CHARACTERISTICS OF PAPER MILL SLUDGE AND ITS UTILIZATION

FOR THE MANUFACTURE OF MEDIUM DENSITY FIBERBOARD

Xinglian Geng
NSERC Research Fellow

S. Y. Zhang†
Senior Scientist and Group Leader

and

James Deng*†
Research Scientist
Forintek Canada Corp.
319 rue Franquet
Saine-Foy, Québec
Canada G1P 4R4
(Received September 2005)

ABSTRACT
De-inking paper sludge (DPS) and primary sludge (PS) containing 20% secondary sludge from a paper
mill were characterized as to their suitability for the manufacture of medium density fiberboard. Com-
pared with DPS, PS had a lower ash content, higher holocellulose content, more and longer fibers, lower
pH, and higher buffering capacity. These characteristics make PS a better fiber resource for fiberboard
than DPS. Fiberboards were manufactured at the Pilot Plant of Forintek (Québec City, QC, Canada)
using virgin spruce-pine-fir fiber (SPF) and PS or DPS at different sludge/SPF weight ratios with 12%
urea-formaldehyde resin. At an equal sludge/SPF weight ratio, PS-SPF panels had much higher
mechanical properties than did DPS-SPF panels. At a PS/SPF weight ratio of 7:3, the mechanical
properties of PS-SPF panels were higher than the requirements of ANSI A208.2-2002 MDF standard for
Grade 120 in terms of internal bond strength, modulus of rupture, modulus of elasticity, and thickness
swelling. With DPS/SPF weight ratios as low as 3:7, the tested mechanical properties of DPS-SPF panels
could meet the require-ments of ANSI A208.2-2002 MDF standard for Grade 120.
Keywords: De-inking sludge, fiberboard, fiber properties, paper mill sludge, primary sludge, secondary
sludge, spruce-pine-fir.

INTRODUCTION and paper industry in Canada produces about 7.1

The forest products industry relies heavily on dry Mt/y of sludge and most of the sludge is
the natural forest, but the pressure to reduce for-est disposed through combustion and landfilling
harvesting is forcing the industry to look for (Beauchamp et al. 2002). How to dispose of or
alternative fiber resources. Sludge is the final solid make use of sludge has been a challenge for the
waste recovered from the wastewater treat-ment pulp and paper industry. Some efforts have been
process in pulp and paper mills. The pulp made to use paper mill sludge for value-added
products, such as gypsum fiberboards or fiber-
board additives ( Oztürk et al. 1992; Scott et al.
* Corresponding author. Forintek Canada Corp., 319, rue 2000; Takats and Simatupang 1993; Davis et al.
Franquet, Sainte-Foy, Québec, Canada G1P 4R4. Fax: +1-
418-659-2922. E-mail: james.deng@qc.forintek.ca 2003). Environmental concerns and governmen-
† Member of SWST. tal regulations coupled with increasing demand

Wood and Fiber Science, 39(2), 2007, pp. 345 – 351

© 2007 by the Society of Wood Science and Technology
346 WOOD AND FIBER SCIENCE, APRIL 2007, V. 39(2)

