A new strategy for the development of monomethylhydrazine (MMH) using the Raschig process is discussed in this publication. The determination of optimal conditions for the synthesis of MMH required the development of ...A new strategy for the development of monomethylhydrazine (MMH) using the Raschig process is discussed in this publication. The determination of optimal conditions for the synthesis of MMH required the development of a kinetic model. In order to validate the results of the calculation, a device for synthesis under pressure (13 bar) by direct injection of the stoichiometric monochloramine, synthesized using microreactor technology, into monomethylamine (MMA) was developed. The experimental data, in accordance with the theoretical results of the kinetic model, make it possible to establish a new process for the synthesis of monomethylhydrazine.展开更多
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, ...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.展开更多
文摘A new strategy for the development of monomethylhydrazine (MMH) using the Raschig process is discussed in this publication. The determination of optimal conditions for the synthesis of MMH required the development of a kinetic model. In order to validate the results of the calculation, a device for synthesis under pressure (13 bar) by direct injection of the stoichiometric monochloramine, synthesized using microreactor technology, into monomethylamine (MMA) was developed. The experimental data, in accordance with the theoretical results of the kinetic model, make it possible to establish a new process for the synthesis of monomethylhydrazine.
文摘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.
