介孔材料水热稳定性的改进及新型介孔碳材料的水相合成
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摘要
1992年，Mobil公司的科学家们利用阳离子表面活性剂与无机硅物种在碱性条件下组装得到了M41S系列介孔硅(铝)分子筛，得到的介孔分子筛具有大的表面积，二维／三维有序排列且尺寸均一可调的孔道，从而将分子筛的规则孔径从微孔范围扩展到介孔领域。科学家们对介孔材料的研究投入了极大的热情，近年来，新的组成、新的结构、新的概念、新的应用层出不穷，介孔材料也成为了一个跨材料、化学、物理、生物等多学科的国际热点前沿领域。介孔材料的研究方兴未艾，对已有材料的性质研究和性能改进，新合成路线的探索，新材料的合成等仍是充满了探求的研究热点。
本论文主要分为两个部分：第一部分中，对介孔氧化硅SBA-15的水热稳定性进行了系统研究，并提出了新的方法提高其稳定性；第二部分中主要是新合成方法的探索以及新材料的合成，通过水相法合成新的介孔碳材料，在水／油体系合成双孔介孔材料。
在第二章中，系统地研究了SBA-15和A1-SBA-15在600以及800℃水蒸汽中的水热稳定性。研究结果表明，SBA-15墙壁上Si-O-Si化学键的交联度以及墙壁厚度是影响其水热稳定性的主要因素。高温焙烧可以有效地提高SBA-15的水热稳定性，但是由于高温焙烧导致的骨架收缩，会降低材料的孔容以及比表面。因此，作者提出了一种碳保护高温焙烧的方法改善材料的水热的稳定性。这种方法处理过后的介孔材料，有着非常高的水热稳定性，在600℃的水蒸汽中可以稳定超过24h，在800℃水蒸汽中稳定超过12h，达到了工业应用的要求。研究结果表明Al-SBA-15的结构很稳定，在800℃水蒸汽中可以稳定12h以上，然而其酸性的稳定性较差，以异丙苯裂化反应为探针，发现600℃处理3 h，其转化率降至＜1％，说明水热处理对其酸性中心的破坏还是很严重的。NMR结果表明，水热处理过程中骨架Al发生了水解变成了非骨架铝，造成了酸性的破坏。
在第三章中，在油包水(W／O)体系中，利用嵌段共聚物P123为模板剂，成功地合成了小孔在5-10nm均一可调，大孔约30nm的双孔介孔材料。液体石蜡由平均碳链为C_(18)-C_(20)的烷烃构成，由于碳链较长，对P123的增容能力较差，因此在与体系中的硅物种组装时会得到两类不同大小的介孔，一种是P123为模板得到的，另一种则是以液体石蜡分子增容P123为模板得到。由于组装是在W／O界面发生，因此，这两类介孔在材料中的存在区域是相互交叉，混合均匀。双孔材料中的小孔是以P123为模板得到的，因此通过调变后处理温度，可以在5-10 nm间连续变化。在材料中还存在这一定数量的微孔(最高达0.08cm~3／g)。另外，得到的材料的具有薄片或者空心球的宏观形貌，厚度为100-200nm。通过改变P123与TEOS的浓度可以有效地控制其形貌。
在第四章中，提出了一种过程简单的水相中合成介孔碳的方法。在碱性溶液中，利用三嵌段共聚物(P123，F127)与低分子量酚醛树脂(苯酚／甲醛)的有机—有机自组装，成功地合成出了一系列具有二／三维有序结构的介孔碳(FDU-14，FDU-15和FDU-16)，并提出了水相中单层氢键诱导有机—有机自组装合成介孔碳的机理。以P123(EO_(20)PO_(70)EO_(20))为模板，合成得到了具有双连续立方结构(Ia3d)的FDU-14，减小溶液中P123／phenol的比例，会发生从Ia3d到p6m的相转变，但无法得到纯的p6m相。以长链烷烃为增容剂，P123为模板，可以成功地合成具有二维六方结构的介孔碳FDU-15(p6m)，通过使用不同链长的烷烃(癸烷，十六烷)，可以在4.1-6.8nm有效地调节FDU-15的孔径。使用具有较大亲水／疏水比的嵌段共聚物F127(EO_(106)PO_(70)EO_(106))为模板，合成得到了具有体心立方结构的介孔碳FDU-16(Im3m)。
在第五章中，通过水相中嵌段共聚物F127与酚醛树脂前驱体自组装的方法合成了介孔碳FDU-16(Im3m)单晶。得到的FDU-16单晶为菱形正十二面体，尺寸约5μm。TEM和SEM研究发现，FDU-16单晶的12个面均为{110}，进一步的研究发现FDU-16晶体生长是从12个{110}面的中心按照layer-by-layer方式生长。采用混合表面活性剂(F127和P123)为模板，成功地得到了具有“铁饼”状形貌的FDU-15。改变表明活性剂浓度，FDU-15的直径可以得在0.5-10μm间调变。FE-SEM实验可以直接观察FDU-15的孔道沿“铁饼”的圆周方向生长。
Ordered mesoporous materials were first discovered by researchers of Mobil Company in 1992. For their unique properties and thus derived great potential application in catalysis, sorption, sensors, biology etc, mesoporous materials soon became one of the hottest research fields in the world. To date, numerous mesoporous materials with variable composition, structure, pore size, functions etc have been obtained, and more synthetic pathways and application fields have been explored and demonstrated. However, there are still a lot of questions to answer and many problems to solve in the research fields on mesoporous materials.
