Some chemical groups involved in the metal-biomass interactions and their pKas. Source: (Eccles, 1999).
\r\n\tThis book will be a self-contained collection of scholarly papers targeting an audience of practicing researchers, academics, PhD students and other scientists. The contents of the book will be written by multiple authors and edited by experts in the field.
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China, in Computational Plasma, Materials and Experimental Fluid Materials, in 2015 and 2012. He also received the M.Phil and M.Sc (Physics) from University of Agriculture Faisalabad (UAF), which is a top-ranking institute in Pakistan. He has been proposed innovative techniques to explore outcomes of complex materials which show his aptitude to comprehend and grip Computational Physics, Molecular Modeling and Simulation techniques, and complex materials together with Experimental understandings. He has been published more than 32 international research papers in well reputed journals, 02 international books and 07 international book chapters, and has presented more than 70 research articles in well known national and international conferences. Currently, Dr. Shahzad is working as an Assistant Professor of Physics in Govt. College University Faisalabad (GCUF) since January 2005. 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Manguin",coverURL:"https://cdn.intechopen.com/books/images_new/3092.jpg",editedByType:"Edited by",editors:[{id:"50017",title:"Prof.",name:"Sylvie",surname:"Manguin",slug:"sylvie-manguin",fullName:"Sylvie Manguin"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"3794",title:"Swarm Intelligence",subtitle:"Focus on Ant and Particle Swarm Optimization",isOpenForSubmission:!1,hash:"5332a71035a274ecbf1c308df633a8ed",slug:"swarm_intelligence_focus_on_ant_and_particle_swarm_optimization",bookSignature:"Felix T.S. Chan and Manoj Kumar Tiwari",coverURL:"https://cdn.intechopen.com/books/images_new/3794.jpg",editedByType:"Edited by",editors:[{id:"252210",title:"Dr.",name:"Felix",surname:"Chan",slug:"felix-chan",fullName:"Felix Chan"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"16643",title:"Biosorption of Metals: State of the Art, General Features, and Potential Applications for Environmental and Technological Processes",doi:"10.5772/17802",slug:"biosorption-of-metals-state-of-the-art-general-features-and-potential-applications-for-environmental",body:'The interactions among cells and metals are present since the life origin, and they occur successfully in the nature. These interactions are performed on cellular envelope (walls and membranes) and in cellular interior. They are based on the adsorption and absorption of metals by cells for the production of biomolecules and in vital metabolic processes (Palmieri, 2001). Some metals such as calcium, cobalt, copper, iron, magnesium, manganese, nickel, potassium, sodium, and zinc are required as essential nutrients to life existence. The principal functions of metals are: the catalysis of biochemical reactions, the stabilization of protein structures, and the maintenance of osmotic balance. The transition metals as iron, copper, and nickel are involved in redox processes. Other metals as manganese and zinc stabilize several enzymes and DNA strands by electrostatic interactions. Iron, manganese, nickel, and cobalt are components of complex molecules with a diversity of functions. Sodium and potassium are required for the regulation of intracellular osmotic pressure (Bruins et al., 2000).
The interactions among metals and biomasses are performed through different mechanisms. For instance, on cellular envelope, the metal uptake occurs via adsorption, coordination, and precipitation due to the interaction among the surface chemical groups and metals in aqueous solution. Similar mechanisms are related in the exopolymeric substances (EPS). On the other hand, specific enzymes in some biomasses can change the oxidation state of the noxious metals followed by formation of volatile compounds, which removes the metal from aqueous solution. Finally, the life maintenance depends on the metal absorption by active transport according with the nutritional requirements of the biomass (Gadd, 2009; Palmieri, 2001; Sen & Sharadindra, 2009).
The removal of metallic ions of an aqueous solution from cellular systems is carried out by passive and/or active forms (Aksu, 2001; Modak & Natarajan, 1995). As such live cells as dead cells do interact with metallic species. The bioaccumulation term describes an active process that requires the metabolic activity of the organisms to capture ionic species. In the active process the organisms usually tend to present tolerance and/or resistance to metals when they are in high concentrations and/or they are not part of the nutrition (Godlewska-Zylkiewicz, 2006; Zouboulis et al., 2004).
Group | Occurrence | pKa |
Carboxylate | Uronic acid | 3-4.4 |
Sulfate | Cisteyc acid | 1.3 |
Fosfate | Polysaccharides | 0.9-2.1 |
Imidazol | Hystidine | 6-7 |
Hydroxyl | Tyrosine-phenolic | 9.5-10.5 |
Amino | Cytidine | 4.1 |
Imino | Peptides | 13 |
Some chemical groups involved in the metal-biomass interactions and their pKas. Source: (Eccles, 1999).
Biosorption is a term that describes the metal removal by its passive linkage in live and dead biomasses from aqueous solutions in a mechanism that is not controlled by metabolic steps. The metal linkage is based on the chemical properties of the cellular envelope without to require biologic activity (Gadd, 2009; Godlewska-Zylkiewicz, 2006; Palmieri et al., 2000; Valdman et al., 2001; Volesky, 2001). The process occurs through interaction among the metals and some active sites (e.g. carboxylate, amine, sulfate, etc.) on cellular envelope. Some of these chemical groups and their respective pKas are described in the Table 1.
Usually, metallic species are not biodegradable and they are removed physically or chemically from contaminated effluents (Ahluwalia & Goyal, 2007; Hashim & Chu, 2004; Tien, 2002). The biosorption is a bioremediation emerging tool for wastewater treatment that has gained attention in the scientific community in the last years (Chu, 2004). It is a promising biotechnological alternative to physicochemical classical techniques applied such as: chemical precipitation, electrochemical separation, membrane separation, reverse osmosis, ion-exchange or adsorption resins (Ahluwalia & Goyal, 2007; Deng & Bai, 2004; Vegliò et al., 2002; Vegliò et al., 2003; Zouboulis et al., 2004). The conventional methods (Table 2) involve or capital and operational high costs, or they are inefficient at low metal concentration (1-100 ppm), or they can be associated to production of secondary residues that present treatment problems (Aksu, 2001; Ahluwalia & Goyal, 2007).
The initial incentives of biosorption development for industrial process are: (a) low cost of biosorbents, (b) great efficiency for metal removal at low concentration, (c) potential for biosorbent regeneration and metal valorization, (d) high velocity of sorption and desorption, (e) limited generation of secondary residues, and (f) more environmental friendly life cycle of the material (easy to eliminate compared to conventional resins, for example) (Crini, 2005; Kratochvil & Volesky, 2000; Volesky & Naja, 2005). Therefore the use of dead biomasses is generally preferred since it limits the toxicity effects of heavy metals (which may accumulate at the surface of cell walls and/or in the cytoplasm) and the necessity to provide nutrients (Modak & Natarajan, 1995; Sheng et al., 2004; Volesky, 2006).
Methodology | Disadvantages | Advantages |
Chemical precipitation | a. Hard separation; b. Generation of secondary residues; c. Commonly inefficient in low metal concentration | a. Simple procedures; b. Generally presents low costs |
Electrochemical treatment | a. Possibility of application in high metal concentration; b. Technique is sensible under determined conditions, as the presence of interfering agents | a. Successful metal recuperation |
Reverse osmosis | a. Application of high pressures; b. Membranes that can foul or peel; c. High costs | a. Effluent purification that become available to recycle |
Ion-exchange | a. It is sensible to the presence of particulate materials; b. Resins with high costs | a. Effective; b. Possibility of metal recuperation |
Adsorption | No efficiency for some metals | Conventional adsorbents (e.g. activated carbon and zeolites) |
Conventional methods of metal removal from aqueous systems. Source: (Zouboulis et al., 2004).
The mechanisms involved in metal accumulation on biosorption sites are numerous and their interpretation is made difficult because the complexity of the biologic systems (presence of various reactive groups, interactions between the compounds, etc.) (Gadd, 2009; Godlewska-Zylkiewicz, 2006; Palmieri, 2001). However, in most cases, metal binding proceeds through electrostatic interaction, surface complexation, ion-exchange, and precipitation, which can occur individually or combined (Yu et al., 2007a; Zouboulis et al., 2004). The uptake of metallic ions starts with the ion diffusion to surface of the evaluated biomasses. Once the ion is diffused to cellular surface, it bonds to sites that display some affinity with the metallic species (Aksu, 2001).
In general, literature describes that the biosorption process takes in consideration: (a) the temperature does not influence the biosorption between 20 and 35 ºC; (b) the pH is a very important variable on process, once it affects the metal chemical speciation, the activity of biomass functional groups (active sites), and the ion metallic competition by active sites; (c) in diluted solutions, the biomass concentration influences on biosorption capacity: in lower concentrations, there is an increase on biosorption capacity; and (d) in solutions with different metallic species there is the competition of distinct metals by active sites (Vegliò & Beolchini, 1997).
The biosorption performance is influenced by physicochemical parameters as: (a) the biomass nature: the physical structure (porosity, superficial area, particle size) and the chemical nature of functional groups (diversity and density); (b) the chemical and the availability of the adsorbate; and (c) the solution conditions, such as: ionic force, pH, temperature and adsorbate concentration (Gadd, 2009; Godlewska-Zylkiewicz, 2006; Crini, 2005).
Environmental demands have received a great focus in public policies of different world’s nations in the last decades. This is resulted of the external pressures of distinct areas as such the media vehicles, the scientific researches, and the greater conscious of the civil society about the environmental topics (Karnitz Jr., 2007; Volesky, 2001). These pressures have intensified the creation of regulatory laws as the water control and handling from anthropogenic activities. The mining and metallurgy wastewaters are considered the big resources of heavy metals contamination (cadmium, chromium, mercury, lead, zinc, copper, etc.) that are noxious in low concentrations (Sen & Sharadindra, 2009). The heavy metal recuperation from industrial effluents is extremely important due the society current requirements by the metal recycling and conservation (Hashim & Chu, 2004). The need for economic and effective methods for heavy metals removal from aqueous systems has resulted in the development of new technologies of concentration and separation (Hashim & Chu, 2004; Karnitz Jr., 2007; Sen & Sharadindra, 2009).
The biosorption of metals is established as research area since the 80s. The literature is mainly associated to the bioremediation of industrial wastewaters with low metal concentration. These works have been focused in the uptake of heavy metals because the metal ions in the environment bioaccumulate and are biomagnified along the food chain (Ahluwalia & Goyal, 2007; Vegliò et al., 2003; Volesky, 2001).
Besides the studies on environmental field of biosorption processes, others applications were investigated in the last few years led to develop the recovery of high demand and/or aggregated value metals such as gold, silver, uranium, thorium, and recently rare earth metals (RE) (Palmieri, 2001). The selection of interest metals in order to apply biosorption processes for recovery have to consider: (a) the environmental risk based on the technologic uses and the market value; and (b) the depletion rate of the metal resources, which is used as an indicator of variations on metal prices (Zouboulis et al., 2004). The price variations of interesting metals are essentially related to the market demands, environmental legislation, and energetic costs (Diniz & Volesky, 2005).
