Hello everyone,
In my current university inorganic lab, I am trying to follow the below synthesis of magnetic ionic liquids for a special project:
Paper:
http://pubs.rsc.org/en/content/articlepdf/2011/cc/c0cc03892j?page=searchSupporting information (including synthesis of compounds):
http://www.rsc.org/suppdata/cc/c0/c0cc03892j/c0cc03892j.pdf I've been able to successfully synthesize the three Na[M(EDTA)] (M=Fe
3+, Cr
3+, Co
3+) complexes, however I've run into a problem when attempting to combine them with the counter ion 1-Ethyl-3-methylimidazolium bromide ([EMIM]Br) to create [EMIM][M(EDTA)] and NaBr (which is lost in the ethanol/water solvent, while the desired is water insoluble).
For the experiment, I dissolve the [EMIM]Br in ethanol (~15 mL) and the Na[M(EDTA)] in water (~20 mL) and add the solutions together followed by a 24 hour stir. Both solutions are miscible and there is no precipitate. However, after 24 hours it appears the Na[M(EDTA)] starting material precipitates out, and rotovaping the remaining colored liquid yields none of the desired product. The pH of the solution is ~7 before and after the stir.
My professor and I are at a loss as to why no product is forming, as we see the reaction as being a non-time sensitive, simple ion exchange reaction. Might anyone be able to shed any light as to what may be happening and any ways to change it? I've thought of trying a different solvent system, but I'm nut sure if it would help. Thanks for you replies!