摘要
以微晶纤维素为原料,丙烯酰氯为衍生化试剂,制备了丙烯酸纤维素,通过红外(FT-IR)、核磁(NMR)、X射线衍射(XRD)和示差扫描量热法(DSC)等手段对其结构及性质进行了表征,研究了反应各因素对产物取代度的影响,当微晶纤维素在氯化锂/二甲基乙酰胺(LiCl/DMAc)溶液中的质量分数为2.0%,反应温度50℃,反应时间4 h,n(纤维素总羟基量)∶n(丙烯酰氯)1∶4时,产物取代度为2.25。通过13C NMR说明该反应条件下能够得到丙烯酸纤维素;扫描电镜表明丙烯酰氯与微晶纤维素发生了反应,改变了微晶纤维素的形态;X射线衍射结果说明丙烯酸纤维素为完全无定型的结构;热分析得出制备的丙烯酸纤维素为纯净物而不是混合物。
Acrylate cellulose was synthesized by the reaction between avicel and acryloyl chloride. It was characterized with Fou- rier Transform Infrared spectroscopy ( FT-IR), Nuclear Magnetic Resonance ( NMR), X-ray Diffraction ( XRD), Differential Scanning Calorimetry ( DSC), etc. Effects of various experimental factors on the substitution degree ( Ds ) of acrylate cellulose were investigated. The results showed that Ds 2.25 can be obtained at the reaction condition of the temperature at 50 ℃, the time for 4 hours , and the molar ratio of 1 : 4 between hydroxyl content of avicel and acryloyl chloride. 13 C NMR showed that acrylate cellulose could be obtained under the condition of reaction. SEM indicated that acryloyl chloride reacted with avicel and changed the configuration of avicel. XRD results displayed that acrylate cellulose was a completely amorphous structure. Thermal analysis revealed that acrylate cellulose prepared was pure substance rather than a mixture.
出处
《林产化学与工业》
EI
CAS
CSCD
北大核心
2013年第3期73-77,共5页
Chemistry and Industry of Forest Products
基金
南京中医药大学林业新技术所基本科研业务费专项资金(CAFINT2011K01)