After cellulose, chitin is the most prevalent biopolymer. The purpose of this work was to produce and characterize chitosan from expended crustacean shells (crab, prawn, and shrimp), primarily from Lagos State in Nigeria. Three main processes—deproteination, demineralization, and deacetylation—were used to manufacture their chitosan. The produced chitosan samples were characterized using Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), and X-ray Fluorescence (XRF) analyses, respectively, for functional components (ligands), surface shape, mineral constituent, and chemical constituent. The crab, shrimp, and prawn shell chitosan absorption altitudes ranged from 3360 to 893, 3775 to 570, and 3761 to 707 cm−1, respectively, in FTIR wavelengths; while both shrimp and prawn shell chitosan showed a clear and small filament lucent shape, the SEM pictures of crab shell chitosan showed a non-permeable, loosen skin semblance made up of protruding openings, tiny threadlike, and mineral form. Additionally, the chitosan found in shrimp shells is permeable and comprises granular layers. The crustaceans' related XRD results showed two tiny altitudes at 20°, 35°, 19.50° and 29.52°, 25.79° and 32.02°. Shrimp and prawn chitosan were both found to contain CaO, with larger proportions of 81.60 and 84.02%, respectively, according to XRF analysis. In general, all of the chitosan samples had amine, amide, carbonyl, carboxylic acid, hydrogen, and hydroxyl ligands (among others), which gave them better metal comity and band capability. As a result, the prepared chitosan of crab, prawn, and shrimp portrayed appropriate attributes for the adsorption techniques.