Evaluation of Sponge Metal Catalysts in a Trickle Bed Reactor for the Continuous Hydrogenation of an Aliphatic Nitro Intermediate

Nine sponge nickel catalysts were assessed for the reduction of an aliphatic nitro group in a trickle bed reactor. Focused beam reflectance measurement (FBRM) was used to assess the mechanical strength and particle size distribution of the catalysts. The continuous reduction of ( S )-7-methyl-7-(nitromethyl)-1,4-dioxaspiro[4.5]decane was investigated using a Raney nickel catalyst in a fixed bed reactor. The use of a Luna ODiSl temperature probe and an FLIR thermal imaging camera were investigated to monitor the catalyst performance while the process was run. A 1.12 kg sample of the aliphatic nitro compound was reduced to the corresponding amine using a single 20 mL reactor containing 43 g of 3111A Raney nickel over a period of 17 h.