05
SYNTHESIS OF ACTIVATED CARBON AND CMC BEADS FROM CORN HUSK FOR
EFFLUENT TREATMENT

Usha Sayed1 and Swati Korgaonkar2
1

Professor, 2Research Scholar
Department of Fibers and Textile Chemistry,
Institute of Chemical Technology, (ICT) Matunga, Mumbai, India
Email: swatikorgaonkar25@gmail.com

How to cite this paper:

Sayed,
Usha
andKorgaonkar, Swati (2022)
Synthesis of activated carbon
and CMC beads from Cornhusk for effluent treatment,
Journal of Global Resources,
Vol. 08 (01)DOI:
10.46587/JGR.2022.v08i01.005

Received: 13 Sep. 2021
Reviewed: 24 Oct. 2021
Revised: 05 Nov. 2021
Final Accepted: 14 Nov. 2021

Abstract: Adsorption of dyes from the effluent is a well-known
and feasible method been used in the industry. In the present
work we are using corn husk agricultural waste as asustainable raw material for synthesizing activated carbon
using biopolymer carboxyl methyl cellulose for formation ofbeads. The beads formed are been used for removal ofreactive ultra-orange RGB , acid telon yellow FG 01, basic
coracryl red C2B. The surface area of beads is 39.87m2/g. The
maximum adsorption of reactive orange RGB , acid telon
yellow and basic coracryl red is 68.25mg/g, 72.54mg/g and30.21mg/g for 50ml of dye solution. The stock solution 0.4g/lof dye solution was prepared for each dye respectively. The
beads formed shows a variable pH from 2 to 12 which isfavourable for textile effluent. This is a green approach to use
the agricultural waste for waste water treatment.
Key word: Corn Husk, CMC Beads, Activated Carbon,
Effluent Treatment, Adsorption.

Journal of Global Resources, January 2022, Volume 08 (01) Usha Sayed and Swati Korgaonkar Page | 45

Introduction
The textile industry plants generally have a lot of effluent consisting of chemicals and dyes. Thedyes used in textile industry consist of functional groups azo, nitro, anthraquinone, carbonyl andothers. According to the figures it is evident that there is about 10000 different dyes and pigments
which is been used industrially and about 7×105 tons of synthetic dyes are produced worldwide.
Due to the inefficiency in textile dyeing in industries tons of dyes are been lost in the effluent
during dyeing and finishing which leads to increasing BOD and COD to very high extent. (Singh
Z. and Chadha P ,2016) The effluent is generally been dumped in the rivers and lakes directly
without any treatment which causes a greater concern for the aquatic life. The dyes decrease theabsorption and reflection of light entering the water which further alters the photosynthetic activityof algae (O. Loannidou, A. Zabaniotou, 2007). Dyes have some carcinogenic functional groups
present in them which can cause severe damage to aquatic life if been exposed for a long durationof time. Industries are been imposed through strict laws due to environmental concerns.
(Bisschops I. and Spanjers H, 2003) The effluent is undergone chemical or physical treatment toremove the hazardous chemicals from the effluent and then exposed it to the river. The dyes also
consist of chlorine compound present in them which is carcinogenic to the aquatic organism aswell as prolonged exposure can cause allergic reason as it is skin irritant.
Activated carbon available commercially are majorly been used due to its large surface
area which makes its suitable for variable applications like agricultural usage, fuel storage,
analytical chemistry, chemical purification, environmental chemistry etc. (El-Hendawy, 2008). The
Biopolymer CMC is a natural polymer available in plants and other natural sources. It is watersoluble polymer. The biopolymers are been used extensively due to its cheaper cost an ample ofavailability. The effluents treatment plant available in industry uses chemical and physicalmethods which are highly expensive. (Sharma S., Ruparelia J. and Patel M, 2011). In the present
study we are focusing on a green approach to use the agricultural waste Corn husk. There isminimal use of chemicals to achieve a good adsorption of dyes which are been used in textile
industry.
Materials and Methods
Materials:
The raw material used is Corn. Husk brought from Matunga market. The chemicals phosphoricacid (85 percent) pure, Calcium chloride anhydrous is obtained from LOBA chemicals. The dyes
Ultra orange reactive dye and Acid telon yellow FG 01 is from Dystar India pvt. ltd. while the Basiccoracryl red is obtained from colourtex industries Ltd.
Methods:a) Synthesis of activated carbon from C. Husk:
10gms of C. husk is been weighed drenched in 75 percent of phosphoric acid overnight. The
solution is heated at 850 C for 1 hour and then filtered through whatmann filter 41. The filtrate id
dried at 600C till the filtrate dries completely. It is then put in the crucible and kept in muffle furnace
at 4500C for 3hours. The activated carbon obtained is then crushed in mortar and pestle into fine
powder. (Arbia W., 2013)b) Synthesis of Activated carbon and CMC beads :The above obtained activated carbon is been characterised and then been used for the bead’s
formation. CMC is been used as a biopolymer.1 percent of CMC is been dissolved in distilledwater. T. The dissolved cmc and activated carbon is been mixed and stirred for 1 hr. in highspeed stirrer. 2 percent NaOH is been used for the formation of beads. The activated carbon
mixture is been added in NaOH solution slowly and been kept for stirring overnight. (Keharia H.
and Madamwar D, 2003) The beads formed are been crosslinked with 2 percent of calcium

