materials

Article
Production of Banana Fiber Yarns for Technical
Textile Reinforced Composites
Zaida Ortega 1, *, Moisés Morón 2 , Mario D. Monzón 3 , Pere Badalló 2 and Rubén Paz 3
1 Departamento de Ingeniería de Procesos, Universidad de Las Palmas de Gran Canaria,
Las Palmas de Gran Canaria 35017, Spain
2 Acondicionamiento Tarrasense Asociación—LEITAT, Terrassa 08225, Spain; mmoron@leitat.org (M.M.);
pbadallo@leitat.org (P.B.)
3 Departamento de Ingeniería Mecánica, Universidad de Las Palmas de Gran Canaria,
Las Palmas de Gran Canaria 35017, Spain; mario.monzon@ulpgc.es (M.D.M.); ruben.paz@ulpgc.es (R.P.)
* Correspondence: zaida.ortega@ulpgc.es; Tel.: +34-928-459641

Academic Editor: Kim Pickring

Received: 11 April 2016; Accepted: 9 May 2016; Published: 13 May 2016

Abstract: Natural fibers have been used as an alternative to synthetic ones for their greener character;
banana fibers have the advantage of coming from an agricultural residue. Fibers have been extracted
by mechanical means from banana tree pseudostems, as a strategy to valorize banana crops residues.
To increase the mechanical properties of the composite, technical textiles can be used as reinforcement,
instead of short fibers. To do so, fibers must be spun and woven. The aim of this paper is to
show the viability of using banana fibers to obtain a yarn suitable to be woven, after an enzymatic
treatment, which is more environmentally friendly. Extracted long fibers are cut to 50 mm length
and then immersed into an enzymatic bath for their refining. Conditions of enzymatic treatment
have been optimized to produce a textile grade of banana fibers, which have then been characterized.
The optimum treating conditions were found with the use of Biopectinase K (100% related to fiber
weight) at 45 ˝ C, pH 4.5 for 6 h, with bath renewal after three hours. The first spinning trials show
that these fibers are suitable to be used for the production of yarns. The next step is the weaving
process to obtain a technical fabric for composites production.

Keywords: banana fibers; enzymatic treatment; yarn; composites; reinforcement; sustainability

1. Introduction
The rising interest in natural fibers in the composites field is undeniable, mainly due to
sustainability, but also because of their good mechanical properties and low cost. The differences
observed among different natural fibers are due to their chemical composition, origin, climate
conditions, etc. On average, vegetable fibers are made of 60%–70% of cellulose, 10%–20% of
hemicellulose, 5%–15% of lignin and up to 2% of pectin and waxes [1].
Banana fiber is obtained from the superimposed leaves forming the pseudostem of the plant,
which currently has no use, apart from a low percentage dedicated to cattle feed. It belongs to Musa
genre, as a monocot. Banana is the most important crop in Canary Islands, which are the most
important producers of bananas in Europe. It is important to highlight that fibers are obtained from
the pseudostems of the plant once the fruit has been harvested, and that each plant only bears fruit
once; this is one of the main benefits of banana fibers in comparison with other natural fibers, as this
one is obtained from an agricultural residue.
The use of natural fibers as reinforcement of polymeric parts has been widely studied, specially
focusing on injection molding technology. In fact, around 21,000 tons of natural fibers were used
in 2003 in the European industry; the most relevant fibers for the industrial production of plastic

Materials 2016, 9, 370; doi:10.3390/ma9050370 www.mdpi.com/journal/materials

Materials 2016, 9, 370 2 of 16

composites are flax, sisal and hemp. Natural fibers are less harmful to humans, machinery and the
environment, thus being realistic alternatives to glass fiber [2].
Some studies have also been carried out for the compression molding technology, some with
long fibers [3,4] and others with woven fibers [5–7], both for thermoset and thermoplastic polymers.
These studies show that specific mechanical properties of natural fibers composites are similar to
those reinforced with glass fiber, although mechanical properties under humid conditions show an
important decrease for the natural fiber composites, due to their moisture absorption. These studies
mainly focus on the production of non-structural parts for the automotive sector [7].
It is known that mechanical properties of composites strongly depend on the orientation of the
fibers, getting better properties when the fiber is woven and placed in the composite in an appropriate
orientation. The BANTEX project (MAT2013-47393-C2-1-R) is aimed at obtaining a composite material
made of woven banana fibers. Woven fabrics have the advantage of enabling the orientation of
the fibers, allowing control of the density of the fabric and its mechanical properties. Nonwovens
provide multiaxial orientation but lower and non-predictable mechanical properties. There is wide
bibliography about the production of composite materials with natural fibers (flax, hemp, jute) in
woven and non-woven fabrics [8–11]; however, no references have been found in the use of banana
fibers to produce them. Furthermore, the use of banana fibers to produce yarns for technical textile
products has not been reported.
Banana fibers are made of cellulose (43.6%), hemicellulose (14%), lignin (11%) and other substances
(such as pectin, wax, 31.4%) [12]. Chemical methods for fiber extraction are usually performed with
NaOH, although other chemicals are also used (KMnO4 , benzoyl chloride, stearic acid, among others);
these processes may cause environmental problems due to the need for treating the residues produced.
Mechanical means are not able to remove the non-cellulosic constituents (lignin). An alternative is
the use of biological processes, such as the immersed [13] or solid state [14] fermentations. Enzymatic
means are considered more environmentally friendly, and also avoid the fibers breakage, while altering
the properties of the cellulosic fibers [15]. There are different parameters which affect the enzyme
choice, such as the type of substrate, composition, size, lignin content, etc. [15]. Previous studies show
Pectinase [16] and Xylanase [17] as the most suitable ones for fiber extraction. Enzymatic treatments
have been applied to hemp, flax or pineapple for fiber refining. Celullases are used to remove fibrils
from the surface and increase the smoothness of the fiber, although this treatment can also damage the
fibers and reduce their mechanical properties. Pectinases are used in the textile industry for retting
and degumming fiber crops, as they are capable of breaking down complex molecules of plant tissues
into simpler ones, such as galacturonic acid [18]; on the other hand, endoglucanases only act on
amorphous celluloses.
Hemicellulases are able to reduce water absorption by pentosan hydrolysis; xylanase and
mannanase are used to dissolve hemicellulose (mainly xylan and glucomannan, respectively) [19].
Tests have been performed using a cocktail of two different enzymes made of pectinase and
hemicellulase. In this research, different formulations of the enzymatic treatment have been applied to
the banana fibers in order to determine the optimal conditions (time, temperature, enzymes content,
bath renewal, fiber/enzymes ratio, etc.) for the refining process, in order to obtain a banana textile
grade fiber. Fibers have been characterized prior to and after the enzymatic treatment, in terms of
length, diameter and thermal stability. The spinning process at the lab scale has taken place, resulting
in the production of a yarn with enough quality to be woven and produce a technical textile suitable
for composite reinforcement.

