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Optimization of the alkali treatment

process of date palm fibres for
polymeric composites
a b c
I. Taha , L. Steuernagel & G. Ziegmann
a
Institute for Polymer Materials and Plastic Processing,
Agricolastrasse 6, 38678 Clausthal-Zellerfeld, Germany
b
Institute for Polymer Materials and Plastic Processing,
Agricolastrasse 6, 38678 Clausthal-Zellerfeld, Germany
c
Institute for Polymer Materials and Plastic Processing,
Agricolastrasse 6, 38678 Clausthal-Zellerfeld, Germany

To cite this article: I. Taha , L. Steuernagel & G. Ziegmann (2007): Optimization of the alkali
treatment process of date palm fibres for polymeric composites, Composite Interfaces, 14:7-9,
669-684

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 Composite Interfaces, Vol. 14, No. 7–9, pp. 669– 684 (2007)
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Also available online - www.brill.nl/ci

Optimization of the alkali treatment process of date palm

fibres for polymeric composites

I. TAHA ∗ , L. STEUERNAGEL and G. ZIEGMANN

Institute for Polymer Materials and Plastic Processing, Agricolastrasse 6,
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38678 Clausthal-Zellerfeld, Germany

Received 1 June 2006; accepted 3 January 2007

Abstract—The global interest in environmentally friendly material over the past few years has led
to the development of new research areas in the field of renewable materials and biocomposites.
Within this scope, several researches have been conducted to modify natural fibres aiming at an
improved compatibility with polymeric matrices. In this study, fibres from the spadix stem of the
date palm tree were treated with sodium hydroxide over different times. The effect of the alkali
treatment on the structure, thermal and mechanical behaviour of the fibres was verified through
chemical analysis, FTIR spectroscopy, TGA, and tensile testing. Comparing the different alkalisation
parameters, promising results are obtained with a 2% sodium hydroxide solution over a treatment time
of 2 h.

Keywords: Date palm fibres; natural fibres; alkalisation treatment; polymer composites.

1. INTRODUCTION

The use of natural fibres has found renewed interest in the past decade on the
research as well as on the industrial scale. In Europe, the integration of hemp,
sisal, flax and jute as reinforcement fibres for polymeric matrices is widespread.
Similarly, exotic plants in Asian regions are being investigated to examine their
adequacy as a source for renewable composite materials. In the Arab regions, the
palm tree is one of the most prevalent trees, which has always been exploited, not
only for its nutritious fruits but also for its secondary products, as plantations are
annually pruned. Date Palm Fibres (DPF) from the Spadix Stem (SS) were dried
and used as ropes and ties. Date Palm Leaf Midribs (DPLM) were cut into strips
for building baskets and fences. It is therefore of great interest to investigate the
adequacy of such high specific strength fibres as a reinforcement for polymeric

∗ To whom correspondence should be adressed. E-mail: iman.taha@tu-clausthal.de

 670 I. Taha et al.

materials in modern applications. The use of biopolymers would additionally offer

the advantages of a 100% biocomposite from renewable resources as such products
are completely biodegradable.
As is the case with other lignocellulosic materials, palm fibres are incompatible
with polymeric materials due to their hydrophilic nature. The presence of free
water and hydroxyl groups accompanied by waxy substances on the fibre surface
immensely hinder an effective adhesion with most binder materials [1]. Even
if a successive bonding could be achieved, the high water absorption of the
cellulose fibres would cause swelling and in turn dimensional instability that would
promote the development of cracks and therewith poor mechanical properties of
the composite. Hence, in order to make use of the high specific properties of
biodegradability, recyclability and low price of natural fibres, they have to be
subjected to treatments such as alkalisation and acetylation to allow molecules to
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penetrate the fibre’s crystalline regions, thus developing a nonpolar fibre surface
compatible with polymeric materials.
The process of alkalisation implies the subjection of a vegetable fibre to an in-
teraction with a fairly concentrated aqueous solution of a strong base to produce
swelling, with resultant changes in structure, dimensions, morphology and mechan-
ical properties (ASTM standard D6942). Thielemans and Woo [2] observed im-
proved mechanical interlocking between the liquid moulding resin and the alkalised
natural fibres due to the increased surface roughness on the one hand as well as due
to the consolidation of weak points in the structure and the removal of cellulose of
low degree of polymerisation on the other hand. Similarly, the removal of impurities
and hemicellulose was proved to contribute to the improvement of the mechanical
properties of lignocellulosics [3 –7].