There is a great variety of biomasses used to achieve the biosorption of metals as such micro and macroalgae, yeasts, bacteria, crustacean, etc. The use of adsorbents from dead organisms has an attractive economic cost because they are originated in less expansive materials in comparison to the conventional technologies. Other economic advantage is the possibility of biosorbent reuse from agro-industrial and domestic wastes (e.g., fermentation processes in breweries and pharmaceutics, activated sludge, sugarcane bagasse, etc.) (Godlewska-Zylkiewicz, 2006; Karnitz Jr., 2007; Pagnanelli et al. 2004; Palmieri et al., 2002). Commonly, the biosorption studies describe applications with native biomasses and with products obtained from biomasses, which are generally biopolymers (polysaccharides and glycoproteins).
The use of biosorbents in native forms from microbial biomasses (e.g. yeasts, microalgae, bacteria, etc.) present a series of problems: the difficulty on separation of cells after the biosorption, the mass loss during the separation, and the low mechanic resistance of the cells (Arica et al., 2004; Sheng et al., 2008; Vegliò & Beolchini, 1997; Vullo et al., 2008). The biomass immobilization makes possible a material with more appropriated size, greater mechanic resistance, and desirable porosity to use in fixed-bed columns (Sheng et al., 2008; Zhou et al., 2005). Besides the immobilization provides the metal recuperation and the column reuse (Sheng et al., 2008; Zhou et al., 2005).
The most common immobilization procedures are: (a) the adsorption on inert supports by preparation of biofilms; (b) the encapsulation in polymeric matrices as calcium alginate, polyacrylamide, polysulfone, and polyhydroxyetilmetacrilate; (c) the covalent linkage on supports by chemical agents; and (d) the cross-linking by chemical agents that form stable cellular aggregated. The most common chemical agents used are formaldehyde, glutaraldheyde, divinylsulfone, and formaldehyde-urea mixture (Vegliò & Beolchini, 1997). An important area that has been developed is the surface modification of biomasses by the insertion of additional chemical groups to increase the biosorption uptake process (Yang & Chen, 2008; Yu et al., 2007a; Yu et al., 2007b). This procedure is used for biomasses with low uptake capacities and in numerous cases the chemical modification also provides the cellular immobilization.
Since the 80s several biosorption processes have been developed in commercial scale. Some commercial applications are described by Wang & Chen (2009):
B. V. SORBEX Inc.: several biosorbents of different biomaterials from biomass as such Sargassum natans, Acophylum nodosum, Halimeda opuntia, Palmira pamata, Chondrus crispus, and Chlorella vulgaris, which can adsorb a broad range of metals and can be regenerated easily;
Advance Mineral Technologies Inc.: biosorbents based in Bacillus sp., but that finished their operations in 1988;
AlgaSORB (Bio-recovery Systems Inc.): biomass Chlorella vulgaris immobilized in silica and polyacrylamide gels that adsorb metals of diluted solution with concentrations between 1-100 mg/L and can undergo more than 100 biosorption-desorption cycles;
AMT-BIOCLAIMTM (Visa Tech Ltd.): biosorbent from Bacillus subtilis immobilized in polyethyleneimine and glutaraldheyde beads, which removes efficiently metals as gold, cadmium, and zinc from cyanide solutions. The biosorbent is not selective, but it presents high metal recuperation (99%) and can be regenerated by sodium hydroxide or sulfuric acid solutions;
BIO-FIX (U. S. Bureau of Mines): biosorbent based in several biomasses, including Sphagnum peat moss, yeast, bacteria, and/or aquatic flora immobilized in high density polysulfone. The biosorbent is selective for heavy metals and it is applied in acid mine drainages. The metals can be eluted more than 120 recycles with solutions of hydrochloric acid and nitric acid.
Additionally the Table 3 presents some biosorbents and their applications in biosorption purposes.
Metal | Biosorbent | Reference |
Gd | Several microorganisms (fungal and bacteria) from sand | Andrès et al., 2000 |
Hg, Cd, and Zn | Ca-alginate and immobilized wood-rotting fungus Funalia trogii | Arica et al., 2004 |
Sm and Pr | Sargassum sp. | Oliveira et al., 2011 |
Cu | Sargassum sp. immobilized in poly(vinyl alcohol) cryogel beads | Sheng et al., 2008 |
Co and Ni | Ulva reticulate, Turbinaria ornata, Sargassum ilicifolium, Sargassum wightii, Gracilaria edulis, and Geledium sp. | Vijayaraghavan et al., 2005 |
Cd, Zn, and Pb | Laminaria hyperborea, Bifurcaria bifurcata, Sargassum muticum, and Fucus spiralis | Freitas et al., 2008 |
Cu and Pb | Activated sludge | Xuejiang et al., 2006 |
La, Nd, Eu, and Gd | Sargassum sp. | Oliveira & Garcia Jr., 2009 |
Pb and Zn | Phanerochaete chrysosporium immobilized in Ca-alginate | Arica et al., 2003 |
Pb | Streptomyces rimosus | Selatnia et al., 2004 |
Pb | Cellulose/chitin beads | Zhou et al., 2005 |
Ni | Sargassum wightii | Vijayaraghavan et al., 2006 |
Cr | Sargassum sp.: raw and chemically modified (treated with NaOH, HCl, CaCl2, formaldehyde, or glutaraldehyde) | Yang & Chen, 2008 |
Cu | Sugarcane bagasse: raw and chemically modified (treated with NaOH and/or citric acid) | Dos Santos et al., 2011 |
Cu, Mo, and Cr | Chitosan: flakes, beads, and modified beads (treated with glutaraldehyde) | Dambies et al., 2000 |
Ag | Lactobacillus sp. | Lin et al., 2005 |
Cd, Cu, and Ni | Aerobic granules | Xu & Liu, 2008 |
Cr and V | Waste crab shells | Niu & Volesky, 2006 |
Cd and Pb | Modified baker’s yeast (treated with glutaraldehyde and cystine) | Yu et al., 2007a |
Eu | Alfafa | Parsons et al.,2002 |
Pb, Zn, Cd, Fe, La, and Ce | Cross-linked Laminaria japonica (treated with propanol and HCl) | Ghimire et al., 2008 |
U, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu | Dictyota dichotoma, Ecklonia stolonifera, Undaria pinnatifida, Sargassum honeri, and Sargassum hemiphyllum | Sakamoto et al., 2008 |
Biosorbents used in some biosorption purposes.
The quantitative information in the biosorption purposes can be obtained from equilibrium analysis on batch experiments (Volesky, 2003). In these experiments are assayed the optimal conditions to perform a more effective biosorption and they may be used in the research of physicochemical models that describe the metal-biomass interactions. Despite of the continuous operation in columns to be the preferential mode for amplifying the biosorption process to a pilot scale (Volesky, 2003), the batch systems serve as pre-stage for an initial evaluation of adsorption phenomena and operational conditions before the application of the process on continuous systems (Gadd, 2009). The main difference between the operational modes refers to transport phenomena involved: in batch systems the diffusive and convective resistances for the adsorption are pronouncedly diminished in relation to column systems, which exhibit smaller mass transfer rates due to dependence of the combination of several parameters.
The physicochemical modeling is based on the analysis of the metal uptake capacity (according with Eq. 1) as function of the assay time (biosorption kinetics) or the equilibrium concentration of adsorbed metal (biosorption isotherms).
where q is the metal uptake that represents the amount of accumulated metal by mass unity or matter moiety of biomass; V is the solution volume; C0 e CEQ are the initial and equilibrium concentrations (in the liquid phase), respectively; and M is the biomass mass.
Physicochemical models differ with regard to the number of adsorbed layers, the type of interactions among the active sites and metals, and the possibility to use the equilibrium constants among the solid and liquid phases. The criteria for choosing an isotherm or a kinetic equation for biosorption data is mainly based on the best adjustment of curve fitting which is often evaluated by statistical analysis. The model chosen should be the one reflecting the best the biosorption mechanisms (Liu & Liu, 2008; Vegliò et al., 2003). The next items exemplify the use of batch systems as much in the optimization of operational parameters as in the physicochemical modeling for the biosorption of metals.
The study of the phase equilibrium is a part of the thermodynamic that relate the equilibrium composition of two phases and it is represented by graphics of concentration in the stationary phase (expressed in biosorption purposes in terms of metal uptake, q) versus the concentration in the mobile phase, both at equilibrium (Godlewska-Zylkiewicz, 2006). Usually the mechanisms of adsorption and ion-exchange are the most used because their concepts are easily extended to other mechanisms of metal retention. The adsorption models in liquid-solid equilibrium are derived of models for gas-solid equilibrium from the Gibbs isotherm and assuming an equation of state for the adsorbed phase. The Table 4 displays some adsorption models used in biosorption studies and the advantages and disadvantage in their utilization.
These models (Table 4) differ in the amount of adsorbed layers, the interaction between the binding sites and the metal (adsorbent-adsorbate, adsorbate-adsorbate, and adsorbent-adsorbent), and the possibility to apply equilibrium constants equations between the liquid and solid phases. Obviously, these considerations for biosorption systems do not explain the mechanisms of metal uptake due to the complexity of the biologic systems, but it supplies parameters that are utilized to evaluate the biosorption performance, such as the maximum metal uptake and the affinity of the active sites by metallic ions (Kratochvil & Volesky, 2000; Palmieri, 2001).
Biosorption of metals in the mostly cases of equilibrium isotherms is modeled according to non-linear functions that are described by Brunauer-Emmet-Teller (BET) type-I isotherms with hyperbolic shape (Guiochon et al., 2006). The general form of the curve q = f(CEQ) is showed on Fig. 1.
Adsorption Model | Equation | Advantages | Disadvantages |
Langmuir | q = (qMAXbCEQ)/(1+bCEQ) | Interpretable parameters | Not structured; Monolayer Adsorption |
Freundlich | q = KFCEQ1/n | Simple expression | Not structured; No leveling off |
Combination Langmuir- Freundlich | q = (qMAXbCEQ1/n)/(1+bCEQ) | Combination of above | Unnecessarily complicated |
Radke- Prausnitz | 1/q = 1/(aCEQ)+1/(bCEQβ) | Simple expression | Empirical, uses 3 parameters |
Brunaer- Emmet- Teller | q = (BCQ0)/{[Cs-C][1+(B-1)C/CS]} | Multilayer adsorption; Inflection point | No total capacity equivalent |
Examples of physicochemical models of adsorption. Source: (Volesky, 2003).
Typical curve of an adsorption isotherm. Source: (Oliveira, 2011).
These isotherms generally are associated mainly to Langmuir and Freundlich besides other models derived of these firsts. The Freundlich model suggests adsorbed monolayers, where the interactions among adjacent molecules that are adsorbed: the energy distribution is heterogeneous due to the diversity of the binding sites and the nature of the adsorbed metallic ions. The Langmuir model considers an adsorbed monolayer with homogeneous distribution of binding sites and adsorption energy, without interaction among the adsorbed molecules (Selatnia et al., 2004).