2. Results

2.1. Fiber Treatments

A design of experiments (DoE) was made for the enzymatic treatment of the fibers, taking into
account the composition and characteristics of banana fibers. Two enzymatic formulations were
Materials 2016, 9, 370 3 of 16

Materials 2016, 9, 370 3 of 16

applied to the fibers: Biopectinase M01 (made of pectinase and hemicellulase) and Biopectinase K
related of
(made to poligalacturonase).
fiber weight (r.f.w.).The chosen
Fiber factors
to bath are treatment
volume ratio was time set toand1:40concentration
for scalabilityofpurposes,
enzymes
related
while to fiber weight
temperature (r.f.w.).
and pH were Fiber to bath volume
fixed according ratio was
to datasheets for set
the to 1:40 for
selected scalability
enzymes: pH purposes,
= 4.5 and
while temperature and pH were fixed according to datasheets for the selected
T = 45 °C. The design of experiments was done using Design Expert 9.0 (Stat-Ease, Inc., Minneapolis,
® enzymes: pH = 4.5 and
T = 45 ˝ C. The design of experiments was done using Design Expert 9.0® (Stat-Ease, Inc., Minneapolis,
MN, USA), varying the treatment time from 1 to 8 h and the enzyme concentration from 1% to
MN,
5% USA), varying the treatment time from 1 to 8 h and the enzyme concentration from 1% to 5% r.f.w.
r.f.w.
The
The DoEDoE was
was applied
applied using
using each
each enzyme
enzyme formulation
formulation withwith varying
varyingthe the treatment
treatment time
time and
and the
the
concentration of
concentration of enzymes
enzymes (r.f.w.),
(r.f.w.), at
at the
the same
same pH
pH and
andtemperature.
temperature. As AsBiopectinase
BiopectinaseM01M01isisless
lessactive,
active,
the amount of enzymes used is 44% higher than for
the amount of enzymes used is 44% higher than for Biopectinase K.Biopectinase K.
The DoE
The DoE isis aaBox–Hunter
Box–HunterCentral
Centralcomposite,
composite,with
withrotation
rotation factor of 1,41.
factor The The
of 1,41. design is (X,Y)–(time,
design is (X,Y)–
concentration).
(time, Scheme
concentration). 1 shows
Scheme the DoE,
1 shows the while Table 1Table
DoE, while lists 1alllists
performed experiments.
all performed experiments.

Scheme
Scheme 1.
1. DoE
DoEfor
foreach
eachenzyme.
enzyme.

Table 1. Treatment conditions (for each enzyme) for the first DoE.
Table 1. Treatment conditions (for each enzyme) for the first DoE.
Test NumberTime (h) Enzyme Concentration (% r.f.w)
Test Number
1 Time (h)
6.98 Enzyme 4.410
Concentration (% r.f.w)
1 2 6.98
4.50 4.9964.410
2 3 4.50
8.01 2.9954.996
3 8.01 2.995
4
4 4.50
4.50
2.9952.995
5 5 4.50
4.50 0.9940.994
6 6 4.50
4.50 2.9952.995
7 7 2.02
2.02 4.4104.410
8 4.50 2.995
8 4.50 2.995
9 0.99 2.995
10 9 0.99
2.02 2.9951.580
1110 2.02
4.50 1.5802.995
1211 4.50
4.50 2.9952.995
1312 6.98
4.50 2.9951.580
13 6.98 1.580
Microscopic observations were carried out to determine the extent of the removal of undesired
Microscopic
compounds observations
(hemicellulose, were carried
pectin) from the out to determine
fibers and their the extent
surface of the removal
structure. of undesired
Biopectinase K tests
compounds (hemicellulose,
showed better pectin) not
results, even though fromenough
the fibers and their
cleanliness surface
was structure.
achieved (FigureBiopectinase
1). K tests
showed better results, even though not enough cleanliness was achieved (Figure 1).
Materials 2016, 9, 370 4 of 16
Materials 2016, 9, 370 4 of 16

(a) (b)
Figure 1. SEM pictures of banana fibers: (a) fibers treated with Biopectinase M01; (b) fibers treated
Figure 1. SEM pictures of banana fibers: (a) fibers treated with Biopectinase M01; (b) fibers treated
with Biopectinase K.
with Biopectinase K.

The following step was the preparation of a new DoE, consisting of 6 experiments performed
Thethe
varying following step was
time, enzyme the preparation
(Biopectinase of a new DoE,
K) concentration, consisting
contact of 6and
surface experiments performed
fiber to bath ratio, in
varying
order to the time, enzyme
determine (Biopectinase
the limit conditions K) concentration,
(summarized contact
in Table 2). surface and fiber
Temperature wastokept
bathatratio, in
45 °C,
order to determine the limit conditions (summarized in Table 2). Temperature was kept at 45 ˝ C, pH at
pH at 4.5 and stirring at 200 rpm.
4.5 and stirring at 200 rpm.
Table 2. Tests to determine limit conditions for Biopectinase K.
Table 2. Tests to determine limit conditions for Biopectinase K.
Enzyme Concentration
Test Number Time (h) Fiber/Bath Ratio Fiber Length (cm)
Test Number Time (h) (% r.f.w)
Enzyme Concentration (% r.f.w) Fiber/Bath Ratio Fiber Length (cm)
1 1 24 24 1010 1/40 1/40 Long Long1 1

