CELLULOSE CHEMISTRY AND TECHNOLOGY

IMPROVING THE BLEACHING PROCESS OF HARDWOOD

CHEMI-MECHANICAL PULP
FARHAD ZEINALY,* MEHRAN KARIMI,** JALAL SHAKHES* and HOSEIN MOHAMMADI***
*

Young Researchers and Elite Club, Karaj Branch, Islamic Azad University, Karaj, Iran
Department of Pulp and Paper Industries, Faculty of Wood and Paper Engineering, Gorgan University of
Agricultural Sciences and Natural Resources, Gorgan, Iran
***
Department of Wood Composites, Faculty of Wood and Paper Engineering, Gorgan University of
Agricultural Sciences and Natural Resources, Gorgan, Iran
Corresponding author: Farhad Zeinaly, [email protected]

**

Received December 31, 2013

In the first phase, the effect of different NaOH to H2O2 ratios on bleaching chemi-mechanical pulp (CMP) was
investigated. The pH of unbleached pulp was 5.25 and its brightness and freeness were 37.5 and 745 ml respectively.
Results indicated that the brightness increased by growing the peroxide charge, but the increase in the NaOH
percentage had inhomogeneous effects. As data showed, the best brightness values were found with 0.75 NaOH/H2O2
ratios. High ratios led to a noticeable upward trend in pulp yellowness, while ratios below 0.75 resulted in lower
brightness. In the second phase, the effects of replacing NaOH by Mg(OH)2 were examined. Results showed that this
replacement determined an improvement in the optical properties and pulp yield. However, the mechanical properties
were similar in both processes. Also, this replacement led to a decrease in the Chemical Oxygen Demand (COD) and
conductivity in the bleaching effluent. The residual peroxide in the Mg(OH)2 bleaching process was higher than in the
NaOH bleaching process.
Keywords: bleaching, hydrogen peroxide, sodium hydroxide, magnesium hydroxide, Chemical Oxygen Demand,
bleaching effluent

INTRODUCTION
Alkaline peroxide bleaching is one of the most
common processes for high yield pulp bleaching.
In this process, the bleaching agent is a
hydroperoxide anion, which is produced by the
decomposition of hydrogen peroxide under
alkaline conditions, according to Equation 1:
H2O2 + OH H2O + HOO
(1)
As Equation 1 indicates, an alkaline
environment is needed to form an active
hydroperoxide anion.1 Also, alkaline conditions
lead to fiber swelling, which causes both
improving of bleach liquor penetration and
accessibility of the chromophore groups.
However,
high
concentration
of
the
hydroperoxide anions causes decomposition of
hydrogen peroxide, especially at elevated
temperatures (Eq. 2). Therefore, it is common
practice to add sodium silicate as a stabilizing and
buffering agent, and also, the pH value must be

controlled by changing the alkali ratio in the

bleach liquor.2
HOO + HOOH HO2 + HO + OH
(2)
Thus, very high pH should be avoided. The
optimum amount of caustic soda depends not only
on the amount of peroxide to be reacted, but also
on the temperature level and the retention time.3
Moreover, high contents of alkali substances, and,
then, high pH values bring about a phenomenon,
which has been called alkaline darkening in the
pulp bleaching process (Eq. 3).3,4 Hence, it is
necessary to find a suitable ratio of alkali to
peroxide in the bleaching process.
Lignin + OH chromophore groups
(3)
This ratio, which depends on the type of pulp,
chemical treatment in the pulping process,
bleaching process conditions etc., is about 0.6 to
0.8. In acid based pulps (acid pretreatments), the

Cellulose Chem. Technol., 50 (2), 285-292(2016)

FARHAD ZEINALY et al.

