A hypercrosslinked conjugated microporous polymer (HCMP‐1) with a robustly efficient absorption and highly specific sensitivity to mercury ions (Hg2+) is synthesized in a one‐step Friedel–Crafts alkylation of cost‐effective 2,4,6‐trichloro‐1,3,5‐triazine and dibenzofuran in 1,2‐dichloroethane. HCMP‐1 has a moderate Brunauer–Emmett–Teller specific surface (432 m2 g?1), but it displays a high adsorption affinity (604 mg g?1) and excellent trace efficiency for Hg2+. The π–π* electronic transition among the aromatic heterocyclic rings endows HCMP‐1 a strong fluorescent property and the fluorescence is obviously weakened after Hg2+ uptake, which makes the hypercrosslinked conjugated microporous polymer a promising fluorescent probe for Hg2+ detection, owning a super‐high sensitivity (detection limit 5 × 10?8 mol L?1).
