Note: Descriptions are shown in the official language in which they were submitted.
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PROCESS FOR MAI~IIdG PAPER
BACIKGROUND OF THE INVENTION
The present invention relates to papermaking pulps, papermaking processes
employing
S the pu.ips, and paper and paperboard products made from the pulps. More
particularly, the
present invention relates to treating papermaling pulp with at least one
microparticle-
containing retention aid system.
Microparticles and other particulate materials have been added to papermaking
pulps
as retention aids. For example, U.S. Patent No. 4,798,653 to Rushmere,
describes a
paperrnaking stock including cellulose fibers and a two-component combination
of an
anionic polyacrylamide and a cationic colloidal silica sol.
One problem with microparticle sols that have been employed in papermaking
pulps
has been with instability. Because of the instability of sots used in
connection with
papemiaking pulps, the sols are often made on-site for immediate delivery to a
papermaking
process. A need exists for a stable microparticle sol retention aid for use in
papermaking
processes which can be formed off site, exhibits a long shelf life, and can be
shipped to a
paperrnaking plant for immediate or future use in a papermaking process.
A need also exists for a papermaking pulp that exhibits even better retention
of fines
and even better resistance to shear forces during a papermaking process. A
need also exists for
a papermaking pulp that produces a paper or paperboard product with improved
strength
' characteristics.
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SUMMARI' OF THE INVENTION .
The present invention relates to the use of a combination of fibrous cationic
colloidal
alumina microparticles and at least one polymer as a retention aid system for
a papermaking
pulp or stock. The fibrous cationic colloidal alumina microparticles can
preferably be a
cationic fibrous acetate salt of boehmite alumina. The fibrous product can be
obtained by
stirring a slurry of water and basic alumina acetate to ensure substantially
complete mixing
thereof, and then reacting the slurry to produce a fibrous cationic acetate
salt of boehmite
alumina preferably having a zeta potential, when measured in deionized water,
of greaterthan
about :LS and preferably having a weight ratio of alunnina to acetate of less
than about 4. The
surface; area to volume ratio ofthe salt is preferably about 50% or greater.
The polymer cm be
a cationic polymer, a nonionic polymer, or an amphoteric polymer used under
cationic
conditions. The polymer is preferably a synthetic nitrogen-containing cationic
polymer, for
example, a cationic polyacrylamide. If nonionic, the polymer can be, for
example, a nonionic
polyac~ylamide or a polyethylene oxide.
The present invention also relates to papermaking pulp or stock that includes
fibrous
cationic, colloidal alumina mieropartieles in combination with at least one
polymer as a
retention aid system.
Exemplary fibrous boehmite alumina microparticles suitable for use in the
retention
aid system of the present invention include the fibrous alumina products
obtainable by the
processes described in U.S. Patent No. 2,915,475 to Bugosh, and those
described in VJO
97/41063. The fibrous cationic colloidal alumina microparticles are preferably
very
stable, preferably have a long shelf life, and preferably can be made off site
and then
shipped to a paper mill for future use.
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The pulps or stocks of the present invention may also contain or be treated
with at least one
coagulant, at least one flocculant, at least one filler, at least one
polyacrylamide, at least one
cationic starch, at least one enzyme, and/or other conventional papermaking
pulp additives.
The resulting pulp or stock is then formed into a wet sheet of pulp or stock
having improved
retention properties compared to a wet sheet made of conventionally treated
pulp. After
drainage and drying, the resulting paper or paperboard preferably exhibits
excellent
opaqueness and/or other physical properties.
It is to be understood that both the foregoing general description and the
following
detailed description are exemplary and explanatory only and are only intended
to provide a
further explanation of the present invention, as claimed. The accompanying
drawings, which
are incorporated in and constitute a part of this application, illustrate
several exemplary
embodiments of the present invention and together with description, serve to
explain the
principles of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
Fig. 1 is a flow chart showing a papermaking process according to an
embodiment of
the present invention;
Fig. 2 is a flow chart showing a papermaking process according to another
embodiment of the present invention;
Fig. 3 is a flow chart showing a papermaking process according to another
embodiment of the present invention;
Fig. 4 is a bar graph comparing the turbidity of various exemplary and
comparative
paperstock formulations;
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Fig. 5 is a bar graph showing the time to achieve drainage of 200 mI of
filtrate from
paperwebs made of various exemplary and comparative paperstock formulations;
Fig. 6 is a bar graph showing the drainage in seconds of various exemplary and
comparative paperstock formulations;
Fig. 7 is a bar graph showing the turbidity of various exemplary and
comparative
paperstock formulations;
Fig. 8 is a bar graph showing the drainage in seconds of various exemplary and
comparative paperstock formulations;
Fig. 9 is a bar graph showing the %TFPR of various exemplary and comparative
paperstock formulations;
Fig. 10 is a bar graph showing the %FPAR of various exemplary and comparative
paperstock formulations;
Fig. 11 is a bar graph showing the freeness in ml of various exemplary and
comparative paperstock formulations;
Fig. 12 is a bar graph showing the %TFPR of various exemplary and comparative
paperstock formulations;
Fig. 13 is a bar graph showing the %TFPR of various exemplary and comparative
paperstock formulations;
Fig. 14 is a bar graph showing the %FPAR of various exemplary and comparative
paperstock formulations;
Fig. 15 is a bar graph showing the %TFPR of various exemplary and comparative
paperstock formulations;
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Fig. 16 is a bar graph showing the %FPAR of various exemplary and comparative
paperstock formulations;
Fig. ~17 is a bar graph showing the %TFPR of various exemplary and comparative
paperstock formulations;
Fig. 18 is a bar graph showing the %FPAR of various exemplary and comparative
paperstock formulations;
Fig. 19 is a bar graph showing the %TFPR of various exemplary and comparative
paperstock formulations;
Fig. 20 is a bar graph showing the %FPAR of various exemplary and comparative
paperstock formulations;
Fig. 21 is a bar graph showing the %TFPR of various exemplary and comparative
paperstock formulations;
Fig. 22 is a bar graph showing the %TFPR of various exemplary and comparative
paperstock formulations;
Fig. 23 is a bar graph showing the %FPAR of various exemplary and comparative
paperstock formulations;
Fig. 24 is a bar graph showing the %TFPR of various exemplary and comparative
paperstock formulations;
Fig. 25 is a bar graph showing the %TFPR of various exemplary and comparative
paperstock formulations; and
Fig. 26 is a bar graph showing the seconds required to drain 400 rril of
filtrate from
paperwebs made from various exemplary and comparative paperstock formulations.
