Regeneration of Raney®-Nickel Catalyst for the Synthesis of High-Value Amino-Ester Renewable Monomers

Aiming to synthesize high-value renewable monomers for the preparation of renewable specialty polyamides, we designed a new protocol. Amino-esters, produced via the hydrogenation of unsaturated nitrile-esters, are alternative monomers for the production of these polymers. A high monomer yield can be obtained using a Raney®-nickel catalyst despite the drawback of fast deactivation. The hydrogenation of 10-cyano-9-decenoate (UNE11) was tentatively reactivated by three different regeneration procedures: solvent wash, regeneration under hydrogen, and regeneration under sonication. Among these procedures, the in-pot catalyst regeneration (H2 30 bar, 150 °C) demonstrated complete activity recovery and full recycling.

Using a Silica Substrate to Monitor the Effectiveness of Radiocarbon Pretreatment

The objective of radiocarbon pretreatment is to eliminate any contaminant carbon from the sample material. Solvent washes and acid-base-acid (ABA) procedures are widely used for this purpose. However, quantitatively analyzing their effectiveness is surprisingly problematic, as it often requires large numbers of 14C measurements or high-precision compositional analysis. The technique presented here involves monitoring the impact of different forms of contamination by measuring their adherence to a non-carbonaceous substrate called Chromosorb®. Firstly, the substrate was used in place of a 14C sample in order to monitor the accrual of carbon contamination during a standard solvent wash and ABA pretreatment. This produced a contamination profile against which modifications to the pretreatment procedure could be compared. Secondly, stocks were prepared of Chromosorb that had been infused with environmental contaminants and with common glues, adhesives, and preservatives. By monitoring the elimination of carbon from these stocks, the effectiveness of different pretreatment procedures could be evaluated and the most problematic of the contaminants for 14C dating could be identified.