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Published: 2019-06-01
Biotechnology
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COCOA SHELL FOR THE PRODUCTION OF ENDOGLUCANASE BY Penicillium roqueforti ATCC 10110
IN SOLID STATE FERMENTATION AND BIOCHEMICAL PROPERTIES
P.C. Oliveira, A.R. de Brito, A.B. Pimentel, G.A. Soares, C.S.V. Pacheco, N.B. Santana, E.G.P. da Silva, A.G. de A.
Fernandes, M.L.O. Ferreira, J.R. Oliveira, M. Franco
777-787
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CO-DIGESTION OF Agave angustifolia Haw BAGASSE AND VINASSES FOR BIOGAS PRODUCTION
FROM MEZCAL INDUSTRY
A.V. Gómez-Guerrero, I. Valdez-Vazquez, M. Caballero-Caballero, F. Chiñas-Castillo, R. Alavéz-Ramírez, J.L.
Montes-Bernabé
1073-1083
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INVESTIGATION OF NOVEL laccase PRODUCING FUNGAL SPECIES AND ITS SUBSTRATE SPECIFICITY
BY WET AND DRY LAB
M. Aftab, A. Tahir, T. Asim, A. Nawaz, Y. Saleem
1233-1243
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Food Engineering
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WATER AND PHYTOCHEMICALS DYNAMIC DURING DRYING OF RED HABANERO CHILI PEPPER
(Capsicum chinense) SLICES
J.A. Olguín Rojas, L.A. Vázquez-León, M.A. Salgado-Cervantes, G. Fernandez-Barbero, A. Díaz-Pacheco, M.A.
García-Alvarado, G.C. Rodriguez-Jimenes
851-864
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Quality and novel indicators of commercial life in Valencia oranges (Citrus sinensis Osbeck)
D.A. Macías-Ojeda, C. Cervantes-Arista, C. Pelayo-Zaldívar, H.B. Escalona-Buendía, I. Alia-Tejacal, J.A. Mendoza-
Espinoza, L.L. Rodríguez Verástegui, F. Díaz de León-Sánchez
979-994
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Transport phenomena
EFFECT OF THE ROTATING REFERENCE FRAME SIZE FOR SIMULATING A MIXING STRAIGHT-BLADE
IMPELLER IN A BAFFLED STIRRED TANK.
A.D. De La Concha-Gómez, J.J. Ramírez-Muñoz, V.E. Márquez-Baños, C. Haro, A.R. Alonso-Gómez
1143-1160
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Environmental Engineering
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BIOREMEDIATION METHODS ASSISTED WITH HUMIC ACID FOR THE TREATMENT OF OIL-
CONTAMINATED DRILL CUTTINGS
M.L. Interiano-López, V.A. Ramírez-Coutiño, L.A. Godinez-Tovar, E. Zamudio-Pérez, F.J. Rodríguez-Valadez
929-937
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Process engineering
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VOLUMETRIC POWER INPUT AS A RELIABLE PARAMETER FOR SCALE-UP FROM SHAKE FLASK TO
STIRRED-TANK BIOREACTOR: PRODUCTION OF A RECOMBINANT GLYCOPROTEIN BY Streptomyces
lividans
R.A. Gamboa-Suasnavart, L.D. Marín-Palacio, L. López-Griego, M.S. Córdova-Aguilar, N.A. Valdez-Cruz, M.A.
