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Chandrakant Thakur, Vimal Chandra Srivastava, Indra Deo Mall & Ajay
Devidas Hiwarkar
To cite this article: Chandrakant Thakur, Vimal Chandra Srivastava, Indra Deo Mall & Ajay
Devidas Hiwarkar (2017): Modelling of Binary Isotherm Behaviour for the Adsorption of
Catechol with Phenol and Resorcinol onto Rice Husk Ash, Indian Chemical Engineer, DOI:
10.1080/00194506.2017.1281770
Article views: 29
Download by: [University of Newcastle, Australia] Date: 20 February 2017, At: 10:09
INDIAN CHEMICAL ENGINEER © 2017 Indian Institute of Chemical Engineers
http://dx.doi.org/10.1080/00194506.2017.1281770
India
b
Department of Chemical Engineering, Indian Institute of Technology Roorkee, Roorkee, Uttarakhand
247667, India
c
Department of Chemical Engineering, University of Petroleum and Energy Studies, Dehradun,
Uttarakhand 248007, India
d
Department of Chemical Engineering, Bundelkhand Institute of Engineering and Technology, Jhansi,
Uttar Pradesh 284128, India
Abstract: The present paper assesses the adsorption capability of rice husk ash (RHA) to adsorb catechol
(C) along with phenol (P) and resorcinol (R) individually and simultaneously from aqueous solution in
both single and binary solutions using batch experiments. Equilibrium isotherm data were collected at
30°C by carrying out experimental runs for 24 h contact time with pre-optimized RHA dosage of
20 mg/L and initial concentration variation of individual components in the range of 50–500 mg/L.
The equilibrium adsorption data for single component were fitted in three adsorption isotherm models,
namely the Langmuir, the Freundlich and the Redlich–Peterson. Equilibrium adsorption data of binary
aqueous solution of catechol–phenol, catechol–resorcinol and the parameter evaluated from single
adsorption isotherm were fitted in various multi-component adsorption isotherm models. Extended
Langmuir model which assumes overlapping of sites for different adsorbates better represented the
binary isotherm data for both catechol–phenol and catechol–resorcinol systems.
Nomenclature
aij competition coefficients of component i by component j, dimensionless
aR constant of Redlich–Peterson isotherm, L/mg
Co initial concentration of adsorbate in solution, mg/L
Co,i initial concentration of each component in solution, mg/L
Ce unadsorbed concentration of the single component at equilibrium, mg/L
Ce,i unadsorbed concentration of each component in the ternary mixture at
equilibrium, mg/L
Ki individual extended Langmuir isotherm constant of each component, L/mg
KF mono-component (non-competitive) constant of Freundlich isotherm of the
single component (mg/g)(L/mg)−1/n
KF ,i individual Freundlich isotherm constant of each component (mg/g)(L/mg)−1/n
KL constant of Langmuir isotherm, L/mg
KL,i individual Langmuir isotherm constant of each component, L/mg
KR constant of Redlich–Peterson isotherm, L/g
m mass of adsorbent per litre of solution, mg/L
n mono-component (non-competitive) Freundlich heterogeneity factor of the
single component, dimensionless
ni individual Freundlich heterogeneity factor of each component, dimensionless
N number of data points
SSE Sum of Square of the Error
qe equilibrium single-component solid phase concentration, mg/g
qe,i equilibrium solid phase concentration of each component in ternary mixture, mg/g
qe,cal calculated value of solid phase concentration of adsorbate at equilibrium, mg/g
qe, exp experimental value of solid phase concentration of adsorbate at equilibrium, mg/g
qm maximum adsorption capacity of adsorbent, mg/g
qmax constant in extended Langmuir isotherm, mg/g
ai constant in SRS model for each component, dimensionless
b constant of Redlich–Peterson isotherm (0 < b < 1)
hi multi-component (competitive) Langmuir adsorption constant of
each component, dimensionless
1. Introduction
Phenol (P) and its derivatives such as catechol (C), resorcinol (R) are widely used as intermedi-
ate and basic products of various chemical industries. Phenol, catechol and resorcinol are
widely present in effluents generated from various industries such as paint, pesticide, coal con-
version, polymeric resin, petroleum refinery, petrochemical and textile [1]. These compounds
are considered to be toxic to aquatic organisms at 5–25 mg/L and impart taste and odour
above 2 μmg/L concentration [2]. United States environmental protection agency (USEPA)
has put phenol in priority pollutants list and proposed stringent limits on the discharge of
phenol [3]. According to usage of water, some of the agencies have recommended phenol con-
centration limit. For drinking water, Bureau of Indian Standards (BIS) recommends phenol
limit of 0.001 mg/L. For potable water, World Health Organization (WHO) recommends
INDIAN CHEMICAL ENGINEER 2017
Modelling of Binary Isotherm Behaviour 3
0.001 mg/L maximum phenol, whereas for wastewater, EPA has put a permissible limit of
0.1 mg/L [4]. Considering the toxicity and maximum permissible limits set by various agencies
all over the world, it is necessary to remove phenolic impurities from wastewater prior to
discharge.
