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Chemical Engineering Science 62 (2007) 7336 – 7343

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Surfactant adsorption onto activated carbon and its effect on absorption with
chemical reaction
Marius Rosu, Anita Marlina, Aydin Kaya, Adrian Schumpe ∗
Institute of Technical Chemistry, Braunschweig University of Technology, Hans-Sommer-Str. 10, 38106 Braunschweig, Germany

Received 21 April 2007; received in revised form 14 July 2007; accepted 12 August 2007
Available online 19 August 2007

Abstract
The effects of surfactant contaminations and activated carbon addition on physical gas absorption, and absorption with fast and instantaneous
reaction (sulphite oxidation, carbon dioxide absorption into sodium hydroxide and monoethanol amine (MEA) solutions) have been studied in
a stirred cell with a flat gas/liquid interface. Surfactants significantly decrease the liquid-side mass transfer coefficient kL even at very small
concentrations. The surfactants can be removed by adsorption onto activated carbon (“surfactant grazing”).
In absorption with fast chemical reaction of the gas (sulphite oxidation), the liquid side mass transfer coefficient kL has no effect on the
absorption rate and, consequently, there are no effects of surfactant and activated carbon. CO2 absorption into sodium hydroxide solution may
occur in the instantaneous absorption regime; then, any change in kL causes a proportional change in the absorption rate. In CO2 absorption into
MEA solution, however, in the instantaneous regime, much stronger effects of surfactant and of its removal by activated carbon are observed.
It is suggested that in the absence of surfactants surface convection (Marangoni instability) may occur in MEA solutions.
䉷 2007 Elsevier Ltd. All rights reserved.

Keywords: Absorption with reaction; Marangoni instability; Surfactant; Activated carbon slurry; Stirred tank

1. Introduction Very strong particle effects have been reported for stirred
cells with a plane gas–liquid interface. Small activated carbon
Sharma and Mashelkar (1968) were the first to report an in- loadings in the range of 0.1–2 kg m−3 have been found to in-
crease in the mass transfer rate in a bubble column by small crease the liquid-side mass transfer coefficient kL in water or
particles. Similar effects were found later by Kars et al. (1979), aqueous solutions by factors of 2 to 3 (Kars et al., 1979; Alper
Alper et al. (1980) and many other researchers (Lindner et al., et al., 1980; Tinge and Drinkenburg, 1992; Ruthiya et al., 2003).
1988; Wimmers and Fortuin, 1988; Quicker et al., 1989; Vinke This “physical enhancement” effect was usually explained by
et al., 1991, 1993). Reviews on how suspended solids can affect an additional adsorptive transport mechanism. The particles
the gas–liquid mass transfer have been given by Beenackers were assumed to adsorb gas at the interface and release it in
and van Swaaij (1993) and Nedeltchev and Schumpe (2007). the liquid bulk (“shuttle” or “grazing” effect). With this model,
High solid loadings lead to high effective viscosity resulting in however, the strength of the effect and the levelling-off at a low
lower values of kL and a (Schumpe et al., 1987a). High load- critical particle loading cS∗ are not easy to explain. Holstvoogd
ings of non-wettable solids may block the interface (Schumpe et al. (1988) have calculated that extremely high activated
et al., 1987b). In non-coalescing liquids, e.g. concentrated salt carbon concentration at the interface, as compared to the bulk,
solutions, fine activated carbon particles may hinder bubble co- was necessary to quantitatively explain the effect. Kaya and
alescence and significantly increase the specific interfacial area Schumpe (2005) have shown that, in a stirred cell with plane
(Lindner et al., 1988; Kluytmans et al., 2003). gas–liquid interface, higher mass transfer coefficient kL can
also be induced by solids with virtually no adsorption capac-
ity for the gas. Rather, some hydrophobicity is required so
∗ Corresponding author. Tel.: +49 531 391 5365; fax: +49 531 391 5357. that surface-active contaminants are adsorbed on the solid and
E-mail address: a.schumpe@tu-bs.de (A. Schumpe). removed from the gas–liquid interface (“surfactant grazing”). It
0009-2509/$ - see front matter 䉷 2007 Elsevier Ltd. All rights reserved.
doi:10.1016/j.ces.2007.08.027
M. Rosu et al. / Chemical Engineering Science 62 (2007) 7336 – 7343 7337

