In situ monitoring of hydrothermal and solvothermal synthesis of molecular sieves

分子筛水热和溶剂热合成的原位监测

• 批准号: 445323933
• 负责人: Professor Dr. Martin Hartmann
• 金额: --
• 依托单位: Erlangen Center for Interface Research and Catalysis
• 依托单位国家: 德国
• 项目类别: Research Grants
• 资助国家: 德国
• 项目状态: 未结题
• 来源: https://gepris.dfg.de/gepris/projekt/445323933?language=en
• 关键词: situ; monitoring; hydrothermal; solvothermal; synthesis

Porous materials, esp. zeolites and metal-organic frameworks (MOF), play a key role in chemical industry as catalysts and adsorbents. The joined project aims at the development of novel spectroscopic techniques applied in a specific combination with already known techniques for a direct comparative and complementary in situ monitoring of the hydrothermal and solvothermal synthesis of zeolites and metal-organic frameworks (MOF), respectively. This will open new perspectives for improving the scientific understanding for the robust preparation of both of these material classes and for their predictable tuning of required properties. The combined use of in situ NMR, Raman, FTIR spectroscopy, along with XRD, ultrasonic spectroscopy, and dynamic light scattering will allow to study the crystal formation processes at atomic-, molecular-, nano- and micrometric levels at the same and real time mode in a time-resolved way. Such specifically combined investigation will give rise to obtain fundamentally new information about the processes at the different stages of molecular sieve formation namely (i) molecular interaction (NMR, Raman, FTIR); (ii) the formation of crystallization nuclei (NMR, Raman, FTIR) and (iii) the crystal growth (US spectroscopy, DLS, XRD).Specific goals of the project include: 1) Elaboration of hydrothermal and solvothermal synthetic procedures adapted to the in situ studies of zeolites BEA and MFI as well as MIL-53-based MOFs for combined application of various in situ techniques; 2) Development and optimization of in situ cells and methodological approaches for the in situ monitoring of hydrothermal and solvothermal synthesis at the atomic, molecular, nano- and micrometric scales using MAS NMR; FTIR, Raman, DLS and US spectroscopic techniques; 3) Elucidation of the effect of the main parameters of hydrothermal synthesis, namely, the method of synthesis (clear solution process, sol-gel synthesis, dry-gel conversion), type of template, type of mineralizing agent and type of heteroatom on the mechanism of zeolites BEA and MFI formation; 4) Unravel the effect of the main parameters of solvothermal synthesis of MOFs, namely, type and amount of solvent, temperature and metal source/ linker ratio on the mechanism of MIL-53 formation.

多孔材料，特别是沸石和金属有机骨架材料（MOF），作为催化剂和吸附剂在化学工业中发挥着关键作用。该联合项目旨在开发新的光谱技术，与已知技术结合应用，分别对沸石和金属有机框架（MOF）的水热和溶剂热合成进行直接比较和补充原位监测。这将为提高对这两种材料类别的稳健制备及其所需性质的可预测调整的科学理解开辟新的视角。原位NMR、拉曼、FTIR光谱、沿着XRD、超声光谱和动态光散射的组合使用将允许以时间分辨的方式在相同和真实的时间模式下在原子、分子、纳米和微米水平上研究晶体形成过程。这种特定的组合研究将导致获得关于分子筛形成的不同阶段的过程的基本上新的信息，即（i）分子相互作用（NMR、拉曼、FTIR）;（ii）结晶核的形成（NMR，拉曼，FTIR）和（iii）晶体生长（US spectroscopy，DLS，XRD）。该项目的具体目标包括：1）对适合于原位研究沸石NH 4和MFI以及MIL-53的水热和溶剂热合成程序的评价。2）开发和优化原位电池和方法学方法，用于使用MAS NMR、FTIR、拉曼、DLS和US光谱技术在原子、分子、纳米和微米尺度上原位监测水热和溶剂热合成; 3）阐明水热合成的主要参数的影响，即合成方法（澄清溶液法、溶胶-凝胶合成、干凝胶转化），模板的类型，矿化剂种类和杂原子种类对沸石分子筛MFI和MFI形成机理的影响; 4）揭示了溶剂热合成MOFs的主要参数，即溶剂的类型和用量的影响，温度和金属源/连接剂比率对MIL-53形成机制的影响。