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chloride to increasing the rate of adsorption of the dye solution. The beads formed are dried andcrushed and been further used for experimentation.
c) Application of formed beads:
The beads which are formed without crosslinking and with crosslinking are been studies for its
adsorption capacity. The Stock dye solution of 0.4 g/L is been prepared for Reactive ultra-orange,
acid telon yellow and basic coracryl red dye. The optimization of the prepared solution at various
adsorption dosage , pH and time is been studied.
[

Results and Discussions
The prepared activated carbon and beads are been characterised for surface area analysis andmethylene blue test for confirming the presence of activated carbon.
a)
BET surface area analysis: BET surface area analysis was done using Micromeritics
ASAP2020, USA instrument. The activated carbon (AC) samples were measured at liquid
nitrogen temperature (77 K)
Table 01: BET Analysis
Properties
Total Surface area, m2 /g
Total Pore Volume, cm3 /g
Average Pore Diameter, Å

CAC
21.86
0.0254
43.12

CACC
26.42
0.0271
39.87

The surface area through BET analysis shows that the surface area before crosslinking (CAC) is
21.86m 2 /g while it is increasing after crosslinking (CACC) i.e., 26.42m 2/g. As the surface area
increases the adsorption capacity also increases.

b)

Methylene blue test: Methylene Blue (MB) value indicates the maximum volume ofstandard MB solution (0.15 percent) decolorized by a fixed amount of AC. Standard MB solution(0.15 percent) was made and allowed to stand overnight (11). Carefully weighed 0.1 g AC was
added to a flask containing 5 mL of MB solution. It was then shaken to decolorize and instead of
conventional method of taking readings after 5 min, readings were taken after 5 min, 6h and 24
h to achieve best results. The entire volume of MB was recorded and then MB value is reported
in mg/g. (Safa Y. and Bhatti H, 2010), (11)Table 02: Methylene Blue Adsorption Test
Carbon loading in g/CAC
0
2.5
5
7.5
10

5min
64.82
208.12219.64237.49249.31

6hrs
138.52476.27657.38842.46904.3924hrs
214.08951.251151.191254.26
1329.31

It is been observed that there is an increase in adsorption with increase in carbon loading. With
increase in activated carbon for the prepared solution there is an increase in adsorption value. It isalso been observed that there is no distinct in adsorption capacity at 10gm of carbon loading. Thisbehaviour is due to presence of carbon and its porous nature. (McKay G., Choy H, 2000) Further withincrease in time the adsorption increases. The readings were taken at 5min, 6 hours and 24 hours
interval which shows an evident increase in adsorption capacity for CAC beads i.e., at 2.5 g of carbon
loading it shows an adsorption of 208.12mg/l 476.27 mg/l and 951.25 mg/l respectively. c)
Characterization of beads through FTIR. The analysis of the surface functional groups present on theACs was done using SHIMADZU 8400 S FTIR spectrophotometer, Japan. Samples were ground to
make a powder and readings were taken in powder form. The organic compounds present 3334.51cm1 NH stretching, 2919 cm-1 NH stretch amine salt, 1726 cm-1 CH bending,1634 cm-1C=C stretch alkene,1371 cm-1NO stretch, 1243.72 cm-1CF stretch, 1155.2 cm-1 SO stretching, 1035.03 cm-1Co stretching.
The fig 2 is given in the fig uploads.

