微波法制备O-羟丙基-N-辛基壳聚糖及其性能表征  

Microwave Synthesis and Characterization of O-Hydroxypropyl-N-octyl Chitosan

作　　者：温俊杰[1] 周莉[1] 王紫威 文彩虹[1] 刘波[1] 

机构地区：[1]深圳大学化学与化工学院,广东深圳518060

出　　处：《应用化学》2015年第2期192-199,共8页Chinese Journal of Applied Chemistry

基　　金：深圳市基础研究项目(JCYJ20130329102614715);深圳市战略新兴产业发展专项资金项目(NYSW20130329010039)~~

摘　　要：通过微波法,由壳聚糖与环氧丙烷反应制备O-羟丙基壳聚糖(HPCS),然后在相转移催化剂四丁基溴化铵作用下与溴化辛烷反应制备成O-羟丙基-N-辛基壳聚糖(C8-HPCS)。中间产物HPCS与目标产物C8-HPCS的结构通过FTIR及1H NMR等技术手段分析得到验证。实验结果表明,当反应时间为50 min,温度为65℃,溴代辛烷用量8 m L,四丁基溴化铵用量0.07 g时,制备所得的C8-HPCS具有较好的综合性能:起泡性为3.9 cm,稳泡性为88.9%,乳化性为78.1%。C8-HPCS的临界胶束浓度(CMC)为0.015 g/L,表面张力约为58.5 m N/m;亲水亲油平衡值(HLB)测定结果为13.44。同步热分析表明C8-HPCS在270℃之前均是稳定的;X射线衍射图谱表明改性后的C8-HPCS为非晶体结构。O-hydroxypropyl-N-octyl chitosan（C8-HPCS） was prepared by reacting 1-octyl bromide with Ohydroxypropyl chitosan（HPCS） under microwave heating. HPCS was prepared with chitosan and propylene oxide in presence of phase transfer catalyst tetrabutylammonium bromide. The intermediate HPCS and the objective product C8-HPCS were characterized by FTIR and1 H NMR spectroscopy. The results show that C8-HPCS has an excellent integrated performance when the reaction time is 50 min,the temperature is 65 ℃,the dosage of bromooctane is 8 m L and the dosage of tetrabutylammonium bromide is 0. 07 g. The foamability,foaming property and emulsibility are 3. 9 cm,88. 9% and 78. 1%, respectively. The critical micelle concentration of C8-HPCS is 0. 015 g/L with the surface tension of 58. 5 m N/m and the hydrophile lipophile balance number is 13. 44. The thermal stability analysis shows that the C8-HPCS is stable up to 270 ℃ and the XRD analysis indicates that the quaternized chitosan is completely amorphous.

关 键 词：微波法 相转移催化法 壳聚糖衍生物 表面活性剂 

分 类 号：O647.2[理学—物理化学] O636.1[理学—化学]