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UNIVERSITI PUTRA MALAYSIA
ALI REZA GOLESTAN BAGH
FK 2015 10
ADSORPTION OF ACID GREEN 25 DYE SOLUTION USING MODIFED AND UNMODIFIED KENAF FIBER
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ADSORPTION OF ACID GREEN 25 DYE SOLUTION USING MODIFED
AND UNMODIFIED KENAF FIBER
By
ALI REZA GOLESTAN BAGH
Thesis Submitted to the School of Graduate Studies, Universiti Putra Malaysia,
in Fulfilment of the Requirements for the Degree of Master of Science
July 2015
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COPYRIGHT
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icons, photographs and all other artwork, is copyright material of Universiti Putra
Malaysia unless otherwise stated. Use may be made of any material contained within
the thesis for non-commercial purposes from the copyright holder. Commercial use
of material may only be made with the express, prior, written permission of
Universiti Putra Malaysia.
Copyright © Universiti Putra Malaysia
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DEDICATION
There are a number of people without whom this thesis might not have been written,
and to whom I am greatly indebted. First and foremost I would like to dedicate this
work to my beloved parents Mrs Hossein and Ms Fariba for providing me with the
opportunity to engage in this project. Without their support I may not have found
myself at Univerciti Putra Malaysia. And also my lovely fiancee SHIRIN for her
unfailing support.
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Abstract of thesis presented to the senate of Universiti Putra Malaysia in fulfilment
of the requirement for the degree of Master of Science.
ADSORPTION OF ACID GREEN 25 DYE SOLUTION USING MODIFED
AND UNMODIFIED KENAF FIBER
By
ALI REZA GOLESTAN BAGH
July 2015
Chairman: Intan Salwani Ahamad, PhD
Faculty: Engineering
Dyes are used widely as coloring in many industries, such as textiles, cosmetics,
leather, printing, foods and plastics. Acid dye comprise the largest class of dye in the
Color. Acid green 25 in particular belongs to the commercial acid dye often used in
textile, hair dye formulation and cosmetic product. The removal of pollutants from
wastewaters is a matter of great interest in the field of water pollution. Amongst the
numerous techniques of pollutant removal, adsorption is an effective and useful
process. In the past few years many approaches have been studied for the
development of low cost and effective adsorbents. Kenaf is one of the best natural
fibers used as adsorbent in adsorption process. The treatment on natural fibres is
widely being used to modified the cellulosic molecular structure. In this study, an
attempt is made the chemical modification characteristics of kenaf fiber. In order to
enhance the adsorption capacity, kenaf fibers have been treated with sodium
hydroxide and trimethylammonium chloride (CHMAC) coupling agent. The
charactristics of kenaf fiber was obtained by using Fourier transform infra-
red(FTIR),scanning electron microscopy ( SEM) , EDX, BET And CHNS-O and the
presence of functional groups such as hydroxyl,amine,lignin and carbonyl group
were detected. In this research adsorption of AG 25 dye on modified and un-
modifed kenaf consider as a problem statement. The samples was investigated under
different pH, dosage of adsorbent, initial dye concentration, contact time and
temperature. The un-modified kenaf adsorbed the maximum amount of 107 mg/g of
AG25 from aqueous solution at pH of 2, temperature of 30 ○C, contact time of 180
min and dosage adsorbent of 0.8 g/l. At the same condition modifed kenaf adsorbed
around 163.94 mg/g of AG25 respectively. According the UV test that was done
befor and after adsorption it was found that Separation of AG25 was carried out
successfully by using a modified kenaf. Equilibrium isotherms and kinetic models
have been measured to assess the capacities of both modify and un-modify kenaf for
AG25 for the sorption process. By comparing the correlation coefficients determined
for each linear transformation of the isotherm analysis of the study revealed that
adsorption behavior was best described by Freundlich model for all modified and un-
modified samples. Lagergren-first-order, Pseudo-second-order and Intraparticle
diffusion models were applied to determine the kinetics of the adsorption process.
