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.

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     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

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