食品科学 ›› 2011, Vol. 32 ›› Issue (4): 1-6.doi: 10.7506/spkx1002-6630-201104001

• 工艺技术 •    下一篇

高取代度淀粉醋酸酯合成工艺优化及结构表征

李海龙,陈 鹏,DIOP Cherif Ibrahima Khalil,谢笔钧,孙智达   

  1. 华中农业大学食品科技学院
  • 出版日期:2011-03-12 发布日期:2017-04-06
  • 基金资助:
    “十一五”国家科技支撑计划项目(2006BAD27B09-4)

Highly Substituted Starch Acetate: Optimization of Synthesis Process and Structural Characterization

LI Hai-long,CHEN Peng,DIOP Cherif Ibrahima Khalil,XIE Bi-jun,SUN Zhi-da   

  1. College of Food Science and Technology, Huazhong Agricultural University, Wuhan 430070, China
  • Online:2011-03-12 Published:2017-04-06

摘要: 以玉米淀粉为实验材料,在催化剂用量、醋酸与醋酸酐体积比、反应时间、反应温度4个单因素试验基础上,利用响应面试验设计法进行试验设计,获得取代度与各单因素的函数关系,并建立高取代度淀粉醋酸酯合成工艺模型。通过回归方程和响应曲面,得到淀粉醋酸酯最佳合成工艺为催化剂用量0.11mL、醋酸与醋酸酐体积比1:1.39、反应时间1.59h、反应温度87.61℃。验证实验结果显示,在此条件下淀粉醋酸酯取代度为2.95。傅里叶红外光谱分析表明,淀粉醋酸酯葡萄糖单元上的羟基逐渐发生酯化,而且随着取代度测定值升高,乙酰基含量增大。扫描电镜照片显示,淀粉醋酸酯表面变得更为粗糙,孔隙增多且呈蜂窝状,说明酯化反应不仅发生在淀粉颗粒表面,同时也发生在淀粉颗粒内部。

关键词: 淀粉醋酸酯, 合成工艺, 响应面法, 取代度, 红外色谱, 扫描电镜

Abstract: To optimize the process for the synthesis of starch acetate from corn starch, the effects of catalyst amount, the volume mixing ratio of acetic acid to acetic anhydride, and reaction time and temperature on the degree of substitution (DS) of starch were evaluation by single factor experiments, and a mathematical model describing the functional relationship between starch DS and the above four variables was set up based on a 29-run, 4-factor, 3-level response surface design coupled with multiple regression fitting. The model was subjected to analysis of variance and response surface analysis, and the results showed that the optimum conditions for the synthesis of starch acetate were as follows: catalyst amount of 0.11 mL and the mixing ratio of acetic acid to acetic anhydride of 1:1.39 by volume for a reaction period of 1.59 h at 87.61 ℃. Validation experiments indicated that the maximum substitution degree of starch acetate was 2.95 under these conditions. FTIR results indicated that the hydroxyl groups in each glucose unit of starch acetate were gradually esterified, and meanwhile the content of acetyl group became higher with the increase of substitution degree. Scanning electron microscopic (SEM) observations revealed that the surface of starch acetate was much rougher, had increased porosity and displayed cellular structure, indicating that the esterification occurred not only on the surface but also inside of starch granule.

Key words: starch acetate, synthesis process, response surface methodology, substitution degree, infrared spectroscopy, scanning electron microscope

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