Table 1
Gas/liquid/solid-systems for which a particle effect on the absorption rate was reported

Gas/liquid/solid system E cS∗ (kg m−3 ) Authors

O2 /glucose soln/Pd-C 2.5 0.4 Lee and Tsao (1972)


CO2 /carbonate buffer/C ≈3 2–3 Alper et al. (1980)
≈2 0.1 Quicker et al. (1987)
O2 /Na2 S soln/C 3–14 6–16 Pal et al. (1982)
3 2 Alper (1987)
O2 /Na2 SO3 soln/C 3 1.5–2 Alper and Deckwer (1983) and Alper and Öztürk (1986)
H2 /nitrate + phosphate soln/Pd-C 2 1 Wimmers (1987)
2–3 0.2 Vinke (1992)
H2 S/I− + I2 soln/sulphur 2–8 ? Mehra and Sharma (1988)
CO2 /water, alkanolamine soln/C 2–9 6 Saha et al. (1992)
H2 S, C2 H2 /FeCl3 2–4 ? Wubs and Beenackers (1994) and Demmink et al. (1998, 2002)
HEDTA soln/sulphur, C

E = enhancement factor, cS∗ = critical solids concentration, C = activated carbon.

is generally recognized that surfactant can be adsorbed on ac- 13 and 73 mm from the bottom, one in the liquid and the other
tivated carbon due to hydrophobic interactions (Svitova et al., in the gas phase. The liquid or suspension volume was kept at
2001; Levitz, 2002; González-García et al., 2004). In a carefully 350 ml. At stirring speeds N up to of 80 min−1 a flat surface of
cleaned (surfactant-free) system, Kaya and Schumpe (2005) the liquid was maintained. The absorption of oxygen from air
found no effect of activated carbon. Rosu and Schumpe (2007) into sodium sulphite (or sulphate) solutions and the absorption
have shown that, for different gases, the effect is independent of pure carbon dioxide (or nitrogen) into sodium hydroxide
from the strongly differing adsorption capacities of activated solutions have been investigated in reactor A at 298.2 ± 0.1 K.
carbon for the respective gas. Kordač and Linek (2006) also Reactor B (Fig. 1b) was a 600 ml steel autoclave with an inner
confirmed the interpretation as “surfactant grazing” by study- diameter of 63 mm. Two six-bladed stirrers, the blades inclined
ing the diffusivity effect on kL . at 45◦ , with 30 mm diameter were mounted at distances of 20
Also for reactive systems enhancement by the addition and 80 mm from the bottom. The liquid or slurry volume was
of activated carbon has been reported by many investigators 332 ml. The surface remained flat up to the stirring speed N of
(Table 1). Sometimes high critical solid concentrations cS∗ and 200 min−1 ; only beyond 600 min−1 the gas would be dispersed
higher enhancement factors are found as compared to the case into bubbles. The absorption of pure carbon dioxide (or pure
of physical absorption. How does this fit into the “surfactant oxygen) into sodium hydroxide (or MEA) solutions has been
grazing” mechanism? In this study, the effects of surfactant studied in reactor B at 293.2 ± 0.1 K.
and activated carbon on absorption with fast and instantaneous Carbon dioxide, oxygen and nitrogen had a purity of
reactions were studied to find an answer. 99.999%; filtered air was used for the oxidation of sulphite. The
powdered solids used were activated carbon (dS : 3–170 m;
2. Experimental Riedel–de Haën) and graphite (synthetic; dS : 1–2 m; Aldrich).
Double-distilled water was used. All chemicals (including
In addition to physical absorption, three different reactions MEA) were of the highest available purity. In reactor A, differ-
have been carried out in the presence and the absence of sur- ent sodium hydroxide purities (99.998% and 98%) were used
factant and activated carbon, respectively: for comparison but gave similar results.
For the determination of kL for oxygen in reactor A, dynamic
• Absorption of oxygen from air into 0.8 M sulphite solution physical absorption into 0.8 M sodium sulphate solution was
catalysed by cobalt sulphate (0.5 × 10−3 –2 × 10−3 M). employed. Any dissolved gas was first desorbed by evacuation.
• Absorption of pure carbon dioxide into 0.5–2 M sodium hy- Then a flow of filtered air was led through the head space and
droxide solutions. the stirrer was started. The slow increase in the liquid phase
• Absorption of pure carbon dioxide into 0.1–1 M monoethanol oxygen concentration was followed with a Clark-type oxygen
amine (MEA) solutions. electrode (Oxical 5, WTW, Germany). The liquid phase mass
balance, in its integrated form
The experiments were carried out in two different stirred cell

