International Journal of Environmental Science and Technology

https://doi.org/10.1007/s13762-018-1890-9

REVIEW

Comparison of different natural fiber treatments: a literature review

B. Koohestani1,2   · A. K. Darban3 · P. Mokhtari4 · E. Yilmaz5 · E. Darezereshki1

Received: 9 October 2017 / Revised: 11 June 2018 / Accepted: 26 June 2018

© Islamic Azad University (IAU) 2018

Abstract
Interests in the use of natural fibers–fillers in composite materials are growing rapidly due to the low cost and high availability.
However, poor surface adhesion and mineralization are the main drawbacks that restrict the use of natural fibers in differ-
ent applications. Thus, it is essential to perform a treatment that can improve the surface properties of natural fibers before
being used in the composites. Such treatments are physical (corona, plasma, etc.), chemical (alkaline, silane, acetylation,
etc.), and biological (enzyme), but the benefits of each treatment considering energy consumption and effluent generation
should be considered more in-depth. Via a literature review, this study investigated the mechanical performance, energy
consumption, and generated effluents of chemical treatments (silane, alkaline, acetylation, and maleated coupling) as the
consequence of fiber treatment to propose a more sustainable treatment at the scope of the treatment section in the factory
of natural fibers–polymer composites (gate to gate). It was shown during this review study that the maleated coupling is a
more sustainable method since it needs no specific energy during the treatment while produces no effluent and improves the
mechanical strength performance of the composites more constantly.

Keywords  Natural fibers–fillers · Physical treatment · Chemical treatment · Biological treatment · Surface properties

Introduction biodegradability and recyclability of the filled composite

The addition of natural fibers/fillers to the composite materi-
als provides several advantages including mechanical perfor-
mance improvement, eco-friendliness, flexibility, cost reduc-
tion, storing biogenic carbon, and biodegradation (Boland
2014; Koohestani et al. 2013; Mohammed et al. 2015). For
example, the addition of lignocellulose fibers (e.g., plant
fibers) decreases the density and cost while increases the
Editorial responsibility: Agnieszka Galuszka.
* B. Koohestani
b.koohestani@modares.ac.ir
1
Mining, and Mineral Processing, Tarbiat Modares
University, Tehran, Iran
2
Université du Québec en Abitibi-Témiscamingue, 445
Boul. de l’Université, Rouyn‑Noranda, QC J9X 5E4, Canada
3
Faculty of Engineering, Tarbiat Modares University, Tehran,
Iran
4
Materials Science and Nano Engineering, Sabanci University,
Orta Mahalle, 34956 Tuzla, Istanbul, Turkey
5
First Quantum Minerals Ltd., Cayeli Bakir Isletmeleri A.S.,
PO Box 42, 53200 Madenli, Cayeli, Rize, Turkey
(Al-Maadeed and Labidi 2014). However, natural fibers
are hydrophilic materials and due to the high specific sur-
face energy are highly prone to the agglomeration; thus,
any treatment that improves the dispersion, adhesion, and
compatibility of which with the composite’s matrix (e.g.,
polymeric) is recommended (Müller et al. 2017; Saba et al.
2014). In addition, specific enzyme systems of degrading
fungi no longer recognize the treated natural fibers (e.g.,
wood fibers) as a nutrient medium while the lowered equi-
librium moisture content no longer promotes decay (Homan
and Jorissen 2004).
A variety of chemical, physical, and biological treat-
ments such as silane, alkaline, acetylation, enzyme, maleated
coupling, plasma, and corona are available to alter the sur-
face properties of the natural fibers (Pickering et al. 2016).
Chemical treatments use a chemical agent to change the
chemistry and surface properties of the natural fibers by
different mechanisms such as the eliminating weak bound-
ary layers, changing the acidity–alkalinity of the fibers, and
constructing a tough and flexible layer on top of the fiber’s
surface (Chand and Fahim 2008). Therefore, when chemi-
cally treated natural fibers embedded within a polymeric
matrix, a highly cross-linked interphase region and chemical

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bonds (e.g., covalent bonding) may be formed between the
fiber and matrix (Kabir et al. 2012; Koohestani et al. 2017b).
However, the growing environmental and energy-saving con-
cerns may lead to the gradual replacement of many chemi-
cal treatments that use a considerable amount of water and
energy while simultaneously producing different effluents
(Shishoo 2007). The physical treatments (e.g., corona and
plasma) on the other hand alter the structural and surface
properties with minor influence on the chemical composi-
tion of the fibers and hence mainly improve the mechanical
bonding between the fiber and matrix (Biagiotti et al. 2004;
Mohammed et al. 2015). In the field of biological treatment,
mainly specific enzymes are used to react with natural fib-
ers and change the properties of the fibers. In this case, the
systems of degrading fungi no longer recognize the treated
natural fibers as a nutrient medium while the lowered equi-
librium moisture content no longer promotes decay (Homan
and Jorissen 2004). To determine which treatment type is
more beneficial and applicable at industrial scale, the con-
sumed amount of energy and generated effluents/by-products
in treatment procedure should be combined with mechanical
performance improvement results of the composites used
treated natural fibers.
Composite materials are composed of two or more dis-
tinct constituents or phases with the properties, noticeably
different from each constituent (Fangueiro 2011). The ther-
momechanical properties, the orientation and distribution
of the reinforcement phase, and the interfacial properties
between the phases provide the ultimate properties and per-
formance of the filled composite. In this form, both fibers
and matrix retain their physical and chemical properties, yet
they produce a combination of the properties that cannot be
achieved with either of which individually (Chung 2010).
The mechanical properties of the composites depend on
the matrix, fibers, and the interface properties. In fact, the
loaded forces transfer from matrix to the fibers and hence
improved interfacial properties transfer the forces more effi-
ciently (Koohestani et al. 2017b).
Fibers as the principal load-carrying members of com-
posites are classified as glass fibers, carbon fibers, ara-
mid fibers, natural fibers, boron fibers, and ceramic fibers
(Mallick 2007). In comparison with synthetic fibers filled
composites, the disposal of composites containing environ-
mentally degradable natural fibers is easier, safer, and less
expensive (Al-Maadeed and Labidi 2014). In addition, the
required amount of energy per produced amount of natural
fibers such as flax fiber (including activation, harvesting and
fiber preparation) is only 9.55 MJ/kg, whereas this energy
for glass fiber is 54.7 MJ/kg (Joshi et al. 2004). The lower
density of natural fibers (~ 1.4 g/cm3) in comparison with
glass fibers (~ 2.5 g/cm3) may also provide a higher specific
strength and stiffness to the filled composites, but the mois-
ture uptake, fungal–insect attack, and poor surface adhesion
to the hydrophobic matrices should also be considered when
natural fibers are used (Yi et al. 2017). Table 1 displays dif-
ferent properties of most common natural and man-made
fibers (Gurunathan et al. 2015; Li et al. 2007).
Natural fibers are generally derived from plant, animal,
or mineral resources (Chandramohan and Marimuthu 2011).
All the plant fibers are composed of cellulose, while animal

