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upgrade fiber quality. The authors found that fractionation prehydrolysis, pressure was released and the digester was
was effective in upgrading the long-fiber component, thus cooled by circulating cold water. Samples were then
increasing the strength indices of paper. Duan et al (2017) collected from the drained off liquor for pH, solid content,
fractionated kraft-based dissolving pulp and treated with lignin and sugars determination. The percentage of
cellulase and found that short fiber fraction had the highest dissolved components was measured gravimetrically.
accessibility, lowest viscosity, and highest cellulase
adsorption capacity, while the opposite was true for the Cooking
long fiber fraction. Duan et al (2016) also studied on a Prehydrolysed jute fibers were cooked in the same
combined process consisting of mechanical refining (R) digester. The following parameters were kept constant in
followed by a low-alkali (5.5% NaOH) cold caustic the kraft process:
extraction (CCE) and finally an endoglucanase (EG) -Active alkali charge was 18 % as Na2O on o.d.
treatment (R-5.5% CCE-EG) was investigated for prehydrolysed jute fiber (sulphidity was 25%).
upgrading paper-grade pulp to dissolving pulp. Results -Liquor to fiber ratio was 6:1.
showed that compared to the conventional process -Temperature was 170ºC. Time required to raise
(9%CCE-EG), the modified process can decrease the temperature was 45 min.
alkali concentration (from 9%to 5.5%) to achieve a similar -Cooking time was 120 min at 170ºC.
hemicelluloses removal while simultaneously enhancing After digestion, pulp was washed till free from residual
the Fock reactivity (from 62.2% to 81.0%). chemicals, and screened on flat vibratory screener
Organic acid dissolves lignin and hemicelluloses from (Yasuda, Japan). The screened pulp yield, total pulp yield
lignocellulosic raw material simultaneously. Thus, pulping and screened reject were determined gravimetrically as
with organic acid may be an alternative process for percentage of o.d. raw material. The kappa number of the
dissolving pulp from jute (Jahan et al 2006, 2007). The resulting screened pulp was determined in accordance with
pulping operation can be carried out at atmospheric Tappi Test Methods (T 236 om-99).
pressure. Acid used in pulping can be easily recovered by Bleaching
distillation and reused in the process (Muurinen 2000). Produced pulp was bleached by D0EpD1 bleaching
Organic acid lignin is characterized with higher phenolic sequence. The ClO2 charge was 1% and temperature was
group compared to proto lignin (Islam, Sarkanen 1993, 70 °C for 45 min in the D0 stage. The pH was adjusted to
Jahan et al 2007) and can be used for many value added 2.5 by adding dilute H2SO4. Alkaline extraction was
products due to its lower molecular weight and higher carried out with 2% NaOH and 0.5%, H2O2 charge,
reactivity (Kubo et al 1998, Nihat et al 2002). The spent temperature was 70ºC for 120 min. In the D1 stage, ClO2
liquor lignin can be used for producing carbon fibers charge were 0.5, pH was adjusted to 4.5 in D1 stage,
(Kadla et al 2002). In this process residual pentosan respectively adding dilute alkali. The pulp consistency was
content in the pulp was very low due to the dissolution of 10% in all stages.
most of the hemicelluloses (Jahan et al 2007). The
dissolved hemicelluloses can be converted to chemicals Pulp fractionation
and fuels (Liu et al., 2013; Tanifuji et al., 2013). Fractionation was carried out with a Bauer-McNett fiber
A number of studies have been carried out on dissolving classifier according to Tappi T233 cm-95 standards. Pulp
pulp from jute in our group (Jahan et al 2007, 2008, 2008a, fibers that were retained on the 50-mesh screen were the
Jahan 2009, Matin et al 2015). In this investigation, an long fiber (LF), the fibers passing through 50-mesh screen
effort was made to produce high purity dissolving pulp but retained on the 100-mesh screen were the middle fiber
from jute fiber with improved reactivity. The objectives of (MF), while the short fiber (SF) was defined as those fibers
this investigation were to fractionation of prehydrolysed that passed through the 100-mesh screen.
kraft pulp from jute, followed by PFI refining and caustic
Evaluation of pulps
extraction to improve the hemicelluloses removal and
Pulp tests were performed according to the Standard
reactivity. A dissolving pulp was also produced from jute
Methods of the Technical Association of the Pulp and
fiber by formic acid process (FA) followed by caustic
Paper Industry (TAPPI, Atlanta, GA): brightness (T 452
extraction. A mass balance was also done in FA process to
om-92); viscosity (T 230 om-89); -cellulose (T 203 om-
integrate the process in biorefinery.