2 2 24 24 10 10 1/40 1/40 5 5
3 24 20 1/40 5
3 24 20 1/40 5
4 48 20 1/40 5
5 4 48 48 2020 1/40 1/80 5 5
6 5 16848 2020 1/80 1/40 5 5
1 This6is a fiber with the
168length obtained from20 1/40extraction procedure; in5this case,
the plant after the mechanical
around 0.6 m.
1This is a fiber with the length obtained from the plant after the mechanical extraction procedure; in
this case, around 0.6 m.
Stability of the Biopectinase K enzyme in the operating conditions was used to determine the
maximum reaction
Stability of the time, determining
Biopectinase the optimum
K enzyme point forconditions
in the operating the bath renewal.
was used Enzymatic activity
to determine the
was determined
maximum reaction through the concentration
time, determining of galacturonic
the optimum point foracid
theinbaththe bath. TheEnzymatic
renewal. poligalacturonase
activity
activity
was was measured
determined throughin the
samples of 5 cm long
concentration banana fiberacid
of galacturonic treatedin theforbath.
24 h, The
withpoligalacturonase
a Biopectinase K
concentration of 50%, at the conditions indicated above. Enzyme activity was
activity was measured in samples of 5 cm long banana fiber treated for 24 h, with a Biopectinase measured each 30 min,K
for the first 4 h,ofevery
concentration 50%, hour
at thefor the following
conditions 4 h and
indicated finally
above. at theactivity
Enzyme end of thewastest (24 h). each 30 min,
measured
Taking
for the first 4into account
h, every hour results obtained
for the followingfrom4 hthe activity
and finallytest,
at thea final
end DoE
of thewas
testperformed,
(24 h). adapting
the treatment
Taking into time and enzyme
account concentration.
results obtained from the Treatment wasaperformed
activity test, final DoE was using Biopectinase
performed, K at
adapting
45 ˝treatment
the C and pH time 4.5, varying the treatment
and enzyme time from
concentration. 3 to 9 h and
Treatment was the enzyme using
performed concentration, related
Biopectinase K to
at
fiber weight, from 25% to 100%. From previous experiments, it was determined
45 °C and pH 4.5, varying the treatment time from 3 to 9 h and the enzyme concentration, related to that an enzymatic
bath should
fiber weight,be renewed
from 25% to every
100%.3 h.From previous experiments, it was determined that an enzymatic
bath The design
should is a Box–Hunter
be renewed every 3 h. Central composite type with a rotation factor of 1.41. The design is
(X,Y)–(time,
The designconcentration).
is a Box–HunterScheme 2 shows
Central the DoEtype
composite andwith
Tablea 3rotation
lists all factor
performed experiments.
of 1.41. The design is
Results concentration).
(X,Y)–(time, of mechanicalScheme testing2 for
showsthetheabove mentioned
DoE and fiberalltogether
Table 3 lists performed with microscopic
experiments.
observations have led to the reduction of experiments in two enzymatic treatments: Biopectinase K
enzyme at 25%, and 100% concentration r.f.w. for 6 h, with bath renewal after 3 h of treatment. These
Materials 2016, 9, 370 5 of 16

treatments will be referred to as Treatment 1 and Treatment 2, respectively. Fibers after Treatment 2
were carried
Materials 2016, 9,to
370a pilot scale yarn production plant for spinning tests. 5 of 16

Scheme 2. DoE
Scheme for for
2. DoE each enzyme.
each enzyme.

Table
Table 3.
3. Treatment
Treatment conditions
conditions for
for Biopectinase K treatments
Biopectinase K treatments in
in the
the last
last DoE.
DoE.

Test Number Time (h) Enzyme Concentration (% r.f.w)

Test Number Time (h) Enzyme Concentration (% r.f.w)
1 6.00 100.00
21 6.00
3.88 100.00
89.00
32 3.88
3.00 89.00
62.50
3 3.00 62.50
44 3.88
3.88 35.91
35.91
55 6.00
6.00 25.00
25.00
6 8.12
8.12 35.91
35.91
77 9.00
9.00 62.50
62.50
8 8.12 89.09
89 8.12
6.00
89.09
62.50
9
10 6.00
6.00 62.50
62.50
10
11 6.00
6.00 62.50
62.50
12
11 6.00
6.00 62.50
62.50
13 6.00 62.50
12 6.00 62.50
14 6.00 35.91
13
15 6.00
6.00 62.50
89.00
14 6.00 35.91
15 6.00 89.00
2.2. Fiber Characterization

2.2.1.Results of mechanical testing for the above mentioned fiber together with microscopic
SEM Microscopy
observations have led to the reduction of experiments in two enzymatic treatments: Biopectinase K
Results of the first DoE (conditions shown in Table 1) were analyzed by SEM microscopy, as fibers
enzyme at 25%, and 100% concentration r.f.w. for 6 h, with bath renewal after 3 h of treatment. These
have not shown good enough macroscopic quality to carry out the characterization tests. Images
treatments will be referred to as Treatment 1 and Treatment 2, respectively. Fibers after Treatment 2
obtained at the same magnification show that fiber depletion does not occur, thus indicating that
were carried to a pilot scale yarn production plant for spinning tests.
performed treatments were not enough to reach the target quality for a textile fiber degree. However,
it can
2.2. also
Fiber be concluded that treatment with Biopectinase K seems to provide better results than
Characterization
Biopectinase M01, as the fibers appear cleaner.
2.2.1.Observations
SEM Microscopycarried out for selected treatments (25% and 100% r.f.w. for 6 h: Treatments 1 and 2)
as well as for virgin fibers, show that treated fibers are cleaner than virgin ones. Furthermore, as
Results of the first DoE (conditions shown in Table 1) were analyzed by SEM microscopy, as
observed in Figure 2, fibers from Treatment 2 are the thinner ones, showing microfibrillation, due to
fibers have not shown good enough macroscopic quality to carry out the characterization tests.
the removal of hemicellulose and pectin, which act as bonding agents between the microfibrils that
Images obtained at the same magnification show that fiber depletion does not occur, thus indicating
form a fiber; these bonding substances can be observed in untreated fiber images.
that performed treatments were not enough to reach the target quality for a textile fiber degree.
However, it can also be concluded that treatment with Biopectinase K seems to provide better results
than Biopectinase M01, as the fibers appear cleaner.
Observations carried out for selected treatments (25% and 100% r.f.w. for 6 h: Treatments 1 and
2) as well as for virgin fibers, show that treated fibers are cleaner than virgin ones. Furthermore, as
observed in Figure 2, fibers from Treatment 2 are the thinner ones, showing microfibrillation, due to
the removal of hemicellulose and pectin, which act as bonding agents between the microfibrils that
form a fiber; these bonding substances can be observed in untreated fiber images.
 Materials 2016, 9, 370 6 of 16
Materials 2016, 9, 370 6 of 16

Figure 2. SEM
Figure pictures
2. SEM ofofbanana
pictures banana fibers: (a)untreated
fibers: (a) untreated fibers;
fibers; (b) fibers
(b) fibers after Treatment
after Treatment 1; (c)
1; (c) fibers fibers
after
afterTreatment
Treatment 2. 2.