Table 1  Physical and Type of fiber Density (g/cm3) Strain at break (%) Tensile strength (MPa) Young’s
mechanical properties of some modulus
natural and man-made fibers (MPa)

Flax 1.4–1.5 1.2–3.2 345–1500 27.6–80

Hemp 1.48 1.6 550–900 70
Jute 1.3–1.46 1.5–1.8 393–800 10–30
Kenaf 1.2 2.7–6.9 295–930 22–60
Ramie 1.5 2–3.8 220–938 44–128
Banana 1.35 5–6 529–914 27–32
Nettle 1.51 1.7 650 38
Sisal 1.33–1.5 2–14 400–700 9–38
Coir 1.2 15–30 175–220 4–6
Pineapple 1.5 1–3 170–1627 60–82
Abaca 1.5 2.9 430–813 33.1–33.6
Bamboo 0.6–1.1 1.3–8 140–441 11–36
Cotton 1.21 3–10 287–597 5.5–12.6
Hardwood 0.3–0.88 – 51–120.7 5.2–15.6
Softwood 0.3–0.59 4.4 45.5–117 3.6–14.3
E-glass 2.5 2.5 2000–3500 70
S-glass 2.5 2.8 4570 86

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International Journal of Environmental Science and Technology

fibers (hair, silk, and wool) consist of proteins. Plant fibers
include stem, leaf, seed fruit, wood, cereal straw, and other
grass fibers (John and Thomas 2008). Wood fibers (soft-
wood or hardwood) are derived from shrubs and trees and
are heterogeneous, hygroscopic, cellular, and anisotropic
solid material composed of cellulose and hemicellulose held
together by lignin. Softwood fibers are comprised of cells,
mostly of one kind, tracheid, that makes the material more
uniform in structure (no vessels or pores in contrast to hard-
woods) (Chand and Fahim 2008; Pickering 2008). Cellu-
lose, as a natural polymer that consists of d-anhydro glucose
­(C6H11O5) and three hydroxyl groups, is resistant to strong
alkali and oxidizing agents but easily hydrolyzes to water-
soluble sugars by acid (John and Anandjiwala 2008). Hemi-
cellulose includes a group of polysaccharides composed of
5–6 carbon ring sugars while exhibits a considerable degree
of chain branching containing pendant side groups giving
rise to its non-crystalline nature. Being hydrophilic and
hydrolysable in acids and soluble in alkali, hemicellulose
holds the cellulose microfibrils together (Verma et al. 2016).
Lignin is a three-dimensional amorphous and hydrophobic
copolymer that composed of hydroxyl and carbonyl groups
while provides rigidity to the plants. It is not hydrolysable
by acids, but it is soluble in hot alkali and readily oxidizes
and condenses with phenol. The main difficulty in lignin
chemistry is that no method has been established to iso-
late it from the fiber. Pectins provide flexibility to the plants
while consist of different types of alcohols (Cristaldi et al.
2010; John and Thomas 2008). Table 2 provides the major
chemical composition of the some common natural fibers
(Gurunathan et al. 2015; Li et al. 2007).
The role of the matrix in composites is to maintain fib-
ers/fillers in place, transfer stress to the fibers, provide a
barrier against environmental damages, and protect the
surface of the fibers against degradation (Mohammed et al.
2015). Composite materials are typically classified by their
matrix type as polymer matrix (PMC), metal matrix (MMC),
ceramic matrix (CMC), and cement-based matrix (CBM) or
reinforcement form as particulates, flakes, whiskers, short
and long continuous fibers (Mallick 2007). The polymeric
matrices are classified into two categories, thermoplastic
and thermoset, while the use of bio-fibers is more common
in thermoplastics (Malkapuram et al. 2009). Polymers that
soften or melt upon heating, called thermoplastics, consist
of linear or branched chain molecules having strong intramo-
lecular and weak intermolecular bonds. Thermoplastics are
either semi-crystalline or amorphous in structure while melt-
ing and solidification of which are reversible (Koohestani
et al. 2017a). Only polyolefins like polyethylene and poly-
propylene (thermoplastics) whose processing temperature
does not exceed ~ 200 °C can be processed with natural
fibers. Thermoplastics are more commonly used with short
fibers via injection molding (Bledzki and Gassan 1999; Pick-
ering 2008). Thermosets have cross-linked or network struc-
tures with covalent bonds between all the molecules (Yu
et al. 2009). They do not soften but decompose on heating