Various conventional treatment methods such as chemical and photo-oxidation, coagu-
lation, aerobic or anaerobic biodegradation, solvent extraction, liquid membrane permeation
and adsorption have been used previously for treatment of organic and phenolic compounds
containing wastewater [5–15]. Compared to all these methods, adsorption is the most attractive
because of its relative simplicity of design, operation and scale up, insensitivity to toxic sub-
stances, low cost and has gained a lot of popularity [1,16–19]. Many researchers have reported
that activated carbon is an efficient material for removal of organic compounds [8–10,20–22].
However, its high initial cost and the need for a costly regeneration system makes it less econ-
omically viable as an adsorbent. Taking these criteria into consideration, many investigators
have done research on more economical adsorbents such as those which can be obtained as
agricultural or industrial wastes/by-products.
India is an agriculture-based economy and huge quantities of agricultural wastes such as
rice husk, baggase are used as fuel in the boilers of various industries such as sugar, pulp
and paper mills. During the burning of these wastes, particles emitted are captured by air par-
ticulate devices. These fly ash particles, such as rice husk ash (RHA) and bagasse fly ash (BFA),
have been tested as an adsorbent by a number of researchers for single and multi-adsorbates
adsorption [23].
RHA has good porosity, high amount of silica and a number of functional groups on its
surface, which make it a good adsorbent. Besides its availability in abundance, make it
highly economical as the only cost involved is the transportation cost from the place of gener-
ation to its place of use as an adsorbent [24]. Consequently, various researchers have used RHA
for adsorptive removal of various types of adsorbates such as metal ions, dyes and organics [25–
29]. Only few studies are reported in the open literature for the multi-component adsorption of
phenolic compounds on various types of adsorbents. Since, actual effluents generated in indus-
tries such as petroleum refineries contain several phenolic compounds; therefore, equilibrium
adsorption data for closely related binary compounds is of utmost importance for the design
of adsorption systems.
The present research work aims to examine individual and simultaneous adsorption behav-
iour of catechol onto RHA from its binary solutions with phenol and resorcinol various multi-
component isotherm models.
Mumbai, India. Various properties of these adsorbates have been listed in Table 1 for compari-
son. The experimental solutions were prepared by diluting the respective stock solution of
phenol, catechol and resorcinol with double distilled water (DDW) and mixing them in the
desired proportion. The concentrations of all the three components were varied between 50
and 1000 mg/L.
The compound was identified by its peak retention time of the components. The calibration
curve between peak areas of HPLC reading versus concentration prepared for both single
and binary components with a correlation coefficient (R2 ) equal to 0.99.
The total amount of adsorbate adsorbed per g of RHA (qe,i ); individual adsorption yield
(Adi %) and total adsorption yields (AdTot %) were calculated using the following expressions
(Equations (1)–(3)):
(Co,i − Ce,i )V
qe,i = , (1)
w
100(Co,i − Ce,i )
Adi % = , (2)
Co,i
100 (C − Ce,i )
AdTot % = o,i , (3)
Co,i
where qe is the amount of adsorbent (mg/g); Co and Ce are the initial and equilibrium concen-
trations of adsorbate, i, in liquid phase (mg/L), respectively; V is the volume of the adsorbate
containing solution and w is the mass of the adsorbent (g).
n
SSE = (qe,i, exp − qe,i,cal )2 . (4)
i=1
In this equation, the subscripts “exp” and “calc” show the experimental and calculated
values, and n indicates the number of measurements. The constants of single-component iso-
therm were further used in the multi-component adsorption model. Many multi-component
isotherm models such as non-modified Langmuir model, modified Langmuir model, extended
Freundlich model were used to analyse the multi-component adsorption behaviour. Single and
multi-component isotherm models used in the present isotherm modelling are listed in the
Table 2.
