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

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 m² ⋅ g^-1 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 m² ⋅ g^-1 ) 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 m² ⋅ g^-1 and a yield of 98 % for TpPa-1.