A COMPUTER MODEL OF THE RECTISOL PROCESS USING THE ASPEN SIMULATOR

by Rosalyn A. preston

SUBMITTED IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF MASTER OF SCIENCE IN

CHEMICAL ENGINEERING

at the

MASSACHUSETTS INSTITUTE OF TECHNOLOGY

December, 1981

Q

Massachusetts Institute of Technology 1981

Signature of Author Signature of Author Certified by

Department of Chemical Engineering
December 7, 1981

Lawrence B. Evans Thesis Supervisor Accepted by Glenn C Williams Chairman, Departmental Graduate Committee
MASSACHUSETTS INSTiTUTE OF TECHMflLOGY JUN 1 13982

Archives

i IRRA!ES

A COMPUTER MODEL OF THE RECTISOL PROCESS USING THE ASPEN SIMULATOR

by

Rosalyn A. Preston

Submitted to the Department of Chemical Engineering on December 7, 1981 in partial fulfillment of the requirements for the Degree of Master of Science in Chemical Engineering

ABSTRACT

A computer model of the Rectisol process for acid gas absorption has been developed with the ASPEN process simulator. The model uses a modified version of the Redlich-Kwong-Soave equation-of-state to represent the phase equilibria for the methanolwater-aromatics-acid gas system. This report describes the development of the physical properties model and the flowsheet simulation. The work is based on the CONOCO design for a commercial scale coal gasification facility. The computer modelling effort was carried out under contract to the Morgantown Energy Technical Center, U. S. Department of

Energy.

TABLE OF CONTENTS
ACKNOWLEDGEMENTS I. II. INTRODUCTION AC:ID GAS

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . PROCESSES . . . . . . .

ABSORPTION

.6
. .

vii

. .

General Features of Acid Gas Absorption
Processes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Absorption Regeneration Solvent Heat

. a.
·
a1

6
·
a

·
a

6

7

a

a
a

a a

Selection

. . . . . . . . . . . . . . . . . . . . . . . . . .a

*

7 9
10

Integration Recovery

*

a

a

Solvent

. . .
. a
* a
a

12
12 13 19

Advantages of the Rectisol Process . . .
Rectisol Process Description . . . . . .

a a a

III. DEVELOPMENT OF PHYSICAL PROPERTIES MODEL

..

.

Selection of the Thermodynamic Model . . a . .

19 21 23

Modified Redlich-Kwong-Soave Equation-of-State
Experimental Phase Equilibrium Data . . . . .

Development of Modified Redlich-Kwong-Soave
Model Parameters . . . . . . . . . . . . . . .

25

Evaluation of the Preliminary Thermodynamic
Model Enthalpy IV. SIMULATION Basis OF for . . . . . . . . Calculations THE the RECTISOL Process Section .. . . .. . .. . . .

27 32 36 36

. . . . . . . . . . . . . . . . . . . . . . . . .

PROCESS Simulation

Absorption Flash Naphtha

. . . . . . . . . . . . Section . . . . . . . .

38
43 43

Regeneration Extractor

. . . . .

. ... . .

Azeotrope Column .... . .
Methanol-Water Column

a .

a
. . .

.a
.

44
49

. . . . .

iii

Hot Regeneration Column
Water Heat Wash Column . . . . . . .

. .
..

*

O

.

.

.

.

·

50 52 52

.... VI. ........ ... CONCLUSION.
a 0
0

·

a

a

a

Exchangers

.

. . . . .

Methanol

Make-up

.

53
e ·

a
·

* a a
·

a a

a a
·

a a

a

Flowsheet

Convergence

53 55
a

V. RECTISOL PROCESS SIMULATION RESULTS

U

a

a

a

a

a

59

APPENDIX A APPENDIX B
APPENDIX APPENDIX C D

OVERALL RECTISOL MODEL ABSORPTION SECTION SIM [LATION
AZEOTROPE COLUMN SIMUIL MTION COLUMN SIMULATION

METHANOL-WATER

APPENDIX E

HOT REGENERATION COLUMI [

SIMULATION

APPENDIX F

WATER WASH COLUMN SIMU LATION

LITERATURE CITED
BIBLI OGRAPHY

iv

Comparison of Equilibrium Loading of Chemical and Physical Solvents . . . . . The Rectisol Process . . . . . . 14 15 16 30 Block Flow Diagram of the Rectisol Computer Model Effect of Solvent Rate and Number of Trays on Carbon Dioxide Absorption . Ternary Diagram for Methanol-Benzene-Water . .. . . . . . . . . 6. .LIST OF FIGURES 1. Process Flow Diagram of the Rectisol Process . 11. . . Process Flow Diagram of the Rectisol Process . 7. 11 Block Flow Diagram of the Rectisol Process . . . . . 9. . . . . . . . . . . . . . McCabe-Thiele Plot for Azeotrope Column .. 45 48 v . . . . . . The Pipeline Gas Demonstration Plant . . . . Henry's Law Constants for Nitrogen in a Methanol and Carbon Dioxide Mixture . .. . . . . . . . . . . . . 4. 2 4 3. . 5. . . 8. . 39 42 10. 2. .

. .. 33 34 . o . Experimental Data for Methanol-Hydrogen SulfideBinary Interaction Redlich-Kwong-Soave 2. . 4. . . 5. . . . . ... . Cooling and Heating Duties for the Rectisol Process .LIST OF TABLES 1. Regenerated Composition 7. .. . . . . . Comparison of Modified RKS Model Predictions with Carbon DioxideNitrogen ... 6. .. . . . .. 3. . . . . . . ... . . . . Parameters for the Modified Equation-of-State Composition of Feed Gas to Rectisol Process Desulfurized Acid Gas Gas Composition Methanol Composition . 58 vi ... . 37 56 56 56 . .

forhis guidance and optimism throughout. to Joe Boston and Paul Mathias for their help with modelling the physical properties. vii .ACKNOWLEDGMENTS I would like to express my appreciation to all the ASPEN staff who gave me help and support on this project. Evans. Professor L. and to Willie Chan and Fred Ziegler for their debugging efforts. especially to Herb Britt and Chau-Chyun Chen for assisting me in almost every aspect. B. I would also like to thank my advisor.

Carbon dioxide produced in the shift reaction must then be washed out with hot carbonate solution to improve the BTU quality of the substitute natural gas. Briefly. generated by cryogenic air separation. are allowed to undergo water-gas shift and methanation reactions simultaneously. 1970. Here. The computer modelling effort took CONOCO's design for a commercial scale coal gasification facility as the basis (CONOCO. shown schematically in Figure 1. the gases from the gas and recovered. final gas treatment involves compression and drying. This simulation was pre- pared as part of a program to transfer ASPEN technology to the Morgantown Energy Technology Center (METC) of the United States Department of Energy. is designed to generate pipeline quality substitute natural gas from coal. Crude synthesis gas is re- covered from the top of the gasifier. light oils and sulfur compounds are removed Following purification. The overall program involved develop- ment of computer models for the major process units in the CONOCO Slagging Lurgi Coal Gasification process. This facility. while the ash is withdrawn in a molten slag form from the bottom. 1 The . Scholz. ification takes place at high pressure in a moving bed slagging gasifier using Lurgi technology. 1969) using the ASPEN process simulator. the process gasifies coal with steam The gas- and oxygen.I. 1980). The synthesis gas is subsequently directed to the Rectisol unit for purification. INTRODUCTION The objective of this work was to develop a computer model of the Rectisol process (Hochgesand.

w 2 cl Cd 0 Cd ro ad4 ordH c-) a) E a) for 3dd 0 E o0 C E E Cd 0 o a.H W 0 o xEC p 0 Cd 0 0\ TO 0 0 :z. co 0o a) CD a. . a) a) fAt o o . 0 e.P t= C a) .

a flexible tool which may be applied in future design and sensitivity studies and in trouble-shooting after process startup. development of the computer model entailed a . the model predicts the composition of the outlet streams for a given set of operating conditions. Therefore. The process is comprised of an absorption section followed by a series of regeneration processes in which the rich solvent is purified and the absorbed compounds recovered. The Rectisol computer model described in this report provides a stream-by-stream heat and material balance for the process. Since Rectisol is a proprietary process licensed by Lurgi Mineraloltechnik GmbH. In addition. the model can be used to assess the effect of various process variables on the composition of the desulfurized gas and acid gas products. distillation Separate models of the absorbers and columns yield a rigorous tray-to-tray analysis Overall. the CONOCO design did not provide any information on the actual process operating conditions. the Rectisol simulation represents of each column.3 The Rectisol process itself features refrigerated methanol as the solvent into which the acid gases in the synthesis gas are absorbed. For this reason. The model also predicts the purity of the regenerated methanol solvent for specific regeneration operating conditions. The input to the simulation is based on the process flowsheet and feed streams from the CONOCO commercial design. The diagram in Figure 2 illustrates the particular Rectisol design proposed for the CONOCO coal gasification facility.

4 .H 34 d i a) o Z ) 0 D ts M *H ~o o oo F ¢ C: O0 z E0 U2 U) W o 0 0 Ho PE-4 a) .H U2 a4 &4 0V m E o : X E-1 Z0 .

it was necessary to perform sensitivity studies on the design variables in order to establish suitable operating conditions. The actual computer model- ling work required testing of several ASPEN models which were still in the development stage. . It was orig- inally intended to use the final Rectisol model to examine the sensitivity of the process to various design variables.5 fair amount of design work to establish reasonable process operating conditions. The following chapters describe the development of the Rectisol model. lack of computer funds curtailed the project once the model was developed. However. Subsequently. The work initially involved a literature search to locate published process data regarding Rectisol. considerable effort was devoted to developing a good thermodynamic model of the system to provide adequate physical properties predictions. Further.

