almost no leaching of the active metal component M, due to the incorporation of the component M into the framework of the anatase crystals.
The third part of the dissertation, i.e., the chapter 8, dealt mainly with the functionalization of mesoporous materials. Two kinds of magnetic core-shell mesostructured materials, namely MTS and MMSU, were prepared respectively by covering the nano-sized magnetic cores, cobalt ferrite, with a sol containing the TS-1 precursors or a sol conventionally used for the synthesis of MSU. The materials prepared were characterized by means of XRD, DRS UV-Vis, SEM, N2-physorption and magnetism determination. It was shown that the MMSU had a morphology of micro-ball with an average diameter of ca. 400 nm and the shell of the micro-ball consisted of the nano-sized MSU particles. The MTS had a morphology of elliptic micro-ball with an average of ca. 200-300 nm, and the shell of the elliptic micro-ball consisted of the nano-sized TS-1 crystals. Both the MMSU and MTS were determined to possess a high BET specific surface area, large pore volume and obvious magnetism. The MTS was also employed as the catalyst for the oxidation of phenol to dihydroxybenzene, and a slightly higher activity was observed over the MTS than over the conventional TS-1. After the reaction, the MTS could be readily recovered by a magnet.
引文
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