2. EXPERIMENTAL

2.1. Materials
Raw samples from the Date Palm Spadix Stem (DPSS) were removed from the
date palms of the Ezbet El-Nakhl region in Egypt. These stems were then rolled
to split into fibres and further left to dry on the field. In the laboratory of the
Institute for Polymer Materials and Plastics Processing, the fibres were shortened
by means of scissors into bundles of around 50 cm in length. Sodium hydroxide
pellets (content
97%) and pure acetic acid (32%) used in this work were supplied
by VWR Germany.

2.2. Alkali treatment

The DPSS fibres were soaked in each 2% and 5% NaOH solution at 23◦ C for 2, 4, 6
and 24 h. The fibres were then taken out of the solution, drained, and washed several
 Alkali treatment of date palm fibres 671

times with tap water to remove any residual NaOH traces sticking on the fibre
surface. Fibres were then neutralised with dilute acetic acid, and finally rinsed again
with distilled water. Finally, they were left to dry overnight in air and additionally
dried at 100◦ C prior to any investigation analysis.

2.3. Testing methods

For the infrared spectral analysis, fibres were cut down to a length of about 5 mm.
The infrared spectra of short cut fibre surface were recorded using a Bio-Rad-7000
FTIR spectrophotometer with photoacoustic detectors. The disappearance of certain
peaks in the FTIR curves was observed; hence chemical analysis of the fibre before
and after treatment was made to ascertain the cause of such a change in the IR
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spectra. The Van Soest method was adopted to determine the chemical composition
of the DPSS [8, 9]. In this method a neutral detergent solution is first applied to
dissolve easily digestible matters such as proteins and lipids [9]. Then, an acid
detergent solution is applied to the fibres, resulting in the digestion of hemicellulose
[8]. The residue of the acid detergent solution is then further treated with 72%
sulphuric acid (H2 SO4 ) to remove cellulose [8]. The residual substance is then
finally brought to ignition for 2 h at 500◦ C in a muffle furnace to burn out lignin,
leaving behind indigestible minerals. The investigated matter is weighed before and
after each step and used to calculate the amount of each cell wall constituent of the
DPSS.
For the determination of the water absorption behaviour of DPSS, samples of
about 0.3 g were conditioned at 20 ± 2◦ C and 65 ± 2% RH for 72 h to water
saturation. The samples were weighed to the nearest 0.001 g (mi ) and subsequently
dried at 103◦ C and measured every couple of hours until no change in weight (i.e.
not more than 0.1%) could be observed within 6 h (mf ). The percentage moisture
content absorbed by the fibres was then calculated as

mi − mf
× 100.
mf

Thermogravimetric measurements were carried out using a Hi Res TGA2950

thermodynamic Analyzer from TA Instruments under air flow. Measurements were
performed at a heating rate of 5 K/min from room temperature to 600◦ C.
Single fibres of DPSS were used as tensile specimens such that a gauge length of
20 mm was ensured. Tensile tests were conducted on a Zwick Universal Testing
Machine with a load cell of 2 kN at a crosshead speed of 1 mm/min. The reaction
force and displacement were recorded and the stress, strain and Young’s modulus
were determined. Fifty single fibres were examined for each treatment method and
the mean value was reported.
 672 I. Taha et al.

