Scalable Production of Low-Molecular-Weight Chitosan: Comparative Study of Conventional, Microwave, and Autoclave-Assisted Methods

The valorization of shrimp shell waste is crucial for promoting sustainability and a circular economy. This study aimed to extract chitin from the exoskeletal residues of deep-water rose shrimp (<i>Parapenaeus longirostris</i>) sourced from the Marmara Sea and synthesize low-molecular-weight chitosan (LMWC) via conventional, microwave-, and autoclave-assisted deacetylation pathways. The shell biomass was subjected to sequential demineralization (1 M HCl) and deproteinization (1 M NaOH), yielding 14.42% chitin. The extracted chitin was then converted to LMWC using the three methods, and the products were characterized using FT-IR spectroscopy, titration, viscometry, SEM, and TGA. The results demonstrated that the autoclave-assisted method achieved the highest degree of deacetylation (DD) at 95%, significantly outperforming the conventional method (81%) and the microwave-assisted method (67%). The autoclave-synthesized chitosan also exhibited the lowest viscosity (33 cP), confirming its low molecular weight. Morphological analysis showed that chitin exhibited a well-defined fibrous structure. After deacetylation, this structure transformed into a rough and porous surface morphology. Thermal analysis further demonstrated that the laboratory-synthesized chitosan exhibited higher thermal stability than the commercial chitosan sample. In conclusion, the autoclave-assisted method proved to be highly efficient for producing low-molecular-weight chitosan with a high degree of deacetylation. However, the conventional method remains the most practical option for scalable industrial production due to its simplicity and well-established infrastructure. Moreover, the laboratory-synthesized chitosan exhibited higher thermal stability, increased porosity, and a higher degree of deacetylation compared to commercially available chitosan, which may offer functional advantages in applications requiring enhanced reactivity, solubility, or thermal resistance. Overall, the findings provide valuable insights into selecting appropriate deacetylation strategies for producing low-molecular-weight chitosan with tailored properties, thereby bridging the gap between laboratory-scale synthesis and potential industrial applications.