Journal of Global Resources, January 2022, Volume 08 (01) Usha Sayed and Swati Korgaonkar Page | 47

Figure 01: FTIRc)

Batch adsorption studies: Adsorption studies were carried out for reactive ultra-orange,
acid telon yellow FG 01, basic coracyl red. The adsorption of the two-adsorbate activated carbon
and CMC (CAC) and with cross linking with CaCl2 (CACC) were optimised for various parameters.
1.1)
Effect of contact time for Reactive ultra-orange RGB:
From table 3 it is been observed that the rate of adsorption initially is higher and as time progresses;
it decreases for both the adsorbents. At the initial stage, higher numbers of adsorption sites areavailable. With increase in time, saturation of adsorption sites takes place thereby reducing theefficiency of adsorption. For CAC it is seen that after 8 hours there is hardly any increase in adsorption
and hence increase in adsorption capacity while that of CACC there is a huge increase in adsorption
capacity as compared to CAC with time. The reason behind such a distinct difference between
adsorption capacities of CAC and CACC beads can be the higher porosity of AC in CACC beads.
Table 03: Effect of contact Time of CAC and CACC on Reactive dye
Time
1
2
4
6
8
16
24
32

CAC
1.54
7.31
11.38
13.43
18.72
19.19
19.23
18.89

CACC
24.87
32.74
43.38
68.91
128.18139.09146.35150.87

1.2: Effect of pH:
To study the effect of pH of dye solution on adsorption capacities of CAC and CACC beads,
50 ml of 400 mg/L dye solution was treated with 0.1 g of adsorbent beads at pH of 2 to 12 at theintervals of 2 by adjusting the pH using 0.1 N of HCl and 0.1 N NaOH. Readings were taken after 12
h. From table 4 it is been observed that with increase in pH there is a decrease in adsorption capacity.
There is a significant higher adsorption at pH 2. The AC loading in CACC decreases due to theavailable number of amine groups, which are solely due to the lower amount of CMC present in CACC.
Thus, the electrostatic attraction in this case is not the predominant mechanism and adsorption may
be only due to weak physical forces like Van der Waal’s, hydrogen bonding, dipole–dipole. (Safa Y.
and Bhatti H, 2010), (11)Table 4: Effect of pH on Adsorption Capacity of Reactive Dye
pH
2
4
6
8
10
12

Adsorption Capacity
CAC
368.56
72.91
46.31
28.09
15.27
10.46

CACC
246.31
185.46141.29108.23108.23108.31

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1.3: Effect of adsorbent dosage:
While checking the effect of adsorbent dosage on adsorption capacity of CAC and CACC beads,
50 ml dye solution of 400 mg/L dye concentration was treated with different adsorbent beads
quantities, 0.05, 0.1 0.15 and 0.2 g at pH 6 and samples were taken after 16 h.
Table 05: Effect of adsorbate dosage on adsorption capacity of Reactive dye
Initial Concentration 400mg/l, Contact Time 16hrs, pH:6
Adsorbent Dosage (g/50ml) of dye solution
Adsorption Capacity in mg/L
CAC
CACC
0.05
15.34
68.42
0.1
13.57
64.89
0.15
10.87
63.67
0.2
10.98
60.25