Pseudo-second order results showed higher coefficient of determination (R2 >0.99)
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values compare to the Lagergren-first-order. The adsorption capacity of the kenaf
fiber increases with the increase in experimental temperature from 303K to 333K.
The negative values of ∆G and positive ∆H obtained indicated that the AG25 dye
adsorption process is a spontaneous and an endothermic.Based on the data od
present investigation,it was concluded that the modified kenaf fiber can be an
effective eco-feiendly and low cost adsorbent to remove acid dye from colored
aqueous solution.
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Abstrak tesis yang dikemukakan kepada senat Universiti Putra Malaysia sebagai
memenuhi keperluan untuk Ijazah Master Sains
PENJERPAN OF ACID GREEN 25 DYE SOLUTION USING MODIFED
AND UNMODIFED KENAF FIBE
Oleh
ALI REZA GOLESTAN BAGH
Julai 2015
Pengerusi: Intan Salwani Ahamad, PhD
Fakulti : Kejuruteraan
Secara umumnya, pewarna telah digunakan secara meluas didalam pelbagai industri
seperti pembuatan plastik, fabrik, kulit, mahupun dalam proses pembuatan makanan.
Asid pewarna merupakan kelas yang terbesar didalam kategori pewarna. Asid hijau
25 adalah merupakan bahan utama yang digunakan didalam industri pembuatan
fabrik, kosmetik, kulit, plastik, pewarna rambut dan juga makanan. Di dalam
konteks pencemaran air, kesan pembuangan bahan tercemar dari sisa kumbahan
merupakan suatu penemuan amat menakjubkan. Dikalangan teknik teknik
pembuangan sisa bahan pencemar, teknik penyerapan adalah merupakan teknik yang
sangat efektif dan berkesan untuk digunakan didalam proses tersebut. Beberapa
tahun sebelumnya, banayk kajian telah dijalankan bagi menghasilkan bahan
penyerap yang efektif dan rendah kos penghasilan. Kenaf merupakan salah satu
daripada gentian semula jadi yang terbaik digunakan sebagai adsorben dalam proses
penjerapan. Rawatan menggunakan gentian asli telah digunakan secara meluas untuk
mengubahsuai struktur molekul selulosa. Dalam kajian ini, usaha pengubahsuain ciri
ciri kenaf menggunakan bahan kimia akan dijalankan. Dalam usaha untuk
meningkatkan kapasiti penjerapan, gentian kenaf telah dirawat dengan natrium
hidroksida dan trimethylammonium klorida (CHMAC). Ciri ciri gentian kenaf telah
diperolehi dengan menggunakan Fourier mengubah infra-merah (FTIR), mikroskop
imbasan elektron (SEM), EDX, BET Dan CHNS-O dan kehadiran kumpulan seperti
hidroksil, amina, lignin dan karbonil kumpulan telah dikesan. Dalam penyelidikan
ini, penjerapan pewarna AG 25 terhadap normal kenaf dan kenaf yang diubahsuai
merupakan penyataan masalah dalam penyelidikan ini. Sampel bagi penyelidikan
telah disiasat mengikut pH yang berbeza, dos bahan penjerap, kepekatan pewarna
awal, masa sentuhan dan suhu. Melalui penyelidikan yang dijalankan, kenaf yang
asli menerjerap jumlah maksimum 107 mg / gAG25 daripada larutan akueus pada
pH 2, suhu 30○ C, masa sentuhan 180 min dan dos adsorben sebanyak 0.8 g / l. Pada
keadaan yang sama, kenaf yang telah diubahsuaikan mampu terjerap sekitar 163.94
mg /g AG25. Melalui ujian UV yang dilakukan pada sebelum dan selepas
penjerapan didapati pengasingan AG25 telah dilaksanakan dengan jayanya dengan
menggunakan kenaf yang diubahsuai. Selain dari itu, suhu keseimbangan dan model
kinetic juga telah diukur bagi menilai kapasiti kedua-dua kenaf yang diubahsuai dan
yang tidak diubahsuai untuk AG25 bagi proses penyerapan tersebut. Dengan
membandingkan pekali korelasi ditentukan bagi setiap transformasi linear, analisis
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garisan suhu kajian menunjukkan bahawa tingkah laku penjerapan telah
digambarkan oleh model Freundlich bagi semua sampel yang diubahsuai dan tidak
diubahsuaikan. Bagi menentukan prosese kinetic penjerapan, tindakan Lagergren
pertama, Pseudo tertib kedua dan model resapan intrapartikal telah digunakan.
