Feasibility of incorporating treated lignins in berboards made

from agricultural waste

Camilo Mancera
a
, Nour-Eddine El Mansouri
b,
, Mara Angels Pelach
b
, Ferrando Francesc
a
, Joan Salvad
c
a
Rovira i Virgili University, Department of Mechanical Engineering, Avinguda dels Pasos Catalans, 26, 43007 Tarragona (Catalonia), Spain
b
LEPAMAP Group, Department of Chemical Engineering, Universitat de Girona, Campus Montilivi, Girona 17071, Spain
c
Catalonia Institute for Energy Research, Bioenergy and Biofuels Division, C/Marcell Domingo, 2, 43007 Tarragona, Spain
a r t i c l e i n f o
Article history:
Received 1 December 2011
Accepted 10 May 2012
Available online 15 June 2012
Keywords:
Fiberboard
Biocomposites
Lignin
Agricultural waste
Natural adhesives
a b s t r a c t
This paper studies the feasibility of incorporating treated lignins in berboards made from Vitis vinifera as
an agricultural waste. The treated lignins are the puried Kraft lignin and the alkaline hydrolyzed Kraft
lignin. V. vinifera raw material and its bers were characterized in terms of chemical composition and the
results were compared to other biomass species. The chemical composition of treated lignins shows that
they have high purity compared to the lignin raw material. The lignin-V. vinifera breboards were pro-
duced on laboratory scale by adding powdered treated lignins to the material that had previously been
steam exploded. Some of the important properties of breboards prepared using the treated lignins as
natural adhesives were evaluated. These properties were density, thickness swelling, water absorption,
modulus of elasticity, modulus of rupture, internal bond strength. The explored levels of treated lignins
vary from 5% to 20%. The results showed that binderless breboards, breboards made from V. vinifera
bers and alkaline hydrolyzed Kraft lignin have weaker mechanical properties. However, the breboards
obtained using puried Kraft lignin have good mechanical and water resistance properties which satisfy
the requirements of the relevant standards specications.
2012 Elsevier Ltd. All rights reserved.
1. Introduction
Fiberboard, a structural and decorative material, is a brous-fel-
ted, homogeneous panel made from lignocellulosic bers that are
combined with a synthetic resin or other suitable bonding system
and then bonded together under heat and pressure (ANSI Stan-
dards, 1994). It is one of the primary products used in the manufac-
ture of value-added wood products.
The growing global population has increased the demand for
various wood products and especially wood panels, leading to a
continuous effort to nd new resources as an alternative to forest
wood. Among these resources, the lignocellulosic materials from
agricultural waste have received considerable attention in the lit-
erature (Seber and Lloyd, 1996; Hague et al., 1998). Vitis vinifera
is the source of one of the most abundant agricultural waste prod-
ucts in Spain. It is a traditional crop cultivated for its fruit and the
production of wine and covers large areas of land. After the prun-
ing season, a large quantity of lignocellulosic material remains in
the elds every year. The average pruning yield per hectare is
about ve tons and there are currently approximately
1,200,000 hectares of grapevines cultivated per year in Spain (Nta-
los and Grigoriou, 2002). Part of the pruning waste is used as fuel,
but large quantities remain unused in the elds, thus increasing
the risks of infestations and re. At present, there are no special
industrial applications derived from the use of V. vinifera bers.
However, the suitability of vine pruning material for particleboard
production using urea formaldehyde resin as a binder has been ex-
plored (Ntalos and Grigoriou, 2002). In addition, different renew-
able biomass, including wheat and soybean straw, were used to
produce medium density berboard (Ye et al., 2007). The results
obtained results compared to berboards made from conventional
softwood bers showed that berboards made from renewable
biomass had weaker mechanical and water resistance properties
than those made from softwood ber. Therefore, V. vinifera can
be considered a potential lignocellulosic agricultural waste product
that could replace wood as a ber source in the production of
berboard.
