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材料研究学报  2012, Vol. 26 Issue (4): 408-413    
  研究论文 本期目录 | 过刊浏览 |
C--6羧基氧化纤维素醋酸酯的制备和性能
王凯, 唐爱民
华南理工大学制浆造纸工程国家重点实验室 广州 510640
Preparation and Property of Oxidized Cellulose Acetate with C–6 Carboxyl Groups
WANG Kai, TANG Aimin
State Key Laboratory of Pulp and Paper Engineering, South China University of Technology, Guangzhou 510640
引用本文:

王凯 唐爱民. C--6羧基氧化纤维素醋酸酯的制备和性能[J]. 材料研究学报, 2012, 26(4): 408-413.
, . Preparation and Property of Oxidized Cellulose Acetate with C–6 Carboxyl Groups[J]. Chin J Mater Res, 2012, 26(4): 408-413.

全文: PDF(918 KB)  
摘要: 以溶解级木浆作为原料, 通过TEMPO(2,2,6,6--四甲基哌啶--1--氧化物自由基)/NaClO/NaClO2氧化体系对纤维素C--6羟基进行氧化, 经过乙酰化处理后制备出C--6位含羧基的氧化纤维素醋酸酯。用红外光谱(IR)、X--射线衍射(XRD)和核磁共振(NMR)等手段表征了产物的结构, 用热重分析(TGA)和差示扫描量热法(DSC)测试了产物的热性能。结果表明: 所合成氧化纤维素醋酸酯的C--6位羧基取代度为0.15, 乙酰基取代度为2.72(其中C--2为0.93、C--3为0.98、C--6为0.81)且取代均匀性较好;
用C--6羟基的选择性氧化预处理可实现纤维素的可控酯化; 产物能溶于DMSO(二甲基亚砜); 产物的晶型由纤维素I型转变成纤维素II型。氧化纤维素醋酸酯在185℃发生玻璃化转变, 在257℃熔融。乙酰基的接入, 使产物的热塑性提高。
关键词 有机高分子材料氧化纤维素醋酸酯TEMPO氧化乙酰化    
Abstract:Oxidized cellulose acetate with a free carboxylic acid group content of 0.93mmol/g on C–6 position of the glucose and a total degree of substitution (DS) 2.72, was prepared by oxidizing the dissolving wood pulp with TEMPO/NaClO/NaClO2 and then reacted with a mixture of acetic acid and acetic anhydride with sulfuric acid as catalyst. The structure of the product was characterized with Fourier transfer infrared spectroscopy, X–ray diffraction analysis, proton and carbon–13 nuclear magnetic resonance. The thermal properties were tested by thermo–gravimetry analysis and differential scanning calorimetry. The results show the product has a good substitution uniformity with C–2, C–3 and C–6 position’s acetyl DS of 0.93, 0.98 and 0.81 respectively. The product can dissolve in dimethylsulfoxide, and has good thermoplastic with a melting point of 257 degree celsius. The acetyl access improves thermoplastic of the product.
Key wordsorganic polymer material    oxidized cellulose acetate    TEMPO–mediated oxidation    acetylation
收稿日期: 2012-05-30     
ZTFLH: 

TB324

 
基金资助:

国家重点基础研究发展计划(973)2010CB732206资助项目。

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