A mathematical model for equilibrium solubility of hydrogen sulfide and carbon dioxide in aqueous

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A mathematical model for equilibrium solubility of hydrogen sulfide and carbon dioxide in aqueous

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SOLUBTLITY OF HYDROGEN

SULFIDE AND

CARBON DIOXIDE IN AQUEOUS

ALKANOLAMINE

SOLUTIONS

R. D. DESHMUKH* and A. E. MATHER

Department of Chemical Engineering. University of Alberta, Edmonton, Alberta, Canada T6G 2G6

(Received 3 April 1979: accepted 26 June W80)

Abstract-A thermodynamic model is proposed for the solubility of the acid gases (H,S and CO,) in alkanolamine

solutions. The model is based on the extended Debye-Hiickel theory of electrolyte solutions. Predicted partial

messures of the acid gases over monoethanolamine solutiom are in good agreement with experimental data over

;he temperature rangeZ-INPC.

PiTItODUCTlON

removal of the acid gases (H2S and CO*) from natural

gas, synthesis gas and refinery gas streams. Processes

utilizing alkanolamine solutions are usually classed as

chemical processes because of the reaction of the acid

gases with the weak bases formed by alkanofamines in

aqueous solution. These processes have the advantage of

being able to reduce the concentration

of HzS and CO,

to tow levels, even if the gas stream is at a low total

pressure. The characteristics

of chemical gas treating

processes

have been discussed

by Richardson

and

OConnell [l]. For the rational design of separation processes, a knowledge of the equilibrium sotubility of the

HZS and CO, in the alkanolamine solution is necessary.

While solubility data for a number of atkanolamines have

been published, the range of temperatures,

partial pressures and concentration

of atkanolamine is so great that

a method of correlation of the solubility data is desirable

for extrapolation and interpolation.

SOLUBILITY MODEL

COJethanolaminelwater

systems was made by Mason

and Dodge[2]; although the method was not described, it

apparently was a curve-fitting approach. At that time the

reactions between alkanolamines and carbon dioxide had

not been studied. Van Krevelen et a!.[31 developed a

method for the prediction of the partial pressures of HzS

and NH, over aqueous solutions. They use pseudoequilibrium

constants

which do not contain activity

coefficients

and relate these pseudo-equilibrium

constants to the ionic strength of the solution. This study

was successful in representing the ammonia-rich region,

but was not useful for the complete range of concentrations. Danckwerts and McNeil141 used this approach

to predict the equilibrium partial pressure of carbon

dioxide over carbonated

amine solutions. The central

feature of this model is the use of pseudo-equilibrium

constants and their dependence

on ionic strength. The

most serious limitation of this model is that the ionic

*Author to whom correspondence should be

addressed.

constants.

Kent and Eisenberg[5] have recently used a modification

of this method to correlate equilibrium solubilities in the

C02/HzS/aminelH20

system. They tried to correlate the

sotubility data using published equilibrium

constants

without any dependence on ionic strength. It was found

that the predicted values deviated significantly from the

experimental

values. Instead of using ionic characterization factors for the dependence

of the pseudoequilibrium constants on ionic strength, they accepted

the values of all but two pseudo-equilibrium

constants

and treated these two as variables to be found by fitting

experimental data.

Atwood d a1.[6] proposed

a method for the catculation of equilibria in the HtS/amine/HZO system. The

central feature of this model is the use of a mean ionic

activity coefficient. The activity coefficients of all ionic

species are assumed to be equal. This assumption is good

at low ionic strengths or if only one cation and one anion

are present in significant amounts. However,

this is

generally

not the case for the COJHzS/alkanolamine/Hz0

system.

This model was utilized by

Klyamer and Kolesnikova[7]

for the COz/amine/H,O

system and was generalized by Klyamer et ai. [S] to make

it applicable to the C02/HzS/amine/H20

system. If the

activity coefficients in the Klyamer et al. model are set

equal to unity, the model is algebraically equivalent to

the Kent and Eisenberg

model. Comparisons

of both

models with experimental data obtained ifi recent years

have been made in papers

by Lee et n1.[9, to].