for fiber materials are encouraging the forest panels were manufactured with or without
products industry to utilize this potential fiber virgin fibers at the MDF Pilot Plant of Forintek
resource for wood fiber-based composite panels. Canada Corp.
Fiberboard panels are one of the most commonly
used furniture and building materials, and the MATERIALS AND METHODS
consumer demand for fiberboard panels has been
increasing over the years. Materials
Sludge discharged from paper mills is divided De-inking paper sludge and PS were
into four categories: 1) primary sludge (PS), which collected from Papiers Stadacona Ltée. in
comes from the production of virgin wood fiber; Quebec City, Canada. The PS was mixed with
2) de-inking paper sludge (DPS), which comes about 20% sec-ondary sludge when it was de-
from the process of removing inks from recycled watered in the paper mill. A urea-formaldehyde
paper; 3) secondary sludge (SS; activated sludge), resin (UF-105) was obtained from Borden
which comes from the second-ary wastewater Chemical Canada Inc. (Quebec, Canada).
treatment system; and 4) com-bined primary and
secondary sludge. Total solid sludge produced by
the Canadian pulp and paper industry comprises Preparation of raw materials for
42% PS, 12% DPS, 26% SS, and 18% combined chemical analysis
sludge (Reid 1997). Primary sludge accounts for The moisture contents of PS and DPS were
the majority of the total solid, and attempts have determined according to ASTM standard (ASTM
been made to use it for hardboard manufacture 1999). The sludge samples were then air-dried for
(Oztürk et al. 1992; Eroglu and Saatci 1993). one week and screened to remove plastic, glass,
Satisfactory hardboard was produced at a 1:4 and other contaminating materials. The screened
weight ratio of PS to wood fiber. De-inking sludge raw materials were ground in a Wiley mill fitted
has been characterized and investigated for use in with a 35-mesh (0.5-mm) screen, and the portion
building materials or fiberboard (Nadelman and that passed the screen was collected. The collected
Newton 1960; Davis et al. 2003). Secondary material was placed in an airtight container to
sludge has been ex-cluded by many researchers balance the moisture content and then used for
because of its bio-logical activity (Scott et al. chemical analysis.
2000). However, it has been reported that
hydrothermally-heated activated sludge could be
used as a binder in the production of hardwood Determination of chemical composition
fiberboard (Lavrent’ev et al. 1978). The use of the of sludge
treated activated sludge enhanced the flexural Ash content, klason lignin content, and holo-
strength of the fi-berboards by 23–32%. cellulose content were determined according to
Tappi Standards (Tappi Test Methods 1993,
Limited information is available on the suit- Tappi Test Methods 1998, Tappi Useful Meth-
ability of sludge for the manufacture of fiber- ods 249 1976).
board. In addition, the properties of fiberboard
made from different kinds of sludge have not been
compared. This study was intended for ex-amining Determination of pH and buffering capacity
the suitability of various sludge for the The value of pH and buffering capacity were
manufacture of fiberboard. DPS and PS were determined with a procedure similar to the pre-
obtained from a paper mill in Quebec City, viously reported method (Johns and Niazi 1980).
Canada. The composition and fiber properties In brief, the sludge sample (25 g, oven-dried) was
were analyzed and their suitability for the manu-
refluxed in 250 ml of distilled water for 20
facture of fiberboard was evaluated in this study.
minutes and then filtered with Whatman #1 filter
The raw materials were refined, and fiberboard
paper. The residue was washed with about 100
 Geng et al.—PAPER MILL SLUDGE FOR MANUFACTURE OF MDF 347