pH of the pulps is acidic (pH<7), and the

consumption of alkali is higher than with other
pulps.5,6 Actually, the initial and final pH in the
pulp bleaching process must be kept at an ideal
value, which for the pH in bleaching at 65 C to
70 C is typically between 8.5 and 9.0.3
The first phase of this research aimed to
investigate the effect of different chemical
consumption values on the optical and physical
properties of CMP, and also to find the best alkali
to peroxide ratio in the bleaching process of CMP.
In the second phase, the effect of replacing
caustic soda by magnesium hydroxide (in the
bleaching process) on the bleached pulp
properties was investigated. The alkali to peroxide
ratio, which was constant according to
calculations done in the first phase, was a
noticeable point in this phase. The peroxide
bleaching with Mg(OH)2 of high yield pulps has
been recently developed in the pulp and paper
industries.7 The associated benefit includes
decreased bleaching cost, decreased chemical
oxygen demand COD, less anionic trash, and
improved optical and physical strength properties
of the bleached pulps.8-10
The nucleophile destruction of conjugated side
chains and of quinones is complemented
favorably by the inability of the hydroperoxide
anion (HOO) to destroy aromatic rings. This
maintains a high proportion of lignin in the pulp
and keeps the opacity high. For bleaching
mechanical pulp, no other similarly simple and
inexpensive nucleophile chemical is available.
Electrophiles would react with the aromatic
structures and either remove lignin or generate the
potential for more chromophores. Today, the
main problem in peroxide bleaching is the amount
of organic material dissolved under the alkaline
bleaching
conditions.
Alkalization
with
magnesium hydroxide or calcium hydroxide can
be an alternative, as they dissolve less lignanes
and polyoses.3 The milder alkalinity of the
Mg(OH)2 system is believed to be the cause of
more effects of this alkali source on pulp and
bleaching process properties, such as the lower
COD formation. The higher COD values of
NaOH were attributed to its strong alkalinity; with
creating a high-pH environment, the longer chain
molecules in the pulp hydrolyze to smaller and
soluble ones.11 Another advantage of the
Mg(OH)2 alkali is its low solubility, which results
in a lower pH.12 The low solubility of Mg(OH)2
allows it to provide a constant alkalinity at
various alkali charges, and also pH values are

286

approximately constant during the bleaching,

while initial and final pH values mark a
significant difference in NaOH-based process.2
EXPERIMENTAL
Materials
Unrefined CMP from a mixture of some hardwoods
(sulfite process) was obtained from Mazandaran Wood
and Paper Company. The wood species used were
hornbeam, beech, and birch in a mixture percentage of
60, 20, and 20, respectively. The brightness of
unbleached pulp was 37.5% ISO, and its freeness was
745 ml (CSF). All chemicals used were of analytical
grade and all chemical charges were calculated based
on oven-dried pulp weight.
Chelation stage
Chelation of pulp was performed at 3% pulp
consistency, pH 4.5-5.5, and 70 C for 30 minutes,
with 0.3% DTPA (Diethylene Triamine Pentaacetic
Acid). Then, the pulp suspension was thickened to
about 25% consistency by 325-mesh Teflon screen.
The filtrate was recycled once to go through the fiber
mat to collect the fines.
Bleaching stage
Bleaching experiments were conducted in
polyethylene bags using the following conditions: 24% H2O2, 1.5-3.0% NaOH or 1.2-2.4% Mg(OH)2, 3%
sodium silicate (water glass), 0.2% Epsom salt
(MgSO4.7H2O), 0.1% DTPA, 10% pulp consistency,
70 C, and 120 minutes. The alkali source in the first
phase was just NaOH. Also, in this phase, the alkali to
peroxide ratio was not constant, as shown in Table 1.
In the second phase, the alkali to peroxide ratio was
constant, which means 0.75 for the NaOH-based
process, and 0.6 for the Mg(OH)2-based process (Table
2). The used values of Mg(OH)2 for hydroxyl ion
production, which was determined by acid titration,
were equal to NaOH in those treatments with the same
peroxide charges. The rate of magnesium hydroxide to
sodium hydroxide consumption was 0.8. The
chemicals were mixed in a beaker in the following
order: water, sodium silicate, sodium hydroxide or
magnesium hydroxide, Epsom salt, DTPA, and then
hydrogen peroxide. The prepared bleach liquor was
then added to the pulp, which had been heated to the
reaction temperature, and good mixing was provided
by kneading. The polyethylene bag was sealed and
placed into a water bath for the desired retention time
at the set temperature. After the completion of the
bleaching time, the pulp sample was cooled down with
cold running water to room temperature and diluted to
1% suspension with deionized water. The well-mixed
pulp suspension was then filtered by a 325-mesh
Teflon screen. The filtrate was recycled once to go
through the fiber mat to collect the fines. The resultant
filtrate was further filtered with a Whatman medium-

