Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
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SIZED PAPER AND ITS USE IN HIGH SPEED CONVERTING OR
REPROGRAPHICS OPERATIONS
Field o:~ the Invention
This invention relates to processes for using alkaline
sized paper in high speed converting or reprographic
operations.
Background of the Invention
The amount of fine paper produced under alkaline
conditions has been increasing rapidly, encouraged by cost
savings, the ability to use precipitated calcium carbonate,
an increased demand for improved paper permanence and
brightness, and an increased tendency to close the wet end
of the paper machine.
Many current applications for fine paper require
particular attention to sizing before conversion or end-use.
Examples are high-speed photocopies, envelopes, forms bond
including computer printer paper, and adding machine paper.
The most common sizing agents for fine paper made under
alkaline conditions are alkenyl succinic anhydride (ASA) and
alkyl ketene dimer (AFB). Both types have reactive
functional groups that are believed to covalently bond to
cellulose fiber, and hydrophobic tails that are oriented
away from the fiber. The nature and orientation of these
hydrophobic tails cause the fiber to repel water.
Commercial Ad's, containing one B-lactone ring (also
known as 2-oxetanone ring), are prepared by the dimerization
of the alkyl ketenes made~from two saturated, straight-chain
fatty acid chlorides, the most widely used being prepared
from palmitic and/or stearic acid. Other ketene dimers,
such as the alkenyl-based ketene dimer (Aquapel~ 421,
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available from Hercules Incorporated, Wilmington, DE,
U.S.A.), have also been used commercially.
Commercial ASA-based sizing agents are prepared by the
reaction of malefic anhydride with olefins containing from
about 14 to about 22 carbon atoms.
Although ASA and AKD sizing agents are commercially
successful, they have disadvantages. On the paper machine,
ASA frequently causes deposits that can result in paper web
breaks and holes in the paper. ASA addition levels above
2.0-2.5 lb/ton of paper generally lead to unacceptable paper
machine runnability, and paper quality problems. However,
addition levels greater than 2.0-'?.5 lb/ton often are
required to size paper grades made with high levels of
filler. Finally, because ASA cannot be shipped and stored
in emulsion form for long periods of time, the papermaker
must prepare the emulsion immediately before use.
For AKD-based sizes, the most frequently cited
shortcoming is the rate of size development on the paper
machine. Often, an extended period of curing is required
before sizing development is complete.
Both types of sizing agent, particularly the AKD type,
have been associated with handling problems in the typical
high-speed conversion operations required for the current
uses of fine paper made under alkaline conditions (referred
to as alkaline fine paper). The problems include reduced
operating speed in forms presses and other converting
machines, double feeds or'jams in high-speed copiers, and
registration errors on printing and envelope-folding
equipment that oparate at high speeds. Recently,
2-oxetanone sizing agents that are not solid at 35°C have
been introduced (e. g., Pre~is~ 2000 sizing agent available
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from Hercules Incorporated, Wilmington, DE) to address the
problem of handling problems in high-speed conversion
operations.
One such handling problem in high-speed conversion
operations has been identified and measured as described in
"Improving the Converting and End Use Performance of
Alkaline Fine Paper," TAPPI 1994 Paler Makers Conference
Proceedings. Book 1 (1994), pages 155-163, the disclosure of
which is incorporated herein by reference. The problem
occurs when using an IBM 3800 high speed continuous forms
laser printer that does not have special modifications
intended to facilitate handling of alkaline fine paper.
This commercially significant laser printer, therefore, can
serve as an effective testing device for defining the
convertibility of various types of sized paper on state-of-
the-art converting equipment and its subsequent end-use
performance. In particular, the phenomenon of "billowing"
gives a measurable indication of the extent of slippage on
the IBM 3800 printer between the undriven roll beyond the
fuser and the driven roll above the stacker.