Trujillo-Roldán
1085-1099
Materials
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Polymers
Thermodynamics
NUMERICAL ANALYSIS OF CO2 TRANSIENT BEHAVIOR IN THE GAS COOLER DURING VARIABLE
START-UP CONDITIONS OF A TRANSCRITICAL REFRIGERATION SYSTEM
J.F. Ituna-Yudonago, J.M. Belman-Flores, F. Elizalde-Blancas, V. Pérez-García, O. García-Valladares, I. Carvajal-
Mariscal
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1101-1118
Energy Engineering
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Vol. 18, No. 3 (2019) 1133-1142
Revista Mexicana de Ingeniería Química
REMOVAL OF CONGO RED DYE USING ELECTROCOAGULATED METAL
CONTENIDO
HYDROXIDE IN A FIXED-BED COLUMN: CHARACTERIZATION, OPTIMIZATION
AND
Volumen 8, número MODELING
3, 2009 STUDIES
/ Volume 8, number 3, 2009
Publicado por la Academia Mexicana de Investigación y Docencia en Ingeniería Química A.C. 1133
Suárez-Vázquez et al./ Revista Mexicana de Ingeniería Química Vol. 18, No. 3 (2019) 1133-1142
The discharge of industrial effluents containing Experiments were carried out in a fixed-bed column
this type of dyes influences the natural appearance of to investigate the effect of the column parameters
the rivers, causes toxicity and has a negative impact on (initial CR concentration, adsorbent mass and feed
aquatic life due to interference with the transmission flow). The column study was optimized using the
of sunlight that decreases the action of photosynthesis response surface methodology. Two different models
(Mendoza-Basilio et al., 2017, Inguez-Fern et al., were applied, the BDST and the Thomas model for
2011). Therefore, there is a need to design efficient the column study.
methods for the removal of CR from aqueous effluents
(Cervantes-Avilés et al., 2017).
Various physical, chemical and biological 2 Materials and methods
methods such as adsorption, flocculation/coagulation,
sonochemical, photochemical, precipitation,
membrane, electrochemical, catalytic or ozonation
2.1 Adsorbent material
(Kumari et al., 2016; Annadurai et al., 2002) (Lachheb
et al., 2002; Shan et al., 2015; Lei et al., 2016; The adsorbent used in this study was obtained
Lin et al., 2015) have been widely used in the from a pilot electrocoagulation (EC) plant using
elimination of CR from residual effluents, but their aluminum electrodes. For this proposes, well water
effectiveness or economic advantage remains currently was treated to remove silica at a concentration
a major problem. Adsorption is considered superior of 49.63 ± 1.8 mg L−1 , and the electrocoagulation
to other techniques because it is economical, with process was able to decrease the concentration to
high performance and easy operation (Téllez-Pérez 6.93±5.85 mg L−1 when a current of 140 A,
et al., 2017). The investigations are directed to use conductivity of 750 mS cm−1 and a flow rate of
low cost adsorbents such as the reuse of agricultural 35 L min−1 was used. The waste sludge obtained
or industrial waste (Aldana-Espitia et al., 2017), in after EC was clarified, sedimented, centrifuged, dried,
this sense a candidate is an Electrocoagulated Metal crushed and finally a particle size of 35-40 mesh
Hydroxide Sludge (EMHS), which is obtained from (geometric diameter of 0.4018 mm) was selected for
an electrocoagulation process, where aluminum or the experiments.
iron electrodes are oxidized that release hydroxides
from these metals. These materials are considered
a waste that can cause environmental and public 2.2 CR solutions
health affects if not properly managed. The EMHS
The stock solution of Congo Red (Molecular
can be used to remove effluent dyes by electrostatic
weight = 696.665 g·mol−1 , Molecular formula =
attraction or surface complexation, what becomes
C32 H22 N6 Na2 O6 S2 ) was prepared by dissolving 1 g of
the motivation of this investigation. When the
CR powder in 1 L of distilled water. All CR solutions
implementation of an adsorption process is required
for the experiments were prepared by diluting the
for the treatment of considerable quantities of effluent
stock solution (1 g·L−1 ). Prior to the addition of
and the implementation on an industrial scale, the
EMHS, the initial pH of the experimental solution was
use of fixed bed columns of continuous flow can
adjusted to the desired experimental conditions with
satisfy this need (Corral-Escarcega et al., 2017).
the appropriate amounts of solutions of 0.1 M HCl or
The response surface methodology (RSM) is a
0.1 M NaOH. The concentration of CR in the sample
mathematical and statistical techniques tool with the
was analyzed using a UV-Vis spectrophotometer
purpose of developing, optimizing and improving
(Genesys 10S, ThermoFisher Scientific, USA) at a
industrial products and processes. This strategy
maximum wavelength of 497.5 nm.
is based on experimental designs which are used
to determine the significant factors that affect an
experiment, among them are a three-level factorial 2.3 Characterization of the adsorbent
design, central composite design (CCD) and Box-
Behnken (Bezerra et al., 2008). The objective of this The identification of the phases present in the
work was to investigate the suitability of the reuse of adsorbent material was carried out by means of the X-
Electrocoagulated Metal Hydroxide Sludge (EMHS) ray diffraction (XRD) technique using an Empyrean
as an adsorbent and to examine the ability to adsorb the Panalytical Ltd. equipment equipped with Cu Kα
CR dye in aqueous solution by continuous operation. radiation (λ = 1.5418 Å).
