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Conception d'un pilote de polycondensation et étude des procédés d'élaboration de polyamides en mileux fondu et dispersé

Abstract : The aim of this work is to develop a condensation polymerization process in dispersed medium allowing to obtain an intermediary polyamide in a divided form which morphology and chemical reactivity are controlled. This process shall ensure an outlet for polyamide 6,6 applications with high added value. For this purpose, it was necessary to design and install a multifunctional pilot of condensation polymerization allowing to carry out the condensation polymer syntheses in a molten state as well as in dispersed medium. The first part deals with the design, the realization and the qualification of the pilot. This one is completely automated and is composed by two reactors of three liters working at maxima temperature and pressure of 300 °C and 30 bars respectively and a heating system bringing the necessary thermal energy at each reactor. The use of this installation was validated by the transposition of various industrial condensation polymerization processes in molten state, in particular, the standard process of polyamide 6,6 synthesis. The second part presents the study and the development of the condensation polymerization process in dispersed medium. This one consists in dispersing the monomers solution (Nylon salt in ethylene glycol or in water) in a continuous phase (hydrocarbons solvent, Shellsol D100) in presence of surfactant, then in carrying out the condensation polymerization in the small droplets to obtain directly polyamide powders. Preliminary studies let to the obtaining of an under pressure process making it possible to product polymer powders with a DPn equal to 30 which appeared as regular spheres with smooth surface. The influence of the process conditions, in particular, stirring speed and surfactant concentration, on the Sauter?s diameter of the particles is investigated and modeled. In addition, a kinetic model of the postcondensation of these powders in dispersed medium is elaborated. It predicts correctly the end-groups concentrations and the number average molecular weight of the powders during the postcondensation
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Virginie Thieblemont. Conception d'un pilote de polycondensation et étude des procédés d'élaboration de polyamides en mileux fondu et dispersé. Autre. Institut National Polytechnique de Lorraine, 2005. Français. ⟨NNT : 2005INPL108N⟩. ⟨tel-01748748⟩



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