2.2.2.2.2.2. Optical
Optical Microscopy
Microscopy
Banana
Banana fibers
fibers werewere observedatatdifferent
observed different magnifications,
magnifications, under
undernormal
normaland
andpolarized light.
polarized light.
Ten individual fibers were measured. Virgin banana fiber had an average diameter of about 200 µm,
Ten individual fibers were measured. Virgin banana fiber had an average diameter of about 200 μm,
while treated fibers show smaller average diameters: 160 µm for fiber after Treatment 1 and 114 µm for
while treated fibers show smaller average diameters: 160 μm for fiber after Treatment 1 and 114 μm
Treatment 2 fibers. Figure 3 shows an image of each type of fiber at the same magnification, where the
for Treatment 2 fibers. Figure 3 shows an image of each type of fiber at the same magnification, where
reduction of the fiber diameter can be clearly observed. Diameters of micro-fibrils measure approx.
the reduction of thefibers
23 µm for virgin fiber diameter
and 16 µm forcan be clearly
treated ones. observed. Diameters of micro-fibrils measure
approx. 23 μm for virgin fibers and 16 μm for treated ones.
Materials 2016, 9, 370 7 of 16

Figure 3. Optical micrographs of virgin banana fibers and their diameters: (a) untreated fibers; (b) fibers
after Treatment 1; (c) fibers after Treatment 2.

2.2.3. Mechanical Properties of Banana Fiber

Up to 10 samples of fiber were tested. Results show a tensile strength of 42.8 ˘ 6.5 cN/tex for
virgin banana fibers. As can be observed in Table 4, the tensile strength of fibers with Treatment 1 is
virtually unchanged, while a reduction of 14% is observed for fiber with Treatment 2.

Table 4. Banana fiber tenacity.

Fiber Tenacity (cN/tex) Standard Deviation

Untreated 42.8 6.5
Treatment 1 42.0 5.4
Treatment 2 36.8 6.3

Table 4 shows the results obtained for mechanical testing of fibers after the selected treatments;
however, as explained in Section 2.1, mechanical tests were also performed for fibers treated according
to Table 3. Results obtained for 6 h treated fibers are summarized in Table 5.

Table 5. Tenacity of the different fibers treated in the last DoE.

Fiber Tenacity (cN/tex) Standard Deviation

62.50% 6 h 28.6 4.7
89.09% 6 h 35.2 6.4
35.90% 6 h 30.7 6.2
Materials 2016, 9, 370 8 of 16

temperature corresponds to the maximal degradation rate, and it is obtained from the weight loss
derivative curve. Results can be more clearly observed in Figure 4.
Materials 2016, 9, 370 8 of 16
Table 6. Degradation temperatures (in °C) of virgin and treated banana fibers.

Fiber
2.2.4. Thermal Stability Left Limit Onset Peak Humidity (%) Ashes (%)
Untreated 180 245 280 6.5 3.8
Table 6 shows the average
Treatment 1 values
220 obtained
300 in321 thermal tests 8.6using thermogravimetric
2.9 analysis
(TGA). It is clearly observed
Treatment 2 how the
245 thermal
290 stability
316 of the fibers
6.1 is increased 1.0significantly due to
the enzymatic treatment. The left limit temperature refers to the temperature at which weight loss
startsIsothermal
(apart fromtests
humidity
(carriedremoval). Onset
out at 220 °C) temperature
show higherisweight
obtained from
loss for the intersection
untreated fiber between
(39.7%); the
an
protractions of the flat part of the curve before the left limit temperature and the
important decrease in this parameter was observed for treated fibers: 25.2% and 15.2% for fibers most important weight
after
loss section 1ofand
Treatments the 2,
curve; as it is needed
respectively. from graphical
This parameter calculations,
confirms the higherit may be anstability
thermal inexact achieved
parameter, but
from
it has been calculated for comparison purposes with bibliography data.
the enzymatic treatments due to the removal of less thermally stable substances (mainly Peak temperature corresponds
to the maximal and
hemicelluloses degradation rate,temperature
pectin). This and it is obtained from the
was chosen as itweight losstemperature
is a usual derivative curve. Results can
in thermoplastic
be more
parts clearly observed in Figure 4.
processing.

Figure 4. TG and DTG curves.

Figure 4. TG and DTG curves.
2.3. Processability: Spinning Process
Table 6. Degradation temperatures (in ˝ C) of virgin and treated banana fibers.
2.3.1. Opening
Fiber Left Limit Onset Peak Humidity (%) Ashes (%)
This stageUntreated
was performed180 in a lab-scale
245 Shirley280opener for short
6.5 fiber. As 3.8
banana fiber shows
high stiffness (around
Treatment360
1 cN/tex)
220compared 300to other321
fibers such as8.6
flax or hemp (1502.9 cN/tex) or cotton
(80 cN/tex), higher amounts
Treatment 2 of245
fiber are collected
290 on the tray, even
316 6.1 when varying 1.0 the blades and
working rates. However, the processed fiber is more open and its processing is improved in the
combing flats. Some
Isothermal testsmechanical
(carried outadjustments couldhigher
at 220 ˝ C) show be done to improve
weight loss forthis first stepfiber
untreated yielding.
(39.7%); an
important decrease in this parameter was observed for treated fibers: 25.2% and 15.2% for fibers after
2.3.2. Revolving Flat Card
Treatments 1 and 2, respectively. This parameter confirms the higher thermal stability achieved from
the enzymatic treatments
This part of the workduewastoconducted
the removal
onofa less
Plattthermally
card withstable
rigidsubstances (mainly
cards, at high hemicelluloses
levels of humidity
andgpectin).
(17 This
water per temperature
dry wasresults
air kg). First, chosenshowed
as it is abroken
usual temperature in thermoplastic
fibers with low interfibrillar parts processing.
cohesion; fibers
are adhered to the drum, the flats ant the comber noils, as shown in Figure 5. Furthermore, an
2.3. Processability:
important amountSpinning
of scrapProcess
is produced during the processing, which reflects the difficulty of
spinning this fiber.
2.3.1. Opening
This stage was performed in a lab-scale Shirley opener for short fiber. As banana fiber shows
high stiffness (around 360 cN/tex) compared to other fibers such as flax or hemp (150 cN/tex) or
cotton (80 cN/tex), higher amounts of fiber are collected on the tray, even when varying the blades
and working rates. However, the processed fiber is more open and its processing is improved in the
combing flats. Some mechanical adjustments could be done to improve this first step yielding.
Materials 2016, 9, 370 9 of 16

2.3.2. Revolving Flat Card

This part of the work was conducted on a Platt card with rigid cards, at high levels of humidity
(17 g water per dry air kg). First, results showed broken fibers with low interfibrillar cohesion; fibers are
adhered to the drum, the flats ant the comber noils, as shown in Figure 5. Furthermore, an important
amount of scrap is produced during the processing, which reflects the difficulty of spinning this fiber.
Materials 2016, 9, 370 9 of 16