Kajian menunjukkan keputusan perintah Pseudo-kedua menunjukkan pekali tinggi
penentuan (R2> 0.99) nilai dibandingkan dengan tindakan Lagergren pertama. Dari
eksperimen yang dijalankan , didapati kapasiti penjerapan gentian kenaf meningkat
dengan peningkatan suhu dari 303K ke 333K. Manakala nilai-nilai negatif yang
diperoleh dari ΔG dan ΔH positif menunjukkan bahawa AG25 proses penjerapan
pewarna adalah spontan dan endotermik. Oleh itu, berdasarkan penyiasatan yang
telah dijalankan, secara kesimpulannya gentian kenaf yang diubahsuai adalah
berkesan, mesra alam dan rendah kos dimana ia berkesan untuk mengeluarkan asid
pewarna daripada larutan akueus berwarna.
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ACKNOWLEDGEMENTS
I wish to express my profound gratitude and thanks to my supervisor Dr. Intan
Salwni Binti Ahmad for her guidance and encouragement throughout the duration of
the study. Gratitude is also extended to my co-supervisor Prof. Dr. Luqman Chuah
b. Abdullah and Dr. Mohsen Nourouzi Mobareke for with helpful comments and
suggestions. This study has been supported by Universiti Putra Malaysia.
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This thesis was submitted to the Senate of the Universiti Putra Malaysia and has
been accepted as fulfilment of the requirement for the degree of Doctor of
Philosophy. The members of the Supervisory Committee were as follows:
Intan Salwni Binti Ahmad, PhD
Senior lecturer
Faculty of Engineering,
Universiti Putra Malaysia
(Chairman)
Luqman Chuah b. Abdullah, PhD
Professor
Faculty of Engineering
Universiti Putra Malaysia
(Member)
Mohsen Nourouzi Mobarakeh, PhD
Lecturer
Faculty of Engineering
Universiti Putra Malaysia
(Member)
BUJANG BIN KIM HUAT, PhD Professor and Dean
School of Graduate Studies
Universiti Putra Malaysia
Date:
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Declaration by graduate student
I hereby confirm that:
this thesis is my original work
quotations, illustrations and citations have been duly referenced
the thesis has not been submitted previously or comcurrently for any other
degree at any institutions
intellectual property from the thesis and copyright of thesis are fully-owned by
Universiti Putra Malaysia, as according to the Universiti Putra Malaysia
(Research) Rules 2012;
written permission must be owned from supervisor and deputy vice –chancellor
(Research and innovation) before thesis is published (in the form of written,
printed or in electronic form) including books, journals, modules, proceedings,
popular writings, seminar papers, manuscripts, posters, reports, lecture notes,
learning modules or any other materials as stated in the Universiti Putra Malaysia
(Research) Rules 2012;
there is no plagiarism or data falsification/fabrication in the thesis, and scholarly
integrity is upheld as according to the Universiti Putra Malaysia (Graduate
Studies) Rules 2003 (Revision 2012-2013) and the Universiti Putra Malaysia
(Research) Rules 2012. The thesis has undergone plagiarism detection software
Signature: Date
Name and Matric No: Ali Reza Golestan Bahg GS31058
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Declaration by Members of Supervisory Committee
This is to confirm that:
the research conducted and the writing of this thesis was under our
supervision;
supervision responsibilities as stated in the Universiti Putra Malaysia
(Graduate Studies) Rules 2003 (Revision 2012-2013) were adhered to.
