Synthesis of the N-butyl chitosan under microwave irradiation
Shitao Yu
Abstract
Shitao Yu
Abstract
High molecular weight chitosan was alkalized under microwave first and then the alkalized chitosan reacted with butyl bromide to synthesize N-butyl chitosan with high molecular weight and high degree of substitution(DS).The effects of alkalization method,alkalization and alkylation reaction temperature,reaction time of alkylation,and the ratio of reactant on the DS of N-butyl chitosan were investigated in detail,and the suitable reaction conditions were obtained as follows:n(sodium hydroxide)∶n(chitosan)=4∶1,viscosity-average molecular weight of chitosanis 1.49×106,microwave reaction alkalization temperature 60 ℃,reaction time 1 h,n(butyl bromide)∶n(alkalized chitosan)=1.4∶1,alkylation reaction temperature 80 ℃,alkalization reaction time 4 h.Under the above conditions,the molecular weight of N-butyl chitosan was 1.48×106 and the DS was up to 78.5%.The structure of alkalized chitosan was confirmed by SEM,the results indicated that the stereoregularity and the inter hydrogen bonds were destroyed.The structure of N-butyl chitosan was characterized by XRD and FT-IR.
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High molecular weight chitosan was alkalized under microwave first and then the alkalized chitosan reacted with butyl bromide to synthesize N-butyl chitosan with high molecular weight and high degree of substitution(DS).The effects of alkalization method,alkalization and alkylation reaction temperature,reaction time of alkylation,and the ratio of reactant on the DS of N-butyl chitosan were investigated in detail,and the suitable reaction conditions were obtained as follows:n(sodium hydroxide)∶n(chitosan)=4∶1,viscosity-average molecular weight of chitosanis 1.49×106,microwave reaction alkalization temperature 60 ℃,reaction time 1 h,n(butyl bromide)∶n(alkalized chitosan)=1.4∶1,alkylation reaction temperature 80 ℃,alkalization reaction time 4 h.Under the above conditions,the molecular weight of N-butyl chitosan was 1.48×106 and the DS was up to 78.5%.The structure of alkalized chitosan was confirmed by SEM,the results indicated that the stereoregularity and the inter hydrogen bonds were destroyed.The structure of N-butyl chitosan was characterized by XRD and FT-IR.
Key concepts: Chitosan, Alkylation, Chemistry, Sodium hydroxide, Nuclear chemistry, Bromide, Polymer chemistry, Microwave irradiation