一锅法制备有机钼催化剂及加氢性能研究  

Preparation of organic molybdenum catalyst by one-pot method and its hydrogenation performance

作　　者：王熺乾 王光耀 赵渊 WANG Xiqian;WANG Guangyao;ZHAO Yuan(Beijing Research Institute of Coal Chemistry,China Coal Research Institute Corporation Ltd.,Beijing 100013,China;State Key Laboratory of Coal Mining and Clean Utilization,Beijing 100013,China;National Energy Technology&Equipment Laboratory of Coal Utilization and Emission Control,Beijing 100013,China)

机构地区：[1]煤炭科学技术研究院有限公司煤化工分院,北京100013 [2]煤炭资源高效开采与洁净利用国家重点实验室,北京100013 [3]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

出　　处：《煤质技术》2022年第4期23-29,36,共8页Coal Quality Technology

基　　金：煤炭科学技术研究院有限公司科技发展基金资助项目(2020CX-II-03)。

摘　　要：制备具有良好分散性的有机钼催化剂对改进煤直接液化催化剂具有十分重要的意义。以钼酸铵为钼源、二硫化碳为硫源,采用一锅法直接合成1种金属钼含量为29.79%、硫/钼比为2.05的有机钼催化剂。利用扫描电镜、X射线衍射谱、X射线光电子能谱、高分辨透射电镜、红外光谱和热重分析仪等手段对钼催化剂及其硫化物进行表征,发现钼催化剂颗粒呈棒状且层间堆积紧密。钼催化剂在硫化后得到球状的二硫化钼颗粒,主要由1~4层、长度5 nm~11 nm、层间距0.65 nm的二硫化钼片层结构组成。钼催化剂经溶解浸渍后在煤粉表面形成尺寸为1μm×0.2μm的棒状结构。少量钼催化剂与铁催化剂共同使用时,相比于单独使用的铁催化剂,共同使用催化剂的煤直接液化反应油产率提高3.53个百分点,转化率提高4.22个百分点。The preparation of organic molybdenum catalyst with good dispersity is of great significance for the improvement of direct coal liquefaction catalysts.An organic molybdenum catalyst with molybdenum content of 29.79%and sulfur/molybdenum ratio of 2.05 was synthesized directly by one-pot method using ammonium molybdate as molybdenum source and carbon disulfide as sulfur source.The molybdenum catalyst and the its sulfide were characterized by scanning electron microscopy,X-ray diffraction,X-ray photoelectron spectroscopy,high resolution transmission electron microscopy,infrared spectroscopy and thermogravimetric analysis.It was found that the molybdenum catalyst was rod-like and dense packing.The spherical molybdenum disulfide particles were obtained by heating molybdenum catalyst and mainly composed of lamellar structure with 1 layers-4 layers,the length of 5 nm-11 nm and the distance of 0.65 nm.The molybdenum catalyst was impregnated to form a rod structure with size of 1μm×0.2μm on the surface of coal powder.When a small amount of molybdenum catalyst was used together with iron catalyst,compared with iron catalyst alone,the oil yield of hydrogenation reaction of coal increased by 3.53 percentage points,and the coal conversion rate increased by 4.22 percentage points.

关 键 词：有机钼催化剂 加氢性能 煤直接液化 一锅法 二硫化钼 分散性 油产率 转化率 

分 类 号：TQ529[化学工程—煤化学工程] TQ426