以离子液合成法制备硅铝型分子筛与分子筛结构的研究
摘要
目前，离子液体作为一种新型的绿色和环境友好溶剂受到了极大的关注。它是由较大的有机阳离子和较小的无机阴离子组成的盐类，与一般的离子化合物不同，它在室温或室温附近呈液态，因而也可以称为低温熔融盐。离子液体具有以下性质：(1)蒸汽压极低、不可燃；(2)溶解能力极佳，可以对各种有机物、无机物及聚合物进行溶解；(3)热稳定性和化学稳定性高、液程宽(-90～300℃)；(4)离子电导率高，电化学电位窗大。目前，在多相催化、有机合成、电化学、分离分析化学等化学化工领域中，关于离子液体应用的研究都有大量的报道。将离子液体用于合成分子筛材料的报道始于2004年，Cooper等以[C_2mim]Br为溶剂和模板剂在常压下合成了磷铝型分子筛AlPO_4-11和其它几种类分子筛材料，而利用离子液体热合成法合成硅铝型沸石分子筛的研究却一直未见报道。
本论文中，首次利用1-乙基-3-甲基咪唑溴盐离子液体通过离子液体热合成法制备了硅铝型分子筛——方钠石。离子液体热合成法与水热和溶剂热合成这些使用分子溶剂的合成方法不同，它将离子液体这种离子化合物同时作为溶剂和模板剂进行分子筛合成。由于离子液体具有液程宽、热稳定性高的特点，在相当宽的温度范围内，离子液体可以作为液体使用，其中的反应可在常压下进行。并且离子液体有很强的自组装能力，它能够在液态下通过氢键形成超分子结构，将离子液体作为模板剂使用，合成过程中不需要另外添加模板剂。我们利用这种方法合成出了晶体呈球形，晶粒约200～500nm的方钠石。通过XRD、BET、SEM等现代表征手段对产物进行表征，考察了晶化时间、晶化温度、硅铝胶与离子液体的比例等合成条件对离子液体热合成沸石分子筛晶化过程的影响，并且对合成机理进行了初步的探讨。研究结果表明：离子液体热合成方钠石，60～90℃为形成方纳石的最佳温度。水与离子液体的比例影响晶化反应的进程，当离子液体与硅铝胶重量比为3时，产品为纯的方纳石；随体系中水含量的增加，样品中出现了X沸石。以Si／Al比为1.1／1～10.0／1的硅铝胶体系合成了方钠石，且结晶度随Si／Al比上升而上升。
Recently, as a new type of green environment-friendly solvent, ionic liquid(ILs) have attracted much interest of the researchers. ILs are salts composed of big organic cations and small inorganic anions. Different from other ionic compounds, melting points of ILs are close to the room temperature. They have unique properties: (1) nonvolatile, nonflammable; (2) good solvents for a wide range of organic, inorganic materials and polymer; (3) high thermal stability and chemical stability, wide range of liquidus temperatures (-90～300℃), (4) good ionic conductivity and large electrochemical window. Up to now, They are widely used in different chemical processes such as heterogeneous catalysis, organic synthesis, electrochemistry and analytical chemistry. However, In contrast to their successful applications above, the use of ILs in zeolite synthesis is still lack of reporting. The research according to the using of ILs in zeolite synthesis was first reported in 2004. Cooper et al. used [C_2mim]Br as both solvents and templates in the synthesis of AlPO_4-11 and molecular sieves with other frameworks under ambient pressure, but there is no report about the synthesis of Si-Al zeolite by this method.
In the thesis, we investigated the synthesis ionic liquid of [C_2mim]Br and the Si-Al zeolite in the synthesized ionic liquids, namely ionothermal process, which is a novel method for zeolite synthesis. ILs can be used as the synthesis solvent, and reactions is conducted under ambient pressure due to their wide range of liquidus temperatures and high thermal stability in a wide range of temperatures. ILs have feature of self-organization since they have extended hydrogenbond systems in the liquid state and "supramolecular" structure is formed. Therefore, the organic cations of ILs can play a role of templates in the synthesis of zeolite, and synthesized process is template free. Sodalite (SOD) zeolite with micropores are successfully synthesized in our experiments, which has spherical morphology with 200～500 nm diameters. The synthesis started from aqueous basic aluminosilicate precursor gels and the zeolite crystallization completes in an imidazolium-based ionic liquid of 1-ethyl-3-methylimidazolium bromide. The effects of weight ratios of aqueous gels to ionic liquids, Si/Al molar ratios in gels and crystallization variables, such as temperature and time, on the crystallization of SOD zeoliet are investigated, and we dicuss the possible mechanism in the ionothermal synthesis. The results showed that a mixture of sodalite and zeolite X is initially formed in ionic liquid at a ratio 1:3 of aqueous gel to ionic liquid, and finally transformed to pure sodalite as the crystallisation time is prolonged. The best temperature of sodalite synthesis was between 60 and 90℃under ambient pressure. The crystallinity of sodalite increased with the increasing of Si/Al from 1.1 to 10. Increasing the ratio of aqueous gel to ionic liquid, zeolite X was favorable to crystallize, and it is the only product in the hydrothermal condition.