ml of distilled water, and the filtrate was made up Manufacture of fiberboard panels
to 500 ml with distilled water. Before the
determination of pH and buffering capacity, the To investigate the effect of the weight ratio of
pH meter was calibrated with standardized buffer SPF to sludge on panel properties, panels were
solutions at pH 4.0 and pH 7.0. For the manufactured using 100% SPF, 100% sludge, and
determination of pH, 50 ml of the extract solu-tion SPF:sludge weight ratios of 3:7 and 7:3. The
was pipetted into a 150-ml beaker. The pH value refined raw materials were mixed at the various
was recorded when the pH meter indicated a DPS/SPF or PS/SPF ratios, and then 12% urea-
constant value. After pH determination, the extract formaldehyde resin (UF105) was applied to the
solution was titrated with 0.025N NaOH solution dry fibers. For each condition, two panels of 610
to pH 8.0 for the determination of acid buffering mm × 610 mm × 10 mm and a density of 950
capacity or with 0.025N H2SO4 solu-tion to pH kg/m3 were made. Press temperature was set at
3.0 for calculation of base buffering capacity. The 180°C and pressing time was 5 minutes.
acid buffering capacity is defined as the quantity
(mmol) of NaOH required to raise the pH of the
solution extracted from 100 grams of oven-dried Test of fiberboard panel properties
sample to pH 8. Similarly, the base buffering
capacity is defined as the quantity (mmol) of
The panels were conditioned at 65 ± 1% rela-
tive humidity and 20 ± 3°C for one week. The
H2SO4 required to lower the pH of the solution internal bonding (IB), modulus of rupture
extracted from 100 grams of oven-dried sample to (MOR), modulus of elasticity (MOE), and
pH 3.0. thick-ness swelling (TS) were tested according
to ASTM standard (ASTM 1999).
Determination of fiber and
particle
size distribution RESULTS AND DISCUSSION
Primary sludge and DPS as received were
suspended in water and then scanned with Characteristics of PS and DPS
QualScanTM (McCarthy Products Company, The moisture contents of DPS and PS were
Seattle, WA, USA) for fiber length and area dis- 61.9% and 193.2%, respectively. As shown in
tributions. Table 1, PS had a much higher moisture content
than did DPS after having been air-dried for the
Refining of raw materials same duration of time (one week). Primary sludge
For the dry process of manufacturing fiber-
board, the moisture contents of the sludge TABLE 1. Characteristics of primary sludge and de-inking
samples as received were too high, and the paper sludge.
sludge had to be dried before panel-making.
PS DPS
Pre-vious research showed that many clumps
Moisture, % 8.18 2.91
were formed after air-or oven-drying and the Ash content of oven-dried
resulting clumps were not easy to break by sample, % 19.50 53.62
blending. Therefore, DPS, PS, and spruce-pine- Klason lignin content of
fir (SPF) samples were refined at steam pressure oven-dried sample, % 27.84 25.69
of 0.75 MPa with pre-heating retention time of Holocellulose content of
oven-dried sample, % 62.73 42.88
3 min-utes and 2500 rpm of refiner speed at the pH 5.65 7.01
MDF pilot plant of Forintek Canada Corp. in Acid buffering capacity,
Quebec City, Canada. The refining process not mmol NaOH/100 g o.d. sample 2.71 0.17
only separated fibers and fines (short fibers and Base buffering capacity,
inor-ganic materials) very well, but also refined mmol H2SO4/100 g o.d. sample 5.18 5.11
the knots in the sludge samples.
348 WOOD AND FIBER SCIENCE, APRIL 2007, V. 39(2)

contained more klason lignin and holocellulose

than DPS. However, DPS had a much higher ash
content than did PS. Paper mill sludge is a mix-
ture of mainly cellulose fibers and inorganic ma-
terials. A higher holocellulose content and a much
lower ash content in PS indicate that it contained
more cellulose fibers than did DPS. Cellulosic
material absorbs more water than in-organic
material, a factor that will directly affect the
dimensional stability of fiberboards. PS had a
lower pH and much higher acid buffering ca-
pacity than did DPS. Their base buffering ca-
pacities were comparable. A lower pH and higher
acid buffering capacity of PS might pro-vide a
better environment for the curing of UF resin FIG. 2. Length distributions of fibers and particles in
primary sludge and de-inking paper sludge.
during the panel-making process than would DPS
(Johns and Niazi 1980), which might further affect
panel strength. same sludge/SPF ratio, PS-SPF panels had a
As illustrated in Fig. 1, DPS contained more higher IB than did DPS-SPF panels. To deter-
fibers and particles with areas of #0.16 mm2, mine the relationship between IB and sludge
but fewer fibers and particles with areas $0.29 proportion, IB was regressed against sludge
mm2 than did PS. More importantly, PS con- per-centage. The relationship of IB-sludge
tained longer fibers ($0.54 mm) than did DPS percent-age was found to be linear and inverse
(Fig. 2). with an R2 as shown in Table 2. Internal
bonding of the PS-only panels was higher than
the require-ment of ANSI A208.2-2002 MDF
Effect of sludge and SPF standard for Grade 130 (ANSI 2002).
weight ratio on A lower pH and higher acid buffering capac-
internal bonding ity of PS promote the development of IB by
providing a better environment for the curing of
As shown in Fig. 3, an increase in the weight UF resin during the pressing process. A higher
ratio of PS to SPF resulted in a decrease in IB.
Similarly, an increase in the weight ratio of DPS
to SPF also resulted in a decreased IB. At the

FIG. 1. Area distributions of fibers and particles in pri- FIG. 3. Effect of the weight ratio of sludge to SPF on
mary sludge and de-inking paper sludge. internal bonding.
 Geng et al.—PAPER MILL SLUDGE FOR MANUFACTURE OF MDF 349