Table 2  The main chemical Type of fiber Cellulose (wt%) Lignin (wt%) Hemicellulose (wt%) Pectin (wt%)
compositions of most common
natural fibers Bark/stem fiber
Flax 71–78 2.2 18.6–20.6 2.3
Hemp 57–77 3.7–13 14–22.4 0.9
Jute 45–71.5 12–26 13.6–21 0.2
Kenaf 31–57 15–19 21.5–23 3–5
Ramie 68.6–76.2 0.6–0.7 5–16.7 1.9
Banana 63–64 5 10 –
Nettle 86 5.4 4 0.6
Leaf fiber
Sisal 47–78 7–11 10–24 10
Curaua 73.6 7.5 9.9 –
Pineapple 80–83 8–12 15–20 2–4
Abaca 56–63 7–9 21.7 1
Henequen 77.6 13.1 4–8 –
Fruit/seed fiber
Cotton 85–90 0.7–1.6 5.7 0–1
Coir 36–43 41–45 0.15–0.25 5.2–16
Oil palm 65 19 0–22 –
Wood
Hardwood 43–47 16–24 25–35 –
Softwood 40–44 25–31 25–29 –

13

and once have been solidified by cross-linking cannot be
reshaped. Common examples of thermosets include epox-
ies, polyesters, and phenol formaldehyde (Pickering 2008).
Thermoset polymers are more commonly used as matrix
material in continuous or long fiber-reinforced composites,
mainly because of the ease of processing due to their low
viscosity (Koohestani et al. 2017a; Mallick 2007; Pickering
2008).
Cement is basically calcium silicate with the ­SiO4 tet-
rahedron building block (Chung 2010). The formation of
the cementitious matrix occurs through the exothermic and
alkaline hydration when water enters the cement crystals
and forms hydrated calcium silicate gel (abbreviated C–S–H,
with the average chemical formula 3CaO·2SiO2·3H2O) and
calcium hydroxide or portlandite (CH as the second major
product of hydration) (Koohestani et al. 2018b). The interac-
tion between the natural fibers and cement may be chemical,
physical, or a combination of both, while chemical bonds
are assumed to be hydrogen bonds and/or hydroxide bridges
(Frybort et al. 2008). In addition, natural fibers may interact
in hydration procedure, adsorb to the cement particles, affect
the surface tension of water, and add some specific chem-
icals to the cement (Koohestani et al. 2013, 2016). Even
though natural fibers bring some advantages to cementitious
materials (e.g., tensile strength improvement), the physical
properties of natural fibers should not be deteriorated in
alkaline condition during the cement hydration (Clauft 2008;
Koohestani 2017; Koohestani et al. 2016; Sobral 2004). The
main drawbacks of natural fibers in cementitious materials
include low elastic modulus, high water absorption, capa-
bility of fungal and insect attack, lack of durability in an
alkaline environment, and containing a wide range of car-
bohydrates that may delay the cement hydration (Koohestani
et al. 2013). In this case, the addition of some complemen-
tary additives such as ­CaCl2 and ­MgCl2 (between 1 and
5%) may accelerate the hydration of cement and overcome
the retarding influence of inhibitors such as phenolic com-
pounds and free carbohydrates (Atadana 2010; Koohestani
et al. 2017a; Mohr et al. 2007; Toledo Filho et al. 2003). In
addition, performing a pre-treatment may also prevent some
common problems of natural fibers in cementitious materi-
als, but it must be clear that the treated fibers do not add
some other chemicals that influence the hydration process
negatively (Koohestani 2017; Švegl et al. 2008).
Life cycle assessment (LCA) is an approach that evalu-
ates the sustainability of a product or an activity based on
the environmental, social, and economic advantages and
disadvantages (Hill 2007; Lopsik 2013; Zaman 2013). In
this approach, environmental consequences will be identified
and quantified by the amount of consumed energy (embod-
ied energy), materials used, and effluents during the entire
life cycle of that product, process, or activity (Clark and
Macquarrie 2008; Nouri et al. 2012). The embodied energy
13
International Journal of Environmental Science and Technology
presents the required amount of energy to prepare, maintain,
and replace a product on its entire life cycle; thus, elevated
consumed amount of energy reduces the sustainability. The
embodied energy that gives an approximate to the global
warming potential is estimated based on the amount of
consumed energy (J) per mass (kg) or volume ­(m3) of the
produced product or activity. The embodied energy for the
preparation of lignocellulosic, glass, and carbon fibers var-
ies between 4–15, 30–50, and 130 MJ/kg, respectively (Hill
2007; Vuure et al. 2013). The LCA method consists of four
parts including goal definition (the aim and scope), life cycle
inventory (pollutant emissions lists and used resources per
functional unit), life cycle impact assessment (classification
of pollutants and pertinent environmental impacts), and life
cycle analysis (interpretation of the consequences and esti-
mate the uncertainties). The most common output from LCA
analysis includes the estimation of greenhouse gases, acidifi-
cation, summer smog, ozone layer depletion, eutrophication,
ecotoxic and anthropotoxic pollutants (Xu et al. 2008). To
provide a more sustainable practice, LCA should be posi-
tioned on the overlap between the economic and environ-
mental lobes (Fig. 1) (Clark and Macquarrie 2008).
There are some review studies in the field of natural fiber
treatments, but this study attempts to make a link between
the consumed amount of energy and produced effluents of
the treatments and mechanical performance improvement of
the composite used treated fibers. The aim was to identify
the sustainability of each treatment type while considering
the results of the treatment in the final product. This review
study was initially started at the University of Quebec in
Abitibi-Temicamingue in 2013 but accomplished at Tarbiat
Modares University in 2017.
Fig. 1  Positioning LCA within the context of sustainable develop-
ment, SA sustainable activity
International Journal of Environmental Science and Technology
Different treatment types
Corona treatment
As a physical treatment, corona method increases the sur-
face energy and oxidizes the surface of natural fibers and
hence improves the compatibility between the hydrophilic
fibers and hydrophobic matrix (Sreekala et al. 2000). An
identical corona apparatus made of two electrodes (usu-
ally made of aluminum) and a dielectric spacer (usually
made of quartz). Through the continuous corona treatment,
an electrical power applies to the surface of the material,
through an air gap, via two electrodes (Pickering 2008).
All the fibers must emplace on electrode’s surface; there-
fore, one side of the fibers mainly exposed to the treatment
and the other side may not influence properly; in compos-
ite materials, however, the entire lateral surface of the fiber
involves in reinforcement (Gassan and Gutowski 2000;
Ragoubi et al. 2010). Figure 2 displays the etching effect
of the corona-treated hemp fiber using scanning electron
microscopy (SEM) micrographs. As displayed in Fig. 2,
while the time of treatment was increased, a coarser fiber
surface was obtained that may improve the interlocking
phenomenon (mechanical bonding) between the fiber and
matrix (Ragoubi et al. 2010).
It is reported that the corona treatment activates the
natural surface sites all along the polymeric chains, which
could react with oxygen to give etching effect. Thus, up to
30% improvement in Young modulus and tensile strength
of hemp and Miscanthus polypropylene composites were
achieved. However, when the source of matrix changed
from polypropylene to polylactic acid, the effectiveness
corona treatment decreased to 20% (Ragoubi et al. 2010,
2012). Based on the literature, it can be concluded that the
corona treatment changed the surface configuration of the
Fig. 2  Corona-treated hemp fiber a untreated, a after 15 min, c after 30 min, d after 40 min
natural fibers, but it is not clear if the fiber was damaged
or not. Interlocking is a weak mechanical bonding, and
the long-term influence of such bonding should be inves-
tigated. In addition, the corona treatment may increase the
surface energy of the fiber thus the surface energy of the
fiber and matrix may become less compatible.
Plasma treatment
This type of physical treatment uses the properties of plasma
to change the surface specification of the fibers by remov-
ing the weakly attached surface layers and/or forming new
functional groups. Plasma treatment can be performed on
both natural fiber and polymeric matrix, while no changes
will occur on the bulk properties of the treated materials
(Pickering 2008). Plasma treatment should be performed in
a molecular gas or a gas mixture that contains molecules
in a vacuum chamber while depending on the type of used
gas, an ionized region that includes high-energy photons,
electrons, ions, and radicals will be formed on the surface
of plasma-treated material (Shishoo 2007). Even though it is
possible to use different gases, oxygen plasma treatment has
been the most popular (Camargo et al. 2018). When argon
replaced with oxygen, the tensile strength of the compos-
ite was decreased (Yuan et al. 2004). When the influence
of plasma treatment was investigated on both sisal fibers
and high-density polyethylene (HDPE) matrix, the plasma-
treated matrix was more efficient to improve the ultimate
mechanical properties of the composite (Martin et al. 2000).
The effect of helium cold plasma treatment on flax fiber and
unsaturated polyester resin matrix was also contradictory,
while some improvement and deterioration were achieved
simultaneously (Marais et al. 2005). When plasma treatment
was applied at the 60 W power and for 15 min, the shear
strength and flexural strength of composite were improved
(Seki et al. 2009). The effectiveness of plasma treatment was
13

