Due to the various anthropogenic activities, the continuous release of organic pollutants is a serious global threat. Thus, developing effective removal and remediation technologies for hazardous pollutants is essential to minimize the adverse effects on human health and the environment. Herein, we developed hyper-crosslinked polymers (HCPs) via catalyst-free solvothermal Friedel-Crafts alkylation reaction using tris-phloroglucinol/tris-resorcinol substituted triazine and dimethoxymethane. The obtained HCPs (HCP-CPF, HCP-CRF) exhibit variation in the surface area, pore size and morphology. The cross-linking of Phloroglucinol-triazine-based planar monomers via methylene spacer leads to porous coral-like morphology with a high surface area (Sarea = 480 m2/g) in HCP-CPF. In contrast, the cross-linking of Resorcinol-substituted triazine-based monomers displayed a fibre network with comparatively low surface area (Sarea = 35.7 m2/g) in HCP-CRF. The presence of densely functionalized multiple hydroxyl groups, good surface area and aqueous dispersibility in HCPs facilitate the fast and efficient removal capacity of various cationic dyes and paraquat herbicide in water. The HCP-CPF displayed fast removal capacity towards the large class of different organic dyes, and it removed 100% of most of the dyes within 10 min from the aqueous solution. Furthermore, the recovery of gold from an aqueous solution is one of the essential and crucial tasks. HCP-CPF and HCP-CRF exhibited a good removal capacity towards Au3+ via in-situ reduction (Qmax = 497.5 mg/g for HCP-CPF and Qmax = 463.33 mg/g for HCP-CRF).