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无催化剂条件下在室温离子液体中制备及表征邻苯二甲酸纤维素衍生物

Preparation and characterization of phthalated cellulose derivatives in room-temperature ionic liquid without catalysts.

作者信息

Liu Chuan-Fu, Sun Run-Cang, Zhang Ai-Ping, Qin Men-Hua, Ren Jun-Li, Wang Xin-Ai

机构信息

State Key Laboratory of Pulp and Paper Engineering, South China University of Technology, Guangzhou 510640, China.

出版信息

J Agric Food Chem. 2007 Mar 21;55(6):2399-406. doi: 10.1021/jf062876g. Epub 2007 Feb 24.

Abstract

Homogeneous modification of cellulose, isolated with 10% KOH from delignified sugarcane bagasse, was performed in room-temperature ionic liquid 1-allyl-3-methylinidazolium chloride with phthalic anhydride in the absence of catalyst. The results showed the degree of substitution of phthalated cellulosic derivatives, ranging from 0.10 to 0.73, increased with the increment of reaction temperature, reaction time, and the molar ratio of phthalic anhydride/anhydroglucose units in cellulose under the conditions given. The products were characterized by FT-IR and solid-state CP/MAS 13C NMR spectroscopy as well as thermal analysis, and the results revealed that the phthalation reaction at C-6, C-2, and C-3 positions of the cellulose all occurred. The thermal stability of the phthalated cellulose was found to decrease upon chemical modification. However, this thermal stability of the phthalated cellulose over 200 degrees C is rather satisfactory.

摘要

从脱木质素甘蔗渣中用10%氢氧化钾分离得到的纤维素,在室温离子液体1-烯丙基-3-甲基咪唑氯盐中,于无催化剂条件下与邻苯二甲酸酐进行均相改性。结果表明,在给定条件下,邻苯二甲酸酯化纤维素衍生物的取代度在0.10至0.73之间,随反应温度、反应时间以及纤维素中邻苯二甲酸酐/脱水葡萄糖单元摩尔比的增加而增大。产物通过傅里叶变换红外光谱(FT-IR)、固态交叉极化/魔角旋转13C核磁共振光谱(CP/MAS 13C NMR)以及热分析进行表征,结果表明纤维素的C-6、C-2和C-3位均发生了邻苯二甲酸酯化反应。发现化学改性后邻苯二甲酸酯化纤维素的热稳定性降低。然而,这种邻苯二甲酸酯化纤维素在200℃以上的热稳定性相当令人满意。

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