88); and alkali solubility S10 and S18 (T 235 cm-85). Alpha-
Material and methods cellulose is the pulp fraction resistant to a treatment in an
aqueous solution containing 17.5% sodium hydroxide and
Materials indicates undegraded, high molecular weight cellulose
Jute (Corchorus capsularis) was collected from content in pulp. Alkali solubilities S10 and S18 provide
Bangladesh Jute Research Institute and all scales were information on the low molecular weight carbohydrates
removed by hand and cut to 2-3 cm length in hand (degraded cellulose and hemicellulose) in pulp. A 10%
chopping machine. sodium hydroxide solution dissolves both degraded
cellulose and hemicellulose (S10) whereas hemicellulose is
Prehydrolysis soluble in an 18% sodium hydroxide solution (S18)
Jute was prehydrolysed by water in 20 L capacity digester. (Christov et al 1996). R10 and R18 were obtained by
Prehydrolysis was carried out at 170ºC for 60 min. The jute subtracting S10 and S18 from 100. R18-R10, or S10-S18 can be
to liquor ratio was 1: 6. The time required to raise to an indication of the dissolved low-molecular-weight
maximum temperature was 50 min. After completing cellulose content. The Fock reactivity of the produced pulp
was determined by modified method, which is described content did not vary significantly between short and long
by Tian et al. (Tian et al., 2013a). The sodium hydroxide fiber fractions. It was expected that pentosan in short fiber
concentration, xanthation temperature, xanthation time, fraction would be higher as most of the hemicelluloses
and carbon disulfide dosage were 9%, 19ºC, 3 h, and 1.3 present vessel, fines and short fibers in wood pulp (Duan
mL, respectively. All pulp properties were analyzed in et al., 2017). But jute is a bast fiber, which is composed of
duplicate. fiber only. Therefore, pentosan content in jute pulp
behaves differently. The α–cellulose content in long fiber
Formic acid pulping of jute fraction was 1.1% higher than the short fiber fraction. But
The jute fiber was refluxed with 84% formic acid water the effect was not pronounced as in wood pulp (Li et al.,
mixture in a hotplate under the following different 2015a). The degraded cellulose (R18-R10) in whole pulp
conditions: was 2%, while the same was 0.8% in long fiber fraction.
-Reaction time: 4 h at boiling 107ºC.
-Material to liquor ratio: 1:8. Alkaline extraction
After desired reaction time, pulp was filtered in a Table 2 shows the effect of alkaline extraction on the purity
buckner funnel and washed with fresh formic acid- water and reactivity of dissolving pulp. The residual pentosan in
followed by hot distilled water. Then the pulp yield was long fiber fractions pulp was 2.2% and 2.0% after alkaline
determined gravimetrically and kappa number (T 236 om extraction at 25ºC and 90ºC, respectively (Table 3) which
99) and pentosan (T223cm01) were determined according corresponds to 35.4% and 41.5% pentosan removal from
to Tappi Test Methods. Formic acid pulp was bleached by the original dissolving pulp. Pentosan removal certainly
conventional D0EpD1 bleaching sequences. increased α-cellulose content in the pulp. The purity of the
alkaline extracted dissolving pulp increased to 96% for
Alkaline extraction long and medium fiber fractions. But the purity of short
Alkaline extraction of prehydrolysed kraft bleached and fiber fraction was only 95%, where α-cellulose content
formic acid (FA) bleached pulps was carried out with 8 % increased by 0.6% and 0.77% after alkaline extraction at
sodium hydroxide at 25ºC and 90ºC for 2h. FA pulp prior 25ºC and 90ºC, respectively. This result is consistence
to bleaching was alkaline extracted at 25ºC for 2 h. The with hemicelluloses removal data (26.2% and 32.9%).
consistency was 10%. After extraction, pulp was filtered After alkaline extraction at room temperature Fock’s
in a buckner funnel and washed with fresh distilled water. reactivity increased to 74.8% from 43.7% and to 77.4% for
The pulp yield was determined gravimetrically and long fiber fraction and from 73.3% for short fiber fraction
pentosan content (T223cm01) was determined by with the reduction of hemicelluloses. With the increase of
following Tappi Test Methods. alkaline extraction temperature, Fock reactivity further
increased, which was consistent with the hemicelluloses
Results and discussion reduction data.