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Additionally, the average crystallite size (d s ) was of the column at particular time intervals and the
calculated using the Scherrer equation (Luo et al., concentration of CR in the effluent was analyzed as
2016): mentioned above. The experiment was stopped when
the concentration of CR in the effluent was equal to
Kλ 90% of the initial concentration
ds = (1)
β cos θ
where d s corresponds to the average crystallite size, K
is the Scherrer constant (0.89), K corresponds to the 2.5 Experimental analysis
wavelength of the X-rays (1.54 Å), β is the broadening
at half of the maximum intensity (FWHM) and θ is the A CCD was used to determine the factors that
Bragg angle. On the other hand, the morphology of affect the adsorption in a fixed bed, and to
the particles as well as the elemental composition of obtain the optimized values that will give the best
the adsorbent material were analyzed by the scanning CR elimination. Three independent variables were
electron microscopy technique coupled with a detector selected, such as, mass of adsorbent (m), initial
for microanalysis by energy dispersion by X-rays concentration of CR dye (C0 ) and feed flow (Q), since
(SEM-EDS) JEOL 6510 LV, JEOL Ltd. For SEM they are significant factors that affect an adsorption
analysis the sample was placed over carbon conductive process in a column process. The variable responses
tape and then sputtered with Au-Pd in order to prepare were breakthrough time (tb ), breakthrough volume
a conductive sample. The SEM images were taken by (Vb ) and saturation time (t s ). The breakthrough
high vacuum mode using secondary electron analysis, time was established as the time required for the
while EDS spectra were carried out at 20 kV and concentration of the dye in the effluent stream to
14 mm of work distance. reach 50% of the concentration of the feed. The
The surface characterization was carried out by breakthrough was the volume treated at tb and was
means of the Fourier Transform Infrared Spectrometry estimated using the following equation:
technique coupled to a total attenuated reflectance
device (ATR-FTIR) in the range of 630 cm−1 to
4000 cm−1 at a resolution of 4 cm−1 . To perform the Vb = Q ∗ tb (2)
analysis, the samples were mixed with KBr in a 1: 100
ratio and pressed to form a thin circular capsule.
where Q is the flow velocity of the dye solution
Finally, the textural properties of the adsorbent
trough the column (ml·min−1 ). The saturation time
were characterized by the N2 physisorption technique
was considered when the exit CR concentration was
using an Auto-sorb 3B Quantachrome Instruments.
90% of the initial CR concentration. A two-level
Additionally, the specific surface area was calculated
randomized factorial CCD was designed for the three
using the Brunauer-Emmett-Teller (BET) method.
independent variables using Design-Expert software
(trail version 7, Stat-Ease, Inc., MN). A total of 20
2.4 Column adsorption experiments were performed according to the CCD
matrix.
Adsorption experiments were carried out on a fixed
bed column of cylindrical borosilicate glass material,
with an internal diameter of 2 cm and 70 cm in
height. The study was carried out at room temperature 2.6 Dynamic models
(24 ± 1°C) with a natural initial pH of the CR dye
of 6.38 ± 0.23. A glass wool filling was placed The description of the dynamic behavior of the
at the bottom of the column as a support for the adsorbate adsorption on the adsorbent is important
packed adsorbent to avoid material loss and achieve for the design of a continuous adsorption process
a good distribution of the fluid during the operation. in a fixed bed column. To predict the breakthrough
At the beginning, the columns were washed with curves and to determine the characteristic parameters
distilled water for one hour to eliminate air bubbles. of the column, mathematical models have been
Subsequently, the solution of the CR dye of known developed for use in the design of continuous fixed bed
concentration was pumped in a continuous downward adsorption columns. In this work, the Thomas, Bohart-
flow through the column using a variable flow Adams and Yoon-Nelson models were used to predict
peristaltic pump. Samples were collected at the exit the effectiveness of the column process.