Differences between the predicted partial pressures and

the experimental

values often were as high as 100%. It

appears that an improved model is necessary for quantitative calculation of the partial pressures of the acid

gases over alkanolamine solutions.

The thermodynamic

framework is based on two types

of equilibria: dissociation of electrolytes in the aqueous

solution and the vapor-liquid equilibrium of the acid gas

species. The dissociation is expressed by the dissociation

equilibrium constant:

K = na,pi

(1)

356

R. D.

is given by:

equilibrium

DESHMUKHand

&YiP = ~$PQHi.

For the solvent,

given by:

water,

(2)

the vapor-liquid

equilibrium

is

MATHER

used up in these reactions. The alkanolamines have two

active groups, viz. -NH2 and -OH. On account of this

bifunctional nature of alkanolamines, the following reactions are possible:

RI-OH + OH- = RI-O- + Hz0

&Y,P

= y;z, fu.

(3

that the activity coefficients

approach

unity in an

infinitely dilute solution. The reference state is that of a

hypothetical ideal solution of unit molality. On the other

hand, the activity coefficient of the solvent approaches

unity as the mole fraction of water approaches

unity.

The reference state is that of pure water at the system

pressure and temperature. Equations (lH3) describe the

conditions

for equilibrium in an aqueous solution in

contact with its vapor. To use these equations to predict

the equilibrium composition, information about Q and y

for atl the components present in the system, as well as

the Henrys constants and equilibrium components

are

required.

The main reactions

occuring in the CO#I&alkanolamine/H20

system are as follows:

Ionization of water:

HZ0 = H + OH-.

Dissociation

A. E.

of hydrogen

(4)

R,-O-

= R&-COO-.

the amount of products is negligibly small (Jensen ef

&.[I 11). Astarita et ~I.[121 report that these reactions

take place only in a basic solution where pH is II or

greater; these reactions can be neglected as the pH of

even a slightly carbonated solution is less than IO.

The chemical reactions 4-10 are accompanied

by the

vapor-liquid equilibria of the volatile species.

Free amine may also be present in the vapor phase.

Under the conditions of interest, the vapor pressures of

the amines are very small and we can assume that the

amine is present only in the liquid phase. The thermodynamic framework enables us to write the equilibrium relations among the reacting species. These equations are as follows:

K, = y(H)y(OH-)m(H+)m(OH-)/a,

(11)

KW = r(H)y(HS-)m~H)m(HS-)/y(H~S)mlH2S)

K,,

sulfide:

+COi

(12)

= y(H*)y(HCOj-)m(H)m

(HC03-Mr(C02)m(C~,)a,

H&Z = H + HS-.

Dissociation

(5)

Ki = r(RRNH,)y(OH-)m(RRNH*)m

of carbon dioxide:

(OH-)lr(RRNH)m(RRNH)a,

(6)

of alkanolamine:

Kzc = y(H)rtS-)m(H)m(S)ly(HS-)m(HS-)

Formation

(8)

= H(CWy(CWm(C9)

(19

MWGY(H2S)P

= H(H&)y(H&m(H&

(19)

of bicarbonate

HCO,-

4uYwp = (P!u)pa,.

(9)

ion:

= H + CO,-.

(10)

alkanolamine. Tertiary amines (TEA and MDEA) lack the

extra hydrogen atom and do not form carbamates

by

reaction 8. In addition to the reactions 4-10, other reactions

maytakeplaceinthesolution.Theaminesreactwithcarbon

dioxide to form heterocyclic compounds. The amines may

react with impurities in the sour gas such as carbonyl sulfide

andcarbondisulfide.Thesereactionshavelittleeffectonthe

(17)

W02MC02P

of bisulfide ion:

HS- = H + S-.

Dissociation

(16)

(CO,-)lr(HCO~-)m(HC09)

+ H.

(15)

KY = rW)r(C03-)m(H)m

of carbamate:

(7)

(14)

KA = y(H+)y(RRNCOO-)m(H+)m(RRNCOO-)ly

(RRNH)y(COZ)m(RRNH)m(COZ)

Dissociation

(13)

(20)

In this work the activity of the water, a,, has been set

equal to its mole fraction, since in most instances the

liquid phase is predominantly water. As well as the effect

of pressure on the fugacity of pure liquid water has been

neglected.