3. RESULTS AND DISCUSSION

3.1. Infrared spectroscopy

The spectral data of the FTIR analysis of unmodified as well as 24 h alkali-treated
(5%) DPSS are presented in Fig. 1. The peak positions of the absorption bands,
corresponding to the vibration groups giving rise to the most probable absorption
bands, are presented in Table 1. From Fig. 1 it can be inferred that several chemical
reactions have taken place during the alkali treatment. It is evident that there was a
visual change in the peaks at 3360, 1730, 1660, 1530, 1380 and 1280 cm−1 .
The peak around 3360 cm−1 arose from O–H stretching vibration, which shows an
increased intensity upon alkali treatment, indicating an increase in the O–H content
of the fibres. This can be attributed to the cleavage of alkali sensitive bonds [4],
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since alkali treatment is known to break the hydrogen bonding in cellulosic hydroxyl
groups [10]. The removal of surface impurities (see peak at 1730 cm−1 ) also implies
the exposure of hydroxyl groups involved in the cellulosic fibre structure [11].
However, the O–H stretching vibrations might also be assigned to the presence of
absorbed water. Eventually, the most probable conjecture is that the occurrence of
such vibration groups is a result of various cumulative effects.
The FTIR peak at 1730 cm−1 , corresponding to C=O stretching vibration,
suggests the existence of carboxylic acid and/or ester groups, which are assumed
to be found in fatty acids. This assumption is supported by the disappearance of this
peak upon alkali treatment due to the removal of the traces of fatty substances from
the fibre surface. Hence, the alkali treatment of natural fibres involves a process of
de-esterification [11, 12].

Figure 1. FTIR spectra of untreated and alkali-treated DPSS.

 Alkali treatment of date palm fibres 673

Table 1.
FTIR spectral data of raw and alkali-treated DPSS

Photoacoustic absorbance (cm−1 ) Possible assignments

DPSS DPSS DPSS
untreated 2% NaOH 24 h 5% NaOH 24 h
3360 3386 3398 O–H stretching
2920 2917 2917 C–H stretching vibration in cellulose
2140 2167 2160 and hemicellulose
1728 – – C=O stretching of carboxylic acid and ester
groups
1661 1651 1654 Absorbed water in crystalline cellulose
1605 1595 1594 Aromatic C=C stretching
1530 – –
1508 1508 1508 Lignin component
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Aromatic skeletal ring vibration due to lignin

– 1462 1462
1426 1421 1422 CH2 symmetric bending
1380 1396 1377 C–H bending
1334 1334 1334 O–H bending
1242 1238 1234 C–O stretching of acetyl (lignin)
1165 1165 1165 Antisymmetric bridge C–O–C stretching
1045 1045 1045 C–O/C–C stretching vibration

A further articulate change can be observed at 1530 cm−1 related to the C=C
stretching vibration. The small peak at this band completely disappeared as a result
of alkalisation, which can be related to the removal of unsaturation present in oil
traces and fatty substances on the fibre surface [12].
It is assumed that alkali treatment has negligible effect on lignin, which is
indicated by the very slight diminishing peak at 1380 cm−1 corresponding to lignin
components [4, 13]. In contrast, the presumption that hemicellulose is effectively
removed by sodium hydroxide treatment is revealed by the diminishing peaks in
the range between 1280 and 1330 cm−1 . These peaks were also found to further
dwindle with higher caustic soda concentration and longer reaction time as can be
depicted from Fig. 2, indicating the increased efficiency in hemicellulose removal.
Moreover, the shoulder at 1660 cm−1 indicating absorbed water became more
prominent with increased reaction time and concentration. The reason therefore
is the increased amount of free hydroxyl groups ready to react.

3.2. Chemical analysis

As anticipated by the FTIR analysis and as can be depicted from Fig. 3 some
reactions have definitely taken place upon the alkali treatment of DPSS fibres, which
resulted in the partial decomposition of hemicellulose.
The treatment of DPSS fibres with alkali does not only attack the fibre constituents
but also effectively liberates them from surface impurities and fatty substances.
Accordingly, the content of surface pectin, waxes and impurities could be reduced
 674 I. Taha et al.
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Figure 2. Effect of alkalisation time on the FTIR spectra of DPSS.

