神华煤直接液化残渣理化特性与分子结构特征研究  

Research on physicochemical and molecular structure characteristics of residue from Shenhua direct coal liquefaction

作　　者：刘敏 赵鹏 陈贵锋 张佳 黄澎 王昊 史权[4] Liu Min;Zhao Peng;Chen Guifeng;Zhang Jia;Huang Peng;Wang Hao;Shi Quan(CCTEG China Coal Research Institute,Beijing 100013,China;National Energy Technology&Equipment Laboratory of Coal Utilization and Emission Control,Beijing 100013,China;Kailuan Energy Chemical Co.,Ltd.,Kailuan Hebei 063000,China;State Key Laboratory of Heavy Oil Processing,China University of Petroleum(Beijing),Beijing 102249,China)

机构地区：[1]煤炭科学技术研究院有限公司,北京100013 [2]国家能源煤炭高效利用与节能减排技术装备重点实验室,北京100013 [3]开滦能源化工股份有限公司,河北开滦063000 [4]中国石油大学重质油国家重点实验室,北京102249

出　　处：《煤化工》2024年第1期109-113,126,共6页Coal Chemical Industry

基　　金：中国神华煤制油化工有限公司科技创新项目(煤液化油渣制中间相沥青中试研究)资助(MZYHG-22-01)。

摘　　要：煤液化残渣制备高端炭材料是目前煤直接液化技术领域研究的热点,该过程实现的关键在于煤液化残渣的深度脱灰,而深度脱灰工艺技术开发需要对液化残渣理化特性与分子结构有深入的认识。以神华煤液化残渣为研究对象,借助TG-DTG探究了液化残渣的失重特性;借助激光粒度仪和透射电镜(TEM)分别研究了液化残渣在洗油和四氢呋喃两种溶剂中的粒度分布特性和颗粒形貌特征;在正负离子(±ESI)和正离子大气压光电离(+APPI)模式下,利用傅里叶变换离子回旋共振质谱仪(FT-ICR MS)对液化残渣的分子结构组成进行了鉴别。研究结果表明:液化残渣的主要失重温区为300℃~600℃,466℃时失重速率最大,此时的活性最高;液化残渣在洗油或四氢呋喃中的粒度呈现百纳米级正态分布,残渣在洗油中粒度分布更为集中且粒径更小;液化残渣中含丰富的N1、N2类含氮杂环以及O1、O2、O3、CH类含氧多环的芳香分子构型。The preparation of high value-added carbon materials from direct coal liquefaction residue is currently a hot spot of research on the direct coal liquefaction technology during which efficient and deep deashing is the key technology.Physicochemical and molecular structure characteristics of the liquefaction residue need to be understood for the development of deep deashing technology.The weight loss property of Shenhua coal liquefaction residue was explored by means of TG-DTG.The particle size distribution and particle morphology of liquefaction residue in washing oil and tetrahydrofuran were studied with laser particle size analyzer and transmission electron microscope(TEM).The molecular structure of liquefaction residue was distinguished by means of FT-ICR MS under the mode of±ESI&+APPI.The research results showed that the main temperature range of weight loss of liquefaction residue was 300℃-600℃.The maximum rate of weight loss reached the highest with the strongest activity at 466℃.The particle size of liquefaction residue in washing oil or tetrahydrofuran presented normal distribution at the level of hundreds of nanometers.The particle size distribution of liquefaction residue in washing oil was more concentrated and smaller.There were abundant molecular structures in liquefaction residue,such as N1,N2 heterocycle and O1,O2,O3,CH polycyclic aromatic compounds.

关 键 词：煤直接液化 液化残渣 失重特性 粒度分布 分子结构 离子回旋共振质谱仪 

分 类 号：TQ536[化学工程—煤化学工程]