For instance, on biosorption of Sm(III) and Pr(III) by Sargassum sp. biomass described by (Oliveira et al. 2011), the Langmuir adsorption model has been founded very accurate, that is approximated for liquid-solid equilibrium by the Eq. 2 and it can be observed in the Fig. 2.
where q is the metal uptake; qMAX is the maximum biosorption uptake that is reached when biomass active sites are saturated by the metals; b is a constant that can be related to the affinity between the metal and the biomass; and CEQ is the metal concentration in the liquid phase after achieving the equilibrium.
Biosorption isotherms for Sm(III) and Pr(III) solutions by Sargassum sp. described by the Langmuir adsorption model. Symbols: (–■–) Sm(III) and (--□--) Pr(III). Source: (Oliveira et al., 2011).
Additionally, it is noteworthy that the shape of the biosorption isotherms (Fig. 2) approaches the profile of irreversible isotherms: the initial slope is very steep and the equilibrium plateau is reached at low residual concentration. This can be correlated to the great affinity of Sm(III) and Pr(III) for the biosorbent (Oliveira et al., 2011).
The models presented on Table 4 are applied for mono-component systems. For systems with more than one metallic species, the mathematical modeling must be modified to take into account the competition of metal by the binding sites (Aksu & Açikel, 2000). Some approaches are listed on Table 5.
Adsorption Model | Equation | Advantages | Disadvantages |
Langmuir | qi=(qMAX,ibiCEQ,i)/ (1+ | Constants have physical meaning; Isotherms levels off at maximum saturation | Not structured; Does not reflect the mechanism well |
Combination Langmuir-Freundlich | qi = (aiCEQ,i1/ni)/(1+ | Combination of above | Unnecessarily complicated |
Surface complexation model | q ~ f(CEQ), could follow e.g. Langmuir | Model more structured: intrinsic equilibrium constant could be used | Equilibrium constants have to be established for different types of binding |
Examples of physicochemical multi-component models of adsorption. Source: (Volesky, 2003).
Biosorption processes tend to occur rapidly, taking from few minutes to a couple of hours and it takes account transfer mass processes and adsorption processes. The biosorption kinetics is controlled mainly by convective and diffusive processes. In a first stage occurs the metal transference from solution to adsorbent surface neighborhood; then in the next step, the metal transference from adsorbent surface to intraparticle active sites; and finally, the metallic ion removal by the active sites via complexation, adsorption, or intraparticle precipitation. The first and second steps represent the resistance to convective and diffusive mass transferences and the last one is quick and non-limiting for the overall biosorption velocity (Selatnia et al., 2004).
Analogously to the biosorption isotherms, the biosorption kinetics in general present hyperbolic shape (as the Fig. 1) and they are described by various models. The models more used in biosorption studies are presented on Table 6.
Adsorption model | Differential equation | Integral equation | Initial adsorption velocity |
Pseudo- first-order | dqt/dt = k1(qEQ - qt) | ln(qEQ - qt) = ln qEQ – k1t | v1 = k1qEQ |
Pseudo- second-order | dqt/dt = k2(qEQ - qt)2 | qt = t/[1/(k2qEQ2)+t/qEQ] | v2 = k2qEQ2 |
Examples of kinetics models used in biosorption studies. Source: (Wang & Chen, 2009).
The pseudo-second-order model is preferred for biosorption of RE (Oliveira & Garcia Jr., 2009; Oliveira et al., 2011) and is represented by the integral Eq. (3).
where qt is the biosorption uptake in the t time of assay; qEQ is the equilibrium metal uptake; and k2 is a constant that represent the metal access rate to biomass in the pseudo-second-order kinetic model. Fig. 3 displays the modeling of samarium and praseodymium biosorption kinetics in Sargassum sp. by the pseudo-second-order kinetics model.
Biosorption kinetics for Sm(III) and Pr(III) solutions by Sargassum sp. described by the pseudo-second-order kinetics model. Symbols: (–■–) Sm(III) and (--□--) Pr(III). Source: (Oliveira et al., 2011).
Generally the biosorption carried out in low pH values (smaller than 2.0) has a non-effective metal uptake (for the cases that metallic cationic species are involved) because the high hydronium concentration makes the competition among these protons more favorable than the metals in solution by the biomass active sites. Moreover the acidic groups in low pH should be protonated according with their pKa values as can be seen on Table 1.
The metal uptake is increased when the acidic groups tend to be deprotonated from their pKa values (Table 1) and the metallic ion presents a chemical speciation that provides greater adsorption performance. In the case of RE biosorption for Sargassum sp. biomass, Palmieri et al. (2002) and Diniz & Volesky (2005) founded that the biosorption of La(III), Eu(III), and Yb(III) is more effective in crescent pH values (2.00 to 5.00) because the quantity of negative ligands is increased, and consequently the increase of the attraction among the ligands and the metallic cations. The optimal pH for Sargassum founded about 5.0. In this pH the carboxyl pKas of mannuronic and guluronic acid residues (3.38 and 3.65, respectively) in the alginate biopolymer (main component of brown algae cellular envelope) are suppressed; so all carboxyl sites should be more available for the adsorption. Towards the RE speciation in distinct pH ranges: (a) in pH < 6.0 prevail the presence of RE3+; (b) between about 6.0 < pH < 9.5 there is the generation of RE(OH)2+ and RE(OH)2+ that remain solubilized or suspended in solution; and (c) from pH ~ 8.5 occurs the precipitation of RE hydroxide. Biosorption of anionic species are very less common and occurs when a metallic complex is formed with a negative global charge, e.g. the AMT-BIOCLAIMTM is able to adsorb gold, zinc, and cadmium from cyanide solution (i.e. cyanide complexes with the metals) in metal-finishing operations (Atkinson et al., 1998).
In general, the literature describes that the biosorption process is not influenced between 20 and 35ºC (Vegliò & Beolchini, 1997). However some biosorbent present considerable differences on biosorption performance as function of the temperature. For instance, Ruiz-Manríquez et al. (1998) studied the biosorption of copper on Thiobacillus ferrooxidans [sic] considering temperatures of 25 and 37 C: the results indicate that there was a positive effect in the biosorption uptake when the temperature was increased, where the increase in the biosorption was of 68%.
Besides the evaluation of the optimal temperature to be used in biosorption purposes, the batch procedures commonly can be utilized to find thermodynamic parameters as enthalpy (ΔH), entropy (ΔS), and Gibbs free-energy (ΔG) through the Eq. 4 and Eq. 5.
where R is the gas constant (8.314 J/(K mol)), T is the temperature, and KEQ is equilibrium constant in determined temperature that corresponds the ratio between the equilibrium metal concentration in the liquid (CEQ) and solid phases (qEQ). In this context, Dos Santos et al. (2011) verified that the chemical modification of the sugarcane bagasse by different treatments lead a more energetically favorable adsorption of copper in comparison with raw material, because the negative increase of the Gibbs free-energy.
The binding of metallic ions biomasses is influenced by other ionic species, such as cations and anions present in solution. Benaissa & Benguella (2004) describe the influence of the presence of cations (Na+, Mg+, and Ca2+) and anions (Cl-, SO42-, and CO32-) on cadmium biosorption for chitin. The presence of these ions in solution inhibits the uptake of cadmium by chitin to different degrees: sodium and chloride ions have no significant. For magnesium, calcium, sulfate, and carbonate ions the effects ranged from a large inhibition of cadmium by calcium and carbonate to a weak inhibition by magnesium and sulfate. These interferences in cadmium biosorption are resulted of the competition among the interesting metal and the counter-ion by the binding sites.
Additionally, Palmieri et al. (2002) studied the lanthanum biosorption by Sargassum fluitans in solution with chloride and sulfate ions: at same pH it was observed higher maximum metal uptake values for the biosorption on presence of chloride, as such can be seen on Fig. 4. In the case of lanthanides, the formation of complexes with chloride or sulfate affects the coordination sphere of metal, leading to an influence on the net charge of the cation. Chloride ions are reported to have an outer sphere character with a less disturbance in the hydration sphere. On the other hand, sulfate and carboxylate anions present inner sphere character more pronounced in the complex formation with lanthanum. The biosorption uptake of lanthanum presents higher value for chloride-based solutions than sulfate-based solutions could suggest that the fewer disturbances on the inner coordination sphere caused by chloride anion facilitate the interaction with carboxylate groups present in the biomass.
Bisorption isotherms for La(III) on Sargassum fluitans from chloride or sulfate-based solutions at different pHs. Symbols: chloride-based solutions at (□) pH 4 and (○) pH 5; and sulfate-based solutions at (■) pH 4 and (●) pH 5. Source: (Palmieri et al., 2002).
After the metal removal from aqueous solutions by the biomass, it is important the metal recuperation from biomass. In this point, it is achieved the metal desorption process, whose aim is the weakening the metal-biomass linkage (Modak & Natarajan, 1995). Generally it can be applied diluted mineral acids and complexing agents as desorbents. Biosorption and desorption isotherms present close behavior characteristic of Langmuir modeling, which has at equilibrium equivalent kinetic rates (Palmieri et al., 2002).
Diniz & Volesky (2005) evaluate the reversibility of the adsorption reaction for the biosorption of lanthanum, europium, and ytterbium by Sargassum polycystum using the desorbent agents: nitric and hydrochloric acids, calcium nitrate and chloride salts, EDTA, oxalic and diglycolic acids. This work as such other studies founded the hydrochloric acid as the best agent for brown algae, with percentage of recovery between 95-100%.
Beyond the perspectives of application of the biosorption in order to optimize the process, the understanding of the mechanisms involved in the biosorption is justifiable for better comprehension of the process and of itself scale-up. This is carried out from qualitative and/or quantitative characterizations by potentiometric titrations, and spectroscopic and microscopic techniques as such FTIR (Fourier transform infrared spectroscopy), SEM (scanning electron microscope), EDX (energy-dispersive X-ray spectroscopy), XPS (X-ray photoelectron spectroscopy), etc. The main objective of the biosorbent characterization has been to indentify the chemical groups involved in the biosorption and the way that these groups perform the metal binding.
The most common technique used is the potentiometric titration, which evaluate the existence of stoichiometric relationships among the metals and the binding sites, and to determine the pKas values of the chemical groups on biomass cellular envelope. The Table 1 summarizes the characteristics of the protonated Sargassum sp. biomass before and after samarium and praseodymium biosorption.
Material | Strong acid groups (mmol/g) | Total amount of acid groups (mmol/g) | Weak acid groups (mmol/g) | Occupancy of binding sites (%) |
Protonated biomass | 0.15 | 1.77 | 1.62 | - |
Sm(III) – loaded biomass | 0.07 | 1.26 | 1.19 | 29 |
Pr(III) – loaded biomass | 0.07 | 1.18 | 1.11 | 33 |
Acid-base properties of protonated Sargassum sp. before and after Sm(III) and Pr(III) biosorption. Source: (Oliveira et al., 2011).
