纳米ZSM-5沸石分子筛因具有更短的扩散路径和更高的催化位点可及性，比传统微孔ZSM-5沸石拥有更长的催化寿命以及优异的产品选择性而备受关注。但是，传统纳米H-ZSM-5沸石是在水热环境下，通过严格控制合成原料的成核和生长行为以及多次离子交换来获得的。这种经典的合成策略由于合成过程与合成体系的复杂性，导致纳米H-ZSM-5沸石分子筛在晶化机理的深度研究及绿色规模化可持续合成方面始终面临挑战。基于科学研究和工业生产的双重需要，迫切需要开发一条工艺过程简单、绿色可持续发展路线以直接制备具有高催化性能的纳米H-ZSM-5沸石催化剂。

近年来，以天然硅铝质黏土替代传统的化学硅铝药品“硅铝同源”直接制备纳米H-ZSM-5沸石催化剂，由于杜绝了工业硅铝药品的使用以及合成原料的均质化步骤，在合成源头与合成工艺等方面实现了绿色可持续化而受到广泛关注，并被研究者们视为是工业上纳米H-ZSM-5沸石分子筛的绿色合成新路线。该路线工业化的关键在于能否克服因天然硅铝质黏土解聚过程中存在的高能耗问题以及如何以更为绿色的手段直接精准调控合成产物的物化性能（如合成晶体的尺寸大小）。现有文献表明，与化学硅铝药品相比，天然硅铝质黏土解聚后形成的高活性硅铝物种与以之为原料制备的ZSM-5沸石晶体间在晶体形貌、孔道结构、酸性质等方面存在一定的构效关系（即黏土基ZSM-5沸石分子筛的“遗传效应”）。如能通过一种构建简单的合成体系，并在此基础上对黏土基纳米H-ZSM-5沸石的晶化机理进行研究，必然可以在更深层次去观察和阐明这种“遗传效应”，从而为具有高催化性能的黏土基纳米H-ZSM-5沸石催化剂精准合成提供研究方向，同时也能对沸石分子筛材料的“基因工程学”研究提供直接的实验数据支撑。基于上述研究动机，本论文围绕黏土基纳米H-ZSM-5沸石分子筛的绿色合成及其性能研究开展了一系列实验，主要研究内容如下：

首先，构建了“三元绿色合成体系”，即以碱熔-酸洗处理过的伊利石黏土为合成硅铝源，基于类固相合成体系，在少量TPAOH作用下，直接合成了形貌高度均一的高硅铝比纳米H-ZSM-5沸石分子筛。以结晶动力学分析了经酸洗-碱熔处理后获得的固体原料(ISR)的化学活性。系统考察了TPAOH使用量对合成样品的结晶度，晶粒形貌的影响规律和合成产物的晶化行为。甲醇制芳烃(MTA)的催化实验表明，与商业ZSM-5沸石催化剂相比，合成的黏土基纳米H-ZSM-5沸石分子筛由于具有更高的比表面积，以及分布均匀的酸性位点，在BTX产物选择性（苯，甲苯，二甲苯）和催化寿命方面更为优秀。该策略不仅可以提高纳米ZSM-5沸石的合成产率，同时也彻底避免了传统纳米ZSM-5沸石分子筛合成工艺中与铵盐的离子交换工艺步骤，降低了具有高催化性能的纳米ZSM-5沸石催化剂的合成成本。