Signature: Signature:
Name of Name of
Chairman of Member of
Supervisory Intan Salwni Binti Ahmad,
PhD
Supervisory Luqman Chuah b. Abdullah,
PhD Committee: Committee:
Signature:
Name of
Member of
Supervisory Mohsen Nourouzi Mobarakeh,
PhD Committee:
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TABLE OF CONTENTS
Page
ABSTRACT i
ABSTRAK iii
ACKNOLOWEDGEMENTS v
APPROVAL vi
DECLARATION viii
LIST OF TABLES xii
LIST OF FIGURES xiv
LIST OF ABBREVIATIONS xvi
CHAPTER
1
1 INTRODUCTION
1.1 Introduction 1
1.2 Problem statement 2
1.3 Research Objectives 3
1.4 Scope of Study 4
2 LITERTURE REVIEW 5
2.1 Water Pollution 5
2.2 Textile Dye 6
2.2.1 Introduction 6
2.2.2 Anionic Dye 7
2.2.3 Environmental detection 10
2.3 Adsorption process 13
2.3.1 Adsorption equilibrium 15
2.3.2 Langmuir isotherm 17
2.3.3 Error function 19
2.3.4 Adsorption Kinetic 19
2.3.5 Intra-particle diffusion model 21
2.3.6 Adsorption thermodynamics 22
2.4 Adsorbent 24
2.4.1 Bio sorbent 24
2.4.2 Kenaf 27
2.4.3 Modification 29
2.4.4 Quaternization on Lignocellulose Fiber 31
3 MATERIALS AND METHODOLOGY 35
3.1 Summary of work 35
3.1.1 Adsorbate 37
3.1.2 Adsorbent 37
3.1.3 Modification 38
3.2 Characterization 40
3.2.1 Boehm Titration 40
3.2.2 Point Zero Charge Determination 40
3.2.3 Preparation of dye calibration curve 40
3.2.4 CHNO-S Elemental Analysis 41
3.2.5 Scanning Electron Microscope (SEM) 41
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3.2.6 BET Analysis 41
3.2.7 Thermogravimetric Analysis (TGA) 42
3.2.8 Energy Dispersive X-Ray (EDX) Analysis 42
3.2.9 Fourier Transform Infrared (FTIR) Spectroscopy
Analysis
42
3.3 Adsorption Experiment 43
3.3.1 Preparation of stock solution 43
3.3.2 Effect of Mercerization 44
3.3.3 Effect of NaOH Ratio in Quaternization Reaction 44
3.3.4 Effect of Initial pH 44
3.3.5 Effect of Dosage 45
3.3.6 Effect of contact time 45
3.3.7 Isotherm Studies 45
3.3.8 Kinetics of the study 46
3.3.9 Effect of temperature 47
3.3.10 Effect of salt 47
4 RESULTS AND DISCUTION 48
4.1 Scanning Electron Microscope (SEM) 48
4.2 BET Analysis 50
4.3 CHNS-O Elemental Analyser 51
4.4 Thermo gravimetric Analysis (TGA) 52
4.5 Point Zero Charge (pHpzc) 55
4.6 Surface Chemistry 55
4.7 Fourier transform infrared spectroscopy (FTIR) 56
4.8 Energy Dispersive X-Ray (EDX) 58
4.9 Batch adsorption 59
4.9.1 Effect of PH 60
4.9.2 Effect of NaOH Mercerization 61
4.9.3 Effect of NaOH and CHMAC 62
4.9.4 Effect of Initial Dosage 63
4.9.5 Effect of contact time 64
4.9.6 Isotherm of the adsorption process 67
4.9.7 kinetik study 73
4.8 Thermodynamic studies 80
5 CONCLUSION AND RECOMMENDATION FOR
FUTUER RESEARCH
83
REFERENCES 84
APPENDICES 99
BIODATA OF STUDENT 103
PUBLICATION 104
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LIST OF TABLES
Table Page
2.1 Typical dyes used in textile dyeing operations.
7
2.2 Different study for removing acid green dye 25
10
2.3 Advantages and disadvantages of dye removal methods
12
2.4 Chemical and physical adsorption characteristics
15
2.5 Different types of Freundlich exponent
17
2.6 Various isotherm studies of dye adsorption by various agricultural
adsorbents
18
2.7 Different kinetic study on adsorption dye using agricultural waste
adsorbent
21
2.8 The effect of temperature on the adsorption of cationic and anionic
dyes by adsorbents based on agricultural solid waste.