reactors at low stirring speeds serving for a flat gas–liquid in- ln(cL − cL ) = −kL at + const., (1)
terface. The experimental setups are schematically represented
in Fig. 1. can be used to determine kL a and, since the surface is flat, also
Reactor A (Fig. 1a) was a 1720 ml jacketed cylindrical glass the liquid-side mass transfer coefficient kL can be deduced.
vessel with an inner diameter of 96 mm; it was equipped with The absorption rate of oxygen from air at atmospheric pres-
four baffles of 10 mm width. The stirrer shaft carried two sure into sulphite solution was calculated from the rate of
rectangular-shaped two-bladed stirrers mounted at distances of sulphite consumption determined by iodometric titration of
7338 M. Rosu et al. / Chemical Engineering Science 62 (2007) 7336 – 7343

Fig. 1. Experimental setup: (a) reactor A and (b) reactor B.

samples taken at regular intervals. Due to decreasing pH, the on suspended particles on the overall absorption capacity of the
rate drops slightly as sulphite is converted into sulphate. From slurry, i.e., the total pressure drop (Pi − Pf ), remained very
a second-order polynomial fit, the rate at 0.7 M sulphite con- minor (< 2%) at the low solid loadings studied.
centration was calculated and used for comparison to kL ac∗L Also for absorption with reaction of CO2 into hydroxide
from physical absorption to obtain the enhancement factor E. and MEA solutions, the pressure decrease from 0.1 to about
The physical absorption rates of pure O2 or N2 into sodium 0.015 MPa was recorded. The CO2 flux j is obtained from the
hydroxide and MEA solutions were determined from the rate slope.
of pressure decrease when saturating the liquid under isochoric Various surfactant contamination levels were studied:
and isothermal conditions. Any dissolved gases were desorbed
by evacuation and, after thermal equilibration, the head space • Clean reactor (Reactor A: treating the closed reactor at 323 K
was filled with the gas. The pressure decrease after starting the three times with acetone/ethanol mixture for 3 h and, after
stirrer was recorded. The volumetric mass transfer coefficient drying, two times for 3 h with double-distilled water at 343 K.
kL a and, since the surface is flat, also the liquid-side mass Reactor B: treating the closed reactor at 373 K once with an
transfer coefficient kL can be determined from the following acetone/ethanol mixture for 8 h and, after drying, three times
relation: for 8 h with double-distilled water at 413 K. The more severe
Pi − pwater procedure in reactor B was more effective but could not be
ln(P − Pf ) = − kL at + const. (2) applied in the glass reactor A.).
Pf − pwater
• “Fingerprint” contamination (touching the clean inside sur-
The reported kL -values are the mean values of at least three face of reactor B with five fingertips).
(and up to five) determinations; the mean standard deviation • “Dust” contamination (leaving the clean reactor B open to
was less than 0.02 × 10−4 m s−1 . The effect of gas adsorption the air overnight).
M. Rosu et al. / Chemical Engineering Science 62 (2007) 7336 – 7343 7339