The strong acid groups counted for only 0.15 mmol/g on protonated biomass, and decreased to 0.07 mmol/g after the biosorption of either Sm(III) or Pr(III). These groups of lowest pKa have been identified as the ester sulfate groups of the fucoidan, which are present on the cell wall of brown seaweeds. Weak acid groups are mainly constituted by carboxylate groups from alginate compounds, which represent more than 90 % of total acid groups, i.e., 1.62 mmol/g. After metal biosorption the titration identified 1.19 and 1.11 mmol/g of weak acid groups for Sm(III) and Pr(III), respectively. Thereby only around 30 % of the acid groups were involved in metal binding (Oliveira et al., 2011).
Another example of the biomass characterization can be observed on Fig. 5, which displays the analysis of SEM-EDX of Sargassum sp. biomass after lanthanum biosorption. The lanthanum presence in the X-ray spectra confirms the adsorption of the metal on the biosorbent surface. In the SEM micrography also is evident the surface colonization by diatoms as well as the assignments of chemical elements from the marine environment (calcium, aluminum, silicon).
Despite of the biosorption in batch systems to available parameters to understand the metal-biomass interaction and to select the best operational condition, the procedures in columns are generally the preferential mode for the biosorption application in the industrial scale-up, once that the process can be performed continuously (Vieira et al., 2008; Volesky, 2003). This operational mode is more appropriate for large-scale applications in industry than other types of reactors as such agitated tanks, fluidized-bed columns, etc. The fixed-bed columns have a series of advantages: they have simple operation, they achieve large yields, and they have ease scale-up from procedures in laboratorial scale (Borba et al., 2006; Borba et al., 2008; Valdman et al., 2001; Vijayaraghavan et al., 2005; Vijayaraghavan & Prabu, 2006). The use of fixed-bed columns allow to avoid separation difficulties between the biosorbent and the effluent (Kentish & Stevens, 2001). This experimental procedure has as limiting step the mass transfer of metal from solution to the biosorbent, since the adsorption reactions do not limit the process due to the fast kinetics (Aksu, 2001; Crini, 2005; Volesky, 2001).
Scanning electronic micrography of Sargassum sp. biomass after lanthanum biosorption and related X-ray spectra. Source: (Oliveira, 2011).
The main methodologies for the concentration, separation, and purification of metals involve a great number of equilibriums and phase transferences, such as the methodologies listed in Table 8.
Methodology | Concentration applied (g/L) |
Solvent extraction | 0.5–500 |
Microporous membranes | 10-2–10 |
Emulsified or supported liquid membranes | 10-4–10 |
Ion-exchange | 10-6 – 1 |
Biosorption | 10-6 – 0.1 |
Separation technologies and concentration ranges applied. Source: (Kentish & Stevens, 2001).
The biosorbents should have several mechanisms of metal uptake, but for column biosorption perspectives these mechanisms are approximated to mainly ion-exchange or adsorption. Generally the chromatographic separations by fixed-bed columns occur by two ways: the frontal analysis and the displacement elution.
On frontal analysis is carried out the metal adsorption for a percolated volume of solution in the column, which produces a mixed zone of metallic ions that spreads to a distance across the column according to the individual and competitive interactions among the metals and the adsorbent. In this process, the mixed zone is composed by several equilibriums among the displaced ions and the retained ions and it moves across the column without to alter your volume. After the mixed zone is displaced to sufficient distance across the column, it is reached an equilibrium which the components are resolved in differentiate heights, i.e. in distinct or enriched zones for each one of the components (Fritz, 2004). Thus the greater interaction among the metals and the biosorbent represents a greater retention of these metals across the column. Therefore, a greater number of distinct affinities of the percolated metals by the adsorbent mean a better possibility of the system to resolve the metals in differentiate heights.
Commonly the frontal analysis performance is mathematically quantified and modeled from the application of approximations and boundary conditions on non-linear material balance equations based mainly for biosorption columns on equilibrium dispersive model (Guiochon et al., 2006). The model assumes that all conditions are due to a non-equilibrium, which is treated into a term of apparent axial dispersion, where it is considered that the dispersion coefficients of the components remain constants. The column is considered unidimensional and radially homogenous, i.e. the properties are constants in a same cross section. When a fixed-bed column is occupied by fluid with a constant linear velocity, the differential mass balance involved is given by the Eq. 6.
where t is the time; z is the axial coordinate with origin on column entrance; q is the metal uptake in the stationary phase; C is the concentration in the mobile phase; v is the linear velocity; (1-ε)/ε is the phase ratio (mobile phase volume/stationary phase volume) and ε is the adsorbent porosity; and DL is a parameter that includes the contributions of the axial dispersion (due to molecular diffusion), the non-homogeneity of the flux (eddy diffusion), and the bed tortuosity.
The terms on Eq. 6 represent respectively: (a) the accumulation in the stationary phase; (b) the convective phenomena; (c) the accumulation in the mobile phase, and (d) the diffusive phenomena. Some approximations should be achieved as such: (a) the column should be considered radially homogenous only in isothermic or isobaric operations; (b) the compressibility of the mobile phase is neglected between 0 and 200 bar in the mostly cases if the volume is altered between 0.5 and 2%; (c) the viscosity in the mobile phase is constant; (d) since the pump provides constant flow rate, the velocity is also constant; (e) the parameter DL is constant; (f) the partial molar volume of the sample components is constant in both phases; (g) the solvent is not adsorbed; (h) constant operational conditions: temperature, pressure, flow rate, physicochemical parameters, porosities, etc. (Guiochon et al., 2006).
There are several parameters that govern the adsorption, which may be modified to find a more effective adsorption and/or a separation with better resolution of the components as such: (a) the column geometry that considers the height and the cross section area of the bed; (b) the homogeneity or the heterogeneity of the adsorbent; (c) the particle diameter and their implications on porosity, packing, and tortuosity of the bed; (d) the number of theoretical plates; (e) the concentration and composition of the solute on mobile and stationary phases; (f) the presence of additives on feeding, e.g. complexing agents, buffers, etc.; (g) the column flow rate; etc. (Guiochon et al., 2006).
In biosorption isotherms, the concentration profiles in the liquid and solid phases change in space and time. Thereby the development and performance of adsorption columns are difficult to reach without an approximated quantitative modeling of the Eq. 6. From perspective of design and optimization of the column processes, the behavior in fixed-bed is described by the effluent concentration profile (C/C0, where C and C0 are the concentration of eluate and eluent, respectively) in function of the time or percolated volume (Nadaffi et al., 2007), i.e. by breakthrough curve, which is showed on Fig. 6. The curve shape is given by a sigmoid function and it is determined by the shape of the equilibrium isotherm, i.e. it is influenced by the transport processes and the adsorbent nature (Chu, 2004).
Schematic representation of the breakthrough curve. Source: (Oliveira, 2011).
In the breakthrough curves (Fig. 6) are determined the breakthrough and saturation times (tb and ts, respectively). The breakthrough time indicates the instant in which the metallic ion is effectively discharged on eluate, and the saturation time corresponds to the instant of metal mass saturation on biomass. The breakthrough time is arbitrarily inferred for C/C0 at 0.05; while the saturation time is defined ideally when C/C0 values reach 1.0 (generally at 0.90-0.95). All optimized system in columns is based on accurate prediction of the breakthrough time under selected operational conditions. When the eluate concentration reaches a predefined level, the column operation is finalized; in this point the regeneration process may be achieved to activate the column for a next operation cycle (Kentish & Stevens, 2001). In order to investigate the alternatives for the separation of metallic species, the breakthrough time is crucial because it represents the interaction between the metal and the biomass; so if the breakthrough time is great, this indicates that the interaction between the metal and the biomass is greater.
The variation between the breakthrough and saturation times depends on the capacity of the column toward the quantity of applied metal (Aksu, 2001). A more efficient adsorption performance will be obtained as greater is the curve slope, i.e. as smaller is the gap between the breakthrough and saturation times (Fig. 6) (Chu, 2004). This gap corresponds to the extension of the mass transfer zone (MTZ) on bed (Nadaffi et al., 2007), which is the bed active region where the adsorption occurs as can be seen on Fig. 7. So the column efficiency will be better in smaller values of height of mass transfer zone which indicate a behavior near to ideality; in that case a step function where the curve inclination between the breakthrough and the saturation tends to zero.
Schematic representation of the movement of the mass transfer zone in fixed-bed column. Symbols: (––) ideal and (––) real cases. Source: (Oliveira, 2011).
Several derivations may be used from the material balance in the Eq. 6 to perform the breakthrough curves such as the models of Thomas, Bohart-Adams, Yoon-Nelson, etc. Some models are described in function of operational and kinetic parameters (e.g. Thomas and Bohart-Adams); in other hand, there are models related to adjustment purely mathematic according with the sigmoid function (e.g. Yoon-Nelson model). For instance the Thomas model is expressed Eq. 7.
where kTh is the Thomas constant; Q is the flow rate; qMAX is maximum biosorption uptake; M is the dry mass of biomass; and V is the volume percolated. The Fig. 8 presents the experimental data for column biosorption of lanthanum by Sargassum sp. adjusted by the Thomas model.
Modeling of breakthrough curve in the column biosorption of La(III) for Sargassum sp. biomass by the Thomas model. Symbols: (■) data of metal concentration on eluate and (––) curve fit for Thomas model. Source: (Oliveira, 2011).
There is broad literature that describes the effects of operational parameters to augment and to improve the biosorption in fixed-bed columns (Hashim & Chu, 2004; Chu, 2004; Kratochvil & Volesky, 2000; Naddafi et al., 2007; Oliveira, 2007; Oliveira, 2001; Valdman et al., 2001; Vieira et al., 2008; Vijayaraghavan et al., 2005; Vijayaraghavan et al., 2008; Vijayaraghavan & Prabu, 2006; Volesky et al., 2003). These parameters modified mainly related are: flow rate, feeding concentration, height of packed-bed column, porosity, mass of biomass, etc. Vijayaraghavan & Prabu (2006) evaluate some variables as the bed height (15 to 25 cm), flow rate (5 to 20 mL/min), and copper concentration (50 to 100 mg/L) in Sargassum wightii biomass from breakthrough curves: each variable evaluated was changed and the others were fixed. Continuous experiments revealed that the increasing of the bed height and inlet solute concentration resulted in better column performance, while the lowest flow rate favored the biosorption (Vijayaraghavan & Prabu, 2006)
Naddafi et al. (2007) studied the biosorption of binary solution of lead and cadmium in Sargassum glaucescens biomass from the breakthrough curves modeled according with the Thomas model (Eq. 7). Under selected flow rate condition (1.5 L/h) the experiments reached a selective biosorption. The elution of the metals in distinct breakthrough times with biosorption uptake in these times at 0.97 and 0.15 mmol/g for lead and cadmium, respectively.