This thesis mainly focuses on two aspects: 1) Systematically investigate the hydrothermal stability of SBA-15 and find effective methods to improve it. 2) Explore new synthetic pathway and synthesize novel materials. Explore an aqueous route to synthesize novel mesoporous carbon materials. Synthesize bimodal mesoporous silica in a W/O system.
In chapter 2, the effect of the pore wall structure, of samples on the hydrothermal stability of pure silica SBA-15 in pure steam at 600 and 800℃, which is similar to industrial condition, was systematically investigated. In the steam of 600℃, SBA-15 materials show very good hydrothermal stability and the materials with thicker walls and more micropores possess better stability. The structures of SBA-15 materials are easily destroyed under steam of 800℃. High-temperature thermal treatment is proved to be an effective method to increase the polymerization degree and improve the hydrothermal stability. Nevertheless it will cause severe shrinkage of the mesopores. A carbon-propping approach was proved to dramatically increase the hydrothermal stability of SBA-15 under such critical condition, in pure steam of 800℃for 12 h. Al-SBA-15 shows very good hydrothermal stability in steam of 800℃(> 12 h). Nevertheless, Al-SBA-15 lost most of its acidity after steam treatment at 600℃for 3 h, which is a result of the hydrolyzation of framework Al.
In chapter 3, novel bimodal ordered mesoporous silica materials possessing tunable small pore of 5-10 nm and large pore of- 30 nm were synthesized by using triblock copolymer P123 as a template and liquid paraffin as a swelling agent in the water-in-oil (W/O) system following a solution sol-gel pathway. The solubility of liquid paraffin in P123 solution is much smaller than that of TMB or other short chain hydrocarbon. Thus, two types of micelles may exist in the liquid paraffin/P123/HCl/ H_2O solution. After the addition of TEOS, bimodal mesoporous materials are formed on the W/O surface as a result of the co-assembly of the two types of micelles with inorganic precursors (TEOS) at the same time. The two length scale pores are all uniform and well-controlled framework pores and homogeneously interconnected. The small pores are derived from the micelles of P123 and the pore size can be easily tuned from 5 to 10 nm by varying the aging temperature. The bimodal mesoporous materials display morphologies of thin sheets or shells of hollow spheres, with a thickness of 100 - 200 nm, which can be tuned by varying the P123 concentration.
In chapter 4, a facile aqueous route to synthesize ordered mesoporous carbon frameworks with tailored mesostructures (Im3m, p6m, and Ia3d) and well controlled morphologies were demonstrated by employing the organic-organic cooperative self-assembly of resols and triblock copolymers. Mesoporous carbons FDU-14 (Ia3d) with bicontinuous cubic structure were synthesized by using Pluronic P123 (EO20PO70EO20) as a template. A mesophase transformation from Ia3d to p6m was observed as the P123/phenol ratio decreased. Hydrocarbons were employed as swelling agents in the organic-organic self-assembly, and 2-D hexagonal (p6m) mesoporous carbons FDU-15 were successfully obtained as a result. The pore size of the obtained FDU-15 can be tuned from 4.1 to 6.8 nm by varying the hydrocarbon molecules. Highly ordered mesoporous carbons FDU-16 with body-centered cubic structure (Im3m) were first obtained from the aqueous route by using Pluronic F127 (EO_(106)PO_(70)EO_(106)) with a large PEO segment as a template. The morphology of the obtained carbons can be controlled on the micrometer scale (FDU-15, FDU-16) or millimeter scale (small pellets of 1-5 mm). One-layer hydrogen bond interaction between resols and PEO segments was proposed to be the essential driving force that induces the organic-organic cooperative assembly.
In chapter 5, 3-D cubic mesoporous carbon FDU-16 single-crystals were prepared by employing an aqueous solution induced organic-organic assembly of triblock copolymer F127 and phenol/formaldehyde resols. The morphologies of the obtained materials are perfect rhombdodecahedron with the uniform size of - 5μm, which are commensurate with the crystallographic point group symmetry (Im3m). The scanning electron microscope (SEM) and transmission electron microscope (TEM) images directly show a layer-by-layer growth mode of face-centered cubic FDU-16 mesostructured carbon single-crystals from the centers of twelve {110} planes. Simultaneously, 2-D hexagonal mesoporous carbon FDU-15 crystals with discus-like morphologies are the products if mixed templates of F127 and P123 are used. The ordered circular mesopore channels with hexagonal packing of FDU-15 can be directly observed by the FE-SEM images.