Such billowing involves a divergence of the paper path
from the straight line between the rolls, which is two
inches (5 cm) above the base plate, causing registration
errors and dropped folds in the stacker. The rate of
billowing during steady-state running time is measured as
the billowing height in inches above the straight paper path
after 600 seconds of running time and multiplied by 10,000.
Typical alkaline AKD sized fine paper at size addition
levels higher than 2.2 lbs. per ton (1 kg per 0.9 metric
ton) of paper often shows an unacceptable rate-of-billowing,
typically of the order of 20 to 80. Paper handling rates on
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other high-speed converting machinery, such as the Hamilton-
Stevens continuous forms press, or the Winkler & Dunnebier
CH envelope folder also provide numerical measures of
convertibility.
European Patent Application No. 0 629 741 A1, discloses
paper sized with 2-oxetanone sizing agent that is a mixture
of alkyl ketene dimer and 2-oxetanone multimers of various
molecular weights. The paper exhibits levels of sizing
comparable to those obtained with current alkyl ketene dimer
and alkenyl succinic anhydride sizes, and gives improved
performance in high speed converting and reprographic
machines.
U.S. Patent No.5,685,815, and European Patent
Application No.O 666 368 disclose paper that is sized with
2-oxetanone sizing agent and that does not encounter machine
feed problems in high speed converting or reprographic
machines. The 2-oxetanone sizing agent is liquid below 35°C
and is prepared from fatty acids having structural
irregularities in their hydrocarbon chains such as carbon-
carbon double bonds and chain branching.
U.S. Patent 5,725,731 discloses sizing compositions for
fine paper that does not encounter rnachine feed problems in
high-speed converting. The sizing compositions are not
solid at 35°C and comprise a mixture of 2-oxetanone
compounds that are the reaction. product of a mixture of
saturated and unsaturated fatty acids.
U.S. Patent No. 5,407,537 teaches a method for using
synthetic reactive sizing compounds which eliminates the use
of an emulsifier and reduces hydrolysis of the sizing
compound d~iring its residence period in the process water.
The preferred synthetic reactive sizing compounds are
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alkenyl succinic anhydrides where the alkenyl group has 8-16
carbon atoms. The possibility of using mixtures of alkenyl
succinic anhydrides and alkyl ketene dimers is disclosed.
U.K. Patent Application GB 2,252,984 A discloses a
sizing composition that is a blend of from 3 to 50 wt.~
alkyl ketene dimer and 97 to 50 wt.~ alkyl or alkenyl cyclic
acid anhydride.
Swedish Patent Application No. 893,906 discloses
packaging board for fluid sized with combinations of alkyl
ketene dimer and alkenyl succinic anhydride.
The alkyl ketene dimers disclosed in U.S. Patent No.
5,407,537, U.K. Patent Application GB 2,252,989 A and
Swedish Patent Application No. 893,906 are solid alkyl
ketene dimers.
There is a need for alkaline fine paper that provides
improved handling performance in typical converting and
reprographic operations. At the same time, the levels of
sizing development must be comparable to that obtained with
the current furnish levels of 2-oxetanone or ASA for
alkaline fine paper.
Summary of the Invention
This invention relates to a process for using paper in
high speed converting or reprographics operations,
comprising the steps of providing paper sized under alkaline
conditions with alkenyl succinic anhydride (ASA) and
2-oxetanone that is not solid at 35°C, and using the paper
in high speed converting or reprographic operations.
Preferably, the 2-oxetanone sizing agent comprises at least
one 2-oxetanone compound that is the reaction product of a
reaction mixture comprising unsaturated monocarboxylic fatty
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acid, where the term "fatty acid" is used for convenience to
mean a fatty acid or fatty acid halide.
In another embodiment, the invention relates to a
process for making paper under alkaline conditions
comprising the steps of providing sizing agent comprising
alkenyl succinic anhydride (ASA) and 2-oxetanone that is not
solid at 35°C, and sizing the paper with the sizing agent.