Since the 1970s, researchers have been studying various ways
of using different kinds of lignocellulosic waste material for ber-
board production. Steam explosion is one of the best ways of pre-
treating lignocellulosic materials for use in the production of
boards and composites because it preserves the ber structure
and separates the lignocellulosic material into its main compo-
nents (Angles et al., 2001). In addition, lignin can easily exude from
the cell wall to the ber surface, and the bers are well separated
during steam explosion treatment (Angles et al., 1999). The ther-
moplastic property of lignin is an important factor in promoting
0956-053X/$ - see front matter 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.wasman.2012.05.019

Corresponding author. Tel.: +34 972 418 456; fax: +34 972 418 399.
E-mail address: nour_eddine.elmansouri@udg.edu (N.-E. El Mansouri).
Waste Management 32 (2012) 19621967
Contents lists available at SciVerse ScienceDirect
Waste Management
j our nal homepage: www. el sevi er. com/ l ocat e/ wasman
the thermal adhesion of the berboard pulp, from which the board
is formed by means of hot pressing (Shao et al., 2009).
Due to the important role of lignin in this kind of board, several
tests have already been conducted (Angles et al., 2001; Velasquez
et al., 2003) to analyze the effects of replacing ber with different
kinds of technical lignins as recovered directly from the pulping li-
quor without further purication or treatment. The best results of
these types of studies were obtained with Kraft lignin, which is a
by-product of sulfate-cooking wood chips. Kraft lignin is mainly
used as a fuel and only a small amount (12%) made available by
the pulp and paper (P&P) industry is commercially used in a wide
range of products. One important application of lignin as a raw
material is as an adhesive for boards in the absence of conventional
phenol formaldehyde or urea formaldehyde resins. Therefore, the
replacement of these synthetic resins is also an important objective
in the sustainability of berboards.
This paper explores the feasibility of incorporating treated lig-
nins as natural adhesives in binderless berboards made from V.
vinifera as an agricultural waste. It deals with the effects of the
addition of treated lignins on the physico-mechanical properties
of V. vinifera berboards.
2. Materials and methods
2.1. Materials
The lignin raw material used in this work was a softwood-
derived Kraft lignin purchased from Ligno-Tech Iberica. The puri-
ed Kraft lignin (PKL) was prepared according to the method re-
ported by Lin (1992). The lignin raw material was treated with
(1%) sulfuric acid several times and washed extensively with hot
water. The alkaline hydrolyzed Kraft lignin (AHKL) was prepared
by its reaction with 2% (wt/wt) sodium hydroxide at 170 C for
90 min according to the optimized conditions reported by Mancera
et al. (2011). The ratio of lignin to sodium hydroxide was xed at
1:10 (wt/wt) and the solid lignin was recovered by precipitation
after lowering the pH of the mixture to 2 and ltration. After dry-
ing the lignin samples at room temperature they were stored in
plastic bags for use as a natural phenolic adhesive in V. vinifera
berboards.
2.2. Fiberboards production
V. vinifera branches came from a plantation in Tarragona, Spain.
They were air-dried and stored in jute bags. The branches were
chipped into splinters smaller than 5 cm using a GA100 Black &
Decker shredder. The chips (200 g dry basis per batch) were sub-
jected to a steam explosion pretreatment in an 8 L digester (see
Fig. 1). The sample was steam exploded at a steam temperature
of 218 C and a pretreatment time of 6 min. The material was rap-
idly depressurized in a 100 L vessel, which helped it to debrillate.
The pulps were ltered and washed with water. The air-dried
steam-exploded pulps were ground and passed through a 4 mm
sieve in a Retest cutting mill. This procedure increased the bonding
area, thus improving the internal bond (Velasquez et al., 2002).