(1/ni )−1
N
SRS qe,i = KF,i Ce,i j=1 aij Ce,j [46]
KR,i Ce,i
Non-modified R–P qe,i = N b,j
[47]
1 + j=1 aR,j Ce,j
KR,i (Ce,i /hR,i )
Modified R–P qe,i = N b,j
[47]
1+ j=1 aR,j (Ce,j /hR,j )
Fig. 1. Equilibrium adsorption isotherms for the individual adsorption of phenol, catechol and resorci-
nol onto RHA. Experimental data represented by points and R–P isotherm fitting represented by lines.
of phenolic rings or due to the symmetric CH3 stretch of the methoxyl group. These peaks get
shifted to higher wave numbers in 2830, 2834 and 2854 cm−1 in phenol-, resorcinol- and cate-
chol-loaded RHA. Blank RHA shows peaks at 1355 and 1593 cm−1. These peaks may be due
to OH deformation and stretch of C = C aromatic rings or due to NH bending, respectively
[30,31]. The band at 1355 cm−1could also be due to both OH in-plane bending and CH
Fig. 2. FTIR analysis of raw RHA, phenol-, catechol- and resorcinol-loaded RHA.
Table 3. Individual adsorption equilibrium uptakes and yields of phenol, catechol and resorcinol
adsorption at different initial concentrations onto RHA
Co Ce qe Ad%
(mmol/L) (mmol/L) (mmol/g) –
Phenol
0.266 0.212 0.003 20.250
2.597 1.421 0.059 45.294
5.173 3.254 0.096 37.112
7.830 5.300 0.127 32.316
10.480 6.774 0.185 35.361
13.510 9.083 0.221 32.773
Catechol
0.229 0.162 0.003 29.434
0.865 0.368 0.025 57.450
2.141 0.906 0.062 57.677
6.747 3.767 0.149 44.167
8.952 4.757 0.210 46.860
13.525 7.430 0.305 45.068
Resorcinol
0.239 0.169 0.004 29.454
0.465 0.238 0.011 48.718
1.164 0.519 0.032 55.448
2.553 1.270 0.064 50.262
5.225 2.960 0.113 43.346
6.687 4.093 0.130 38.795
8.958 5.092 0.193 43.156
13.510 7.947 0.278 41.176
bending [32]. The strong band observed around 1091 cm−1 may be assigned to C–O stretching.
In the adsorbate-loaded RHA spectra, not only the intensity of these bands increases but also
shift in peaks is observed indicating utilization of these groups for adsorption purpose [33]. Two
different types of electron donor–acceptor interactions may occur on the RHA surface. RHA
surface has both carbonyl and amine groups, which are electron donors. These may interact
with aromatic ring (electron acceptors) of the phenolic adsorbates [34,35]. It may be seen
that the adsorbate-loaded RHA has a much sharper peak in the range of 3200–3400 cm−1
when compared to blank RHA, which has a broader peak (3320–3600 cm−1). Thus, amine
group seems to be more helpful in the adsorption of phenolic adsorbates.
adsorption removal efficiency (Ad%) decreases with an increase in the initial concentration. At
higher concentrations, the driving force required to overcome the resistance to the mass transfer
of adsorbate between the solution and the solid phases becomes greater, and thus the equili-
brium uptake increases. For higher initial concentration, the trend was similar in the present
study for all the adsorbates (phenol, catechol and resorcinol) adsorption onto RHA. At high
initial concentrations, adsorbate molecules already adsorbed resist adsorption of new mol-
ecules and the Ad% decreases. However, at lower initial concentration, Ad% increased with
an increase in initial concentration (up to a certain value) because of the higher driving force
and very small presence of adsorbate on the adsorbent.