TABLE 2. R2 of linear regression of panel properties against PS-SPF panels had a higher MOR than did
sludge percentage of all fibrous raw materials (sludge and DPS-SPF panels. At a 7:3 of PS:SPF weight
SFP).
ratio, the MOR of PS-SPF panels was higher
PS DPS than the re-quirement of ANSI A208.2-2002
Internal bonding 0.76 0.80 MDF standard for Grade 120.
MOR 0.99 1.00
MOE 0.68 1.00
Thickness swelling 0.45 0.98 Effect of sludge and SPF weight ratio on the
panel MOE
content of inorganic substances in DPS might As shown in Fig. 5, the MOE of PS-SPF and
obstruct the development of board strength DPS-SPF panels decreased with increased weight
(Grigoriou 2003). About 15 – 20% secondary ratio of sludge to SPF. MOE was re-gressed
sludge is always mixed with PS when it is de- against the sludge percentage of fibrous raw
watered and discharged by the paper mill. As materials. The relationship of MOE-DPS
stated above, secondary sludge contained in the percentage was found to be linear and inverse
received PS might contribute to the mechanical
with R2 1.00, but the R2 of the linear regres-sion
strength of PS-SPF panels.
of MOE-PS percentage was only 0.68 (Table 2).
At the same weight ratio of sludge to SPF, PS-SPF
Effect of sludge and SPF weight panels had a higher MOE than did DPS-SPF
ratio on the panels. Even if the panels were made with 100%
panel MOR PS as fibrous raw material, the MOE of the panels
was still higher than the require-ment of Grade
The effect of the sludge and SPF weight ratio 120 in ANSI A208.2-2002 MDF standard. To
on the panel MOR is illustrated in Fig. 4. In- obtain a satisfactory MOE accord-ing to the same
creasing PS or DPS proportion in the panels re- standard, as much as 30% DPS could be used as
sulted in a decreased MOR, and the decreases fibrous raw material.
seen with DPS-SPF panels were more signifi- Studies on fiber size distribution of PS and DPS
cant than those seen with PS-SPF panels. MOR indicated that PS contained more and longer fibers
was regressed against the sludge percentage of than did DPS. Cellulose fibers have a relatively
the fibrous raw materials, and the relationship
high length-to-coarseness ratio, and much of the
of MOR-sludge percentage was found to be
fiberboard strength is derived from the fibers. This
linear and inverse with a very high R2 as shown explains why PS panels had
in Table 2. At the same ratio of sludge to SPF,

FIG. 4. Effect of the weight ratio of sludge to SPF on FIG. 5. Effect of the weight ratio of sludge to SPF on
MOR. MOE.
350 WOOD AND FIBER SCIENCE, APRIL 2007, V. 39(2)

CONCLUSIONS

Primary sludge mixed with 20% secondary

sludge contained more and longer fibers than did
DPS, and it had a much lower ash content. Com-
pared to DPS, PS also had a lower pH but higher
acid buffering capacity. These properties made PS
more suitable as a fiber material for the
manufacture of fiberboard than DPS. At the equal
weight ratio of sludge to SPF, MDF panels made
of PS and SPF had much higher mechani-cal
properties than did DSP-SPF panels. The di-
mensional stability could be further improved by
the application of wax. With 12% UF resin, it is
FIG. 6. Effect of the weight ratio of sludge to SPF on possible to replace 70% of SPF fiber with PS fiber
thickness swelling. or 30% of SPF fiber with DPS fiber in the
manufacture of MDF and the panel properties
meet the ANSI A208.2-2002 standard for Grade
much higher MOR and MOE than did DPS pan- 120. This study showed that PS had an excellent
els when other process parameters were held potential for the manufacture of fiberboard.
constant.