本论文主要分为两个部分：第一部分中，对介孔氧化硅SBA-15的水热稳定性进行了系统研究，并提出了新的方法提高其稳定性；第二部分中主要是新合成方法的探索以及新材料的合成，通过水相法合成新的介孔碳材料，在水／油体系合成双孔介孔材料。
在第二章中，系统地研究了SBA-15和A1-SBA-15在600以及800℃水蒸汽中的水热稳定性。研究结果表明，SBA-15墙壁上Si-O-Si化学键的交联度以及墙壁厚度是影响其水热稳定性的主要因素。高温焙烧可以有效地提高SBA-15的水热稳定性，但是由于高温焙烧导致的骨架收缩，会降低材料的孔容以及比表面。因此，作者提出了一种碳保护高温焙烧的方法改善材料的水热的稳定性。这种方法处理过后的介孔材料，有着非常高的水热稳定性，在600℃的水蒸汽中可以稳定超过24h，在800℃水蒸汽中稳定超过12h，达到了工业应用的要求。研究结果表明Al-SBA-15的结构很稳定，在800℃水蒸汽中可以稳定12h以上，然而其酸性的稳定性较差，以异丙苯裂化反应为探针，发现600℃处理3 h，其转化率降至＜1％，说明水热处理对其酸性中心的破坏还是很严重的。NMR结果表明，水热处理过程中骨架Al发生了水解变成了非骨架铝，造成了酸性的破坏。
在第三章中，在油包水(W／O)体系中，利用嵌段共聚物P123为模板剂，成功地合成了小孔在5-10nm均一可调，大孔约30nm的双孔介孔材料。液体石蜡由平均碳链为C_(18)-C_(20)的烷烃构成，由于碳链较长，对P123的增容能力较差，因此在与体系中的硅物种组装时会得到两类不同大小的介孔，一种是P123为模板得到的，另一种则是以液体石蜡分子增容P123为模板得到。由于组装是在W／O界面发生，因此，这两类介孔在材料中的存在区域是相互交叉，混合均匀。双孔材料中的小孔是以P123为模板得到的，因此通过调变后处理温度，可以在5-10 nm间连续变化。在材料中还存在这一定数量的微孔(最高达0.08cm~3／g)。另外，得到的材料的具有薄片或者空心球的宏观形貌，厚度为100-200nm。通过改变P123与TEOS的浓度可以有效地控制其形貌。
在第四章中，提出了一种过程简单的水相中合成介孔碳的方法。在碱性溶液中，利用三嵌段共聚物(P123，F127)与低分子量酚醛树脂(苯酚／甲醛)的有机—有机自组装，成功地合成出了一系列具有二／三维有序结构的介孔碳(FDU-14，FDU-15和FDU-16)，并提出了水相中单层氢键诱导有机—有机自组装合成介孔碳的机理。以P123(EO_(20)PO_(70)EO_(20))为模板，合成得到了具有双连续立方结构(Ia3d)的FDU-14，减小溶液中P123／phenol的比例，会发生从Ia3d到p6m的相转变，但无法得到纯的p6m相。以长链烷烃为增容剂，P123为模板，可以成功地合成具有二维六方结构的介孔碳FDU-15(p6m)，通过使用不同链长的烷烃(癸烷，十六烷)，可以在4.1-6.8nm有效地调节FDU-15的孔径。使用具有较大亲水／疏水比的嵌段共聚物F127(EO_(106)PO_(70)EO_(106))为模板，合成得到了具有体心立方结构的介孔碳FDU-16(Im3m)。
在第五章中，通过水相中嵌段共聚物F127与酚醛树脂前驱体自组装的方法合成了介孔碳FDU-16(Im3m)单晶。得到的FDU-16单晶为菱形正十二面体，尺寸约5μm。TEM和SEM研究发现，FDU-16单晶的12个面均为{110}，进一步的研究发现FDU-16晶体生长是从12个{110}面的中心按照layer-by-layer方式生长。采用混合表面活性剂(F127和P123)为模板，成功地得到了具有“铁饼”状形貌的FDU-15。改变表明活性剂浓度，FDU-15的直径可以得在0.5-10μm间调变。FE-SEM实验可以直接观察FDU-15的孔道沿“铁饼”的圆周方向生长。
Ordered mesoporous materials were first discovered by researchers of Mobil Company in 1992. For their unique properties and thus derived great potential application in catalysis, sorption, sensors, biology etc, mesoporous materials soon became one of the hottest research fields in the world. To date, numerous mesoporous materials with variable composition, structure, pore size, functions etc have been obtained, and more synthetic pathways and application fields have been explored and demonstrated. However, there are still a lot of questions to answer and many problems to solve in the research fields on mesoporous materials.