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DETAILED DESCRIPTION OF THE PRESENT INVENTION
The present invention relates to the use of a combination of fibrous cationic
colloidal
alumina microparticles and a polymer as a retention aid system for a
papermaking pulp. More
than one type of microparticle can be used and more than one type of polymer
can be used.
Paper and paperboard products made according to the method preferably exhibit
excellent
opaqueness and/or other desirable physical properties. Sheets of pulp from
which the paper
and paperboard products are made preferably exhibit excellent drainage and/or
excellent
retention of pulp fines.
The fibrous cationic colloidal alumina microparticles can preferably be a
cationic
fibrous acetate salt of boehmite alumina. The fibrous product can be obtained
by stirring a
slurry of water and basic alumina acetate to ensure substantially complete
mixing thereof, and
then reacting the slurry to produce a fibrous cationic acetate salt of
boehmite alumina. The
fibrous microparticles preferably have a zeta potential of greater than about
25 and/or
preferably have a weight ratio of alumina to acetate of less than about 4. The
surface area to
volume ratio of the salt is preferably about 50% or greater.
The fibrous cationic colloidal alumina microparticles can be added in any
amount
sufficient to improve the retention of fines when the pulp or stock is formed
into a wet sheet
or web. Preferably, the fibrous cationic colloidal alumina microparticles axe
added in an
amount of at least about 0.05 pound per ton of paperstock, based on the dried
solids weight of
both the microparticles and the paperstock, and more preferably in an amount
of at least about
0.2 pound per ton of paperstock. Even more preferably, the fibrous cationic
colloidal alumina
microparticles are added in an amount of from about 0.3 pound per ton of
paperstock to about
5.0 pounds per ton of paperstock, for example, from about 0.3 pound to about
1.0 pound per
i . i
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wo ouh,sz~7 pcT/usonnm,><
ton, based on dried solids weight of the paperstock. For purposes ofthis
patent application, the
terms "pulp", "stock", and "paperstock" are used interchangeably.
Exemplary fibrous boehmite alumina microparticles suitable for use in the
retention
aid system of the present invention include the fibrous alumina products
described in U.S.
Patent No. 2,915,475 to Bugosh, and those described in WO 97/41063. The
fibrous
cationic colloidal alumina microparticles preferably have one or more of the
following
benefiits: they are very stable; they have a long shelf life; and/or they can
be made off
site arid then shipped to a paper mill for future use. The pulps or stocks of
the present
invention may also contain or be treated with at least one coagulant, at least
one
flocculant, at least one filler, at least one polyacrylamide, at least one
cationic starch,
at least one enzyme, and/or other conventional papermaking pulp additives, or
combinations thereof. The resulting pulp or stock is then formed into a wet
sheet of
pulp or stock and preferably has improved retention properties compared to a
wet
sheet made with no microparticles or polymer. After drainage and drying, the
resulting paper or paperboard preferably exhibits excellent opaqueness and/or
other
I S physical properties.
The polymer is preferably added to the papermaking pulp after addition of the
fibrous
cationic colloidal alumina microparticles, though any order of addition can be
used.
Preferably, the polymer can be any polymer which does not adversely affect the
formation of
pulp or paper. Preferably, the polymer is a medium to high molecular weight
synthetic
polymer, for example, a cationic nitrogen-containing polymer such as a
cationic
polyac~ylarnide. The polymer can be cationic, nonionic, or amphoteric. If
amphoteric, the
polymer is preferably used under cationic conditions. At least one other
polymer of any kind
can be used in addition to the polymers recited above so long as the at least
one other polymer
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does not substantial 1y adversely affect the retention properties of the
present invention. The at
least one other polymer can preferably be a polyamidoamineglycol (PAAG)
polymer.
The polymer preferably has a molecular weight in the range of from about
100,000 to
about ?5,000,000, and more preferably from about 1,000,000 to about
1S,000,000, though
other :molecular weights are possible.
The polymer can preferably be a high molecular weight linear cationic polymer
or a
crossliinked polyethylene oxide. Exemplary high molecular weight linear
cationic polymers
and shear stage processing suitable for use in the pulps and methods of the
present invention
are described in U.S. Patent Nos. 4,753,710 and 4,913,775.
The polymer is preferably added before the various significant shear steps of
the
papernnaking process. The fibrous cationic colloidal alumina microparticles
can be added
before or after the various significant shear steps of the papermaking
process. According to
some c;mbodiments of the present invention, the polymer can be added before
the fibrous
cationic colloidal alumina microparticles and before at least one significant
shear step in the
papermaking process. If the polymer is added before the fibrous cationic
colloidal alumina
microparticles, the microparticles can be added before or after a final shear
step of the
papermaking process. Although it is preferable to add the polymer to the
papermaking pulp
before the last shear point in the papermaking process, the polymer can be
added after the last
shear point.
The fibrous cationic colloidal alumina micropartieles preferably form bridges
or
networks between various particles. The polymer is preferably partially
attached (e.g.,
adsorbed) onto the surfaces of particles within the stock and can provide
sites of attachment.
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Aqueous cellulosic papermaking pulp or stock can be treated by first adding
the
polymer to the pulp or stock, followed by subjecting the paper stock to high
shear conditions,
followed by the addition of the fibrous cationic colloidal alumina
microparticles prior to sheet
formation. As discussed above, the polymer can be cationic, nonionic, or
amphoteric under
cationic conditions. Alternatively, the polymer can be added simultaneously
with the fibrous
cationic colloidal alumina microparticles.
Preferred cationic polyacrylamides for use as the retention system polymer are
described in more detail below. If a cationic polyacrylamide is used as the
cationic polymer,
the cationic polyacrylamide can have a molecular weight in excess of 100,000,
and preferably
has a molecular weight of from about 1,000,000 and 18,000,000. The combination
of the
polymer and the fibrous cationic colloidal alumina microparticles preferably
provides a
suitable balance between freeness, dewatering, fines retention, good paper
formation, strength,
and resistance to shear.