Figure 3. Effect of alkali treatment on the chemical composition of DPSS.

from 21% in untreated fibres to 15% upon a 24 h treatment with a 2% concentrated

sodium hydroxide solution. It is expected that even such a humble modification
would lead to improved characteristics for composite materials. The removal of
surface impurities exposes new hydroxyl groups to the surface, hence increasing the
number of reactive sites available for reaction with other chemicals in case of further
treatment, or with the polymeric matrix in case of a direct integration process.
 Alkali treatment of date palm fibres 675

3.3. Water absorption

The effect of alkali treatment on the water absorption behaviour of DPSS fibres as
seen in Fig. 4 is very low. However, it can be depicted that the water absorption
of alkali treated fibres (between 11 and 12%) lies slightly below that of the
untreated ones (13.7%). Several citations state increased water absorption upon
alkalisation treatment [4, 13, 14]. However, Salgado-Delgado et al. [15] also
observed the reduced water uptake of alkali treated fibres, which was attributed
to the replacement of the hydrogen in the hydroxyl group by sodium. Ray et al.
[5] has observed an initial reduction of absorbed water in alkali treated fibres up to
a certain treatment time, after which a renewed increase in water uptake could be
recorded. Hence, the water absorption behaviour of natural fibres primarily depends
on the chemical composition and the amount available of each constituent. In this
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work it is assumed to have two competing forces. On the one hand, water uptake is
supposed to decrease as a result of the partial elimination of hemicellulose, which
is considered one of the main elements responsible for the hydrophilic behaviour
of natural fibres, due to its hydroxyl and other oxygen containing groups [16]. On
the other hand, water absorption is expected to increase since the efficient removal
of surface impurities exposes new hydroxyl groups available as reaction sites. In
addition, the breakage of hydrogen bonds between the hydroxyl groups of the
cellulose through alkalisation leads to the increased OH concentration [11], which
additionally enhances water uptake. As a result, no significant change in the water
uptake behaviour could be detected.
Consequently, at higher reaction times, the trend towards reduced fibre hy-
drophilicity is not warranted, since it is probably not predictable which compet-
ing effect would prevail. At low reaction times, it can be observed that the higher

Figure 4. Effect of sodium hydroxide concentration and reaction time on the water absorption
behaviour of DPSS.
 676 I. Taha et al.

sodium hydroxide concentrated solution (5%) results in water absorption values

slightly below these of higher concentration (2%).

3.4. Thermogravimetric analysis

Thermogravimetric measurements describing the thermal behaviour as illustrated
in Fig. 5 definitely show the improvement of the thermal behaviour of DPSS fibres
treated with NaOH. Generally the degradation behaviour of DPSS can be divided
into several steps. Between 100◦ C and 200◦ C, non-combustible products such
as carbon dioxide, traces of organic compounds and water vapour are developed.
The first degradation behaviour starts at 240◦ C due to the decomposition of
hemicellulose. Between 240 and 350◦ C the fibre loses over 50% of its initial weight.
The second stage is characterized by the start of cellulose degradation. Finally,
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around 22% by weight is lost at temperatures between 430 and 470◦ C leaving
behind ash and indigestible minerals. The last degradation behaviour is attributed
to the decomposition of non-cellulosic substances such as lignin and other high-
molecular weight residues. The remaining weight at stabilisation correlates with
the percentage of ash [17].
Comparing the behaviour of alkalised DPSS at different treatment times, it can be
observed that the first and second stages were shifted towards higher temperatures,
maintaining the same degradation rate. However, the degradation stage of the non-
cellulosic substances is found to take place at a higher rate, such that complete
thermal decomposition could still be observed at about 500◦ C. These findings

Figure 5. TGA curves of DPSS treated with 2% NaOH solution.

 Alkali treatment of date palm fibres 677
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Figure 6. DTG curves of DPSS treated with 2% NaOH solution.

can directly be obtained from the differential Thermogravimetric curves (DTG)

presented in Fig. 6.
According to Mohanty et al. [16], the thermal degradation of natural fibres is
known to take place in the order of hemicellulose, cellulose and finally lignin.
Hence, the shift in degradation temperatures of treated DPSS fibres can be attributed
to the effective removal of hemicellulose as suggested through FTIR measurements
and chemical analysis. This seems to be in agreement with the findings reported by
Sundquist, which state that the alkali treatment causes similar effects as heat treating
fibres for a certain period of time, resulting in the destruction of hemicellulose
and further extractives on the one hand, and the rearrangement of cellulose on
the other hand. Hence, the absence of hemicellulose shifts the TGA degradation
curve towards higher temperatures, since the lignocellulosic structure left behind
is composed of a greater amount of lignin: this has been reported to contribute
to char formation, which insulates and protects other components from thermal
decomposition. Identical observations have been made by Al-Khanbashi et al.
[18] for palm date mesh fibres, as well as for other plant fibres, such as sisal,
jute and hemp [19]. Similarly, Sreekala et al. [11] observed a rise in the initial
degradation temperature of NaOH treated oil palm fibres. The first decomposition
peak at 275◦ C was shifted towards temperatures about 350◦ C which he attributed
to the depolymerization of hemicellulose and the cleavage of glucosidic linkages of
cellulose. The final peak at 475◦ C can be explained by the development of charred
residues and the burning of high-molecular-weight residues.
 678 I. Taha et al.