Chemi-mechanical pulp

fast filter paper to remove residual fines, and then used

for determining the conductivity and COD load of the
bleaching effluent.
Pulp mechanical testing
Bleached pulps were refined to a target freeness
(350 ml CSF), using a Labtech PFI machine according

to the TAPPI standard methods. Handsheets were

prepared and optical, physical and mechanical
properties were measured. All steps of handsheet
making and measurement of paper properties were
done according to the TAPPI standard methods.13

Table 1
First phase bleaching conditions
Treatment
code
A1
A2
A3
B1
B2
B3
C1
C2
C3

H2O2,
%
2
2
2
3
3
3
4
4
4

NaOH,
%
1.20
1.50
1.80
1.80
2.25
2.70
2.40
3.00
3.60

Alkali ratio
(NaOH/H2O2)
0.60
0.75
0.90
0.60
0.75
0.90
0.60
0.75
0.90

Table 2
Second phase bleaching conditions
Process type
NaOH-based process
Treatment code
A
B
C
H2O2, %
2
3
4
NaOH, %
1.50
2.25
3.00
Mg(OH)2, %
Alkali ratioa
0.75
0.75
0.75
a
NaOH or Mg(OH)2/H2O2

RESULTS AND DISCUSSION

First phase
In this phase, the ratio of alkali (NaOH/H2O2)
was investigated to modify the bleaching process
to gain the best properties of the bleached pulp.
As shown in Table 3, the optical properties of the
bleached pulps were raised by a peroxide charge
increase. Also, at equal peroxide charges, the
treatments at 0.75 alkali ratio showed the best
optical properties.
In the peroxide bleaching process, the alkali is
needed to activate hydrogen peroxide by forming
reactive hydroperoxide anion species. However, a
too high concentration of hydroperoxide anions,
with a high pH value, causes the decomposition of
hydrogen peroxide, especially at elevated
temperatures. Therefore, it is common practice to
add sodium silicate as a stabilizing and buffering
agent.2 Furthermore, a high level of alkaline
substances and accordingly, high pH values

Mg(OH)2-based process
D
E
F
2
3
4
1.20
1.80
2.40
0.60
0.60
0.60

determine the creation of new chromophore

groups in the pulp (Eq. 3).3,4 Hence, the
yellowness of the bleached pulp was increased by
intensifying the alkali rate at the same peroxide
charge (Table 3).
As shown in Table 3, the opacity of the
handsheets was decreased by raising the peroxide
charge for all alkali amounts, but the opacity
values had the least quantity at the alkali ratio of
0.75. Also, the opacity had an inverse relationship
with the brightness value and it increased along
with an increase in yellowness.
The opacity property of paper sheets is
influenced by thickness, porosity, value and type
of filler, bleaching degree of fibers, coating, and
the like.13 Porosity increases light scattering in
paper layers, thus, it reinforces the opacity. The
bonding area was enhanced, and so porosity
decreased, as the bleaching degree increased.

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FARHAD ZEINALY et al.

Figure 1 shows the yield of bleached pulp

under various bleaching conditions. At constant
peroxide levels, the yield of bleaching was
decreased by the increase in alkali charge.
The selectivity of the bleaching process is one
of the best factors to evaluate and to measure the
process efficiency. This factor is the rate of
brightness increase to yield loss, which is
determined by Eq. 4:

B.s. = (F.b. - I.b.)/Y.l.

