随着煤基碳材料的发展，石墨烯及石墨烯氧化物等二维碳纳米材料已成为目前新型材料中重要研究领域并成为研究热点。为查明煤基氧化石墨烯的化学成分组成和分子结构特征，以北京西山矿区侏罗纪门头沟系的8号煤层无烟煤为碳源，对京西原煤样和脱灰样进行了工业分析和元素分析，京西煤属于品质较好的低灰、低挥发分和特低硫无烟煤，脱灰后京西无烟煤的灰分产率从初始的9.26%下降到0.65%，表明矿物得到了有效去除。利用改良的Hummers氧化还原法制备煤基氧化石墨烯，并对制备的氧化石墨烯进行了核磁共振碳谱(13C-NMR)、扫描电子显微镜(SEM)、能量色散X-射线光谱(EDS)和X射线光电子能谱(XPS)等分析手段测试。通过Origin软件对所得数据进行分析和图谱拟合，得到了所制备煤基氧化石墨烯产品的元素比和产品结构参数。研究表明：京西煤基氧化石墨烯的芳香结构以苯、萘、蒽和菲为主；脂肪碳以次甲基、环烷烃的形式存在，其中含氧官能团以酚羟基和醚氧基为主，还含有大量的羧基。在此分析数据的基础上，构建了京西煤基氧化石墨烯的分子结构模型，并运用13C-NMR预测软件ACD/CNMR predictor对其进行了结构修正，所得到的GO-JX分子结构模型与试验核磁共振图谱较一致。

With the development of coal-based carbon materials,graphene,graphene oxide and other two-dimensional carbon nano materials have become an important research field in new carbon materials. In order to clarify the chemical composition and molecular structure characteristics of coal based graphene oxide,coal based graphene oxide was prepared by modified Hummers oxidation-reduction method with anthracite from No.8 coal seam of Jurassic Mentougou coal measures in Xishan mining area of Beijing as carbon raw material. The roximate and ultimate analysis of Jingxi coal sample and demineralization coal sample were carried out. The results shown that Jingxi coal is low ash yield,low volatile and ultra-low sulfur anthracite with good quality. After demineralization,the ash yield of Jingxi anthracite decreased from 9.26 wt% to 0.65 wt%,indicating that the minerals have been effectively removed. The prepared graphene oxide was analyzed by 13C-NMR,SEM,EDS and XPS. The data were analyzed and fitted by Origin,and the element ratio and structure parameters of the product were obtained. The results showed that the aromatic structure of Jingxi coal based graphene oxide was mainly benzene,naphthalene,anthracene and phenanthrene; the aliphatic carbon was in the form of methylene and cycloalkanes,in which the oxygen containing functional groups were mainly phenolic hydroxyl and ether oxy,and also contained a large number of carboxyl groups. On the basis of the analysis data,the molecular structure model of Jingxi coal based graphene oxide was constructed and modified by the 13C-NMR prediction software ACD/CNMR predictor. The molecular structure model of GO-JX was consistent with the experimental NMR spectra.

0 引言

1 样品的制备与试验方法

   1.1 矿物脱除

   1.2 氧化石墨烯的制备

   1.3 测试方法

2 结果与讨论

   2.1 工业分析和元素分析

   2.2 核磁共振碳谱分析

   2.3 扫描电子显微镜测试分析

3 分子模型的基本结构

   3.1 芳香结构

   3.2 脂肪碳结构

   3.3 杂原子结构

4 模型的构建和结构优化

   4.1 模型的构建

   4.2 模型的优化

5 结论