Removal prior to shift conversion of the carbon monoxide and water to hydrogen and carbon dioxide favors the equilibrium hydrogen concentration. is important for many industrial plants producing a gaseous intermediate or final product. hydrogen is generated together with a substantial quantity of carbon dioxide. In the production of substitute natural gas by coal gasification.6 II. on the other hand. Rectisol is just one example of the many acid gas absorption processes. Since carbon dioxide has no heating value. General Features of Acid Gas Absorption Processes Removal of acid gases. The separation may occur at several points in the process. However. and a regeneration section where the acid gases . further treating to remove carbon dioxide may be required. All sulfur bearing compounds. In addition. these processes feature an ab- sorption section in which the acid gases are absorbed into a liquid solvent. primarily carbon dioxide and hydrogen sulfide. since carbon dioxide is pro- duced in this reaction. must be removed before methanation to avoid poisoning the methanation catalyst. In general. the discussion serves to present the basic design variables which must be considered in designing a process to remove acid gases. it must be separated out of the final pipeline gas to raise the overall BTU value. ACID GAS ABSORPTION PROCESSES This section discusses the general features of acid gas absorption processes in order to provide some background for the detailed description of the Rectisol process.

which requires less height. The details of each section are discussed below. Thus. a packed column design.7 are recovered to yield a lean solvent of sufficient purity for recycle. Plate columns generally operate at lower efficiency. The gas stream is contacted with the solvent in an absorber column where it flows counter-current to the downflowing liquid. In addition. Absorption Acid gases are removed from the sour gas by absorption into a liquid solvent. A recycled sol- vent of higher purity will absorb a greater quantity of gas per pass. 1979). and to reduce the gas concentration in the solvent to a low level prior to its recycle to the absorber. may be preferable when a large concentration of acid gas is to be absorbed (Kohl and Riesenfeld. the processes usually include a final wash to recover solvent carried over with the acid gas stream. Regeneration The solvent regeneration section serves two functions: namely. However. thereby reducing the solvent recirculation rate. the fact that the absorption rate increases with an increase in temperature justifies operating some absorption processes at elevated temperature. to recover the absorbed acid gases from the solvent. highlighting the major factors affecting each section. such . Most absorbers operate at low temperature where equilibrium favors absorption. The tradeoff must therefore be considered between regeneration costs andthe costs associated with a higher recycle rate. The column itself may contain pack- ing or trays. as dictated by the economics of the specific design.

the purity of the treated gas is limited by the degree of regeneration. a vacuum flash may be employed to remove the dissolved gases further. heat is required to raise the system to the solvent boiling point. If flash desorption is not adequate. As such. However. Although some of this heat may be obtained through heat exchange of the hot overhead gases and hot regenerated solvent . This heat is frequently supplied in the form of steam through the stripper reboiler. The choice is determined by the nature of the solvent and the desired purity. 1970). Flash desorption represents the cheapest method where the pressure of the solvent is let down in several stages. to supply the heat of desorption and further to supply the heat of vaporization for the solvent vapors. In this case. There are three primary methods of regeneration. the gases may be stripped from the solvent following a single flash. Gas solubility tends to decrease with increased temperature. The gas will approach equilibrium with the fresh- ly regenerated solvent which it contacts in the final stage of the absorber (Hochgesand. Further. This effect is augmented by heating the solvent to its boiling point so that solvent vapors provide some stripping action.8 as larger equipment and higher pumping requirements. the regeneration step can be a sig- nificant energy consumer. The final stage is usually atmospheric. Heat must be sup- plied to the stripper to provide the heat of desorption and to vaporize the stripping medium (often steam). Hot regeneration provides the most complete regeneration and consequently leads to the highest purity for the feed gas.

1972). good heat transfer properties and low heat capacity to minimize heating requirements. into the liquid phase. stability. The solvent should also have low volatility to prevent excessive solvent losses in the gas stream by vaporization. Chemical and physical solvents have . heat exchanger losses make external heating necessary (Hochgesand. the absorption process must be rever- sible so that the solvent will release the gas components with relative ease to yield both gas and solvent of high purity. The absorption process involves transfer of the acid gases from the gas phase. The acid gas components may be absorbed into the solvent by physically dissolving or by reacting chemically with an active solvent component. 1970). In the case of a chemical solvent. the solvent must have a high sol- vency for the acid gas constituents at reasonable operating conditions. through the gas-liquid interface. Foremost. It is highly undesirable for the solvent to form an irreversible compound with any of the feed gas constituents since this may lead to appreciable solvent losses. Despite the varied chemical nature of these solvents. the absorbed gases then react reversibly to form compounds. Other desirable character- istics include low viscosity for minimal pumping costs. In addition. and low corrosivity. Solvent Selection A variety of solvents are employed to absorb acid gases. all should exhibit certain characteristics to render them suitable as solvents. Finally. low cost and availability are obviously desirable (Nonhebel.9 with the incoming solvent.

As a result.10 several distinguishing characteristics which account for the different absorption mechanisms. The same behaviour dictates the method of Physical solvents are easily regenerated by flash desorption. provided Henry's Law applies. As the diagram in Figure 3 shows. a saturated chemical solvent subjected to a pressure reduction will release only a fraction of the total absorbed gas. and physical solvents the choice for purifying high pressure concentrated streams. This distinction makes chemical solvents the best choice for purifying gas streams at low gas partial pressures. thereby raising the overall absorption rate (Kohl. regeneration. chemical reactions increase the liquid film coefficient. In a chemical absorption system. Some form of reboiling is required to effect adequate regeneration (Hochgesand. 1970). the loading of a chemical solvent rises rapidly at low gas partial pressure. However. Since chemical absorption is more rapid than physical absorption. but then reaches a point of saturation beyond which little absorption occurs. Riesenfeld. most acid gas absorption Often the rich solvent processes are highly heat integrated. the equilibrium loading of a physical solvent increases in direct proportion to partial pressure. chemical systems require fewer trays and thus smaller towers. may be preheated and the lean solvent cooled by heat exchange. The absorption process is exothermic so that the solvent . 1970). In contrast. although stripping or hot regeneration may be used for greater purity. Heat Integration Solvent regeneration usually takes place at higher temperature than absorption.

(NT.TVTAT. 1970 .'T/1XTr1Z' Figure Chemical Solvent -ical e nt Pads I I I I I I I I I I I I I I I I I I I Gas Partial Pressure Pdes I I :ium Re ference: Hochgesand.11 3 COMPARISON OF EQUILIBRIUM LOADING np' rT4.-.MTTAT. ATTh T.

Firstly. the gas streams may be washed with water or other suitable wash solutions to recover the vaporized solvent leaving the absorption or regeneration sections. At this temperature level. the absorption process is carried out at low temperatures. generally between O°F and -75°F. the hydrogen sulfide may be totally removed with only a fraction of the carbon dioxide. since Rect- ifier and is therefore at high pressure. isol favors absorption of hydrogen sulfide over carbon dioxide. both hydrogen sulfide and carbon dioxide are highly soluble in the methanol. Rectisol is ideal for high pressure processes since the equilibrium loading of a physical solvent is directly proportional to pressure. Advantages of the Rectisol Process The Rectisol process employs refrigerated methanol as a physical solvent to absorb both hydrogen sulfide and carbon dioxide. CONOCO design. Methanol has a Thus. This means that additional cooling beyond heat exchange is necessary. According to the literature. Solvent Recovery To minimize the solvent losses from the system. Such selective removal is important . high vapor pressure compared to most solvents.12 temperature is raised within the absorber. 1970). although the solubility of hydrogen sulfide exceeds that of carbon dioxide by a factor of 5-6 (Hochgesand. the synthesis In the gas comes directly from the gasFurther. the low temperature is also desirable to reduce the methanol losses due to vaporization. Rectisol has several attractions supporting its application in the CONOCO design.

taken from the CONOCO commercial design report. Rectisol Process Description This section discusses the specific design of the Rectisol process developed as part of the CONOCO Slagging Lurgi Coal Gasification commercial design. if the sulfur compounds are recov- ered with a low concentration of carbon dioxide. Figure 4 shows a simpli- fied block flow diagram of the process. such as a Claus Plant. Purified gas is then directed to the joint shift/methanation section.13 for two reasons. briefly below. 1970). as mentioned earlier. However. . Firstly. utilities would be needlessly consumed in removing a high proportion of the carbon dioxide at this stage (Hochgesand. the gas stream may be handled directly in a sulfur recovery unit. In the Rectisol unit.is displayed in Figures 5 and 6. A copy of the Rectisol process flowsheet. since carbon dioxide removal prior to shift conversion and methanation is not necessary. the synthesis gas produced in the gasification section is treated to remove the undesirable sulfur compounds and to recover any light oils in the gas. it may be attractive to remove a fraction of the carbon dioxide on account of the equilibrium considerations associated with the subsequent water-gas shift reaction. without overloading the sulfur plant or without recourse to further separation. The removed sulfur compounds proceed to the sulfur The details of each section are outlined recovery unit. indicating the major process sections. Secondly.

0 C12 10 Iz cil a) "I PL.CA E0 H4P- b4 . (a C U2 tr1 L r C 0 U) I Xaa A_ 0 IIH q P-) .0 * Fr 0 U) .

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water and hydrogen cyanide are removed with some of the acid gas. hydrogen cyanide and water are physically absorbed with refrigerated methanol. in the prewash section. The ensuing process steps are devoted to solvent regeneration in which acid gases are recovered from the methanol to yield a lean solvent of sufficient purity for recirculation. . The cooled gas then proceeds to the absorption sec- tion where the sulfur compounds. all the naphtha. This column produces an overhead composed of naphtha. The high purity The remaining naphtha layer is decanted and sent to storage. carbon dioxide. The absorption process occurs at high pressure and low temperature in two stages. the rich solvent streams from the prewash and main wash absoprtion sections are separately flash regenerated. A mixture of methanol and water is recovered in the bottoms which is subsequently separated in the methanol-water column. methanol-water-naphtha liquid is fed to the azeotrope column. naphtha. In the first step. The pressure of the solvent is reduced causing a frac- tion of the acid gases to desorb. the remaining sulfur compounds and a portion of the carbon dioxide are absorbed. Here a liquid-liquid separation is attained on adding the water rich bottoms from the water wash column.17 The feed gas is first cooled to absorption conditions by heat exchange with the purified gas and by supplemental refrigeration. while in the main wash section. The liquid from the prewash flash regenerator is sent to the naphtha extractor to recover the absorbed naphtha. hydrogen sulfide and methanol.

