Sun Xiao-Feng, Sun RunCang, Sun Jing-Xia
College of Forestry, The North-Western Sciences and Technology University of Agriculture and Forestry, Yangling, People's Republic of China.
J Agric Food Chem. 2002 Oct 23;50(22):6428-33. doi: 10.1021/jf020392o.
An investigation of the acetylation of rice straw with acetic anhydride at 100 and 120 degrees C for 1-4 h with four tertiary amine catalysts (pyridine, 4-dimethylaminopyridine, N-methylpyrrolidine, and N-methylpyrrolidinone) or without catalyst in a solvent-free system was undertaken, and the extent of acetylation was measured by weight percent gain, which increased with the extent of reaction time and temperature and the amounts of catalyst used. 4-Dimethylaminopyridine was found to be the most effective catalyst of those studied. At a concentration of 7% of the catalyst in acetic anhydride, a weight percent gain of 15.4% was realized, compared with 11.2% for the noncatalyst reaction, after 0.5 h of exposure to the system at 120 degrees C. Characterization of acetylated straw was performed by FT-IR, CP MAS (13)C NMR, and thermal studies. Interestingly, the acetylated straw is significantly hydrophobic and does not get wet with water, thereby offering potential for the better utilization of cheap waste materials as natural sorbents in oil cleanup.
在无溶剂体系中,研究了在100℃和120℃下用乙酸酐对稻草进行乙酰化反应1 - 4小时,使用四种叔胺催化剂(吡啶、4 - 二甲基氨基吡啶、N - 甲基吡咯烷和N - 甲基吡咯烷酮)或不使用催化剂的情况,并通过增重百分比来测量乙酰化程度,该程度随反应时间、温度以及所用催化剂的量的增加而增加。在所研究的催化剂中,发现4 - 二甲基氨基吡啶是最有效的催化剂。在120℃下将体系暴露0.5小时后,当催化剂在乙酸酐中的浓度为7%时,实现了15.4%的增重百分比,相比之下,无催化剂反应的增重百分比为11.2%。通过傅里叶变换红外光谱(FT - IR)、交叉极化魔角旋转(13)C核磁共振(CP MAS (13)C NMR)和热分析对乙酰化稻草进行了表征。有趣的是,乙酰化稻草具有显著的疏水性,不会被水浸湿,因此为更好地利用廉价废料作为石油清理中的天然吸附剂提供了潜力。