(4)
where B.s.: Bleaching selectivity; F.b.: Final
brightness; I.b.: Initial brightness; Y.l.: Yield loss
(100-pulp yield).
The selectivity factor had the highest amount
at 0.75 alkali ratio (Fig. 2). Thus, the ratio of 0.75
was chosen as the optimum alkali ratio for the
second phase of hardwood CMP bleaching.

Table 3
Pulp optical properties in the first phase
Treatment
code
A1
A2
A3
B1
B2
B3
C1
C2
C3

Alkali
ratio
0.60
0.75
0.90
0.60
0.75
0.90
0.60
0.75
0.90

Brightness,
%
70.2
72.6
70.9
72.6
74.0
73.5
74.6
76.0
75.4

Opacity,
%
88.4
88.2
88.3
87.6
87.6
87.7
87.0
86.7
86.8

Yellowness
index
6.17
6.10
6.19
5.88
5.82
5.91
5.63
5.24
5.35
0.6 Alkali ratio

0.6 Alkali ratio

96.5

0.75 Alkali ratio

96.2
96.0

8.61

0.9 Alkali ratio

96
95.6

0.9 Alkali ratio

8.5

95.7

8.17 8.11

95.5
94.9

95

Selectivity

95.5
Yield, %

0.75 Alkali ratio

8.77

94.9
94.7

94.5

8
7.59
7.5

7.27 7.27
7.06

94.3

94

6.65

6.5

93.5

6
2

3
Peroxide charge, %

Figure 1: Yield of bleached pulps in the first phase

3
Peroxide charge, %

Figure 2: Bleaching selectivity in the first phase

Initial pH

13

Final pH
12

pH

11
10
9
8
7
6
A

B
NaOH-based process

Mg(OH)2-based process
Treatment code

Figure 3: Initial and final pH in the Mg(OH)2 and NaOH processes

288

Chemi-mechanical pulp

Table 4
Pulp optical properties at second phase
Process type
Treatment code
Brightness, %
Opacity, %
Yellowness index

NaOH-process
A
B
C
72.6
74.2
76.0
88.2
87.5
86.7
6.10
5.82
5.24

Second phase
Magnesium hydroxide is an alkali substance
consisting of one magnesium cation and two
hydroxide anions bound by an ionic bond. This
alkali has low solubility in water and so its
alkalinity is less than that of sodium hydroxide.14
In the conventional bleaching process (NaOH
alkali source), alkalinity or hydroxide anion
concentration was high at the beginning of
bleaching, as a result of the high solubility of
caustic soda in water (Fig. 3). The pH values in
this process were not constant during the reaction
time, so the highest and lowest values were
observed at the initial and final time, respectively.
The inhomogeneous pH has been reported to have
negative effects on pulp bleaching.2 A high
concentration of the hydroxide anion leads to an
increase in the hydroperoxide anion, and a too
high concentration of the hydroperoxide anions
causes the decomposition of hydrogen peroxide,
especially at elevated temperatures. Therefore, it
is a common practice to add sodium silicate as a
stabilizing and buffering agent. By using
Mg(OH)2 in the bleaching process, a
homogeneous pH will be established during pulp
bleaching, because this alkali has low solubility in
water (Fig. 3).
As shown in Table 4, the brightness values of
the Mg(OH)2-based process were higher than
those of the NaOH-based process at the same
H2O2 charge, but no significant difference in
opacity was observed between the two bleaching
processes. The yellowness values of the bleached
pulps by the Mg(OH)2-based process were lower
than those of the NaOH-based process at the same
H2O2 charge.
These results can be explained by the milder
alkalinity of Mg(OH)2, because of that, alkaline
darkening decreased. The phenomenon of alkaline
darkening appears because of a high
concentration of the hydroxide anion in the pulp
suspension environment.3,4 The low solubility of
Mg(OH)2 contributed to a constant alkalinity at
various alkali charges, and also as shown in
Figure 3, pH values were approximately constant