18 The hot regenerator serves to strip the main wash solvent of the gases that were not desorbed during flash regeneration. the azeotrope column and the naphtha extractor. The methanol overhead from the methanol-water column is also fed to this unit where the methanol vapors. After further refrigeration. act as the stripping medium. This total gas stream is finally water washed to recover any vaporized methanol prior to being sent to the sulfur plant. . in conjunction with those generated in the reboiler. The remaining methanol is cooled by heat ex- change with the naphtha extractor feed and the hot regeneration column feed. A portion of the regenerated methanol from the hot regeneration column bottoms is used as reflux for the methanolwater column. The acid gases are recovered in the overhead and com- bined with the gases from flash regeneration. the regenerated methanol is recirculated to the absorption section.

nitrogen. DEVELOPMENT OF PHYSICAL PROPERTIES MODEL Accurate representation of the phase equilibria was es- sential to the simulation work in view of the lack of process data. N 2. and CH30H. carbon monoxide and methane. In order to simplify the system. Moreover. CH4 . and the C2 . all the sulfur compounds are treated as hydrogen sulfide. H 2 S. C3. These simplifications H2 .19 III. which are significantly polar. reduce the system to the following nine components: C0 2. system is highly The presence of methanol and water. H 2 0. to: Thus. C4 compounds are lumped into the methane component throughout this work. C 6 H6 . which are supercritical. considerable effort was devoted to developing a good thermodynamic model. The conventional method invokes a liquid act- ivity coefficient model to represent the liquid and an equationof-state for the vapor. the system is described according iYiPT wherei xf = vapor fugacity coefficient PT = total pressure . the physical properties estimation was esp- ecially important since the hydrogen sulfide-carbon dioxidenitrogen-hydrogen-methanol-water-aromatics non-ideal. Selection of the Thermodynamic Model There are two approaches to modelling the phase behaviour of a mixture. The naphtha in the feed is represented as benzene since coalderived liquids are generally aromatic. CO. render this system hard to describe. Therefore. and hydrogen.

liquid mole fractions The alternative approach uses a single equation-of-state to describe both the vapor and liquid phases. the activity coefficient is normalized to 1. As such. As O'Connell (1977) points out.0 at infinite dilution and the Henry's Law constant becomes the standard state fugacity. An alternative model applicable to polar . 1981). How- ever.20 Xi = liquid activity coefficient fol= liquid reference fugacity 1 yixi = vapor. the standard state fugacity is that of the pure liquid at the system temperature and pressure. It is meaningless. Mathias (1981) has demonstrated that this model is effective in describing the coexisting vapor and liquid phases for systems such as methanol-water. On the other hand. ASPEN has recently adapted the Redlich-Kwong-Soave (RKS) equation-of-state to improve its ability to represent systems containing highly polar compounds. however. equation-of-state models have generally proved to be inadequate for predicting the non-idealities of mixtures containing polar substances (Mathias. thus. In this case. there are difficulties associated with referencing to the Henry's Law constant for multicomponent solvents since the constant is dependent on solvent composition. the composition dependence of the standard state fugacity should be built into the thermodynamic model. Noncondensable components in the mixture present a problem with regard to establishing the reference fugacity for the activity coefficient approach. Generally. it is necessary to follow the unsymmetric convention. to consider a pure liquid state for a supercritical component and.

must evaluate the chemical equilibrium for the dimerization process.08664 RT ci 22 P . accounting for the intermolecular attractive . as Mathias (1981) notes. the 'a' parameter may be regarded as an attractive parameter. ci ci To some extent. Modified Redlich-Kwong-Soave Equation-of-State The basic Redlich-Kwong-Soave equation is given by RT a V .b V( + b) where 'a' and 'b' are functions of critical temperature and pressure as follows a = (T)a ac= 0. 1979). The particular equation-of-state that was chosen was the modified version of the Redlich-KwongSoave model which is described in the next section.21 systems is the Perturbed Hard Chain equation-of-state (Gmehling et al..42748 R Tci P b = 0. so that the equation rests on a weak theoretical foundation. Consideration of the difficulties and inaccuracies associated with the activity coefficient model approach led to the selection of an equation-of-state to correlate the Rectisol system for this work. the model components by assuming that they dimerize. In addition. dimers are rarely observed experimentally. In this case. Such treatment proves to be a major drawback for this equation-of-state since it augments the computational effort substantially. the model handles polar Thus.

Boston and Mathias (1980) recommend a different expression for the supercritical region = exp(c (1 .3p Mixtures are represented by the above equations using the one-fluid theory.15613ao 2 = acentric factor. The ASPEN work has introduced the polar parameter. taken from the work of Graboski and Daubert (1978). the 'b' parameter is a repulsive term. On the other hand.55191 .Tr)(0a7 .Tr) T r = reduced temperature m p = function of acentric factor = polar parameter The correlation for m.5m d= cc 1 to extrapolate into +0. c(T) is used to correlate pure component vapor pressure data and has been modified by ASPEN to the following form 05 = 1 05) + m(1 . is m = where . 1 jj 1 i 3 .p( .48508 . For supercritical components.T)) with c = 1 +0.a. p. ' - a = .: bi f1 xix .22 forces. This means that the parameters 'a' and 'b' become quadratic mole fraction averages with the following form a zzx x.b. in the expression for to improve the vapor pressure predictions.Tr .0.1.. This parameter is empirical and must be determined by fitting experimental pure component vapor pressure data. representing the finite volume occupied by the component.

K0 a 1 .Kbij . deviation of the behaviour of a binary pair from that predicted according to the basic mixing rules. Prausnitz (1980) indicates that his experience has been good in employing only binary experimental data to predict multicomponent equilibria.a. are expressed as linear functions of the absolThese parameters account for the ute temperature in Kelvin. 13 ° 1 (b 2 b i )(1 . As the work proceeded towards determining the parameters for . Experimental Phase Equilibrium Data The physical properties model requires only binary interaction parameters in order to describe a multicomponent system. the binary interaction parameters. published multicomponent data are not available for the specific Rectisol system.) l13ai 5 (1 . values for these parameters may be established by fitting binary phase equilibrium data alone. This deficiency made it necessary to rely on experimental binary equilbrium data to a great extent.Kbi i + T ) 1000 2 As these equations show. Kai and Kb . four parameters. in cases where the critical conditions are exceeded. multicomponent predictions may be unreliable even if the binaries are fit well.K1 i T ) j 1000 b.23 where 0 aij = (a. He cautions that. In the absence of multicomponent vapor-liquid equilibrium data. K Any combination of these 'a' K a' Kb'Kb' K0 K may be used to fit binary vapor-liquid equilibrium (VLE) data to the modified RKS equation-of-state. provided that the system is well removed from the critical for each component. Unfortunately.

. This decision reduced the data fitting to the 21 possible interactions of the gas components with methanol. Justification for this simpli- fication lay in the fact that the non-idealities of the liquid phase were expected to dominate over the vapor phase non-idealities. presenting quaternary data for the hydrogen sulfide-carbon dioxide-nitrogenmethanol system (Rousseau et al. benzene and water themselves.24 the modified RKS model. For instance. A literature search revealed experimental phase equilibria for each of the binary pairs. These data initially served as a comparison for the multicomponent equilibria predicted by the preliminary physical properties model. Subse- quently. the data adequately spanned the temperatures where a given interaction was most relevant. In order to maintain the data fitting effort at a manageable level. benzene and water and the interactions between methanol. varying from -75°F in the absorption section to as high as 250°F during solvent regeneration. 1981). gas-liquid non-idealities are most . provide Although this information did not complete temperature coverage. leading ultimately to an improvement in the model predictions. the results of a recent study at North Carolina State University became available. To minimize the degree of extrapolation. it was initially decided to ignore the interactions between two gas components. the parameter estimation work called for data covering as wide a temperature range as possible. The temperatures in the Rectisol process span a broad range. the quaternary data were used to improve the binary parameter estimates. as Prausnitz notes (1980).

1 (Xlil) . methanol and water. only the most recent was selected for the model development unless these data appeared to be generally inconsistent with previous data. In cases where more than one data set were located for a binary pair.25 important at the lower end of the temperature range where absorption takes place. the high temperature processes mostly involve the separation of benzene. K. DRS employs the maximum-likelihood This analysis recog- principle in reducing experimental data. Cr1 1 in which the superscript 'o' stands for the value adjusted according to the thermodynamic model.2 o 2 + o. On the other hand. a. K. e x2 2 + . while 'e' refers to the . Development of Modified Redlich-Kwong-Soave Model Parameters Fitting the modified RKS model to binary experimental data involved adjustment of a combination of the four interaction parameters. P. nizes that experimental data contain random measurement errors which it takes into consideration. The best estimates for the combination of parameters were generated for each set of binary data using the ASPEN Data Regression System (DRS). The system creates an objective function comprised of sum-of-squares terms for each observed variable. as discussed previously. assuming that the errors are randomly distributed about zero with a normal distribution. for example: N e 2 1 (Pi-Pi) -T i ) T. K.. K1. The standard deviation associated with a particular measurement is supplied by the user.

While this anomaly causes no computational difficulty. ations were adopted for this work. One notable example is the benzene-water system for which all four parameters are essential to modelling the observed liquid immiscibility.001. the term (1 . in the final set of interaction parameters. large parameter values are necessary to represent the equilibrium. pressure . in the case of benzene and water.0. In DRS. it does mean that the model must be considered to be purely empirical .003. Many of his recommend- For instance. as Prausnitz suggests: temperature .0.1 mmHg. Prausnitz (1980) presents an informative discussion of the methods of estimating parameters. two parameters adequately correlate the equilibrium data. liquid mole fraction . additional parameters are included for some pairs if these improve the fit significantly.K1 T ) and the analogous term for the 'b' paraaij aij 100-0 meter must have a positive value. the follow- ing values were used for the standard deviation of the measured variables. the Britt-Luecke (1973) generalized least-squares algorithm computes estimates for the model parameters such that the objective function is minimized. The terms are summed over all data points. the parameters must satisfy the equilibrium constraint that the fugacities of all equilibrium phases are equal.0. in order for the 'a' and 'b' parameters in the fundamental RKS equation to retain their theoretical significance. Unfortunately. It should be noted that.26 experimental value. rendering the above terms negative. At the same time. The data regression work demonstrated that.050°C.K 0 . in most cases. How- ever. vapor mole fraction .

less than 6 percent. 1981. Whiting. Further work in this area lay beyond the scope of this project. Prausnitz.27 as far as benzene and water are concerned. The maximum error in the liquid composition for a set of binary data was. the binary parameters exhibit a high degree of correlation which indicates that the parameters are not uniquely determined. on the whole. Further. may be better represented using the recently proposed mixing rules based on the localcomposition concept (Boston. such as the benzene-water mixture. In other words. In general. 1981). Evaluation of the Preliminary Thermodynamic Model The preliminary thermodynamic model of the Rectisol system was comprised of the modified RKS equation-of-state with interaction parameters generated by regression of binary . It has been suggested that highly non-ideal mixtures. ing chapter. the benzene-water experimental data adequately cover the temperature range of importance in the Rectisol process. there may be some concern about using the equation-of state to extrapolate information. good agreement was obtained between the experimental binary data and the thermodynamic model predictions. a comparison with experimental data demonstrates that the model provides a good prediction of the liquid-liquid equilibrium for the methanol-benzenewater system. However. For a given This comparison is illustrated in the follow- binary pair. As such. the experimental data may be rep- resented by several alternate parameter combinations with little loss of accuracy.