It may also be seen in Fig. 2 that the adsorption capacity of RHA for catechol is greater
than that of resorcinol and phenol. Adsorption process is mainly influenced by solubility,
polarity, position of the hydroxyl group and interactive force between the adsorbate in the
aqueous phase and the RHA [7,25,26,28]. Solubility of resorcinol is much higher than catechol
[9]. This may be the reason for lower adsorption capacity of resorcinol compared to that of cate-
chol. In addition, the polarity of adsorbates influences the adsorption of phenolic derivatives.
The dipole moment of catechol (2.620 D) is much larger than that of resorcinol (2.071 D) and
phenol (1.22 D), respectively [36]. Therefore, the interaction between the RHA with catechol is
expected to be much stronger than that of resorcinol and phenol. Suresh et al. [9] found that the
ortho-position greatly enhances the adsorption energy of compound such as catechol. Thus
Table 4. Isotherm parameter fitted on isotherm model for the removal of phenol, catechol and resorcinol
by RHA
3.32Ce,C
Catechol qe,C = 0.991 0.0006
1 + 63.34Ce,C
0.121
2.87Ce,R
Resorcinol qe,R = 0.975 0.0007
1 + 61.86Ce,R
0.161
cumulative effects of solubility, polarity and position of the hydroxyl group probably increased
the absorbability of catechol when compared to resorcinol and phenol onto RHA [37].
Substitution of functional groups on benzene ring provides different inductive and reson-
ance effects [38]. π-donating strength of the host aromatic ring is known to be enhanced by the
substitution of hydroxyl group, which is an electron-donating functional group. This increases
the adsorption affinity of the phenolic compounds to the RHA [39]. FTIR analysis shows that
the interaction between RHA and adsorbates, and between phenol catechol and resorcinol
happens with the help of aromatic ring (electron acceptor) and –OH groups. Since π–π disper-
sive interactions become stronger with an increase in the number of hydroxyl groups [8,9],
therefore, the adsorption of phenol is less than the catechol and resorcinol onto RHA.
Table 5. Comparison of individual and total adsorption equilibrium uptakes and yields found at different
catechol (C) concentrations in the absence and presence of increasing concentrations of phenol (P)
Table 6. Comparison of individual and total adsorption equilibrium uptakes and yields found at different
catechol (C) concentrations in the absence and presence of increasing concentrations of resorcinol (R)
values for catechol–phenol and catechol–resorcinol systems are summarized in Tables 5 and 6,
respectively.
It may be seen that the equilibrium uptake of catechol decreases with an increase in phenol
and resorcinol concentration and vice versa. For instance, at 2.14 ± 0.01 mmol/L initial cate-
chol concentration, in the absence of phenol and resorcinol concentration, adsorbed catechol
quantities at equilibrium are found to be 0.062 (Table 3). However, in the presence of
5.232 mmol/L phenol, adsorbed catechol quantities at equilibrium are found to be
0.057 mmol/g (Table 5). Similarly, in the presence of 4.462 mmol/L of resorcinol, adsorbed
catechol quantities at equilibrium are found to be 0.065 mmol/g (Table 6). Thus, the combined
effect of catechol–phenol and catechol–resorcinol on the total sorption is antagonistic.
During individual adsorption, the adsorption capacity of RHA for catechol is greater than
that of resorcinol and phenol. Therefore, it is expected that the adsorption removal efficiency
(AdC%) of catechol will be higher than the Adtol% in the binary adsorption. However, at
some experimental points (Tables 5 and 6), Adtol% > AdC%. It may be noted that at some of
these points, the difference is marginal and within experimental error. Significant difference
is observed only for those experimental runs in which the initial concentration of catechol is
high and that the initial concentration of other adsorbate is low. At higher initial concentration,
significant amount of catechol adsorption takes place in short time due to higher driving force;
however, adsorbed catechol molecules repel more adsorption of catechol and AdC% decreases.
For the other adsorbate, since its initial concentration is lower, its Ad% is higher and it overall
increases the Adtol%.
