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This research focuses on the feasibility of sustainable biocomposites for thermal insulation created from corn starch and reinforced with jute spinning mill waste, specifically evaluating the effect of caustic soda (NaOH) treatment on the quality of biocomposite materials. Here, the jute fibers used were not clean because these fibers were collected from jute fibers waste. So it was necessary to clean the fibers and 15% (w/w) caustic soda (NaOH) showed more cleaning efficiency than 5%, 10%, and 20% (w/w) NaOH solution. After that, the composite material was made from caustic soda–treated and caustic soda–nontreated jute fibers. Then, the physical properties of composite materials were checked comparing with insulation foam for identifying the thermal insulation properties. Tensile strength, shore hardness, density, water absorption, and thermal conductivity were among the key performance indicators evaluated. The tensile strength, flexural strength, shore hardness, density, water absorption, thermal conductivity, SEM view, and surface smoothness were checked for 15% NaOH‐treated and NaOH‐untreated jute fibers and make compression with insulation foam to detect the thermal insulation of the biocomposite. Here, 15% caustic‐treated sample showed good results than the untreated sample. Overall, integrating caustic‐treated jute waste into corn starch‐based composites is a realistic and ecologically suitable alternative to typical thermal insulating materials, with higher mechanical properties, adequate thermal performance as well as being beneficial to the environment. [ABSTRACT FROM AUTHOR]