Bioresource Technology 100 (2009) 4731–4735

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Bioresource Technology
journal homepage: www.elsevier.com/locate/biortech

Bleaching Miscanthus x giganteus Acetosolv pulps with hydrogen peroxide/acetic

acid. Part 1: Behaviour in aqueous alkaline media
Juan José Villaverde, Pablo Ligero, Alberto de Vega *
Department of Physical Chemistry and Chemical Engineering, University of A Coruña, 15071 A Coruña, Spain

a r t i c l e i n f o a b s t r a c t

Article history: Miscanthus x giganteus bark samples subjected to fractionation by the Acetosolv process under optimal
Received 21 March 2009 conditions were bleached using hydrogen peroxide and acetic acid in aqueous media under alkaline con-
Received in revised form 22 April 2009 ditions. The influence of the main operational variables in the bleaching of Acetosolv pulps of M. x gigan-
Accepted 26 April 2009
teus (i.e. hydrogen peroxide concentration, 3–7%; temperature, 55–75 °C; pH 9–11), obtained after
Available online 23 May 2009
treatments, have been assessed on pulp yield, kappa number, viscosity and brightness of bleached pulps.
For this purpose, a rotatable and orthogonal second-order factorial design of experiments was used, in
Keywords:
order to identify the optimum operating conditions. The obtained empirical mathematical models dem-
Miscanthus x giganteus
Acetosolv
onstrate that, in general, the bleaching was efficient, achieving pulps with kappa numbers below 10. The
Bleaching chemical composition and physicochemical properties of the bleached pulps fulfilled the requirements
Modelling for forthcoming bleaching stages. Moreover, an alkaline extraction stage to eliminate saponifiable groups
Chelating agents of Acetosolv pulps was studied, as well as the necessity of use chelating agents in the stage with hydrogen
peroxide.
Ó 2009 Elsevier Ltd. All rights reserved.

1. Introduction cals, peroxyacids (strong oxidant compounds) were also studied

in chemical pulp bleaching. Peroxyacetic acid is among the most
Currently, the paper industry is still reluctant to use raw mate- used of the peroxyacids (Jääskeläinen et al., 2000). The pH at which
rials other than hard- and softwoods. Each day, however, more peroxyacid is produced is very important. In acidic media, peroxy-
industries are understanding the importance of new lignocellulosic acetic acid (CH3CO3H), an electrophilic species, is dominant,
raw materials in a model of sustainable development, due to a whereas in basic media the peroxyacetate ion ðCH3 CO 3 Þ, a nucleo-
shortage of traditional woods and decisions taken by many govern- phile, is dominant.
ments for the introduction of technologies based on new renew- Despite the abundance of scientific literature on peroxyacids as
able sources. Cellulose produced by Ligno-Cellulosic Feedstock bleaching agents, few references seem to exist in relation to the
(LCF) biorefineries (Kamm and Kamm, 2004) from nonwood fibres bleaching of lignocellulosic pulps with the nucleophilic species
may be the most important raw material in the future biobased (Delagoutte et al., 1999; Pérez et al., 2006) and none with the
economy through the production of bulk chemicals, new materials, use of mathematical models to estimate the quality of bleached
fuels and energy. LCF organosolv biorefineries could contribute to Miscanthus x giganteus pulp as a function of bleaching variables,
large economic benefits from the valorisation of fractionated prod- with a view to optimize the operating conditions. Therefore, in or-
ucts. These biorefineries fractionate the biomass into its main com- der to fill this gap, a detailed study of the influence of independent
ponents (cellulose, hemicelluloses, lignin and extractives) by variables in the bleaching of Acetosolv M. x giganteus pulp (viz.
organic solvents, and then each fraction is processed. To upgrade hydrogen peroxide concentration over dry pulp, temperature, and
pulps for subsequent uses, such as paper production or dissolving pH) on pulp yield, kappa number, viscosity and brightness, was
pulp manufacture, residual lignin must be removed from a solid performed. A rotatable and orthogonal second-order factorial de-
matrix by using a number of solubilising and/or oxidizing agents. sign was used, with the aim of identifying the optimum operating
For this purpose, chlorine and chlorine dioxide were commonly condition.
used for years. Nevertheless, important restrictions related to the
environmental impact associated with their use, have focused re-
search efforts in the search of new bleaching processes that avoid 2. Materials
chlorinated compounds, in the so-called Totally Chlorine Free (TCF)
sequences. In an effort to find more selective oxygenated chemi- 2.1. Raw material

