响应面法优化羧甲基壳聚糖的制备工艺

Synthesis of Carboxymethyl Chitosan and Optimization by Using Response Surface Methodology

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Y1和N-位取代度Y2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。最后获得制备羧甲基壳聚糖的最佳工艺条件为：氯乙酸用量为5.71g、w（NaOH）=54%、碱化时间7h、反应温度40℃。在此工艺条件下，得到产物的Y1=72.13%，Y2=28.57%，与回归模型的预测结果很接近,相对误差值仅为0.22%和0.26%。

Abstract:

Carboxymethyl chitosan(CMC) was prepared by reacting of chitosan with chloroacetic acid. The structure of CMC was characterized by Fourier transform infrared spectrum (FTIR), nuclear magnetic resonance spectrum (1HNMR), environmental scanning electron microscope (ESEM) and X-ray diffraction (XRD). In addition, the effects of chloroacetic acid dosage, lye concentration, alkalization time, and reaction temperature on the O-substitution degree (O-DS,Y1) and N-substitution degree(N-DS,Y2) were investigated. Furthermore, on the basis of single factor experiment, the corresponding technological parameters were optimized by using the BBD mathematical model in Box-Behnken experimental principle of response surface methodology (RSM). It was found that that the optimal processing for the preparation of carboxymethyl chitosan were as follows: chloroacetic acid dosage 5.71 g, lye concentration(NaOH) content 54%, alkalization time 7h, and the reaction temperature 40℃. The products has highest DS, Y1=72.13%,Y2=28.57%. In comparison with predictive results of the regression model, the relative error is only 0.22% and 0.26%. respectively.