离子液体介质中OSAS的制备与表征及乳化性质分析

doi:10.16085/j.issn.1000-6613.2019-1218

摘要/Abstract

摘要：

以玉米淀粉（CS）为原料，辛烯基琥珀酸酐（OSA）为酯化剂，在无催化剂条件下，在1-烯丙基-3-甲基氯化咪唑离子液体（AMIMCl）介质中，通过均相酯化反应制备辛烯基琥珀酸淀粉酯（OSAS）。利用红外光谱（FTIR）、X射线衍射（XRD）、扫描电镜（SEM）、热重-红外联用仪（TGA-FTIR）、凝胶渗透色谱（GPC）和偏光显微镜（POM）对产物结构、热特性、相对分子质量及乳化性质进行分析。结果表明，制备OSAS的较佳工艺条件为：时间2h，温度90℃，淀粉质量分数6%，OSA与淀粉脱水葡萄糖单元（AGU）摩尔比可根据所需产品的取代度在0.03～0.24范围内选取。FTIR分析表明，CS已成功发生了酯化反应；XRD与SEM证明所得OSAS为无定形形态的细小颗粒聚结物；TGA-FTIR测试表明，在氮气环境中，OSAS中所接入的辛烯基琥珀酸酯基团能稳定至200℃；GPC与POM证明AMIMCl介质中制备的OSAS是优良的大分子乳化剂。

关键词: 离子液体, 酯化, 制备, 结构表征, 乳液

Abstract:

Octenyl succinic anhydride modified starch (OSAS) was prepared without catalyst in the ionic liquid of 1-alkyl-3-methylimidazolium chloride (AMIMCl), by employing corn starch (CS) as raw material, and octenyl succinic anhydride (OSA) as esterification agent. The structure, thermal characteristics, relative molecular mass and emulsification properties of the product were analyzed by FTIR, XRD, SEM, TGA-FTIR, GPC and POM, respectively. The results showed that the OSAS could be prepared with the following optimum conditions: the reaction time was 2h, the reaction temperature was 90℃, the starch mass fraction was 6%, and the molar ratio of OSA to statch dehydration glucose unit (AGU) was in between 0.03 to 0.24 according to the degree substitution of the desired product. FTIR analysis showed that CS had been esterified successfully. XRD and SEM results indicated that the OSAS were amorphous aggregates of fine particles. TGA-FTIR test showed that the octenyl succinate group in OSAS was stable under 200℃ in nitrogen atmosphere. GPC and POM proved the OSAS prepared in AMIMCl had excellent emulsification properties.

Key words: ionic liquids, esterification, preparation, structure characterization, emulsions

中图分类号:

TS236

何强, 石海信, 王爱荣, 王梓民, 爨珊珊, 王锋. 离子液体介质中OSAS的制备与表征及乳化性质分析[J]. 化工进展, 2020, 39(7): 2802-2809.

Qiang HE, Haixin SHI, Airong WANG, Zimin WANG, Shanshan CUAN, Feng WANG. Preparation and characterization of OSAS in ionic liquid and its emulsification properties[J]. Chemical Industry and Engineering Progress, 2020, 39(7): 2802-2809.

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