PAPER PHYSICS

Ultrasonic treatment of secondary fibers to improve

paper properties
Mauro Manfredi, Rubens Chaves de Oliveira, Juliana Cristina da Silva and Rafael Ignacio Quezada Reyes
KEYWORDS: Paper strength, Ultrasound, Secondary susceptible to the negative effects of the refining process
fiber, Recycling. (Minor et al. 1993; Peixoto 2002, Peixoto, Oliveira
2003). Even when conducted at low intensity, the refining
SUMMARY: The refining is the mainly techniques used
of secondary fibers may cause damages in fiber structures
to recover paper quality during the recycling process.
and excessive fine production. To avoid this loss in fiber
However, this technique also results in undesirable
quality, it is necessary to develop a new technology able
effects. In this study the potential of ultrasonic treatment
to promote fiber swelling and external defibrillations with
to develop the mechanical properties of recycled waste
less fiber damage.
papers was evaluated. Ultrasonic energies were applied at
Some studies have already proved the efficiency of
20 kHz with an intensity of 190 Watts into 1 liter batches
ultrasonic vibration to develop paper properties (Laine et
of re-pulped OCC at consistencies of 0.5 to 4%, pH levels
al. 1977; Laine, Goring 1977; Won, Lee 1996; Brodeur,
of 7 and 10, and time increments of 5, 10 and 20
Gerhardstein 1998; Tatsumi et al. 2000; Peixoto 2002;
minutes. Sheets were made and evaluated for bulk, ring
Poniatowski, Walkinshaw 2005; Josefsson 2010). Some
crush test, tear index and tensile index. Pulps were
of them showed that the action of ultrasound is similar to
additionally processed in a PFI mill and compared with
mechanical refining, but results in less damage to fiber
the results of the ultrasound trials at equivalent oSR. Pulp
structures (Laine et al. 1977; Laine, Goring 1977;
consistencies didn’t affect the ultrasonic treatment. The
Brodeur, Gerhardstein 1998; Peixoto 2002; Josefsson
use of higher pH and treatment time favored the
2010).
development of paper properties. To the same value of
The ultrasonic treatment promotes external
tensile index, the ultrasonic treatement produced sheets
defibrillation (Laine et al. 1977; Laine, Goring 1977;
with higher bulk than the PFI. The results indicate that
Tatsumi et al. 2000; Peixoto 2002; Josefsson 2010) and
the ultrasonic treatment of the pulp can be used to
internal defibrillation (Laine, Goring 1977; Tatsumi et al.
improve the properties of recycled waste paper.
2000; Peixoto 2002; Josefsson 2010) of fibers. These
ADDRESSES OF THE AUTHORS: Mauro Manfredi actions result in more fiber swelling and the formation of
(mauro.manfredi@ufv.br), Rubens Chaves de Oliveira more interfiber bonds. Compared to refining, the
(rchaves@ufv.br), Rafael Ignacio Quezada Reyes ultrasound treatment is less harmful to the bulk, for the
(Rafael.reyes@ufv.br), Juliana Cristina da Silva same increase in mechanical properties of paper (Laine et
(jcsfloresta@yahoo.com.br). Universidade Federal de al. 1977; Laine, Goring 1977; Won, Lee 1996; Peixoto
Viçosa, Departamento de Engenharia Florestal, 2002). It suggests that ultrasonic radiation act mainly
Laboratório de Celulose e Papel, campus, Viçosa-MG, causing the external defibrillation than the fiber walls
Brazil. Postal Code: 36570-000. collapses.
Corresponding author: Mauro Manfredi The ultrasound technology is also attractive because it
permits to control the modifications of fibers by handling
In the last 10 years, the consumption of recycled waste the frequency and the power of the waves (Brodeur,
paper in Brazil increased 60%. Industries have been Gerhardstein 1998). Another advantage is that ultrasound
working hard to develop new processes and techniques to
can be applied in different points in the process, such as
increase recycled paper quality and have achieved larger
tubes, tanks and towers.
participation in the paper market. The creation of new
Ultrasound may modify fiber structure through a
technologies is an important alternative to obtain a better
phenomenon called cavitation. Ultrasonic wave
process and better paper quality. propagating in liquid creates forces that induce pressure
In general, recycled waste paper has presented less variation. In the moment of low pressure vapor cavities
mechanical strength and optical quality than paper made
are formed. While pressure increases, the cavities are
from primary fibers. During the paper production
compressed until collapse. The collapse releases energy
process, fibers undergo structural modifications that
as a shock wave that can affect the physical structure. The
affect the fiber ability to form paper. The structural cavitation process results in pressure up to 200 atm and
modification results in reduced intrinsic fiber strength, temperatures higher than 5000°C producing high velocity
less fiber swelling and less external defibrillation (Minor,
jet that affects the fiber surface (Thompson, Manning
Atalla 1992). Fiber swelling contributes to the increase in
2005)
the contact area between fibers. A larger contact area
The present study aimed to develop the mechanical
between fiber surfaces, even external defibrillation,
properties of recycled waste paper by ultrasonic treatment
favors the formation of fiber bonds, thus increasing paper of the fibers, thus contributing with knowledge that will
strength. help the recycled waste paper industry to reach larger
To recover the ability to form paper it is usually
participation in paper market.
necessary to refine the fibers. However, since secondary
fibers have been previously refined, they become more