The polymer composition of the retention system is added in an amount
effective to
preferably improve the drainage or retention of the pulp compared to the same
pulp but having
no polymer present. The polymer is preferably added in an amount of at least
about 0.05
pound of polymer per ton of paperstock (or pulp), based on the weight of dried
solids of both
the polymer and the paperstock, and more preferably in an amount of at least
about 0.1 pound
per ton of paperstock. The polymer can be added in an amount of from about 0.2
pound per
ton of paperstock to about 2.5 pounds per ton of paperstock, based on the
dried solids weight
of the paperstock, though other amounts can be used.
If the polymer is a cationic polymer or an amphoteric polymer under cationic
conditions, the polymer is preferably added in an amount of from about 5 grams
to about 500
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grams per ton of paperstock on a dry basis, more preferably from about 20
grams to about 200
gram:., and even more preferably from about 50 grams to about 100 grams per
ton of
paper;stock on a dry basis, though other amounts can be used.
If the polymer is cationic, any cationic polymer or mixture thereof can be
used and
preferably conventional cationic polymers commonly associated with papermaking
can' be
used i.n the pulps or stocks of the present invention. Examples of cationic
polymers include,
but are not limited to, cationic starches and cationic polyacrylamide
polymers, for example,
copol~~rners of an acrylamide with a cationic monomer, wherein the cationic
monomer may be
in a neutralized or quatennized form. Nitrogen-containing cationic polymers
are preferred.
Exemplary cationic monomers which may be copolymerized with acrylamide to form
prefer~~ed cationic polymers useful according to the present invention,
include amino alkyl
esters .of acrylic or methacrylic acid, and diallylamines in either
neutralized or quaternized
form. l~xemplary cationic monomers and cationic polyacrylamide polymers are
described in
U.S. Portent No. 4,894,119 to Baron, Jr., et al.
The polymer may also be a polyacrylamide formed from comonomers that include,
for
example, 1-trimethylammonium-2-hydroxypropylmethacrylate methosulphate. Other
exarnpiLes of cationic polymers, include, but are not limited to, homopolymers
ofdiallylamine
monomers, homopolymers of aminoallylesters of acrylic acids, and polyamines,
as described
in U.S. Patent No. 4,894,119. Co-polymers, ter-polymers, or higher forms of
polymers may
also be used. Further, for purposes of the present invention, a mixture of two
or more
polymers may be used.
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In embodiments wherein the polymer contains a cationic polyacrylamide,
nonionic.
acrylamide units are preferably present in the copolymer, preferably in an
amount of at least
about 30 mol% and generally in an amount of no greater than 95 mol%. From
about 5 mol%
to about 70 mol% of the polymer is preferably formed from a cationic
comonomer.
The papermaking pulp or stock can be any conventional type, and, for instance,
can
contain cellulose fibers in an aqueous medium at a concentration of preferably
at least about
50% by weight of the total dried solids content in the pulp or stock. The
retention system of
the present invention can be added to many different types of papermaking
pulp, stock, or
combinations of pulps or stocks. For example, the pulp may comprise virgin
and/or recycled
pulp, such as virgin sulfite pulp, broke pulp, a hardwood kraft pulp, a
softwood kraft pulp,
mixtures of such pulps, and the like.
The retention aid system can be added to the pulp or stock in advance of
depositing the
pulp or stock onto a papermaking wire. The pulp or stock containing the
retention aid system
has been found to exhibit good dewatering during formation of the paperweb on
the wire. The
pulp or stock also exhibits a desirable high retention of fiber fines and
fillers in the paperweb
products under conditions of high shear stress imposed upon the pulp or stock.
In addition to the retention aid system used in accordance with the present
invention,
the papermaking pulp or stock according to the present invention may further
contains other
types of microparticles, for example, a synthetic hectorite microparticle
additive. One or more
different types of secondary microparticle additives, different from the
fibrous cationic
colloidal alumina microparticles, may be added to the pulp at any time during
the process. The
secondary microparticle additive can be a natural or synthetic hectorite,
bentonite, zeolite,
non-acidic alumina sol, or any conventional particulate additives as are known
to those skilled
i
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in the art. Exemplary synthetic hectorite microparticle additives include
LAPONITE available
from Laporte Industries, and the synthetic microparticles described in U.S.
Patent Nos.
5,57:1,379 and 5,015,334. If included in the pulps or stocks of the present
invention, a
synthetic hectorite microparticle additive can be present in any effective
amount, such
as from about 0.1 pound per ton of paperstock, based on the dried solids
weight of
both nhe microparticles and the paperstock, to about 2.0 pounds per ton of
paperstock.
Preferably, if a synthetic hectorite microparticle is included, it is added to
the pulp or
stock in an amount of from about 0.3 pound on a dry basis per ton of
paperstock to
about 1.0 pound per ton of paperstock, based on dried solids weight of the
paperstock,
~ougih other amounts can be used.
In addition to the fibrous cationic colloidal alumina micropaiticles retention
aid system
used in accordance with the present invention, the papermaking pulps or stocks
according to
the present invention may further contain a coagulant/flocculant retention
system having a
different composition than the retention system of the present invention.
The papermaking pulps of the present invention may also contain a conventional
papermaking pulp-treating enzyme that has cellulytic activity. Preferably, the
enzyme
composition also exhibits hemicellulytic activity. Suitable enzymes and enzyme-
containing
compositions include those described in U.S. Patent No. 5,356,800 to Jaquess,
U.S. Patent
No. fi,342,381 to Jaquess, and International Publication No. WO 99/43780.
Other exemplary papermaking pulp-treating enzymes are BUZYME~" 2523
and BUZYME'~ 2524, both available from Buckman Laboratories International,
Inc., Memphis, Tennessee. A preferred cellulytic enzyme composition
preferably contains from about 5 % by weight to about 20 ~ by
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weight enzyme. The preferred enzyme composition can further contain
polyethylene glycol,
hexyl~ene glycol, polyvinylpyrrolidone, tetrahydrofuryl alcohol, glycerine,
water, and other
conventional enzyme composition additives, as for example, described in U.S.
Patent No.
5,356"800. The enzyme may be added to the pulp in any conventional amount,
such as in an
amount of from about 0.001 % by weight to about 0.100% by weight enzyme based
on the dry
weight of the pulp, for example, from about 0.005 % by weight to about 0.05%
by weight.
In a preferred embodiment of the present invention, an enzyme composition is
included in the pulp or stock and contains at least one polyamide oligomer and
at least one
enzyrr~e. The polyamide is present in an effective amount to stabilize the
enzyme. Exemplary
enzyme compositions containing polyamide oligomers and enzymes are described
in
International Published Application No. WO 99/43780.