本论文中，首次利用1-乙基-3-甲基咪唑溴盐离子液体通过离子液体热合成法制备了硅铝型分子筛——方钠石。离子液体热合成法与水热和溶剂热合成这些使用分子溶剂的合成方法不同，它将离子液体这种离子化合物同时作为溶剂和模板剂进行分子筛合成。由于离子液体具有液程宽、热稳定性高的特点，在相当宽的温度范围内，离子液体可以作为液体使用，其中的反应可在常压下进行。并且离子液体有很强的自组装能力，它能够在液态下通过氢键形成超分子结构，将离子液体作为模板剂使用，合成过程中不需要另外添加模板剂。我们利用这种方法合成出了晶体呈球形，晶粒约200～500nm的方钠石。通过XRD、BET、SEM等现代表征手段对产物进行表征，考察了晶化时间、晶化温度、硅铝胶与离子液体的比例等合成条件对离子液体热合成沸石分子筛晶化过程的影响，并且对合成机理进行了初步的探讨。研究结果表明：离子液体热合成方钠石，60～90℃为形成方纳石的最佳温度。水与离子液体的比例影响晶化反应的进程，当离子液体与硅铝胶重量比为3时，产品为纯的方纳石；随体系中水含量的增加，样品中出现了X沸石。以Si／Al比为1.1／1～10.0／1的硅铝胶体系合成了方钠石，且结晶度随Si／Al比上升而上升。
Recently, as a new type of green environment-friendly solvent, ionic liquid(ILs) have attracted much interest of the researchers. ILs are salts composed of big organic cations and small inorganic anions. Different from other ionic compounds, melting points of ILs are close to the room temperature. They have unique properties: (1) nonvolatile, nonflammable; (2) good solvents for a wide range of organic, inorganic materials and polymer; (3) high thermal stability and chemical stability, wide range of liquidus temperatures (-90～300℃), (4) good ionic conductivity and large electrochemical window. Up to now, They are widely used in different chemical processes such as heterogeneous catalysis, organic synthesis, electrochemistry and analytical chemistry. However, In contrast to their successful applications above, the use of ILs in zeolite synthesis is still lack of reporting. The research according to the using of ILs in zeolite synthesis was first reported in 2004. Cooper et al. used [C_2mim]Br as both solvents and templates in the synthesis of AlPO_4-11 and molecular sieves with other frameworks under ambient pressure, but there is no report about the synthesis of Si-Al zeolite by this method.
In the thesis, we investigated the synthesis ionic liquid of [C_2mim]Br and the Si-Al zeolite in the synthesized ionic liquids, namely ionothermal process, which is a novel method for zeolite synthesis. ILs can be used as the synthesis solvent, and reactions is conducted under ambient pressure due to their wide range of liquidus temperatures and high thermal stability in a wide range of temperatures. ILs have feature of self-organization since they have extended hydrogenbond systems in the liquid state and "supramolecular" structure is formed. Therefore, the organic cations of ILs can play a role of templates in the synthesis of zeolite, and synthesized process is template free. Sodalite (SOD) zeolite with micropores are successfully synthesized in our experiments, which has spherical morphology with 200～500 nm diameters. The synthesis started from aqueous basic aluminosilicate precursor gels and the zeolite crystallization completes in an imidazolium-based ionic liquid of 1-ethyl-3-methylimidazolium bromide. The effects of weight ratios of aqueous gels to ionic liquids, Si/Al molar ratios in gels and crystallization variables, such as temperature and time, on the crystallization of SOD zeoliet are investigated, and we dicuss the possible mechanism in the ionothermal synthesis. The results showed that a mixture of sodalite and zeolite X is initially formed in ionic liquid at a ratio 1:3 of aqueous gel to ionic liquid, and finally transformed to pure sodalite as the crystallisation time is prolonged. The best temperature of sodalite synthesis was between 60 and 90℃under ambient pressure. The crystallinity of sodalite increased with the increasing of Si/Al from 1.1 to 10. Increasing the ratio of aqueous gel to ionic liquid, zeolite X was favorable to crystallize, and it is the only product in the hydrothermal condition.
引文
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