From table 5 it was observed that with increase in the absorbent dosage there is adecrease in adsorption capacity. However, with increasing adsorbent dose, the quantity of dye
adsorbed on to the unit weight of the adsorbent gets reduced. This may be attributed tooverlapping or aggregation of adsorption sites, leading to a decrease in total adsorbent surface
area available to the dye and an increase in diffusion path length. (13)1.4: Effect of AC loading:
While investigating effect of AC loading, 50 ml of dye solution of 400 mg/L concentration was
treated with 0.1 g of adsorbent at pH 6 and the samples were taken after 16 h. In this case, CAC
beads were considered as beads with composition 0 g of AC / 1 g of CMC and the AC dosage
was increased as 2.5, 5.0, 7.5 and 10 g of AC / 1 g of CMC.
Table 06 : Effect of Adsorbent dosage on adsorption capacity of Reactive dye
Initial Concentration 400mg/l, Contact Time 16hrs, pH:6
AC Loading g / g of CMC
Adsorption Capacity, mg/g
0
3.84
2.5
18.65
5
40.87
7.5
60.42
10
69.65

It can be observed from the table 6, that as the concentration of AC in CMC beads isincreased, the adsorption capacity increased linearly. As concentration of AC is increased in CMC
beads, more and more AC gets embedded inside the beads and also on the surface of beads. As
AC is having higher surface area, higher numbers of adsorption sites are available and hence
adsorption capacity increases with increase in AC loading.
1.5: Adsorption Isotherm:
To investigate the type of adsorption isotherm for CAC and CACC beads, dye solution of variable
initial concentrations such as 200, 400, 600, 800 and 1000 mg/L were treated with adsorbent at
pH 6 and the samples were taken after 16 h. The study was subjected to three different models
i.e., Langmuir isotherm, Freundlich isotherm and Temkin isotherm. On the basis of R2 values, it
can be concluded that applicability of the model in case of CAC was in the following order,
Langmuir > Temkin > Freundlich. Hence Langmuir was found to be the best suited model for CAC
beads (11). The equilibrium factor value (Rl) is found to be 0.55 showing favourability to Langmuirmodel. monolayer adsorption capacity of the CAC beads (Q0 ) of 52.04 mg/g. Bonding energy
was found to be 0.0043 L/mg. There is a high correlation coefficient of 0.99 according to theLangmuir adsorption , which indicates that there is strong interaction between the dye molecules
and CMC.

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Table 07: Adsorption Isotherm for adsorption of Reactive dye
Isotherm
LangmuirParameters
Q 0, mg/g
B, L/mg
R2
RLn
Kf , (mg/g)(L/mg)1/n
R2
Bt, J/mol/kAt, L/g
R2

Freundlich

TemkinCAC
52.04
0.0043
0.99
0.55
2.27
2.08
0.94
214.04
0.03
0.98

CACC
287.580.00180.997
0.7924
1.418
1.408
0.996
46.7
0.02
0.965

On the other hand, in case of CACC beads, applicability of adsorption isotherms on thebasis of R2 values was observed in the following order, Langmuir > Freundlich > Temkin. BothLangmuir and Freundlich isotherm models were found to have similar values of R2 as 0.997 and
0.996, respectively, which are near to unity. However, the calculated qeq values from Langmuirmodel agreed well with the experimental values, covering most of the data points as in shown intable 7. It can, therefore, be concluded that both Langmuir and Freundlich isotherm models show
applicability in case of CACC. In case of CACC beads, monolayer adsorption capacity (Q0 ) was
found to be very high compared to CAC beads, possibly due to highly porous nature of AC.
Positive values of heat of adsorption (Bt) obtained from Temkin isotherm, 214.04 J/mol/k and 46.7
J/mol/k, for CAC and CACC beads, respectively, show that adsorption of dye is endothermic.
1.6: Adsorption Kinetics:
To investigate the adsorption kinetics, the beads were treated with dye solution of 400 mg/L at
pH 6. Samples were taken at interval of 20, 40, 60, 80, 100, 120, 240, 360, 480, 600, 720, 840,
960, 1080, 1200, 1320, 1440, 1560, 1680, 1800, 1930, 2040 and 2160 min. Three adsorption
kinetics were studied, namely, pseudo first order kinetics, pseudo second order kinetics and intraparticle diffusion kinetics.
Table 08: Adsorption Kinetics for Adsorption of Reactive dye
Kinetic ModelFirst-order

Second-order

Intra-particle
Experimental

Parameter
K1, mg/g/min
qeq, mg/g
R2
K2, mg/g/min
qeq, mg/g
R2Kid, mg/g/√t
I, µg/gqeq, mg/g
R2qeq, mg/g