Further. overpredicting the bubble point pressure by as much as 30 percent and overestimating the nitrogen in the vapor at the expense of the carbon dioxide. the predicted Henry's Law constants for nitrogen in mixed methanol-carbon dioxide and methanol-hydrogen sulfide solvents exhibited unexpected behaviour.28 data. mix =Zixi ln HN. To assess the validity of the model. In an effort to ameliorate the situation. Bubble point calculations using the experimental liquid composition and temperature permitted a comparison of the predicted bubble point pressure and vapor composition with the actual data. as just described. the predicted equilibria for the hydrogen sulfide-carbon dioxidenitrogen-methanol subsystem were checked against the data presented by the North Carolina State University team (Rousseau et al. The experi- mental data appeared to be consistent with the approximate relationship that ln HN with ~~. hydrogen sulfide-nitrogen) were regressed from binary data and included in the model. parameters modelling the gas-gas interactions (carbon dioxide-nitrogen.. considering them to obey the simple mixing rules without correction. Unfortunately. the model did not prove to represent the data adequately. The resulting improvement in the model predictions was not considered sufficient. = solvent mole fraction on solute free basis 21 However. This model neglected any gas-gas interactions. 1980) x. 1981). rather than displaying linearity on a logarithmic basis according to the above expression. the predicted Henry's Law constants increased initially with a small increase in the . i(Prausnitz. hydrogen sulfide-carbon dioxide.

-This means that they employed a separate equation In their model. the vapor mole fraction of nitrogen is overpredicted. The abnormal solubility behaviour is in part re- sponsible for the deviations between the predicted and experimental compositions. The apparant success of Rousseau et al. The lower results from utilizing the quaternary data in estimating the parameters for the physical properties model.29 amount of dissolved carbon dioxide or hydrogen sulfide. it was concluded that the vapor interactions between carbon dioxide and nitrogen are strong and conceal any non-idealities in the liquid. a small amount of dissolved gas in the methanol results in an unexpectedly high Henry's constant and consequently a lower solubility for nitrogen. which is discussed in detail in the following section. the vapor is represented by for each phase. Therefore. This fact makes the system It did not appear possible to isolate the vapor and liquid behaviour from binary data using a single equation-of-state. The upper two demonstrate the improve- ment in the behaviour of the constant on inclusion of the gasgas interactions. hard to analyze. Figure 7 illustrates the variation of the The plot in- Henry's Law constant with solvent composition. In the model. cludes three curves. From an analysis of the experimental data and the model predictions. the RKS equation-of-state with interaction coefficients set . The constants appeared to reach a maximum before decreasing to the Henry's Law constant for nitrogen in pure carbon dioxide or hydrogen sulfide. (1981) in modelling the quaternary system may be attributed to the fact that they adopted the activity coefficient approach.

2_) 0oo n 0 0 0 0 0 0 CM cn V 0 0 0 0 0 -A- 0 V C 0 0 0 omq'e 'ueosjqTN oJ us!suoo M 1j sRJuaH . EOZ m 00 00 Oi *H z r.H H CD Q ¢ a4 > E1 -I o .30 0 .i 0 C E-q Z X 0H i--. R~ 0 ~: 0 0 o*H . I--a) 0 0 H* () Z~ v N < 0 0 O\ 0C) C1.tH zO P4 H 0 .. Z Cl.

several parameters were fixed before the final DRS run rather than fitting all the gas-gas interactions with the quaternary data. it appeared that the 'a' parameter. Hydrogen sulfide-nitrogen gas interactions appeared less significant. which are both subcritical. So that the DRS runs would converge. The effect of the vapor interactions for the hydrogen sulfide-carbon dioxide pair. the attractive term in the basic equation. due to the liquid phase parameter. In working with the modified RKS equation.for subcritical components since the modified RKS equation only reduces to the original RKS equation at conditions below the critical. hydrogen sulfide and nitrogen. For the final model.31 to the standard vapor values available from separate vapor phase studies. while the repulsive 'b' term could be considered as representing the liquid. Having established the vapor behaviour in this manner. could be treated as the vapor term. the liquid behaviour could be considered independently. was modelled with the . could The remaining non-idealities then be reflected in the 'b' It should be noted that this approach is only suitable . so the original parameters developed from binary data were used. it was decided to use the quaternary experimental data in the data regression runs to generate improved parameter estimates for the interactions between carbon dioxide. This observation suggested that the vapor interactions could be isolated from those in the liquid by fixing the interaction parameter for the 'a' term to the standard RKS vapor value reported in the literature.

32 standard RKS value for K (Graboski and Daubert, 1978). Data

a

regression of the quaternary data then established parameter estimates for estimates liquid K aKtrge for carbon dioxide-nitrogen and th the nd Kb The resultant

for hydrogen sulfide-carbon dioxide.

model predictions agree substantially better with the experimental data as the comparison in Table 1 shows. The bubble

point pressure predictions still appear to deviate from the data, especially at the higher pressure levels, however. Table 2 displays the final parameter estimates, indicating the literature source of the data. This table shows that the

final set includes values for several additional gas pairs which were readily available from previous work (Mathias, 1981). The parameter set is stored in a user library under RKAKIJ, to be called directly by the simulation program.

Enthalpy Calculations
In order to guarentee reliable enthalpy predictions from the modified RKS model, enthalpy data should be included in the data regression runs to determine interactions parameters. However, such data were not available for the Rectisol system. Under these circumstances, the Lee-Kesler equation-of-state was favored over the modified RKS equation-of-state for enthalpy calculations. The former correlation has a good reputation

for predicting reasonable mixture enthalpies based on the pure component properties.

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On account of the lack of actual oper- ating conditions. this work adopted the approach of developing a viable Rectisol design based on the CONOCO design flowsheet and feed composition. While the process flowsheet shows detail of the sequence of operations and the destination of all intermediate streams. heaters and pumps represent the Rectisol process. The information presented in the CONOCO Commercial Design Report consists solely of the feed and product compositions and a process flowsheet. Therefore. The feed gas composition. no specifics are provided for the process operating conditions. it was impossible to develop a simulation that would match the CONOCO design. To minimize the computer time and cost associated with simulating a complex cyclic process such as Rectisol. splitters. SIMULATION OF THE RECTISOL PROCESS Basis for the Process Simulation The proprietary nature of the Rectisol process restricts the amount of process data disclosed in the literature. pressure and temperature displayed in Table 3 were taken for the process model. In this simulation. Detailed simulation of the other process units using ASPEN established the remaining operating conditions necessary to achieve the desired separation. a series of simple unit operations such as mixers.36 IV. flashes. Rigorous simulation of the staged separation units is performed . The literature search located typical absorption temperature and pressure ranges only. a simplified process model was assembled.

9 299.2 Propane Propylene Butane Butylene Nitrogen Hydrogen Sulfide Carbonyl Sulfide Carbon Disulfide Thiophene Hydrogen Cyanide Naphtha Water Total Temperature.0 0.1 13.9 2.0 8. psia 4. OF Pressure.1 471 1 18.8 1.7 2.3 95 427 .7 131.2 1.4 trace 23.37 Table 3 COMPOSITION OF FEED GAS TO RECTISOL PROCESS Component Hydrogen Carbon Monoxide Carbon Dioxide Methane Ethane Ethylene lbmol/hr 1909.6 41.1 0.8 6982.7 4052.

In designing the absorbers. external to the overall flowsheet.38 on a stand-alone basis. For a given degree of absorption. The development and design philosophy employed in each of the major process sections is discussed in detail below. indicating the correspondence between the model and the actual design flowsheet. and the operating pressure. A block flow diagram of the overall flowsheet simulation is shown in Figure 8. H2SABS1. Appendix A contains the computer input and output for the simplified Rectisol model. which is ASPEN's rigorous model for multistage vapor-liquid fractionation. the temperature of the entering gases and solvent. Hochgesand (1970) indicates that for the Rect- isol process the methanol circulation rate greatly affects the process economics. the designer must establish the number of trays. The results of such rigorous simulations established the splits to be used in the simplified model. where the bulk of the hydrogen sulfide absorption occurs. since it influences the size of all process . and a main wash section. PREWASH2. Each section was simulated independently using RADFRAC. these parameters then dictate the required solvent rate. where the units are modelled by separator blocks. Absorption Section The hydrogen sulfide absorber consists of two separate sections. The results of these simulations were used to set the degree of absorption in the overall flowsheet simulation in which two mixers and two separators (PREWASH1. a prewash section. which removes all the water and naphtha from the synthesis gas. H2SABS2) model the absorption section.

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40 equipment. a heat balance shows that the feed may be cooled by heat exchange to -30°F without supplemental refrigeration. Sasol report such temper- ature levels for their Rectisol operation. Further. This pressure of 421 psia is the pressure of the gasifier overhead less an allowance of 6 psi for the pressure drop through the heat exchange train. The design for the prewash absorber features six theoretical trays and a solvent rate set at 25 percent greater than the theoretical rate required to absorb all the naphtha. 1957). 1968).. economics rarely With the same con- justify compressing the feed gas further. Herbert. According to Hochgesand (1970). 1956). sought to minimize the methanol solvent rate. the absorbers are designed to operate at the maximum pressure compatible with the other units.15 psi pressure drop per stage (Treybal. sideration in mind. regeneration costs etc. pumping costs. In the current design. therefore. the absorbers are designed as The pressure drop through the column is based trayed columns. Since high pressure favors physical absorption. 1977. The design of the absorption section. although there is some evidence in the literature to suggest that trayed columns are more common for Rectisol (Maddox. the absorbers are designed to operate at low temperature with the recirculating methanol cooled to -75 °F 0 and the feed gas cooled to -30°F. on the rule-of-thumb of 0. although this study did not examine the detailed heat exchange between the feed and desulfurized gas. This . Absorption columns may contain packing or trays. which appear to be typical (Hoogendoorn.

