作　　者： ; ; ; ;

机构地区： 中国林业科学研究院林产化学工业研究所国家林业局林产化学工程重点开放性实验室

出　　处： 《化学试剂》 2013年第8期733-737,740,共6页

摘　　要： 合成了1-甲基-3-丁基咪唑醋酸盐([Bmim]OAc)、1-甲基-3-丁基咪唑碳酸盐([Bmim]2CO3)及1-甲基-3-丁基咪唑氢氧化物([Bmim]OH)离子液体,由FT-IR、1HNMR、13CNMR和元素分析对结构进行了确证。首先用离子液体对壳聚糖碱化,再令碱化后壳聚糖与溴代十六烷进行烷基化反应,制备高取代度的N-十六烷基化壳聚糖。用FT-IR、XRD对烷基化产物进行了表征。考察时间、温度及物料配比对N-十六烷基壳聚糖取代度的影响,得到较佳的反应条件:n([Bmim]OH)∶n(壳聚糖原料)=3∶1,40℃碱化1 h,n(溴代十六烷)∶n(碱化后壳聚糖)=2∶1,烷基化反应温度85℃,反应时间3.5 h,在该条件下十六烷基壳聚糖的取代度达到75%以上。离子液体具有重复使用性,反应后的离子液体重复使用3次后,N-十六烷基壳聚糖的取代度仍>75%。 The [ Bmim ] OAc, [ Bmim ] 2 CO3 and [ Bmim ] OH ionic liquid were synthesized and the structure were confirmed by IR, ^1HNMR,^13 CNMR and elemental analysis. First, chi-tosan was alkalized by ionic liquid. Then the alkalized chi-tosan reacted with bromohexadecane. And thus N-cetyl chi-tosan with high degree of substitution（DS） was produced. The structure of alkylation product was characterized by IR and XRD. The effects of time, temperature and the ratio of reactant on the DS of N-cetyl chitosan were investigated. The suitable reaction conditions were found as follows ： n （ [ Bmim ] OH ） ： n（chitosan） =3： 1,the chitosan was alkalized for 1 h with alkalization temperature 40 ℃ , n （ bromohexadecane ） ： n（alkalized chitosan） = 2 ： 1, the alkalized chitosan reacted for 3.5 h with alkylation reaction temperature 85 ℃. Under above conditions, the DS of N-cetyl chitosan can be over 75 %. The reusability of the ionic liquid was also investigated, and it was found that the DS still could be kept above 75% after the [ Bmim] OH ionic liquid was reused for 3 times with-out any retreatment.

关 键 词： 碱性离子液体 碱化 烷基化 十六烷基壳聚糖

领　　域： [理学] [理学]