Equations

(llH20)

describe

the thermodynamic

equilibrium

in the COz1H2S/aminelFL0

system.

The following balance equations for the reacting species can be formed:

Electroneutrality:

m(H) + m(RRNHz)

+ m(HC03-)

= m(OH-) + m(HS-)

+ m(RRNCOO-)+

2m(S)+

2m(C%).

(21)

357

Mass balances:

tnA = m(RRNH) + m(RRNH2)

+ m(RRNCOO-)

(22)

+ m(C03)

+ m(RRNCOO-)

(23)

124)

m&H&

PeneRobinson[28]

equation

of state. The activity

coefficients take into account interactions between solute

species in the liquid phase. In this work, the extended

Debye-Hiickel

expression given by Guggenheim[29] has

been used to obtain yk:

is determined by titration (also called the stoichiometric

concentration)

and n(C0,)

and a(HzS) are the mole

ratios in the liquid phase (carbon to nitrogen and sulfur to

nitrogen). These ratios are the usual experimental values

which are obtained in solubility experiments.

The equilibrium constants and Henrys constants needed

for predictionof theequilibriumcomposition

were obtained

from the literature where possible. The references are given

in Table 1. It should be noted that the most reliable

measurements

of the dissociation

constants of the alkanolamines

are those of Bates and coworkers.

They

report acidic dissociation constants, KbL. These are related

to the basic dissociation constant, Ki,usedhere by the

equation:

the Debye-Hiickel

law and

represents

the electrostatic

forces. The second term

takes into account short-range Van der Waals forces.

The quantity A is related to the dielectric constant of the

solvent and b, may be considered a constant. Edwards et

a/.[301 used eqn (26) in their model for correlation of the

equilibria in dilute solutions of NH1, COZ, HzS, SO2 and

HCN in water. The interaction parameters in eqn (26),

show

a weak dependence

on ionic strength

AJ

(Scatchard[31])

and temperature

(Edwards et al. [30]).

The interaction

parameters

for all pairs of species

present in the mixture must be known to estimate

activity coeficients.

Edwards et al. [30] used a procedure

described by Bromley[32] to estimate some of the interaction parameters.

This procedure

cannot be applied

system since the

Ki= KJKbh(25) directly to the C021H2S/amine/H20

parameters needed (entropies of the ions and salting-out

coefficients) have not been determined for all the species

Values of Kbh for DEA and TEA have also been

present in this system. In the next section the method

reported[l7,

181, but only over the temperature

range

used to estimate these interaction parameters

will be

b5oC.

described. Pitzer[33] has proposed

a more accurate

Equilibrium

constants

for carbamate

formation

in

expression

than the extended Debye-Hiickel

equation

MEA and DEA solutions are available only at 18C.

for activity coefficients and this equation was used by

Jensen ef nL[ll] used the Bjerrum expression to calEdwards et al.[34] in extending their previous work to

culate the equilibrium constant. McNeil[f9] studied the

more concentrated

solutions.

Beutier and Renon [35J

same reaction, but used a different method to anafyse his

have also used Pitzers expression to calculate the equilresults. For moderate degrees of carbonation,

the caribria

in the

NHnlC02/H20,

NH3/H2S/H20

and

bamate is the main product of the reaction and it is

NH,/S02/HZ0

systems.

Even though the reactions

unfortunate that this key reaction has received so little

occuring in these systems have been well-studied, Beuattention from researchers.

Table I. Source of dissociation constants

Variable

%

RlC

RlY

KiWEA)

Temperature

K2Y

RC02

H-S

Henrys constants

Range

Reference

O0

- 150 %

olofeson

00

- 250

Rao

25O

- 250

"c

Read

O0

KAWW

K2C

and

25O

00

and

Bates

I ac

Jensen

- 150 %

uyukov

Oc

Hepler

and

O0

- 350

- 330

DC

"c

b3]

p4)

Warned

Pinching

et

al.

et

al.

