Elsevier

Fluid Phase Equilibria

Volume 392, 25 April 2015, Pages 43-48
Fluid Phase Equilibria

Determination and correlation of liquid–liquid equilibrium data for the dichloromethane + water + N,N-dimethylacetamide + NaCl system

https://doi.org/10.1016/j.fluid.2015.02.022Get rights and content

Abstract

The (liquid + liquid) equilibrium (LLE) data for the quaternary system dichloromethane (DCM) + water + N,N-dimethylacetamide (DMAC) + NaCl have been determined at (298.15 and 308.15) K and atmospheric pressure. The experimental data were correlated by using Othmer–Tobias equation, and all the linear correlation coefficients were approximate to 1. Both NRTL and UNIQUAC models were adopted to correlate the LLE data, the model parameters were regressed by nonlinear least-squares method, then the LLE data of the quaternary system were calculated. The comparison between calculated and experimental data shows good agreement. The results show that the enlargement of two-phase region occurred with an increase of salt concentration in initial aqueous phase, and adding salt to the system is beneficial to increase the selectivity of solvent.

Introduction

In industrial applications, especially in the production of medical intermediates, the waste liquor is usually drained off with the different concentrations of DMAC and a small quantity of DCM. Direct emissions would cause significant pollution and loss of DMAC [1]. The study of efficiently separating and recovering DMAC from the waste liquor possesses an important significance on industry and environmentally sustainable development. At present, there is relatively little research on the liquid–liquid equilibrium (LLE) for the system containing salt. Ghalami-Choobar et al. [2] has studied the salt effect on the LLE of water + propionic acid + cyclohexanol system, the salt effect of methyl acetate + methanol + water system has been studied by Huang et al. [3], The LLE data for the quaternary system water + acetic acid + MTBE + NaCl have been determined by Zhang and Wang [4]. However, the research on the LLE data for quaternary system DCM + water + DMAC + NaCl has not been reported in the literature yet.

As a basic work, we have already determined the LLE data for the ternary system DCM + water + DMAC, the LLE data obtained are shown in Table 2 [5]. In order to investigate the salt effect on this system, we have determined the LLE data for the DCM + water + DMAC + NaCl system with different content of NaCl at 298.15 K and 308.15 K, respectively. The experimental data were correlated by using the NRTL and UNIQUAC models, the results indicated that the experimental data agreed well with the calculated LLE data, the above data and calculation methods are helpful for separating and recovering DMAC from waste liquor in industrial applications.

Section snippets

Materials and apparatus

All of the chemicals used in this work were analytical grade and without further purification. The gas chromatography was used in this work to check the purity of these substances. The source and mass fraction of the chemical reagent are given in Table 1.

The liquid–liquid equilibrium cell was made of glass by our group, the quaternary system was mixed with a magnetic stirrer (DF-101S type), and heated at a constant temperature in the water bath (uncertainty is ±0.1 °C.). The masses were

LLE experimental data

The LLE data for the DCM + water + DMAC + NaCl system were determined at 298.15 K and 308.15 K, respectively. Mass fractions of NaCl (xs) in the salt solutions were 0%, 2% and 5%, respectively. The experimental data were given with desalination as shown in Table 3, Table 4, the LLE data were very closed compared with Table 2 when mass fractions of NaCl (xs) in the salt solutions was 0% at 298.15 K and 308.15 K, respectively. The liquid–liquid equilibrium phase diagrams were drawn as illustrated in Fig. 2

Conclusions

In this paper, the LLE data and the quaternary phase diagrams for the system DCM + water + DMAC + NaCl have been obtained at (298.15 and 308.15) K and atmospheric pressure. The results show that it is obviously for the salt effect on this system with addition of NaCl. The two-phase region of ternary system is relatively smaller without addition of NaCl, the enlargement of two-phase region and the decrease of solubility of DMAC in aqueous phase and solubility of water in organic phase occurred with an

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