不同介质下木质素降解转化为香兰素的研究.docVIP

不同介质下木质素降解转化为香兰素的研究 摘要：本论文首先利用N-甲基咪唑与溴代正丁烷反应合成了离子液体中间体：溴化1-丁基-3-甲基咪唑([Bmim]Br)，进而用[Bmim]Br分别与醋酸钾、KOH进行阴离子交换反应，合成离子液体： 1-丁基-3-甲基咪唑醋酸盐（[Bmim]OAC）和氢氧化1-丁基-3-甲基咪唑([Bmim]OH)。通过核磁共振对所合成的离子液体进行了结构表征和确认。接着，研究木质素在这两种离子液体中降解得到香兰素的情况，并和以NaOH的碱性溶液为反应介质的实验进行对照。实验结果表明，NaOH碱性溶液作为反应介质得到的香兰素产率较高。最后研究了在NaOH的碱性溶液中木质素降解转化为香兰素的较优条件，考察木质素氧化过程中催化剂用量和反应温度的变化对香兰素的产量的影响。实验结果表明，最佳工艺条件为： 在NaOH的碱性溶液（PH=11~12）中，催化剂量为木质素重量的10%，反应温度为100℃，反应时间为3h。在最佳工艺条件下，香兰素的收率为8.1%。10554 关键词：木质素；香兰素；离子液体 Study on degradation of lignin for synthesize vanillin in different medium Abstract: In this paper ,the intermediate of ionic liquid : 1-Butyl-3-methylimidazolium Bromide was prepared which are generated from N－methylimidazole with butyl bromide. Then we used the intermediate synthesizes two ionic liquids through anions exchange with potassium acetate and potassium hydroxide. The two ionic liquids are [Bmim]OAC and [Bmim]OH. And their structures were characterized confirmed by 1HNMR.Then, degradation of lignin for synthesize vanillin were studied in two ionic liquids and the alkaline solution of sodium hydroxide was placed in the control experiment. The experimental results shows that the alkaline solution of sodium hydroxide as reaction medium was better. Finally , the better conditions of lignin for synthesize vanillin were studied in the alkaline solution of sodium hydroxide. The influence of process factors, such as amount of the catalyst and reacting temperature upon the yield of vanillin were investigated. The optimal reaction condition as following, medium is in the alkaline solution of sodium hydroxide （PH=11~12）, the catalyst amount is 10% according to the quantity of lignin,reacting temperature is 100 ℃，reaction time is 3h,the best yield of vanillin was about 8.1%. 1.前言 1.1 木质素的简介 1838年法国农学家P.Payen用硝酸处理木材时，发现除剩下像纤维状的物质之外，还有一部分含碳量比纤维状物质还高的物质，前者他定义为ldquo;Celluloserdquo;后者1857年由F.Schuze定义为ldquo;Ligninrdquo;，从此开始了对木质素的研究。接着，十九世纪六十年代初德国学者K. Freudenberg根据生物合成实验的结果提出了针叶材木质素结构的模型图，从中很容易看出木质素基本单元是苯基丙烷，充