高比表面积氮化钼的合成技术及工艺条件研究  

STUDY ON THE SYNTHESIS OF MOLYBDENUM NITRIDE HAVING HIGH SPECIFIC SURFACE AREA

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作  者:王洪发[1] 郭瓦力[1] 吴剑华[1] 王欢[1] 

机构地区:[1]沈阳化工学院化学工程学院,沈阳110142

出  处:《石油炼制与化工》2007年第5期14-18,共5页Petroleum Processing and Petrochemicals

摘  要:采用溶胶-凝胶法制备负载型氮化钼的前驱体,采用流化床反应器、三级脱水、循环未反应氮化剂的流化氮化新工艺实现了氮化钼的批量合成。采用正交试验方法确定较优氮化条件为:空速70000h-1,氢氮体积比4,在375~550℃区间的升温速率1.2℃/min,氮化终温650℃,氮化钼前驱体MoO3的质量分数10%。采用BET,XRD,SEM等方法对制备的氮化钼及其前驱体进行表征,结果表明,采用溶胶-凝胶法制备的前驱体活性组分分散均匀,制备的氮化钼比表面积较大,当MoO3负载量(质量分数)超过15%后可以明显看到氮化钼的衍射峰。The precursor of supported molybdenum nitride was prepared by sol-gel method using a novel process involving fluidized bed reactor,three-stage dehydration and nitriding agent recycle to realize the batch scale synthesis of molybdenum nitride. The optimum nitridation conditions were obtained by the result of test designed with orthogonal method and showed as followed: a space velocity of 70 000 h^-1,a H2/N2 volume ratio of 4,a heating speed of 1. 2 ℃/min in the temperature range of 375 550 ℃,a nitriding temperature of 650 ℃ and a MoO3 content of 10%. The prepared molybdenum nitride and its precursor were characterized by techniques such as BET,XRD and SEM. Results showed that the active components dispersed homogeneously in said precursor,the obtained molybdenum nitride exhibited high specific surface area and crystalline peaks of γ-Mo2 N were found in XRD chart for samples having MoO3 content more than 15 %.

关 键 词:氮化钼 制备 氮化 溶胶-凝胶 比表面积 活性组分 

分 类 号:TQ426.6[化学工程]

 

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