The objective of this study was to prepare high purity
dissolving pulp from jute. To this end, the pulp obtained
was fractionated into long and short fibers followed by Table 1 - Dissolving pulp properties of fractionated pulp from
cold and hot alkali extraction with and without PFI refining jute in prehydrolysis kraft process.
of fractionated pulps. Table 1 shows dissolving pulp Whole Long Medium Short
properties of whole pulp and fractionated pulp. Our target pulp fibres fibres fibres
was to get high purity and high reactivity dissolving pulp. Pentosan (%) 3.4 3.4 3.3 3.1
It is clear from Table 1 that Fock reactivity increased with Fock reactivity (%) 49.4 43.7 60.3 73.3
decreasing fiber size. The reactivity of long fiber fraction R10(%) 92.9 94.8 92.3 91.8
was only 43.7% which increased to 73.3% with short fiber R18 (%) 94.9 95.6 94.8 94.8
fraction. Short fiber fraction contained mainly fragmented α-Cellulose (%) 94.6 95.6 94.6 94.5
fiber; consequently, increased surface area and exposed Viscosity (mPa.s) 9.2 9.4 9.3 7.1
cellulose surface for reaction.
As shown in Table 1, α–cellulose content in long fiber
fraction was higher than short fiber fraction. Pentosan
Table 2- Alkaline extraction dissolving pulp from jute.
Long fibres Medium fibres Short fibres
Temperature (ºC) 25 90 25 90 25 90
Yield (%) 98.3 97.0 98.0 97.3 97.4 97.1
Pentosan (%) 2.2 2.0 2.2 2.1 2.3 2.1
Fock reactivity (%) 74. 8 76.2 78.9 87.9 77.4 89.3
R10(%) 97.8 97.7 97.8 97.8 96.4 97.4
R18(%) 97.6 97.8 97.4 97.7 96.9 97.6
α-Cellulose (%) 96.5 96.4 96.1 96.3 95.1 95.3
Viscosity (mPa.s) 8.0 7.89 8.5 7.3 7.3 7.0
Table 3 - Effect of refining on dissolving pulp properties of fractionated pulp from jute.
Content Long fibres Medium fibres Short fibres
Temperature (ºC) 25 90 25 90 25 90
Refining and alkaline extraction result indicates that residual hemicelluloses are mainly
Table 2 shows the effect of refining on the alkaline responsible for reactivity. Short fiber fraction showed
extraction of the fractionated pulp. Hemicellulose removal higher reactivity than long fiber fraction. This result
from short fiber fraction was better than long fiber fraction. complied with the reported data (Tian et al 2014).
Mechanical refining followed by alkaline extraction
Organic acid pulping of jute
decreased pentosan content by 0.86% with long fiber,
Organic acid pulping process dissolves both lignin and
while the same declined by 1.26% for short fiber fraction
hemicelluloses simultaneously from the lignocelluloses,
at 25ºC (Tablse 1 and 3). But the pentosan removal in
which lower down residual pentosan content in the pulp
alkaline extraction at 90ºC was more pronounced than at
(Jahan et al., 2007). Therefore, formic acid process was
25ºC. At the 90ºC, pentosan removal was 1.66% and
evaluated for producing high purity dissolving pulp
1.75% for long and short fiber fractions, respectively.
