先锋褐煤可溶有机质中含氮化合物的组成和结构特征（英文）  

Composition and structural characteristics of nitrogen-containing species in the soluble organic species of Xianfeng lignite

作　　者：肖剑[1] 赵云鹏[1,2] 丁曼[1] 魏贤勇[1] 宗志敏[1] 

机构地区：[1]中国矿业大学煤炭加工与高效利用教育部重点实验室,江苏徐州221116 [2]太原理工大学煤科学与技术省部共建国家重点实验室培育基地,山西太原030024

出　　处：《燃料化学学报》2017年第4期385-393,共9页Journal of Fuel Chemistry and Technology

基　　金：supporded by the Fundamental Research Funds for the Central Universities(China University of Mining and Technology,2015QNA25);Open Foundation from State Key Laboratory Breeding Base of Coal Science and Technology Co-founded by Shanxi Province and Ministry Education(MKX201502);Priority Academic Program Development of Jiangsu Higher Education Institutions~~

摘　　要：先锋褐煤在高压釜中用等体积的甲醇/甲苯溶剂300℃下热溶得到热溶物和热溶残渣,利用X射线光电子能谱(XPS)分析了先锋褐煤及其热溶残渣中氮的形态,利用气相色谱/质谱(GC/MS)和电喷雾傅里叶变换-离子回旋共振质谱(ESI FT-ICR MS)分析了热溶物中含氮化合物的组成和结构特征。研究表明,先锋褐煤中氮形态含量顺序为季氮>吡啶氮>吡咯氮,而季氮在热溶过程中更易溶出。GC/MS共检测出热溶物中20种含氮化合物,并且大部分为胺类化合物。ESI FT-ICR MS检测出热溶物中300多种含氮化合物,大部分含氮化合物含一个或三个氮原子。含一个氮原子的含氮化合物主要以N_1O_1、N_1O_2和N_1O_xS_(1-2)类化合物为主,而含三个氮原子的含氮化合物主要以N_3O_xS_(1-2)(x=1-12)类化合物为主。含一个氮原子的含氮化合物的等效双键数和碳数随氧原子数增加而增加。Xianfeng lignite（XL）was firstly thermal dissolved in the isometric toluene/methanol mixed solvent at 300℃in a stainless-steel autoclave to afford a soluble portion（SPXL）and a residue（RXL）,then the nitrogen forms in XL and RXLwere characterized with X-ray photoelectron spectroscopy（XPS）analysis,and the nitrogen-containing species（NCSs）in SPXLwere identified using gas chromatography/mass spectrometry（GC/MS）and electrospray ionization Fourier transform ion cyclotron mass spectrometry（ESI FT-ICR MS）analyses.The results showthat the amount of nitrogen forms in XL is in the order of quaternary-Npyridinic-Npyrrolic-N,while quaternary-N in XL is easily dissolved out during thermal dissolution.In total 20 NCSs were detected in SPXLby GC/MS,and most of them are amines.Over three hundreds of NCSs were identified in SPXLby ESI FT-ICR MS,and most of them are the NCSs containing one or three nitrogen atoms.The NCSs containing one nitrogen atom are mainly dominated by N1O1,N1O2 and N1OxS（1-2） class species,while most of NCSs containing three nitrogen atoms are N3OxS（1-2） class species（x=1-12）.The double bond equivalent（DBE）values and carbon number of the NCSs containing one nitrogen atom increase with increasing number of oxygen atoms.

关 键 词：褐煤 热溶 含氮化合物 碳数 等效双键数 

分 类 号：TQ530[化学工程—煤化学工程]