竹屑加压液化制备甲基糖苷和酚类物质  

Preparation of Methyl Glucoside and Phenols from Pressurized Liquefaction of Bamboo

作　　者：苏秋丽[1] 蒋剑春[1,2] 冯君锋 李芳琳 徐俊明 

机构地区：[1]中国林业科学研究院林产化学工业研究所生物质化学利用国家工程实验室国家林业局林产化学工程重点开发性实验室江苏省生物质能源与材料重点实验室,江苏南京210042 [2]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》2017年第6期81-88,共8页Chemistry and Industry of Forest Products

基　　金：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(CAFYBB2014ZD003)

摘　　要：以竹屑为原料,通过加压液化获得产物甲基糖苷和4种不同相对分子质量的酚类物质,采用多种方法分析了产物组成和结构,考察了不同温度对液化过程的影响,阐明了加压液化过程中木质纤维结构变化规律和产物形成机理。结果表明:绝干竹屑40 g,当m(竹屑)∶m(甲醇)=1∶12,浓硫酸1 g,反应时间10 min,反应温度200℃时,液化产物得率为87.83%,其中甲基糖苷得率48.17%,酚类得率39.66%。通过气相色谱-质谱联用(GC-MS)、高效液相色谱(HPLC)分析产物,结果表明:在液化过程中,纤维素和半纤维素在较低温度下分解,较高液化温度更有利于木质素分解。温度过高时甲基糖苷会进一步分解为酯类和糠醛类化合物。通过对液化残渣的X射线衍射(XRD)、傅里叶红外光谱(FT-IR)分析显示,120~200℃非结晶区的纤维素、木质素和半纤维素部分降解,残渣纤维结晶度相对原料提高6.12%~40.33%,超过200℃,纤维结构完全破坏。Bamboo sawdust was used as the raw material for pressurized liquefaction to obtain methyl glucoside and four kinds of phenols at different temperatures. The products composition and structure were analyzed by various methods. In addition, the variation of structure of lignoceUulosic biomass in liquefaction process and the formation mechanism of liquefied products were investigated. The results showed that when liquefaction conditions were 40 g bamboo sawdust, m （bamboo） ： m （ CH3 OH） = 1 ： 12, the dosage of sulfuric acid 1 g, reaction time 10 min, and reaction temperature 200 ℃, the yield of liquefied product was 87. 83% with 48.17% methyl glucoside and 39. 66% phenols. The components and contents of methyl glucoside and phenols were characterized by gas chromatography-mass spectrometer （GC-MS） and high performance liquid chromatography （HPLC） analysis. The results showed that the degradation temperatures of cellulose and hemicellulose were low and the high temperature was beneficial to the degradation of lignin. The liquefaction residue was characterized by X-ray diffraction （XRD） and Fourier transform infrared spectrum analysis（FF-IR）. The results showed that the crystal index of cellulose in the residue of 120 - 200 ℃ degradation was 6. 12% - 40. 33% higher than that in the raw material. The reason could be explained as that thedecomposition of lignin and hemicellulose in the amorphous region was destroyed partly during 120- 200 ℃, however, the structure of amorphous region and crystalline region was destroyed completely in the 220 ℃.

关 键 词：液化机理 甲基糖苷 杂多酚 纤维结构 相对结晶度 

分 类 号：TQ35[化学工程]