TITLE:
A New Strategy for the Preparation of N-Aminopiperidine Using Hydroxylamine-O-Sulfonic Acid: Synthesis, Kinetic Modelling, Phase Equilibria, Extraction and Processes
AUTHORS:
E. Labarthe, A. J. Bougrine, Véronique Pasquet, H. Delalu
KEYWORDS:
Natural Asset; Financial Value; Neural Network
JOURNAL NAME:
Advances in Chemical Engineering and Science,
Vol.3 No.2,
April
29,
2013
ABSTRACT:
A new
strategy for the synthesis of N-aminopiperidine (NAPP) was developed using
hydroxylamine-O-sulfonic acid (HOSA). A systematic study of NAPP formation and
degradation reactions was carried out in diluted medium, in order to identify
products and to establish a kinetic modelling. Principal parameters have been
defined, in particular, that obtaining high yields (>90%) requires non
stoichiometric conditions. The extraction and purification processes were also
studied. NAPP isolation and piperidine recycling were optimized after the
establishment of the various solid-liquid-liquid and liquid-vapour implied
phase diagrams. At least, a calorimetric study of solvatation and reaction
enthalpies was undertaken in order to estimate reactor heating temperature in
the case of anhydrous synthesis. The combination of our kinetic, thermodynamic
and calorimetric data allows the establishment of two process schemes: one
using pure piperidine, the other, a 66 w% titrating azeotropic solution in
piperidine.