马来松香木薯淀粉酯的微波合成(英文)

Microwave-assisted Synthesis of Maleated Rosin-cassava Starch Ester

在微波辐照下,通过木薯淀粉与马来松香酰氯(MPA-C l)的O-酰化反应合成了不同取代度的马来松香木薯淀粉酯(MRCSE),利用FT-IR、NMR、X射线衍射(XRD)和元素分析对MRCSE进行了表征。探讨了反应条件对MRCSE取代度的影响,通过单因素试验得出最佳合成工艺条件为:木薯淀粉0.5 g,MPA-C l 3.4 g,吡啶体积25 mL,淀粉活化时间1.5 h,反应温度110℃,功率700 W,反应时间1.5 h,物质的量比1∶1(马来松香酰氯-葡萄糖单元中羟基数)。并测试了DS为0.170的MRCSE的特性黏度和溶解性能。结果表明,与原料木薯淀粉相比,MRCSE的特性黏度降低、溶解性能变好,尤其可溶于冷水,即MRCSE是一种新型水溶性淀粉衍生物。

Maleated rosin-cassava starch esters （MRCSE） of different degree of substitution （Ds ） were synthesized by O-acylation of cassava starch with maleopimaric acid chloride （MPA-Cl） under microwave irradiation. By single factor experimentation, the optimal conditions for the synthesis of MRCSE were obtained as follows ： cassava starch 0.5 g, MPA-Cl 3.4 g, reaction time 1.5 h, reaction temperature 110℃, microwave power 700 W, pyridine amount 25 mL, activation time of cassava starch 1.5 h, and molar ratio 1 ： 1 （maleated rosin chloride to the hydroxyl group per D-glucose unit）. The resulted MRCSE was characterized by means of FT-IR, NMR, XRD, and elemental analysis. Also, the effect of reaction conditions on the Ds of MRCSE has been studied. The intrinsic viscosity and solubility of MRCSE with Ds value of 0. 170 were measured. The results showed that the modified starch esters have lower intrinsic viscosity and better solubility than the raw cassava starch, especially water-solubility, indicating that MRCSE is a novel water-soluble starch derivative.