If an enzyme composition is included, it can include a combination of two or
more
different enzymes. The enzyme composition can include, for example, a
combination of a
lipase and a cellulose, and optionally can include a stabilizing agent. The
stabilizing agent
may be; a polyamide oligomer as described herein.
One particular additive for use according to the methods of the present
invention is a
cationic starch. Cationic starch may be added to the pulp or stock of the
present invention to
form a starch treated pulp. Starch may be added at one or more points along
the flow of
papennaking pulp through the papermaking apparatus or system ofthe present
invention. For
instance, cationic starch can be added to a pulp at about the same time that
the acidic aqueous
alumina sol is added to the pulp. Preferably, if a cationic starch is
employed, it is added to the
pulp or combined with the pulp prior to introducing the fibrous cationic
colloidal alumina
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microparticles to the pulp. The cationic starch can alternatively or
additionally be added to the
pulp after the pulp is first treated with an enzyme, a coagulant, or both.
Preferred cationic
starches include, but are not limited to, potato starches, corn starches, and
other wet-end
starches, or combinations thereof
Conventional amounts of starch can be added to the pulp. An exemplary amount
of
starch that can be used according to the present invention is from about 5 to
about 25 pounds
per ton based on the dried solids weight of the pulp.
A biocide may be added to the pulp in accordance with conventional uses of
biocides
in papermaking processes. For example, a biocide may be added to the treated
pulp in a blend
chest after the pulp has been treated with the optional enzyme and polymer.
Biocides useful in
the papermaking pulps according to the present invention include biocides well
known to
those skilled in the art, for example, biocides available from Buckman
Laboratories
International, Inc., Memphis, Tennessee, such as BUSANTM biocides.
The pulps or stocks of the present invention may additionally be treated with
one or
more other components, including polymers such as anionic and non-ionic
polymers, clays,
other fillers, dyes, pigments, defoamers, pH adjusting agents such as alum,
microbiocides, and
other conventional papermaking or processing additives. These additives can be
added before,
during, or after introduction of the fibrous cationic colloidal alumina
microparticles.
Preferably, the fibrous cationic colloidal alumina microparticles are added
after most, if not
all, other additives and components are added to the pulp. Thus, the fibrous
cationic colloidal
alumina microparticles can be added to the papermaking pulp after the addition
of enzymes,
coagulants, flocculants, fillers, and other conventional and non-conventional
papermaking
additives.
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The addition of the retention system in accordance with the present invention
can be
practiced on most, if not all, conventional papermaking machines.
A flow chart of a papermaking system for carrying out one of the methods of
the
present invention is set forth in Figure 1. It is to be understood that the
system shown is
exemplary of the present invention and is in no way intended to restrict the
scope of the
invention. In the system of Figure l, an optional supply of enzyme composition
at a desired
concentration is combined with a flowing stream of papermaking pulp to form a
treated pulp.
The supply of pulp shown represents a flow of pulp, as for example, supplied
from a pulp
holding tank or silo. The supply of pulp shown in Figure 1 can be a conduit,
holding tank, or
mixing tank, or other container, passageway, or mixing zone for the flow of
pulp. The supply
of enzyme composition can be, for example, a holding tank having an outlet in
communication with an inlet of a treated pulp tank.
The pulp treated with the enzyme composition is passed from the treated pulp
tank
through a refiner and then through a blend chest where optional additives, for
example, a
biocide, may be combined with the treated pulp. The refiner has an inlet in
communication
with an outlet of the treated pulp tank, and an outlet in communication with
an inlet of the
blend chest.
According to the embodiment of Figure I, the pulp treated in the blend chest
is passed
from an outlet of the blend chest through a communication to an inlet of a
machine chest
where optional additives may be combined with the treated pulp. The blend
chest and machine
chest can be of any conventional type known to those skilled in the art. The
machine chest
ensures a level head, that is, a constant pressure on the treated pulp or
stock throughout the
downstream portion of the system, particularly at the head box.
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From the machine chest, the pulp is passed to a white water silo and then to a
fan
pump. The retention system polymer ofthe present invention is preferably
introduced into the
flow of pulp between the silo and the fan pump. The supply of retention system
polymer
composition can be, for example, a holding tank having an outlet in
communication with a
line between the white water silo and the fan pump. As pulp passes from the
fan pump to a
screen, the fibrous cationic colloidal alumina microparticles are preferably
added.
Conventional valuing and pumps used in connection with introducing
conventional additives
can be used. The screened pulp passes to a head box where a wet papersheet is
made on a wire
and drained. In the system of Figure 1, drained pulp resulting from
papermaking in the
headbox is recirculated to the white water silo.
Tn the embodiment shown in Figure 2, the fibrous cationic colloidal alumina
microparticles are added first to the refined treated pulp between the white
water silo and the
fan pump. The retention system polymer is added after the fan pump and before
the screen.
Another embodiment of the present invention is shown in Fig. 3. A pulp
optionally
treated with a cationic starch is refined, passed to a blend chest, passed to
a machine chest,
and then passed to a white water silo. Between the white water silo and the
fan pump the
retention system polymer is preferably added to the pulp. The fibrous cationic
colloidal
alumina microparticles are preferably added after the pulp passes through the
screen and just
prior to sheet formation in the head box.
The apparatus of the present invention can also include metering devices for
providing
a suitable concentration of the fibrous cationic colloidal alumina
microparticles or other
additives to the flow of pulp.
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A cleaner, for example, a centrifugal force cleaning device, can be disposed
between,
for instance, the fan pump and the screen, according to any of the embodiments
of Figures 1-3
above.
S EXAMPLES
In the examples below, various components used in the examples are
abbreviated. In
the examples, the component identified as "Octasol" is a fibrous cationic
colloidal alumina
microparticle sol available from Associated Octel. When followed by a
numerical value, for
example, Octasol 0.5, the numerical value represents the amount of pounds on a
dry basis of
the Octasol microparticles per ton of paperstock based on the dried solids
weight of the
paperstock. "Octasol 3.0", for example, means the paperstock is treated with
3.0 pounds on a
dry basis of Octasol per ton of paperstock based on the dried solids weight of
the paperstock.
