Thermodynamic of phase equilibria applied to the definition of the extraction and purification conditions of the N-aminopyrrolidine

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

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Source https://theses.hal.science/tel-00858111
Author Frangieh, Marie-Rose
Maintainer CCSD
Last Updated May 9, 2026, 21:13 (UTC)
Created May 9, 2026, 21:13 (UTC)
Identifier NNT: 2011LYO10016
Language fr
Rights https://about.hal.science/hal-authorisation-v1/
contributor Hydrazines et Procédés (HP) ; Université Claude Bernard Lyon 1 (UCBL) ; Université de Lyon-Université de Lyon-SNPE-Institut de Chimie - CNRS Chimie (INC-CNRS)-Centre National de la Recherche Scientifique (CNRS)
creator Frangieh, Marie-Rose
date 2011-01-21T00:00:00
harvest_object_id a9267972-b6aa-4d66-80fb-45a2637675bb
harvest_source_id 3374d638-d20b-4672-ba96-a23232d55657
harvest_source_title test moissonnage SELUNE
metadata_modified 2026-03-31T00:00:00
set_spec type:THESE