Column desorption is used for the metal recovery, but this procedure under selected conditions may be operated to carry out chromatographic elution by the displacement of the adsorbed components in enriched fractions containing each metal (Diniz & Volesky, 2006). This is resulted of the simple drag of the previous separation on frontal analysis. Nevertheless the eluent may present differential affinity by the adsorbed solutes, so there is the possibility to use the procedure to promote a more effective separation of the components. The chromatographic elution is dependent of the parameters referred to frontal analysis and of the composition and concentration of the displacement solution. Desorption profiles are given as bands or peaks whose modeling are associated directly to mathematic approximations by Gaussian functions that may be modified or not exponentially (Guiochon et al., 2006).
A typical column desorption with hydrochloric acid from Sargassum sp. previously submitted to biosorption of lanthanum is showed on Fig. 9, which is represented by lanthanum concentration in eluate as function of the volume.
Column desorption of La(III) from Sargassum sp. biomass with HCl 0.10 mol/L. Symbols: (–■–) metal concentration on eluate. Source: (Oliveira, 2011).
On Fig. 9 can be seen that after the start of the acid percolation occurs a quick increase of concentration until the maximum to 5.08 g/L for lanthanum. Parameters as the recovery percentage (p) and concentration factor (f) are obtained from biosorption and desorption curves. The recovery percentage is resulted of the ratio between the values of metal recovery on desorption and maximum metal uptake on biosorption, while the concentration factor refers to the ratio between the saturation volume on biosorption and the effective recovery volume on desorption. Both measure the efficiency of the desorbing agents in the metal recovery. For instance, these parameters obtained from Fig. 9 were 93.3% and 60.4 times of recovery percentage and concentration factor, respectively; which are expressive and satisfactory for the column biosorption purposes (Oliveira, 2011).
For biosorption and desorption processes, other important aspect is the biosorbent reuse for recycles biosorption-desorption according the cost benefit between the biosorption capacity loss during desorption steps and the metal recuperation operational yield (Diniz & Volesky, 2006; Gadd, 2009; Godlewska-Zylkiewicz, 2006; Gupta & Rastogi, 2008; Volesky et al., 2003). Oliveira (2007) performed the neodymium column biosorption by Sargassum sp. and the subsequent desorption in three recycles. In these experiments was observed that occurs a decrease in mass metal accumulation through the cycles. Accumulation decrease from first to third cycle in 22%, which is due to the partial destruction of binding sites on desorption procedures, and the binding sites blocking by neodymium ions strongly adsorbed. The result showed that the biomass may be used for recycle finalities.
The loss in performance of the adsorption during the recycles can has numerous origins. Generally they are associated to the modifications on chemistry and structure of the biosorbent (Gupta & Rastogi, 2008), and the changes of access conditions of the desorbent to the metal and mass transfer. Low-grade contaminants in the solutions used in these procedures may accumulate and to block the binding sites or to affect the stability of these molecules (Volesky et al., 2003).
Composites have been defined as materials made by mixing more than two chemically and physically dissimilar components together, physically or chemically, to form one new material [1, 2, 3]. In a composite, there is the continuous component known as the matrix and there is the discrete or discontinuous component called the fillers. In the composite material, both the matrix and the fillers come together to act as one material. The filler is the load bearing component of the composites while matrix bind the fillers together, which is the reinforcing material [4, 5]. There are different types of composites. These include: ceramics matrix composites (CMC), polymer matrix composites (PMC) and metal matrix composites (MMC) [6, 7, 8]. PMC’s are of great interest around the world today with notable advantages that include its light weight, high stiffness, high strength and the ease of fabrication [9, 10, 11, 12]. Polymer composites have been reported to be in use for numerous years with a market share reported to have increased tremendously in the last decade [9]. This has been attributed to the introduction of environmentally friendly natural fibers from plant sources. The processing and application of polymer composites requires a good understanding of all the factors that governs the relationship between all components that makes up the composite [4, 13, 14, 15]. The structure-property’s relationship of any polymer composite is of fundamental importance right from their design which includes material selection. Many research have tried to explain the relationship through various experimental designs [16, 17, 18]. One important factor that was generally accepted to have pronounced impact on the processing and application properties is the interfacial interaction between the matrix and the fibers. This interfacial interaction can vary from mere physical interfacial to real chemical interaction [3, 11, 15, 19, 20, 21, 22]. To properly understand which interaction has taken place, a good understanding of the materials involved is necessary. Therefore, this chapter seeks to give an insight explanation to the different types of matrixes and fibers available for polymer composite preparation and their possible interactions.
\nPolymer composites is an heterogeneous components material and so their properties, will be governed by factors such as component properties, composition of the individual components, chemical and physical structures and interfacial interactions [17, 23, 24]. Although, all the factors are equally important, the first three can be controlled before processing while the interfacial interactions can only be determined after processing and the extent of interaction can only be predicted using the necessary characterization techniques. Particle/particle interactions in polymer composites induce aggregation while filler/matrix interactions lead to an interphase development which yields characteristics which are modifications of those of the individual component [25]. In order to achieve a good migration of stress from the matrix to the fibers, a strong interaction is necessary, such as coupling that creates covalent bonds between the polymer matrix and the fibers. Although, secondary forces like Van der Waal forces or hydrogen bond may occur amongst the components [26, 27, 28].
\nFor polymer composites filled with natural fibers, there are conditions that are necessary for the natural fiber polymer composites (NFPCs) to be able to carry out the objective principle effectively. These include (i) the length of fibers used must be sufficiently long, (ii) the orientation of the fibers must be in sync with that of the load, and (iii) the interfacial adhesion must be sufficiently strong enough [29, 30]. Therefore, the type of interfacial adhesion determines the performances of the NFPCs (such as barrier properties, mechanical and thermal properties). Other types of interactions reported include electrostatic forces, inter diffusion and mechanical interlocking.
\nIn polymer composite preparation, the polymer matrix serves as the binding material (binder). It helps to hold the fillers in position and also helps to transmit stress within the material [31, 32, 33]. Therefore, if the interfacial interaction is poor, the transmission of an externally applied stress will be poorly done, leading to failures in the material. To ensure that there is a good stress transfer in polymer composites, the right polymer matrix is selected. Polymers are known for their unique properties which differ from one polymer to the other, even within the same group. Based on this, polymers are categorized on the basis of their chemical behavior (i.e. thermoplastic or thermosetting) or on the basis of their source (i.e. synthetic or natural). Thermoplastic are polymers that once processed and are harden to shape, can be reprocessed again and again as desired. Examples are polyethylene (PE), polypropylene (PP), poly(caprolactone) (PCL), poly(lactic acid) (PLA). Thermosetting are polymers that once processed at an elevated temperature and are set into shape, can harden and cannot be reprocessed again. Examples are polyesters, epoxies. Also these polymers are either synthesized or are obtained from nature. Table 1 shows a list of polymer matrices grouped into natural and synthetic. All these influence the choice of polymer matrix.
\nBiodegradable polymer matrices | \n|
---|---|
Natural | \nSynthetic | \n
Polysaccharides—starch, cellulose, chitin Proteins—collagen/gelatin, casein, albumin, fibrogen Polyesters—polyhydroxyalkanoates (PHAs) Other polymers—lignin, lipids, shellac, natural rubber | \nPoly(amides) Poly(anhydrides) Poly(amide-enamines) Poly(vinyl alcohol) Poly(vinyl acetate) Polyesters—poly(glycolic acid), poly(actic acid), poly(caprolactone), poly(orthoesters), poly(ethylene oxides), poly(phosphazines) | \n
Some common polymer matrices used for composite preparation [34].
Fibers are one form of fillers that can be used to prepare polymer composites. Researchers have fibers in natural or synthetic forms [35, 36, 37, 38, 39]. Fibers such as aramid, carbon and glass are known as synthetic fibers. Due to increased environmental awareness, synthetic fibers are now being replaced with natural fibers which are more environmental friendly [5, 40, 41, 42]. Natural fibers have emerged as a viable alternative to their synthetic counterparts in polymer reinforcement, owing to the large scale research output [40]. Natural fibers are obtained from natural source such as minerals, animals or plants [34]. Fibers from plant sources consist of cellulose, while those obtained from animal sources consist of proteins (wool, silk and hair). Natural fibers offer large diversity in terms of sources. Plant fibers are generally categorized based on their location with the plant as illustrated in Figure 1 [4].
\nRepresentation diagram showing the classification of natural fibers based on the part of plants they are extracted from [43].
Fibers from plant source have been widely used in preparing polymer composites [44, 45, 46, 47, 48, 49]. This is because of the availability and the easy of processing them. Plant fibers can further be classified a primary fibers, or secondary fibers [40, 50]. Primary fibers are the fibers obtained from plants, which were specifically grown for their fiber recourses. However, in cases where the fibers are by-products of other primary use of the plant, the fibers are referred to as secondary fibers (Figure 2).
\nSchematic classification of natural fibers as primary and secondary fibers [50].
The mechanical properties and morphology of these fibers are influenced greatly by the value of the ratio of fiber diameter to the cell wall thickness which by extension is influenced by the extraction methods used [40, 51, 52]. These factors dictate the type of interaction that will occur between the plant fibers and the polymer matrix, whether thermoplastic or thermoset [53, 54]. Natural fibers are good materials for many applications as they provide reinforcement properties at very low cost with low density, good strength and stiffness [8]. Their advantages over synthetic fibers have been well documented and they are based generally on environmental sustainability which include health and safety concerns [55, 56].
\nWith a careful selection of appropriate preparation, some level of desired interaction at the interface can be achieved. The processing of NFPCs has the ability to influence the final properties if carefully handled. Polymer composites can be prepared using the existing methods and technologies. These include injection molding, compression molding, blow molding, electro spinning, batch mixing or continuous mixing methods (extrusion), solution casting [34]. Different researchers have employed different methods to achieve their goal or specific property improvement. An experiment to toughen polylacticle/poly(butylenes succinate co-adipate) blends was reported [57]. This was achieved through melt blending (batch mixing) of the mixture in the presence of a reactive compatibilizer tripheny phosphate. Polypropylene/carbon nanotube composites were prepared using a twin screw extrusion mixer [58]. Their intention was to characterize the rheological behaviors and develop a model for the flow inside the machine. To investigate the micro mechanical characteristics of jute fiber/polypropylene composites, Liu et al. prepared the PP reinforced jute fiber Mat using film—stacking methods [7]. This was done by placing two layers of pre-dried non-woven jute mats in a mixture with three layers of PP films. In trying to prepare a novel composite films of polypyrrole-nanotube/polyaniline, Zhang et al., used facile solvent-evaporation method [59]. Also, recycling of biodegradable polymers for composites preparation has been done using extrusion processing [60]. The earlier mentioned methods of processing of polymer composites can be grouped into three primary systems, namely: solution blending, in-situ polymerization and melt blending [61].
