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Ionothermal synthesis and characterisation of Mn-, Co-, Fe- and Ni-containing aluminophosphates
Microporous and Mesoporous Materials ( IF 4.8 ) Pub Date : 2018-06-26 , DOI: 10.1016/j.micromeso.2018.06.045
Muhammad Mohsin Azim , Annegret Stark

Metalloaluminophosphates (MAPOs) containing different metal ions (Mn3+, Mn2+, Co2+, Fe2+ or Ni2+) were synthesised in ionic liquids to investigate the effect of changing ionic liquid structure, reaction time, the nature of metal ions, and the initial metal/Al as well as F/Al ratios. A combination of XRD, 13C CP MAS NMR, SEM images, Volhard titration, UV-Vis, thermogravimetric and nitrogen sorption measurements were performed to characterise the resulting MAPOs. The AFI framework of manganese-containing aluminophosphate (MnAPO) was prepared in an efficient way using MnF3 in 1-butyl-3-methylimidazolium bromide ([C4mim]Br) as both solvent and structure-directing agent (SDA). It was found that the resulting framework type can be altered by changing the ionic liquid's structure (cation, anion or alkyl chain) and this also influences the manganese content in the framework. Furthermore, tetramethylammonium fluoride ([Me4N]F) was employed as both mineraliser and co-SDA in the presences of [C4mim]Br for the formation of Mn-, Fe-, Co- and NiAPOs. The resulting framework type is dependent on the amounts of [Me4N]F and the nature of metal precursor, and as a result, the LTA, the SOD or a mixture of two framework types was obtained. The extent of substitution of metal atoms is directly dependent on the initial [Me4N]F/Al ratio, and metal cation (Fe2+ > Ni2+ > Co2+ > Mn2+) employed. The presented study leads to the first description for the ionothermal synthesis of MnAPO (CHA or LTA) and NiAPO (LTA), and offers efficient synthesis compared to previously reported ionothermal or hydrothermal methods.



中文翻译:

含锰,钴,铁和镍的铝磷酸盐的电热合成和表征

在离子液体中合成了包含不同金属离子(Mn 3+,Mn 2 +,Co 2 +,Fe 2+或Ni 2+)的金属铝磷酸盐(MAPOs),以研究改变离子液体结构,反应时间,分子性质的影响。金属离子,初始​​金属/铝以及F / Al比。结合XRD,13 C CP MAS NMR,SEM图像,Volhard滴定,UV-Vis,热重和氮吸附测量来表征所得的MAPO。使用MnF 3在1-丁基-3-甲基咪唑鎓溴化物([C 4mim] Br)作为溶剂和结构导向剂(SDA)。发现可以通过改变离子液体的结构(阳离子,阴离子或烷基链)来改变所得骨架的类型,这也影响了骨架中锰的含量。此外,在[C 4 mim] Br存在下,将氟化四甲基铵([Me 4 N] F)用作矿化剂和共SDA,以形成Mn-,Fe-,Co-和NiAPOs。所得骨架类型取决于[Me 4 N] F的量和金属前体的性质,结果,获得了LTA,SOD或两种骨架类型的混合物。金属原子的取代程度直接取决于初始的[Me 4 N] F / Al比和金属阳离子(Fe使用2+  > Ni 2+  > Co 2+  > Mn 2+)。提出的研究导致对MnAPO(CHA或LTA)和NiAPO(LTA)的电热合成的第一个描述,并且与以前报道的电热或水热方法相比,它提供了有效的合成方法。

更新日期:2018-06-26
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