The gas from the prewash absorber proceeds to the main wash section where all the hydrogen sulfide and part of the carbon dioxide are removed. Figure 9 shows a plot of carbon dioxide in the The rel- outlet gas versus solvent rate and number of trays. the basis for the ab- sorber feed composition did not account for the small amount of recycled hydrocarbon gas. ative insensitivity of the required amount of solvent to the . while achieving complete removal of hydrogen sulfide. the methanol rate is restricted to the minimum that ensures complete naphtha absorption. Given the objective of the prewash absorber to recover the naphtha with as little hydrogen sulfide as possible.follows the recommendation of Kohl and Riesenfeld (1979). A sensitivity study to the number of trays in the main wash absorber indicated that an increase from six to ten trays results in a reductions of only 2 percent in the required methanol rate. The methanol solvent rate to the main wash section was determined so that the degree of carbon dioxide removal agreed with the information presented in the CONOCO Commercial Design Report. This means that the predicted carbon dioxide gas removal in the overall simulation is not in complete agreement with the CONOCO commercial design. the feed is preflashed so that any liquid may bypass the absorber. 1973). This preflash simulates what would actually occur in the bottom of the absorber. In order to improve the performance of the RADFRAC model for the prewash absorber. However. It is unusual for an absorber to contain less than six or more than ten theoretical trays (Perry and Chilton.

42 Figure 9 EFFECT OF SOLVENT RATE AND NUMBER OF TRAYS ON CARBON DIOXIDE ABSORPTION 260 d~ o 0 220 02 in Feed )er d 180 q. D- l 3000 3400 3800 4200 4600 5200 Methanol Solvent Rate.C\2 ro 140 0 0O . . lbmol/hr .

Flash Regeneration Section In the flash regeneration section. the main wash and prewash absorbers operate with 3100 lbmol/hr and 330 lbmol/hr of circulating methanol respectively. The pressure of downstream processes dictate the In this simulation. with an intermediate pressure of 75 psia. the intermediate pressure must minimize the amount of hydrogen sulfide and carbon dioxide desorbed while recovering as much of the desired hydrocarbon gases as possible. In the final simulation. a fraction of the absorbed gases are recovered from the rich solvent by a reduction in pressure. the main flash regenerator is designed to flash the main wash solvent to 30 psia in two stages. FLSHRG1. Naphtha Extractor In the naphtha extractor. The three flashes are simulated as two-phase adiabatic flashes (PRWSFLSH. Since the vapor from the first flash is recycled to the absorption section. The output from simulating both the prewash and main wash absorbers rigorously is included in Appendix B. The feed . An intermediate pressure of 75 psia represents an appropriate compromise. Similarly. regenerator flashes the prewash solvent to 30 psia. FLSHRG2).43 tower size justified designing the main wash absorber with six trays. the methanol-water-naphtha-gas stream is allowed to separate into two liquid phases to permit removal of the naphtha-rich phase from the system. allowing sufficient pressure head to feed the water wash column without further compression. the prewash flash final flash pressure.

while all the water and remaining methanol are recovered in the bottoms. Preliminary simulation of the column using RADFRAC suggested that a good separation is possible in this column. published data were not located at the actual separation temperature. Azeotrope Column The objective of the azeotrope column lies in removing the residual naphtha and dissolved gases from the methanolwater mixture. the prewash flash bottoms is preheated to 50°F. This simulation indicated that all the gas components and naphtha are distilled in the overhead along with a small portion of the methanol. the naphtha extractor is represented by a feed mixer (NEXMIX) followed by a three-phase adiabatic flash at 30 psia (NEXSEP). In the overall model. The plot in Figure 10 illustrates the comparison between the predicted separation at 38°F and experimental data at 77°F. The design pressure is 30 psia.44 consists primarily of the bottoms from the prewash flash regenerator to which a water-rich stream is added to effect the liquid-liquid separation. yielding an uncontaminated methanol-water stream. At these conditions. The water source is the bottoms In order to ensure that the naphtha extractor operates without any of the water icing. 5 psi higher than the water wash column to which any vapors are directed. Unfortunately. from the water wash column. As the name of the . the physical properties model predicts a phase separation into two liquid phases which are in reasonable agreement with liquid-liquid experimental data for the methanol-benzene-water ternary.

45 d) a) N a) wIu 1 9 I4 I 1-1 M a) C .

A revealing method of interpreting tray-to-tray output uses the idealized McCabe-Thiele techniques (Russell.0 While this ratio appears to leads to satisfactory operation. Development of a feasible design for the azeotrope column involved setting the distillate rate. a reflux ratio of 2. The behaviour of the column proved to be highly senThe amount of material in the sitive to the reflux ratio. and . a high reflux ratio is necessary to ensure adequate vapor flow throughout the column. Seeing that the split between the overhead and the bottoms was well defined in the preliminary study. difficulties were encountered in obtaining a converged RADFRAC solution at lower reflux ratios. rectifying section of the column depends directly on the reflux ratio.4 mole methanol at 128.8°F). the reflux ratio. the distillate rate could be established purely by material balance considerations. 1981). and the feed entry point. This tool provides valuable insights despite the non-ideality of the particular system. the overhead may be expected to contain benzene and methanol in their azeotropic compositions (61. In the final design. If methanol and benzene are iden- tified as the two components which require separation. be substantially higher than the minimum reflux ratio. Since such a large percentage of the feed (94 mole percent) ultimately appears in the bottoms product. Further simulation of the column with RADFRAC demonstrated that in the overhead methanol and benzene may indeed reach their azeotropic composition on a methanol plus benzene basis.46 column suggests. the number of theoretical trays.

the feed enters at the third stage. In Figure 11 suggests that a slight improvement in the column efficiency may be realized with the feed located at the second stage. where compositions are plotted on a logarithmic scale for clarity. assuming constant molar overflow. the azeotrope column feed is preheated by heat exchange with the waste water from the methanol-water column. The diagram also shows that the physical properties model predicts an azeotrope composition close to that reported. The equilibrium compositions were This type of plot taken directly from the RADFRAC output. identified pinch points. the minimum reflux ratio.47 all the compositions are normalized on a methanol plus benzene basis. as . For in- stance. as well.0. a McCabe-Thiele x-y diagram may be prepared. sheet. the feed must be greater than 82 percent liquid in order to meet the desired distillate rate. The final temperature of the waste water was taken to be 118°F. the final design. it can be seen that increasing the number of trays would not improve the separation. Higher degree of vaporization results in insufficient In the actual process flow- vapor in the stripping section. The feed quality plays a significant role in the column design. with a reflux ratio of 2. Fig- ure 11 displays such a diagram for the upper portion of the azeotrope column. predicts the maximum percentage of vapor permitted in the feed for the column to operate as desired. Given the fixed distillate rate of 45 lbmol/hr a simplified material balance analysis. Since the overhead lies at this composition. and indicated the optimum feed location during the column design.

.i . 4z O rG HEq4 I 0 -I I . N: 0 \0 I~~~~ -. I .I.I :: . t.Ii: ! I ..$ XO _ IT . . i I mq N i (2) i i . e 4ffll It I f. .j . I I. 11 I I : . .. . J ¢ I I m .? Ai' CD _ t I I I !---- . . II I N 4t.e7 _ N is \0 .! i I i I . .. i Nj i U. !. I 0' 3a %t 0 . H¢ a) x4 C) _. mm+mw i I I. I Ii i' iI I ' 0 o Io A. i I o In i i IvWg I I Ill c - I ii : I ) I. i I i NJ I 11 . I - I"t~ E 4 -[ - - - I I I1 IL 4 4~D lp v 1-H0 H _ +Hg _ - .48 o w !15. 'CA - ¢ 0 o 0 E0 . b : aio 0 4 J.I I. I' 'li 1 I · I ' i q o i N i 2 0i I 10 D P -g I 0 i 1D.l 0 10Y .

the column is designed to yield a 99 percent pure methanol distillate. This same diagram showed that the minimum reflux ratio occurs at a value of approximately 0. This heat exchange results in an all liquid azeotrope column feed at a temperature of 96°F. are highly composition dependent. Methanol-WaterColumn The methanol-water stream from the azeotrope column bottoms is separated in the methanol-water column. In addition. design introduces the feed on the nineteenth stage from the top which is the optimal stage according to the McCabe-Thiele technique. converging is a consequence of the non-ideality of the system in which the outside loop variables for RADFRAC. a McCabe-Thiele diagram pro- vided initial estimates of the number of stages required to effect the desired separation at a given reflux ratio. and to examine the sensitivity to various design parameters. .9.49 indicated on the CONOCO flowsheet. for this simulation. This simulation required 40 outside loop iterThe difficulty in ations to achieve a converged solution. The rigorous simulation of the azeotrope column is shown in Appendix C. A RADFRAC model was used to develop the column design. the desired methanolThe final water separation requires 25 theoretical trays.2 for the column design. namely Kvalues and enthalpy. At such a reflux ratio. This general rule was followed in chosing a reflux ratio of 1. Perry (1973) indicates that setting the reflux ratio 30 percent higher than the minimum reflux ratio generally minimizes the combined operating and fixed costs. In this sim- ulation.