The abbreviation "XP9" used in some of the examples represents the same
Octasol
formulation identified as "Octasol" in other examples. The abbreviation "782"
also represents
the same Octasol product identified as "XP9" and as "Octasol" in the examples
below. The
particular Octasol product that was used in the Examples below is identified
by Associated
Octel as "Octasol 782," with the exception of Octasol products 1317 and 1318
identified in
Table 8.
In the examples below, the abbreviation "594" represents BUFLOC~ 594,
available
from Buckman Laboratories International, Inc., which is a high molecular
weight cationic
polyacrylamide having an average molecular weight of from about 5,000,000 to
about
7,000,000 units and a 21% charge density. The abbreviation "5031" represents
BUFLOC~
5031 available from Buckman Laboratories International Inc., which is a low
molecular
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weight cationic polyamine having a 100% charge density and a molecular weight
in the range
of from about 100,000 to about 300,000.
The abbreviation "CP3" represents POLYFLEX CP3TM and "CP2" represents
POLYFLEX CP2TM, both available from Beckman Laboratories International, Inc.,
which are
anionic micropolymers used as microparticle retention systems. The
abbreviations "5450" and
"XP8-558R" represent BUFLOCc~ 5450 available from Beckman Laboratories
International,
Inc., which is a cationic synthetic hectorite microparticle system.
The abbreviations "silica", "8671 ", and "N 8671 " represent powdered silica
available
from Nalco Chemical Co. under the tradename "Nalco 8671 ". The abbreviations
"org 21" and
"org" represent ORGANOPOL 21, available from Ciba Geigy, which is a high
molecular
weight polyacrylamide cationic polymer having a charge density of from about
20% to about
25%. The abbreviations "Bentonite" and "Bent" represent a bentonite colloidal
system
available from Ciba Geigy as HYDROCOL O. The abbreviation "5376" represent
BUFLOC~
5376, available from Beckman Laboratories International, Inc., which is a
cationic
diallyldimethylammonium chloride having a 95% charge density and a molecular
weight of
about 500,000. The abbreviation "606" represents "BUFLOC~ 606", available from
Beckman
Laboratories International, Inc., which is an anionic polyacrylamide having a
charge density of
from about 30% to about 32% and a molecular weight in the range of from about
14,000,000
to about 18,000,000. The abbreviation "5057" represents BUFLOC~ 5057,
available from
Beckman Laboratories International, Inc., which is a non-ionic polyacrylamide
having a 0%
charge density and a molecular weight of about 15,000,000. The abbreviation
"597" represents
BUFLOCC~ 597, available from Beckman Laboratories International, Inc., which
is a cationic
modified polyethylene imine having a 100% charge density and a molecular
weight of from
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about 2,000,000 to about 3,000,000. The abbreviation "5545" represents BUFLOC~
5545,
available from Buckman Laboratories International, Inc., which is an anionic
polyacrylamide
having a 30% charge density and a molecular weight of from about 17,000,000 to
about
20,000,000.
The acronyms PCC, ASA, and PAC also appear in the examples below. The acronym
PCC represents powdered precipitated calcium carbonate which is used as a
filler material.
The acronym ASA represents a sizing agent comprising alkenyl succinic
anhydride available
as Buckman 151 from Buckman Laboratories International, Inc. The acronym PAC
represents
polyaluminum chloride in the form of a very low molecular weight cationic
charged
dipolymer available from Buckman Laboratories International, Inc., as BUFLOC~
5041 or
BUFLOC~ 569.
EXAMPLE 1
The performance of the OCTASOL fibrous cationic colloidal alumina
microparticles,
available from Associated Octel, was tested as a retention aid against
comparative
microparticle technologies used in conventional newsprint furnish.
PROCEDURE:
Test were conducted at a paper mill designated paper mill 1. Drainage was
performed
using a small screen through which 500 ml samples were drained. Mixing was
carried out in a
food blender. Drainage was performed using a modified Schopper Riegler method.
Equipment used for the modified Shopper Riegler drainage test included the
following: a Modified Schopper Riegler (MSR); a 1000 mL graduated cylinder; a
stopwatch; a
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5-gallon plastic bucket; wires for MSR; a vacuum flask and funnel (for
retention); Whatman
ashless filter papers (for ash retention); a turbidity meter; a hemocytometer;
and a microscope.
Obtaining Samples:
A sample to be tested was taken from the headbox. Enough samples were taken
for
multiple tests. For each test, 1000 ml was required. Because temperature has
an impact on
drainage, the test was run immediately after the samples were taken. For lab
studies with the
retention aids, the furnish was kept at the same temperature as the headbox
temperature.
Testing the Sample:
If the MSR was cold and the sample was hot, the MSR was warmed up by running
hot
water over the outside and inside of the MSR. If no hot water was available,
cold water was
used. All tests were conducted in the same way. It was imperative that the MSR
wire was
devoid of any fibers or fines. The wire was backflushed with water before the
test was run.
Good fiber, fines, and filler distribution in the sample was ensured by
agitating the fiber slurry
in the bucket. 1000 ml of the slurry was measured in a graduated cylinder and
poured into the
MSR while holding the plunger down. The graduated cylinder was placed under
the MSR.
The plunger was then released and the stop watch started at the same time. The
time required
for drainage of the sample in incremental units of 100 ml was measured and
recorded. The
incremental units of 100 ml chosen were purely empirical. For example, very
slow stock
samples were instead measured at 100, 150, and 200 ml drainage times.
Sometimes it took
' several tests in order to determine the starting volume tests. The different
levels of polymers
in the various samples were compared, and for this purpose, furnish samples
were obtained ofF
of the machine before addition of the retentionldrainage aid. Drainage and
retention values
were compared against blank furnishes to determine improvement. To measure
retention
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performance, the MSR filtrate was filtered through a pre-weighed filter paper,
dried in an over
at from 105° C to 120° C, and weighed again. The weight
difference was recorded in mg/ml
Drainage times were compared based on different levels of additives (i.e.,
starch,
polymer, or microparticles) of different furnishes. Drainage times were highly
dependent on
variables such as temperatures, furnish types, and refining. Drainage times
were recorded in
seconds for each volume level. The total suspended solids was estimated with a
turbidity
meter. The filtrate could also have been filtered to determine suspended
solids. Solids contents
of MSR filtrate could be reported in mg/ml and used to indicate the retention
capabilities of
different systems, with Iower numbers indicating better retention.