CAC
1.28×10^ -03

CACC
1.87×10^ -03
11.86
0.87

1.52×10^ -04

158.250.95
1.537×10^ -05

16.89
0.98
1.18
0.29
56.38
0.92
14.87

178.84
0.99
10.45
3.47
175.81
0.94
160.47

It can be clearly seen in table 8, that CAC beads adsorption follows pseudo second ordermodel from the beginning of adsorption process. Pseudo first order kinetics was observed as
better fit for CAC adsorption after the maximum adsorption was achieved. Maximum adsorption(almost 50 percent) was achieved within initial 4 h and the equilibrium attained within 8 to 10 h.
Higher correlation value (R2) of 0.98 for second order kinetics indicates chemisorption
mechanism. It can be observed that up to 4 h, CACC beads follow second order kinetics; from 4
to 8 h first order kinetics is followed and thereafter again second order. However, for overall
duration of adsorption, pseudo second order model proved to be best fit with maximum correlation
value of 0.99. (12) The reason behind such dramatic shift of model can be attributed to the
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presence of porous AC and its higher rate of adsorption. Also, pseudo second order adsorption
constant for CACC beads was found to be almost 10 times higher than that of CAC beads, which
can be explained only by physio sorption of AC. Similarly, the adsorption was been examined forthe other three dyes.
Acid Tellon yellow FG01
From table 9 it is been observed that the rate of adsorption initially is higher and as time
progresses; it decreases for both the adsorbents. In case of CAC beads, adsorption capacity ofacid tellon yellow FG 01 was continued even after 8 h, unlike RR2 where equilibrium wasobserved within 8 h. Also, adsorption capacity for acid dye (42.19 mg/g) was observed to behigher as compared to Reactive dye(18.89 mg/g), which may be as a result of lower molecularweight of acid dye which helped in better penetration of dye molecule. In case of CACC beads,
rate of adsorption was observed to be very much more for initial 2 to 6 h, which gradually
increases until equilibrium is achieved after 16 h.
Table 09: Effect of contact Time of AC and CAC on Acid dye
Time
1
2
4
6
8
16
24
32

CAC
7.25
9.87
13.54
18.62
28.35
38.65
42.54
42.19

CACC
20.87
28.97
34.52
55.63
102.81105.61108.61112.89The mere observation from table 10 was been made that both adsorbents have higher
adsorption in acidic pH instead of alkaline. For CAC beads, adsorption was highest in pH rangeof 2 to 4, which then decreased up to pH 10 with no change thereafter till pH 12.
Table 10: Effect of pH on adsorption capacity of Acid dye
pH
2
4
6
8
10
12

Adsorption Capacity
CAC
42.12
46.37
35.09
16.52
12.61
10.82

CACC
104.23100.89100.02
92.8
87.56
75.62

The reason behind higher adsorption in acidic pH can be protonation of amine groups of
CMC molecule which will attract negative dye anions, similar to the anionic dye (Reactive dye).
In case of CACC beads are concerned, adsorption was highest (104.23 to 92.8 mg/g) in the rangeof pH 2 to 8, from where it decreases rapidly to 75.62 mg/g at pH 12. The increased range of pH(4 to 8) of maximum adsorption, observed in case of CACC beads, can be due to physicaladsorption by AC.
Table 11: Effect of adsorbate dosage on adsorption capacity of Acid dye
Initial Concentration 400mg/l, Contact Time 16hrs, pH:6
Adsorbent Dosage (g/50ml) of dye solution
Adsorption Capacity in mg/L
CAC
CACC
0.05
50.32
72.54
0.1
28.25
67.16
0.15
24.3
56.35
0.2
19.45
52.46