297 Nordic Pulp & Paper Research Journal Vol 28 no. 2/2013

Materials and Methods
The unbleached OCC (Old Corrugated Container), the
main type of paper recycled in Brazil, was chosen as fiber
source. The morphological features of the OCC fibers
were determined using Galai CIS-100. The average
values for length, width, coarseness and fines rate were
respectively 1.09 mm, 32.01 µm, 12.96 mg.100m-1 and
19.21.
Initially, the OCC was maintained in distilled water for
12 h. Then it was disaggregated, dried (at around 70% of
moisture) and kept in a plastic bag in the refrigerator.
Handsheets with 120 g.m-² were made for compression
tests and with 60 g.m-² for other tests, according to
TAPPI 205 sp-95. The handsheets were kept in an
environmentally controlled room at 23±1°C and humidity
around 50±2%.
The Virsonic 475 was used to ultrasonification at 190 W
and wave frequency of 20 kHz generated by a
piezoelectric tranducer. In each operation, 1 liter of pulp
was treated at a different consistency inside the beaker.
The beaker was used on a magnetic stirrer to propitiate a
homogenous treatment of the fibers. A ½” titanium probe
was inserted 1 cm deep in the fiber suspension at a
temperature of 30°C. During the treatment, the
temperature increases to the maximum of 40°C.
Pulp consistency, pH and treatment time were
evaluated. The results for the pulp consistency tested
were 0.5%, 1%, 2% and 4%. The treatment times used
were 5, 10 and 20 minutes. All those combinations were
tested at pH 7 and pH 10. Sulfuric acid and sodium
hydroxide were used to control the pulp pH.
The pulp was also refined in a PFI refiner to compare
the ultrasonic treatment and the mechanical refining. The
number of revolutions was chosen aiming to reach similar
values of the tensile index of the ultrasonificated pulp.
The PFI refining was performed according to TAPPI 248
sp-00. The pH of the pulp was adjusted to 7 or 10 prior to
the PFI refining.
The tension and the compressing tests were performed
in the Instron 4204 equipment. The determination of the
tear index and air permeance tests were made using the
equipments Elmendorf and “Gurley” porosity meter,
respectively. All tests were performed according to Tappi
Standards Methods.Ring Crush Test
1100
R² = 94.9
1050
RCT (N.m-1)
1000
950
900
R² = 90.3
850
800
0 5 10 15
Time (min)
0.5% 1% 2% 4%
Fig 1. Effect of the pH, pulp consistency and time of the
ultrasonic treatment in the resistance to compression (RCT).
PAPER PHYSICS
To statistical analyses were used the method of identity
of regression model at 95% significance. The Curve
Expert 4.0 software system was used to obtain the
models.
The fine contents and coarseness of the pulp, and the
average length and average width of the fibers were
determined. Every material with length smaller than
0.07 mm was considered fine content. The software
considered only material between 0.07 mm and 3 mm of
length to determine fiber dimensions. The analyses were
performed in Galai CIS-100 equipment and Wshape
software system. For such, the pulps were diluted to
0.001% consistence. These pulps were left at rest for at
least 8 hours before each analysis.
Results
Effect of ultrasonic treatment
Fig 1 shows that the ultrasonic treatment increased paper
resistance to compression forces (evaluated by the Ring
Crush Test). A similar behavior was observed when the
effects of treatments performed at pH 7 and pH 10 were
compared. However, the highest values of the properties
were reached when the ultrasonic treatment was
performed at alkaline condition.
The pH effect is evident when the non-ultrassofinicated
pulps (time zero) are compared. In alkaline conditions,
fiber walls are more hydrated and can be easily collapsed.
Therefore, the highest values observed at pH 10 are
probably due to the isolate effect of the alkali on fiber
structure, and not because of the effect of pH on
ultrasonic wave actions.
The statistical analysis shows no differences in the
results for different pulp consistencies (0.5, 1, 2 and 4%).
Therefore, every pulp consistency evaluated is
represented by only one line (to each pH value) in the
graphic.
Fig 2 shows that ultrasonification increased the tensile
index of the handsheets. According to the statistical
analysis, pulp consistency did not affect the results and
all pulp consistency evaluated is represented by the same
curve. On the other hand, pulp pH severely affected the
development of paper strength. When the treatment was
performed in alkaline condition, we observed a
significant effect even in the first minutes.
Tensile Index
37
R² = 96.3
Tensile Index (N.m.g-1)
35
33
31
pH 10 pH 7
29
pH 7 R² = 96.6 pH 10
27
25
20 0 5 10 15 20
Time (min)
0.5% 1% 2% 4%
Fig 2. Effect of the pH, pulp consistency and time of the
ultrasonic treatment in the tensile index.
Nordic Pulp & Paper Research Journal Vol 28 no. 2/2013 298
PAPER PHYSICS Bulk Tear Index
2,20 10,0
R² = 0.93 pH 7 R² = 85.0