23
2.9 Agricultural production in malaysia (Ton/year)
25
2.10 Pervious adsorption study by low cost adsorbent
26
2.11 Different adsorption study on kenaf
29
2.12 Different treatment on kenaf fiber 31
2.13 Some research done for removing water contaminant using
quaternized lignocellulose
33
3.1 Characteristic of AG25 dye
37
3.2 Chemical composition of kenaf fibers
38
3.3 Liner and non-liner kinetic equation
46
3.4 Thermodynamic equations
47
4.1 BET surface areas and pore volumes of un-modify and modify
kenaf
50
4.2 Classification of pore diameters
51
4.3 Elemental analysis by CHNS-O for kenaf
51
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4.4 Surface chemistry analysis for modified and un-modified kenaf
fibre
56
4.5 Elemental analysis of modified and un-modified kenaf by EDX
58
4.6 Different studies on dye removal by bio sorbent.
67
4.7 Category of equilibrium parameter RL
68
4.8 Liner and non-liner isotherm equation
68
4.9 Isotherm constant for linear models to removal AG25 by kenaf
71
4.10 Isotherm constant for nonlinear models to removal AG25 by kenaf
73
4.11 Linear and nonlinear form of kinetic model equation
74
4.12 Parameters of pseudo-first and pseudo-second order kinetic models
for adsorption of AG25 by un-modify kenaf.
78
4.13 Parameters of pseudo-first and pseudo-second order kinetic models
for adsorption of AG25 by modify kenaf.
78
4.14 Parameters of interparticl diffusion model for adsorption of AG25
by un-modify and modify kenaf
80
4.15 Effect of temperature parameter 82
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LIST OF FIGURES
Figure Page
2.1 Different type of acid dye structure
8
2.2 Molecular structure of AG25 dye
9
2.3 Fixation of dye on cellulosic fiber
10
2.4 Adsorption process
14
2.5
Cellulose structure
24
2.6 Kenaf plant
28
2.7 Lignocellulose quaternization reaction scheme
34
3.1 Flow chart for acid green dye adsorption process on kenaf fiber
36
3.2 Chemical treatment on raw kenaf fiber in producing modified
adsorbent.
39
4.1 SEM for kenaf
49
4.2 TGA plots for Modified kenaf
52
4.3 TGA plots for Un-Modified kenaf
53
4.4
DTG plot for modifed kenaf
53
4.5 DTG plot for un-modifed kenaf
54
4.6 The examine pHPZC of biosorbent for modified, and un-modified
kenaf
55
4.7
FTIR spectra of modified and un-modified kenaf
57
4.8 Effect of initial pH on removal ofAG25 by un-modified and
modified kenaf
60
4.9 Effect of NaOH in adsorption AG25
62
4.10 Effect of un-mofiied and modified kenaf dosage on removal of
AG25.