the column is represented by a mixer and separator block (MWMIX. the overhead vapors proceed directly to the hot regeneration column to act as reflux. Detailed output from the RADFRAC simulation is located in Appendix D. Increasing the reflux ratio from 1. The column is designed with 10 theoretical stages with the main wash solvent and methanol distillate feeds located on the third and sixth stages from the top.0 or greater.0. a total condenser is included on the overhead. Hot Regeneration Column The purpose of the hot regeneration column is to strip the main wash solvent completely of the acid gases remaining after fash desorption. These simulations indicated that it is poss- ible to strip essentially all the acid gases from the methanol at reflux ratios of 1. with those generated in the reboiler. Methanol from the methanol-water colThe methanol vapors. respectively.0 to 2.0 does not . MWSEP) with the reflux rate calculated by the Fortran paragraph REFLUX. acting as the total condenser. combined umn is also fed to this column. the overhead vapor contains less than 0. In the actual flowsheet.5 to 2. strip the acid gases from the solvent.50 In the RADFRPAC model of the column. Since the methanol overhead and the hot regeneration column bottoms differ very little in composition. the hot regeneration column is. in essence. however. At the same time. In the overall flowsheet.07 mole percent methanol vapor. The column was simulated with RADFRAC at reflux ratios ranging from 0.

the overhead may contain a significant percentage of methanol vapor and. The detailed RADFRAC simulation of this column established the splits for the separator (HTRGSEP) representing the column in the overall flowsheet.5 reflux ratio. at low reflux ratios. On the other hand.51 improve the separation significantly. the column can be refluxed by condensing the methanol. the design of the hot regen- in the water wash column. at a reflux ratio of 0. methanol accounts for 98 percent of the condensate which is condensed at 97°F. at a 0. The overhead At column temperature varies greatly with the reflux ratio. therefore. the separation is inadequate. However. and increased methanol losses on the other. beyond the scope of this work. a reflux ratio of 1.0 was selected where the methanol losses are negligible.5. a significant amount of the methanol is lost with the acid gases. Some of this may be subsequently recovered Thus. The RADFRAC model is included in . The temperature is low enough so that the acid gases require no further refrigeration prior to the water wash column. Under these circum- stances. ratios exceeding 1. Such a trade-off lay For the purpose of this sim- ulation. eration column must consider the trade-off between a high condenser duty requiring refrigeration on one hand.0. the overhead contains practically no methanol and must be cooled to -40°F or less in order to condense sufficient material for reflux. For instance. Appendix E. resulting in approximately 13 mole percent methanol in the overhead.

The rate of water addition was deter- mined from experimental data so that the subsequent liquidliquid separation in the naphtha extractor would yield a methanol-water phase containing less than 1 mole percent benzene. as an input stream. Heat Exchangers The naphtha extractor feed/regenerated methanol. The water-rich stream from this unit is sent to the naphtha extractor to effect the liquid-liquid separation. The absorber feed gas cooling train is handled by a series of heaters. which represents the other side of the exchanger. The heat duty calculated in one heater is passed to the second heater. The results from simulating this column as a four stage absorber with RADFRAC (see Appendix F) demonstrate that such a water rate is sufficient to ensure no methanol carryover with the acid gas. exchange with the purified gas. The split in duty between the two regenerated methanol coolers is determined so that the naphtha extractor feed (prewash flash bottoms) is preheated to 50°F to ensure operation of the naphtha extractor without any icing. In the simplified flowsheet. . azeotrope feed/waste water. the water wash column is modelled with a separator block (H20WSH) which separates the feed according to the distribution predicted by the rigorous model.52 Water Wash Column Methanol vapor is recovered from the combined acid gas streams in the water wash column. however. and hot regenerator feed/regenerated methanol heat exchangers are each modelled using two heaters. The simulation does not model the detailed heat An enthalpy balance.

while the regenerated methanol from the hot regeneration column (RGMETC2) is considered as a product stream. the regenerated methanol recycle stream is broken. This simplification is possible since the stream composition is well defined and the stream rate is maintained at the design rate by the methanol make-up stream. Thus. The flowsheet is converged with an ASPEN generated tear stream set using the Wegstein convergence method. Three . any methanol lost from the recycle stream. The CONOCO Design Basis shows that the purified gas is heated to 77°F after heat exchange. Methanol Make-up A methanol make-up stream contributes to steady operation of the hydrogen sulfide absorbers by maintaining the methanol circulation at the design rate.53 indicates that the heat removed from the feed gas in cooling the gas to -30°F is sufficient to heat the purified gas to 67°F. Flowsheet Convergence To facilitate the convergence of the overall flowsheet which contains several recycle loops. The make-up stream replaces In the simulation. the absorber feed temperature may be achieved through heat exchange with the purified gas without any supplemental refrigeration. the meth- anol solvent to the absorption section (RGMETC) is treated as a feed stream. a Fortran paragraph (MAKEUP) calculates the required make-up rate. Such treatment permits the flowsheet to be divided into two subsystems which can be converged separately. More specifically.

54 material streams and two heat streams must be converged to converge the entire flowsheet. .

2 percent water and 2 ppm hydrogen sulfide. . as was mentioned earlier. the methanol circulation rate in the simulation could be increased. Therefore.55 V. The comparison shows that the ASPEN model predicts This discrepancy a higher yield of each gas constituent. The composition of the regenerated methanol calculated by the rigorous simulation of the hot regeneration column is shown in Table 6. The acid gas and the desulfurized gas are related by material balance since virtually all the gases are recovered in these two streams. The predicted composition of the desulfurized gas is compared with the composition from the CONOCO Design Basis in Table 4. To improve the agreement between the simulation and the design. the degree of absorption predicted by the ASPEN model is lower than that accomplished by the CONOCO design.8 percent purity. the lower degree of absorp- tion shown by the ASPEN model leads to a lower acid gas recovery as compared to the CONOCO design. contaminated only by 0. Therefore. stems from the fact that the methanol circulation rate was established based on the fresh feed gas composition which neglected the recycled hydrocarbon gas. RECTISOL PROCESS SIMULATION RESULTS The process simulation provides a stream-by-stream heat and material balance which is shown in the simulation output in Appendix A. Table 5 presents the acid gas composition for both the design and the simulation. The model predicts that it is possible to regenerate the methanol to 99.

13 8.6 0.1 Nitrogen Hydrogen Sulfide & Carbonyl Sulfide 13409 8 0 1.0 ACID GAS COMPOSITION Component ASPEN Model lbmol/hr 0o.8 o0.7 159.9 0.o 0.56 Table 4 DESULFURIZED GAS COMPOSITION Component ASPEN Model lbmol/hr 1909.o Table 6 Water Naphtha Methanol 5.Butane Hydrogen Sulfide Nitrogen 173.2 41.0 0.3 CONOCO Design lbmol/hr 2.90 0.6 0.9 16.6 0.84 .0 o0.4 485.0 Water Naphtha Methanol Table 5 o0.6 41.0 4037.0 REGENERATED METHANOL Component Hydrogen Sulfide ASPEN Model lbmol/hr Water Methanol 3817.1 0.Butane 4.7 15.4 4048.6 2.0 1907.0 0.5 0.0 Hydrogen Carbon Monoxide Carbon Dioxide Methane .9 0.7 CONOCO Design lbmol/hr Hydrogen Carbon Monoxide Carbon Dioxide Methane .2 125.6 138.0 139.4 499.

a higher methanol circulation rate or a lower absorption feed gas temperature is required. The deviation may be attributed to the differences in the design basis for the simulation and the actual CONOCO design.86 MMBtu/hr. is 16. the calculated frigeration duty. The heat balance predicts that the refrigeration duty to cool the recirculating methanol is 10. heating duty is significantly higher than that for the CONOCO design. The heating duty represents the steam heat required to reboil the azeotrope column.80 MMBtu/hr. In order for the simulation to match the degree of carbon dioxide absorption in the CONOCO design. The total predicted cooling duty. Both of these design changes would raise the reAs Table 7 demonstrates. . As such.57 Table 7 shows the heating and cooling duties calculated by the process simulation. the methanol-water column and the hot regeneration column. including both refrigeration and cooling water duty. This is lower than the duty quoted for the CONOCO design. the heating duty is highly sensitive to the specific column design.

10 25.96 .22 10.63 16.07 11.80 18.31 1.58 Table 7 COOLING AND HEATING DUTIES FOR THE RECTISOL PROCESS ASPEN Model MMBtu/hr Refrigeration and Cooling Water Duty Solvent Refrigeration CONOCO Design MMBtu/hr Hot Regeneration Column Condenser Azeotrope Column Condenser 10o86 4.76 Steam Heating Duty Azeotrope Column Reboiler Methanol-Water Column Reboiler Hot Regeneration Column Reboiler 4.75 10.

The effect of a design modification to one of the major process units may be examined using the rigorous standalone model. An enhancement of the . this project was concluded. before a valid comparison could be made at an increased methanol circulation rate. The current basis for the methanol circulation rate. It is difficult to assess the validity of the computer model in view of the lack of published process data. The results of this simulation may then be trans- ferred to the overall simulation to assess the impact of the change on the process as a whole. and the methanol circulation rate. CONCLUSION The process model described in this report represents a viable Rectisol process. the model may be employed to consider the trade-offs between such variables as the absorption temperature.59 VI. a minor adjustment of the main wash solvent rate to approximately 3400 lbmol/hr from the current 3100 lbmol/hr is expected to bring the model predictions in line with the design basis. due to lack of computer funds. In addition. based on the CONOCO design. However. the degree of regeneration. renders this comparison meaningless.which is not consistent with the CONOCO basis. The model demonstrates that the synthesis gas may be desulfurized and the methanol solvent may be regenerated with reasonable operating conditions. One point of comparison lies in the predicted compositions for the desulfurized gas and acid gas. Unfortu- nately. The Rectisol computer model was developed as a flexible tool which may be applied in future design work or sensitivity studies.

.60 Rectisol model by linking it to the ASPEN Cost Estimation Subsystem and Economic Evaluation Subsystem would permit these design changes to be evaluated from an economic standpoint.

