光谱学与光谱分析, 2014, 34 (12): 3415, 网络出版: 2014-12-08   

X射线光电子能谱与13C核磁共振在生物质碳表征中的应用

Characterization of Biochar by X-Ray Photoelectron Spectroscopy and 13C Nuclear Magnetic Resonance
作者单位
北京师范大学环境学院水环境模拟国家重点实验室, 北京100875
摘要
近年来, 生物质碳(biochar)作为新型吸附剂被广泛研究。 但由于制备biochar的生物质原料和热解温度的不同, 使biochar的结构和组成存在差异, 从而影响其对污染物的吸附。 目前关于biochar的结构和组成的研究还不够全面。 因此, 结合了能谱与光谱分析的手段, 对biochar的结构和组成进行了深入的分析。 选取木质类(柳树枝条)和草类(水稻秸秆)作为原料, 分别在不同热解温度(300, 450和600 ℃)下制得biochars, 并对biochars样品进行元素分析、 X射线光电子能谱分析(XPS)和固态13C核磁共振(13C NMR)研究, 以阐明不同热解温度和生物质来源的biochars的结构和组成。 结果显示: biochar的H/C, O/C和(O+N)/C的比值随着热解温度的升高而降低;草类biochar比木质类biochar具有更高的灰分含量和表面极性;木质类biochar的矿物主要分布在样品颗粒内部, 其表面被有机质覆盖, 而草类biochar部分矿物暴露在样品颗粒表面;13C NMR显示低温制得的biochar主要由芳香碳、 脂肪碳、 羧基和羰基碳组成, 高温制得的biochar主要由芳香碳组成, 且低温制得biochars中, 木质类biochars比草类biochars含有更高的木质素的残留碳结构, 这是由于木质类biochars原材料中含有更高的木质素。
Abstract
The wood (willow branch) and grass (rice straw) materials were pyrolyzed at different temperatures (300, 450 and 600 ℃) to obtain the biochars used in the present study. The biochars were characterized using elementary analysis, X-ray photoelectron spectroscopy (XPS) and solid state 13C cross-polarization and magic angle spinning nuclear magnetic resonance spectroscopy (13C NMR) to illuminate the structure and composition of the biochars which were derived from the different thermal temperatures and biomass. The results showed that the H/C, O/C and (O+N)/C ratios of the biochars decreased with the increase in the pyrolysis temperatures. The surface polarity and ash content of the grass-derived biochars were higher than those of the wood-derived biochars. The minerals of the wood-derived biochars were mainly covered by the organic matter;in contrast, parts of the mineral surfaces of the grass-derived biochars were not covered by organic matter. The 13C NMR of the low temperature-derived biochars revealed a large contribution of aromatic carbon, aliphatic carbon, carboxyl and carbonyl carbon, while the high temperature-derived biochars contained a large amount of aromatic carbon. Moreover, the wood-derived biochars produced at low heat treatment temperatures contained more lignin residues than grass-derived ones, probably due to the existence of high lignin content in the feedstock soures of wood-derived biochars. The results of the study would be useful for environmental application of biochars.

徐东昱, 金洁, 颜钰, 韩兰芳, 康明洁, 王子莹, 赵烨, 孙可. X射线光电子能谱与13C核磁共振在生物质碳表征中的应用[J]. 光谱学与光谱分析, 2014, 34(12): 3415. XU Dong-yu, JIN Jie, YAN Yu, HAN Lan-fang, KANG Ming-jie, WANG Zi-ying, ZHAO Ye, SUN Ke. Characterization of Biochar by X-Ray Photoelectron Spectroscopy and 13C Nuclear Magnetic Resonance[J]. Spectroscopy and Spectral Analysis, 2014, 34(12): 3415.

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