Mg(OH)2-process
D
E
F
73.2 75.9 77.8
88.1 87.3 86.5
5.75 4.73 4.11

during the bleaching process. Vice versa, the

sodium hydroxide is an excellently soluble alkali,
which leads to a heavy load of hydroxide anion in
the primary reaction. Thus, there was a significant
difference between initial and final pH in the
NaOH-based process, under these conditions new
chromophore groups were created in the pulp (Eq.
3).3
It may be noted from Table 5 that both
processes led to similar mechanical properties.
Also, the mechanical properties improved by
increasing the chemical charges. Factually, more
reactions and a more intense process under high
chemical charges resulted in a higher fiber
collapsibility and more bonding areas. Therefore,
the mechanical properties improved, and paper
bulk decreased.
According to Table 6, the Mg(OH)2-based and
the NaOH-based bleaching processes produced
bleached refined pulps with similar tensile and
burst strength. The tear strengths of the Mg(OH)2bleached pulps were higher than those of the
NaOH-bleached pulps. Little bleaching damage of
the Mg(OH)2-based process, as well as the higher
beating of the Mg(OH)2-bleached pulp led to an
increase in tear strength.15
Figures 4 and 5 indicate that the initial
freeness of the bleached pulps, and the refining
values to reach the target freeness (350 ml)
decreased by increasing the chemical charges for
both bleaching processes. Fiber swelling,
improvement of fiber collapsibility, removal of
hydrophobic compounds and creation of
hydrophilic functional groups upon a decrease in
the DP of macromolecules, as well as the
unbraiding structure of the fiber at high chemical
charges, are all possible reasons for this.12,16
Conventionally bleached pulps had lower
initial freeness than those of the Mg(OH)2-based
process (Fig. 4). Moreover, the refining values of
conventionally bleached pulps to reach the target
freeness were lower than those of the Mg(OH)2
bleached pulps (Fig. 5). These results can be
explained by the stronger reaction conditions of
the NaOH-based process and accordingly, the

289

FARHAD ZEINALY et al.

higher production of hydrophilic functional

groups and fiber swelling in this process.16-17
Figure 6 shows the yield of bleached pulp
under various bleaching conditions. Evidently, the
bleaching yield from the Mg(OH)2 process was
higher than that of the NaOH process. The
difference increased significantly as the chemical
charges rose because the bleaching conditions

were more severe for the NaOH process. For

example, at 4% peroxide charge, the bleaching
yield was 97.18% for the Mg(OH)2 process,
compared to 95.54% for the NaOH process. The
yield gained from the Mg(OH)2 process would
represent a significant economic benefit for the
pulp and paper factories that would adopt this
process.

Table 5
Mechanical properties of unrefined pulps
Process type
Treatment code
Tensile index (Nm/g)
Burst index (KN/g)
Tear index (mNm2/g)
Bulk (cm3/g)

A
31.1
2.21
6.67
2.42

NaOH-process
B
C
36.5
39.5
2.24
2.26
6.70
6.72
2.39
2.35

Mg(OH)2-process
D
E
F
30.9
35.8
39.2
2.19
2.22
2.26
6.66
6.72
6.74
2.43
2.40
2.36

Table 6
Mechanical properties of refined pulps
Process type
Treatment code
Tensile index (Nm/g)
Burst index (KN/g)
Tear index (mNm2/g)
Bulk (cm3/g)

NaOH-process
B
C
64.5
67.1
4.81
5.02
7.80
7.78
2.11
2.05

A
63.2
4.69
7.65
2.19

700

8600

682

678

8550

Mg(OH)2

8500

670
661
660

8400

8400
8350

8300

8300

645

8250

640

8200
8150

630
2

Figure 4: Initial freeness of Mg(OH)2 and NaOH

bleached pulps

Figure 5: Refining value of Mg(OH)2 and NaOH

bleached pulps
NaOH

97.79

98

Mg(OH)2
97.18

97.51
97.5

Yield, %

97
96.5

Peroxide charge, %

Peroxide charge, %

96.23
95.96

96

95.54

95.5
95
94.5
94
2

Peroxide charge, %

Figure 6: Pulp yield of Mg(OH)2 and NaOH processes

290

Mg(OH)2
8450

8450

671

650

NaOH

8550
8500

8500
PFI, rev.

Freeness, ml

NaOH

688

690
680

Mg(OH)2-process
D
E
F
63.9
64.6
66.8
4.72
4.84
4.98
7.91
7.98
8.02
2.21
2.11
2.06