Brief DPSCription Qf the Drawings
Figures 1 and 2 are graphs of the level of natural aged
sizing obtained at several addition levels with (a) 2-
oxetanone that is not solid at 35°C, (b) alkenyl succinic
anhydride (ASA) and (c) blends of ASA and 2-oxetanone that
is not solid at 35°C.
Detailed Dgscri~tion of the Invention
Hereinafter, the term "fatty acid" will be used for
convenience to mean a fatty acid or fatty acid halide. The
person of ordinary skill in the art will recognize that this
term is used herein when referring to fatty acids for use in
making sizing compositions, since fatty acids are converted
to acid halides, preferably chlorides, in the first step of
making 2-oxetanone compounds, and that the invention may be
practiced by starting with fatty acids or with fatty acids
already converted to their acid halide. Further, the person
of ordinary skill in the art will readily recognize that
"fatty acid" generally refers either to pure fatty acids or
fatty acid halides, or to a blend or mixture of fatty acids
or fatty acid halides since fatty acids are generally
derived from natural sources and thus are normally blends or
mixtures.
The 2-oxetanones of this invention are disclosed in
U.S. Patent Nos. 5,685,815 and 5,725,731. The 2-oxetanones,
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which may be a blend of 2-oxetanones, are not solid at 35°C
(not substantially crystalline, semicrystalline or waxy
solids, i.e., they flow on heating without heat of fusion).
Preferably, the 2-oxetanones are not solid at 25°C, and more
preferably not solid even at 20°C. Even more preferably,
the 2-oxetanones are liquid at 35°C, more preferably liquid
at 25°C, and most preferably liquid at 20°C.
The 2-oxetanones in accordance with this invention are
a mixture of compounds of the following general class:
R"
n
in which n is preferably 0 to 6, more preferably 0 to 3, and
most preferably 0; R and R", which can be the same or
different, are saturated or unsaturated, straight chain or
branched alkyl groups having B to 24 carbon atoms; R' is a
saturated or unsaturated, straight chain or branched alkyl
group having 2 to 40 carbon atoms, preferably 4 to 32 carbon
atoms; and wherein at least 25~ of the R and R" groups in
the mixture of compounds is unsaturated.
The 2-oxetanones may comprise a mixture of 2-oxetanone
compounds that are the reaction product of a reaction
mixture comprising unsaturated monocarboxylic fatty acids.
The reaction mixture may further comprise saturated
monocarboxylic fatty acids and dicarboxylic acids.
Preferably the reaction mixture for preparing the
mixture of 2-oxetanone compounds comprises at least 25 wt~
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unsaturated monocarboxylic fatty acids, and more preferably
at least 70 wt~ unsaturated monocarboxylic fatty acids.
The unsaturated monocarboxylic fatty acids included in
the reaction mixture for preparation of 2-oxetanone
- compounds preferably have 10-26 carbon atoms, more
preferably 14-22 carbon atoms, and most preferably 16-18
carbon atom. These acids include, for example, oleic,
linoleic, dodecenoic, tetradecenoic (myristoleic),
hexadecenoic (palmitoleic), octadecadienoic (linolelaid~c),
octadecatrienoic (linolenic), eicosenoic (gadoleic),
eicosatetraenoic (arachidonic), cis-13-docosenoic (erucic),
trans-13-docosenoic (brassidic), and docosapentaenoic
(clupanodonic) acids, and their acid halides, preferably
chlorides. One or more of the monocarboxylic acids may be
used. Preferred unsaturated monocarboxylic fatty acids are-
oleic, linoleic, linolenic and palmitoleic acids, and their
acid halides. Most preferred unsaturated monocarboxylic
fatty acids are oleic and linoleic acids, and their acid
halides.