The ground-pretreated material was air dried to 7% moisture
content and mixed with lignin samples in different proportions
(5%, 10%, 15%, and 20%). The testing boards were shaped from
the previous mixture by hand using a forming box (150 mm in
length and 50 mm in width). Boards were prepared with a target
thickness of 3.0 mm. After the material was placed in the mold, it
was hot pressed in a three-stage cycle (Angles et al., 1999). The
used hot press was a Polystat 300 S type build by Schwabenthan
in Berlin. The three stages involving: (1) pressing at temperature
of 205 C and pressure of 12 MPa for 4 min, (2) a breathing period
or pressure relaxation for 1 min, and (3) pressing at temperature of
205 C and pressure of 12 MPa for 5 min.
2.3. Physical and mechanical characterization
The boards were characterized using European standards. The
mechanical properties measured were: internal bond (IB) (EN319,
1993), modulus of elasticity (MOE), and modulus of rupture
(MOR) (EN310, 1993). Dimensional stability was characterized by
measuring: thickness swelling (TS), and water absorption (WA)
(EN317, 1993). Additionally, the density of the boards was deter-
mined (EN323, 1993). Boards were conditioned at 20 C and 65%
RH before any physical or mechanical tests were conducted, and
the dimensions of the test pieces were determined on the basis of
the EN325 standard (EN325, 1993).
2.4. Chemical characterization
The chemical composition of raw materials (lignin and V. vinif-
era), treated lignins and ber were determined according to ASTM
standard methods. The chemical properties analyzed were mois-
ture content (ASTM E871-82, 2006), ash content (ASTM D1102-
84, 2001), and Klason lignin (KL) (ASTM D1106-96, 2007). The
carbohydrates from the Klason lignin hydrolysis test were ana-
lyzed using HPLC (Yuan and Chen, 1999) to determine cellulose
and hemicellulose content. Acid-soluble lignin (ASL) was also
determined using the UV absorption method (Kaar and Brink,
1991). The Phenolic and aliphatic hydroxyl groups for the alkaline
hydrolyzed Kraft lignin were determined by the proton nuclear
resonance magnetic method according to the procedure reported
by El Mansouri et al. (2011). Triplicate samples were used to deter-
mine the chemical properties.
Fig. 1. Steam explosion reactor.
C. Mancera et al. / Waste Management 32 (2012) 19621967 1963
2.5. Statistical analysis
One-way analysis of variance (ANOVA) and t-tests were used to
test (a = 0.05) for signicant difference between factors and levels.
When the ANOVA indicated a signicant difference among factors
and levels, a comparison of the means was undertaken to identify
which groups were signicantly different from other groups at 95%
condence level.
3. Results and discussion
Table 1 shows the results of chemical composition of V. vinifera
raw material and pulp, compared with pine and eucalyptus wood
results from literature. A comparison of these results revealed
the following: The lignin content in V. vinifera raw material was
lower than pine pinaster and higher than eucalyptus globulus.
The cellulose content in V. vinifera raw material was lower than
of pine and eucalyptus wood. The holocellulose is the moiety of
cellulose and hemicellulose in the bers. The holocellulose of V.
vinifera was lower than of pine and eucalyptus wood. The ash con-
tent of V. vinifera which is composed of silicates and mineral com-
ponents (Na, Fe, Mn, K, etc.) was higher than of pine and eucalyptus
wood. Therefore, V. vinifera chemical composition revealed med-
ium cellulose and high lignin percentages that suggested its suit-
ability as alternative source of wood bers used in berboards.
The V. vinifera raw material was submitted to a steam explosion
process at a temperature of 218 C and a pretreatment time of
6 min, according to the procedure reported in experimental part.
The obtained pulp exhibits a higher cellulose and lignin content
with zero extractives and very lower hemicelluloses content. The
latter are reported to be responsible of poor berboard physical
properties such as water absorption and thickness swelling.
Table 2 shows the results of ash, carbohydrates, Klason, and
acid-soluble lignin contents with the total OH-groups in the lignin
samples. The lignin rawmaterial had a lower percentage of total lig-
nin (KL + ASL) than of a puried Kraft lignin and alkaline hydrolyzed
Kraft lignin because of its high content of ash and carbohydrates.