also dependent on the length of fibers, while 6 mm treated
sisal fiber provided the best mechanical properties improve-
ment (Xiaowen et al. 2004).
Silane treatment
Silane is an inorganic compound with the general chemical
formula of ­SiH4 that consist of hydrophilic–hydrophobic
compounds joined to the silicon molecule and may undergo
coagulation by introduction of a coagulant agent to form
silanol (SiOH) groups initially and then siloxane bridges
(Choy et al. 2015; Koohestani et al. 2018a; Xie et al. 2010).
It undergoes several stages of hydrolysis, condensation, and
bond formation during the treatment process. During the
treatment, one end of the silanol reacts with the hydroxyl
group of the fiber, while the organic part of the organosilane
may also react with the polymeric matrix (Kabir et al. 2012).
The vinyl silane–natural fiber chemical interaction is shown
in Eqs. 1 and 2 (Li et al. 2007). Alkaline pre-treatment is
also recommended before silane treatment (natural fibers
immersion in NaOH solution for 10 or 30 min), but the fibers
need to excessively be washed to become neutral (Keijzer
et al. 2013; Lu et al. 2014).
( ) H2 O
CH2 CHSi OC2 H5 3 �������→
� CH2 CHSi(OH)3 + 3C2 H5 OH
(1)
CH2 CHSi(OH)3 + Fiber−OH → CH2 CHSi (OH)2 O − Fiber + H2 O
(2)
To estimate the efficiency of silane-treated natural fibers
in composites, herein some literature reviews are studied and
compared. The treatment of henequen fiber with methacry-
loxy silane (A-174 from Sigma-Aldrich) at 70 °C resulted in
mechanical strength improvement (Valadez-Gonzalez et al.
Table 3  Influence of silane-treated natural fibers on mechanical properties of composites
Silane treatment
Agent(s) used Amount
Amino silane (Huda et al. 2008) 5%
Glycidoxypropyl silane (Nishino et al. 2006) 4%
NaOH + amino silane (Huda et al. 2008) 5% + 5%
NaOH + methoxy-ethoxy silane (Valadez- 2% + 1%
Gonzalez et al. 1999b)
NaOH + xylene + vinyl silane (Herrera-Franco 2% + 1.5% + 0.015%
and Valadez-Gonzalez 2004)
NaOH + methoxy-ethoxy silane + dicumyl 2% + 1% + 0.5%
peroxide (Valadez-Gonzalez et al. 1999a)
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International Journal of Environmental Science and Technology
1999a). When bamboo fibers were treated with organosul-
fur silane (Si-69 from HB Chemicals), 70% improvement in
tensile strength plus a decrease in the curing time of poly-
meric composites was observed. In addition, 13% improve-
ment in flexural strength of henequen-HDPE composite was
achieved while there was no change in flexural modulus
(John and Anandjiwala 2008). The treatment of 5% silane
on pineapple leaf fibers also improved the impact strength of
the fiber and matrix up to 47% with the polylactic acid-based
matrix. The best impact strength improvement (86%) and
the best flexural strength improvement (45%) were achieved
when silane treatment was combined with alkali treatment
(Huda et al. 2008). Table 3 summarizes the collected data
from some silane treatment experiments performed in dif-
ferent studies.
As demonstrated in Table 3, silane-treated natural fib-
ers improved the mechanical properties of the composites
in most cases especially when combined with alkaline pre-
treatment. Based on the reviewed studies, the amount of used
silane agent varied between 1 and 5% while the hydrolysis
time, silane chemistry, temperature, and pH were the main
factors that affected the effectiveness of the silane treatment.
Alkaline treatment
Alkaline treatment or mercerization is one of the most used
chemical treatments in different applications (Adams et al.
2016). The mercerization is a process that fibers interact
with a concentrated aqueous solution of a strong base to
swell with resultant changes in the structure, dimension,
morphology, and consequently mechanical performance
(ASTM-D 1965). This type of treatment removes a certain
amount of lignin, wax, and oils while depolymerizes the
fiber cell wall (Kabir et al. 2012). In addition, the treatment
Fiber/matrix (%) Changes in mechanical properties
Pineapple/polylactic acid ↑ 47% Impact strength
40/60 ↑ 27% Tensile modulus
Kenaf/polylactic acid ↑ 20% Tensile strength parallel to fiber axis
60/40 ↑ 20% Tensile strength perpendicular to fiber
axis
Pineapple/polylactic acid ↑ 86% Impact strength
40/60 ↑ 45% Tensile modulus
Henequen-HDPE ↑ 23% Tensile strength
20/80
Henequen-HDPE ↑ 10% Longitudinal tensile strength
46/54 ↑ 43% Transverse tensile strength
No changes in Longitudinal modulus
Decreases in Transverse modulus
Henequen-HDPE ↑ 23% Tensile strength
20/80
International Journal of Environmental Science and Technology

