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Nanocomposites adsorbents were fabricated from different types of plant biomass and functionalized multiwalled carbon nanotubes decorated with silver nanoparticles (Ag/f-MWCNTs).  A set of adsorption experiments were performed to determine the effect of solution pH, agitation time, adsorbate temperature, adsorbent dose, initial dye concentration, and desorption of the dyes in order to validate the efficiency of these nanocomposites to eliminate rhodamine B (RhB) and malachite green oxalate (MGO) from aqueous solution.  The results obtained showed an increase in RhB and MGO uptake with increased contact time, adsorbent dose, and initial concentration of RhB or MGO.  The optimum uptake was observed at pH 3 for RhB and pH 7 for MGO.  Kinetics studies showed that the adsorption of MGO and RhB proceeded according to the pseudo-second order and Elovich models, respectively.  Equilibrium data obtained from the uptake of RhB and MGO were best described by the Langmuir and Sips isotherm models.  The thermodynamic parameters (ΔG°, ΔH° and ΔS°) of the adsorption process revealed that the uptake of RhB and MGO by the adsorbents was entropy-driven, feasible, and spontaneous.  The composites demonstrated higher uptake capacities than Ag/f-MWCNTs for the removal of MGO.  Meanwhile, the reverse was the case in the elimination of RhB.  The nanocomposite materials demonstrated good capacity to eliminate MGO and RhB from aqueous systems, and have shown the ability to be reused.  Hence, these nanomaterials are suitable for wastewater treatment at the industrial scale.


Title Page                                                                                                                            i

Declaration                                                                                                                         ii

Certification                                                                                                                        iii

Dedication                                                                                                                          iv

Acknowledgement                                                                                                             v

Abstract                                                                                                                              vi

Table of content                                                                                                                  vii

List of Tables                                                                                                                      viii

List of Figures                                                                                                                    ix

Abstract                                                                                                                              x




1.1 Background of the Study                                                                                             1

1.2 Statement of the Problem                                                                                             2

1.3 Aim and Objectives                                                                                                      4

1.4 Justification of the Study                                                                                             5

1.5 Scope of the Study                                                                                                       5




2.1 General Outline of Dyes                                                                                               6

2.1. Organic Dyes in Water                                                                                                6

2.1.1. Rhodamine B                                                                                                            6

2.1.2. Malachite green oxalate                                                                                            7

2.2. Conventional Methods of Removing Organic Dyes                                                   8

2.2.1. Photodegradation                                                                                                     8

2.2.2. Chemical oxidation                                                                                                   9

2.2.3. Biological treatment of organic dyes                                                                        9

2.3. Adsorption                                                                                                                   10

2.3.1. Types of adsorption                                                                                                  10 Physical adsorption (Physisorption)                                                                      10 Chemical adsorption (Chemisorption)                                                                   11



3.1. Materials                                                                                                                      13

3.1.2 Chemicals                                                                                                                  13

3.2. Preparation of Composite Samples (Biomass-Ag/f-MWCNTs)                                  13

3.3. Characterization of Adsorbent                                                                                    14

3.4 Adsorbate Preparation                                                                        14

3.5 Determination of Dye Concentrations                                                                         14

3.6 Batch Adsorption Experiments                                                                                    14

3.6.1. Kinetics studies                                                                                                        15

3.6.2. Adsorption isotherms                                                                                               16

3.6.3. Desorption studies                                                                                                                                            18

3.7. Data Analysis                                                                                                                                                        18




4.1. Characterization of Pristine and Dye-loaded Adsorbents                                           19

4.2. Batch Adsorption Experiments                                                                                     32

4.2.1. Effect of PH                                                                                                             32

4.2.2. Effect of adsorbent dose                                                                                          35

4.2.3. Effect of contacts time                                                                                             37                            

4.2.4. Adsorption kinetics                                                                                                  39

4.2.5. Effect of initial concentration of RhB or MGO                                                       47

4.2.6. Effect of solution temperature                                                                                 47

4.2.7. Adsorption isotherm                                                                                                 48     

4.2.8. Thermodynamic parameters of adsorption                                                               59

4.2.9. Desorption studies                                                                                                    63




