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

Three synthesis procedures of the covalent-organic framework (COF) TpPa‑1 are studied with the purpose of setting the most promising one in a fast and green way, leading to a more environmentally-friendly and sustainable process. By conventional heating, good crystallinity and high BET specific surface area (SSA) up to 1007 m2g-1 are achieved at oC 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 m2g-1 obtaining yields close to 98% (versus 90% of the hydrothermal synthesis). The water-assisted mechanochemical synthesis is also an environmentally-friendly synthetic approach reaching, by heating at 170 oC in a two-step process (10+10 min), high crystallinity, and the BET SSA and yield of 960 m2g-1 and 98%, respectively, for TpPa-1.