63
4.11
Effect of contact time for different concentration of AG25 on
adsorption by un-modified kenaf
65
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4.12
Effect of contact time for different concentration of AG25 on
adsorption by modified kenaf
65
4.13
Langmuir isotherm plots for un-modified kenaf
69
4.14
Freundlich isotherm plots for un-modified kenaf
69
4.15
Langmuir isotherm plots for modified kenaf
70
4.16
Freundlich isotherm plots for modified kenaf
70
4.17 Langmuir and Freundlich isotherm plots for un-modified kenaf
72
4.18
Langmuir and Freundlich isotherm plots for modified kenaf 72
4.19 Pseudo first-order kinetics plot for the adsorption of AG25 by un-
modified kenaf
75
4.20 First-order kinetics plot for the adsorption of AG25 by modified
kenaf
75
4.21
Pseudo-second-order kinetics plots for the adsorption of AG25
on un-modified kenaf
77
4.22 Pseudo-second-order kinetics plots for the adsorption of AG25
on modified kenaf
77
4.23
Intraparticle diffusion plots for the adsorption of AG25 on
modified kenaf
79
4.24
Intraparticle diffusion plots for the adsorption of AG25 for un-
modify kenaf
80
4.25
Effect of temperature on adsorption AG25 82
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LIST OF ABBREVATIONS
aF Freundlich constants
bF Freundlich constants
C constant
Ce equilibrium concentration (mg/L) of AG25 dye
C0 initial concentration (mg/L) of AG25 dye
q Adsorption
q0 Empirical Langmuir constant which represents
maximum adsorption capacity
qt Adsorption capacities at time t
qcal Calculated adsorption
qe Amount adsorbate adsorbed per unit weight of adsorbent
at equilibrium
qexp Experimental adsorption
R Universal gas constant (8.314 J/mol-K)
R2 Correlation coefficient
di diffusion coefficient (cm2/s)
∆S standard entropy of adsorption (J/mol K)
∆G standard Gibbs energy of adsorption (kJ/mol)
∆H standard enthalpy of adsorption (kJ/mol)
Kc equilibrium constant
Kf Freundlich multilayer adsorption capacity (mg/g)
kid intraparticle diffusion rate (mg/g min1/2)
KL Langmuir equilibrium constant of adsorption (L/mg)
k1 pseudo first order rate constants for adsorption
k2 pseudo second order rate constant (g/mg min)
M weight of adsorbent (g)
qe amount adsorbed on adsorbent (mg/g)
qm Langmuir monolayer adsorption capacity (mg/g)
qt amount adsorbed at time t (mg/g)
RL dimensionless equilibrium parameter
R2 correlation coefficient
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ɑL Langmuir isotherm constant (L/mg)
T temperature (K)
t time (min)
V volume (L)
pHpzc Point Zero Charge
SEM Scanning Electron Microscopy
BET Brunauer, Emmett and Teller
EDX Electron Dispersive X-ray
TGA Thermogravimetric Analysis
DTG Derivative thermal gravimetry
FTIR Fourier transform infrared
CHNS-O Carbon, Hydrogen, Nitrogen, Sulfur - Oxygen
Wt.% Weight percentage
pHf Final Ph
pHI Initial pH
∆pH pHi - pHf
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CHAPTER 1
INTRODUCTION
1.1 Introduction
Unsafe water and inadequate sanitation and hygiene are important
contributors to approaching 1.8 million deaths due to disease related to
pollution water every year (Clasen et al., 2014). Effectively manage the
safety of drinking water supplies are required in order to prevent waterborne
disease. Water suppliers in more than 40 countries are implementing
according to water and sanitation program, while over 20 countries have a
policy or regulation to promote water safety planning according to World
health organization(Gleick, 2014).
The discharge of dyes in the environment is a topic of worry for both
toxicological and esthetical reasons. Manufactures such as cloth, leather,
paper, credit cards and so forth use dyes in order to color their products and
also consume substantial volumes of water. Therefore, the presence of dyes
in effluents is a major concern due to their adverse effects on many forms of
life (Noroozi and Sorial, 2013).
It is recognized that public perception of water quality is greatly influenced
by the color. The color is the first contaminant to be recognized in
wastewater (Garg et al., 2004b). The presence of even very small amounts
of dyes in water less than 1ppm is, for some dyes, highly visible and
undesirable. It is estimated that more than 100,000 commercially available
dyes with over 7×105 tons of dyestuff are produced annually and this
effluent has high BOD loading and long lasting color that is aesthetically
and environmentally unacceptable (Allen et al., 2004). In Malaysia, the
Environmental Quality Act 1974 and Environmental Quality Regulations
1979 were set up to prevent irresponsible discharge of effluent from textile
industries into the watercourse (Aziz et al., 2007).