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Suárez-Vázquez et al./ Revista Mexicana de Ingeniería Química Vol. 18, No. 3 (2019) 1133-1142
Fig. 1. Characterization of EMHS: a) X-ray diffraction, b) ATR-FTIR c) SEM, and d) elemental analysis.
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It was observed that, X1 , X2 , X3 , X2 X3 , X22 and Therefore, the ANOVA analysis indicated the
X32 were significant terms in the model for tb . The applicability of the models to predict the response
value F = 26.11 with a low probability value p- variables (tb , Vb and t s ) for the continuous adsorption
value < 0.0001 and a R2 = 0.9592 indicated that of CR in a fixed bed column by EMHS within the
the regression model was statistically significant for limits of the experimental range evaluated. The good
tb . For the model of Vb , the variables X1 , X2 , X3 , fit of the models was also verified by the correlation
X12 , X22 and X32 were significant. The model showed coefficient between the experimental values and the
a value F = 9.20 with a low probability value p- values predicted by the models of the response
value 0.0009 and a R2 = 0.8923. In the case of the variables (Fig. 2), where it is observed that the points
model t s , the variables X1 , X2 , X3 , X2 X3 , X12 , X22 are close on a straight line of 45 degrees, which
and X32 had statistical significance with a high value confirms the fit to the models.
F = 47.94, low probability value p-value < 0.0001
and R2 = 0.9743, made the model t s , statistically 3.4 Combined effect of process variables
significant.
3.4.1 Effect of adsorbent dose and initial
concentration in breakthrough time
The combined effect of the adsorbent dose and initial
concentration of CR in the breakthrough time is
shown in the contour plot of Fig. 3a. With the
experimental range evaluated, it is observed that the
breakthrough time decreased with the increase of the
initial concentration of the CR dye and increased
with the gain of the adsorbent dose. This behavior
is due to the fact that an increase in the amount
of adsorbent bed generates a greater availability of
active sites for the adsorption process. In this way the
CR dye contaminant molecules experienced a longer
contact time with the adsorbent material, making the
breakthrough time longer.
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3.5 Optimization
To maximize the response variables, a numerical
optimization was used. As a standard, the objectives
for each independent variable were selected “in
the range”, while the desired objectives in terms
of breakthrough time, breakthrough volume and
saturation time, were defined as “maximize”. The
desirability ramp for the numerical optimization
diagram is presented in Fig. 4 from the results,
a breakthrough time of 67.71 min, a breakthrough
volume of 1312.2 mL and a saturation time of 120.83
min can be predicted with a desirability of 0.929
with the following optimal conditions: adsorbent dose
of 8 g, initial concentration of 20 mg.L−1 and a
flow rate of 20 mL.min−1 . In order to confirm
the adequacy and reproducibility of the statistically
Fig. 3. Response surface contour plots for optimized conditions, these results were compared
breakthrough time as a function of the independent with the profile obtained in run 14 of the experimental
variables: a) Adsorbent dose and Initial concentration, matrix, which satisfies the optimized conditions, Fig.
b) Adsorbent dose and Flow rate, and c) Initial 5. As a result, a breakthrough time of 72 min, a
concentration and Flow rate. breakthrough volume of 1440 mL and a saturation
time of 128 min, therefore, the values are very close
Considering the experimental range, the to those predicted in this study obtained. The results
breakthrough time decreased with increasing both suggest that the developed system is an attractive and
the initial CR concentration and the flow velocity in powerful alternative solution for the improvement of
the system. This is due to the fact that an adsorbent the CR continuous adsorption system by EMHS.
material has a number of active sites, which saturate in
a shorter time due to the greater presence of molecules
at the entrance of the process. In the same way, 3.6 Modeling the data in column
increasing the flow rate decreases the residence time
3.6.1 Thomas model
of the CR solution through the column, which means
that the contaminating molecules do not have enough The Thomas model is one of the most commonly used
time to capture the available sites on the adsorbent models to describe the performance of a column and
surface. the prediction of breakthrough curves.
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Table 4. Dynamic parameters for the CR adsorption according Thomas, Bohart-Adams and Yoon-Nelson models.