5.1 Conclusion                                                                                                                    64

5.2 Recommendations                                                                                                        64                    








2.1:  Distinctions between physisorption and chemisorption                                                 10     

3.1: Kinetics models investigated for the adsorption of RhB and MGO                                15

3.2: Isotherm models used to describe the uptake of RhB or MGO by AMC, FEC, AXC, AMB, FEB, AXB, and Ag/f-MWCNTs.                                                                                                              17                              

4.1: Kinetics parameters for the adsorption of MGO onto AMC, AMB, FEC, FEB, AXC, AXB and Ag/f-MWCNTs adsorbents                                                                                                     42                                  

4.2 Kinetics parameters for the adsorption of RhB onto the adsorbents AMC, AMB, FEC, FEB, AXC, AXB and Ag/f-MWCNTs.                                                                                                              43                               

4.5   Comparison of the Langmuir maximum adsorption capacities for RhB and MGO onto AMC, AMB, FEC, FEB, AXC, AXB and Ag/f-MWCNTs with those of other sorbents.                                  50                                                                                  

4.6: Isotherm parameters for the adsorption MGO onto the adsorbent AMC, AMB, FEC,FEB,AXC,AXBandAg/f-MWCNTs.                                                                                                                    53                                                

4.7:  Isotherm parameters for the adsorption RhB onto the adsorbents AMC, AMB, FEC, FEB, AXC, AXB and Ag/f-MWCNTs                                                                                                               56            

4.8: Thermodynamic parameters for the adsorption of RhB and MGO onto AMC, AMB, FEC, FEB, AXC, AXB and Ag/f-MWCNTs.                                                                                                     61         

4.9  Percentage desorption of RhB and MGO by using ethanol or acetone [Experimental conditions: 10 cm3 of either acetone or ethanol, 50 mg of (RhB or MGO)-loaded absorbent, agitation speed 120 rpm, contact time 30 min, and solution temperature 22 °C].                                                                       63










2.1: Structure of rhodamine B [molar mass: 479.02 g mol-1; acid dissociation constant (pKa): 3.71; solubility in water: 15 g dm-3; density: 1.31 g cm-3 (20 °C); melting point:210-211°C](33)                6

2.2: Malachite green oxalate (MGO) [molar mass: 927.02 g mol-1; acid dissociation constant

       (pKa): 6.9; solubility in water: 60 g dm-3; melting point: 164 °C]                                                     

4.1   Raman spectra of pristine adsorbent and RhB-loaded adsorbent                                   20

4.2   Raman spectra of pristine adsorbent and MGO-loaded adsorbent                                 22

4.3   FTIR spectra of unloaded adsorbents compared with the spectra of RhB and MGO-loaded adsorbents                                                                                                                                       23                                                                                    

4.4     (a)  FESEM micrographs of RhB-loaded absorbents compared with the pristine adsorbents              26                                                                                                                                                   

4.4     (b) FESEM micrographs of RhB-loaded absorbents compared with the pristine adsorbents. 26                                                                                                                             

4.5     (a) FESEM micrographs of MGO-loaded absorbents compared with the pristine adsorbents             27                                                                                         

4.5     (b) FESEM micrographs of MGO-loaded absorbents compared with the pristine adsorbents 28                                                                                        

4.6     FTIR spectra of AMC, AMB, FEC, FEB, AXC, AXB, Ag/f-MWCNTs and Funtumia elastica plant extract.                                                                                                                           31

4.7    Effect of pH on the adsorption of (a) MGO and (b) RhB onto AMC, AMB, FEC, FEB, AXC, AXB and Ag/f-MWCNTs [conditions: 25 cm3 of 100 mg dm-3 RhB or MGO, 24 h equilibration time, 50 mg adsorbent dose, agitation speed 120 rpm, temperature 22 °C]. 34                                                                              

4.8  Effect of adsorbent dose on the adsorption (a) MGO and (b) RhB by AMC, AMB, FEC, FEB, AXC, AXB and Ag/f-MWCNTs [conditions: 25 cm3 of 100 mg dm-3 MGO/RhB, 24 h equilibration time, pH  7 (MGO) and pH 3 (RhB), agitation speed 120 rpm, temperature 22 °C].                                      36      