\nThis involves the formation of the composites through dissolution of the polymer and fibers in a suitable solvent and subsequent drying of the solvent after the processing of the composites [62, 63, 64]. In solution casting, obtaining the right solvent that will dissolve the polymer and be removed with easy is a major task, although there are water-soluble polymers [65, 66]. Examples are polyvinyl pyrrolidone (PVP), polyvinyl alcohol (PVA), poly(ethylene oxide) (PEO) and poly(ethylene-co-vinyl acetate) (PEVA). Many others are dissolved using non-aqueous solvents such as chloroform, xylene, benzonitrile, tetrahydrofuran (THF), toluene, dimethylformanide (DMF) and acetone [67, 68, 69].
\nSolution casting helps to avoid thermo-mechanical degradation usually observed with the other methods of polymer processing which involve heating and vigorous mixing. It is used mostly for film formation. The amount of solvent used in this method makes solvent casting environmentally unsustainable. In addition, most of the organic solvents are hazardous to health and are temperature sensitive. Sur et al., in their work, prepared polysulfone nanocomposites using solution casting at elevated temperature [70]. To improve miscibility amongst the fibers and polymer matrix, the fibers were soaked using the solvent separately first before mixing with the dissolved polymer. In some cases, researchers coated the fibers with selected polymers to improve the fibers miscibility and interaction [71]. In general, solution casting is preferred for polymers with poor thermal stability and susceptible to thermo-mechanical degradation.
\nFor the past decade now, melt blending has become a method of choice in the processing or preparation of natural fiber composites. It involves the heating of the polymer matrix up to 10–30°C above its melting point and then introduced the fiber into the molten polymer with thoroughly mixing under shear [72]. Melt blending has gained much ground in terms of acceptability, because of the existent compatibility with existing processing technology (such as injection molding and extrusion) [73, 74, 75]. These methods are environmentally friendly and do not involve the use of hazardous solvents. Many research works have reported the use of melt blending method [58, 76, 77]. One area of concern is the processing condition and the level of interaction between the fibers and the polymer matrix used. According to [61], to obtain good distribution of the fibers within the matrix, which is one of the conditions for improved mechanical and thermal properties, there should be a favorable enthalpy of interaction between the fibers and the polymer matrix. This results in good distribution of the fiber inside the matrix. In the absent of this favorable energy, the fibers will be poorly dispersed. The conditions for processing natural fiber composites will be discussed elaborately in subsequent sections.
\nThis technique involves the polymerization of a monomer in the presence of another polymer, mostly in small quantities [78]. In-situ polymerization has been described as one of the important methods for compatibilizing polymer blends [79]. It allows the formation of covalent bonding between constituents which can result into graft or block copolymers that ultimately results in the development of a stable interface [72]. In-situ polymerization is noted to yield specific properties with conventional melt blending methods. Furthermore, it allows the preparation of composites with high fiber weight fraction because the homogeneity of the resultant composites is much greater than that obtainable from melt blending and solution casting [80]. Most thermoset NFPCs are prepared using in-situ polymerization methods [17, 78, 81]. According to Bounor-Legaré et al. [82], subject to the nature and reactiveness of the organic or inorganic precursors and the processing factors, different types of functionality can be fashioned.
\nThe preparation of natural fiber polymer composites with good strength is dependent largely on some factors mainly connected to (i) the fiber properties, (ii) the polymer matrix and (iii) the fiber-matrix interface properties. The strength and stiffness of any polymer composite is a direct function of the reinforcing fiber properties [83]. On the other hand, the matrix helps to keep in position the fibers and also helps in the transferal of load from fibers to fibers [84]. This segment dwells on the factors that contribute to the fiber-matrix relationship.
\nNatural fibers used for NFPC are abounded and can be sourced from different kind of plants and from any part of the plant. Figure 2 shows the classification of NF as primary and secondary fibers.
\nPlant fibers contain primarily cellulose, hemicellulose and lignin [85, 86]. However, the component of interest is the cellulose. It is a linear polymer of D-glucose units that are linked by β-1,4-glycosidic bonds. They are hydrophilic with the hydroxyl groups in each unit available to form hydrogen bonds which could be inter or intra molecular. This property helps the cellulose chain to be more stiff and enhance its rigidity [87, 88]. Cellulose is a semi crystalline polymer. However, because cellulose is surrounded by cementitious materials such as lignin and hemicelluloses, the percentage content of cellulose in any plant fiber determines its usefulness [87]. Table 2 gives a summary of % cellulose content in some selected plant fiber.
\nFiber type | \nCellulose (wt%) | \nHemicellulose (wt%) | \nLignin (wt%) | \n
---|---|---|---|
Abaca | \n12 | \n56–70.2 | \n5.6–12 | \n
Bagasse | \n17 | \n32–55.2 | \n19.9–25.3 | \n
Banana | \n9.4–22 | \n60–65 | \n5–32 | \n
Bamboo | \n11–17 | \n26–43 | \n21–31 | \n
Coir | \n4–6 | \n32–46 | \n32.7–45 | \n
Cotton | \n5.5–12.6 | \n82–96 | \n0.5–1 | \n
Flax | \n27.6–70 | \n60–81 | \n2–3 | \n
Hemp | \n6–70 | \n68–92 | \n2.9–13 | \n
Jute | \n26.5 | \n45–84 | \n5–26 | \n
Kapok | \n4 | \n13.16–64 | \n5.54–22 | \n
Kenaf | \n6.26–53 | \n37–72 | \n9–21 | \n
Pineapple | \n1.44 | \n80–85 | \n4.6–12.7 | \n
Ramie | \n24.5 | \n68–91 | \n0.6–9.25 | \n
Sisal | \n9.4–22 | \n43–78 | \n4–12.0 | \n
Percentage cellulose contents of some selected plants [18].
To increase this percentage of cellulose in the fibers, the material is subjected to different kinds of modification including alkaline treatment. Alkaline modification helps to remove the hemicelluloses, lignin and all other water soluble contents of the fibers, and by extension, increase the cellulose content [60, 89]. Some researchers have been able to extract nanocellulose crystals with improvement in the modification processes [90]. This includes the bleaching of the alkaline treated fibers and then subjecting them to acid hydrolysis, giving rise to better quality cellulose at the nanoscale [91, 92, 93, 94]. The treatment given to the fibers confirm on them increased rigidity with cleaner surfaces which exposes more of the hydroxyl groups to any further chemical modification [95, 96, 97]. Figure 3 shows SEM images of raw fibers and those treated at different condition. It can be seen that those treated with alkaline and then acid hydrolysis give a pulp like morphology.
\nSEM micrographs of untreated, alkaline treated and acid hydrolyzed treated fibers [73].
These nanoscale cellulose fibers have been reported to lead to improved interfacial interaction [91, 92, 93, 94, 96, 97, 98]. Although, fibers possess hydrophilic properties in nature and polymers are hydrophobic, to improve the interfacial interaction, further chemical modification of the fiber surface may be carried out. As earlier mentioned alkaline treated cellulose, especially the nanocellulose, have high concentration of hydroxyl groups on the surfaces that allow for their sites to chemically alter the natural fibers (NF). Different methods and strategies have been employed to achieve this by researchers as shown in the schematic diagram by [41, 73] given in Figure 4. Such chemical modification should be mild in order to prevent any deterioration of the other use properties.
\nTypical chemistry modification for cellulosic fibers [41, 73].
Furthermore, the physical properties, morphology and even the nano structure of the cellulose polymers depend greatly on the origin of the natural plant fibers and the processes and procedures of extraction. The extraction of nanocellulose from sisal, pineapple leaf and coir has been carried out [73, 99]. The results showed rod-like structures that are more separated with long, flexible and entangled morphology, especially from the banana rachis. This confirmed that the morphology and other physical properties of cellulose crystals is a function of the source of fiber. Furthermore, Le Bras et al. concluded in their work that the degree of crystallinity of the nanocellulose and its crystal structure depends on the method of extraction [100]. This was after the mechanical properties of the extracted nanocellulose were compared to each other and to those of their sources. Apart from this, the modified fibers have more uniform morphological structures. Also, there are reports that the thermal degradation property of natural fibers depends greatly on the level of modification given to the fibers (via acid hydrolysis, bleaching and alkaline treatment) and the source of the fibers [35]. This is because the nanocellulose obtained from such processes is more crystalline and rigid with uniform morphology. The factors that contribute to the variation in the lignocellulosic biomass include age of the plant, weather, plant type, soil nutrient, initial processes [87]. More recently, researchers have reported to have modified cellulose to allow for the introduction of functionalities to the polymer chains [41, 73]. The raw fiber can be pretreated using periodate oxidation and carboxymethylation techniques to introduce carboxyl and aldehyde functionalities which in turn could form covalent bonds with other functional groups such as amine. Fibers pretreated with bacterial method were modified with xyloglucan. This improved the wettability and cell adhesion for biomedical applications [101]. Chemical modification of cellulose fiber surfaces can lead to increased viscosity thereby reducing the shear thinning effect expected during processing. Therefore, fiber type, its modification and functionality can greatly improve fiber-matrix interfacial interaction, leading to improved performance properties.
\nNFPCs have exhibited significant potential for application in diverse sectors such as food packaging [102], fire retardant paperboard for semi structural applications [103], flexible printed electronics applications [104], etc. Nevertheless, there are numerous challenges to solve particularly associated with the development of proper large scale processing systems. The processing step of these materials is crucial because it is related to their final performance. Further studies are needed to prepare cellulose-based nanocomposites on industrial scale,
\nNatural fibers have the tendency to agglomerate in the polymer matrix as a result of formation of hydroxyl group’s hydrogen bonding. This hydrogen bond formation leads to poor dispersion of the fibers within the matrix and by extension poor matrix-fiber interaction [73, 105]. The dispersity of the polar fiber which is hydrophilic in nature is worsened by the nonpolar hydrophobic nature of the polymer matrix. This factor has limited the extent of applicability of natural fiber polymer composites. In order to expand the areas of application, the fibers would need to be consistently and uniformly distributed within the matrix. To enhance the dispersity of these fibers in their polymer matrices, the modification and functionalization discussed earlier will become very important. The OH groups could be replaced by more hydrophobic organic moieties to help increase the affinity amongst the polymer matrix and the modified fibers. This will reduce the possibilities of hydrogen bonding and increase the dispersity in the matrix. The functionalization of the fibers may depend on the end use application. Yang et al., improved celluloses’ suspension in aqueous media by acrylamide grafting on the surface by redox initiation grafting of extracted nanocellulose [106]. This led to improved self-assembly of the lyotropic state. Also, phosphorylation techniques with negatively charged phosphoric acid as phophoryl donor were used to modify the cellulose surfaces at the nanoscale level by [107]. Furthermore, with the right conditions, the hydroxyl groups were oxidized to dialdehyde using NalO4 [108]. Bae et al., used bimolecular nucleophilic substitution to replace the hydroxyl groups with long hydrophobia alkyl chains, in order to impart hydrophobicity to the cellulose polymer chain [109]. Also polycaprolactone diol (PCL) long chains were suggested for the surface modification of cellulose using what they referred to as click chemistry and esterification reactions [110]. Although it was reported that greater grafting yields were detected with the click chemistry when compared to the esterification method. The pretreatment given to the fibers also affects the extent to which the fiber surface can be modified.