M. x giganteus from an experimental plantation, established as

* Corresponding author.
E-mail address: [email protected] (A. de Vega). part of the EU AIR Miscanthus Productivity Network near Santiago

0960-8524/$ - see front matter Ó 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.biortech.2009.04.052
4732 J.J. Villaverde et al. / Bioresource Technology 100 (2009) 4731–4735

de Compostela (Spain), was used in this study. Plants were har- Zj  Zj

Xj ¼
vested, manually stripped of leaves and core, air dried for two DZ j
weeks and ground to pass through a 1 cm sieve. Once in the labo-
ratory, the ground substrate was allowed to attain its equilibrium where Z j is the value of the variable j in a specific experiment, Z j is
moisture content and finally stored in hermetic polypropylene the arithmetic mean of the minimum and the maximum values ap-
containers. plied to the variable j, and DZ j is the mid-point of the variation
range of each variable, that is:

2.2. Characterization of the raw material and cellulose pulps Z jmax  Z jmin
DZ j ¼
2
For all experiments, kappa number (KN), intrinsic viscosity (VIS) This way the different normalised variables are restricted between
and ISO brightness (BR) were measured according to TAPPI stan- the values 1 (which corresponds to the lowest treatment value)
dards (T 236, T 230 and T 525, respectively). Pulp yields (PY) were and + 1(corresponding to the highest value).
determined gravimetrically after oven drying until they reached a The following experimental results were analysed as dependent
constant weight. Saponifiable groups (as NaOH equivalent) were variables: PY, KN, VIS and BR of the resulting pulps; and submitted
determined by KOH–ethanol saponification (Abad et al., 2002; to multivariate regression against the independent variables using
Dapía et al., 2002). polynomial fit functions such as:

2.3. Acetosolv fractionation X

3 X
3 X
DV ¼ b0 þ bi X i þ bii X 2i þ bij X i X j þ b123 X 1 X 2 X 3
i¼1 i¼1 i<j
Mixtures of ground M. x giganteus bark, water and acetic acid
(weight percentage with respect to cooking liquor = 90%, liquid/ where DV represents each of the dependent variables (system re-
wood ratio = 12 by weight), were heated to boiling point in a sponses), and Xi and Xj are the normalised independent variables.
3000 cm3 glass reactor. Hydrochloric acid (weight percentage with The different values of b0, bi and bij represent the fitting parameters
respect to cooking liquor = 0.15%) was added when the boiling by which, due to normalisation, we can determine and compare the
started, and the mixtures refluxed, with stirring, at atmospheric effects of each of the independent variables on the dependent vari-
pressure for 55 min. The pulps were then filtered, treated four ables (experimental results).
times with 85% acetic acid (in w/v proportions of 0.4, 0.4, 0.2 and All calculations were performed with a statistics module of
0.2 with respect to the initial dry weight of M. x giganteus), and Excel.
washed repeatedly with distilled water until neutrality. The pro-
cess and reaction conditions used here have been optimized in pre-
3. Results
vious works (Ligero et al., 2005).
Unbleached Acetosolv pulps presented the following character-
2.4. Bleaching
istics: PY: 59.9%; KN: 17.3; VIS: 964 cm3/g; and BR: 33.2%. The
main inconvenience in these pulps comes from extensive acetyla-
The bleaching tests with alkaline treatments (E-stages) and
tion during pulping. Acetylation was observed by several authors
peroxyacetic alkaline treatments (Pab-stages) were carried out at
(Saake et al., 1998; Abad et al., 2002, 2003; Dapía et al., 2002,
the desired consistency in sealed polyethylene bags immersed in
2003) and is recognized as a drawback in the first bleaching stages
a thermostatic water bath at the desired temperature. Samples
due to the important alkali demand derived from the unavoidable
were kneaded several times during the reaction. Before Pab-
saponification that takes place in much TCF bleaching stages. Also,
stages, pulps were soaked with an aqueous solution at the
VIS in cupriethylenediamine solution (CED) and alkaline resis-
appropriate pH and filtered to remove the remaining liquid. This
tances reduce their value with the increase of saponifiable groups
was repeated three times to achieve the desired pH. After each
(Saake et al., 1998). Miscanthus Acetosolv pulps showed important
bleaching treatment, the pulps were washed with aqueous solu-
signs of such saponifiable groups (8.0%) that become clear by com-
tion at pH 11.
paring FTIR spectra of unbleached and bleached pulps. Unbleached
E-stage was performed at 10% consistency for 60 min, changing
pulp has an intense absorption band at 1740 cm1 (pure band of
temperature between 60 and 80 °C, and NaOH concentration be-
unconjugated C@O stretching vibration) (Pandey and Theagarajan,
tween 4% and 6%.
1997; Vázquez et al., 2002) that disappears after an alkaline treat-
Pab-stage was performed at 10% consistency, and the rest of
ment. Therefore, in order to eliminate saponifiable groups, a first
variables were changed as follows: time, 15–90 min; temperature,
alkaline extraction stage (E-stage) was chosen, which was con-
55–75 °C; hydrogen peroxide concentration, 3–7%; acetic acid in
nected with a second stage of acetic acid in the presence of hydro-
double molar ratio respect to hydrogen peroxide (Jääskeläinen
gen peroxide to form the consequent peroxyacetate.
et al., 2000); and pH 9–13.
A first set of experiments, designed to evaluate the influence of
the temperature, was carried out by setting values for a number of
2.5. Experimental design variables (consistency: 10%; sodium hydroxide concentration: 4%;
time: 60 min) while the temperatures used were 60, 70 and 80 °C.
A rotatable and orthogonal second-order factorial design To determine whether the E-stage could produce a significant ef-
(Akhnazarova and Kafarov, 1982) was used to fit experimental data fect on the next step, the pulps were subsequently subjected to a
to polynomial equations and to quantify the effects of the indepen- Pab-stage under identical conditions: consistency 10%, 60 min,
dent variables (IV) on the parameters defining the progress of peracetic acid 7% (in dry pulp basis, assuming quantitative conver-
bleaching. Factorial designs have been used extensively to examine sion of hydrogen peroxide to peroxyacetate, according to literature
the behaviour of bleaching with organosolv pulps (Jiménez et al., (Jääskeläinen et al., 2000) by mixing the acid and hydrogen perox-
2008; López et al., 2002, 2003). According to standard procedures ide in the molar ratio 2:1, at 75 °C and pH 11. The results (Table 1)
in experimental design construction and analysis, the independent show that the main effect of the E-stage is a solubilisation of mate-
variables (hydrogen peroxide concentration, temperature, and pH) rials more than any other. But unlike what was expected, it does
were normalised in accordance with: not produce much delignification, in view of the relatively small
 J.J. Villaverde et al. / Bioresource Technology 100 (2009) 4731–4735 4733

Table 1
Results of the E-stage.

Accumulated yield (%) Kappa number Viscosity (cm3/g) ISO brightness (%)
Unbleached pulp 59.9 17.3 964 33.2
Influence of temperature on E-stage 4% NaOH – 60 °C 49.6 19.6 1114 37.3
Pab-stage 47.8 14.8 1010 41.8
4% NaOH – 70 °C 51.6 18.6 1134 36.3
Pab-stage 48.8 14.4 922 46.6
4% NaOH – 80 °C 51.1 17.6 1047 37.5
Pab-stage 50 13.3 895 45.7
Influence of alkali concentration on E-stage 4% NaOH – 70 °C 51.6 18.6 1134 36.3
Pab-stage 48.8 14.4 922 46.6
5% NaOH – 70 °C 52.4 16.1 1009 41.4
Pab-stage 49.7 13.1 1028 49.4
6% NaOH – 70 °C 49.9 15.7 1063 42.3
Pab-stage 47.3 11.4 944 50.7

