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C for
10min with a solid to liquor ratio (S:L) of 1:8(w/w), and that mass removal increased with extraction time
and temperature. The hemicelluloses removal reached 65.5% at 170
C with hold times of 10, 20 and 30min after the set tem-
perature was reached. The solid to liquor (S:L) ratio was xed at
1:8 (by weight) and held constant in all experiments. At the end of
treatment, the solidresidue was recoveredby ltrationandwashed
with distilled water. The solid fraction was used for soda pulping
process.
The severity factor was used to describe the synergic effect of
time and temperature of treatment on extraction results as well
as for comparison with the obtained results in the other studies.
It calculated by means of Eq. (1) in which T representing reaction
temperature (
C), T
r
is a reference temperature and is an empir-
ical parameter related to activation energy and temperature, and
t is reaction time (min). According to literature for autohydrolysis
process of lignocellulosic materials at a constant temperature, the
reference temperature and are 100
C and 14.75
C, respectively
(Ligero et al., 2011; Wang et al., 2011).
Severity factor = Log
10
t exp
T T
r
(1)
Y. Hamzeh et al. / Industrial Crops and Products 43 (2013) 365371 367
2.2.3. Holocellulose determination
Holocellulose was measured following the procedure origi-
nally pioneered by Zobel and McElwee (1966). The carbohydrate
(holocellulose) fraction of the pre-extracted samples was isolated
by removing the lignin from the sample using the acid chlorite
method. Air-dried ber (2.5g) was placed into an Erlenmeyer ask,
and a quantity of stock solution A (made fromacetic acid (0.5mL),
NaClO
2
(1g) and distilled water (80mL)) was added. The ask was
placed in a hot-water bath (702
C for 60min
and the pulp consistency was 10%. In the D
1
stage, the end pH was
xed at 4. The ClO
2
charge in the D
1
was 0.5% at a temperature of
80
C for
10min, which resulted in a moderate (60.6%) removal of hemicel-
luloses, was selected for pulping and bleaching study.
3.3. Pulping process
For the current study, the main aim of pulping is to produce
bleached pulp frombagasse bers that will upgrade the economic
value of the process. The results of studies on soda pulping of pre-
extracted and un-extracted (control) of bagasse conducted during
this investigation are given in Table 3. The cook at 11% active alkali
gave pulps that had a high Kappa number, and contained too much
uncooked material that was difcult to disintegrate into bers, so
it was not possible to make handsheets from them. Hence, the
amount of active alkali was chosen at 14%. Analysis of pulps pre-
paredusing14%activealkali showedthat either ligninprecipitation
had occurred, and/or lignin within the ber walls had not been
sufciently removed, as indicated by the high Kappa number. To
obtain bleachable-grade bagasse soda pulps, the charge of active
alkali used had to be increased. With increasing the active alkali
charge from 11% to 17%, the Kappa number decreased, screened
yield increased and screened rejects decreased. An increase in the
active alkali above 17% generally led to limited improvements in
the screened pulp yield and Kappa number. Kraft pulping with 17%
active alkali was sufcient to ensure almost complete elimination
of non-cellulosic matter.
Table 3 also shows the effect of pre-extraction on the soda pulp-
ing of bagasse. It is seen that the pre-extraction of bagasse resulted
in lower Kappa number of pulp for the control samples with con-
siderable lowering of pulp reject. Similar results were observed for
hot-water pre-extraction of bagasse followed by alkaline pulping
(Jahan et al., 2009). In the previous studies, a higher pulp viscos-
ity fromextracted bagasse than that fromuntreated bagasse have
been reported that attributed to the removal of hemicelluloses
Fig. 1. Effects of severity factor on the extraction yield and extraction (extraction
yield: , current study; , Lei et al. (2010); , Jahan et al. (2009) and extraction
liquid pH: , current study; , Lei et al. (2010); , Jahan et al. (2009)).
Y. Hamzeh et al. / Industrial Crops and Products 43 (2013) 365371 369
Table 3
Laboratory soda pulping results for pre-extracted and control bagasse samples.
Properties 11% active alkali 14% active alkali 17% active alkali
Extracted Control Extracted Control Extracted Control
Overall yield, %
a
52.5 45.1 53.9 43.3 56.9 51.1
Screen yield, % 45.3 34.5 46.6 40.6 56.9 51.1
Reject, % 6.3 10.6 3.2 2.5 0.0 0.0
Kappa no. 40 54 26.6 28.4 18.6 19.3
a
Based on OD bagasse.
and higher ratio of cellulose to hemicelluloses in extracted bag-
gase (Jahan et al., 2009; Lei et al., 2010). Hemicelluloses compared
to cellulose have high accessibility to acidic or alkaline hydrol-
ysis. This is due to their amorphous structure and much lower
degree of polymerization. During the pre-hydrolysis, some hemi-
celluloses and lignin were removed and delignication was thus
improved. The extracted bagasse had a more open structure due
to the hemicelluloses and lignin removal (Jahan et al., 2012). After
pre-hydrolysis, lignin migrated to the surface of bagasse. There-
fore the delignication was faster for pulping of extracted samples.
So, pulping of extracted bagasse yielded a lower Kappa number
even with lower alkali charge. In general, the total pulp yield and
Kappa number decreased with increasing alkali charge and bleach-
able grade pulp obtained from both un-extracted and extracted
bagasse at 17% alkali charge, thus these pulps chosen for bleaching
study.
