响应面法优化羧甲基壳聚糖的制备工艺  

Process Optimization for Preparation of Carboxymethyl Chitosan by Response Surface Methodology

作　　者：郭睿[1] 刘爱玉[1] 郭煜 李欢乐[1] 杨江月[1] 程敏[1] 

机构地区：[1]陕西科技大学教育部轻化工助剂化学与技术重点实验室,陕西西安710021

出　　处：《精细化工》2016年第8期872-879,共8页Fine Chemicals

基　　金：陕西省科技统筹创新工程计划项目(2014KTCL01-11);陕西省科学技术研究发展计划项目(2013K11-19)~~

摘　　要：以壳聚糖(CTS)和氯乙酸为原料,合成了羧甲基壳聚糖(CMC)。采用红外光谱(FTIR)、核磁共振氢谱(1HNMR)、环境扫描电镜(ESEM)和X-射线衍射(XRD)对其结构进行了表征。考察了氯乙酸用量、碱液浓度、碱化时间和反应温度对其O-位取代度(Y_1)和N-位取代度(Y_2)的影响。并在单因素实验的基础上,利用响应面法Box-Behnken实验设计原理中的BBD数学模型,优化了壳聚糖羧甲基化的工艺参数。结果显示:制备羧甲基壳聚糖的最佳工艺条件为,氯乙酸用量5.71 g、w(NaOH)=54%、碱化时间7 h、反应温度40℃。在此工艺条件下,得到产物的Y_1=0.721 3,Y_2=0.285 7,与回归模型的预测结果很接近,相对误差值为0.22%和0.27%。Carboxymethyl chitosan（ CMC） was prepared by reaction of chitosan with chloroacetic acid.The structure of CMC were characterized by Fourier transform infrared spectrum（ FTIR）,H-nuclear magnetic resonance spectrum（1HNMR）,environmental scanning electron microscope（ ESEM） and Xray diffraction（ XRD）. In addition,the effect of chloroacetic acid dosage,sodium hydroxide（ Na OH）mass concentration,alkalization reaction time and reaction temperature on the CMC O-position degree of substitution（ Y1） and N-position degree of substitution（ Y2） were investigated. Furthermore,on the basis of single factor experiment,the technological parameters of chitosan carboxy methylation were optimized by using the mathematical model of BBD in Box-Behnken experiment design principle of response surface methodology. The results indicated that the optimal conditions for the preparation of carboxymethyl chitosan were as follows： chloroacetic acid dosage 5. 71 g,Na OH mass concentration54%,alkalization reaction time 7 h,and the reaction temperature 40 ℃. Under the above conditions,the CMC Y_1 and Y_2 reached 0. 721 3 and 0. 285 7. This result is very close to the predictive result of the regression model,and the relative error value is 0. 22% and 0. 26%.

关 键 词：羧甲基壳聚糖 工艺优化 响应面法 回归模型 功能材料 

分 类 号：O632[理学—高分子化学]