The saturated monocarboxylic fatty acids used to
prepare the 2-oxetanone compounds used in this invention
preferably have 10-26 carbon atoms, more preferably 14-22
carbon atoms, and most preferably 16-18 carbon atoms. These
acids include, for example, stearic, isostearic, myristic,
palmitic, margaric, pentadecanoic, decanoic, undecanoic,
dodecanoic, tridecanoic, nonadecanoic, arachidic and behenic
acids, and their halides,'preferably chlorides. One or more
of the saturated monocarboxylic fatty acids may be used.
Preferred acids are palmitic and stearic.
The alkyl dicarboxylic acids used to prepare the
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2-oxetanone compounds for use in this invention preferably
have 6-44 carbon atoms, and more preferably 9-10, 22 or 36
carbon atoms. Such dicarboxylic acids include, for example,
sebacic, azelaic, 1,10-dodecanedioic, suberic, brazylic,
docosanedioic acids,. and C36 dimer acids, e.g. EMPOL 1008
available from Henkel-Emery, Cincinnati, Ohio, U.S.A, and
their halides, preferably chlorides. One or more of these
dicarboxylic acids can be used. Dicarboxylic acids with
9-10 carbon atoms are more preferred. The most preferred
dicarboxylic acids are sebacic and azelaic acids.
When dicarboxylic acids are used in the preparation of
the 2-oxetanones for use in this invention, the maximum mole
ratio of dicarboxylic acid to monocarboxylic acid (the sum
of both saturated and unsaturated) is preferably about 5. A
more preferred maximum is about 4, and the most preferred
maximum is about 2.
The mixture of 2-oxetanone compounds may be prepared
using methods known for the preparation of standard ketene
dimers. In the first step, acid halides, preferably, acid
chlorides, are formed from a mixture of fatty acids, or a
mixture of fatty acids and dicarboxylic acid, using PCi3 or
another halogenating, preferably chlorinating, agent. The
acid halides are then converted to ketenes in the presence
of tertiary amines (including trialkyl amines and cyclic
alkyl amines), preferably triethylamine. The ketene
moieties then dimerize to form the 2-axetanones.
The alkenyl succinic'anhydrides (ASA) used for blending
with 2-oxetanones in this invention are described by C.E.
Farley and R.B. Wasser in "The Sizing of Paper, Second
Edition", edited by W.F. Reynolds, Tappi Press, 1989, pages
51-62, which is incorporated herein by reference. ASA's are
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composed of unsaturated hydrocarbon chains containing
pendant succinic anhydride groups. Liquid ASA's, which are
preferred in the processes of this invention, are usually
made in a two-step process starting with an alpha olefin.
The olefin is first isomerized by randomly moving the double
bond from the alpha position. In the second step the
isomerized olefin is reacted with an excess of malefic
anhydride to give the final ASA structure as indicated in
the following reaction scheme.
Isomerized Malefic Alkenyl Succinic
0
~o
+ ~~o
o
0
Olefin Anhydride Anhydride(ASA)
If the isomerization step is omitted, ASA's that are solid
at room temperature may be produced.
The starting alpha olefin is preferably in the C-14 to
C-22 range and may be linear or branched. For the purpose
of this invention, it is more preferred that the ASA's be
prepared by reaction of mal~ic anhydride with olefins
containing 14-18 carbon atoms. 'Typical structures found in
ASA's are disclosed in U.S. Patent 4,040,900, which is
incorporated herein by reference in its entirety.
A variety of ASA's are commercially available from
Albemarle Corporation, Baton Rouge, La.
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Representative starting olefins for reaction with
malefic anhydride to prepare ASA's for use in this invention
include: octadecene, tetradecene, hexadecene, eicodecene, 2-
n-hexyl-1-octene, 2-n-octyl-1-dodecene, 2-n-octyl-1-decene,
2-n-dodecyl-1-octane, 2-n-octyl-1-octane, 2-n-octyl-1-
nonene, 2-n-hexyl-1-decene and 2-n-heptyl-1-octane.
In the blends of ASA and 2-oxetanone, the maximum
weight ratio of 2-oxetanone to ASA is preferably about 9:1.
