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Optimization of N, N, N-trimethylchitosan synthesis by factorial design

Year: 2011

Journal: Polymer International 2011, 60 (6) pp 910-915, 20121211

Authors: Douglas de Britto, Fernando R Frederico, Odilio B Garrido Assis

Organizations: Embrapa—CNPDIA, Rua XV de Novembro 1452, CP 741, 13560-970, São Carlos, SP, Brazil; Faculdade de Engenharia Química, UNICAMP, Campinas, SP, Brazil

Factorial design analysis was applied to optimize the synthesis, via a new route, of N, N, N-trimethylchitosan, based on dimethylsulfate as a methylating agent. The responses analyzed were weight yield, solubility and average degree of quaternization. Temperature was verified as the most important variable, as it caused the most variation in the response. X(T) = - 54.52, - 9.50 and - 7.25, respectively, for weight yield, solubility and degree of quaternization. A sharp decrease in the viscosimetric and gel permeation chromatography parameters proved that severe depolymerization took place at high reaction temperatures. Contact angle measurements showed a decrease in the hydrophilic character of over-methylated samples.