This study explores the viability of mechanosynthesis (MS) as an environmentally friendly approach for producing hypercrosslinked polymers (HCPs) from various coal tar products (CTPs): creosote, phenolic oil, naphthalene oil, and depleted naphthalene oil (DNO). Thus, aiming to convert dangerous industrial byproducts into high-value materials. Benzene was used as a model molecule, for which a 20–30-minutes reaction time proved optimal for benzene-derived HCPs with high surface area. HCPs produced from CTPs by mechanosynthesis were highly dependent on precursor and reaction conditions. The two most promising CTPs, namely those derived from creosote and DNO, were synthesized with a low catalyst and/or crosslinker content, contrary to literature findings. Creosote- and DNO-derived HCPs with the highest surface areas, ∼500 m2 g−1, were tested as methylene blue (MB) adsorbents and showed a maximum adsorption capacity of 10.2 gMB per 100 g sample, similar to that achieved by other HCPs with higher surface areas.