Various techniques have been employed for the removal of dyes from
wastewaters, such as coagulation, chemical oxidation, and membrane
separation process, electrochemical and aerobic and anaerobic microbial
degradation. Each of these methods have inherent limitations (Padhi, 2012).
Adsorption is a well-known equilibrium separation process and an effective
method for water decontamination applications. Adsorption has been found
to be superior to other techniques for water re-use in terms of initial cost,
flexibility and simplicity of design, easy of operation and insensitivity to
toxic pollutants (Feng et al., 2013). Adsorption also does not result in the
formation of harmful substances. The main adsorbent used in dye removal is
activated carbon. However, activated carbons are expensive due to their
regeneration and reactivation procedures (Namasivayam and Kavitha,
2002). In recent years, an inexpensive adsorption method has been
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developed for the removal of contaminates, which are highly toxic,
including dyes, from wastewater (McKay et al., 1999).
The low cost of agricultural waste adsorbents can be viable alternatives to
activated carbon for the treatment of contaminated wastewater containing
different classes of dyes. Anionic dyes include many compounds from the
most varied classes of dyes, which exhibit characteristic differences in
structure but possess a common feature; water-solubilizing, ionic
substituents (Ren et al., 2006).
Bio-adsorption processes are particularly suitable for the treatment of
solutions containing dye. Acid dyes are used with silk, wool, and
polyamide, modified acrylic and polypropylene fibers. They have good
water solubility. On the other hand, they have a harmful effect on human
beings since they are organic sulphonic acids (Attia et al., 2006).
Raw agricultural solid wastes such as leaves, fibers, fruits peels, seeds etc.
and waste materials from forest industries such as sawdust, bark etc. have
been used as adsorbents (Gong et al., 2005). Kenaf is one of the recent bio
sorbents currently being used for removing dye from waste water(Wang et
al., 2014). Kenaf is a warm-season, herbaceous plant originated from
Western Africa which can be related to cotton, okra and hibiscus. Many
potential uses for kenaf exist because of the unique properties of each type
of kenaf, constituted by sheaves of narrower fibers surrounded by a
lignocellulose cover. In order to increase the adsorption capacity of the
adsorbent, researchers have followed different modification methods (Akil
et al., 2011).
1.2 Problem Statement
Acid dyes which comprise the largest class of dye in the Color Index are
anionic compounds mainly used for dyeing nitrogen-containing fabrics like
wool, polyamide, modified acryl and silk. These compounds are the most
difficult to remove, even by activated carbon (Valix et al., 2004).
Acid Green 25 in particular belongs to the commercial acid dye often used
in textiles, hair dye formulation and cosmetic products. This dye has also
been known as Acid Green Anthraquinone (Ayad and El-Nasr, 2012).
Moreover, this dye has good water solubility (Cheung et al., 2007).
Activated carbon in particular is capable of adsorbing many different dyes
with high capacity. However, due to the high price and regeneration cost,
activated carbon is not a preferred adsorbent. Therefore, another cheaper
and more economical alternative adsorbent is needed and kenaf has been
identified (Cuerda-Correa et al., 2008).
Malaysia has realized the diverse possibilities of commercially exploitable
derived products from kenaf, and the National Kenaf Research and
Development Program has been launched in an effort to develop kenaf as a
possible new industrial crop for Malaysia(Edeerozey et al., 2007b). The
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government has allocated RM12 million for research and further
development of the kenaf-based industry under the 9th Malaysia Plan
(2006–2010) in recognition of kenaf as a commercially viable crop (Akil et
al., 2011).
Adsorption of dye using kenaf fiber has been studied by some researchers.
The adsorption ability of kenaf fiber can determined by chemical natural
and pore structure, which can also be improved by treatment. Chemical
modification or treatment of natural fibers, including kenaf, is generally
carried out using reagents which contain functional groups that are capable
of bonding with the hydroxyl group from the natural fibers (George et al.,
2001).
