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采用一步法合成N-烯丙基吡啶氯盐离子液体([APy]Cl),用红外光谱(FT-IR)和核磁共振(1H-NMR)进行结构表征,并与常用有机溶液(二甲基亚砜(DMSO)、N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAc)及吡啶)配成复合溶剂,测定并比较对棉浆粕的溶解能力。结果表明,四种复合溶剂均为纤维素的优良溶剂,其中在[APy]Cl/DMAc复合溶剂中溶解性能最佳,在100℃、DMAc质量分数为40%时,溶解度能达到12.25%。利用FT-IR、X射线衍射(XRD)和热重分析(TGA)对溶解再生前后纤维素膜的结构进行分析。结果表明,四种复合溶剂均为纤维素的直接溶剂,可将晶型由Ⅰ转变成Ⅱ,热稳定性良好。

N-allylpyridinium chloride ionic liquid(Cl) was synthesized by one-step process,and its structure was characterized by 1H nuclear magnetic resonance spectrum(1H-NMR) and Fourier transform infrared spectra(FT-IR).The dissolubilities of cotton pulp in Cl/common solvents(dimethylsulfoxide(DMSO),N,N-dimethylformamide(DMF),N,N-dimethylacetamide(DMAc) or pyridine) were measured and compared.The results show that four kinds of compound solvents are excellent solvent for cellulose,and the solubility in Cl/DMAc is better than in several other solvents under the same conditions.When the content of DMAc is 40%,the solubility of cotton pulp is up to 12.25% at 100 ℃.The original cellulose and the regenerated cellulose were analyzed by FT-IR,Xray diffraction(XRD) and thermogravimetric analysis(TGA),respectively.The results show that these compound solvents are non-derivatizing solvents for cellulose and,make the crystal form of regenerated cellulose transform from celluloseⅠto celluloseⅡ.Furthermore,the regenerated cellulose shows good thermal stability.

参考文献

[1] Maki-Arvela, P.;Anugwom, I.;Virtanen, P.;Sjoholm, R.;Mikkola, J. P. .Dissolution of lignocellulosic materials and its constituents using ionic liquids - a review.[J].Industrial Crops and Products,2010(3):175-201.
[2] 刘雁红,邓宇.棉秆纤维素在离子液体中溶解及分离的工艺参数[J].农业工程学报,2009(09):259-263.
[3] 李云台,刘华.新型再生纤维素纤维的性能对比与鉴别[J].棉纺织技术,2003(09):31-34.
[4] A. M. A. Nada;H. Abou Yousef;S. El-Gohary .Thermal degradation of hydrolyzed and oxidized lignins[J].Journal of thermal analysis and calorimetry,2002(1):265-273.
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