diminution of KN just after this stage (Table 1). However, it is clear In order to study the effects of experimental variables in perox-
from the values of VIS, and confirmed by FTIR spectra, that the yacetate bleaching, consistency and time were fixed at 10% and
main chemical effect was the removal of saponifiable groups. There 60 min, respectively, and a rotatable and orthogonal second-order
were no significant differences in the behaviour of the system at factorial design of experiments was carried out to assess the influ-
different temperatures, except an increase in BR at 70 °C, which ence of the next three variables, in the ranges mentioned: hydro-
was not improved by raising the temperature to 80 °C. Therefore, gen peroxide concentration (3–7%), temperature (55–75 °C) and
the chosen temperature was 70 °C, in preference to the other two pH (9–11). Table 2 shows the structure of the experimental design
studied, and used in the consequent experiments. together with the results obtained in each case for PY, KN, VIS and
Once this temperature was adopted, a new series of experi- BR.
ments (Table 1) was conducted to determine the best concentra- The fitting of the experimental results by means of least square
tion of sodium hydroxide. The experimental conditions were the multiple regression is shown in Table 3. The different parameters
same as those mentioned above, except the temperature was fixed of the model, their significance levels, and several statistical values
at 70 °C. We studied the variation of alkali concentration at values indicate the goodness of fit of the mathematical models.
of 4%, 5% and 6%. The results reflect a growing delignification with Results show an acceptable fit between the experimental data
the increase of alkali concentration, obtaining the largest differ- and the polynomial models except for PY. For this variable, the
ences in kappa number (21%) going from 4% to 6% of alkali. On small variations found (94.0–99.0%) make the experimental error
the other hand, no significant changes in VIS and BR of pulps ob- relatively important, which reduces the significance of the effects
tained from 5% to 6% of alkali were observed, so 6% was chosen of the variables and is reflected in the statistical analysis, because
to obtain the highest delignification. none of them were significant at the 90% or 95% confidence level.
Therefore, the data show that the best results (higher delignifi- Also, as a result of the small variations, the surface responses for
cation levels with a decrease of 35% for KN and an increase of this variable are essentially flat and parallel to the horizontal plane
51% for BR) were obtained working at 70 °C and with a 6% NaOH for any representation of IV–IV–PY.
concentration. With these values, the delignification proceeds with For all other IV, pH was always the most influential variable,
a significant brightness increase and a moderate attack on cellu- especially for KN, producing more delignified pulps as pH increases
lose. Hereafter, it will be used in all cases the next set of variables (Fig. 1 and Table 3). This effect becomes more important in the sec-
for the E-stage: consistency 10%, 60 min, 70 °C and 6% of sodium ond half of the studied interval (10 < pH < 11). Also, a synergic ef-
hydroxide. fect between pH and hydrogen peroxide is observed for pH and

Table 2
Experimental design structure and results of the peroxyacetate treatment of Acetosolv M. x giganteus pulps.

N° exp. H2O2 concentration (% o.d.p.) T (°C) pH PY (% o.d.p.) KN BR (ISO%) VIS (cm3/g)

1 3 55 9 94.7 15.1 40.1 1076
2 7 55 9 94.8 14.8 42.3 1084
3 3 75 9 95.8 14.5 42.1 1121
4 7 75 9 98 14.2 40.8 1100
5 3 55 11 94.7 13.8 43.3 1144
6 7 55 11 95.5 11.5 48.8 1011
7 3 75 11 95.4 12.2 51.6 1119
8 7 75 11 94.2 9.9 52.7 984
9 1.64 65 10 97.4 14.3 41.6 1145
10 8.36 65 10 96.9 13.8 50.5 1146
11 5 48.2 10 94.9 14.7 45.4 1116
12 5 81.8 10 97.3 14.3 50 1183
13 5 65 8.32 98.8 15.1 47.7 1146
14 5 65 11.68 99 9.2 51 832
15 5 65 10 98.8 14.8 43 1136
16 5 65 10 97.5 14.4 43.7 1145
17 5 65 10 94 15.1 43.7 1183

Consistency = 10%; Time = 60 min.

4734 J.J. Villaverde et al. / Bioresource Technology 100 (2009) 4731–4735

Table 3
Regression parameters for each variable, and goodness of fit and signification of
regression equations.

Factor Name PY KN BR VIS

Coefficient Coefficient Coefficient Coefficient
b0 96.90* 14.78* 43.64* 1155.4*
b1 H2O2 0.078 0.442* 1.645 20.45
b2 T 0.566 0.371** 1.496 8.910
b3 pH 0.232 1.547* 2.684* 47.67*
b12 0.013 0.000 0.988 3.875
b13 0.338 0.500** 0.713 31.88
b23 0.613 0.25 1.463 14.13
b123 0.513 0.000 0.113 3.375
b11 0.316 0.308 0.304 5.717
b22 0.687 0.148 0.887 4.302
b33 0.303 0.979* 1.471 61.05*
R 0.6556 0.9781 0.8841 0.8801
Std error 2.1223 0.6192 3.2186 67.2291
F 0.4523 13.2539 2.1489 2.0624
Sig F 0.8720 0.0025 0.1808 0.1943
FLOF 0.5962 4.1629 94.6374 10.3939
Sig FLOF 0.7042 0.2030 0.0105 0.0897
*
Indicates significant at a 0.05 level.
**
Indicates significant at a 0.10 level. Fig. 2. pH and hydrogen peroxide concentration effect on BR of pulps at a constant
temperature of 55 °C.

