农林生物质定向液化制备甲基-α-D-葡萄糖苷的研究  

Preparation of Methyl-α-D-glucoside from Fractionation of Direct Liquefied Lignocellulosic Biomass

作　　者：冯君锋 蒋剑春[2,3,4,5,6] 徐俊明[1,2,3,4,5,6] 王奎[1,2,3,4,5] 苏秋丽[2,3,4,5] 杨中志[2,3,4,5] 

机构地区：[1]中国林业科学研究院林业新技术研究所,北京100091 [2]中国林业科学研究院林产化学工业研究所 [3]生物质化学利用国家工程实验室 [4]国家林业局林产化学工程重点开放性实验室 [5]江苏省生物质能源与材料重点实验室,江苏南京210042 [6]江苏强林生物能源材料有限公司,江苏溧阳213364

出　　处：《林产化学与工业》2016年第4期23-30,共8页Chemistry and Industry of Forest Products

基　　金：中国林科院林业新技术所基本科研业务费专项资金(CAFINT2013C05);中国林科院中央级公益性科研院所基本科研业务费专项资金(CAFYBB20142D003);国家自然科学基金资助项目(31422013)

摘　　要：以硫酸为催化剂、甲醇为溶剂,在反应温度为200℃、压力6 MPa、反应时间为10 min的条件下,考察竹材、甘蔗渣、杨木、桉木、松木和麦秆6种原料的定向液化,通过对定向液化的产物进行过滤、中和、萃取分离和旋蒸等一系列分级处理操作,得到甲基糖苷类化合物。结果显示:6种原料的液化率均在78%以上,甲基糖苷类化合物主要为甲基-α-D-葡萄糖苷(MLG)和甲基-α-D-木糖苷,其分别来自于纤维素和半纤维素的甲醇酸解,并且甲基糖苷类化合物的得率均为原料质量的40%左右;其中甘蔗渣加压液化制备甲基糖苷类的效果最好,甲基糖苷类GC含量86.81%。将甲基糖苷类化合物进行脱色和重结晶处理,得到甲基-α-D-葡萄糖苷晶体,对其进行HSQC NMR、FT-IR和X射线单晶衍射分析可知,实验所制备的甲基-α-D-葡萄糖苷晶体纯度几乎接近于标准样品,具有规则的晶体结构,晶体属于正交晶系,空间群为P212121。Directional liquefaction（methlysis） of lignocellulosic biomass （bamboo, bagasse, poplar, eucalyptus, pine and wheat straw） were investigated in the presence of sulfuric acid as catalyst at 200 ℃ for 10 min. The methyl glycosides （MG） in liquid products could be obtained via stepwise treatments of filtering neutralization, and extracting, followed by rotary evaporation. Both hemicellulose and cellulose （holocellulose） in the lignocellulosic biomass could convert into methyl glycosides, mainly methyl-α- D-xyloside and methyl-α-D-glucoside （MLG）, and the yield of MG was about 40%. GC content of MG could reach 86.81%. At the same time, decolorization and purification of MG was also investigated for preparation of pure MG crystals. According to the results of HSQC NMR,FT-IR and X-ray diffraction by a single crystal, the prepared MLG had high purity dose to the standard sample and regular crystal structure of orthorhombic system and space group P212121.

关 键 词：生物质 定向液化 甲基葡萄糖苷 

分 类 号：TQ35[化学工程] TK62[动力工程及工程热物理—生物能]