of natural fibers with aqueous sodium hydroxide (NaOH)
may promote the ionization of the hydroxyl groups to alkox-
ides. Since the alkaline treatment removes hemicellulose,
lignin, and pectin as the main compositions of natural fib-
ers, a decrease in tensile strength of fiber itself may occur
(Anand and Anbumalar 2017; Gurunathan et al. 2015). This
condition is identical for the natural fibers in cementitious
materials since the generated calcium hydroxide (portlan-
dite) during the cement hydration is an alkaline material.
Equation  3 represents the reaction of natural fiber with
sodium hydroxide alkaline agent (Williams et al. 2011).
Fiber−OH + NaOH → Fiber−O−Na + H2 O (3)
Some experiments in the field of alkaline treatment
reviewed and compared herein to evaluate the effectiveness
of this treatment type. It is reported that the alkaline treat-
ment increased the surface tension of sisal fibers and hence
improved its adhesion to the epoxy resin while improved
the compressive strength and decreased the water uptake
of the composite (Bisanda 2000). When coconut fiber was
treated with different chemicals including hydrogen per-
oxide ­(H2O2), NaOCl (sodium hypochlorite), and NaOCl/
NaOH, peroxide was more effective to change the fiber
morphology, thermal stability, and wax/fatty acid resi-
due removal (Brígida et al. 2010). The alkali-treated jute
fibers improved the tensile and flexural strength of the
jute–epoxy composite, but the impact behavior was not
affected and the fatigue behavior was negatively influenced
(Gassan and Bledzki 1999). It is also noticeable that the
mechanical properties of transverse, longitudinal, and
radial sections of alkaline-treated fibers were not similar
(Van de Weyenberg et al. 2006; Vuure 2008); for example,
the axial modulus of jute fibers was 38.4 GPa, whereas the
transverse modulus was only 5.5 GPa (Cichocki Jr and
Thomason 2002). Some literature reviews in the field of
alkaline treatment are summarized in Table 4.
Based on Table  4, alkaline treatment improved the
mechanical properties in most cases, but some contro-
versy results are also achieved especially when a pre-load
was combined with alkaline treatment that can be attrib-
uted to the removal of natural fibers main compositions.
NaOH was the main alkali agent for the alkaline treatment,
whereas LiOH and KOH could also be used and compared
specifically since lithium interacts more efficiently with
hydroxyl groups of cellulose (Xu et al. 2010).