This thesis mainly focuses on two aspects: 1) Systematically investigate the hydrothermal stability of SBA-15 and find effective methods to improve it. 2) Explore new synthetic pathway and synthesize novel materials. Explore an aqueous route to synthesize novel mesoporous carbon materials. Synthesize bimodal mesoporous silica in a W/O system.
In chapter 2, the effect of the pore wall structure, of samples on the hydrothermal stability of pure silica SBA-15 in pure steam at 600 and 800℃, which is similar to industrial condition, was systematically investigated. In the steam of 600℃, SBA-15 materials show very good hydrothermal stability and the materials with thicker walls and more micropores possess better stability. The structures of SBA-15 materials are easily destroyed under steam of 800℃. High-temperature thermal treatment is proved to be an effective method to increase the polymerization degree and improve the hydrothermal stability. Nevertheless it will cause severe shrinkage of the mesopores. A carbon-propping approach was proved to dramatically increase the hydrothermal stability of SBA-15 under such critical condition, in pure steam of 800℃for 12 h. Al-SBA-15 shows very good hydrothermal stability in steam of 800℃(> 12 h). Nevertheless, Al-SBA-15 lost most of its acidity after steam treatment at 600℃for 3 h, which is a result of the hydrolyzation of framework Al.
In chapter 3, novel bimodal ordered mesoporous silica materials possessing tunable small pore of 5-10 nm and large pore of- 30 nm were synthesized by using triblock copolymer P123 as a template and liquid paraffin as a swelling agent in the water-in-oil (W/O) system following a solution sol-gel pathway. The solubility of liquid paraffin in P123 solution is much smaller than that of TMB or other short chain hydrocarbon. Thus, two types of micelles may exist in the liquid paraffin/P123/HCl/ H_2O solution. After the addition of TEOS, bimodal mesoporous materials are formed on the W/O surface as a result of the co-assembly of the two types of micelles with inorganic precursors (TEOS) at the same time. The two length scale pores are all uniform and well-controlled framework pores and homogeneously interconnected. The small pores are derived from the micelles of P123 and the pore size can be easily tuned from 5 to 10 nm by varying the aging temperature. The bimodal mesoporous materials display morphologies of thin sheets or shells of hollow spheres, with a thickness of 100 - 200 nm, which can be tuned by varying the P123 concentration.
In chapter 4, a facile aqueous route to synthesize ordered mesoporous carbon frameworks with tailored mesostructures (Im3m, p6m, and Ia3d) and well controlled morphologies were demonstrated by employing the organic-organic cooperative self-assembly of resols and triblock copolymers. Mesoporous carbons FDU-14 (Ia3d) with bicontinuous cubic structure were synthesized by using Pluronic P123 (EO20PO70EO20) as a template. A mesophase transformation from Ia3d to p6m was observed as the P123/phenol ratio decreased. Hydrocarbons were employed as swelling agents in the organic-organic self-assembly, and 2-D hexagonal (p6m) mesoporous carbons FDU-15 were successfully obtained as a result. The pore size of the obtained FDU-15 can be tuned from 4.1 to 6.8 nm by varying the hydrocarbon molecules. Highly ordered mesoporous carbons FDU-16 with body-centered cubic structure (Im3m) were first obtained from the aqueous route by using Pluronic F127 (EO_(106)PO_(70)EO_(106)) with a large PEO segment as a template. The morphology of the obtained carbons can be controlled on the micrometer scale (FDU-15, FDU-16) or millimeter scale (small pellets of 1-5 mm). One-layer hydrogen bond interaction between resols and PEO segments was proposed to be the essential driving force that induces the organic-organic cooperative assembly.
In chapter 5, 3-D cubic mesoporous carbon FDU-16 single-crystals were prepared by employing an aqueous solution induced organic-organic assembly of triblock copolymer F127 and phenol/formaldehyde resols. The morphologies of the obtained materials are perfect rhombdodecahedron with the uniform size of - 5μm, which are commensurate with the crystallographic point group symmetry (Im3m). The scanning electron microscope (SEM) and transmission electron microscope (TEM) images directly show a layer-by-layer growth mode of face-centered cubic FDU-16 mesostructured carbon single-crystals from the centers of twelve {110} planes. Simultaneously, 2-D hexagonal mesoporous carbon FDU-15 crystals with discus-like morphologies are the products if mixed templates of F127 and P123 are used. The ordered circular mesopore channels with hexagonal packing of FDU-15 can be directly observed by the FE-SEM images.
引文
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