Table 4
Influence of initial pH and time on the main characteristics of pulps for values out of
the experimental design.

Initial Pulp yield Kappa Viscosity Brightness

pH (accumulated %) number (cm3/g) (%ISO)
11 51.3 11.1 1011 50
11.5 49.3 10.3 898 44.8
12 49.2 10.9 810 52.4
12.5 47.7 10.1 748 49.7
13 39.4 7.3 561 49.9
Time (min)
15 51 13 1025 42.4
30 53.2 11.7 966 46.3
45 53.7 11.4 974 43.7
60 51 11.2 987 48.9
75 48.9 11.3 946 49.8
90 49.9 10.7 982 51.4

most convenient temperature, and this value was used in all sub-
sequent experiments.
Fig. 1. pH and hydrogen peroxide concentration effect on kappa number of pulps at In an attempt to look for possible KN drops outside the limits of
a constant temperature of 75 °C. the experimental design, a new set of experiments were performed
in which the pH was varied in steps of 0.5 units between 11 and 13.
Table 4 shows that the kappa number does not decrease signifi-
peroxide concentration levels above 11 and 7%, respectively, while cantly until pH 13. However, the viscosity dramatically decreased,
no relevant effect was found at lower pH and peroxide concentra- almost linearly with pH. No clear effects were observed for BR in
tions. Minimum values of KN (slightly above 10) are predicted this set of experiments, affording results in a limited range of
when IV are set at their highest values. Something similar happens 45.0–52.0%. In view of these results, pH 11.0 was selected for a well
with BR, being here the effects of different signs: pH and peroxide balanced bleaching without severe cellulose damage.
loads are the most influential factors, principally for the highest Furthermore, a kinetic monitoring of the system was carried out
levels, where predicted BR values are the highest and are close to in order to decide whether a more extended treatment could im-
50% (Fig. 2). Furthermore, the maximum BR (53.2%) is predicted prove the results. A substantial improvement in KN is obtained
when all IV are at their upper extreme. All these results show that by increasing the treatment time from 15 to 30 min (Table 4). KN
pH and peroxide load must be set at 11 and 7%, respectively, to ob- could be reduced even more, but changes are much lower than ob-
tain a well delignified pulp with a high brightness. served in the range 15–30 min VIS is slightly affected in this inter-
In relation to temperature, it was not significant in any case at a val, decreasing from 1025 to 966 cm3/g, which still is a very good
confidence level of 95%. The mathematical models can be used to value. Regarding BR, it rose almost linearly with time until 51.4%
predict the system behaviour in relation to temperature; doing after 90 min; however, after 30 min, the pulp presented a relatively
so at a fixed pH of 11 and a peroxide load at 7% drops KN by only high BR (46.3%), which represents an increase of 11.5% from the
one unit when temperature rises from 55 to 75 °C. Therefore, in or- initial value. In view of these results, 30 min was selected as the
der to get suitable energy efficiency, we have chosen 55 °C as the most appropriate time for subsequent experiments.
 J.J. Villaverde et al. / Bioresource Technology 100 (2009) 4731–4735 4735

Table 5
Results of the addition of DTPA (1%) and MgSO4 (1%) on the peroxyacetate (Pab) treatment of Acetosolv Miscanthus pulps (10% consistency, 7% peroxide, pH 11, 30 min and 55 °C).

DTPA added MgSO4 added Pulp yield (% o.d.b.) Kappa number Viscosity (cm3/g) Brightness (%ISO)
No No 99.4 11.1 982 37.5
No Yes 98.4 12.8 1085 35.7
Yes No 99.8 12.6 1089 37
Yes Yes 98.7 12.3 1112 34.9

Finally, the effect of chelating agents was investigated. A new References

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