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表面活性剂改性Mo-Ni-NH3/γ-Al2O3催化剂的分散性及孔结构的表征 被引量:3

Characterization of Dispersity and Pore Structure of Surfactants-modified Mo-Ni-NH_3/γ-Al_2O_3 Catalysts
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摘要 采用纳米自组装方法以钼镍铵溶液作为浸渍液制备贯穿性介孔Mo-Ni-NH3/γ-Al2O3催化剂。利用BET比表面积测试法(BET)、CO吸附原位红外、X射线衍射(XRD)、透射电子显微镜(TEM)等表征手段,考察了表面活性剂、助溶剂种类、用量在自组装过程中对催化剂的分散性及孔结构的影响。结果表明,改性后催化剂TOP-3的孔性质最好,其比表面积为183 m^2·g^-1,孔容为0.46 m^3·g^-1,平均孔径为10.11 nm,且孔道在10-30 nm处高度集中,高达35.63%;红外CO原位吸附结果证明了Mo^2+,Mo^4+和Ni^2+活性中心的存在,且均以线式吸附态吸附CO;从XRD分析可发现催化剂NOP-3、NOP-4在2θ=15.9°,20.8°,22.2°和30.8°处出现了Al2(Mo O4)3的(111),(102),(021),(312)4个晶面的特征衍射峰,而TOP系列催化剂的特征峰弥散,说明TEA与OP-20复配可以改善金属的分散性。TEM表征结果证明了15-20 nm贯穿性多孔结构的存在,且分散均匀。此结构有利于大分子扩散,适合于重油加氢处理。 Using Mo-Ni-NH3 as impregnation solution,the penetrating mesoporous Mo-Ni-NH3/ γ-Al2O3 catalyst was prepared by nano self-assembly technique.The influence of dosage of different surfactants such as CTAB,OP-20,TW-80,OP-10,assistantagentia TEA and NS on dispersity and pore structure of catalyst in the process of self-assembly was investigated by BET,insitu FTIR of adsorbed CO,XRD and TEM.The results showed that the modified catalyst TOP-3was better than the others,which has a specific surface area of 183 m^2·g^-1,a pore volume of 0.46m^3·g^-1and an average pore size of 10.11 nm,and its pore distribution of 10 nm-30 nm was greatly concentrated,and reached up to 35.63%.The adsorption of active site of Mo^2 +,Mo^4 +and Ni^2 +was at the presence of linear adsorption state which could be proved by the in-situ FTIR of adsorbed CO.There were four characteristic crystal plane diffraction peaks of(111),(102),(021) and(312) for Al2(Mo O4)3at 15.9°,20.8°,22.2° and 30.8° by the XRD analysis for NOP-3 and NOP-4.While the fact that the characteristic peaks of TOP catalysts were dispersive showed that the composites of TEA and OP-20 improved the dispersity obviously.The penetrating mesoporous structures in uniform dispersion between 15 nm and 20 nm could be obtained by TEM images.The structure features were beneficial to residue hydrotreating.
出处 《分析测试学报》 CAS CSCD 北大核心 2016年第4期388-393,共6页 Journal of Instrumental Analysis
基金 中国石油化工集团资助项目(总合-JQ1416) 中国海洋石油总公司资助项目(20140331)
关键词 表面活性剂 介孔催化剂 自组装 孔结构 表征 surfactant mesoporous catalyst self-assembly pore structure characterization
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