Table 4  Influence of alkaline treatment on mechanical properties of composites

Alkaline treatment
Agent(s) used Amount and time Fiber/matrix (%) Changes in mechanical properties

NaOH (Huda et al. 2008) 5%, 2 h Pineapple leaf/polylactic acid ↑ 79% Impact strength
40/60 ↑ 36% Tensile modulus
NaOH + load (Goda et al. 2006) 15% + 0.049–0.098 N, 2 h Ramie fibers ↑ 4–18% Tensile strength
↓ 30–75% Tensile modulus
NaOH (Bachtiar et al. 2008) 0.25 M, 1 h Sugar palm/epoxy ↑ 16.4% Tensile strength
25/75 ↑ 14% Tensile modulus
NaOH (Joseph et al. 1996) 5%, 72 h Sisal/LDPE ↑ 22% tensile strength
30/70 ↑ 31.5% Tensile modulus
NaOH (Gassan and Bledzki 1999) 25%, 20 min Jute/epoxy ↑ 120% Tensile strength
40/60 (volumetric) ↑ 150% Tensile modulus
NaOH (Rout et al. 2001) 2%, 1 h at 300 °C Coir/polyester ↑ 26% Tensile strength
17/83 ↑ 15% Flexural strength
NaOH (Ray et al. 2001) 5%, 8 h Jute fiber (no matrix) ↑ 79% Tensile modulus
Jute/vinylester ↑ 20% Flexural strength
35/65 ↑ 23% Flexural modulus
NaOH (Nam et al. 2011) 5%, 72 h Coir/poly butylene succinate ↑ 54.5% Tensile strength
25/75 ↑ 142% Tensile modulus
↑ 45.7% Flexural strength
↑ 97.4% Flexural modulus
NaOH (Valadez-Gonzalez et al. 1999b) 2%, 1 h Henequen-HDPE ↑ 4% Tensile strength
↑ 30% Interfacial shear strength
NaOH + tension (Kim and Netravali 2010) 2% + 0.005 N, 2 h Sisal fiber ↑ 21.5% Tensile strength
↑ 39% Tensile modulus
Sisal/soy protein resin ↑ 12.2% Tensile strength
↑ 36.2% Tensile modulus

