United States Environmental Protection Agency Air and Energy Engineering Research Laboratory Research Triangle Park NC 27711 Research and Development EPA/600/S7-87/004 May 1987 &EPA Project Summary Vapor/Liquid Equilibria of Constituents from Coal Gasification in Refrigerated Methanol Te Chang, R. M. Rousseau, and J. K. Ferrell A thermodynamic framework was es- tablished for developing a model of the phase equilibria of mixtures of meth- anol and the major constituents found in gases produced from coal. Two ap- proaches were used to model the equi- librium behavior: (1) an equation of state was used to describe both gas and liquid phases, and (2) an equation of state was used to describe the gas, while a solution model involving activ- ity coefficients was used to describe the liquid. The approach chosen for each species was based on the component volatility. An experimental apparatus was constructed to obtain data against which the model predictions could be tested. The apparatus was evaluated by comparison of experimental P-T-x data on mixtures of carbon dioxide (CO2) and methanol with those from the liter- ature. The comparison was favorable. P-T-x-y data on mixtures of CO2, methanol, and water, and mixtures of COfe nitrogen, and methanol at temper- atures in a range of -30 to 25°C and pressures up to 54 atm (5472 kP) were obtained. Comparisons of the calcu- lated and measured values of bubble point pressures and/or liquid composi- tions of the dissolved gases were satis- factory. This Project Summary was devel- opad by EPA's Air tnd Energy engineer- ing Research Laboratory. Research Tri- angle Park, NC, to announce key findings of the research project that Is nimy documented In a separata report of the same title (see Project Report ordering Information at back). Introduction The objective of this effort was to de- velop a thermodynamic framework that could be used to describe the equi- librium behavior of methanol with com- pounds found in the gas produced from coal. The approach that was taken di- vided the constituents into three groups: Group I consisted of supercriti- cal components. Group II consisted of compounds that are normally gases at the conditions of interest, and Group III contained compounds that are liquids at the conditions of interest. This divi- sion was used to select either an equa- tion of state or an activity coefficient for- mulation of the equilibrium criteria. Once this selection was made, appropri- ate parameters in the formulation were evaluated from binary data obtained from the literature and experiments that were part of this study. With the pa- rameters evaluated in this way, it is pos- sible to predict the behavior of systems containing any number of the compo- nents from Group I, II, and/or III. Accomplishments/Results A vapor/liquid equilibrium (VLE) ap- paratus was developed along with a sampling technique and analytical method to obtain equilibrium data on systems having high gas solubilities. Good data were obtained from this ap- paratus for C02 solubilities in methanol with and without an inert gas (nitrogen), and in mixtures of methanol and water. However, low solubilities of nitrogen in methanol cannot be measured accu- rately. ------- Bubble point pressure variance pro- vided a useful objective function in the parameter search procedure for both equation-of-state and activity coeffi- cient methods. This search procedure, which includes a bubble point pressure calculation, does not require measure- ment of vapor-phase composition. Mathias' polar correction factor im- proved the calculation of vapor pres- sures with the Soave-Redlich-Kwong (SRK) equation of state for polar com- pounds of methanol and water, but this factor may not be necessary for ethyl mercaptan and dimethyl sulfide. Temperature-dependent binary interaction parameters in the extended SRK equation of state have greatly im- proved the accuracy of correlations of methanol-containing binary VLE sys- tems consisting of constituents from coal gasification. Temperature- independent binary interaction parame- ters are satisfactory for gas/gas mix- tures. These parameters are applicable in a broad range of temperatures. Phase equilibrium calculations using the extended SRK equation of state were satisfactory for mixtures of meth- anol/gas systems as long as the gas component had a mole fraction in the liquid less than 0.6. They did not pro- vide satisfactory predictions for those systems at high gas concentrations in the liquid phase. However, absorption- stripping processes that condition syn- thetic gas mixtures operate at liquid cir- culation rates that maintain the levels of dissolved gases below those at which the equation of state loses its accuracy. The extended SRK equation of state tends to predict false liquid/liquid/gas (LLG) three-phase equilibria in metha- nol/light-hydrocarbon and methanol/ acid-gas systems. This is believed to be caused by the quadratic mixing rules for interaction parameters. The use of the optimized parameter sets enables the equation of state to predict the behavior of a methanol- containing multicomponent system; comparisons between experimental data and bubble point pressure calcula- tions for methanol/H2/N2, methanol/CO/ N2, and methanol/CO2/H2O mixtures were good. A simple gas solubility calculation using the extended SRK equation of state was effective in calculating mixed- gas solubilities in a pure solvent and pure-gas solubilities in a mixed solvent. The activity coefficient models using the four-suffix Margules, Wilson, and UNIQUAC equation are excellent for bi- nary systems that contain condensable components (those from Groups II and III). They are especially useful in de- scribing the vapor/liquid equilibrium behavior of systems containing volatile liquids; e.g., methanol, mercaptans, and sulfides. The determined parame- ters in these models may be used to describe the multi-component system without further adjustment, but there is no guarantee for describing the behav- ior of a system containing a supercriti- cal component. The Wilson and UNIQUAC equations are superior to the four-suffix Margules equation for most of the systems stud- ied. The former two equations have a good built-in temperature-dependent relationship and do not predict false phase separations for methanol/acid- gas and methanol/light-hydrocarbon systems. Recently developed equations of state—which include density depend- ent mixing rules based on the two-fluid, local composition theories—should be useful in future applications describing the vapor/liquid equilibrium behavior of systems having components covering a broad range of densities or with polar or hydrogen-bonding components. Coal- produced gas that is conditioned with a physical solvent is an example of such a system. T. Chang, R. Rousseau, and J. Ferrell are with North Carolina State University, Department of Chemical Engineering, Raleigh. NC 27695, N. Dean Smith is the EPA Project Officer (see below). The complete report, entitled "Vapor/Liquid Equilibria of Constituents from Coal Gasification in Refrigerated Methanol," (Order No. PB 87-165 627/AS; Cost: $ 18.95, subject to change) will be available only from: National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 Telephone: 703-487-4650 The EPA Project Officer can be contacted at: Air and Energy Engineering Research Laboratory U.S. Environmental Protection Agency Research Triangle Park, NC 27711 United States Environmental Protection Agency Center for Environmental Research Information Cincinnati OH 45268 Official Business Penalty for Private Use $300 EPA/600/S7-87/004 0000329 PS * CHICAGO ------- |