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林产化学与工业

林产化学与工业 ›› 2011, Vol. 31 ›› Issue (6): 55-60.

• 研究报告 • 上一篇    下一篇

松香酸淀粉酯的合成与结构表征

唐世华1,2, 李景权1, 覃浩鹏1, 杨酉宝1, 林宇1   

  1. 1. 广西民族大学 化学与生态工程学院, 广西 南宁 530006;2. 广西林产化学品开发与应用重点实验室, 广西 南宁 530006
  • 收稿日期:2011-01-12 修回日期:1900-01-01 出版日期:2011-12-30 发布日期:2011-12-30

Synthesis and Structure Characterization of Rosin Starch Ester

TANG Shi-hua1,2, LI Jing-quan1, QIN Hao-peng1, YANG You-bao1, LIN Yu1   

  1. 1. College of Chemistry and Ecological Engineering,Guangxi University for Nationalities, Nanning 530006, China;2. Key Laboratory of Development and Application of Forest Chemicals of Guangxi, Nanning 530006, China
  • Received:2011-01-12 Revised:1900-01-01 Online:2011-12-30 Published:2011-12-30

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摘要： 以二甲基酰胺(DMF)/LiCl为溶剂,由淀粉与松香酰氯通过O-酰化反应合成了取代度(Ds)为0.125 2的松香酸淀粉酯 (RSE)。利用FT-IR、固体 13C NMR、XRD和SEM对目标产物进行了分析和表征,测试了目标产物的溶解性能和透明度。基于单因素试验数据,利用响应面软件优化,建立了数学模型,得出最佳合成条件为:反应时间 6.5 h,温度 95 ℃,吡啶 3.5 mL,活化时间 52.5 min,DMF用量 29 mL,松香酰氯与葡萄糖单元中羟基物质的量之比1∶1。此条件下得到的RSE产率为 65.89 %,取代度为0.125 2。结果表明,淀粉经松香酯化改性后,结晶度降低;透明度由原淀粉的 99.66 % 降低为 91.67 %,疏水性增强。

关键词: 松香酰氯, 淀粉, 松香酸淀粉酯, 响应面

Abstract: In the presence of DMF/LiCl solvent, rosin starch ester with the degree of substitution (Ds) of 0.125 2 was synthesized by O-acylation of starch with rosin acid chloride. The target product was analyzed and characterized by means of FT-IR, solid state 13C NMR, XRD and SEM. The reaction conditions were studied with single factor experiments and response surface methodology. A reaction model and the optimum conditions were obained. The optimum synthesis conditions were as follows: reaction time 6.5 h, reaction temperature 95 ℃, pyridine amount 3.5 mL, activation time of starch 52.5 min, DMF 29 mL and molar ratio 1∶1 (rosin acid chloride/the hydroxyl group per D-glucose unit). Under optimal conditions, the yield of RSE and Ds were 65.89 % and 0.125 2, respectively. Furthermore, its solubility and diaphaneity were determined. The results showed that compared with the unmodified starch, the crystal linity and diaphaneity of the target product decreased, and its hydrophobicity increased.

Key words: rosin acid chloride, starch, rosin starch ester, response surface methodology

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