More preferably the maximum is about 4:1, and most
IO preferably about 2:1. The minimum ratio of 2-oxetanone to
ASA is preferably about 1:9. More preferably the minimum is
about 1:4, and most preferably about 1:2.
Generally the sizes of this invention are utilized in
the form of dispersions or emulsions, which can be prepared
by methods well known in the art. It is preferred that the
sizes be utilized as internal sizing agents, i.e., added to
the paper pulp slurry before sheet formation. The ASA and
2-oxetanone sizing components may be preblended before
addition, or added separately.
The paper of this invention is preferably sized at a
total size (i.e., ASA plus 2-oxetanone) addition rate of at
least 0.5 lb (0.2 kg), more preferably at least about 1.5 lb
(0.8 kg), and most preferably at least about 2.2 lb/ton (1
kg/0.9 metric tons) or higher. It may be, for example, in
the form of continuous forms bond paper, perforated
continuous forms paper, adding machine paper, or envelope-
making paper, as well as Converted products, such as copy
paper and envelopes.
Preferably the alkaline paper made according to the
process of this invention contains a water soluble inorganic
salt of an alkali metal, preferably sodium chloride (NaCl).
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However, the paper of this invention will often be made
without NaCI as well.
There are several advantages to the process of this
invention for using paper in high speed converting or
reprographics operations as compared to the process where
the paper is sized with either ASA alone or 2-oxetanone that
is not solid at 35°C alone. First, at moderate to low size
addition levels, the paper of this invention has a higher
level of natural aged sizing (sizing after aging for 7 days
at room temperature) than does paper sized with an
equivalent amount of 2-oxetanone that is not solid at 35°C.
Second, the paper is produced with a lower level of paper
machine deposits than paper produced at equal levels of
sizing using ASA size. Third, better on-machine sizing is
obtained with ASA and 2-oxetanone that is not solid at 35°C
than is obtained when using 2-oxetanone that is not solid at
35°C alone. This is often important for runnability on the
paper machine.
Furthermore, the process of this invention is also an
improvement over the process where the paper is sized
utilizing A.SA and solid alkyl ketene dimers. When solid
alkyl ketene dimer is used, special equipment must be
employed to melt the alkyl ketene dimer in order to prepare
aqueous dispersions. This melting step is not necessary for
use of liquid 2-oxetanone.
The paper of this invention does not encounter
significant machine-feed problems on high speed converting
machines or in reprographic operations. In particular, the
paper according to this invention can be made into a roll of
continuous forms bond paper having a basis weight of about
15 to 24 lb/1300 ftz (6.8 to 10.9 kg/121 mz) and that is
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sized at an addition rate of at least about 1.5 lb/ton (0.68
kg/0.9 metric ton), and that is then capable of running on
the IBM Model 3800 high speed, continuous-forms laser
printer with no significant machine feed problems.
Further, the preferred paper, according to the
invention, that can be made into sheets of 8 1/2 x 11 inch
(21.6 cm x 28 cm) reprographic cut paper having a basis
weight of about 15-24 lb/1300 ft2 (6.8 to 10.9 kg/121 m2),
is capable of running on a high speed laser printer or
copier. When the paper is sized at a total size (i.e., ASA
plus 2-oxetanone) addition rate that is preferably at least
about 1.5 lb/ton (0.68.kg/0.9 metric ton), and more
preferably at least about 2.2 lb/ton (1 kg/0.9 metric ton),
it is capable of running on the IBM model 3825 high-speed
copier without causing misfeeds or jams at a rate of more
than 5 in 10,000 sheets, preferably at a rate of no more
than 1 in 10,000 sheets. By comparison, paper sized with
standard AKD has a much higher rate of double feeds on the
IBM 3825 high speed copier (14 double feeds in 14,250
sheets). In conventional copy-machine operation, 10 double
feeds in 10,000 is unacceptable. A machine manufacturer
considers 1 double feed in 10,000 sheets to be unacceptable.