The content of both ash and carbohydrates can be lowered by wash-
ing the lignin raw material with 1% (wt/wt) sulfuric acid and hot
water (Lin, 1992) or by its treatment under alkaline conditions
(Mancera et al., 2011). This is clear if we compare the results of
the lignin raw material and the treated lignins. Therefore, the trea-
ted lignins had high total lignin content above 94% (wt/wt) and they
are characterized by carbohydrates content less than 2% (wt/wt),
which is similar to that found in milled wood lignins by Hortling
et al. (1991). The high content of carbohydrates in lignin raw mate-
rial implies that there are more chemical linkages between lignin
and carbohydrates in this lignin than in puried and alkaline hydro-
lyzed Kraft lignins. On the other hand, both acid-soluble lignin (ASL)
and Klason lignin (KL) can undergo polycondenstaion reaction with
other wood components when lignin was used as natural adhesives
for berboard manufacturing. Moreover, the presence of carbohy-
drates can also participate in this reaction, and therefore, the
strength and water resistance of the manufactured berboard can
be improved.
The results of physico-mechanical properties of berboards are
shown in Figs. 26. The experimental factors studied were the
types of treated lignins added in four quantities: 5%, 10%, 15%,
and 20%. These levels were chosen on the basis of the research
groups previous experiences in producing berboards with exter-
nally added lignin and the literature review (Angles et al., 1999;
Velasquez et al., 2003). All the berboards obtained had densities
from 1376 to 1386 kg m
3
for binderless berboards and from
1358 to 1380 kg m
3
for lignin-berboards and were classied like
High Density Fiberboard (HDF).
The modulus of rupture (MOR) and modulus of elasticity (MOE)
were analyzed together because they came from the same bending
assay. Fromthe Fig. 2 it can be seen that for puried Kraft lignin the
berboard increased in strength as the amount of lignin was in-
creased. Fiberboards made with this lignin type had higher
strength values than binderless berboards. It is particularly inter-
esting to note that the strength of berboards made with just 5% of
puried Kraft lignin was almost the double of that of binderless
berboard. More interesting are the results for berboards made
with 10% added lignin, which shows MOR value that passed the
relevant standard specications. The incorporation of 20% lignin
resulted in berboards with MOR values (55 MPa) that were two
times higher than those obtained for binderless berboards
(24 MPa). This provides a good indication that the incorporation
of puried Kraft lignin is able to improve the MOR of berboards
made from V. vinifera. However, for the alkaline hydrolyzed Kraft
lignin (AHKL) the maximum MOR value was reached with the
incorporation of 5% of this lignin, after which it start to decrease
when the percentage of added AHKL was increased, even returning
the MOR to practically the initial values at 20% added AHKL. This
indicates that part of the AHKL added develops lignin networks
connecting the ber between them, but when the lignin quantity
is increased internal defects arise when lignin molecules gather
together.
For the puried Kraft lignin it can be seen from Fig. 3 that the
MOE values of berboards increased as the percentage of this lig-
nin was increased. The results show that incorporating this lignin
type stiffened the berboards. A similar trend was observed by
other authors (Velasquez et al., 2003). The results also show that
the MOE of the berboards signicantly increased as the lignin
loading increased to 20%. Thus, the results illustrate that this lignin
enhances the stiffness of berboards. However, for alkaline hydro-
lyzed Kraft lignin the maximum MOE value was reached with the
addition of 5% of this lignin after which it starts to decrease with
increasing the percentage of added AHKL.
The internal bond (IB) refers to the strength of the bond be-
tween bers, which is important because it ensures that the boards
will not delaminate during post-processing. Overall, the internal
bond of the berboards was improved with the incorporation of
puried Kraft lignin. The results displayed in Fig. 4 shows that b-
erboards made with just 15% and 20% puried Kraft lignin had an
IB that meets the relevant standard specications. The results also
Table 1
Results of chemical analysis of Vitis vinifera raw material and pulp compared to literature results for pine and eucalyptus wood.
