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MOCVD法制备Ru/HSAG氨合成催化剂
浙江工业大学化学工程学院,浙江 杭州 310032
Preparation of Ru/HSAG Catalysts for Ammonia Synthesis via Metal-Organic Chemical Vapour Deposition Technology
College of Chemical Engineering, Zhejiang University of Technology , Hangzhou 310032, China
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摘要 采用金属有机物化学气相沉积技术(MOCVD)将羰基钌升华至已浸渍KNO3和Ba(NO3)2的高比表面石墨(HSAG)上,制备了一系列Ru/HSAG催化剂。采用X射线衍射、透射电镜(TEM)和N2物理吸附等表征手段,考察了催化剂的物相和表面结构性质及氨合成催化活性。结果表明,以化学气相沉积技术制备的催化剂,能使钌均匀地分散于载体中,形成较小的钌粒子,从而得到高活性的氨合成催化剂。羰基钌的加热温度对升华速率有很大影响,但对沉积效果和催化活性没有明显影响,负载的羰基钌含量对催化剂活性有显著影响。羰基钌在130 ℃开始分解,并在175 ℃达到最大分解速率,因此合适的升华温度为110~130 ℃。催化剂的钌负载量(质量分数)从3.2%增至6.0%时,低反应温度(375 ℃)下,氨合成活性明显提高。在实验负载量范围内,TEM显示钌纳米粒子的粒径变化不大,基本保持在2 nm左右。
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严海宇
黄仕良
韩文锋
刘化章
关键词 氨合成化学气相沉积羰基钌高比表面石墨    
Abstract:Ruthenium catalysts supported on high surface area graphite (HSAG), impregnated with KNO3 and Ba(NO3)2,was prepared via metal-organic chemical vapour deposition technology (MOCVD) with tri-ruthenium dodecacarbonyl as the Ru precursor. The catalysts were characterized by X-ray diffraction, N2 physical adsorption and transmission electron microscope. The activity of the Ru catalyst for ammonia synthesis was evaluated. The results showed that the sublimation rate of tri-ruthenium dodecacarbony depends on temperature under vacuum and dark conditions. It is confirmed that uniform dispersion can be achieved via MOCVD route with Ru nanoparticle sizes around 2 nm. As Ru3(CO)12 commences to decompose at 130 ℃ and reach maximum decomposition rate at 175 ℃, the sublimation temperature is suggested to be 110—130 ℃. With the increase in Ru loading from 3.2% to 6.0%, as evidenced by TEM experiments, Ru nanoparticle size keeps unchanged (around 2 nm), while the activity for ammonia synthesis is enhanced dramatically, especially at low temperature (375 ℃).
Key wordsammonia synthesis    chemical vapour deposition    tri-ruthenium dodecacarbonyl    high surface area graphite   
收稿日期: 2014-03-13     
作者简介: 严海宇(1989—),男,硕士研究生;刘化章(1940—),男,教授,通讯联系人。E-mail:cuihua@zjut.edu.cn。
引用本文:   
严海宇,黄仕良,韩文锋等. MOCVD法制备Ru/HSAG氨合成催化剂[J]. 化学反应工程与工艺, 2014, 30(5): 446-451.
Yan Haiyu,Huang Shiliang,Han Wenfeng et al. Preparation of Ru/HSAG Catalysts for Ammonia Synthesis via Metal-Organic Chemical Vapour Deposition Technology[J]. 化学反应工程与工艺, 2014, 30(5): 446-451.
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