4.9 Effect of contact time on the adsorption of (a) MGO and (b) RhB by AMC, AMB, FEC, FEB, AXC, AXB and Ag/f-MWCNTs [conditions: 25 cm3 of 100 mg dm-3, equilibration time, pH 7 (MGO) and pH 3 (RhB), agitation speed 120 rpm, temperature 22 °C].                                                                  38                                                       

4.10  Comparison of the various kinetics models fitted to the experimental data of MGO        onto (a) AMC, (b) AMB, (c) FEC, (d) FEB, (e) AXC, (f) AXB and (g) Ag/f-MWCNTs and (pseudo-first order, pseudo-second orde, intraparticle diffusion, Elovich  ).                                                               45                                                                                                                              

4.11  Comparison of the various kinetics models fitted to the experimental data of RhB onto (a) AMC, (b) AMB, (c) FEC, (d) FEB, (e) AXC, (f) AXB and (g) Ag/f-MWCNTs (pseudo-first order, pseudo-second order, intraparticle diffusion, Elovich).                                                                         46    

4.12  Effect of temperature on the adsorption of RhB onto (a) AMC, (b) AMB, (c) FEC, (d) FEB, (e) AXC, (f) AXB and (g) Ag/f-MWCNTs [Conditions: 25 cm3 of 10 to 100 mg dm-3, 24 h contact time, 20 mg adsorbent dose, pH 3, agitation speed 120 rpm]                                                           51

4.13  Effect of temperature on the adsorption of MGO onto (a) AMC, (b) AMB,(c) FEC, (d) FEB, (e) AXC, (f) AXB and (g) Ag/f-MWCNTs [Conditions: 25 cm3 of 10 to 100 mg dm-3, 24 h contact time, 20 mg adsorbent dose, pH 7, agitation speed 120 rpm]                                                           52                                        





The discharge of coloured effluents produced from textile, leather, paper making, plastics, food, rubber, cosmetics, and dye manufacturing industries, into the aquatic body has posed a high degree of threat to man, plants and aquatic biota (fauna and flora) ( Hayeeye et al., 2017).  This is due to the non-biodegradable nature of some of the pollutants and their stability to light, heat, and oxidizing agents ( Wang et al., 2006).  Effluents are composed of different kinds of pollutants ranging from dyes to heavy metal ions.  These pollutants bio-accumulate in plants and in most cases lead to phytotoxicity of the plants.  However, the food chain creates a link through which man ingests these pollutants, and hence, health challenges such as pain, vomiting, skin irritations, severe headaches, and acute diarrhoea are inevitable ( Baek, et al., 2010).  

Most dyes used in the industries are designed to be very reactive and are known to have good properties that make their demand and application high.  Meanwhile, these dyes are very problematic due to their high solubility.  About 20-40% of the widely used cationic dyes are often discharged alongside with industrial effluents; acid dyes are also very difficult to remove from wastewater, these challenges are often blamed on the high solubility of these dyes ( Konstantinou and Albanis, 2004, Choy et al., 2004).  Basic dyes are not exempted, as they are the brightest class of dyes with high tinctorial values ( Inbaraj and Sulochana, 2006).  The colour impact of dyes on water bodies reduces the penetration of light into the water bodies, hence the dissolved oxygen and photosynthetic processes are negatively affected, and this affects the growth of aquatic organisms ( Huang et al.,2008). Hence, this study seeks to fabricate nanocomposite materials as potential agents for decontamination.  To accomplish this, acid-functionalized multiwalled carbon nanotubes decorated with metallic silver nanoparticles were sandwiched and modified with plant biomass to enhance the binding affinity of the adsorbents as well as the antimicrobial potential of the nanocomposites.