Chemical Vitis vinifera Vitis vinifera pulp Pine pinaster
a
Eucalyptus globulus
a
Ash content (%) 3.70 1.80 0.54 0.57
Extractives (%) 13.30 0.00
Lignin
b
(%) 24.00 37.20 26.20 20.00
Cellulose (%) 43.60 63.20 55.90 52.80
Hemicelluloses (%) 19.10 1.70 13.70 27.70
Holocellulose (%) 62.70 64.90 69.60 80.50
a
Serrano et al. (2010).
b
Lignin (%) = klason lignin (%) + acid-soluble lignin (%).
1964 C. Mancera et al. / Waste Management 32 (2012) 19621967
show that the effect of lignin on the IB became more evident as
more puried lignin was added. Thus, the results indicate that
puried Kraft lignin plays a positive role in improving the IB of b-
erboards made from V. vinifera. However, for alkaline hydrolyzed
Kraft lignin the maximum IB value was reached at 15% of this lig-
nin, after which it starts to decrease by increasing the amount of
lignin to 20%. It can be also seen that berboards made with 5%
and 10% of lignin resulted in higher strength values than binderless
berboards.
Since the values of mechanical properties depend on the
bonding strength among bers and individual ber strength, bet-
ter inter-ber bonds should contribute to an improvement in
bending strength when ber of the same quality is used. These
inter-ber bonds are due mainly to: (i) hydrogen bonding be-
tween bers, (ii) the condensation reaction in lignin polymer,
(iii) the cross-linking reaction between lignin and polysaccha-
rides, and (iv) the formation of covalent bonds between the
Table 2
Details of chemical composition and hydroxyl groups of lignins sample.
Chemical composition Lignin raw material Puried Kraft lignin (PKL) Alkaline hydrolyzed Kraft lignin (AHKL)
Ash content (%) 27.20 0.40 1.05
Klason lignin (%) (KL) 61.10 94.20 95.85
Acid-soluble lignin (%) (ASL) 4.95 2.85 0.65
Carbohydrates (%) 3.35 1.48 0.60
Total OH-groups content (%) OH-phenolic (%) 4.10
a
5.00
OH-aliphatic (%) 10.09
a
12.00
a
El Mansouri and Salvado (2007b).
0
10
20
30
40
50
60
M
O
R

(
M
P
a
)
Binderless fiberboard Alkaline hydrolyzed Kraft lignin Purified Kraft lignin
Fig. 2. Mean modulus of rupture (MOR) of berboards.
0
1000
2000
3000
4000
5000
6000
7000
8000
M
O
E

M
P
a
Binderless fiberboard Alkaline hydrolyzed Kraft lignin Purified Kraft lignin
Fig. 3. Mean modulus of elasticity (MOE) of berboards.
0
0.2
0.4
0.6
0.8
1
1.2
1.4
I
B

(
M
P
a
)
Binderless fiberboard Alkaline hydrolyzed Kraft lignin Purified Kraft lignin
Fig. 4. Mean internal bond strength (IB) of berboards.
0
2
4
6
8
10
12
14
16
W
A

(
%
)
Binderless fiberboard Alkaline hydrolyzed Kraft lignin Purified Kraft lignin
Fig. 5. Mean water absorption (WA) of berboards.
0
2
4
6
8
10
12
T
S

(
%
)
Binderless fiberboard Alkaline hydrolyzed Kraft lignin Purified Kraft lignin
Fig. 6. Mean thickness swelling (TS) of berboards.
C. Mancera et al. / Waste Management 32 (2012) 19621967 1965
constituents of lignocellulosic polymers (Back, 1987; Suzuki et al.,
1998; Okuda et al., 2006a, 2006b; Zhou et al., 2011). It is well
known that covalent bonds result in intermolecular forces that
are much stronger than those of hydrogen bonds. In addition, -
bers with lignin-rich surfaces improve the mechanical properties
of berboards through the mechanical entanglement of the
melted lignin molecules under pressure and temperature, possi-
bly accompanied by the formation of covalent bonds (Okuda
et al., 2006a, 2006b; Quintana et al., 2009).