Mathias. M. Chem. Britt. V. CONOCO. W. J. G. Boston. Canadian 15. 49. Alder.. (1977). 34.. Eds: D. 62 (7). Quarterly Technical Progress Report for Period 1 Oct. Eng. Hoogendoorn. 233 (1973). F. MA. J. 448 (1978). Ritchie." Presented at Second International Conference on Phase Equilibria and Fluid Properties in the Chemical Process Industries. Chem. 132 (1957). D.. 22... Ind. Chem.I. J. J. J. Sci.. S. B." Published by Dechema. Gerrard. Ind. H. E. Dechema Chemistry Data Series. Ind... 694 (1971). Dev. 1980a.. 6. C.. Chem. "Phase I: The Pipeline Gas Demonstration Plant.. 1980. Eng. Erdol und Kohle. Graboski. Phys... P. Des. "Phase Equilibrium in a Third Generation Process Simulator. 2. J M. M. Deutsche Gesellschaft fur Chemisches Apparateweses. Process Herbert. 951 (1979). . Eckermann. Bahrens. Donnelly. D. C. "Vapor-Liquid Equilibrium Data Collection. Eng. West Berlin. 1980. 17 (4). 623 Gmehling. Lui. (1956). Chem. R. Energy Laboratory and Chemical Engineering Department... Technometrics. J. G. M. Houghton. Inc.. 37 (1970). Clarke. D.. N. Daubert. 1979. Chem. D.T. Chem. McLean. 3 (6). 2. J. Hanson. M. H. N. M. Eng. L Evans. Cambridge. "Phase I: The Pipeline Gas Demonstration Plant. 9. P. Prausnitz. Eng.. Biotechnol. Brit. Design and Evaluation of Commercial Plant. Chem.. (1971). R. Appl.. J. T. 748 (1957).. Glew. 77 Hochgesand. Process Design and Preliminary Project Engineering Design". Cook." FE-2542-26... Thermo. I. W. Personal communication. March. 238 (1957). Luecke. G. V2. J. J. D. D. Salomon. 753 (1972). Chem. F Katz. 514 (1954).. W. Sci..1979 to 31 Dec. W. 26 (4). .. M. Chem. D. R. FE-2542-28. Vol. Battino.LITERATURE CITED Boston.. Eng. 46 (3). E. H. A. F.

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Treybal. H. Chem.CO. J. 1." John M. V... 1977. Kermode. 247 (1977/1978).. vol. 238 (1957). J. A. R..N 2." Ind.. L. W. M. Salomon.. E. M. 88 (1979). G." Adv."Mass Transfer Operations. J. J.. I. R."Gas and Liquid Sweetening. 1979. Prausnitz.. H.. Inc. Hochgesand. J." Second Edition. New Jersey: Prentice-Hall. L. "Rectisol and Purisol. . 406 (1969). 62 Hoogendoorn. 15. Maddox." Fertilizer Science and Technology Series. "Rectisol: A Low-Temperature Scrubbing Process for Gas Purification. 1981. Partridge. P. Campbell. 1968. W. "Molecular Thermodynamics of Fluid-Phase Equilibria-" Englewood Cliffs. "Production of Ammonia Synthesis Gas by Purification and Shift Conversion of Gas Produced from Coal. Erdol und Kohle. New York: Marcel Dekker. 37 (1970). Jungfer." Fuel Processing 2 3 Technology. 2. M. 1973. Acid Gas Absorption Kohl.. G. 233. "Computer Calculations for Multicomponent Vapor-Liquid and Liquid-Liquid Equilibria... "Sasol: World's Largest Oil-from-Coal Plant. New York: McGraw-Hill. J. Eng. "Wilson Parameters for the System: H2 ." The Chemical Engineer. Cry. Prausnitz. C. 1969. J. Linde. Scholz." Brit. (7). R..C0 . "A Versatile Phase Equilibrium Equation of State. 77 (1956). Riesenfeld. W. Chem. Inc. Ranke. "Ammonia.. Physical Properties Models Davis.CH4 ." Englewood Cliffs. M. "Gas Purification... New Jersey: PrenticeHall." Submitted for publication.CH 0H and H2 0. N. Eng. 5. C. Eng.H2 S. . 1980.. F..BIBLIOGRAPHY Rectisol Process Herbert. 2." Houston: Gulf Publishing Company. Mathias.

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APPENDIX A Overall Rectisol Model .

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APPENDIX B Absorption Section Simulation .

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. * J 0-1 0 .c r. o fai~aofazm ) CZ I.C I ' )( -a0 w -tt-r De 00o0o a M Cnt(D vO0 FFrF mm 00 1..i ( . -0 ) 0 coIc C'4IT''. I. * * * .N . 0 cc _..Mm .! 0_-0N NN N" N 'qm C CN M'0MOWW0 LU CN 44 CE 4 4 4 4 ' IV It I t .M C0 rN. w m I" * > 1 . . t.co - 0000000o 0000000ow I- U) )t0 )0 CI C " ~.0 LOQ 1. U1 . . . co 0)0. (n woI W co U( U't V) z C) a...N CI C4C4 .II.-. LU U laLuJ m rv LU 3 . a.Cl 0 r.0.an uzl I .cn C 3 I 0C1C1NC4 o waoD0 0-'-r0 0 40 r-u W(D D(D o 00o ) r-0 ' tD co w r.D .L 3 0 I W Lu Zi z U) CLI a: U.0. 'D 0 ..I t-03 _.~0. " o --II/) U * 3' 0-Jo ... J C~ 1 i) *j o q 2: I-4 00 .ax0 .)' .u 00 Cl U) 0O-C') . . LUJ n. )-i = U) C T 0 0ctL U-I 000000 000000cqCa. mmmmmma Oazom .~ ( . C .o. C..9 (00 . I-. IT C')(x0 I0 .C 0 (0 cl o 0 D 0C O C' 0 0M 0.. .M M .OF 0. i U) .( c-Cl L. W .. LU "-> <4). 03 0 .-- . . * U 0 0) a) I0 . 3 L * * n m i Lu i LL1 0-mCl0 r. 3 2I LU U) : z z :3:s ~ ... 0 * r- Dc0r e. . . ffi m < .tD 0) 0) 0) (0 * MCUOLr INCrCD al * I0o r-w . VI vvvvvvv : CO * 0C0co(Dt. go O- se D LO (D CfQ rOCN Nt LZ a - O m ro 0) 0 tU I. .0.to .. LO-d Oo)M c LL 0 CZ x.- 0 0 a0 * * *x *L z LU 0.0'0 '00)' . - L o _ CZ <aoa Ixz w..m O . . . . 0 ) U) 0 t - .w 0 co co 00 +14 N 01 LU c-O0 o0 .o.wco o mm i oc -i-i m o I I 01 a Ox: = IIIItmx m tcnz LU - mmm-Omo (DD 0 c co .1 . . 4 4 U LU n m 0000000 -NNNNN -ENNNNN L ---- N.N N NCfCi('dN a: 4 Ic) N w UX Dr.o. c 0 z 0 > zI CY cl 0I 0. C'. - - N C N 1 C' Ui t 00 L C4 0!co (D . a: L. C. Z IC a- ~Z NO _ D L.

dLU 3 *Otl (cc(0 4 I 1D-t * Lf C cn v O VWW M mw womom D 0 LnC-MN vw 1 C lOm t-mO M0 * * CI Co ML Cou * Q a. 0. ~ . . 1.0. .Un t. CIICO . b-I ~~ ~ ~ ~ ~ ~ ~ IO~~S ~ ~ OO I X ~ ~ ~~~~~~~~000 ~~ * 'Il Cl~~~~~~~~ *... 0. (7 0) . O 00 :[ -J -JU nr LUI LU -J UL. tD .i . L). 0s w . -J L I- 0 0. .IT F . 0 V to M no O N . Ci.- ~ uMWD M t~---------. . tr 0 L O I. . . 0 aM . .O .J ~. - .LU C.M O-C 00 ~Y 0 * 4 V t ON *. ~ om vr-oma ~ m . ) W (D C Oa <Dcw P) . O . CIW0LflU o a ao-XtD 00OIOC~4 tzDuwc . ~ WOw .) Ix -Ju. -ho z a IL t/2 CZ .-. N NNNNNr )urr0ata . (3 cx *OVOWOMMN--Nmo 4 . 0 CZ 0 .-. .~~~~C 0 ~ ~ ~ . -. 4 uJ 0 z 0 -- * * 4 tcKJ . FC W z 0 z 0 u. . . aU . w uz if a if Lo . 0 0 00 0 0 00 0 0 0000000000 I I I I S I I S I S 0 0 wm o c~w o t O O---------n >O -U) O r-O tD U. CZn.. .*aD .C 0U 4 I- UOLU rO- CO L D - aa 0 0 -s (4 cT U) 4 ~-.

. . U) z U) 0 Z 0 L UJ UU) U) U UC) -i I-.U L LU uJu (z LU rIX C) n. I -4 z W LU U) I.4UJ0 U7 UJ U I C I-. z U) UX F!.(n W U) ~ U1 0 CZIZ Oi U) U) U) .LU 0 C14 0) "I 0 z 0 " Z -i I-..J -C z 0 z 0 U) LU w .Q N J U) W LUU . Ui m I-W9 < Fj Z WO U1 LUX :C I _J ) ..~e4 -J w U) U1 WJlU W W 0 UJ - I-- z U z 0 (0 40 LU ui x U) - .

aU a z 0 I-N '. v) 0 + co . U) 14 ~u' I. 0D3 LU 0 -M z 0 z Lu In CO IX I.04 0 U7 LU " I-03 z LLU 0. c. UE M0 U 4 z 4 LU~- LUI2 ( L U) IX4< I.wC LU LJ 1.LU - .IuJ o WV U)U) LU 03 wLU el 0 0 .O . LUI4 r ( LU 4 .U)= O ..Z LL.i () ~ua = LU 1) A LU 0.LU 4 0. CZ ~ev.:E 0.

z Z 0 I- 000000~0~000'-'. LU I. -J 1-4 U.1. > uL Z LU > .0 LU . 1.jU a 4 . > z 0 U . . 0 m~ 0 C3 -J I 3 3 1 U) uz U) Q~O < .U . LU> Ji O" O OOOO U'- 3 30 :E £1o mwu .3 - z WZN> Z 1-1 0 I-CD - a. c)o o o o o az 0o 0 oo'D 0-06 0 0~ rCr C) o~ Od COOOOOOMQW 0 _ O + OO D UD Go O t 7 C N O C1 in ::CO tl I 0 Z wu z 1w I-i wo0 I-Un Z tn3 0 31.4 0.. _..Z 0 .4 0 z 0 . 0o= ') m *l~ LU z 0 0 LU 3 J I&. .1)Z ( z .. 0 0 I.4 LLIU) U) a LUi LU LL z 0. a: a a a a a: w m c a I- z 0 (U I.4 U) 0I C ZLU~ZLm ' -I 0. 3 I.4 (A IL I.4 m ) IU ) C lI "l W D Cl00I >l @l U)1000Z11001 I-J ( 0 0o . L.O o ? §ot-t- (D +- 0000 _ CI Cl ClD Q -r-It-e) N C IT-M0 C _ ODC14 c O _c LU ( C' nQ-QO z 3 3mZ z 0 3 0 > U 0 LU -Jo( LU LJ > 0000000 c U) 1 000000'q- 0n0 C o o I Z§ ~m go--l'-Cl O 0 ClC)) C. LUJ J. 0000 00m0r-w0000 0C') N 0D O 00 r. 0 -000000000 mmmmmmmmmm 0 ..