In the aquatic ecosystem, bioaccumulation and bio-magnification aid the stability of these hazardous materials in the food web (Gupta et al.,1990, Halliday and Beszedits, 2006).  In humans, the toxicological implication of these substances when ingested include, but are not limited to, biochemical, physiological or behavioural defects (Patil and Shinde, 1988 ; Lian et al., 2009). Meanwhile, above the threshold limits of these contaminants, disastrous environmental and ecological problems are also inevitable ( Tsai et al., 2013).  The water body receives a vast amount of dyes and heavy metals from industrial activities such as printing, mining, smelting, electroplating, steel smelting and the manufacturing of fertilizers, pesticides, herbicides, alloys, pulp, ceramics, glass, textiles, and leather, amongst others (Wahi et al, 2005, Mittal et al.,2009, Asfour et al., 1985).

In this work two cationic dyes were of interest.  Considerable research has been carried out on the effect of exposure to high concentrations of RhB or MGO.  These studies have demonstrated the high potential of RhB or MGO to cause cancer, neurotoxicity, and reproductive and developmental diseases in man ( Dawood and Sen, 2012)The intravenous median lethal dose (LD50) of RhB and MGO are very small, this indicates how toxic both dyes can be.  Hence, the need for necessary safety measures for the usage of MGO and RhB is important ( Mittal and Mishra 2014).  Several methods, which include chemical oxidation ( Neamtu et al., 2004), reverse osmosis ( Gupta et al.,1990), coagulation and flocculation ( Halliday and Beszedits  1986), biological treatments ( Patil and Shinde 1988), and photo-degradation  ( Lian et al 2009,  Baek et al, 2010, Tsai et al, 2013, Wahi  et al., 2005), have been developed for the removal and recovery of dyes from wastewater.  Some of these methods are known to have limitations such as high cost of maintenance, high energy consumption, longer retention time, ineffective at low dye concentrations and generation of secondary waste.  Hence, there is an urgent need for the development of effective and economically viable technologies for the removal of dyes from wastewater.  Adsorption is quite popular due to its user-friendly nature and high efficiency, as well as the accessibility of a wide range of adsorbents.  It is worth mentioning that activated carbon has demonstrated high competence for the removal of dyes from contaminated water (Mittal et al.,2009), however, this is due to the high porosity and large surface area of activated carbon.  Meanwhile, the drawback to the application of activated carbon in adsorption processes includes high cost and low regeneration efficiency.  Intensified efforts have therefore been geared towards the development of inexpensive and effective alternatives to activated carbon.  Materials such as wood ( Asfour et al., 1985), Fullers earth and fired clay ( McKay et al.,1987), fly ash ( Khare et al, 1987), biogas waste slurry ( Namasivayam and Yamuna, 1992, Namasivayam and Yamuna (1992), waste orange peel ( Namasivayam et al., 1996 ), banana pith ( Namasivayam,and Kanchana  1992), peat ( Ramakrishna and Viraraghavan,  1997), chitin ( Mc Kay et al, 1983), chitosan ( Juang et al, 1997), silica (McKay,1984), jute stick powder ( Panda  et al., 2009), peanut hull ( Gong et al., 2005), jute processing wastes (.Banerjee  and Dastidar, 2005), soy meal hull ( Arami, et al., 2006), rice husks ( Mckay et al., 1987), maize stalks ( Meye  et al., 1992), hazelnut shells ( Doğan  et al., 2006), bottom ash and de-oiled Soya ( Gupta et al., 2009, Gupta et al.,2006), wheat bran and rice bran (. Wang and Chen, 2009), jackfruit peel ( Hameed, 2009), spent brewery grains ( Jaikumar, 2009), sunflower seed hull ( Thinakaran, 2008) and papaya seeds (Hameed, 2009), Guava (Psidium guajava) leaf powder ( Ponnusami et al.., 2008), Posidonia oceanica (L.) fibers . (Ncibi et al., 2008). pumpkin seed hull ( Hameed and  El-Khaiary, 2008), amongst many other examples, have been applied as adsorbents for the removal of dyes from aqueous solutions.  However, there are scarce or no report on the application of agro-waste materials as adsorbent modifiers.