The paper of this invention in the form of a roll of
continuous forms bond paper having a basis weight of about
15-24 lb/1300 ftZ (6.8 to 10.9 kg/121 m2) can be converted
to a standard perforated continuous form on a continuous
forms press at a press speed of about 1300 to 2000 feet (390
m to 600 m) per minute or more. The preferred paper
according to the invention, in the form of a roll of
continuous forms bond paper having a basis weight of about
15-24 lb/1300 ft2 (6.8 to 10.9 kg/121 m2), and that is sized
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at an addition rate of at least about 2.2 lb/ton (1 kg per
0.9 metric ton) can be converted to a standard perforated
continuous form on the Hamilton-Stevens continuous forms
press at a press speed of at least about 1775 feet (541 m)
per minute, preferably at least about 1900 feet (579 m) per
minute.
The paper of this invention can also be made into a
roll of envelope paper having a basis weight of about 15-24
lb/1300 ft2 (6.8 to 10.9 kg/121 m2) that is sized at an
addition rate of at least about 2.2 lb/ton (1 kg/0.9 metric
ton). The paper can be converted into at least about 900
envelopes per minute, preferably at least about 1000 per
minute on a Winkler & Dunnebier CH envelope folder.
The paper of this invention can be run at a speed of at
least about 58 sheets per minute on a high speed sheet-fed
copier (IBM 3825) with less than 1 in 10,000 double feeds or
jams.
The paper of this invention is capable of running on a
high speed, continuous-farms laser printer with a rate of
billowing at least about 10~ less, preferably about 20~
less, than that produced when running on the same printer, a
roll of continuous forms bond paper having the same basis
weight and sized at the same level with an AFB size made
from a mixture of stearic and palmitic acids, after 10
minutes of running time.
The paper of this inventicn is capable of running on a
high speed sheet-fed copier (IBM 3825) at a speed of about
58 sheets per minute with at least about 50~ fewer,
preferably about 70~ fevrer, double feeds or jams than the
number of double feeds or jams caused when running on the
same copier, sheets of paper having the same basis weight
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and sized at the same level with an AKD size made from a
mixture of stearic and palmitic acids.
The paper of this invention is also capable of being
converted to a standard perforated continuous form on a
continuous forms press at a press speed at least 3~ higher,
preferably at least 5$ higher, than paper having the same
basis weight and sized at the same level with an AKD size
made from a mixture of stearic and palmitic acids.
Experimental Procedures
All parts, percentages, etc. herein are by weight
unless otherwise specified.
Paper for evaluation on the IBM 3800 was prepared on a
pilot paper machine. To make a typical forms bond paper-
making stock, the pulp furnish (three parts Southern
hardwood kraft pulp and one part Southern softwood kraft
pulp) was refined to 425 ml Canadian Standard Freeness
(C.S.F.) using a double disk refiner. Prior to the addition
of the filler to the pulp furnish (10~s medium particle-size
precipitated calcium carbonate), the pH, alkalinity and
hardness of the papermaking stock were adjusted using the
appropriate amounts of HZSO" NaHC03, NaOH, and CaCl2, to pH
7.8-8.0, alkalinity 150-200 ppm, and hardness 100 ppm.
The 2-oxetanone compounds were prepared by methods
used conventionally to prepare commercial 2-oxetanone
compounds i.e., acid chlorides from a mixture of fatty acids
are formed using a conventional chlorination agent, and then
the acid chlorides are dehydrochlorinated in the presence of
a suitable base. ASA was Alkenylsuccinic Anhydride C16C18,
obtained from Albemarle Corp., Baton Rouge, LA.
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Emulsions of the ASA/2-oxetanone blends were prepared
immediately before use by methods described by C.E. Farley &
R.B. Wasser, in "The Sizing of Paper (Second Edition)",
edited by W.F. Reynolds, Tappi Press, 1989, pages 51-62,
which is incorporated herein by reference in its entirety.