The binary adsorption data of catechol–phenol and catechol–resorcinol aqueous solution
onto RHA have been fitted to the various multi-component isotherm models using SSE error
function. The multi-component non-modified R–P model (Equations (5) and (6)) showed poor
fit to catechol–phenol and catechol–resorcinol experimental data.
3.321Ce,C
qe,C = ; qe,P
1 + (63.336Ce,C
0.121
+ 28.722Ce,P
0.186
)
1.080Ce,P
= , SSE = 0.0682, (5)
1 + (63.336Ce,C
0.121
+ 28.722Ce,P
0.186
)
3.321Ce,C
qe,C = ; qe,R
1 + (63.34Ce,C
0.121
+ 61.86Ce,R
0.161
)
2.87Ce,R
= , SSE = 0.048, (6)
1 + (63.34Ce,C
0.121
+ 61.86Ce,R
0.161
)
To improve the accuracy of non-modified R–P model, Bellot and Condoret [44] incorpor-
ated an interaction term, hRP,i , in the competitive non-modified R–P model to formulate the
modified competitive R–P model. All the modified R–P coefficients (hRP,i ) estimated were
found to be slightly less than 1.0, indicating that the use of hRP,i increased the fitting in modified
3.321(Ce,C /0.67)
qe,C = ; qe,P
1 + (63.336(Ce,C /0.67)0.121 + 28.722(Ce,P /0.163)0.186 )
1.08(Ce,P /0.163)
= , SSE = 0.0040, (7)
1 + (63.336(Ce,C /0.675)0.121 + 28.722(Ce,P /0.163)0.186 )
3.321(Ce,C /0.49)
qe,C = ; qe,R
1 + (63.34(Ce,C /0.49)0.121 + 61.86(Ce,R /0.323)0.161 )
2.871(Ce,R /0.323)
= , SSE = 0.0051. (8)
1 + (63.34(Ce,C /0.49)0.121 + 61.86(Ce,R /0.323)0.161 )
Similarly, use of interaction terms for Langmuir model (hL,i ) in the modified Langmuir
model (Equations (11) and (12)) significantly improved the fit of the non-modified Langmuir
model (Equations (9) and (10)) as shown by decrease in SSE values:
2.224 × 0.0212Ce,C
qe,C = ; qe,R
1 + (0.056Ce,R + 0.0212Ce,C )
0.805 × 0.056Ce,R
= , SSE = 0.0135, (10)
1 + (0.0212Ce,C + 0.056Ce,R )
0.51 × 0.137Ce,C
qe,C = ; qe,R
1 + (0.137Ce,C + 0.167Ce,R )
0.51 × 0.167Ce,R
= , SSE = 0.0039. (14)
1 + (0.137Ce,C + 0.167Ce,R )
Constant Ki in the extended Langmuir model reflects the affinity between RHA and the
adsorbates in the binary system. The value of Ki for catechol–phenol was found to be 0.017
and 0.02 L/mmol and for catechol–resorcinol was found to be 0.137 and 0.1667 L/mmol,
respectively. The overall total adsorbate uptake (qmax ) for catechol–phenol and catechol–resor-
cinol by RHA was found to be 2.96 and 0.51 mmol/g respectively, which is much lower than the
sum of the maximum total capacities of catechol–phenol (2.22+0.85 = 3.07 mmol/g) and cate-
chol–resorcinol (2.22+0.81 = 3.03 mmol/g) resulting from the single-component adsorption.
Thus, it seems that catechol and resorcinol compete more when compared to catechol and
phenol for same adsorption sites present on RHA.
Sheindorf–Rebhum–Sheintuch (SRS) model is applicable to those systems where each
component individually obeys the single-component Freundlich isotherm and that the
adsorption energies of sites are exponentially distributed [46]. The adsorption competition
coefficient (aij ) describes the inhibition to the adsorption of component i by component j.
For systems which are represented by the SRS model, product of the competition coefficients
aij and a ji is close to unity [25,47–49]. The binary adsorption of catechol–phenol and catechol–
resorcinol onto RHA can be represented by following form of SRS equations (Equations (15)
and (16)):
For the simultaneous adsorption of catechol and phenol onto RHA, product of aPR and
aRP was found to be much less than 1; therefore, SRS model was not able to satisfactorily rep-
resent the binary sorption data for the catechol and phenol. Results are similar for catechol–
resorcinol system.