3.4. Bleaching and unrened pulp properties
As mentioned earlier, the main objective of this part of the
study was to evaluate the effect of pre-extraction on the brightness
of pulps using an ECF bleaching method. In general, the bright-
ness of the extracted bagasse pulps was higher than those of
un-extracted ones due to lower hemicelluloses contents. It is an
important observation because it provides another advantage over
un-extracted pulp. After bleaching, the overall pulp yield, on the
basis of original material, became narrower between pre-extracted
and un-extracted bagasse. In addition, it was found that the pre-
extracted pulps could be easily bleached to 87.5% ISObrightness by
a D
0
ED
1
sequence.
In general, mechanical properties of pre-extracted pulps were
decreased. It is seen that the tensile and burst indices of pre-
extracted pulps were lower than un-extracted ones. However, no
differences in tear index were observed (Table 4), indicating that
the ber strength remains unaffected, but the inter-ber bonding
decreases with extraction. A similar phenomenon reported in sev-
eral studies and attributed to the removal of hemicelluloses from
the pre-hydrolyzed rawmaterials (Sousa et al., 2007; Duarte et al.,
2011). The extraction of hemicelluloses fromlignocellulosic mate-
rials prior to pulping decreases the berber bonding capacity,
Table 4
Results of D
0
ED
1
bleaching of obtained soda pulps from pre-extracted and control
bagasse.
Properties Extracted Control
Initial Kappa no. 18.6 19.3
Total ClO
2
charge, % 2.5 2.5
Brightness, % 87.5 86.2
Bleaching yield, % 95.0 93.2
Overall yield, %
a
56.9 51.1
Tensile index, Nm/g 42.46 49.33
Tear index, mNm
2
/g 4.14 4.06
Burst index, kPa m
2
/g 2.62 2.78
a
Based on OD bagasse.
consequently lowering the Scott bond, tensile and burst indices of
paper (Jahan et al., 2009).
3.5. Effect of dry strength additives on mechanical properties
Data on mechanical properties of papers made fromun-treated
and treated pulps by adding diluted acidic chitosan solution and
cationic starch solution to the pulp suspension are presented
in Fig. 2. The improvement effects of used dry-strength addi-
tives were higher for pre-extracted bagasse. When high amount
of dry-strength additives employed, no signicant differences in
mechanical properties observed between extracted and control
samples. Duarte et al. (2011) investigated the effect of surface com-
position on the bers total surface charge and zeta potential using
a Mtek SZP 06. They observed that a change in hemicelluloses
content (achieved by modied pulping) from 20% to 15% did not
affect the zeta potential. Therefore, the surface absorption of pre-
extracted bers is as well as control. In other words, pre-extracted
bers can absorb same amount of dry-strength additives.
The results demonstrate that the addition of chitosan can con-
siderably increase mechanical properties. Chitosan application has
a uniqueeffect onthemechanical properties; for instance, at 1%chi-
tosan, the increases intensile andburst indices were about 27.5and
13.3% more than the control (Fig. 2a). A similar trend was observed
for treated paper with cationic starch. However, the increase less
than 1% was low. This indicates that chitosan should be used based
on end-product quality requirements and the cost effectiveness of
the process. However, all mechanical properties increased when
Fig. 2. Effects of dry-strength additives on the mechanical properties of pre-
extracted and control handsheets.
370 Y. Hamzeh et al. / Industrial Crops and Products 43 (2013) 365371
the chitosan was added to furnish. But, the effect of chitosan on
the properties of handsheets under pre-extraction condition was
better than un-extracted condition (Fig. 2b). This indicates that the
un-extracted condition is less suitable than the extracted method
when chitosan and cationic starch are used presumably, due to
higher porosity of extracted pulps increasing adsorption of dry-
strength additives on the ber surfaces (Kontturi et al., 2008).
Dry-strength additives have positive effects on the mechanical
properties through improving inter-ber bonding. The added chi-
tosan molecules were supposed to act as crosslinkers by binding to
neighboring cellulose bers. It was also suggested that the inter-
action of chitosan with the ber would lead to a further increase
in berber bonding due to the explicit polycationic character
of the chitosan. Once binding and crosslinking between bers has
occurred, the yet unbound parts of the chitosan molecule have the
required geometry to enhance more hydrogen bonding. As a result,
the chitosan would attach itself to larger segments of the cellu-
lose ber and tend to shorten the distance between the individual
cellulose bers (Ashori et al., 2005). Fig. 3 is an idealized represen-
tation of the cellulosic berchitosan system, showing the bonding
between two cellulose molecules and two chitosan molecules. In
addition, it is reportedthat there is anincrease inthe surface rough-
ness as extraction takes place, which is reected in the increase
of the kink index. So, extracted bers may absorb more additives
compared with control ones (Sousa et al., 2007; Lei et al., 2010;
Duarte et al., 2011).
Fig. 4 shows the mechanical properties of handsheets produced
by the mixtures of chitosan and cationic starch. The data demon-
strate that the additionof cationic starchinthe concentrationrange
0.51.5% increases both mechanical properties of the handsheets
(Fig. 4a). At 0.5% cationic starch and chitosan, the increase in burst
index was 3.5 and 5%respectively compared to the control (Fig. 4b).
As in the case of chitosan, the effect was higher when the dosage
Fig. 3. Idealized representation of bond formation in the cellulosic berchitosan
bonding system.
of polymer was higher. The increase in mechanical properties was
signicantly lower than chitosan sized papers.
4. Conclusions
The main goal of current work was to evaluate the viabil-
ity of the integrated pulp mill biorenery concept. Based on the
experimental results the optimized conditions for hot-water pre-
extraction of bagasse were found to be: maximum temperature
170