Thermodynamic of phase equilibria applied to the definition of the extraction and purification conditions of the N-aminopyrrolidine
type: Dataset
description: This global work is related to the synthesis, extraction and purification of a new exocyclic hydrazine with cosmetic applications, the N-aminopyrrolidine (NAPY). Firstable, the optimization of the synthesis conditions by the Raschig way are carried out by studying the influence of two parameters, the reagents’ molar ratio and the temperature, on the yield of the reaction. Due to the very low hydrazine content in the reaction liquors (≈5%w of NAPY), the extraction and purification of the useful product are often linked to successive demixing and distillation operations. The determination of these separation conditions requires then the knowledge of thermodynamics’ properties of the phase equilibria in these unitary steps. The optimization of the demixing needs then the study of the solid-liquid-liquid ternary solution NaOH/Pyrrolidine/Water. In this aim, three isothermal isobaric sections were studied, by combination of ATI (Isoplethic Thermal Analysis) and chemical analysis. The diameter and modulus method was developed in order to determine the composition of the critical point of the demixing curve. The distillation steps involve the liquid-vapor ternary system NAPY/Pyrrolidine/Water. The limit binary system Water/Pyrrolidine was determined by ebulliometry under atmospheric pressure. For a better understanding of the heteromolecular interactions in the liquid phase, two others liquid-vapor binary systems Water/Amine were obtained. The study of the ternary liquid-vapor system lad us to deduce two various distillation schemes. Once the synthesis and extraction conditions defined, a global process scheme was proposed, and NAPY was obtained in conformity with the cosmetical specifications
identifier: NNT: 2011LYO10016
issued: 2026-05-09T21:13:59.220137
language: fr
modified: 2026-05-09T21:13:59.220142
contact point: Organization
  fn: CCSD
keyword: amine
keyword: analyse-thermique-isoplethique
keyword: chimothechemical-sciencesother
keyword: ebulliometrie
keyword: ebulliometry
keyword: equilibre-entre-phases
keyword: hydrazine
keyword: infoeu-reposemanticsdoctoralthesis
keyword: isoplethic-thermal-analysis
keyword: n-aminopyrrolidine
keyword: phase-equilibria
keyword: pyrrolidine
keyword: raschig-way
keyword: synthese-raschig
keyword: theses
landing page: https://theses.hal.science/tel-00858111

Thermodynamic of phase equilibria applied to the definition of the extraction and purification conditions of the N-aminopyrrolidine
type: Distribution
format: HTML
issued: 2026-05-09T21:13:59.221767
modified: 2026-05-09T21:13:59.200548
access URL: https://theses.hal.science/tel-00858111

test_moissonnage_selune
type: Agent