Since Iijima re-discovered carbon nanotubes (CNTs) in 1991, CNTs have been intensively studied.  Due to their unique physical and chemical properties, CNTs have been used in different fields for a variety of applications ( Fagan et al., 2004, Ajayan, 1993).  The effectiveness of CNTs for the uptake of organic and inorganic pollutants have been studied and the results obtained were comparable to carbon-based adsorbents that are used for commercial applications ( Kerdnawee et al., 2017).  Metal doped multiwalled carbon nanotubes (M/MWCNTs), commonly described as nanohybrids, have found extensive application in the medical field as the MWCNTs play the role of a delivery agent for the zero-valent metal, which turns ionic in the cytoplasm of a bacteria cell.  Of the various metals, silver nanoparticles, in particular have been extensively employed in diverse areas such as, biological labelling, surface enhanced Raman scattering (SERS), photography optoelectronics, catalysis, photonics, antimicrobial agents, and water remediation practices ( Sun and Xia, 2002, Taheri et al., 2014).  Metallic silver-decorated multiwalled carbon nanotubes (Ag/f-MWCNTs) may find good environmental application as adsorbents for water decontamination and as water disinfectant.

Treatment of wastewater before discharge is the only way to ensure a comprehensive healthy ecological environment.  To achieve this, Annona muricata petals (AMB), Funtumia elastica husk (FEB), and Acacia xanthophloea stem bark (AXB) were used to modify the nanohybrid, Ag/f-MWCNTs, and form nanocomposite, materials, namely, Annona muricata petal composite (AMC), Funtumia elastica husk composite (FEC) and Acacia xanthophloea stem bark composite (AXC) respectively.  These nanocomposite materials (AMC, FEC, and AXC) were investigated as low-cost adsorbents for the removal of RhB and GMO from aqueous solution.  The effects of influential parameters, such as agitation time, adsorbent dose, initial adsorbate concentration, solution pH, and solution temperature were studied.  To the best of our knowledge, the application of agro-waste as adsorbents modifier has not been exhaustively researched and hence this investigation pursues and discusses the potential of low-cost adsorbents fabricated from silver nanoparticles, MWCNTs and agro-waste (modifiers) for the removal of RhB and MGO from simulated wastewater.



This study aims to synthesize novel nanocomposites with good polarity and excellent dispersion in the aqueous phase that also possess decontamination properties.  This is hoped to be achieved by carrying out the following objectives.

(1)       To functionalize commercially obtained pristine-MWCNTs with a mixture of concentrated nitric and sulphuric acids,

(2)       To synthesize metallic silver nanoparticle decorated functionalized multiwalled carbon nanotubes by making use of the extract from the husk of the Funtumia elastica plant (nanohybrid (Ag/f-MWCNTs)),

(3)       To modify the metallic silver nanoparticle decorated multiwalled carbon nanotubes with Funtumia elastica husk (FEB), Annona muricata petals (AMB), or Acacia xanthophloea stem bark (AXB) so as to enhance the polarity and water dispersibility of the composites,

(4)       To characterize the composites by making use of techniques such as transmission and scanning electron microscopy, and Fourier transform infrared spectroscopy (FTIR), and Raman spectroscopy,

(5)       To evaluate the adsorption potential of the composites, modifiers, and Ag/f-MWCNTs for the removal of rhodamine B (RhB), and malachite green oxalate (MGO) from aqueous solution, considering the influence of pH, contact time, adsorbent dose, initial adsorbate concentration and temperature on the adsorption process,



Anthropogenic activities involving the introduction of chemical, physical, microbial and radioactive substances into aqueous media are responsible for increased pollution, hence, exacerbating the scarcity of clean water. Wastewaters containing several toxic pollutants are regularly generated by industries, and are taken through little or no further treatment before their disposal into the environment. Unfortunately, most pollutants are water soluble and eventually end up in groundwater, rivers, streams and oceans through various natural processes. Water pollution before limits the availability of water, posing serious environmental and health challenges to its dependents and can lead to death and the spread of diseases. To avert this problem, a crucial need exists for the remediation of wastewater produced by industries in order alleviate water scarcity and generate freshwater to cater for human needs.



This concept was adopted to produce AMC, FEC, AXC, AMB,M FEB, AXB and -Ag/fMWCNTs for the removal of the RhB and MGO from aqueous solutions.


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