• Defined contamination with non-ionic surfactant isode- activated carbon. For fingerprint contamination there is an about
canol heptaethoxylate (Lutensol䉸 ON 70, BASF, Germany). fourfold increase in the absorption rate by activated carbon
The surfactant is a mixture of homologues with differ- addition, i.e., the fingerprints’ effect is quite comparable to that
ent ethoxy-chain lengths; the mean molecular weight is of the non-ionic surfactant.
0.47 kg mol−1 . The desired surfactant concentration in the
range of 0.01 kg m−3 up to the critical micelle concentration 3.2. Absorption with fast chemical reaction (sulphite
of 0.6 kg m−3 was adjusted by adding 1 ml of appropriately oxidation)
concentrated surfactant solution with a syringe through a
sampling port of reactor A. When absorbing oxygen into sodium sulphite solution in the
fast reaction regime (19 < Ha < 160  Ei ≈ 104 ), there is no
The static surface tension of the solutions was measured with effect of the surfactant (Fig. 4). Here
the du Nouy (ring) method (Krüss K11, Hamburg, Germany).  
∗m−1 0.5
m + 1 km,n cBn DA cL
Ha = , (3)
3. Results and discussion 2 kL2
c B DB
3.1. Physical absorption Ei = 1 + , (4)
zc∗L DA
For physical absorption of oxygen and nitrogen into sodium
sulphate and sodium hydroxide solutions, the mass transfer co-
efficient kL strongly decreased by the addition of small amounts
of the surfactant isodecanol heptaethoxylate (Fig. 2). At sur-
factant concentrations higher than 0.1 kg m−3 , the mass trans-
fer coefficients in the particle-free liquids are similarly low at
about 41 of the ones in the clean systems.
The sodium hydroxide and the MEA concentration, respec-
tively, have little effect on the physical absorption of oxygen.
This means that no significant contaminations are introduced
with these analytical grade chemicals (Fig. 3). A slight de-
crease is expected due to lower gas diffusivity than in pure wa-
ter. The kL reduction by the considered two types of accidental
contaminations is similar in sodium hydroxide and MEA solu-
tions, with fingerprints having the stronger effects in both cases.
This trend agrees with the observations of Kaya and Schumpe
(2005). The high absorption rate at a clean interface can be re-
gained by the addition of activated carbon. Correspondingly,
the surface tensions of 0.5 M NaOH solutions with dust con-
tamination (64.9 mN m−1 ) and with fingerprint contamination
(60.5 mN m−1 ) are exactly back to the value of 72.5 mN m−1
of uncontaminated solutions after the addition of 0.5 kg m−3 Fig. 3. Effect of the MEA and NaOH concentration, respectively, on the
physical absorption of oxygen (reactor B).

Fig. 2. Reduction of the liquid-side mass transfer coefficient for O2 in


sodium sulphate solution and for N2 in sodium hydroxide solutions with the Fig. 4. Effect of the isodecanol heptaethoxylate concentration C on the oxygen
isodecanol heptaethoxylate concentration C (reactor A). flux into sulphite solution at different catalyst concentrations (reactor A).
7340 M. Rosu et al. / Chemical Engineering Science 62 (2007) 7336 – 7343

Fig. 5. Effect of the activated carbon concentration cS on the oxygen flux Fig. 7. Effect of surfactant concentration C on the carbon dioxide absorption
into sulphite solution at different catalyst concentrations (reactor A). rate into sodium hydroxide solutions (reactor A).