US]

(111

[203

Scholes

Strafelda

c21

@ 2I

I?31

and

Cuta and

Ryzhenko

O0

Kepler

b5]

- 50 *c

- 300

and

Zel'venskii

Ellb

P 2;

Lee

@7]

and

Mather

R. D.

358

DESHMUKH and

the interaction

parameters

to render the expression

manageable. It appears that Pitzers expression is too

complicated for use in aIkanolamine solutions given the

present knowledge regarding the reactions occurring in

the solution.

MGTHODOF

!ZOLUTlON

Twelve species exist: HsS, CO*, RRNH, HS,

S,

HCOI-, COa, RRNHz+, RRNCOO-, H, OH-, H20.

Hence there are twenty-three

unknowns (mi and ri) for

all species and the mole fraction water. To solve for the

unknowns,

there are twenty-three

independent

equations: seven chemical equilibria, three mass balances,

electroneutrality,

the use of eqn (26) for the eleven

activity coefficients and the vapor-liquid equilibria. The

problem is one of solving a system of non-linear algebraic equations. Browns method [36,37] was chosen

for this purpose. It is an efficient procedure which is

baaed on a partial pivoting technique, The successive

substitution nature of Browns method is analogous to

Gaussian elimination in linear systems of equations. To

obtain fast convergence with Browns method, the variables and the functions are normalized so that they are

all of the same order of magnitude. The molalities and

the partial pressures in the C0JH2S/amine/Hz0

system

range over several orders of magnitude. To normalize the

variables, the equations were formulated

in terms of

their logarithms. The functions were normalized so that

the convergence criteria could be expressed as If(x)1-CE

where c is a small positive constant. For example, eqn

(I I) was normalized by writing it as:

f, = 1 - y(H+)y(OH-)m(H+)m(OH-)IK~,.

(27)

manner. A FORTRAN program for the calculation of the

equilibrium compositions

was written, The sequence of

calculations is as follows:

(1) The temperature, concentration

of the ,amine. and

either the acid gas partial pressure or the acid gas mole

ratios in the liquid are specified.

(2) The equilibrium constants, the Henrys constants,

the dielectric constant of water, and the binary-interaction parameters are calculated.

(3) A preliminary solution is calculated by setting all

activity coefficients and fugacity coefficients equal to

unity.

(4) The preliminary estimate is refined using Browns

method for the solution of the system of non-linear

equations.

(5) The equilibrium composition

is determined

from

the converged solution.

In the COJH2S/alkanolamine/Hz0

systems, the direct

prediction of the equilibrium composition is not possible

since some of the equilibrium constants and the specific

interaction parameters are unavailable. These parameters

can be obtained by least squares fitting of experimental

data.

&,I be the array of the interaction

I-etB=[/%.B*.....

A. E.

MATHER

errors in predictions.

We wish to find the interaction

parameters

B* that minimize

s = IEI. When s is

minimum,

a$afii=O,

i=1,2

,...,

44.

unknown Bs, However, such a procedure is not feasible

because of the excessive computational effort involved.

To simplify the calculations, the following assumptions

may be made.

(1) The-interaction

parameters for the species which

are present

in very small concentrations

can be

neglected.

(2) The effect of the Bs on the errors in prediction is

assumed to be additive.

When a certain chemical species is present in a very

small concentration,

it has little effect on the equilibria.

The concentration

of that species may be neglected from

the balance equations. A reduced set of equations can be

solved in terms of a smaller set of variables. For example, if S is present in a very small amount, its concentration can be ignored from the charge balance and the

sulfur balance equations.

The equations

(except the

equilibrium relation for the dissociation of the bisulfide

ion) can he solved for the variables (excluding S-).

Secondly, the term &jmf in the extended Debye-Htickel

theory may be neglected if nt, is small.

The additivity assumption implies that the total deviation in predictions may be expressed as a sum of the

individual deviations

due to each of the interaction

parameters.

Let p be the predictions

using B=

[0, 0,L. _,03 and let P be the measured values. Therefore,

I? = P - p is the total error. The effect of the interaction

parameters can be found by setting jth parameter to a

small number, say A& Let the new predictions

be

P(A&). This means that setting the jth parameter to A/3,

has caused a deviation of [P(A&) -m in the predictions.