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From table 11, it is been observed that CAC beads adsorption capacity decreased from50.32 mg/g to 19.45 mg/g as adsorbent dosage is increased from 0.05 to 0.2 g/ 50 ml dye solution,
whereas in case of CACC beads, adsorption capacity decreased from 72.54 mg/g to 52.46 mg/g.
It can be justified as increase in adsorption dosage is causing decrease the adsorption density.
This is due to the lower amount of the dye available per unit mass of adsorbent.
From table 12, observation is been made that adsorption capacity increased linearly from27.45 mg/g to 79.82 mg/g, with increase in concentration of AC in beads. The rate of increase indye adsorption in case of acid dye is lower compared to that of reactive dye. This may be due tomolecular weight difference. As in case of reactive dye , molecular weight is higher compared toacid dye , hence reactive dye was observed to have higher affinity for AC and hence higher rateof adsorption.
Table 12: Effect of Adsorbent Dosage on Adsorption Capacity of Acid Dye
Initial Concentration 400mg/l, Contact Time 16hrs, pH:6
AC Loading g / g of CMC
Adsorption Capacity, mg/g
0
27.45
2.5
42.61
5
57.21
7.5
64.38
10
79.82

Table 13: Adsorption Isotherm for Adsorption of Acid Dye
Isotherm

LangmuirFreundlich

TemkinParameters
Q 0, mg/g
B, L/mg
R2
RL
n
Kf, (mg/g) (L/mg)1/n
R2
Bt, J/mol/kAt, L/g
R2

CAC
29.87
0.01080.96
0.3084
4.35
6.48
0.91
517.08
0.27
0.94

CACC
155.610.00260.95
0.6234
2.08
4.18
0.97
73.47
0.02
0.93

On the basis of R2 values, it can be concluded that applicability of the model in case of
CAC was in following order, Langmuir > Temkin > Freundlich. Hence Langmuir was found to be
the best suited model for CAC beads. It indicates homogeneous structure of adsorbent. Also,
sorption is taken place at definite sites, indicating presence of chemisorption. The CACC beads
were observed to follow Freundlich isotherm model with correlation coefficient of 0.97, rather thanLangmuir model (0.95) and Temkin model (0.93). Applicability of Freundlich model denotes
presence of heterogeneous surface because of both AC and CMC. Also, it can also be stated that
CACC beads are following multilayer adsorption, which can be main reason behind such higher
adsorption abilities of CACC.
It can be denoted from correlation coefficient value of 0.94 that CAC beads are following
pseud second order kinetics instead of pseudo first order kinetics (0.86) and intra particle diffusion(0.93). It is been observed that for initial 8hr CAC beads are following intraparticle diffusion andonce equilibrium is reached its following first order kinetics. In case of CACC beads, it can beobserved that adsorbent is following intra particle diffusion for 16 h and once equilibrium isachieved it is following second order adsorption.

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Table 14 : Adsorption Kinetics for Adsorption of Acid dye
Kinetic ModelFirst-order

Second-order

Intra-particle

Experimental

Parameter
K1, mg/g/min
qeq, mg/g
R2
K2, mg/g/min
qeq, mg/g
R2Kid, mg/g/√t
I, µg/gqeq, mg/g
R2qeq, mg/g

CAC-2.56× 10^-03
42.87
0.86
3.29 X10-05
54.68
0.94
-0.74
1.08
50.19
0.93
43.6

CACC
-1.42× 10^-03
107.150.87
8.72 X10-06
130.58
0.97
-6.29
2.35
104.21
0.98
102.48Conclusions
The synthesis of activated carbon beads using corn husk agricultural waste and CMC biopolymer
for studying the adsorption characteristic of reactive ultra-orange dye, acid tellon yellow FG01 ,basic coracryl red and direct red dye is been carried out successfully. The CMC beads werecrosslinked with calcium chloride forming ionic bond, studies showed an increase in adsorption
capacity as compared to the non-crosslinked CMC beads. The variable pH range of crosslinked
beads i.e., from 2 to 12 makes its suitable for actual textile effluent which is generally alkaline innature. The CAC beads are following Langmuir adsorption isotherm irrelevant of the adsorbate.
While the CACC beads are following Freundlich for acid and basic dye on the basis of coefficientof correlation values while reactive and direct dye are following both Freundlich and Langmuir
isotherm due to presence of activated carbon. The kinetics were also been studied for both CAC
and CACC beads showing second order kinetics for both the adsorbent indicating chemisorption.
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