According to Fig. 7, a comparable behaviour of DPSS treated with a 5% concen-

trated NaOH solution could be detected. The effect of the treatment concentration
on the thermal behaviour is illustrated in Fig. 8. It is obvious that an alkali treatment
of DPSS fibres generally causes a shift of the decomposition temperature towards
higher values. However, from Fig. 8 it can be concluded that the positive influence
of this treatment does not increase with increasing concentrations. At a solution
concentration of 5%, the initial degradation temperatures again fell back towards
lower values. Several researches report analogous observations. Mwaikambo and
Ansell [12] expect to find lower thermal stability at treatments above 8%, related to
the decrease in cellulose crystalline length and the increase in amorphous cellulose.

3.5. Mechanical properties

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Literature has cited several, also contradicting effects of alkali treatment on the
tensile properties of natural fibres. It is in this case legitimate to ascribe the varying
effects not only to the alkalisation conditions (time, temperature and concentration)
but also to the chemical composition of the fibre, its origin and its growth conditions.
Hence, it was necessary in this work to independently find the influence of alkali
treatment on DPSS and not to depend on previous work. However, the literature
references seem to agree, as also verified by the current work, that alkali treatment
of natural fibres increases their strength [18, 19]. The removal of surface impurities
and acids in addition to the partial dissolution of hemicellulose evokes structural
changes within the fibre, which leads to the formation of a lignin–cellulose complex
of higher strength [11]. Furthermore, Al-Khanbashi et al. [18] stated that alkalisa-
tion induces a decreased spiral angle of the cellulose microfibrils, which in turn
implies increased strength properties. Last but not least, the fibrillation process of
individual fibres leads to the formation of finer fibres of smaller diameter, which
enhances their mechanical behaviour [6]. Care must be taken not to carry the
fibrillation process to excess, since greater fibrillation leads to the increase of fibre
ends available for crack initiation within a composite.
As can be depicted from Fig. 9, alkali-treated DPSS indeed undergo an increase
in strength applying a 2% and 5% concentrated solution, respectively. However, it
is evident, as anticipated by various citations that this increase ends after a certain
period of reaction time and then decreases. Reaction time leading to highest tensile
strength has been found to lie between 2 h and 4 h. After 5 h of alkali treatment,
the tensile strength was in fact found to deteriorate, but was observed to remain
at a value of around 600 MPa, which still involves a 50% increase related to the
intrinsic value of 400 MPa. On the one hand, in the untreated fibre, hemicellulose
remains dispersed in the interfibrillar region separating the cellular chains from
one another, which causes them always to be in a state of strain. However, when
hemicellulose is removed by the action of alkali, the internal strain is released and
the fibrils become more capable of rearranging themselves compactly; this results in
a close packing of the cellular chains, which leads to higher tensile strength [4]. On
the other hand, the reduction in strength at extended alkalisation can be attributed
 Alkali treatment of date palm fibres 679
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Figure 7. TGA curves of DPSS treated with 5% NaOH solution.

Figure 8. TGA curves of DPSS treated for 2 h in 2% and 5% NaOH solution.