Fig. 6. Combined effects of surfactant and activated carbon loadings on the


oxygen flux into sulphite solution (2 × 10−3 M CoSO4 , reactor A).
Fig. 8. Effect of the activated carbon loading cS on carbon dioxide absorption
into 2 M sodium hydroxide solution (reactor A).
with n = 0, m = 2 and z = 2 for sulphite oxidation. The obser-
vations agree with the theory of absorption with fast chemical
the higher the activated carbon loading needed to increase the
reaction predicting no effect of kL (E = Ha):
absorption rate up to the value of the surfactant-free system.
 0.5
∗ m+1 ∗m−1 ∗
Similar trends as for 2 M NaOH solution were observed for
j = HakL cL = n
km,n cB DA cL cL . (5) the two lower concentrations (results not shown). Note that the
2
absorption rate is lower in the surfactant-free system without
Activated carbon has no effect (Fig. 5), i.e., there is no ex- solids than in the carbon slurries, probably, because of surfac-
tra contribution by adsorptive transport (“shuttle effect”). Also tant contamination of the glass reactor from a previous run.
when activated carbon is added to surfactant contaminated sys- The effects of surfactant and activated carbon on the carbon
tems (Fig. 6), as expected based on Eq. (5), there is no effect dioxide absorption into sodium hydroxide solution can be un-
of higher kL on the oxygen flux. derstood by considering the absorption regime. At the lowest
sodium hydroxide concentration of 0.5 M, the CO2 absorption
3.3. Absorption with instantaneous chemical reaction takes place close to the instantaneous regime since Ei = 18
(CO2 /NaOH) and Ha = 25 (in the absence of surfactant) and up to Ha = 105
(with surfactant). These values are estimated as described by
Contrarily to sulphite oxidation, the flux of CO2 into sodium Darmana et al. (2007) except for the CO2 solubility since the
hydroxide solution is much lower in the presence of the non- listed salting-out parameters do not agree with the original val-
ionic surfactant isodecanol heptaethoxylate than in a surfactant- ues of Weisenberger and Schumpe (1996). Ha and Ei are as
free system (Fig. 7). The absorption rate increases by the defined in Eqs. (3) and (4) with n = m = 1 and z = 2.
addition of activated carbon, presumably, due to adsorption of At the highest NaOH concentration (2 M) the following ab-
the surfactant (Fig. 8). The higher the surfactant concentration, sorption parameters are estimated: Ei = 198 and Ha = 84
M. Rosu et al. / Chemical Engineering Science 62 (2007) 7336 – 7343 7341

Fig. 9. Variation in the surfactant effect on CO2 absorption into 2 M NaOH Fig. 10. Effects of activated carbon and graphite powder concentrations on
solution with the partial pressure: ratio of the flux into surfactant-free activated CO2 absorption into 0.1 M MEA solution (reactor B).
carbon slurry (1 kg m−3 ) and particle-free surfactant solution (reactor A).

(in the absence of surfactant) and up to Ha = 290 (with surfac-


tant). At all NaOH concentrations the experimentally observed
enhancement (j/kL cL ∗ ) hardly varies upon surfactant addition,

i.e., the CO2 flux decreases in proportion to the mass transfer


coefficient kL as expected in the instantaneous regime:

j = E i kL cL . (5)
The effect of adding the activated carbon (Fig. 8) corresponds
to the surfactant effect on kL (Fig. 2). However, at lower CO2
∗ , the value of E (Eq. (4)) increases
partial pressure and lower cL i
and the absorption regime gradually changes to the fast reac-
tion regime. This can be checked by comparing not only the
initial fluxes but also those at lower pressures. Note that with
decreasing pressure the liquid phase composition changes but
it is the same at the same pressure. In Fig. 9 the ratio of the
flux to surfactant-free 2 M NaOH solution with activated carbon
(1 kg m−3 ) is related to the flux at the lowest and the highest
surfactant concentration (without solids). The surfactant effect,
and so the effect of the activated carbon, indeed vanishes at
lower pressure where the fast absorption regime is approached.

3.4. Absorption with surface convection (CO2 /MEA)


Fig. 11. Effect of contaminants on CO2 absorption at various sodium hy-
droxide and monoethanol amine concentrations, respectively (N =200 min−1 ,
In reactor B the effects of likely inadvertent contaminations, reactor B).
dust and fingerprints, have been studied for CO2 absorption into
MEA solutions. The activated carbon concentrations needed to
remove the contaminants are similarly low as in the case of The particle effects on CO2 absorption into MEA and NaOH
non-reactive systems (cf. Figs. 10 and 3). Graphite has almost solutions in reactor B are compared in Fig. 11. In NaOH solu-
the same effect as activated carbon although it has practically tions the effect of activated carbon is again of the same order
no adsorption capacity for CO2 . After removing the carbon par- as the effects of the surface-active contaminants on kL (Fig. 3)
ticles by rinsing, the flux remains high (open circle). Clearly, as found for instantaneous reaction in reactor A. Compared to
the results cannot be explained with a shuttle mechanism. This this, much stronger effects of activated carbon addition were
does not exclude a shuttle mechanism, in principal, but no sig- observed for CO2 absorption into MEA solutions. When relat-
nificant contribution is left for it. Among the broad size dis- ing the absorption rate at an activated carbon concentration of
tribution of the activated carbon particles there are fines in the 1 kg m−3 to the one in the contaminated system without par-
order of the film thickness; if the fines would enable an addi- ticles, the apparent enhancement EP of CO2 absorption due
tional “shuttle transport”, the particle effect should not level off to addition of activated carbon particles can be very high in
at still low carbon loadings. the CO2 /MEA system (Fig. 12). The instantaneous absorption
7342 M. Rosu et al. / Chemical Engineering Science 62 (2007) 7336 – 7343