If 6s are small, this deviation is proportional

to the

magnitude of /3; i.e.

PO3j)- FIIS, = D%W,) - PllW,

Define C, = [P(A&) - P]/A& Since the total deviation

the sum of the individual deviations,

CT = c

is

B,C,.

CT =X.B

where X = [C,, C2,. . . , C,]. We wish to find B so that CT

is the best estimate of &, i.e. we wish to minimize the

squared error q = IJ!? - CT\*.

q =

(EO-CTy(E?-cCT).

Substituting CT = X . B and expanding

349

loo00

aq/a& = - 2IXEY

+ 2IXXB.

loo0

:. XXB = Xti

I

B

g

loo

B = (XX)-X@.

c

LL

using the computer program described above. The

method can be extended to determine the equilibrium

constants outside their range of measurement. Define

K = K. exp 6 The exponential function is used to ensure

that K is always positive. Given an initial estimate of K,

f can be determined by the least squares fitting as

described above.

AP?LICATtON TO MONOETHANOLAMINE (MEA) !XUlTIONS

hampered by the lack of information regarding the

specific interaction parameters for monoethanolammonium ions and carbamate ions. As well the equilibrium

constant for carbamate formation is available only at

WC and the equilibrium constant for the dissociation of

MEA is known only between

0 and 50C. In the

COJHtS/MEA/HtO

system, the only species which are

present in significant concentrations are the free amine

and the monoethanolammonium,

carbamate. bicarbonate

and bisulfide ions. This means that the interaction

parameters for the other species (CO,, H& OH-, H+,

S and CO,) will have little effect on the observed

equilibria. However, at very high loadings, the concentration of the free CO2 and free HIS are also high. The

important interaction

parameters

are /3(RNHTRNHz).

/3(RNHrRNHCOO-),

B(RNHrHCO,-),

@(RNHr

HS-), /3(RNHz-RNHCOC-),

@(RNH,+-HCO,-)

and

p(RNH*-HS-)

where R = -CH,CH,OH.

The first of

these can be determined from the correlation of Atwood

et a1.[6]. It should be noted that there are no mixture

parameters

in the list. The parameters for the

COJMEA/H20

system and the H2S/MEA/Hz0

system

are

sufficient

to predict

the

equilibria

in the

C0,1H2S/MEA/H,0

system and hence the parameters

may be determined from data for the three component

systems.

The partial pressures

of HZS over 2.5 N and 5.0 N

MEA solutions at 25, 40. 60. BO, loo and 120% have

been reported by Lee et al.[38]. These data were used to

determine

/3(RNHrHS--).

fi(RNH2+-HS-)

and the

equilibrium constant for the dissociation of MEA at

IOWC. Figures 1 and 2 show the comparison between the

predictions and the experimental data. The agreement is

good for both 2.5 N and S.ON MEA solutions at all

temperatures.

Thepartialprersuresof

COzover 1.0 N,2.5 N.3.75 Nand

5.0 NMEAsolutionsat

25,#,W,W.

1Wand 120C have

been measured by Lee et al. [lo]. The equilibrium constant

for carbamate formation at WY!, as well as the fi(RNH,

t

2

(I)

10

1.0

0.1

0.2

0.1

0.6

0.8

1.0

1.4

a.*

Fig.

10000

I.

t

,.;t

0.2

( ,

01

Ratio

, ,

0.8

06

Mole

10

in Liquid,

1.2

1.4

H&MEA

Table 2. Specific interaction parametersfor MEA

kg/mole

B(RNtlt- HS-)

~CRNH,+

B(RNHt

w-1

URNH*

HCO,-)

Rt4~~00-)

0.0375

0.005

liCO,-)

B(RNH*+-

BIRN~+

RNHCOO-)

0.0245

0.0375

0.063

0.006

R. D. DE-SHMUKH

and A. E. MATHER

3&l

HCO,-1, fi(RNHz+-HCOs-),

fi(RNH,RNHCOO-)

and

,9(RNH,-RNHCOO-)

were determined from these data.