production. Formic acid (FA) treatment produced of pulp
Arnoul-Jarriault et al (2015) attempted to convert
of 58.8% yield with kappa number 23.1, which was
softwood kraft pulp (paper grade) into dissolving grade
subsequently alkaline extracted with 8% alkali at 25ºC to
pulp by cold caustic extraction process (CCE) under the
produce dissolving pulp (data are not shown). The alkaline
conditions of NaOH charge, 3 to 12% and temperature,
extracted pulp was bleached by D0EpD1 sequences. As
25ºC to 110°C. The results showed that NaOH
shown in Table 4, α-cellulose content in bleached FA pulp
concentration had a predominant effect on xylan and
was 94.3%, which increased to 97.4% after alkaline
glucomannan removal. The best removal was observed
extraction at 25ºC. The α-cellulose content did not increase
below 40ºC or above 80ºC. Our results agree with the
with the increase of alkaline extraction temperature. It is
experimental data obtained by Arnoul-Jarriault et al
well established that cold caustic extraction effectively
(2015).
removed hemicelluloses from the pulp provided that alkali
As shown in Table 2, α-cellulose content increased in all
concentration is high (Sixta 2006). Li et al (2015) showed
pulps after alkaline extraction because of removal of
that the combined mechanical refining and CCE at 4%
hemicelluloses. The increase in α-cellulose content after
NaOH led to a decrease in the hemicellulose content from
refining followed by extraction at 25ºC was higher than the
9.5% to 5%, which was comparable with the CCE with 8%
alkaline extraction at 90ºC. The α-cellulose content
NaOH where of hemicelluloses content decreased from
increased by 2.22% and 0.67% for long fiber fraction and
9.5% to 4.6%. Also it was observed in previous section that
1.55% and 1.34% for short fiber fraction after alkaline
refining followed by CCE did not improved purity of
extraction at 25ºC and 90ºC, respectively. According to
dissolving pulp from jute. Therefore, FA pulp was not
pentosan removal results, α-cellulose content in pulp after
refined prior to CCE. Alkaline extraction at 25o and 90ºC
alkaline extraction at 90 ºC was supposed to be higher,
removed 30.1% and 51% pentosan, respectively, from the
though, according to the results of Table 2, the values were
original pentosan content of 3.56% in bleached FA pulp.
similar. This can be explained by degradation of α-
As shown in Table 4, the ‘‘R18-R10,’’ value in CCE FA
cellulose during alkaline extraction at higher temperature,
pulp was 1.3% which was equal to untreated FA pulp. This
which is evident from viscosity data (Table 3). There was
indicated that CCE with 8% NaOH did not degrade the
no direct relation found on fiber fractionation. This can
dissolving pulp. But alkaline extraction at 90ºC increased
also be explained by R10 and R18 results. The degraded
degraded cellulose to 1.8%.
cellulose R18-R10 in all fractionated pulps was higher with
alkaline extraction at 90ºC than at 25ºC. As for example,
Table 4 - Alkaline extraction of dissolving pulp from jute by formic
degraded cellulose in long fiber fractions was 1.06% at
acid process.
25ºC and 1.56% at 90ºC (Table 3).
Fock’s reactivity increased to 73% with long fiber Properties Formic Alkaline extraction,
fraction and 75.32% with short fiber fraction at 25ºC on acid temperature (ºC)
refining followed by alkaline extraction. With the increase pulp 25 90
of alkaline extraction temperature, Fock reactivity further Pentosan (%) 3.6 2.5 1.7
increased, which was consistent with the hemicelluloses R10 (%) 93.7 96.5 96.0
reduction data. Zhao et al (2017) showed that xylanase R18(%) 95.0 97. 8 97.8
treatment improved Fock reactivity from 21.6% to α-cellulose (%) 94.3 97.4 97.7
31.77%, which further increased to 32.42% by the Fock reactivity (%) 63.2 72.4 73.4
sequential refining followed by xylanase treatment. This
Fig 1 - Proposed biorefinery in dissolving pulp production process from jute by formic acid treatment
25ºC increased pulp purity to 97.4% and reactivity to caddis. Bangladesh Journal of Scientific and Industrial
72.4%. Therefore, it can be concluded that FA process Research, 42(4), 425-434.
with CCE is suitable for producing high purity dissolving Jahan, M. S. (2009): Studies on the effect of prehydrolysis and
pulp from jute. The FA process also fractionates lignin and amine in cooking liquor on producing dissolving pulp from jute
hemicelluloses for biofuel, biochemicals and biomaterials, (Corchorus capsularis). Wood science and technology, 43(3-4),
which adds value and compensate price of jute. 213-224.
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