Fritz and Schlunder [50] gave an extended Freundlich isotherm for binary mixtures of phe-
nolic substitutes on activated carbon. Extended Freundlich isotherm gives better fit for systems
with significant non-ideal effects and heterogeneous surfaces [51]. Since RHA surface is hetero-
geneous and Freundlich model represented the mono-component isotherm data, therefore,
Fig. 3. Comparison of the experimental and calculated qe values for catechol and phenol adsorption
from a binary mixture of catechol and phenol.
Fig. 4. Comparison of the experimental and calculated qe values for catechol and resorcinol adsorption
from a binary mixture of catechol and resorcinol.
Fig. 5. Binary adsorption isotherms of simultaneous catechol and phenol adsorption onto RHA. The
surfaces are predicted by the extended Langmuir model and the symbols are experimental data: (a) cate-
chol uptake and (b) phenol uptake.
Fig. 6. Binary adsorption isotherms of simultaneous catechol and resorcinol adsorption onto RHA. The
surfaces are predicted by the extended Langmuir model and the symbols are experimental data: (a) cate-
chol uptake and (b) resorcinol uptake.
Table 7. Comparison of surface area of low-cost adsorbents and their capacity for the adsorption of
phenolic compounds
Notes: SD: saw dust; SDC: saw dust carbon; CFA: coal fly ash; HDTMA-Mt: hexadecyl trimethyl ammonium bromide,
montmorillonite; RHA: rice husk ash.
extended Freundlich model also gave satisfactory fit to the binary experimental equilibrium
data (Equations (17) and (18)).
0.89 0.82
0.052Ce,C 0.036Ce,P
qe,C = ; qe,P = , SSE = 0.0797, (17)
0.01
Ce,C + 14.985Ce,P465.22 0.001
Ce,P + 1.55Ce,C
1.55
10.671 77.474
0.0517Ce,C 0.0457Ce,R
qe,C = ; qe,R = , SSE = 0.034. (18)
9.791
Ce,C + 0.001Ce,R 0.2040 76.634
Ce,R + 11.669Ce,C
205.117
The comparisons of the experimental and calculated qe values of catechol–phenol and cate-
chol–resorcinol in mixtures are also presented by the parity plots in Figs. 3 and 4, respectively.
To determine the best fit model for both binary adsorption system SSE values of different iso-
therm models were compared. Extended Langmuir model (SSE = 0.0041 and SSE = 0.0039)
showed best-fits for the experimental adsorption data of catechol–phenol and catechol–resor-
cinol, respectively, for binary systems onto RHA. It seems that component of both binary
compete for the same adsorption sites on RHA. Thus, extended Langmuir model which
assumes overlapping of sites for different adsorbates better represents the isotherm data.
Figs. 5 and 6 show a 3D diagram plotted on the basis of smooth surface generated from the
multi-component extended Langmuir model. The experimental data are shown by points on
the same surface. The fit of the surface to the experimental data points is satisfactory.
Table 7 compares the adsorption capacity for removal of phenolic compounds and surface
area of some low-cost adsorbents. It may be seen that the adsorption capacity and surface area
differ widely in their values for different adsorbents. RHA used in the present study shows good
adsorption for phenol, resorcinol and catechol.
4. Conclusion
The equilibrium adsorption of phenolic compounds was studied for single components and for
binary component catechol–phenol and catechol–resorcinol systems onto low-cost adsorbent
RHA. Adsorption equilibrium data were obtained by batch mode experiment performed at
30°C. Various isotherm models were used to interpret the adsorption data of the investigated
single and binary systems. Langmuir, Freundlich and R–P isotherm models shows quite
similar results, of which R–P was found to be marginally better isotherm model for the
single-component adsorption. Extended Langmuir model showed better fit for binary com-
ponent adsorption for catechol–phenol and catechol–resorcinol systems among various
multi-component isotherm models. RHA showed higher adsorption capacity for catechol
when compared to resorcinol and phenol. The binary adsorption equilibrium data showed
competitive adsorption behaviour.
Disclosure statement
No potential conflict of interest was reported by the authors.
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