13

Acetylation treatment
The acetylation treatment is based on the replacement of
hydroxyl groups of fiber with the acetyl group ­(CH3CO) that
consequently removes the moisture and provides hydropho-
bicity (Kabir et al. 2013). In addition, acetylation treatment
increases the roughness of the fiber surface and thus pro-
vides better mechanical interlocking with the matrix (Pick-
ering et al. 2016). Neither acetic acid nor acetic anhydride
is sufficiently reactive with natural fibers; hence, a soaking
pre-treatment with acetic acid followed by acetic anhydride
treatment is recommended (Ali et al. 2018). After treatment,
the fibers should be washed periodically with distilled water
to become free of acid followed by air-drying. The chemical
reaction of acetic anhydride with natural fibers is mentioned
Eq. 4 (Chand and Fahim 2008; Kabir et al. 2012; Li et al.
2007).
Fiber−OH + CH3 −C(=O)−O−C(= O)−CH3
(4)
→ Fiber−OCOCH3 + CH3 COOH
Acetylation of flax fibers with 0.052% of catalyst (based
on the mass of fibers) caused 45% degree of acetylation
after 3 h. When the amount of catalyst increased more than
0.052%, the treatment became deleterious and damaged the
fibers. A higher degree of acetylation decreased the mois-
ture absorption in flax fibers, but 18% degree of acetyla-
tion provided the highest tensile and flexural properties to
flax fibers (Bledzki et al. 2008). The acetylation treatment
removed the non-crystalline constituents of the fibers and
hence improved the surface topography and consequently
the stress transfer at the interface (Zafeiropoulos et al. 2002a,
b). The acetylation treatment of banana fibers increased the
tensile strength of the composite, but not the tensile strength
Table 5  Influence of acetylation treatment on mechanical properties of composites
Acetylation treatment
Agent(s) used Amount(s)
Acetic anhydride (Bledzki et al. 2008) 18%
NaOH pre-treated + acetic acid (Joseph 4% for 2 h + 50% for 5 min
et al. 2006)
NaOH pre-treated + acetic acid (Joseph 4% for 2 h + 50% for 5 min
et al. 2005)
NaOH pre-treated + acid acetic (Luz et al. 1.5% for 1 h + (465 g for 90 g
2008) fiber, additional 165 g acid
acetic)
13
International Journal of Environmental Science and Technology
of the fiber itself (Joseph et al. 2005, 2006). In addition, the
acetylation treatment increased the mass of the natural fibers
(up to 16.3%) and changed the bulk properties of the fibers
(Zafeiropoulos et al. 2002b). Table 5 presents the results of
different studies in the field of acetylation treatment.
Maleated coupling treatment
In the field of maleated treatment, a series of standard func-
tional polymers are available in the market (e.g., Dupont Fus-
abond and Epolene trade names) that can be freely blended
with raw materials (fibers and polymers) and extruded dur-
ing the composite manufacturing process. Thus, there is no
need for a dedicated operation when this treatment type was
performed. Such functional polymers are produced by the
modification of base polymers (e.g., polyethylene) using
maleic anhydride grafting (Bhattacharya and Misra 2004).
This treatment type modifies both the fiber surface and poly-
meric matrix thus improving the interfacial bonding between
the fiber and matrix (Faruk et al. 2012). Maleic anhydride
removes the hydroxyl groups of the cellulose to make it com-
patible with polymeric matrix while simultaneously forms
carbon–carbon covalent bond between the treated fiber and
polymer. This covalent bonding between hydroxyl groups of
the fiber and anhydride groups of the maleic makes a bridge
interface for the efficient interlocking (Zhou et al. 2016).
For instance, polypropylene (PP) chain allows maleic anhy-
dride to be cohesive by producing maleic anhydride grafted
polypropylene (MAPP). Then the treatment of cellulose fib-
ers with the hot MAPP copolymers provides covalent bonds
across the interface. The reaction mechanism of MAPP and
fiber can be explained by activation of the copolymer at
170 °C and esterification of cellulose fiber. Thus, the surface
energy of natural fiber and polymeric matrix becomes more
Fiber/matrix Changes in mechanical properties
Flax/polypropylene ↑ 35% Tensile strength
5% fiber ↑ 20% Tensile modulus
Banana/phenol formaldehyde ↑ 56% Tensile strength in outdoor
weathering
↑ 75% Tensile strength in soil
burial
Banana fiber ↓ 27% Tensile strength
↓ 80% Tensile modulus
Banana/phenol formaldehyde ↑ 36% Tensile strength
↑ 800% Tensile modulus
Cellulose/PP ↓ 1% Tensile strength
10% fiber ↓ 1.25% Flexural strength
Cellulignin/PP ↓ 1% Tensile strength
10% fiber ↓ 1.14% Flexural strength
International Journal of Environmental Science and Technology
similar, while the wettability and interfacial adhesion are
also improved (Santos et al. 2008). The effectiveness of this
treatment type on the total performance of polymer-based
composites filled with natural fibers is discussed in the liter-
ature; for instance, when jute fibers were immersed in 0.5%
MAPP solution in toluene at 100 °C for 5 min, 72.3, 30, and
24.2% increase in flexural, tensile, and impact strength were
achieved respectively plus 61% decrease in water uptake in
jute fiber polypropylene-based composites (Zafeiropoulos
2011). However, an increase in the MAPP concentration
from 0.5 to 1% influenced the mechanical properties nega-
tively (Mohanty et al. 2004). Between different amounts of
maleated coupling agents on jute and flax fibers, 3% was
the optimum amount (Keener et al. 2004). Table 6 presents
and compares the achieved results of different studies used
maleated treatment in natural fiber/polymer composites.
Enzyme treatment
Using enzymes to treat natural fibers are well established due
to the simplicity of the method (Faruk et al. 2012). Enzymes
are biological catalysts with a remarkable diversities, reac-
tions, and structures that accelerate the chemical reaction
while themselves do not undergo any permanent chemi-
cal change. The main role of the enzymes in the treatment
process is to degum the natural fibers while improving the
cleanliness, homogeneity, fineness, and softness (Koncze-
wicz and Kozłowski 2012). All known enzymes are proteins
composed of one or more polypeptide chains (Cavaco-Paulo
and Gübitz 2003). The enzyme treatment is more rapid but
delicate over the chemical treatment since should be per-
formed at the atmospheric pressure below 100 °C with a
pH of 4–8, while the addition of chelators such as ethylen-
ediaminetetraacetic acid (EDTA) to enzyme mixtures can
increase the efficiency of this treatment type (Konczewicz
Table 6  Influence of maleated treatment on mechanical properties of composites
Maleated coupling agent
Agent(s) used Amount(s) (%)
Maleated anhydride polypropylene 2 Aspen/polypropylene
(MAPP) (Xue et al. 2007)
MAPP (Mutje et al. 2006) 4 Hemp/PP
Maleated Anhydride Polyethylene 1.7
(MAPE) (Han et al. 2008)
3.5
MAPE (226D) (Lu et al. 2005) 3 Thermomechanical pulp/HDPE
and Kozłowski 2012). However, the high cost associated
with the enzymes and the appropriate choice of enzymatic
agents restrict the use of this method (Dam 1999; Koncze-
wicz and Kozłowski 2012). When enzyme treatment was
performed on abaca fibers using fungamix, 45% increase in
tensile strength of abaca polypropylene was achieved. While
at the same condition MAPP increased the tensile strength
up to 40% (Bledzki et al. 2010). When enzyme treatment
was combined with a pre-treatment using ethylene diamine
tetramethylene phosphoric acid (EDTMPA), higher amounts
of wax, pectin, lignin, and other non-cellulosic compounds
were removed from hemp fiber (George et al. 2014; Han
et al. 2008), whereas the total porosity of the hemp fibers
increased up to 270% after 4 h resulting in fibers mechanical
strength deterioration (Buschle-Diller et al. 1999).
Natural fiber treatments in cementitious materials
To overcome the unwanted problems of natural fibers in
cementitious materials, different methods and materials
are examined. For example, using water-repellent agents
or fiber impregnation with sodium silicate and sodium
sulfide decreased the potential water absorption of the fib-
ers (Ghavami 1995). The silane treatment on natural fibers
especially when combined with pyrolysis pre-treatment also
improved the durability and adhesion of bagasse fibers by
changing the dimension of fibers, reducing the setting time,
and increasing the curing temperature. The pyrolysis pre-
treatment at 200 °C (for 2 h) increased the density (bulk and
apparent) of fibers up to 10% and increased the porosity bulk
density of the fibers up to 7 and 45%, respectively, while
decreased the apparent density and water uptake up to 18
and 23%, respectively (Bilba and Arsene 2008). The positive
influence of pyrolysis and silane treatment on hardwood and
softwood fibers when used in cementitious materials were
Fiber/matrix (%) Changes in mechanical properties
↑ 32% Tensile strength
30/68 (25 °C) ↑ 19% Flexural strength
Aspen/polypropylene ↑ 41% Tensile strength
50/48 (25 °C) ↑ 33% Flexural strength
↑ 36% Tensile strength
30/66 ↑ 58% Tensile modulus
↑ 44% Flexural strength
Bamboo/HDPE ↑ 30% Tensile strength
29.5/68.8 ↑ 5% Tensile modulus
Bamboo/HDPE ↑ 44% Tensile strength
29/67.5 ↓ 18% Tensile modulus
↑ 58% Tensile strength
47/50 ↑ 11% Tensile modulus
13