REFERENCES
Effect of sludge and SPF
AMERICAN NATIONAL STANDARDS INSTITUTE (ANSI). 2002.
weight ratio on Median Density Fiberboard (MDT) for Interior Applica-
thickness swelling tions. ANSI A208.2-2002. Composite Panel Association,
Gaithersburg, MD.
As illustrated in Fig. 6, TS of DPS-SPF panels ASTM STANDARD D1037-99. 1999. Standard test methods
were slightly improved when DPS content in- for evaluating properties of wood-base fiber and particle
creased. With the addition of PS to SPF, TS also panel materials.
BEAUCHAMP, C. J., M.-H. CHAREST, AND A. GOSSELIN. 2002.
increased, but the difference was not significant. Examination of environmental quality of raw and com-
Increase in PS content from 30% to 100% did not posting de-inking paper sludge. Chemosphere 46:887 –
result in a further increase in TS. To deter-mine 895.
the relationship between TS and the weight ratio DAVIS, E., S. M. SHALER, AND B. GOODELL. 2003. The incor-
of sludge to SPF, TS was regressed against the poration of paper deinking sludge into fiberboard. Forest
sludge percentage. The relation between TS and Prod. J. 53(11/12):46 – 54.
EROGLU˘, V., AND A. M. SAATÇI. 1993. Reuse of sludge from
DPS percentage was linear with R 2 0.98, but the pulp and paper industry pilot and full scale applications.
R2 of linear regression on TS against PS Water Sci. Technol. 28(2):17 – 26.
percentage was only 0.45 (Table 2). PS-SPF GRIGORIOU, A. H. 2003. Waste paper-wood composites
bonded with isocyanate. Wood Sci. Technol. 37:79 – 89.
panels had a higher TS than did DPS-SPF panels
JOHNS, W. E., AND K. A. NIAZI. 1980. Effect of pH buffering
at the same weight ratio of sludge to SPF. This capacity of wood on the gelation time of urea-
could be explained by the difference in their formaldehyde resin. Wood Fiber 12:255 – 263.
chemical composition. A higher mineral content LAVRENT’EV, S. P., S. N. DMITRIEV, Y. I. CHERNOUSOV, V. A.
and a lower holocellulose content in DPS has been KOLMOGORTSEV, AND V. S. STARTSEV. 1978. Study of the
shown to contribute to the reduced swelling of possibility of using activated sludge in the production of
manufactured boards (Grigoriou 2003). fiberboards. Pages 64 – 68 in V. F. Filatenkov, ed.
Vodopol’zovanie Ochistka Proizvod. Stochnykh Vod.
In comparison, TS of all panels were slightly Vses. Nauchno-Issled. Inst. Tsellyul.-Bum. Prom-sti.
higher than the requirement of ANSI A208.2- Leningrad, USSR.
2002 MDF standard. However, this problem NADELMAN, A. H., AND L. P. NEWTON. 1960. A
could be solved by the application of wax. practical ap-
 Geng et al.—PAPER MILL SLUDGE FOR MANUFACTURE OF MDF 351

proach to utilization of solids from deinking mill effluent. Bull. NO.814. Ed. National Council for Air and Stream
Tappi J. 43:120 – 128. Improvement, USA.
ÖZTÜRK, I., V. EROG˘LU, AND A. BASTÜRK. 1992. Sludge uti- TAKATS, P., AND M. H. SIMATUPANG. 1993. Suitability of fi-ber
lization and reduction experiences in the pulp and paper sludge as reinforcing material for manufacturing of
industry. Water Sci. Technol. 26:2105 – 2108. gypsum fiberboards. Inorganic-bonded Wood Fiber
REID, I. 1997. Solid residues generation and management Comp. Mater. 3:97 – 103.
by Canadian pulp and paper mills in 1995. TAPPI TEST METHODS. 1993. T211 0m-93, Ash in wood and
Miscellaneous report MR 352. Ed. Pulp and Paper pulp.
Research Institute of Canada, Pointe-Claire, Canada. ———. 1998. T222 om-98, Acid-insoluble lignin in wood
SCOTT, C. T., J. SIMONSEN, D. KLINGENBERG, AND S. ZAUSCHER. and pulp.
2000. Beneficial use of pulp and paper industry residuals: TAPPI USEFUL METHODS. 1976. 249, Delignification of un-
extrusion for the manufacture of building panels. Tech. bleached pulp (chlorine gas method).