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用于高效制备共价有机框架TpPa-1的绿色快速策略

Green and Fast Strategies for Energy-Efficient Preparation of the Covalent Organic Framework TpPa-1.

作者信息

Martínez-Visus Íñigo, Ulcuango Matías, Zornoza Beatriz, Coronas Joaquín, Téllez Carlos

机构信息

Instituto de Nanociencia y Materiales de Aragón (INMA), CSIC-Universidad de Zaragoza Zaragoza, Zaragoza, 50009, Spain.

Chemical and Environmental Engineering Department, Universidad de Zaragoza Zaragoza, Zaragoza, 50018, Spain.

出版信息

Chemistry. 2023 Mar 13;29(15):e202203907. doi: 10.1002/chem.202203907. Epub 2023 Feb 9.

DOI:10.1002/chem.202203907
PMID:36652540
Abstract

Three synthesis procedures for the covalent-organic framework (COF) TpPa-1 are studied with the purpose of setting up the most promising one in a fast and green way, leading to a more environmentally friendly and sustainable process. With conventional heating, good crystallinity and a high BET specific surface area (SSA) of up to 1007 m  ⋅ g are achieved at 170 °C for 3 days using water as the quintessential green solvent. However, the application of microwave radiation in the synthesis for this crystalline porous polymer allows reaction times to be shortened to 30 min while maintaining structural and textural properties (BET SSA of 928 m  ⋅ g ) and obtaining yields close to 98 % (vs. 90 % in the hydrothermal synthesis). The water-assisted mechanochemical synthesis is also an environmentally friendly synthetic approach; with heating at 170 °C in a two-step process (10+10 min), high crystallinity is achieved, a BET SSA of 960  m  ⋅ g and a yield of 98 % for TpPa-1.

摘要

研究了共价有机框架(COF)TpPa-1的三种合成方法,目的是以快速且绿色的方式确定最具前景的方法,从而实现更环保、更可持续的过程。采用传统加热方式,以水作为典型的绿色溶剂,在170°C下反应3天,可获得良好的结晶度和高达1007 m²·g的高BET比表面积(SSA)。然而,在这种结晶多孔聚合物的合成中应用微波辐射,可将反应时间缩短至30分钟,同时保持结构和织构性质(BET SSA为928 m²·g),并获得接近98%的产率(相比水热合成中的90%)。水辅助机械化学合成也是一种环保的合成方法;在170°C下分两步加热(10 + 10分钟),可实现高结晶度,TpPa-1的BET SSA为960 m²·g,产率为98%。

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