Therefore, the poor results obtained for berboards made with
alkaline hydrolyzed Kraft lignin can be attributed to its high hydro-
xyl group content. The maximum values of the mechanical proper-
ties are reached much earlier than in puried Kraft lignin. Thus, the
much higher hydroxyl content accelerates the condensation reac-
tion in lignin and between lignin and polysaccharides. When the
hardened network formation in polycondensates is too rapid, early
immobilization of the network occurs, causing a lower density of
crosslinking and hence lower strength (El Mansouri et al. 2007a).
This is the case for alkaline hydrolyzed Kraft lignin.
Water absorption (WA) and thickness swelling (TS) are physical
properties related to the dimensional stability of the boards. These
properties give us an idea of how the boards will behave when
used under conditions of severe humidity and are especially
important regarding boards that are to be used externally. From
Fig. 5 it can be seen that the berboards water absorption de-
creases with the increase of the percentage of incorporated puri-
ed Kraft lignin. The incorporation of 20% of this lignin has
signicantly decreased water absorption and thus improved the
water resistance of the berboards. However, for the alkaline
hydrolyzed Kraft lignin the minimal WA was reached with the
incorporation of 5% of this lignin type after which it start to in-
crease with increasing the percentage of added lignin.
It is well known that lignocellulosic materials absorb water by
forming an hydrogen bond between water and hydroxyl groups
of cellulose, hemicellulose, and lignin in the cell wall (Rowell
et al., 1976). However, from the results shown in Fig. 6 it can be
seen that the puried Kraft lignin added externally was able to re-
duce the water absorption of V. vinifera bers, possibly because of
the non-polar hydro-carbon chains and aromatic rings in the lignin
molecules (Rozman et al., 2000). On the other hand, there are two
possible ways in which the lignin could reduce water absorption:
(1) by bulking the cell wall and (2) by plugging the lumen of the
cell wall. The rst possibility is likely because the cell wall is
bulked by lignin; this makes it hydrophobic and water cannot
enter and swell up the cell wall. The second possibility is unlikely
because the lignin is too big to enter into the cell wall.
Thickness swelling of lignocellulosic material occurs when the
cell wall is bulked by water. The results clearly show that ber-
boards without puried Kraft lignin had higher TS than those made
with lignin. Of particular note are the results found for berboards
made of 20% externally added puried Kraft lignin, which show 4
times less TS than binderless berboards. Thus, it is clear that
externally added puried Kraft lignin was able to reduce the extent
of swelling in berboards, because swelling was reduced as lignin
levels increased. These results clearly indicate that lignin is able to
reduce the amount of water that enters and swells the cell wall.
However, for the alkaline hydrolyzed Kraft lignin, the minimal TS
was reached with the incorporation of 5% of lignin, after which it
starts to increase with increasing the amount of incorporated AHKL
lignin into berboards.
4. Conclusions
V. vinifera chemical composition revealed medium cellulose and
high lignin percentages that suggested its suitability as alternative
source of wood bers used in berboards. The puried Kraft lignin
and alkaline hydrolyzed Kraft lignin samples showed a high purity
and differences in hydroxyl group content.
The produced binderless berboards, berboards made from V.
vinifera bers and alkaline hydrolyzed Kraft lignin have weaker
mechanical properties. However, the breboards obtained using
puried Kraft lignin have good mechanical and water resistance
properties which satisfy the requirements of the relevant stan-
dards specications.
Acknowledgments
The authors would like to thank Ligno-Tech Ibrica S.A., for sup-
plying the lignin raw material. We would also like to express our
sincere appreciation to Rovira i Virgili University for the award of
a scholarship, the Spanish Ministry of Science and Technology for
its nancial support under Project Number ENE2007-65033-ALT
and the Autonomous Government of Catalonia for providing -
nance under Project Number 2005SGR-00580.
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