The emulsions were prepared using Stalok 400 cationic starch
(available from A.E. Staley Manufacturing Co., Decatur IL)
at a level of 3:1 starch to sizing agent.
Wet-end additions of sizing agent, quaternary-amine-
substituted cationic starch (0.758 for Example 3, and 0.5~
for Examples 1 and 2), alum (0.2~), and retention aid
(0.025 0 were made. Stock temperature at the headbox and
white water tray was controlled at 110°F (43.3°C).
The wet presses were set at 40 psi(2.8 kg/cm2) gauge.
A dryer profile that gave 1-2~ moisture at the size press
and 4-6~S moisture at the reel was used (77 feet (23.4 m) per
minute). Approximately 35 lb/ton (15.9 kg/0.9 metric ton)
of an oxidized corn starch, Stayco C (A. E. Staley
Manufacturing Co,, Decatur IL), and 1 lb/ton (0.45 kg/0.9
metric ton) of NaCl were added at the size press (130°F
(54.4°C), pH 8). Calender pressure and reel moisture were
adjusted to obtain a Sheffield smoothness of 150 flow units
at the reel (Column #2, felt side up) .
A 35-minute roll of paper was collected and converted
on a commercial forms press to two boxes of standard 8 1/2"
x 11" (21.6 x 28 cm) forms. Samples were also collected
before and after each 35 minute roll for testing natural
aged sizing and basis weight (46 lb/3000 ft2,
20.8 kg/279 m2), and smoothness testing.
The converted paper was allowed to equilibrate in the
printer room for at least onE day prior to evaluation. Each
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box of paper allowed a 10-14 minute (220 feet (66.7 m) per
minute) evaluation on the IBM 3800. All samples were tested
in duplicate. A standard acid fine paper was run for at
least two minutes between each evaluation to reestablish
initial machine conditions.
In order to establish whether a sizing agent
contributed to difficulties in converting operations, paper
was made on a pilot paper machine, converted into forms, and
then printed on an IBM 3800 high speed printer. The
runnability on the IBM 3800 was used as a measure of
converting performance. Specifically, the height in inches
to which the paper billowed between two defined rolls on the
IBM 3800 and the rate at which billowing occurred was used
to quantify converting performance. The faster and higher
the sheet billowed, the worse the converting performance.
The Hercules Size Test (HST) is a standard test in the
industry for measuring the degree of sizing. This method
employs an aqueous dye solution as the penetrant to permit
optical detection of the liquid front as it moves through
the sheet. The apparatus determines the time required for
the reflectance of the sheet surface not in contact with the
penetrant to drop to a predetermined percentage of its
original reflectance. All HST testing data reported measure
the seconds to B0~ reflection with lg formic acid ink mixed
with naphthol green B dye unless otherwise noted. The use
of formic acid ink is a more severe test than neutral ink
and tends to give faster test times. High HST values are
better than low values.
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Example 1
In this example a 1:1 blend of 2-oxetanone and alkenyl
succinic anhydride was evaluated for sizing efficiency at
several addition levels. For comparison, samples of
2-oxetanone and ASA alone were run under the same
conditions.
The 2-oxetanone was prepared by the usual procedures
using Emersol-221 as the feedstock. Emersol-221, available
from Henkel-Emery, Cincinnati, OH, had the following
composition:
oleic acid 73~
linoleic acid 8
palmitoleic acid 6
myristoleic acid 3
linolenic acid 1
saturated fatty acids 9.
The ASA was Alkenylsuccinic Anhydride C16C18, obtained
from Albemarle Corp., Baton Rouge, LA.
The eval~.:ation data are in Table 1 and presented
graphically in Figure 1. The data indicate that the
natural-aged sizing for the ASA/2-oxetanone blends is less
than that of ASA alone but greater than that for 2-oxetanone
alone at equivalent size addition levels.