Tear Index (mN.m².g -1)

2,18
9,5
Bulk (cm³.g-1)

2,16 pH 10
2,14
9,0
2,12 pH 10
R² = 79.0
2,10 R² = 0.90 8,5 pH 7
2,08
2,06 8,0
0 5 10 15 20 0 5 10 15 20
Time (min) Time (min)

0.5% 1% 2% 4% 0.5% 1% 2% 4%
Fig 3. Effect of the pH, pulp consistency and time of the Fig 4. Effect of the pH, pulp consistency and time of the
ultrasonic treatment in the bulk. ultrasonic treatment in the tear index.
When the pulps were not ultrasonificated, the values of a) Ring Crush Test - pH 7
the tensile index of the pulp at pH 10 condition was not
1300
higher than the value of the tensile index of the pulp at pH
7 condition. This fact suggests that the pH does not 1200
influence the tensile index just by affecting the swelling of

RCT (N.m-1)
the fiber wall, but it even makes the fiber wall more 1100 R² = 0.99
susceptible to the action of ultrasonic waves. Therefore, 1000
alkaline conditions allow using shorter treatment times.
The tensile index of papers is severely influenced by the 900 R² = 0.91
fiber to fiber contact area and fiber surface features. We 800
suggest that when pulp ultrasonification at alkaline 19 21 23 25 27 29 31 33 35 37
condition favors external defibrillation or fiber collapse. Schopper Riegler
Fig 3 shows the effect of the ultrasonic treatment of the
pulp performed at pH 7 and pH 10, at different time and b)
pulp consistency. According to the statistical analysis, Ring Crush Test - pH 10
pulp consistency did not affect the results. We observed 1300
that the pH condition did not influence the action of the R² = 0.97
1200
ultrasonic treatment. The ultrasonic treatment decreased
RCT (N.m-1)

the bulk of the handsheests similarly in both pH 1100

conditions. The differences in the values observed at
different pH conditions are due to the effect of the pH on 1000
fiber structure, and not to the action of ultrasonic waves.
900 R² = 0.91
This hypothesis is supported by the fact that the initial
bulk of the handsheests at pH 7 is higher than its initial 800
bulk at pH 10, and this difference remains over the 19 21 23 25 27 29 31 33 35 37
treatment time. Schopper Riegler
Fig 4 shows that the ultrasonic treatment slightly
increased the tear index of the handsheets. This result
PFI Ultrasound
must be associated to the best fiber network formation. It
is important to notice that ultrasonification did not Fig 5. Effects of the ultrasonic treatment and PFI refining on pulp
decrease the tear index while increasing the treatment strength, at pH 7(a) and pH 10(b).
time. This behavior suggests that the intensity of the
treatment time applied did not affect the intrinsic fiber
strength. Comparison between ultrasonic treatment and PFI
The effect of the ultrasonic treatment on the tear index Fig 5 shows that the ultrasonic treatment is less efficient
was not enhanced by the alkaline condition. According to to increase pulp resistance to the compression forces
the statistical analysis, pulp consistency did not affect the (RCT) than the PFI refining for the same °SR increment.
results. Fig 6 shows that at the same value of °SR, the PFI
The results of this experiment showed that the ultrasonic refining showed to be more effective to increase the
treatment is able to increase pulp strength, as reported in tensile index of the handsheets than the ultrasonic
the literature (Laine et al. 1977; Laine, Goring 1977; Won, treatment. When the treatments were performed at
Lee 1996; Brodeur, Gerhardstein 1998; Tatsumi et al. alkaline condition, for low values of °SR, the ultrasonic
2000; Peixoto 2002). However, the development of these treatment was more effective to increase the tensile index
properties is somewhat different from that observed when than the refining in PFI (Fig 6b). The effect of pH on PFI
the conventional refining is used. The Fig 5, 6 and 7 was basically the increase of °SR due to the effect of
compare these two technologies using the Schopper alkali on fibre swelling.
Riegler (°SR) as reference