For repeated tests, the sample was taken from the same place along the
papermaking
system. It was ensured that the furnish composition was the same for the
repeated test.
Repeated tests that did not agree within reason with a corresponding original
test were
suspect.
The MSR was kept clean and constantly rinsed with water to keep residual
fibers from
building up on the sides. The screen was periodically cleaned to remove resin
build-up, and
brushed clean with a mild detergent. The wires were checked to make sure bent
or damaged
wires were not used. All tests were conducted in the same manner and at the
same
consistency.
Paper mill 1 employed a paperstock or furnish comprising 30 wt% recycled
corrugated
cardboard, 60 wt% recycled box cardboard, and 10 wt% ONP. The Hb conductivity
of the
pulp measured 0.4 meq/L and had a cationic demand. The pH of the paperstock
was 7.4.
Additives combined with the paperstock included PCC in an amount of 280 pounds
per ton of
paperstock based on the dried solids weight of the paperstock. The PCC was
added before the
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screens. ASA was added in an amount of 2.1 pounds per ton of paperstock at a
point along the
paper mill process where the paperstock was in the form of a thin stock. The
ASA was added
before the fan pump. Before the screens, the Floc 594 was added in an amount
of 2.6 pounds
per ton of paperstock and after the screens CP3 was added in an amount of 4.5
pounds per ton
of paperstock before the headbox.
Furnish used: stock from Newsprint (85% TMP, 15% Broke) pH: 7.6
Polymer addition was constant at 1 pound per ton of paperstock, based on the
dried
solids weight of both the polymer and the paperstock.
AlI microparticle dosages were calculated on dry basis.
The results of the test are shown in Tables 1-4 below. In each of Tables 1-4,
the
column headings "100", "150", and "200" represent the number of milliliters of
filtrate
collected that drained through the wire. The corresponding numbers underneath
the column
headings represent the number of seconds needed for the respective number of
milliliters (ml)
of filtrate to drain through the wire and be collected. For example, in the
first entry of Table 1,
the paperstock identified as "Blank", (having no microparkicle retention
system) required 14
seconds for 100 ml of filtrate to be drained through the forming wire and
collected, required
32 seconds for 150 ml of filtrate to be collected, and required 62 seconds for
200 ml of filtrate
to be collected. In Tables 1-4 the turbidity, measured in units of NTU, is
listed in the last
column of each table such that, for example, the turbidity of the
"Blank" sample listed in Table 1 was 232 NTU. For each of the various examples
tested and
reported in Tables 1-4, the microparticle additive, if used, was added at the
same respective
point in the respective papermaking process and each of the retention polymers
was added at
the same respective point in the respective papermaking process.
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In conclusion, OCTASOL worked as well as the bentonite system. The performance
was better than a dual component system (5031/5376 with 594). The comparisons
can be seen
in Tables 1-4 below.
The results reported in Table 1 are shown graphically in Figs. 4 and S. The
results
reported in Table 2 are shown graphically in Fig. 6. The results reported in
Table 3 are shown
graphically in Figs. 7 and 8.
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TABLE 1
100 150 200 Turbldlty
Blank 14 32 62 232
594 11 26 46 141
5511 11 20 36 99
Octaso10.5159412 26 46 123
Octaso11.0/59411 24 43 120
Octaso13.0159410 21 36 97
Octasol0.5/55118 16 29 61
Octaso11.0155118 17 32 69
Octaso13.0/55118 18 31 65
5511/Octaso11.09 19 34 80
5511/Octaso13.09 23 37 83
5511!5450 5 11 18 42
0.5
5511/54501.0 5 10 16 ~44
5450 0.5/55119 18 34 86
54501.0/5511 10 22 37 111
Bentonite 9 19 33 91
4/Org 21
Bentonite 8 16 30 88
6lOrg 21
Org 21/Bentonite11 22 40 112
4
Org 21IBentonite9 20 36 95
6
TABLE 2
100 150 200 Turbidity
Blank 14 32 62 232
5511 11 20 ~ 36 99
Octaso11.0155118 17 29 69
5511/54501.0 5 10 16 44
Bentonite 9 19 33 91
410rg 21
Bentonite 8 16 30 88
6lOrg 21
'
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TABLE 3
100 ~ 150 200.Turbidity
Bfank 21 48 70 232
Octaso11.0/59411 24 43 120
Octaso13.0/59410 21 36 97
53761.0/594 12 32 49 138
5376 3.0/59413 27 43 105
5031 '1.0/59411 35 49 143
50313.0/594 12 29 46 118
TABLE 4
100 150 200 Turbidity
Blank 21 43 70 232
Octaso11.0/59412 26 47 126
Octaso13.0/59411 25 45 109
53761.0/594 12 27 49 138
5376 3.0/59413 25 43 105
50311.0/594 11 28 49 143
50313.01594 12 29 46 118
Octasol 1.015511
Octaso13.0/551112 25 47 116
'
5376 1.0/5511
5376 3.0!551111 24 44 127
5031 1.0!5511
5031 3.0/5511
54501.0/55118 18 30 88
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EXAMPLE II
The performance of the OCTASOL microparticles was tested against comparative
microparticle technologies.
PROCEDURE:
Testing was done at different commercial paper mills.
Information about the respective paperstocks used is shown on the graphs
attached.
The components of the furnish or paperstock are listed on the graphs shown as
Figs. 9-
12 attached hereto. The %TFPR and %FPAR results are shown in Table 5 for the
paperstock
described in Table 5. The results from Table 5 are shown graphically in Figs.
9 and 10. The
freeness test results for various examples are shown in Table 6 and
graphically depicted in
Fig. 11. Table 7 shows the % TFPR for yet another paperstock. The results
reported in Table 7
are shown graphically in Fig. 12.
In conclusion, the medium charged sample OCTASOL (XP9) performed well. Old and
new samples of the XP9 performed about the same, indicating good stability of
the
microparticle sol. The results show that OCTASOL performs well on alkaline
fine paper.