Materials 2016, 9, 370 9 of 16

Figure 5. Adherence of the fibers to the drum during the carding process.
Figure 5. Adherence of the fibers to the drum during the carding process.
To try to improve
Figure the efficiencyofofthe
5. Adherence thefibers
process,
to thebanana fibersthe
drum during were mixed
carding with cotton at different
process.
ratios:
To try 50/50 and 70/30
to improve the(banana/cotton).
efficiency of the Cotton is acting
process, in this
banana yarn were
fibers as a supporting
mixed with fiber. Fibers,
cotton atafter
different
ratios: 50/50 and 70/30 (banana/cotton). Cotton is acting in this yarn as a supporting fiber.the
passing
To through
try to the
improve Shirley
the opener,
efficiency of were
the blended
process, together
banana fibersmanually
were and
mixed then
with processed
cotton at in
different Fibers,
revolving
afterratios:
passing50/50 flat
andcard.
through 70/30It (banana/cotton).
the can still be
Shirley observed
opener, Cotton
werethat part ofinthe
isblended
acting fibers
this yarnadhere
together to the
as a supporting
manually anddrum
thenand
fiber. the cards
Fibers, afterin the
processed
althoughthrough
passing in a smaller proportion,
the Shirley getting
opener, werea veil with together
blended better interfibrillar
manually adhesion
and then(Figure 6) and
processed less
in the
revolving flat card. It can still be observed that part of the fibers adhere to the drum and the cards
scraps produced.
revolving flat card. It can still be observed that part of the fibers adhere to the drum and the cards
although in a smaller proportion, getting a veil with better interfibrillar adhesion (Figure 6) and less
although in a smaller proportion, getting a veil with better interfibrillar adhesion (Figure 6) and less
scraps produced.
scraps produced.

Figure 6. Veil cohesion for 50/50 blend of banana and cotton fibers.

As expected, when Figureincreasing the ratio

6. Veil cohesion of banana
for 50/50 blend offiber up and
banana to 70%,
cottonthe behavior in the carding
fibers.
process is more Figure similar6.toVeilthiscohesion
for 100% forbanana
50/50 blend
fiber,ofwith
banana
more and cotton fibers.
damaged fibers and increased
adherence to the when
As expected, drumincreasing
and the card flats of
the ratio (relating
bananato theup
fiber 50/50 blend).
to 70%, An optimization
the behavior in the
in the carding
machinery
process
As expected, could
is more whenleadincreasing
similar totoanthisimprovement
forthe100%ratio inofthe
banana carding
fiber, fiber
banana stage
with upfor
more banana
todamaged
70%, the fibers,
fibersachieving better
and increased
behavior in the carding
processability.
adherence
process is more to similar
the drumtoand thistheforcard
100% flats (relating
banana to the
fiber, 50/50
with moreblend). An optimization
damaged fibers andinincreased
the
adherence Further
machineryto the testslead
could
drum were conducted
andtothean card using
improvement
flats polyester
in the
(relating conventional
tocarding
the 50/50stage fibers
for
blend). Anasoptimization
banana support fiber,
in at
fibers, achieving theabetter
50/50
machinery
ratio. Results were similar to those obtained with the cotton blend. Finally, wool was also used, in
processability.
could lead to an improvement in the carding stage for banana fibers, achieving better processability.
order to increase
Further tests the
wereamount
conducted of banana
usingfiber in theconventional
polyester mix, taking advantage of the natural
fibers as support fiber, atcurling
a 50/50 in
Further tests were conducted using polyester conventional fibers as support fiber, at a 50/50 ratio.
wool Results
ratio. as a cohesion element;
were similar to blends were made
those obtained with with
the 50%
cottonandblend.
70% of banana
Finally, fibers.
wool wasThe alsoprocedure
used, in
Results
waswere
order
similar
identical
to increase to theto one
those
amount
obtained
followed for with
of banana cotton. the the
fiber inThis
cotton
blend blend. Finally,
can beadvantage
mix, taking processed wool awas
ofinthe
also used,
conventional
natural curling
in
rubin
in
order
to increase
device
wool the
asunder amount of
industrial
a cohesion banana
conditions,
element; fiber
blends were in
althoughthe mix,
madeatwith taking
a lower advantage
50% production
and 70% of rate of
banana the natural
thanfibers. curling
conventional cotton. wool
The procedure in
as a was
cohesion
Figure element;
7 shows
identical tothe blends
theresult
one of thewere
followed made
carding
for with
process
cotton. 50%
for
This 70%and
blend 70%be of
banana/30%
can banana fibers.
wool blends.
processed in The procedure
a conventional rubin was
identical
devicetounder
the one followed
industrial for cotton.
conditions, This blend
although can be
at a lower processed
production rateinthan
a conventional
conventionalrubincotton.device
Figure 7 shows the result of the carding process for 70% banana/30% wool blends.
Materials 2016, 9, 370 10 of 16

under industrial conditions, although at a lower production rate than conventional cotton. Figure 7
shows the result of the carding process for 70% banana/30% wool blends.
As a result of the experiments performed, it is observed that banana fibers can be spun to get
yarn, although the machinery should be adapted to the high stiffness of these fibers. Better results are
obtained when blending banana fibers with other softer fibers; at this stage, the most suitable blend to
be obtained at industrial
Materials 2016, 9, 370 scale would be this with wool. 10 of 16

Materials 2016, 9, 370 10 of 16

Figure 7. Veil of banana-wool blend 70/30.