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TABLE 1
Size Addition Natural;
Aged
Level, Lb/Ton Sizing, (HST)
of
Ex~g.~lment. Sizing Aaent. Dry Paper Seconds
lA 2-Oxetanone 1.5 2
(comparative)
1B 2-Oxetanone 2.25 82
(comparative)
1C 2-Oxetanone 3.0 143
(comparative)
1D ASA 1.1 34
(comparative)
lE ASA 1.4 153
(comparative)
1F ASA 1.7 186
(comparative)
1:1
1G 2-oxetanone/ASA 1.9 91
1:1
1H 2-oxetanone/ASA 1.8 116
1:1
lI 2-oxetanone/ASA 2.25 194
Example 2
In this example blends of 2-oxetanone and alkenyl
succinic anhydride at two ratios were evaluated for sizing
efficiency at several addition levels. For comparison,
samples of 2-oxetanone sizing agent alone and ASA alone were
run under the same conditions.
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The 2-oxetanone and ASA were the same as those used in
Example 1.
The results are in Table 2 and presented graphically in
Figure 2. The data demonstrate that at the 2-oxetanone/ASA
ratios of 3:1 and 65:35 the natural aged sizing is less than
that of ASA alone but greater than that with 2-oxetanone alone
below about 2.75 lb/ton addition level.
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Table 2
Size Addition Natural Aged
Level, Lb/Ton Sizing, (HST)
of
Experiment sizing Agent Dry Seconds
Paper
2A 2-Oxetanone 1.5 2
(comparative)
28 2-Oxetanone 2.25 50
(comparative)
2C 2-Oxetanone 3.0 289
(comparative)
2D ASA 1.1 34
(comparative)
2E ASA 1.4 178
(comparative)
2F ASA 1.7 226
(comparative)
3:1
2G 2-oxetanone/ASA 1.5 14
3:1
2H 2-oxetanone/ASA 2.25 128
3:1
2I 2-oxetanone/ASA 3.0 217
65:35
2J 2-oxetanone/ASA 1.5 13
65:35
2K 2-oxetanone/ASA 2.25 165
65:35
2L 2-oxetanone/ASA 3.0 223
Example 3
In this example blends of 2-oxetanone and ASA at 3 ratios
were tested for their effects on the runnability of a difficult
to convert grade of alkaline fine paper on the IBM 3800. A
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comparative experiment, 3A, utilizes Hercon~ 70 sizing agent, a
dispersion containing alkyl ketene dimer prepared from a
mixture of palmitic and stearic acids, available from Hercules
Incorporated, Wilmington, DE. The materials utilized in the
remainder of the experiments were as described in Example 1.
The evaluation data are in Table 3. The data show that
the 2-oxetanone/ASA blends at all 3 ratios tested produced
paper that ran on the IBM 3800 with good to very good
runnability. Moreover, at the 3.0 lb/ton addition level all
three ratios tested produced paper that ran on the IBM 3800
with runnability better than that of paper made with
Hercon~ 70.
Table 3
Size Addition IBM 3800
Level, Lb/Ton Converting
Experiment Sizing AcTer~t of Dry Paper Performance'
3A Hercon~70 3.0 2.5
(comparative)
1:1
3B 2-oxetanone/ASA 3.0 2
1:3
3C 2-oxetanone/ASA 3.0 1.5
3:1
3D 2-oxetanone/ASA 3.0 1
2 0 *
IHM Runnability
1 - Very 2.1 in/sec))
Good
(Billowing
rate
x 10<
2 - Good 1-6.2 in/sec)
(Billowing
rate
x 10
= 2.
3 - Poor 6.2-16.7 in/sec)
(Billowing
rate
x 10
=
4 - Very > 16.7 in/sec)
Poor
(Billowing
rate
x 10'
_
It is not intended that the examples given here should be
construed to limit the invention, but rather they are submitted
to illustrate some of the specific embodiments of the invention.
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Various modifications and variations of the present invention
can be made without departing from the scope of the appended
claims.
