Vapour-liquid equilibrium measurements at moderate pressures using a semi-automatic glass recirculating still.

M.Sc.Eng. University of KwaZulu-Natal, Durban 2014.Vapour-liquid equilibrium (VLE) data of high accuracy and reliability is essential in the development and optimization of separation and chemical processes. This study focuses on satisfying the growing demand for precise VLE data at low to moderate pressures, by development of a computer-aided dynamic glass still which is semi-automated. The modified dynamic glass still of Joseph et al. (2001) was employed to achieve precise measurement of phase equilibrium data for a pressure range of 0 to 500 kPa. The study involved the assembling and commissioning of a new moderate pressure dynamic still and various peripheral apparati. The digital measurement and control systems were developed in the object-oriented graphical programming language LabVIEW. The digital proportional controller with integral action developed by Eitelberg (2009) was adapted for the control of pressure and temperature. Pressure and temperature measurements were obtained by using a WIKA TXM pressure transducer and Pt-100 temperature sensor respectively. The calculated combined standard uncertainties in pressure measurements were ±0.005 kPa, ±0.013kPa and ±0.15kPa for the 0-10 kPa, 10-100 kPa and 100-500 kPa pressure ranges respectively. A combined standard uncertainty in temperature of ±0.02 K was calculated. The published data of Joseph et al., (2001) and Gmehling et al,. (1995) for the cyclohexane (1) and ethanol (2) system at 40kPa and 1-hexene (1) + N-methyl pyrrolidone-2 (NMP) (2) system at 363.15 K respectively served as test systems. NMP is regarded as one of the most commonly used solvents in the chemical industry due to its unique properties such as low volatility, thermal and chemical stability. As a result the isothermal measurement of 1-hexene (1) + N-methyl pyrrolidone-2 (NMP) (2) system were conducted at 373.15 K constituting new VLE data. A further system comprising 1-propanol (1) and 2-butanol (2) was also measured at an isothermal temperature of 393.15 K. The measured data were regressed using the combined and direct methods. The equations of state of Peng-Robinson (1976) and Soave-Redlich-Kwong (1972) combined with the mixing rules of Wong-Sandler (1992) in conjunction with a Gibbs excess energy model was utilized for the direct method. The activity coefficient models namely Wilson (1964) and NRTL (Renon and Prausnitz, 1968) were chosen to describe the liquid non-idealities while the vapour phase non-ideality was described with the virial equation of state with the Hayden and O’ Connell (1975) correlation. Thermodynamic consistency of the measured data was confirmed using the point test of Van Ness et al. (1973) and the direct test of Van Ness (1995)