Determination of the operating parameters of an evaporator crystallizer

Abstract

This work involves the study of the solid/liquid equilibrium in the NaCl–NaOH–H2O ternary system. The aim is to optimize the operating conditions of an evaporator–crystallizer used in a hydrazine extraction process. The latter is conducted at industrial scale using the Raschig method, a general method for preparing hydrazines for aerospace and pharmaceutical applications. The extraction process includes the use of a Kestner type evaporator–crystallizer to first isolate hydrazine and water by evaporation and then separate two salts: sodium hydroxide, recovered as an aqueous solution, and sodium chloride which crystallizes. However, problems related to the co-precipitation of NaCl–NaOH may be encountered in industry, leading to the clogging of installations. Therefore, it is necessary to ensure that only NaCl crystallizes while maintaining NaOH in liquid state. Knowledge of the equilibrium phases of the NaCl–NaOH–H2O ternary system is thus required, particularly the liquid/solid phase. Phase equilibrium experiments were performed by isoplethic thermal analysis (ITA) and chemical titrations over the temperature range of 313 to 353 K at atmospheric pressure. ITA is an isobaric and isothermal method developed in our laboratory and based on the measurement of the thermal effects associated with transformations in a system (appearance or disappearance of a phase) when its composition is changed. The NaCl crystallization domain was fully determined and the operating parameters of the device were defined precisely as a function of temperature and composition of the Kestner loop.