This article explores using biomass, namely rice husks, as a reinforcement material in thermoplastic copolyester (TPC) composites. Rice husks were subjected to three chemical pretreatments: single-stage sulfuric acid hydrolysis, first-stage sulfuric acid hydrolysis followed by a second-stage methanesulfonic acid (MSA) treatment, and first-stage sulfuric acid hydrolysis followed by a second-stage sodium hydroxide alkali treatment. We studied the effects of these treatments on the rheological, thermal, interfacial, and mechanical properties of composites. The fibers were mixed with polymers at high shear rates and temperatures, and 3D-printed filaments were produced using a desktop 3D printer. The printed parts were analyzed using tensile tests, torque and viscosity measurements, and thermogravimetric analysis to obtain their mechanical, rheological, and thermal properties. SEM imaging was performed to understand the fiber–polymer interface and how it affects the other properties. The results showed that first-stage sulfuric acid hydrolysis followed by a second-stage pretreatment of the fibers with MSA showed better fiber–polymer adhesion and a 20.4% increase in stress at 5% strain, a 30% increase in stress at 50% strain, and a 22.6% increase in the elastic modulus as compared to untreated rice husk composites. These findings indicate that readily available and inexpensive rice husks have significant potential for use in natural fiber-reinforced composites when pretreated using dilute sulfuric acid followed by methane sulfonic acid hydrolysis.