299 Nordic Pulp & Paper Research Journal Vol 28 no. 2/2013
 PAPER PHYSICS

a) Tensile Index - pH 7 a) Bulk - pH 7

45 2,25
R² = 0.90
Tensile index (Nm.g-1)

2,20
41
R² = 0.99 2,15

Bulk (cm³.g-1)
37 2,10
2,05
33 2,00
R² = 0.98
R²= 0.93 1,95
29
1,90
25 1,85
19 21 23 25 27 29 31 33 35 37 19 21 23 25 27 29 31 33 35 37
Schopper Riegler Schopper Riegler

b) Tensile Index- pH 10 b) Bulk - pH 10

45 2,25
Tensile index (Nm.g-1)

R² = 0.99 2,20
41 R² = 0.85
2,15

Bulk (cm³.g-1)
37 2,10
2,05
33 2,00
R² = 0.98 1,95
29
1,90 R² = 0.99
25 1,85
19 21 23 25 27 29 31 33 35 37 19 21 23 25 27 29 31 33 35 37
Schopper Riegler Schopper Riegler

PFI Ultrasound PFI Ultrasound

Fig 6. Effects of the ultrasonic and PFI refine on the tensile Fig 7. Effects of the ultrasonic treatment and PFI refine in the
index of the handsheets, at pH 7(a) and pH 10(b).
Fines bulk of the handsheets at pH 7 (a) and pH 10 (b).
27 The properties suggest that ultrasonificated fibers are less
R² = 0.99 collapsed than refined fibers.
26 Based on the results and discussion, is hypothesized that
Fines rate (%)

the ultrasonic treatment promotes the development of

25
24
R² = 0.96
23
28 29 30 31 32 33 34 35 36 37 38 39 40 41 42
Schopper Riegler
PFI Ultrasound
Fig 8. Fine content of ultrasonificated and refined pulp.
Fig 7 compares the effects of PFI refining and
ultrasonification on the bulk. For the same increases in
°SR, the bulk was less affected by the ultrasonic
treatment than by PFI refining. It suggests that the
ultrasonic treatment results in less fiber wall collapses
or/and less fine production, compared to the PFI refining.
The analyses of the fibrous material showed that, for the
same °SR, the ultrasonic treatment produces more fines
than the PFI (Fig 8). The data refer to treatments
performed at pH 7. The fines content and degree of fibers
wall collapses are the mainly factors that affect the °SR
of the pulp. Thus, for the same °SR, the ultrasonificated
pulp has more fine materials and higher bulk.
Additionally, to the same fine content of 25%, the air
permeance of ultrasonificated pulp was considerable low
(6.2 s/cm³) than the permeance of PFI pulp (8.7 s/cm³).
paper properties mainly by creating external defibrillation
and producing fines. This conclusion is similar to those
observed by other authors (Laine et al. 1977; Laine,
Goring 1977; Won, Lee 1996; Tatsumi et al. 2000;
Peixoto 2002), who report that the ultrasonic treatment
defibrillates the external layers of fibers, produces fines
and increases paper strength.
Conclusions
The ultrasonic treatment of pulp proved to be technically
efficient to develop the mechanical properties of the
recycled waste paper. The effects of pulp
ultrasonification are higher when the treatment is
performed in alkaline condition. Pulp consistency did not
affect the action of ultrasonic waves.
Ultrasonic waves defibrillate the external layers of
fibres, generate fines and cause low impact on bulk.
Mechanical refining can be replaced by the ultrasonic
treatment in order to produce recycled papers with higher
bulk.
Acknowledgements
The authors gratefully acknowledge the financial support from
National Counsel of Technological and Scientific Development
(CNPq).

Nordic Pulp & Paper Research Journal Vol 28 no. 2/2013 300
PAPER PHYSICS
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Manuscript received November 26, 2012
Accepted March 27, 2013