Figure 7. Veil of banana-wool blend 70/30.
Table 7 shows a summary Figure
of the 7. Veil of banana-wool
conditions blend
followed for the70/30.
drawing frame process.
Table 7 shows a summary of the conditions followed for the drawing frame process.
Table 7 shows a summary
Table of the
7. Conditions for conditions followed
drawing frame for the
the blends withdrawing frame process.
banana fibers.
Table
Table 7. Conditions
Parameter
7. Conditions fordrawing
for drawing frame
1st
frame the the
Stage 2blends
blendsndwithwith
Stage banana
3rd
banana fibers.
Stage
fibers.
Feed slivers (number) Nappa 4 2.65
Parameter
Parameter 1st Stage
1st Stage 2nd Stage 3rd Stage
2nd4Stage
Joining slivers (number) – 6 3rd Stage
Feed
Feed slivers slivers
(number) (number) Nappa 4 2.65
Previous stretching (rate)Nappa 1.3 1.34 1.3 2.65
Joining
Joining slivers slivers (number) – – 4 6
Total(number)
stretching (rate) 9 64 3.5 6
PreviousPrevious
stretching stretching
(rate)
Output title (g/m)
(rate) 1.3 1.3
4
1.3
2.651.3 1.3 1.3
4.6
Total stretching (rate)
Total stretching (rate) 9 9 66 3.5 3.5
Gauge of the rubin (mm)
Output title (g/m)title (g/m)
Output 4 4 2.65
2.65 4.6 4.6
Gauge ofGauge Wool (mm)
the rubin blend (%) 50/58/45 50/58/45 50/58/45
of the rubin (mm)
Polyester
Wool blend (%) blend (%) 50/58/45 48/45/42 48/45/42
50/58/45 48/45/42 50/58/45
Wool blend (%) 50/58/45 50/58/45 50/58/45
Cotton
Polyester blend blend (%) 48/45/42
(%) 38/35/32 38/35/32
48/45/42 38/35/32 48/45/42
Polyester
Cotton blend blend (%) 38/35/32
(%) (method) 48/45/42 48/45/42
38/35/32 48/45/42 38/35/32
Pressure Springs Springs Springs
Pressure Cotton blend (%) Springs
(method) 38/35/32 38/35/32
Springs 38/35/32
Output rate (mm/min) 20 20 20 Springs
Output ratePressure
(mm/min) (method) 20Springs 20
Springs Springs 20
Figure 8 shows Output
images of rate
the(mm/min) 20
drawing sliver obtained 20
for different 20 They were spun after
blends.
to obtain8 the
Figure rovings
shows and then
images twisted
of the drawingto obtain
sliverthe yarns and
obtained fortwo ply yarns
different (Figure
blends. 9). were spun after
They
Figure 8 shows images of the drawing sliver obtained for different blends. They were spun after
to obtain the rovings
to obtain andand
the rovings then twisted
then twistedtotoobtain
obtain the yarnsand
the yarns andtwo
twoply
ply yarns
yarns (Figure
(Figure 9). 9).

Figure 8. Drawing sliver of the banana fiber blended with: (a) cotton; (b) polyester; (c) wool.

Figure
Figure 8. Drawing
8. Drawing sliver
sliver ofofthe
thebanana
banana fiber
fiber blended
blendedwith:
with:(a)(a)
cotton; (b)(b)
cotton; polyester; (c) wool.
polyester; (c) wool.
Materials 2016, 9, 370 11 of 16
Materials 2016, 9, 370 11 of 16

Figure
Figure 9. Picturesshowing:
9. Pictures showing:(a)(a) rovings
rovings obtained
obtained withwith the three
the three blends;
blends; (b) banana/wool
(b) banana/wool yarn; (c)yarn;
2 ply
(c) 2 ply banana/wool
banana/wool yarn. yarn.

As a result of the experiments performed, it is observed that banana fibers can be spun to get
2.4. Yarn Characterization
yarn, although the machinery should be adapted to the high stiffness of these fibers. Better results
Table 8 shows
are obtained average results
when blending bananaobtained for banana
fibers with and banana/PP
other softer yarn.
fibers; at this This
stage, theyarn
mostwas made
suitable
with the
blend blends
to be made
obtained at of 70% banana
industrial scalefibers
wouldand 30%with
be this wool.wool.
The yarn containing PP fiber was made
twisting a banana yarn with PP yarn (330 dtex), at 90 laps/m, in an S sense. Tests on a conventional
flax/PP
2.4. Yarn yarn were also conducted for comparison. It is observed that banana/PP yarn has higher
Characterization
tenacity than flax/PP yarn and also that elongation at the break is higher for the banana yarn than for
Table 8 shows average results obtained for banana and banana/PP yarn. This yarn was made
flax/PP yarn.
with the blends made of 70% banana fibers and 30% wool. The yarn containing PP fiber was made
twisting a banana yarn with PP yarn (330 dtex), at 90 laps/m, in an S sense. Tests on a conventional
Table 8. Mechanical properties of yarn.
flax/PP yarn were also conducted for comparison. It is observed that banana/PP yarn has higher
tenacity than flax/PPProperty
yarn and also that elongation at the break
Banana Yarn is higher
Banana/PP Yarnfor theFlax/PP
bananaYarn
yarn than for
flax/PP yarn.
Title of the yarn (tex) 166 166 166
Strength of breaking load (cN) 910 1910 1310
Table
Coefficient of variation (%)8. Mechanical
11.2properties of yarn.4.9 12.4
Tenacity (CN/tex) 5.5 11.5 7.9
Property
Elongation at break (%) Banana13.0Yarn Banana/PP 19.7 Yarn Flax/PP
4.5 Yarn
Title of the
Coefficient yarn (tex)
of variation (%) 166
21.3 166
6.4 166
26.5
Strength of breaking load (cN) 910 1910 1310
Coefficient
3. Discussion of variation (%) 11.2 4.9 12.4
Tenacity (CN/tex) 5.5 11.5 7.9
3.1. Microscopy
Elongation at break (%) 13.0 19.7 4.5
Coefficient
As explained inofthe
variation
Results(%) 21.3after the enzymatic
section, fibers 6.4 treatment appear 26.5 cleaner and
defibrillated, where this effect is more observed at higher enzymes concentration. In addition, it was
3. Discussion
proven that Biopectinase K provided better cleanliness than Biopectinase M01. Polygalacturonase
(Biopectinase K) belongs to the pectinases family, while Biopectinase M01 consists in a blend of
3.1. Microscopy
hemicellulases and pectinase. Pectin hydrolysis has been found useful for banana fiber cleaning, at
45 ˝ C
Asfor
explained in the
90 min [16]; Results defibrillation
however, section, fibersdoesafternottheoccur
enzymatic
and fibertreatment
diameterappear
does cleaner
not seem and
to
defibrillated, where
be affected. The this effect
Fangamyx is morewas
enzyme observed
used to at treat
higher enzymes
abaca fibersconcentration.
[20], resultingIninaddition, it was
the presence of
proven that Biopectinase
defibrillation K provided
and a reduction better
in diameter, cleanliness
although than Biopectinase
less significant (from 145M01. Polygalacturonase
to 130 µm) than the one
(Biopectinase
observed in thisK) work
belongs to the pectinases
for banana fibers. Hemp family, while
has also Biopectinase
been treated using M01 consists
enzymes in a blend of®
(SIHA-Panzym
hemicellulases and pectinase.
DF, pectinase) with Pectin
the final aim hydrolysiscomposites,
of producing has been found useful
resulting in afor bananaoffiber
decrease 42%cleaning, at
in the cross
45 °C for[21].
section 90 min [16]; however, defibrillation does not occur and fiber diameter does not seem to be
affected.
CottonThefibers
Fangamyx
show aenzyme
diameter was
of used to treat
15.6 µm, and abaca fibers
it is well known[20],that
resulting in the
they are the purest
presence of
fibers
defibrillation and a ones,
among the natural reduction
beinginmainly
diameter, although
constituted ofless significant
cellulose (frommeasured
[22]; fibrils 145 to 130for
μm) than the
treated one
banana
observed in this work for banana fibers. Hemp has also been treated using enzymes (SIHA-Panzym®
DF, pectinase) with the final aim of producing composites, resulting in a decrease of 42% in the cross
section [21].
Materials 2016, 9, 370 12 of 16