by surfactants can have strong effects but is hard to avoid. In


physical absorption, the liquid side mass transfer coefficient kL
may be lower by a factor of up to 3. Activated carbon can bring
back the high absorption rate at a clean interface by adsorbing
the surfactant (“surfactant grazing”).
In absorption with fast chemical reaction, the absorption rate
is independent of the liquid side mass transfer coefficient and
there is no effect of surfactant. In the instantaneous absorption
regime, the absorption rate again depends on kL and the par-
ticle effect by surfactant adsorption is of the same order as in
physical absorption. However, CO2 absorption into MEA so-
lutions may benefit from surface convection (Marangoni insta-
bility) unless this is suppressed by surfactants. The removal of
surfactants by adsorption onto activated carbon can then have
a very strong effect on the absorption rate.
Fig. 12. Apparent “enhancement” of CO2 absorption into MEA solutions by
addition of activated carbon (1 kg m−3 ) with and without stirring (reactor B). Notation

regime can explain only a small part of the effect since the a specific interfacial area (referred to liquid vol-
variation of kL (Fig. 3) is much smaller. ume), m−1
High absorption rate and heat released at the interface may A(B) gas (liquid) phase reactant
∗)
cL (cL (saturation) concentration of gas A in the liquid
lead to local variations in the surface tension and liquid den-
sity and induce surface convection (Marangoni instability). The phase, kmol m−3
Marangoni effect can considerably increase the mass transfer cS particle concentration, kg m−3
rate. For the CO2 /MEA system, Marangoni instability has been cS∗ critical cS -value at which the kL -increase levels
described previously (Brian et al., 1967; Hikita et al., 1979). off, kg m−3
Surfactants change the interfacial properties (Lee et al., 1980; C surfactant concentration, kg m−3
Vázquez et al., 1996) and may reduce or block interfacial con- dS particle diameter, m
vection. Surfactant removal by adsorption onto the solids then DA (DB ) diffusivity of gas (A) and liquid (B) phase reac-
enables surface convection, again. tant, m s−2
The onset of surface convection upon particle addition has a E(Ei ) chemical enhancement factor (for instantaneous
stronger effect when the surface renewal rate is low as without reaction)
any stirring or at low MEA concentrations when convection is Ep “enhancement” by particle addition
fully suppressed by surfactant. Thus the relative effect on the Ha Hatta number
absorption rate is strongest at low MEA concentration while j molar interfacial gas flux, kmol m−2 s−1
the Marangoni effect itself becomes stronger at higher MEA kL liquid-side mass transfer coefficient, m s−1
concentration. Dust and fingerprints act similar but only “fin- km,n reaction rate constant,
gerprint contamination” can hinder surface convection at high kmol1−m−n m−3(1−m−n) s−1
MEA concentration (Fig. 11). Activated carbon adsorbs any m(n) reaction order with respect to A(B)
surfactants and enables surface convection at all MEA concen- N stirring speed, min−1
trations studied. This leads to much higher molar flux of carbon p partial pressure, Pa
dioxide. Pi (Pf ) initial (final) total pressure, Pa
The Marangoni effect might explain the high enhance- t time, s
ment by activated carbon reported for some reactive systems T temperature, K
(Table 1) whereas for physical absorption Emax is usually about z stoichiometric factor
3. Higher critical activated carbon concentration cS∗ may result
from higher contamination levels, e.g., when using technical- Acknowledgement
grade MEA (Saha et al., 1992). As small surfactant contamina-
tions suffice to induce surface rigidity, a clean system is hard The authors are grateful for financial support by the
to achieve unless by using activated carbon as an adsorbent. Volkswagen Foundation.

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