其次，为避免传统天然硅铝质黏土解聚过程伴随的高能耗、高污染问题，提出了一种在类固相体系内，利用酸蒸汽解聚天然硅铝质黏土的绿色低能耗方法，并在“三元绿色合成体系”的基础上以酸蒸汽解聚天然伊利石产生的活性硅铝物种为原料，在微量TPAOH作用下，直接快速制备了具有高结晶度、形貌均一、且单分散的黏土基纳米H-ZSM-5沸石分子筛。通过引入陈化过程，成功的解耦了沸石分子筛晶体的成核与生长过程，从而在纳米水平实现了对合成的纳米H-ZSM-5沸石颗粒尺寸的精准可控合成(56 – 176 nm)。此外，详细讨论了合成条件（如陈化时间，TPAOH用量）对合成的纳米H-ZSM-5沸石分子筛物化性质的影响，并以甲醇制丙烯(MTP)为反应探针，对合成的纳米H-ZSM-5催化剂的催化行为进行了评价。实验结果表明，与商业ZSM-5沸石催化剂相比，合成的纳米H-ZSM-5沸石由于具有高度贯通的孔道结构，均匀分布的酸性位点以及均一的纳米晶体尺寸和全骨架整体式多级孔等优点，因此表现出更高的催化寿命以及丙烯产物的选择性(154 h, 50.97%; 56 h, 32.83%)。

最后，通过对不同解聚时间下解聚天然伊利石产生的活性硅铝物种的细致表征，从而在晶体结构、形貌、元素组成以及硅、铝元素化学环境等方面分析并总结了天然伊利石黏土“自上而下”的解聚行为。采用沸石分子筛的晶化动力学为研究手段，对酸蒸汽处理天然硅铝质黏土形成的具有天然硅铝质黏土拓扑结构的硅铝物种的化学活性进行了计算。研究发现，酸蒸汽解聚天然黏硅铝质土所获得的固体硅铝物种与化学硅铝药品以及传统热活化-酸/碱处理解聚的天然硅铝质黏土具有相似的高化学活性。再次，根据对不同晶化时间下获得的合成样品的表征结果，提出了一种基于天然硅铝质黏土拓扑结构与有机模板剂(TPAOH)相互作用的原位重构机制，以阐明黏土基纳米H-ZSM-5沸石分子筛的晶化机理，并从晶体结构转变、元素组成等方面，分析黏土基活性硅铝物种与黏土基纳米H-ZSM-5沸石分子筛之间的“遗传效应”。最后，对合成策略的普适性进行了扩展性研究，从而为丰富黏土基纳米H-ZSM-5分子筛的“材料基因工程学”研究提供实验数据。

Nano-ZSM-5 zeolites have shorter diffusion pathways and higher catalytic site accessibility, leading to longer catalytic lifetimes and good product selectivity than conventional ZSM-5 zeolites, which have attracted much attention. However, the nano-H-ZSM-5 zeolite is obtained in the hydrothermal environment by strict control of the nucleation and growth behavior of the synthetic material. The complexity of the synthesis process and the synthesis system of this strategy leads to great challenges in the preparation of green and sustainable synthesis of nano-H-ZSM-5 zeolite single crystals and the in-depth research of its crystallization mechanism. For scientific research and industry products, it is necessary to develop a facile and green sustainable route for the synthesis of nano-H-ZSM-5 zeolite single crystals with high crystallinity and defect-free crystals.

Recently, the direct preparation of nano-H-ZSM-5 zeolite via the “silica-alumina homologation” of depolymerized natural clay has attracted much attention since the use of industrial chemical silica-alumina products and homogenization steps can be avoided, thereby rendering this approach a green and sustainable route. The key to the industrialization of this synthetic route is to overcome the high energy consumption and pollution problems in the process of depolymerization of natural silica-alumina clay into highly active silica and aluminum species and to precisely regulate the physical and chemical properties of the synthesized products (such as the size of the synthesized crystals) in a greener route. The literature shows that there is a certain structure-activity relationship between the highly reactive silica and aluminum species formed by the depolymerization of natural silica-alumina clay and the ZSM-5 zeolite crystals which are prepared from them in terms of crystal morphology, pore structure, and acid properties compared with chemical raw materials i.e., the "genetic effect" of clay-based ZSM-5 zeolite compared. If the crystallization mechanism of clay-based nano-H-ZSM-5 zeolite can be investigated by building a simple synthesis system, it will certainly reveal and elucidate the “genetic effect” at the molecular level, thus providing data for the research of "genetic engineering of zeolite materials". To achieve the above research objectives, a series of works have been carried out in this study, and the detailed results are as follows:

Firstly, a green and sustainable minimalist synthesis system was developed to directly synthesize highly homogeneous nano-H-ZSM-5 zeolite with high silica-alumina ratios based on a solid-phase-like synthesis system by using alkali-melting-acid-washing treated illite clay as the synthetic silica and aluminum source with a very small amount of TPAOH. The chemical activity of the leached illite(ISR) was analyzed by crystallization kinetics and the effect of the amount of TPAOH used on the crystallinity, and morphology of the synthesized samples was carefully investigated. In addition, the crystallization behavior of the synthesized products was also carefully studied. The catalytic experiments for methanol to aromatics (MTA) showed that the synthesized clay-based nano-H-ZSM-5 zeolite (~ 300 nm), with higher specific surface area and uniformly distributed acidic sites, was superior in BTX product selectivity (benzene, toluene, xylene) and catalytic lifetime compared with commercial ZSM-5 zeolite catalysts. This strategy not only improves the yield of nano-ZSM-5 zeolite, but also completely avoids the ion-exchange process step with ammonium salts in the conventional nano-ZSM-5 zeolite synthesis process, which greatly reduces the synthesis cost of nano-ZSM-5 zeolite catalysts with high catalytic performance.

Secondly, to avoid energy consumption and pollution problems in the depolymerization of natural silica-alumina clays. A green and low-energy method for depolymerization of natural silica and aluminous clays by acid vapor treatment in a solid-phase-like system is proposed, and based on the “ternary green synthesis system”, the active silica and aluminous species produced by depolymerization of illite are used as raw materials to prepared highly crystalline, monodisperse nano-H-ZSM-5 zeolite catalysts with monolithic full skeleton hierarchical structure with a very small amount of TPAOH. The experimental results showed that the nucleation and growth behavior of the clay-based ZSM-5 zeolite could be decoupled by regulating the aging time, and the grain size of the synthesized ZSM-5 zeolite could be precisely controlled (56 – 176 nm). The effect of the synthesis conditions (such ais aging time and amount of TPAOH) on the physical and chemical properties of the synthesized nano-H-ZSM-5 zeolite single crystal was discussed in detail. The catalytic behavior of the synthesized nano-H-ZSM-5 single-crystal catalyst was evaluated using methanol to propylene (MTP) as the reaction probe. The experimental results show that compared with commercial ZSM-5 zeolite catalyst, the synthesized nano-H-ZSM-5 zeolite single crystal shows higher catalytic life and selectivity of propylene products (154 h, 50.97%; 56h, 32.83%) due to its highly penetrating pore structure, uniformly distributed acid sites, uniform nano crystal size and full skeleton monolithic hierarchical pore structure.

Finally, the "top-down" depolymerization behavior of natural illite clay was analyzed and summarized in terms of crystal structure, morphology, elemental composition, and the chemical environment of Si and Al elements by carefully characterizing the active silica-alumina species produced by depolymerizing natural illite at different depolymerization times. Then, the chemical activity of silica-alumina species with natural clay topology obtained by acid steam treatment of natural clays was calculated by using the crystallization kinetics of zeolite. It was found that the solid silica-alumina species obtained by acid vapor depolymerization of natural clays have similar high chemical activity as chemical silica-alumina chemical products and natural clays depolymerized by conventional thermal activation-acid/alkali treatment. Furthermore, based on the characterization of synthetic samples obtained at different crystallization times, an in-situ reconstitution mechanism based on the interaction of natural clay topology with organic templating agents(TPAOH) is proposed to elucidate the crystallization mechanism of clay-based nano-H-ZSM-5 zeolite single crystals and to reveal the relationship between clay-based active silica-alumina species and clay-based nano-H-ZSM-5 zeolite single crystals in terms of crystal structure transformation, elemental composition, etc. The "genetic effect" between clay-based reactive silica-alumina species and clay-based H-ZSM-5 zeolite single crystals is revealed. Finally, the generalizability of the synthesis strategy is extended to provide experimental data to enrich the “material genetic engineering” of clay-based nano-H-ZSM-5 zeolites.

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