fibers show a diameter around 16 µm, while virgin ones are around 23 µm; this shows also the
cleanliness degree achieved after the enzymatic process with the removal of pectin and hemicellulose.

3.2. Mechanical Properties of Banana Fiber

Virgin banana fibers (42.8 cN/tex) show higher tenacity than hemp (23.6 cN/tex [23]), jute
(23.9–27.6 cN/tex [24]) or cotton (24–36 cN/tex [25]), while having a lower tenacity than flax
(59.9 cN/tex [26]), sisal (57.2 cN/tex [27]) or rayon (56 cN/tex [26]). Treated banana fibers show better
results than hemp, jute or cotton, while showing reduced compared to untreated flax or hemp. Fibers
obtained from Colombian plantains exhibit a tensile strength of 47 cN/tex [28].
From Tables 4 and 5 it can be observed that enzyme concentrations over 25% r.f.w. result in lower
mechanical properties due to the most intensive cleaning process. As explained in Section 2.2.1, the
fiber surface appears cleaner with the highest concentration of enzymes, leading to the defibrillation of
the fibers into the cellulosic microfibrils, a fact which explains the stiffness decrease. An increase in the
mechanical properties of flax has been reported after fiber retting [29]. The authors explain this by the
lower diameter and weight of the fibers once they have been retted (from 47.1 to 72.8 cN/tex). Other
research also shows a decrease in the mechanical properties due to their treatment and processing;
hemp tenacity is reduced from 23.6 to 8.5 cN/tex after being immersed in an 18% NaOH solution
for 30 min at room temperature [23], while varying from 29.8 to 24.9 cN/tex after mercerization with
NaOH 22% solution for 60 min [30].

3.3. Thermal Stability

Comparing data obtained from TGA tests summarized in Table 6 with those obtained for major
constituents in the fiber (cellulose, hemicellulose and lignin), it is possible to infer the extent of
hemicellulose and lignin removal because of the enzymatic treatment.
Hemicellulose degradation temperatures are found between 220 ˝ C and 278 ˝ C (pectin also
degrades at this temperature range [31]); it was found that weight loss at this stage is significantly
decreased due to the enzymatic treatment (from 30.6% to 21.3% and 12.2% for virgin fibers, 25% and
100% 6 h treated fibers). From these results, it can be inferred that part of the hemicelluloses have been
degraded during the enzymatic treatment. Following the degradation step, which takes place between
278 ˝ C and 360 ˝ C, corresponding to cellulose degradation; the weight loss in this part of the curve
increases with the enzymatic treatment, that is, the amount of cellulose is higher in fibers which have
been treated. This corresponds to the previous observation of the lower content in hemicelluloses, and
with the higher fineness of the fibers, as hemicelluloses act as a bonding agent among the cellulosic
fibrils. Peak temperature for all fibers correspond to the degradation of cellulose, and degradation rates
go from 1.0 wt%/˝ C for virgin fibers to 2.0 wt%/˝ C for treated ones (pure cellulose has a degradation
rate of 2.8 wt%/˝ C [32]). The difference between the pure cellulose and the banana fibers may be
due to the presence of non-cellulosic compounds, such as lignin, in the fibers. Higher temperatures
lead to lower decomposition rates, related to lignin degradation; lignin degrades from the beginning
of the test until 900 ˝ C [32]; degradation of fibers until 900 ˝ C show higher residues for virgin fiber;
this is also observed in ash content at the end of the test (1100 ˝ C), being 3.8% for virgin and 25%
treated fibers; and only 1% for 100% treated ones. This ash could be due to the presence of inorganic
compounds in banana fibers, non-affected by enzymatic treatments.
An increase in the thermal stability due to the enzymatic treatment is clearly shown by the three
temperatures shown in Table 6; other authors have also reported increases from 10 to 20 ˝ C due to the
fiber treatment, either chemical or enzymatic [20,33].

3.4. Yarn Characterization

Other authors show a tenacity for flax yarn of 14.8 cN/tex [34] and 16 cN/tex for bamboo yarn [35].
Banana/PP yarns show around 46% higher tenacity than flax/PP yarn, also with a lower coefficient of
variation; this means that the banana/PP samples are more homogeneous. Banana fiber has lower
Materials 2016, 9, 370 13 of 16

tenacity (5.5 cN/tex) than previously reported yarn, although Banana/PP yarn is tougher than for
the flax/PP one. The toughening is achieved by the type of yarn Core Spun and using the optimum
torsion laps between banana/wool and PP yarn.
The spinning process has been slightly modified from the conventional process, especially for card
clothing and the machine parameters like speed, distance and position of the cylinders. The 3 stage
drawing frame is necessary to achieve a good mix of banana and wool fibers, and to obtain regular
good yarn tenacity.

4. Materials and Methods

4.1. Materials
Banana fibers were produced at the Universidad de Las Palmas de Gran Canaria (ULPGC) facilities
(Las Palmas de Gran Canaria, Spain), by means of a patented system by ULPGC. This prototype
equipment enables extracting fiber from the leaves by scraping it in two stages: linear scrapping
and rotational scrapping (potential production rate 90 kg/h). Afterwards, the long fiber (0.5–1 m) is
chopped in a developed machine, in the context of this research work, for cutting the fiber with a high
level of uniformity. The fiber was cut into small lengths according to the requirements of the enzymatic
treatment (45 mm). Enzymatic coctels used were obtained from BIOCON (Les Franqueses del Vallès,
Spain), Biopectinase M01 and Biopectinase K, containing pectinase and hemicellulase.
Conventional fibers were obtained from Innotex Center CTF (Terrassa, Spain). Cotton fibers used
in the blend with banana fibers were 28 mm long and had 3.8 in micronaire. PP fibers were cotton-like
cut, 38 mm length and 330 dtex fineness. Polyester fibers were cotton-like cut, conventional mat,
38 mm long, 1.5 dtex. Finally, wool fibers had 65 mm length and 23 µm fineness.