The interaction parameters which were obtained from the

dataon the three-component

systems are presented in Table

I. Figures 3 and 4compare some of the predictions with the

experimental

data. The agreement is good at all temperatures and normalities. The agreement shown on Figs.

14sameasureofthegoodnessof

fitofthemodel,sincethe

parameters were obtained from the experimental data.

The partial pressures of mixtures of CO1 and H2S over

Lee et al.[9] in 2.5.N solution and by Lee ef al.[39] in

5.0 N solution. The parameters obtained above were used

to predict the equilibria for the mixtures of CO, and H2S

in the MEA solutions. Figure 5 illustrates the effect of

CO, on the solubility of H2S in the 2.5 N MEA solution

at lWC, while Fig. 6 shows the reverse. Similar plots for

the 5.0 N solution at 100C are presented in Figs. 7 and 8.

On the whole, the agreement of predicted partial pressures with experimental values is much better than that

10000~

wooo

lax,

B

f

100

F

g

10

1.0

0.1

0.2

0.4

0.6

0.8

1.0

1.2

1.4

0.2

0.4

MOle

solutions.

0 6

0.8

Ratio in Liquid,

1.0

1.2

1.4

H.$VMEA

solutions at 100C.

1OOW

loo00

1WO

1000

s

f

2

-r

f

d

g

i!

0.

z

h

N

100

100

h

N

8

10

10

1.0

1 .o

0.10

0.1

0

0.2

0.4

0.8

I.0

12

1.1

02

0.4

0 6

0.8

1.0

1.2

1.4

solutions at 100C.

0.2

0.4

Mole

Fig.

Q.6

Ratio

0.8

in Liquid.

1.0

I.*

1.1

Mole

H@/MEA

F&

8.

solutions at IOLPC.

of models proposed previously. Generally, the predictions tend to bracket the experimental

data. At hiih

loadings, the agreement is poorer and the predicted partial pressures are lower than the experimental

values.

This suggests that interaction parameters such as p(COr

HS-) and /3(H&HCO,-)

become important at these

conditions.

Directions for improvement

of this model

include the use of parameters involving COz and H,S. To

determine

these parameters.

equilibrium data for the

C0JH2S/Hz0

system

would

be needed.

Reliable

experimental data for the carbamate formation equilibria

would also be helpful to predict sotubilities over wide

ranges of temperature.

Ackmwledgemenf-This

work was supported

Research Council of Canada.

361

by the National

X

Y

Ratio

in Liquid.

COzlMEA

solutions at IOOV.

vector of deviations

mole fraction in vapor phase

charge on an ion

Greek svmbols

mole ratio in the liquid phase, moljmol

specific interaction coefficient in extended

Hiickel equation

activity coefficient

a small perturbation

a small tolerance

stoichiometric

coefficient

product

summation

fugacity coefficient

Debye-

Subscripts

NOTATION

:

B

C

E

Ii

I

I

K

m

P

P

:

B

X

activity

constant in Debye-Hiickel

equation

vector of /3s

vector of deviations in predictions

vector of errors in predictions

Henrys cpastant, kg Pa mol-

ionic strength = 0.5 Z miz?, mol kg-

identity vector

equilibrium constant

molality, mol/kg solvent

pressure, partial pressure, kPa

vector of partial pressures

squared error

gas constant, J mol- K-

squared error

temperature, K

mole fraction in liquid phase

bh

i

i

A

w

IC

2C

1Y

2 I

component i

dissociation of amine

carbamate formation

water

ionization of hydrogen sulfide

dissociation of bisulfide ion

ionization of carbon dioxide

dissociation of bicarbonate ion

Superscripts

0 reference state

0 base case, fi = 0

REFERENCES

Pmt. Lks. Lkv. 1975 14 467.

[21 Mason J. W. and Dodge B. F., Tmns. A.I.ChE. 193632 27.

R. D. DESHMUKHand A. E. MATHER

362

Rec. True. Chim. 1949 68 191.

[4] Danckwerts

P. V. and McNeil1 K. M.. Trans. Inst. Chem.

Engng I%7 45 T32.

Proc. 1977655(Z)

[51 Kent R. L. and Eisenberg B., IJydrocarbon

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