In the present study, the ability of novel carbon microspheres (CMs) derived from a date palm (Phoenix dactylifera) biomass using a hydrothermal carbonization (HTC) process and activated using phosphoric acid in removing methylene blue dye was investigated. Three types of palm-based wastes (seeds, leaflet and inedible crystallized date palm molasses) were used and converted to CMs via HTC process. The prepared samples were then activated using phosphoric acid via incipient wetness impregnation method. The CMs samples before and after activation were analyzed using scanning electron microscopy (SEM), elemental analysis and scanning (CHNS), Fourier Transform-Infrared (FTIR) and Brunauer–Emmet–Teller (BET) method. The samples exhibited high BET surface areas after activation (1,584 m2/g). The methylene blue adsorption results showed good fittings to the Langmuir and Redlich-Peterson isotherm models for all activated samples. The maximum adsorption capacity achieved was 409.84 mg/g for activated CM obtained from the palm date molasses, indicating high potential for application as dye-based adsorption materials.