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TABLE 5
Top
20% hard whites
40% manfold white
ledger
40% hogged (tabloid
news)
pH - 7.9
cationic demand
- .6 meq/L
%TFPR %FPAR
Blank 30.3 12.5
594 1 73.4 30.2
XP9 1/594 1 81.9 37.4
XP9 2/594 1 83.6 40.2
XP9 5/594 1 85.1 42.3
594 llCP3 1 81.2 39.2
594 1/CP3 2 84.3 41.8
5450 1/594 1 79.8 37.9
594 1/5450 1 76.7 36.4
594 1/silica 1 79.8 36.1
594 1/silica 3 81.2 36.4
OrgBent 4 74.6 30.4
OrgBent 6 75.9 33.1
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TABLE 6
Freeness ml
Blank 510
59411b 590
594 2 !b 630
0.5 XP91594 610
1
1 XP9/594 630
1
2 XP9/594 640
1
594 1/XP9 620
1
5941/5450.5 600
594 1/5450 610
1
5450 1/594 610
1
594 1/silica 590
1
594 1/silica 610
3
Org 2lBent 540
4
Org 2lBent 560
6
594 1/CP3 610
1
594 1/CP3 620
2
XP9 1/606 580
1
50312!594 600
1
5031 1/XP9 600
1/594 1
5031 2/XP9 620
1/594 1
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TABLE 7
Back 100%
ONP
pH 7.85
catinoic demand
O.SS meq/1
TFPR
Blank 36.1
S94 1.4 53.6
S4S01/5941.458.4
5941.4/S4S0SS.1
1
XP91/5941.453.8
XP9 2/S9454.6
1.4
Bent 4lOrg49.9
.S
Bent 6lOrg52.1
.S
S94 1.4/silica53.9
1
S94 l.4lsilica54.6
3
S94 1.4/CP254
1
5941.4/CP254.9
2
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Table 8 shows % TFPR results for various examples tested. In Table 8, the
examples
which have been designated "PAC first" are examples wherein the PAC was added
before the
retention system polymer and microparticles. The results from Table 8 are
shown graphically
in Fig. 13. The results reported in Table 8 and shown in Fig. 13 were from
examples run at
paper mill 2. Figs. 14-16 show various other test results achieved from the
examples run at
paper mill 2.
On paper mill 2, for each of the paperstocks described on the graphs shown in
Figs.
13-16, PCC was added to the paperstock in an amount of 280 pounds per ton
before the
screens. ASA was added to the paperstock in an amount of 2.1 pounds per ton at
a point
during the papermaking process where the paperstock was in the form of a thin
stock.
BLTFLOC~ 594 was added in an amount of 2.6 pounds per ton of paperstock before
the
screens. CP3 was added in an amount of 2.3 pounds per ton after the screens.
PAC was added
in an amount of 4.5 pounds per ton before the headbox. The addition of these
additives Were
all based on a dry basis and on the dried solids weight of the paperstock.
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TABLE 8
%TFPR
2 594 2.6 CP3 2,30 86.9% 4.516/t
PAC
first
5545 1 782 1.00 81.8% 4.51b/t
PAC
first
9 5545 0.5 782 1.00 80.6% 4.5
lb/t
PAC
first
12 5545 1.0 1318 1.00 80.6% 4.5
Ib/t
PAC
first
14 5545 1.0 8671 1.00 80.3% 4.5
lb/t
PAC
first
5545 1.0 782o1d1.00 80.0% 4.5
lb/t
PAC
first
3 594 2.6 CP3 2.30 79.8%
6 5545 0.5 782 1.00 79.4%
8 594 1.3 782 2.00 79.4% 4.5
lblt
PAC
first
11 5545 1.0 1317 1.00 79.2% 4.5
Ib/t
PAC
first
13 5545 1.0 5450 1.00 78.6% 4.5
Ib/t
PAC
first
4 5545 1 782 1.00 77.8%
7 594 1.3 782 1.00 76.8% 4.5
Ib/t
PAC
first
1 None 73.3%
5545 1.0 782 1 81.4% 2.251b/t
PAC
first
16 5545 1.0 782 3 81.3% 4.5
lb/t
PAC
first
17 5545 1.0 782 1 80.1% 4.5
Ib/t
PAC
first
18 5545 1.0 782 3 79.4% 2.251b/t
PAC
first
19 5545 1.0 782 2 79.4% 2.251b/t
PAC
first
5545 1.0 782 2 79.0% 4.5
lb/t
PAC
first
21 5545 0.5 782 2 77.8% 2.25
Ib/t
PAC
first
22 5545 0.5 782 1 ?6.4% 4.5
Ib/t
PAC
first
23 5545 0.5 782 1 75.6% 2.251b1t
PAC
first
24 5545 0.5 782 2 75.5% 4.5
lb/t
PAC
first
5545 0.5 782 3 74.7% 2.25
16/t
PAC
first
26 5545 0.5 782 3 74.6% 4.5
Ib/t
PAC
first
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At paper mill 3, various examples were tested using a paperstock having an Hb
conductivity of 420 and a pH of 8.5. The grade of the paperstock was a 20
pound weight grade
of Snowland bible paper. The components of the various examples are shown in
the attached
Figs. 17 and 18 as are the compositions of the paperstocks and additives
provided for all
examples on paper mill 3. The additives used in paper mill 3 and graphically
reported in Figs.
17 and 18 include PCC added in an amount of 160 pounds per ton, TiOz added in
an amount
of 280 pounds per ton, HERCON 79 added in an amount of 7.8 pounds per ton, and
CATO
232 starch added in an amount of 17 pounds per ton, with all amounts being
based on a dry
basis and on the dried solids weight of the paperstock. In addition, BUFLOC~
594 was added
before the screens in an amount of 0.5 pound per ton and POLYFLEX CP2TM was
added in an
amount of 0.98 pound per ton before the screens.
On paper mill number 4, a paperstock having the composition and properties
described
in Figs. 19 and 20 was modified and tested. A HYDREX additive was added to the
paperstock
in an amount of 15 pounds per ton of paperstock before the primary fan pump. A
CATO 15A
starch was added to the paperstock in an amount of 25 pounds per ton of
paperstock at the
machine chest. At the blend chest, alum was added in an amount of 6 pounds per
ton of
paperstock and V-BRITE was added in an amount of 20 pounds per ton of
paperstock. After
the screens, ACCURAC 182 was added in an amount of 0.28 pound per ton of
paperstock. All
additions were on a dry basis and each ton of paperstock was based on the
dried solids weight
of the paperstock. The % TFPR for each of the examples tested and the
composition of the
retention system of each example tested are sat forth in Fig. 19. The % FPAR
and the
compositions of each retention system of each example tested are shown in Fig.
20.