 680 I. Taha et al.
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Figure 9. Effect of alkalisation conditions on the tensile strength of DPSS.

to the dissolution of alkali soluble components [4, 13, 18] creating voids in the
fibre structure accompanied by a swelling behaviour, which results in a sharp drop
in linear density and in turn in mechanical properties. Al-Khanbashi et al. [18]
were able to observe notched grooves on the fibre surface that might be a reason
for the drop in fibre tensile properties at high alkali concentrations. Furthermore,
the open structure of the fibres, as described by the results of FTIR analysis cause
increased water absorption which is also a major factor in mechanical behaviour
[20].
Figures 10 and 11 illustrate the elongation at break and the tensile modulus of
alkali-treated DPSS under the above mentioned treatment conditions, respectively.
Against the anticipated behaviour given by [4], which suggests a more brittle
behaviour of alkali-treated fibres, the tensile strain of DPSS was found to follow
a similar trend as the change in tensile strength, giving rise to the strain at break up
to a limit of around 5% after a treatment time of 2–4 h, after which a stable value
higher than the original one, could be observed. This behaviour can be explained
by the removal of alkali soluble amorphous components, leaving behind the more
labile crystalline structure of the fibrous material.
The behaviour of Young’s modulus at different alkali concentrations seems to be
contradictory. Whereas a small increase was observed within the first couple of
treatment hours at higher concentration, followed by a reduction at higher treatment
times, the behaviour is the exact opposite for the low alkali concentration of 2%.
Although this behaviour is not comprehensive, some tentative explanations can be
made. First, according to the REM photos presented in previous work [17], raw
DPSS fibres involve silica particles that are to a large extent washed away through
 Alkali treatment of date palm fibres 681
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Figure 10. Effect of alkalisation conditions on the tensile strain of DPSS.

Figure 11. Effect of alkalisation conditions on the tensile modulus of DPSS.

the alkali treatment. It is conceivable that the removal of such impurities imparts
the fibre additional elasticity, which in turn implies the reduction in the modulus
of elasticity. Incorporating the above results and discussions, it is suggested that
the 2% concentrated solution is more efficient compared to 5%. Furthermore, the
removal of hemicellulose also affects the tensile modulus in two contradictory ways.
 682 I. Taha et al.

On the one hand, the extraction of hemicellulose reduces the fibre diameter, which
implies less required tensile force and reduced elastic modulus. On the other hand, it
is also this removal of hemicellulose that allows the fibrils to rearrange themselves
in a more compact manner leading to increased fibre strength and modulus [4].
However, if the rearrangement does not take place during the treatment process, the
fibrils would have to position themselves during tensile testing, which gives false
results of the Young’s modulus during the first tension stage. Hence, the measured
properties are the result of two competing actions within the fibre structure, and it
can probably not be foreseen which effect would predominate.

4. CONCLUSIONS
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Generally speaking, the alkali treatment of DPSS fibres showed positive potential
for a successful application of date palm fibres into polymeric matrices. The
changes in chemical composition upon alkalisation were ascertained by chemical
and FTIR analysis, revealing the complete removal of surface impurities in addition
to the partial elimination of hemicellulose. It was observed, as asserted by
other citations, that the lignin and cellulose components of the fibre remain
unchanged, and that the latter is the main influential element on mechanical
properties. However, the chemical changes imply structural alterations that lead to
modified physical and mechanical properties. Analysis revealed a reduced water
uptake of the lignocellulosic material, which is mainly related to the reduced
amount of hemicelluloses and which is known to be the main reason for high water
absorption characteristics. Similarly, the removal of fatty surface substances in
addition to hemicellulose improved the thermal behaviour of DPSS. These structural
changes within the fibre cell walls allowed for the rearrangement of the cellulosic
chains and hence for the elimination of voids and the consolidation of weak points
leading to improved tensile behaviour.
From this study it can be concluded that physical and mechanical properties are
not directly related to increased treatment conditions. Lignocellulosics have to
be considered as a complex system that is being affected by several competing
activities during the alkalisation process. For DPSS fibres it was found that the
optimum properties were achieved at relatively short treatment times of 2 h and 4 h
and alkali concentrations of 2% and 5% NaOH, respectively. For future research
on the development of DPSS-reinforced polymer composites, these conditions will
provide a basis for ensuing modifications.
It is intended to continue work on the surface modification of palm fibres, and to
conduct further analysis for the better understanding of their structural behaviour.
Finally, it is the aim of this work to process palm fibre composite materials with
various thermoplastics and to examine their physical and mechanical behaviour and
thence their adequacy and applicability as construction materials.
 Alkali treatment of date palm fibres 683

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