Aniline → Phenazine

Participants

Reaction Steps

To the dried material, 350 ml of deionized water was added, mixed vigorously and filtered through a Buchner funnel. The top layer was a shiny white layer of solid material. The bottom portion, primarily ZSM-5 appeared to be dull white in color. The top layer—about 8 gms, was treated further with addition of about 30.5 gms of 25% aqueous TMA(OH) and 300 ml of deionized water. The loading was done for four hours at about 45° C. The resulting slurry was filtered and then dried in a vacuum desiccator for twenty four hours at 42° C. The dried material showed two layers of solid. The material, although it was not hard and therefore easier to grind failed the coupling reaction test which consisted of reacting aniline and nitrobenzene in that it produced significant amounts of phenazine. It is estimated that the material used in the coupling reaction test had a TMA(OH) content of about 33 wt. %. It is apparent that TMA(OH) loading at such a high level causes the ZSM-5 crystal structure to collapse.

Provenance & Evidence