Testing was also conducted on an uncoated acid paper at paper mill 5. The
results of
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retention tests conducted on the paperstock at paper mill 5 are reported in
Figs. 21-23. The
composition of the paperstock tested and properties of the paperstock from
which results are
reported in each ofFigs. 21-23 are shown in Figs. 22 and 23. As with other
examples set forth
herein, in instances such as the testing on paper mill number 5 wherein the
various
components of the paperstock add up to over 100%, the percentages are to be
considered as
parts by weight as opposed to percents by weight.
Additives combined with the paperstock on paper mill 5 included a HYDREX
filler
added in an amount of 60 pounds per ton of paperstock, a CATO 215 starch added
in an
amount of 20 pounds per ton of paperstock, alum added in an amount of 22
pounds per ton of
paperstock, with all amounts being based on a dry basis and on the dried
solids weight of the
paperstock. After the screen, ACCURAC 182 (AGC 182) was added in an amount of
0.3
pound per ton of paperstock. Before the screen NALCO 8671 was added in an
amount of 0.5
pound per ton of paperstock. At the end of the process but before the forming
wire an
additional 0.6 pound per ton of ACC 182 was added. The 0.3 pound per ton
addition of ACC
182 was equivalent to an addition of 0.94 wet pound of the product. The
addition of the 0.5
pound per ton of NALCO 8671 was equivalent to an addition of 3.3 wet pounds of
the
product. The final addition of the 0.6 pound per ton of the ACC 182 was
equivalent to an
addition of 1.9 wet pounds of the product.
EXAMPLE III
The performance of the OCTASOL microparticles as a retention aid was tested
against
comparative microparticle technologies in alkaline fine paper.
PROCEDURE:
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Drainage and retention were performed using a small screen through which 700
ml
samples were drained. Mixing was carried out in a food blender. 700-ml samples
were used
for both drainage and retention.
A Britt Jar test was performed at 750 rpm.
Drainage was performed using a modified Schopper Riegler.
Furnish used: 70% HWD Freeness aprox. 450
30% SWD pH 8.3
Chemicals added to furnish: 30% PCC
5 1b. Cationic starch (Sta-lock 400)
per ton of dried solids.
Polymer addition was constant at 1 pound per ton of paperstock based on the
dried
solids weight of both the polymer and the paperstock.
OCTASOL dosage for this test was calculated on an as received basis (a 15 wt%
solution of microparticles).
An alkaline fine paperstock (furnish) was tested on paper mill 6 and the
drainage time
required to collect 200, 300, and 400 ml, respectively, of filtrate was
measured. The % TFPR
values of many different examples are reported graphically in Figs. 24 and 25.
The drainage
time in seconds to collect 400 ml of filtrate is reported for many different
examples in Fig. 26.
The data used to achieve the graphical results shown in Figs. 24-26 is
reported in Tables 9-12
below.
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OCTASOL
TESTING
Alkaline fine furnish
TABLE 9
Polymer dosage
constant ~ 1 IblT
200 300 400
BLANK 8
12 60
Octasot 0.5/5944 8 28
Octaso11.0/5g4 4 9 23
Octaso13.01594 4 .8 18
594/Octaso10.5 5 11 45
594/Octaso11.0 4 10 30
594/Octaso13.0 4 ~ 12 '
27
Octaso10.51606 5 13 42
Octaso11.01606 4 11 30
Octasol3.0/606 4 10 25
606lOctaso10.5 4 15 '
45
606/Octaso11.0 4 13 31
606/Octaso13.0 4 12 28
Octaso10.5l5.0574 9 37
Octaso11.0/50574 10 30
Octasot 3.0/50574 11 27
505710ctasol 4 11 43
0.5 .
5057/Octaso11.04 11 35
5057/Octaso13.04 10 29
Octasol0.5l597 4 9 38
Octasol1.0/597 4 11 26
Octaso13.01597 4 10 26
597IOctaso11.0 4 12 34
597IOctaso13.0 4 11 25
594/CP3 0.5 4 9 29
594/CP31.0 4 7 18
594/CP3 3.0 4 10 22
594IXP8-5588 3 6 25
0.5
594/XP8-55881.03 6 17
594/XP8-5588 3 7 23
3.0
XP8 0.5/594 3 8 28
XP8 1.0/594 3 7 ~ 19
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TABLE 10
TFPR
BLANK 65.7
594 76.8
Octaso11.0/59484.T
Octaso13.0159486.5
50311.0/594 78.4
50313.0/594 82.g
53761.01594 79.7
5376 3.0/594 .80
594/CP31.0 84.5
594/CP3 3.0 86.6
594/5450 1.0 84,
9
594/5450 3.0 85.1
5941N86711.0 80.3
594/N86713.0 84.6
5g4/Bentonite79.9
4.0
594/Bentonite82,g
6.0
TABLE 11
594/Mlcrofloc92.8
1.0
594/Microflocg5,7
3.0
50311.0/606 78.9
50313.0/606 81:2
5376 1.0/606 78,
9
5376 3.0!606 80,8
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TABLE 12
200 300 400
BLANK 8 12 60
Octaso10.515944 8 28
Octaso11.015944 9 23
Octaso13.0/5944 8 18
594/CP3 0.5 4 9 29
594/CP31.0 4 7 18
594/CP3 3.0 4 10 22
594/XP8-5588 3 6 25
0.5
594/XP8-55881.03 6 17
594/XP8-5588 3 7 23
3.0
XP8 0.5!594 3 8 28
XP81.0/594 3 7 19
CA 02409047 2002-11-14
WO 01/88267 PCT/USO1/07951
-3 8-
Comparable results were obtained using the combination of BUFLOC~ 594 with the
fibrous cationic colloidal alumina microparticles compared with the current
microparticle
technologies available and tested.
Better performance was obtained using a cationic polyacrylamide (PAM) in
combination with the OCTASOL compared to using an anionic or a non-ionic PAM.
Adding
the OCTASOL prior to the PAM proved to be much more effective.
The method and apparatus of the present invention provide excellent drainage
and/or
retention of fines. Resulting paper and paperboard made according to the
method of the
present invention exhibit excellent opaqueness and other desirable physical
properties.
It will be apparent to those skilled in the art that various modifications and
variations
can be made to the embodiments of the present invention without departing from
the spirit or
scope of the present invention. Thus, it is intended that the present
invention covers other
modifications and variations of this invention within the scope of the
appended claims and
their equivalents.