Chemi-mechanical pulp

Table 7
Properties of the bleaching effluent in the second phase
Process type
Treatment code
Residual H2O2 (%)
COD (kg/t)
E.C (ms/cm)

NaOH-process
A
B
C
9.5
14.0
18.0
43.5
54.3
69.9
0.74
0.98
1.51

One of the main problems in alkaline peroxide

bleaching is the amount of organic material
dissolved under the alkaline conditions.
Alkalization with magnesium hydroxide can be an
alternative, as less lignanes and polyoses are
dissolved.3 The milder alkalinity of the Mg(OH)2
system is believed to have many effects on pulp
and bleaching process properties, such as the
lower COD formation.
The COD load of the filtrate from the
Mg(OH)2-based bleaching was 37-55% lower
than that from the NaOH process (Table 7). COD
may come from dissolved carbohydrates, lignin,
and other organic substances in the bleaching
filtrate.11 The decrease in COD indicates
preserving of pulp yield and lowering of effluent
clean-up requirements.18 With a noticeable
reduction in COD formation, the costs associated
with effluent treatment would be significantly
lower when using the Mg(OH)2-based process.
This prediction was confirmed by the results
obtained at a paper mill in Eastern Canada, which
realized a 25-40% reduction in effluent treatment
cost after implementing the Mg(OH)2 peroxide
bleaching process.11 Also, the electrical
conductivity (E.C.) values were very low in the
Mg(OH)2 system (Table 7), and remained
constant at higher consumption levels of
magnesium hydroxide. Less conductivity means
less ionic trash in the paper machines, and lower
retention aid requirements.2
The residual peroxide level in the Mg(OH)2
process is very high, as compared to NaOH
bleaching. There is a potential to recycle the
peroxide in the post-bleaching filtrate back into
the bleaching liquor;18 therefore, the total
peroxide consumption in the Mg(OH)2 process
would be lower than that of the conventional
process.
CONCLUSION
In the first phase, the best ratio of alkali to
peroxide was determined as 0.75. This alkali ratio
in constant peroxide charge resulted in the highest
brightness and the lowest yellowness and opacity

Mg(OH)2-process
D
E
F
14.2
20.5
26.5
27.3
29.6
31.8
0.36
0.43
0.47

of the bleached pulp. The bleaching selectivity

factor reached its highest value at the 0.75 alkali
ratio, upon a constant charge of NaOH.
In the second phase, the Mg(OH)2 peroxide
bleaching process produced bleached CMP with
better yield and optical properties, and similar
mechanical properties, in comparison with the
NaOH peroxide bleaching process. However, the
Mg(OH)2-based process led to higher tear
strength of the refined pulp samples, compared to
the conventional process. The refining value (350
ml freeness) of the NaOH bleached pulp samples
was lower than that of the Mg(OH)2 bleached
pulps. Also, the initial freeness of the NaOH
bleached pulps was lower than that of the
Mg(OH)2 bleached pulps.
The greatest advantage of magnesium
hydroxide over sodium hydroxide is its low
chemical oxygen demand (COD), which means
higher yield for the same reaction time and, in the
case of hardwood pulp bleaching, an increase in
bulk as well. At the different chemical charges of
the Mg(OH)2-based process, the residual peroxide
is considerably greater than that resulting from the
conventional process, indicating that the
Mg(OH)2
system
has
fewer
peroxide
decomposition reactions. Mg(OH)2 prevents some
of the hydroperoxide ion decomposition reactions,
by releasing alkali more slowly, due to its low
solubility.
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