1.3 Research Objectives
There are several different kinds of raw and natural agricultural wastes
which have been used as a cheap adsorbent to remove dye from waste
water(Yagub et al., 2014). kenaf is a commodity crop grown in the
temperate and tropical areas. Previous findings indicated that plantation of
kenaf capable absorbs nitrogen and phosphorous that is present in the soil
and, also accumulates carbon dioxide at a significantly high rate(Ismail et
al., 2014) .Therefore, it has been actively cultivated in recent years,
especially for Malaysia. Generally, kenaf consists of an outer bast fiber and
inner core fiber. Between these two fiber layers, kenaf bast fiber is suitable
used for paper, textile and composite materials. In contrast, kenaf core fibers
mostly make into absorbent materials(Kamal, 2014). Recently, there is
growing interest to use kenaf as an adsorbent to remove pollutant from
wastewater(Akubueze et al., 2014). The adsorption capacity of kenaf
depends on many factors, such as raw materials, modification process, pore
structure and surface functionalities. Recent studies by various search
groups have shown that modified bio sorbents exhibit good potential for the
bio sorption of heavy metals and dyes from contaminate (Du et al., 2014).
The aim of this study is develop quaternized kenaf as novel adsorbent to
remove Acid green dye 25 (AG25) from aqueous solution. The objectives of
this study are:
1. To synthesize modified kenaf adsorbent by quaternization using N-(3-
chloro-2- hydroxyproply) trimethylammonium chloride (CHMAC) and
NaOH as quaternization agent.
2) Investigation of the effect of various parameters which include pH,
dosages of adsorbent, initial dye concentration and different contact
time, kinetics and thermodynamic study on AG25 adsorption behavior
of modified and UN-modified kenaf to find the optimal conditions for
highest dye adsorption capacity.
3. Compare modified and un-modified results to find evidence to prove the
effect of modification.
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1.4 Scope of Study
This thesis is divided into five chapters, followed by appendices at the end.
Chapter 1 describes a brief background on the status of water pollution and
its effects on plants and animals. It comprises the problem statements that
provide some basis and rational for identification of the research direction to
be followed. Chapter 2 (Literature Review) includes discuss of literatures
related to the removal of dye from aqueous solution. The comparison of the
similar work was tabulated for a clearer view. Chapter 3 describes the
materials and methods employed in this study. Chapter 4 (Results and
Discussion) shows all the observation and data collected from this study.
Chapter 5 establishes the conclusions and future work recommendations
from the current study. In this study, the surface of kenaf was modified with
NaOH and CHMNA, to increase the potential adsorption capacity of
modified kenaf. Characterization of the surface of un-modified and
modified was done through CHNS-O elemental analysis, Boehm surface
chemistry technique, Brunauer–Emmett–Teller (BET), thermo gravimetric
analysis (TGA) and fourier transform infrared spectroscopy (FTIR). The
adsorption behavior of AG25 on modifed and un-modified was studied
under different pH, dose of adsorbent, contact time and temperature by
using batch adsorption study. To optimize the design of an adsorption
system for the adsorption of adsorbates, it is important to establish the most
appropriate correlation for the equilibrium curves. Various isotherm
equations Such as Langmuir, Freundlich adsorption isotherms were studied.
In order to examine the controlling mechanism of adsorption processes such
as mass transfer and chemical reaction for the kinetic of adsorption AG25
on modified and un-modifed kenaf, pseudo-first–order, pseudo-second-order
and inter particle diffusion model were used.
The study of the equilibrium and isotherms, kinetics and mass transfer
model of the dye adsorption process were done to justify that modified
kenaf shows the highest adsorption property. Adsorption has become one of
the alternative treatment techniques for waste water containing dye.
Basically, adsorption is a mass transfer process by which a substance is
transferred from the liquid phase to the surface of a solid and becomes
bound by physical and chemical interactions (Kurniawan et al., 2006). In
this study, chemical modification was used to quaternized kenaf fiber and
uses it as an adsorbent to remove AG25 acid dye from aqueous solution.
Acid green 25 is an acid dye commonly found in waste water and is the
major by-product in textile process in Malaysia.
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