\nDuring the processing of NFPCs, the processing temperature, mixing speed and residence time are all important for any melt blending process while for in-situ polymerization; the temperature and curing time are of importance [58, 78, 79]. For NFPCs to be prepared via melt blending, the temperature must not be too high to avoid the degradation of the natural fibers. Since natural fibers are thermally stable below 200°C, above this temperature, the integrity of the fibers cannot be guaranteed. Therefore, polymers with higher melting temperature may not be used in the preparation of NFPCs or alternative processing methods are applied. One factor to bear in mind is that the polymer must be molten enough to wet the fibers. This means that the Gibb’s free energy of interaction tend towards negative. As the fibers are added, the viscosity increases. This increase is dependent on weight percentage of fibers added [13]. However, if the shear rates are increased it could minimize the effect of the increased viscosity [75, 77, 111, 112, 113]. Good fiber-matrix interaction can only be achieved if the polymer can wet the fiber surfaces properly. The resident time for processing the NFPC is also very important, one cannot use the same processing time as used for the neat polymer or blends, for NFPC, if other parameters are to remain the same. As mentioned earlier, the addition of fibers leads to change in viscosity; therefore NFPC will require more time to achieve good wettability. However, the option of increasing the shear rate or mixing speed might compensate for the change in viscosity. Therefore it may be possible to use the same resident time during processing. It must be mentioned that every option has its advantages and disadvantages. For example, longer time and increased mixing speed may lead to thermomechanical degradation [75].
\nIn the preparation of composites, additives are added to help improve specific properties. For example, nanoparticles are added to enhance the mechanical and thermal properties through better crystallinity growth and stabilization of phase morphology [114, 115].
\nCompatibilizers are added to increase interfacial interactions amongst polymer-polymer in blends and polymer-fibers in composites [10, 41, 116]. The use of compatibilizers to improve interfacial interaction is widely reported [117]. In a series of works by Kamaker and other co-researchers [118, 119, 120], it was reported that Jute/PP composites’ mechanical properties were improved drastically, when 3 wt% maleic anhydride grafted polypropylene (MAHgPP) was used to treat the Jute/PP composites as coupling agents. The tensile strength increased from 29.82 to 59.13 MPa, a 98% increase. Also, the bending strength was reported to increase from 49.97 to 87.66 MPa, a 75.4% increase. In related work, the tensile, flexural and dynamic strength of Jute/PP composites were enhanced by approximately 50% when the jute fibers are treated with 0.1 wt% MAHgPP solution of toluene, although the impact strength was negatively affected [121, 122]. Li et al., investigated two different kinds of silanes as coupling agents to treat sisal fibers surfaces [15]. The coupling agents were diluted in acetone to 6% concentration before use. A 24 h immersion of the sisal fibers was done using the coupling solution after which it was washed with acetone and dried up in the oven for 4 h at 60°C. Their results showed that the sisal surfaces were etched and they were very rough, which led the unbundling of the fiber bundle into smaller fibers, as seen in Figure 3. This increased the operative surface area presented for contact with the polymer matrix. Although, it was reported that the interaction at the interface was more of mechanical interlocking with less of chemical bonding. Therefore, the observed increase in load was due to frictional shear stress transferal across interface. Other coupling agents which had performed relatively well, have also been reported by other researchers [11, 123, 124]. However, to chemically modify the surface properties of the cellulose fibers to the extent that they can in turn influence the polymer composites properties significantly, it is suggested that the fibers should be modified to its nanoscale [125, 126].
\nNanocellulose particles are derived from rigorous chemical modification of plant fibers using a combination of alkaline and acidic solution in phases. At the nanoscale chemical modification is relatively easier; large numbers of the OH groups at the surface are more exposed; the amorphous components of the fibers have been eliminated, leaving only the crystalline part of the cellulose material. The nanoscale cellulose fibers when modified have wide application [127, 128]. Filler or additives can be described as materials which are added to the matrix in low percentages ranging from 0.1 to 5 wt% in order to improve performance and impact some special properties [129]. Some of the fillers are low-cost, allowing for a cost effective measure for the enhancement of performance properties. In addition, they can improve the processing of the material by controlling the viscosity of the resin [130]. Common fillers used in NFPCs include metal particles, nanosize cellulosic materials (CNCs), silica, nano-clay, maleic anhydride (MA) and carbon nano-tubes (CNT) [131]. Mohanty et al. showed that better interfacial adhesion existed amongst the fiber/matrix owing to filler addition in the NFPC as evident from the SEM micrographs of the fractured tensile samples; this resulted in the improvement of the mechanical properties [132]. Mechanical properties enhancement were resultant from the adding of fillers at low wt% which has led to the consistent assembly observed and enhanced stress transfer amongst the fiber and the matrix [1]. Meanwhile, at higher wt% of fillers, there was deterioration in the properties of the NFPCs, due to agglomeration of the fillers and the interfacial adhesion between the polymer matrix and fiber were noticed to be weak. Furthermore, it was suggested that the rise in tensile modulus and the fall in impact strength of the NFPCs with clay fillers were as a result of the polymer matrix improved cross-link density, which led to a decrease in the stiffness of the composite, hence reduced the impact strength [130, 133]. While in other studies, aluminum powder was used as fillers and in others, modified clay improved the impact strength of the composite, as the SEM micrographs revealed the existence of less voids and rise in density along with improvement in stiffness resultant from better interfacial adhesion amongst the fiber and the matrix in the presence of the modified clay [134, 135]. Other advantages of filler addition to sisal fiber reinforced polymer composites are increased moisture absorption or reduced water uptake as reported by [135, 136].
\nThe addition of nanoparticles to NFPC to improve their interfacial properties has gained more popularity in recent time. Nanoparticles incorporation into polymer composites has been reported to improve their strength and young’s modulus, as can be seen from earlier discussion. The addition of these nanoparticles at very low concentration of approximately 0.1–1.0% had influenced the mechanical properties of the NFPCs [137]. The modifications of the particles by some researcher have led to improved chemical interactions when added to the composites. Thereby improving interfacial bonding and by extension, mechanical and thermal properties [138, 139, 140]. Moreover, the addition of inorganic nanoparticles has helped to improve both thermal and mechanical [131]. This has influenced the crystallization process during processing of the composites. The improved crystallinity can encourage superior mechanical interlocking of the polymer-fiber interface.
\nHybrid fibers are a combination of two or more different fibers to make a composite. The addition of glass and/or carbon fibers to form hybrid fibers has also contributed to improving the composite properties. Allamraju et al., reported an increase in the compression and tensile strength of Jute/glass hybrid fibers epoxy composite, as a result of percentage increase in mass fraction of jute fibers [141]. Their results showed that the measured strengths increased as the fiber load increases from 6 to 9%, after which there was a decrease. The 9 wt% jute fibers that was reported as the optimal loading was attributed to higher stiffness of the composites and an improved fiber-matrix adhesion.
\nHybrid composites are prepared by the combination of two or more different type, shape or size of reinforcement [142]. The crossbreed composite properties is completely dependent on many elements such as, extent of intermingling of fibers, fibers orientation, fiber surface roughness, compatibility between the fibers and their matrix, and the property of the individual fibers [143]. Recently, investigations on the properties of the crossbreed composites were centered on the natural/synthetic fibers, natural/natural fiber and natural/synthetic/additive modified reinforced polymer composites. Essentially for applications that required such hybrid/crossbreed composites with stiffness and high strength, but the employment of pure natural fiber polymer composites is difficult.
\nThe popularity of these crossbreed types of composites is increasing rapidly owning to their capability to provide freedom to tailor the composites and achieving properties that cannot be acquired in composite encompassing only one kind of material [13, 144]. One of the major reasons for creating crossbreed NFPCs is to utilize the pluses of the fibers and lessen some drawbacks [145]. Another reason is based on economy, which is to decrease the cost of the finished composite product. Even though the usage of natural fibers in composites is less costly in comparison to the orthodox reinforcements, there are significant differences in the costs of natural fibers. Therefore, partially substituted cotton fibers in a composite made with wood fibers could offer very huge benefits in terms of the performance of the composite and also in the manufacture prices. The hybridization of wood flour- polypropylene composites with waste cone flour (20–40 wt%) was reported the composite was said to have been negatively affected in terms of their flexural properties and water resistance of the composite [146]. However, adding pine cone flour (10 wt %) to the composite revealed no substantial consequence on the measured properties, i.e. water absorption and flexural strength properties. This means it is economically advantageous. Further research showed that reducing the amount of pine cone flour added to the composite lead to positive improvement.
\nHybrid composites of sisal fibers and short banana fibers were also prepared using a polyester [147, 148]. From the result obtained, the tensile strength of the polyester composite was observed to rise as the volume fraction of the banana fiber was increased. On the other hand, the impact strength of the composites was affected negatively with increasing volume fraction of the banana fibers. Nevertheless, the impact strength improved with rise in total content of the fibers used. The observed properties were ascribed to two factors: (i) the lower microfibrillar angle of the banana fibers (11°) as compared to that of sisal (20°) and (ii) the better compatibility between the polymer matrix and banana fibers, which decreased the possibility of fiber pullout.
\nIn the same vain, Venkateshwaran et al., prepared the same hybrid of banana and sisal fibers using epoxy resin in order to determine the optimal quantity of banana fibers with regard to its tensile properties [149]. The results revealed that about 50% of the complete fiber content added was good enough to impact significantly on the tensile strength of the composite. The differences in the morphologies of the different fibers have been shown to be of significant advantage when used as hybrid in a composite [142].
\nFurthermore, Fernandes et al., prepared hybrid composites of cork and coir fiber using high density polyethylene (HDPE) matrix [150]. With a coupling agent present, adding 10 wt% coir fibers to the composite caused a 30% rise in tensile maximum strength and a 39% rise in the tensile modulus. The overall effect of the coir fiber on the hybrid composites was very evident when compare to the single fiber composite, even with the coupling agent. Therefore, it can be said that the hybridization of NFPCs, most especially with natural/natural fibers, presented an efficient, sustainable and high economical way of improving the performance of the composites at a reduced cost. Also the addition of compatibilizers is still a necessity in order to create the needed covalent interactions required to enhance the performance characteristic property [151].