4.2. Methods

4.2.1. Fiber Teatments

A design of experiments (DoE) was made for the enzymatic treatment of the fibers, taking into
account the composition and characteristics of banana fibers. Two enzymatic formulations were
applied to the fibers: Biopectinase M01 (made of pectinase and hemicellulase) and biopectinase K
(made of poligalacturonase). The variable parameters chosen are treatment time and concentration of
enzymes related to fiber weight (r.f.w.). Fiber to bath volume ratio was settled to 1:40 for scalability
purposes, while temperature and pH were fixed according to datasheets for the selected enzymes:
pH = 4.5 and T = 45 ˝ C.

4.2.2. Fiber Characterization

Fibers were characterized by means of thermogravimetric and isothermal analysis, microscopy,
and fineness. Thermogravimetric analyses (TGA) were run to determine potential thermal degradation
of fiber; a Mettler Toledo TGA/DSC1 analyzer (Mettler Toledo, Toledo, OH, USA) was used at a
heating rate of 5 ˝ C/min in air atmosphere (10 mL/min). Isothermal studies were also carried out by
keeping the fibers at 220 ˝ C for 150 min, in air atmosphere with 10 ml/min of air flow. Three replicas
were performed for these tests. Microscopic observations of fibers were carried out in an Olympus
BX51 optical microscope (Olympus, Tokyo, Japan), at different magnifications and under polarized
light; 10 samples were measured for each type of fiber (5 measures in each fiber). SEM microscopy was
made in a Tabletop Phenom device (Phenomworld, Eindhoven, The Netherlands) in the fiber direction
to observe its surface. Mechanical tests of fibers were performed according to UNE EN-ISO standard
5079:1996, in a constant elongation gradient dynamometer from Instron (mod. 4501) (Norwood, NJ,
USA); samples were conditioned at 20 ˝ C ˘ 2 ˝ C and 65% ˘ 4% humidity for 24 h. These conditions
were also kept during testing. 10 samples were tested, at 10 mm/min.
Materials 2016, 9, 370 14 of 16

4.2.3. Spinning Process

Once fibers were treated by enzymatic means and characterized, fibers were introduced into a
lab-scale spinning plant. A Shirley opener for short fiber (SDL Atlas, Rock Hill, SC, USA) was used
before introducing the fibers into the carding flats. The absolute humidity during fiber processing
was 17 g/kg dried air, as previous experiences have shown that stiff fibers have better processability
when working at high humidity rates. Due to the difficulty of banana fibers spinning (because of their
high stiffness), they were mixed with cotton, polyester and wool. Once the wick was produced, the
following step was carried out in an industrial twist roving Electro-Jet (Electro-Jet S.A., Gurb, Spain).
The spinning process took place in a continuous ring spinning machine, from Pinter (Pinter S.A.,
Santpedor, Spain). The yarn was then twisted in a ring twister from Galan Textile Machinery
(Terrassa, Spain); the filaments were twisted at 400 laps/m, in an S sense; and the spindles ratio
was 2000 laps/min with a production of 5 m/min.

4.2.4. Yarn Characterization

Produced yarns were characterized to determine their title and stiffness. Mechanical testing was
carried out following the standard procedure scheduled. UNE-EN ISO 2062-2010 (Method A) was
followed, using a constant elongation gradient dynamometer INSTRON (Class 0.5) (Instron, Norwood,
NJ, USA). Samples were conditioned for 24 h at 20 ˝ C ˘ 2 ˝ C y 65% ˘ 4% r.h. Specimens were 250 mm
long, tensile speed was 250 mm/min and a pretension of 0.5 cN/tex was applied. 20 replicas were
tested. Title was determined following the standard method of UNE-EN ISO 2060:1996.

5. Conclusions
‚ The enzymatic treatment has proven to be useful for banana fiber treatment, achieving an
improvement in terms of cleanliness and fibrillation.
‚ The most effective enzyme for banana fiber treatment is poligalacturonase (Biopectinase K),
showing a high specific activity and being specific for substrates not damaging the cellulosic
structure of fibers.
‚ Long duration treatments (24 h, 48 h and 7 days) did not provide good results, due to enzyme
deactivation. 6 h was optimal to obtain a textile grade banana fiber.
‚ Optimal conditions for banana fiber enzymatic treatment are: 100% Biopectinase K, 6 h; 45 ˝ C,
pH = 4.5, with bath renewal after 3 h.
‚ Stability studies have demonstrated that over 80% of its activity takes place in the first 3 h;
afterwards, the enzyme activity decreases reaching 12% 24 h later.
‚ Enzymatic treatments improve the thermal stability of fibers by the removal of pectin and
hemicellulose, while producing a slight decrease in mechanical properties, probably due to
defibrillation found under SEM observations.
‚ Banana fiber can be spun to produce yarns, mixed or not mixed with other fibers, while the most
suitable for industrial scale-up without major equipment changes would be the blend of banana
fiber and wool.
‚ Banana/PP yarn shows higher tenacity than flax/PP yarn and is more homogeneous.

Acknowledgments: The authors acknowledge the Spanish Ministry of Economy and Competitiveness, as well as
Fondo Europeo de Desarrollo Regional (FEDER) funds, as research was conducted under the BANTEX project
(code: MAT2013-47393-C2-1-R). Publishing costs in open access are also covered by the BANTEX project.
Author Contributions: Moisés Morón and Zaida Ortega conceived and designed the experiments; Mario D. Monzón,
coordinator of the research project, took part in the improvement of the fiber system extraction in terms of
cleanliness of fiber and efficiency of the extraction process; together with Rubén Paz, they designed the equipment
for fiber chopping; Rubén Paz manufactured this equipment and provided the fiber for the enzymatic treatments;
Moisés Morón and Pere Badalló were in charge of the enzymatic treatments and fiber spinning; Zaida Ortega
performed the characterization tests. Moisés Morón and Zaida Ortega analyzed the data; Zaida Ortega wrote
the paper.
Materials 2016, 9, 370 15 of 16

Conflicts of Interest: The authors declare no conflict of interest. The founding sponsors had no role in the design
of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript, and in the
decision to publish the results.

Abbreviations
The following abbreviations are used in this manuscript:
r.f.w. related to fiber weight;
TGA Thermogravimetric Analysis;
DoE Design of Experiments;
SEM Scanning Electron Microscope.

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