also approved elsewhere (Arsène et al. 2007; Blankenhorn
et al. 2001; Pehanich et al. 2004). The natural fiber immer-
sion in slurry silica is another solution that can improve the
compatibility of fibers within the cementitious materials
(Motta et al. 2010; Toledo Filho et al. 2003).
Evaluation of different treatments
System description, goal, and scope
The best way to compare different natural fiber treatments is
to use life cycle assessment from cradle to grave. However,
due to the lack of sufficient data from different industrial
sectors, it is not possible to perform a comprehensive LCA
analysis in this literature study. Instead, we simply consid-
ered the generated effluents and consumed energy (embod-
ied energy) between the selected treatments limited to the
treatment section within the WPC manufacturing (from gate
to gate, Fig. 3). In addition, based on the literature review,
we considered the overall mechanical performance improve-
ment of the composites used treated natural fibers as a cri-
terion to emphasize the importance of the treatment type.
However, in a comprehensive LCA analysis of natural fibers
treatment, the embodied energy for transportation, prepara-
tion, and disposal of raw materials, treatment agents, the
final product, and effluents/by-products should be consid-
ered simultaneously while linking with the potential fossil
resource depletion and global warming.
Variables in energy consumption of the treatments
Since the comparison between different treatments is limited
within the scope of treatment section in WPC manufactur-
ing (Fig. 3), the major energy consumption and effluents of
each treatment type are considered and compared. Herein,
between different chemical treatments discussed, silane,
alkaline, and acetylation contain wet chemical treatment
process in contrast to the maleated treatment. Due to the
available maleated standard products in the market, there
is no need for an extra process to modify the natural fib-
ers in this treatment type; thus, no effluents and specific
energy will be produced and required during the maleated
Fig. 3  Schematic treatment
process of natural fibers/fillers
13
International Journal of Environmental Science and Technology
treatment (Koohestani et al. 2017b, 2018c). However, wet
chemical treatment contains several steps mainly fibers
dipping/impregnation in an aqueous solution followed by
drying and curing to finalize the treatment; thus, significant
effluents and energy might be generated and consumed. It
is also noticeable that the natural fibers drying procedure
apart from being a major source of energy consumption may
also emit the toxic gas to the atmosphere. Prior to the final
treatment, a pre-treatment may also be applied (e.g., drying
or immersing in the chemicals) that increases the ultimate
energy consumption and effluents/by-products generation.
Total energy consumption of different treatments
To evaluate the total consumed amount of energy per unit
of treated natural fiber, the source of fiber and energy were
constant (wood fiber and electricity). It was assumed that 1-h
drying process using the oven at 120 °C consumed 1.1 kW
and 1-h lab mixing using normal mixer used 216 W energy.
Between the investigated chemical treatments, performing a
pre-treatment is more routine in silane and acetylation treat-
ments; in all the investigated treatments the concentration
of the chemical agent is approximately changed from 1 to
5%. The time of treatment in acetylation and alkaline treat-
ments is approximately 2 h, whereas in silane treatment it
is extended to 12 h due to the gradual reactivity of silane
molecule (needs to be hydrolyzed and condensed). Since
maleated treatment accomplishes during the composite man-
ufacturing process, there is no specific time and effluent for
which are allocated. Figure 4 displays the amount of used
energy for different chemical treatments.
As can be seen from Fig. 4, the amount of energy con-
sumed is allocated into the treatment process (mixing, dry-
ing, and washing) and effluents (pre-defined for manage-
ment). As the amount of effluents is increased, the pertinent
energy consumption was also elevated. The alkaline (NaOH,
2 h mixing, washing, 6 h of drying at 120 °C) and acetyla-
tion (1-h NaOH pre-treatment at 30 °C followed by soaking
in acetic acid for 1 h at 30 °C finalized with 5-min soaking
in acetic anhydride, washing and drying at each section)
treatments used approximately 10 and 17.5 kW, respectively
(Fig. 4). Silane treatment divided into two types including
with and without pre-treatment. The amount of used energy
International Journal of Environmental Science and Technology
Fig. 4  Energy consumption for
different chemical treatments
per unit of natural fiber
is higher in silane treatment (12 h mixing at 60 °C using
hexane solvent deposition method followed by washing and
drying) due to the procedure longevity and extended by the
addition of a pre-treatment. When comparing pre-treated
acetylation and silane (1-h pre-treatment with NaOH, 12 h
of mixing at 60 °C using hexane solvent deposition method,
washing and drying at each section) treatments, the efflu-
ents energy requirement is higher in acetylation due to the
additional pre-treatment operation while the process energy
for the silane treatment is higher because of the elevated
procedure time duration (12 h). Even though the physical
(plasma and corona) and biological (enzyme) treatments
contain no effluents, we did not consider them due to the
lack of information regarding the energy consumption used
in these methods.
Discussion and conclusion
In the scope of this study, it was shown that maleated
treatment has no effluents output or does not need a spe-
cific energy to treat natural fibers in a dedicated section;
thus, it can carefully be said that the maleated is the most
sustainable treatment between the studied treatments, but
more investigation in this regard is necessary. Maleated,
acetylation, alkaline, and silane treatments displayed a
32–58, 27–56, 4–54.5, and 20–45% improvement in tensile
strength of polymer-based composites containing treated
natural fibers. A pre-treatment addition to the final treat-
ment can drastically increase the energy consumption and
effluent generation in the scope of fiber treatment. In this
case, the mechanical property improvement of the final
composite should be considered and compared between
different treatment types to select a more suitable method
with lesser energy consumption and effluents generation.
However, financial concerns including the costs of chemical
agents should also be considered even though it was out of
the scope of this study. If the mechanical properties of the
composites containing treated natural fibers are improved,
it may be possible to reduce the amount of fibers, but due to
the high availability and low price of natural fibers over the
synthetic fibers, it is not recommended. Instead, the focus
should be on the use of various treated fillers (e.g., mineral
fillers) interchangeably or complementary with other treated
or non-treated fibers/fillers to have the most of treatment
influence on the total performance of composite materials.
Acknowledgements  The authors of this work want to appreciate the
UQAT professional and technical staffs for their helpful support and
assistance. This study was accomplished by Elite Iranian Organization
Research Grant (No. 316/5603).
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