\nNatural fibers mixed with synthetic fibers hybridization could provide the desirable strength of a composite due to their synergistic effects [152]. Conversely, as a result of environmental impacts and disposal issues relating to the synthetic fibers in addition to hybrid strength requirements for specific applications, the final fiber ratio would be a 50:50 ratio (natural: synthetic). This ratio, offers a balance and intermediary mechanical properties in comparison to mechanical properties of either the synthetic or sisal fiber composites. Natural/natural fibers hybridization in a composite could be beneficial as a result of the possible disparity in cellulose quantity of the natural fibers used. This has a substantial effect on the composites mechanical properties and individual fibers have their distinctive characteristics which can be tailored for defined applications. A combination of such fibers together can bring about the needed properties for such application and still remain environmentally friendly. These biocomposites could be used in secondary/tertiary structures and other applications that require low stiffness and strength. Senthilkumar et al., highlighted that the enhancement in the mechanical properties of the hybrid composites was due to the strong impact from the type of polymer matrix used, fiber treatment technique, individual fiber loading and fiber choice [153]. Additionally, the enhancement in mechanical properties for natural/synthetic hybrid fiber reinforced composites was more significant than that of natural/natural hybrid fiber reinforced composites. It is the fiber/matrix interface adhesion that is responsible for the significant disparity observed in their mechanical properties for natural/synthetic fiber reinforced composites when compared to that of natural/natural hybrid fiber reinforced composite which displayed weak interfacial adhesion, more fiber pull out when under stress and uneven natural fiber distribution in the developed hybrid composites [153].
\nThe general resolve for combining any two fiber kinds together in a single composite is to preserve the advantages of the two fibers in the new material and eliminate to the barest minimum their individual drawbacks [145, 154, 155, 156, 157]. The synthetic fibers are known to possess good mechanical properties and thermal stability. They also lead to increase in overall weight of the composite, thereby eliminating the light weight advantage a complete natural fiber composite bears. However, the idea of combining natural fibers and synthetic fiber is influenced by the following parameters [152, 158, 159].
Relative amount of fiber
Elastic properties of the fiber
Failure stain ratio
Fiber strength distribution
Degree of dispersion and uniformition
Matrix properties
In summary, the addition of other component to NFPCs has led to reduction in some of the problems associated to their fiber-matrix interface. Compatibilization have helped reduce fiber agglomeration, water absorption and improved dispersity in the matrix.
\nThe application of NFPCs comes with different requirements. These requirements are specific to application demands which include mechanical properties, thermal stability, transparence, conductivity and operational temperature. These factors are not unconnected to the factors considered before processing. For mechanical and thermal stability, the design of the NFPCs are considered from the point of improved interfacial interaction, using compartibilizers, fiber surface modification, addition of other chemical components and lastly reducing the fibers to nanosizes.
\nThe automotive industry is one of the major end user playing a key role in the utilization of NFPCs. In the early ‘90s, Mercedes-Benz was the first, as a carmaker, to use NFPC, by building panels for doors with jute fibers [160]. This resulted in other car makers following suite, utilizing natural fibers comprising polymer composites for parcel shelves, headrests, upholstery, door panels, etc. The widespread adoption can be linked to the advantages of NFPCs, relating to the impact on the environmental, cost, elastic modulus and weight. No matter the applications, it was always a necessity to increase the mechanical properties of the composites via pre-treatment techniques (as discussed earlier). The fibers which have been treated were used in several ways, in order to obtain non-woven structures, mats, etc. [9]. Researchers have shown that subjecting natural fibers to some form of distinct treatment could lead to the development of high-quality composites with mechanical properties which are similar to those of glass fiber composites [160]. An outcome that would have ordinarily been very difficult to achieve because of natural fibers’ hydrophilic nature which encourages water molecule absorption and agglomeration with no adhesion to the polymer matrix; This is the challenge and much works is ongoing to overcome this challenges [160, 161].
\nFor conductivity, the addition of inorganic nanoparticles has been used and this has served a dual purpose of also improving the mechanical and thermal properties. Transparency is best impacted on NFPCs by the use of nanocellulose modified or not, with careful selection of the matrix. Some of the biodegradables are considered as having transparent properties including PLA. For water and gas permeability, applications are numerous with good water permeability. Such composites can be applied in water filtration processes, while for low water permeability composites; can be applied in packaging.
\nResearchers have reported positive impact of cellulose fibers on moisture and gas barrier performances for biodegradable polymers after modification with nanosize celluloses [162, 163]. Ambrosio-Martin and his colleagues prepared biodegradable composites of PLA using CNCs [164]. They reported improvements of barrier properties of oxygen and water which was due to the addition of well-dispersed OLLA-BCNCs. The researchers hypothesized that the nanofillers were able to make a tortuous path for the permeation of gas and water, thereby acting as blocking agents inside the polymeric matrix and hence, causing an increase to the barrier properties of the material. In these materials, the CNCs good level of dispersion within the polymer matrix, the morphology and its orientation led to enhanced tortuosity effects, thereby, heightening the barrier properties of the materials [165, 166]. Sanchez-Garcia and co-workers did similar work on PLA biodegradable materials and reported a decrease in the water permeability capacity and oxygen of approximately 82 and 90% respectively on addition of CNC to the PLA matrix [167]. In contrast, Espino-Pérez et al., highlighted results that were entirely opposite after compounding PLA with n-octadecyl-isocyanate-grafted-CNCs [168]. In their publication, it was clear that there was no reduction in oxygen permeability on adding CNCs into PLA. Apart from investigations about the tortuosity effects and barrier properties, researchers have tried to relate the improvement observed for the barrier properties to the materials crystallinity changes on addition of the nanofillers to the polymer matrix [169]. Fortunati et al, highlighted the improvements in barrier properties of PLA/CNC nanocomposites as well as increased crystallinity simultaneously, which was attributed to the addition of CNCs [170]. Espino-Pérez and co-workers investigated CNC/PLA nanocomposites using a high D-lactic acid content (a material which under normal processing conditions cannot crystallize) as matrix [171]. In conclusion, they indicated that the tortuosity effect of CNC on the oxygen barrier properties is limited. Although, after addition of modified CNS, significant improvement in the water vapor barrier properties was observed. They reported the swelling of unmodified CNCs due to absorption of water as a result of their hydrophilicity, which encouraged the pathway for mass transport and this property was not demonstrated when modified CNCs were employed because the surface modification caused the reduction in the hydrophilicity of the nanoparticles [172]. Follain et al., also reported that other elements can be considered to be significant in moisture and gas barrier performances of CNC-based nanocomposites [173]. They indicated that the formation of a 3D network and close interfacial adhesion between PCL chains and CNC can result in the matrix having structural defects, which encourage transfer of gas. Hence, their results highlighting the barrier properties of CNC-based nanocomposites allow for the conclusion that the tortuosity effect is influenced by CNCs, CNC surface chemistry, the structure of the nanocomposite. Also, that change(s) in crystallinity of the host matrix play a vital role on moisture and gas barrier performances of the material.
\nBiodegradation has been described as a vital prerequisite for biomedical materials, agricultural mulches and the packaging industry, as a result of the high level of consumption of these materials. Thus, the preparation of biodegradable polymers with improved properties is necessary but not without its own challenges. However, it will be exceptional to alleviate the concerns of landfills, chiefly in countries which are yet to adopt the technique of composting. A lot of research output has shown enhanced biodegradation for a number of polymer matrices when cellulosic fibers are added to them [174, 175]. However, the surface modification of the cellulose fibers negatively influences the matrix degradation because it reduces the number of OH group on the cellulose surface and so decreases the hydrophilicity [176]. Pinheiro and co-workers prepared poly (butylene adipate-co-terephthalate) PBAT-based composites with modified and unmodified cellulose fibers [174]. They presented from their results that the addition of unmodified cellulose fibers caused more weight reduction and this was attributed to the hydrophilic properties of the nanocrystals that hastened the hydrolysis of PBAT. In another related work, Monhanty et al, reported similar findings and also highlighted that the hydrophilic properties of the reinforcement encourages the degradation of the polymer [177]. The crystal size [178] and crystallinity of the polymer matrix [179, 180] have also been reported to playing a vital role in the degradation degree of the matrix, considering that regions which are crystalline are relatively unaffected by hydrolysis [178, 179, 180, 181, 182].
\nThe use of other methods such as micro-fibrillation, laser, and ionomer to enhance the mechanical properties of materials have been reported. Choudhury and co-workers highlighted the capacity to improve the tensile and flexural properties of NFPCs by ionomer treatment of natural fibers [183]. The improvement was as a result of uniform stress dissemination and good dispersion of the fibers inside the matrix. This enhancement in mechanical properties by the microfibrillation was largely ascribed to the larger interaction observed between the polymer and fibers after the treatment by micro-fibrils and aggregates.
\nThe selection of polymer matrix in all these areas of application becomes very important and sensitive. Although there are general purpose polymers with little or no health concerns for examples PP, PE, HDPE. When these polymers are compounded with NFs, their composites become more susceptible to microorganism attack, thereby making them biodegradable.
\nThe dependence of performance properties on a strong fiber-matrix interface cannot be over emphasized. Fiber-matrix interfacial interactions are very important properties of all polymer composites. The performance properties are highly dependent on the kind of fiber-matrix interfacial bonds formed. These bonds can be physical or chemical in natural. The physical interaction includes interlocking between the matrix and the fibers, which is as a result of the rough edges of splits caused by the various surface treatments subjected to the fibers. While chemical interactions include the formation of bonds from the weak Van der Waal force to a strong covalent bond. The chemical bonds can be induced by (i) the type of surface treatment given to the fibers, which be either be a chemical or biological treatment and (ii) the deliberate addition of selected compatibilizers which confirm specific functionality on either the fibers or the polymer matrix. Furthermore, the addition of nanoparticles has been reported to help improve interfacial interactions through the direct participation in the crystallization processes which increases rigidity of the polymer matrix and thus enhances the physical interlocking at the interface. The use of hybrid fibers of polymer blends is another way of improving the interfacial interaction in NFPCs. Hybrid fibers can be natural/natural or natural/synthetic. While the natural/synthetic hybrid fibers clearly have better thermal and mechanical properties, their effect on the environment will always be of great concern. With appropriate surface treatments, natural/natural hybrid fibers have been reported to display improved thermal stability and good mechanical properties. Also, the use of polymer blends has resulted in improved interactions. The choice of processing methods and conditions can undermine the kind of and extent of interaction formed. While the in-situ polymerization is used for thermosets, it mostly leads to the formation of covalent interactions. The thermoplastics are prepared using melt blending which mostly gives rise to interlocking or at most Van der Waal force types of interaction at the interphases, although compatibilizer can be added the form covalent interactions. However, melt blending processes are more prone to thermomechanical degradation, which is likely to affect the blends performance properties. In conclusion, to ensure that the materials with the required properties are developed, it is necessary that the factors discussed above are properly considered.
\nThe financial assistance of the University of Zululand and the National Research Foundation, South Africa through the South African Research Chair Initiative (SARChI) is hereby acknowledged. OSJ thanks the National Research Foundation (NRF) for a postdoctoral fellowship and funding under South African Research Chair for Nanotechnology.
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