APPENDIX E Hot Regeneration Column Simulation .

0 J m > 0 'N. 0CQ O 3 LA..0 ao Z 0 ZJ O Z - \ I In.. 1 (O c i J( UD. 0 I (< 401- n 7 Z W LW I In *C) ID aL 00N.j4 < -4 tv M U< 0-0 CZ'IJ cxw0N. Q Z O @. Q Z 0 > W J I0 U I a Z < Y W 0Z0. O- Z X N. . 0. W ul C V)CI( O O steJ 0. 00 Q NLOCNCWJ II "a I I at 2 a~i .4 ' O -0(d - o -- 11 0u 00 CLX3 I .o C 0l 0 Z tN I oaa 0 Z CP .00. Q Cfwf )uLZ C. I-i 0Z CZLA. U.. Q.C.* U.U I -J Eq(JNb Iw IO I- 0 ~ .0 O-O . a t0 N. 00oN 0 II 3 0.CZ CZl"I Ct -3.Q . 0 C vs0 0 O "I N O Z I X J Qe Z Zc IO Z Z 0 sZ II > eniI 00 0 U ~.1 -)J o -1-U) Ql OU Z 4 0 Z. ')<Z 0 0 o _ 11 0a C-4~~~~~C N0 0> > 0 In :1: I @'ee > I U.. U t 0 () U( IO cL (oc *-.J0 4 N Q0 Z ZO II N If Z ~0 C N 0 I 0 Q I 0 N 00 ( I 0 ~~~N I W0ZD O~ O .) O 0 I w - l i= - Q O~w 0. (Z (O -J w Q<N 0 . .~ # 00 a 0 CY 0 I X > 0 O 1-.-U.0I O LUZ (O U71 u). O 0i-| Z 1-0 0 Z3-1 n. "- 00 7 4 -JO 1-ZZ 0 I Q' - 1 J a1. CY0r0.01 CZ xO cQ' O 1 I > 0 ) CD (A CL Y O1 ix 0 c0 0 w 03 Z3 10.I I 0. "DI 0 < u) 11.

ZZc - 0.. .'- UU'I Z00 . 0** - *u. 0 O0 c .. Ix-Cym 0 W00 -JJ wU.W - -4 L 1 D Z m7 X* *. ~ z~~~~~. W I. o * ) 1oo z L' > 0 z W 0.U.. *U00S* . . Z o ILL U. 0 * .. @-. In . U . * . 0 0: '. WW OX C t3 Jm 0 -*z.LLJ 0.4i co . . . Q W ..... 0W .oo _ c N #oo ooo.4 . . .. .LA - (LFI- Z OW l U L.. 0 Z0043 I-' 0-J U I-.- J OJ U L W 4 0.-~~~~~~~~~~~~~~~~~~~~~~~~z : ~ ~ (A . U *~Jf * > z **xW ZC *- . . ..L U 0I*Z_ Cfl* flV) * 0 0*0 (J > 4 00.. ~ ~ .J c . .I) 0 0-. CO CD. LAC>) :r Z W 0 J@O 0...... . co 0gVV _. z Z /.

W 4.. -j Wm L I-Z~~ 0. O W W I o z O -0W 0 I. o lI0I tJ uJ C3 C tt~ W 0 I I 0. 0 r-t Ln O It oawcq . z 0 0 et'- 0 W LU 3 V) > X 0 L) XY uaIf er~~ InI 0 WL 0Inx _jm? W- c. m W > > Z tl tS 1 "rl ICt u.- 000 CeI.0Z 0- 0 0 0 )N 0000 0 0 0 0 0)Ie Om )Ln o r-w ! 0 0 0 ~'0 M 0 - (a CY)Mn no 0 LO 0)0 *OWU~. YO > t tz rty) . I. .tN-ocoN..~O00 C~ | O.q.. 0.U..0 N04 aY) IT qq00-- 4'.. I-- 0 I- 4 CZ -Wq 'q" . . . C*e I CN 04N N-0- 000 .Z?5.c. !co 00O CN NtlD N N C. Ot0)0 W00 Oz 0 ZZ0 < 0... zt Z O 0 In Wm I- I-r zIU 31 > W .O 0 CN(N 00 '88 0 I 0 0 C O0M M . Ck' o U. WAJ 0. . Z I - OO=m 00 I-CZ z"WIn :L) 1t CN 0 I O U U Z~I O O 0 ~ 0. cot~ N .co ' 'N CNCe4C JCN..t 'OI I 0..'N 1'. (a I-.._o_ I .. -C U.-J C . . Z ~z 4 -x J - i. flI .uJ NZ Lt 4 I - OI I IY In I IIY I- *M *-00 izJJ . . . coIfn LO I an " 0 (N . t.-0 J cD. t Co ~o I . p qD'qI I I I 0 w m- _ ~O C Ct I a0 I I.. I. J W n 3: ) 0 NN( ) (DO Ie IL . (N N N1 v.C_. I I-N7 OW t i-I t/I 0O 3 -J m W 00Cm "0000 0 + 0 Ifl c 0 0 Iz .1 4 t?)I aJ . L~ l I- U C- *Y *U z 0 > z 0 W Z a. I 3 -J O 4.<c/ tA 0 oO O0 N o.. tx W ca: nun I 0OOI > _ IW zt Z C t0t ^ Z 0 II Int et In 3 O 0 * - 4 zt I O ~ CZ ui Z 0. .

a Z LU 0.)3 0 Zw1 - QOOZ I I Z 0N O .4 o0 w LAJ 4 - ZZ 00 I-.< Z 0 0. 0 i. . C LA WU O Z WWO.tO O .a.4 . . . . )U)UU)U) U)U)0U U UUU))UUU)) ~z W~~ s tn E:E~ mL I^. .t >fiM OY . W O E _0 C400 0O I C( e IClCdN(OzDI tDO U)0OIC' I :> QF-t U) 1W U)1 0 F.W 4L F-_FW W cox01 4U Ln UiLJ U)U) _ 40 W E x0ICNCNCrd O000Z100 I TM( 1 = MOO C )0I I ~~D0 -. U.- -e. UJ. . U) . -~<ZZZZZZ z ~~ 0 UW ZZZZZZZZZ CNOC zK - - W Z o Z U uj WI 0 V) X o 0.U 2 V) z 4 FZ U) >000000000 F- a. .NW U.LJj O .Y ILIO . .

. 0 0 4 LI) 3 n n(n nxIO4 (A 0 S:n 0n (An U) >YXSO>Uy n X>-IOO~j>-n> j zm YY OC wx=> . Y a 0 I I '-I>-. CO. 0 0 . Wj C. U) X X X X X X X X X x X X C C J. I En y > U.) OX 0.-.X 0. O 0.4 >S ~.(N 0~00 000 0 N C C oAx x In 0 0.. WI- 0 C 2' (n :> _j > j > _j > _j M 0 . 1 u) XX 0a~no>>JZxXX> X -J U. 0. In _J C ix NU W X O O O x x sX XE O >OOC x C = X Yx E y o g N 4N.J w I . I. a V) 4 0. I 3 C9a oj X -r>- 0000 00888> Wi > V : o Xu) X " O O O O O > -J .I fn(n Vn n n U ) n n n y y n Qi 3 CDin > .1 X -.n> 0(OH > 0.x U n -(0) . 0. %y) W z W ..4 Li z 0 Cl I-. . 0 0 0 xx 0004X40 000 0 0 X0J0 -OQ x O° (N o0 z u) C z C..JUJ i-. 0z Wn 0. 0..4 - xxxxxxxxxxzxxxxJ II O>>sz > X> xxoo-i I X X I ww . m X(9 9 Vnt > > S z Y > xC9-4 0. 0 8 -J W z 0 I- 0 0 8 0 30 0 . 4 0. aD 0 O I- X x Zx 'N (N *> -j 2 z Yf 000w (n> > .4m 3X 0 UX sX IV : z 0 z 0 X > j -X -j P.. 0 'a0' I9 9 I .. 0.C.

on C C) t (fSl I UZ0DCD IZlLL WQ aaa0 * * zh CZ . 0 F F.LO O co . 4 . 0 0. .r- w wwN 0I tD _T 0 N 0 . _ 0 0 0 0 + 0 1fl . O 00 . .< W Q 0 >tO 0 0 > t tJZ Ic ) IC.*ig20m o8 o8 . z NO WU CI O I C Nj N C O V)c nOCD o oW NI< s.C*0o) 0C'C' q'in|c 40 N N4 O Un <Z NO -r 0co oLO .) -J z 0 UJ I- 41-F c LU OW| l.. UU tY iIm 0 i 0 i -C 0 * z o *0 * z 00 o I 0'. I tO ( 0 . 0 C. CZ I-I I I1 W C L LLO ~ I o 000 z O .C'3 0 z 4 -J .- v r.-J ~-Z 0 > I- z4 0 Iz U) Z "W I- ~ 0. . * IUU Z W2 z :E. 000 .-M .J C4CN4i .W CD 4 . O~ O N 000 00 u' tOO_ * LO -0co . UL Q 0 W o 0 I.L 4 0 OON O 0 Cn 0 U U) IT 0 0 cn + L U -N Cl 0 4 O UJ CD tl 0 t uj LAJ O co 0 0 u 0'J 000*C' C N0 Z^ -' 0 O tDS tu UUtJ S W tJ '-0 ~ ~~~~ z 4 -j I 0 . = 0 Q :2 _- II < 0 zI u .

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APPENDIX F Water Wash Column Simulation .

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