Thomas Bohart-Adams Yoon-Nelson
kT h =0.00413mL.min−1 .mg−1 KBA = 7.1 × 10−4 L.mg−1 .min−1 kY N =0.0826 min−1
q0 =3.57 mg.g−1 NBA =9.01 mg.L−1 τ =75.86 min
R2 =0.9611 R2 =0.9795 R2 =0.9611
This model follows Langmuir’s adsorption- were obtained from the slope and the intersection,
desorption kinetics and assumes a negligible axial respectively, of a linear graph of ln C0C−C
0
t
against t.
dispersion in the adsorption of the column, since the
driving force of the speed obeys to the reversible
kinetics of the second order, considering that the
3.6.3 Yoon-Nelson model
adsorption is not limited by the chemical reaction,
but is controlled by mass transfer in the interface
The Yoon-Nelson model assumes that the rate of
(Granados-Correa et al., 2009). The linearized
decrease of the adsorption probability for each
equation of the Thomas model can be expressed by:
adsorbate molecule is proportional to the adsorption
! probability and the adsorbate advance probability in
C0 kT h q0 m
ln −1 = − kT hC0 t (6) the adsorbent (Fu et al., 2015). The linear equation can
Ct Q
be expressed by:
where kT h (mL.min−1 .mg−1 ) is Thomas’s constant
rate; q0 (mg.g−1 ) is the absorption in equilibrium of C0
!
the adsorbate per g of the adsorbent; C0 (mg.L−1 ) ln = kY N t − τkY N (8)
C0 − Ct
is the concentration of the adsorbate at the inlet; Ct
(mg.L−1 ) is the output concentration at time t; m (g)
the mass of adsorbent, Q (mL.min−1 ) the flow rate and where kY N (min−1 ) is the velocity constant, τ (min)
t (min) the flow time. With a linear representation of is the time required to observe an advance of 50%
ln(C0 /Ct − 1) against time t, the values of kT h y q0 adsorbate. The parameters kY N y τ of the model
were determined from the slope and the intersection were obtained from the slope and the intersection,
of the graph, respectively. The experimental data of the respectively, of the graph of ln C0C−C
0
t
against t. These
column adsorption was adjusted to the Thomas model factors can be visualized in table 4.
to determine the Thomas velocity constant (kT h ) and The fitting of the obtained experimental column
the equilibrium concentration (q0 ). The results of the data to different models has been compared in terms
calculated coefficients are listed in Table 4. of R2 values. The correlation coefficients (R2 ) obtained
from the models of Thomas, Adams-Bohart and Yoon-
3.6.2 Bohart-Adams model Nelson show that they are suitable kinetic models to
describe the adsorption of CR on EMHS in a fixed bed
The Bohart-Adams model is generally used for the column.
description of the initial part of the breakthrough curve
(Yagub et al., 2014). The linearized equation can be
expressed as follows:
!
Ct KBA N0 Z
ln = kBAC0 t − (7)
C0 U
where, N0 (mg.L−1 ) is the adsorption capacity of
the column, U (cm.min−1 ) is the linear velocity,
KBA (L.mg−1 .min−1 ) is the constant of the Bohart-
Adam model and Z (cm) is the height of the bed
of the column. The Adams-Bohart adsorption model
was also applied to the experimental data for the Fig. 5. Breakthrough curve for dynamic adsorption of
description of the advance curves, and the results CR by EMHS in optimal conditions (m= 8 g, C0 = 20
are presented in Table 4. The values of kBA and N0 mg.L−1 , Q= 20 mL.min−1 )
1140 www.rmiq.org
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All authors of this research work disclose there is not Granados-Correa, F., Jiménez-Becerril, J. (2009).
any financial institution and personal relationship with Chromium (VI) adsorption on boehmite.
other people or organization that could inappropriately Journal of Hazardous Materials 162, 1178-
influence this work. 1184.
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Kumari, S., Mankotia, D., and Chauhan, G. S. (2016). Mendoza-Basilio, C. A., Yee-Madeira, H., Ramirez-
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Environmental Chemical Engineering 4, 1126- aqueous solution in order to reuse treated water.
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using activated Prunus Dulcis as biosorbent: K. (2009). Adsorptive removal of hazardous
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