BACKGROUND OF THE INVENTION
FIELD OF THE INVENTION:
[0001] This invention relates to the art of papermaking, particularly to treating a paper
products with pressure and heat to improve its wet strength while preserving its folding
endurance. This invention, more specifically, relates to Kraft paper products, bleached
or unbleached paper products produced from SCMP and sulfite pulps, TMP paperboard.
TMP paperboard means thermomechanical pulp paperboard. The term "SCMP" process means
semichemical mechanical pulping process.
Description of the Prior Art:
[0002] The kraft process is a method of preparation of an aqueous slurry of fibers by treatment
of a suitable renewable raw material. In most pulping process, a considerable portion
of the natural lignin in wood, grass or other vegetative matter is rendered soluble
by chemical reaction with one or more nucleophilic reagents. In the kraft process,
the nucleophilic reagents are sulfide and hydroxide ions, which are used under highly
alkaline conditions. Variations of the kraft process include the earlier practiced
soda process, using hydroxyl ions derived from metals in Group IA of the periodic
table, namely lithium, sodium, potassium, rubidinium and cesium. A second variation
involves the use of anthraquinone (AQ) or substituted anthraquinones as additional
nucleophiles. Anthraquinone can be used in the soda process, in which case the process
is known as the soda-AQ process, or in the kraft process which is then known as the
kraft-AQ process. Such variations in the kraft process are well known in the industry
and pulps prepared by any of these variations can be used in practicing the present
invention.
[0003] If desired, the soda-AQ, kraft and kraft AQ pulps can be rendered white by application
of suitable bleaching agents. Such agents are usually electrophilic in nature and
may include chlorine, chlorine dioxide, sodium hypochlorite, hydrogen peroxide, sodium
chlorite, oxygen and ozone. Use is often in sequential stages and a suitable nucleophilic
agent, customarily hydroxyl ion, may be used in intermediate stages. "Kraft paper"
is paper made from pulp produced by the kraft process. Bleached kraft paper, because
of its low lignin content, has low wet strength; hence it is desirable to develop
this quality of bleached kraft products.
[0004] Linerboard is a medium-weight paper product used as the facing material in corrugated
carton construction. "Kraft linerboard" is linerboard made from pulp produced by the
kraft process.
[0005] The thermomechanical pulping process is a method of producing an aqueous slurry of
fibers by mechanical treatment of a suitable renewable raw material. In most pulping
processes, a considerable portion of the natural lignin in wood, grass or other vegetative
matter is rendered soluble by chemical reaction with one or more nucleophilic reagents.
Such nucleophilic reagents are not used in thermomechanical pulp production. Instead,
fibers are liberated from a thermally softened source material, usually wood chips,
by passage through a suitable shredder or disc refiner operating under ambient steam
pressure at a temperature of 120-150°C or more. Such fibers are usually brittle and
sheets prepared from them are brittle and have little or no wet strength.
[0006] As used herein, "TMP pulp" is pulp produced as described above, by a thermomechanical
process. Despite the fiber brittleness, TMP pulp has the advantage of avoiding the
odor, disposal problems, and other drawbacks of chemical pulp production. "TMP paperboard"
is a medium-weight paper product made from TMP pulp. It is notoriously weak when wet,
and inflexible, compared with products identically made from more flexible pulps such
as kraft pulps. Hence, a process for improving both the wet strength and flexibility
of TMP paper products is desirable.
[0007] In the art of making kraft paper products, TMP paperboard and SCMP paperboard, it
is conventional to subject felted fibers to wet pressing to unite the fibers into
a coherent sheet. Pressure is typically applied to a continuous running web of paper
by a series of nip rolls which, by compressing the sheet, both increases its volumetric
density and reduce its water content. The accompanying Fig. 1 shows in simplified
diagramatic form a typical papermaking machine, including a web former and three representative
pairs of wet press rolls. Also shown are drying rolls whose purpose is to dry the
paper to a desired final moisture content, and a calender stack to produce a smooth
finish. At least some of the rolls are ordinarily heated to hasten drying. (The drawing
is simplified - there are many more drying rolls in actual practice.)
[0008] The semichemical mechanical pulping process is a method of production of an aqueous
slurry of fibers by treatment of a suitable renewable raw material. In most pulping
processes, a considerable portion of the natural natural lignin in wood, grass or
other vegetative matter is rendered soluble by chemical reaction with one or more
nucleophilic reagents. Minimization of the lignin portion solubilized and removed
whilst so altering the lignin as to permit recovery of fibers by the mechanical action
of a disk or other refiner or shredder in a condition of little damage is the goal
of the SCMP process. It is also the goal of certain related processes known as the
chemimechanical process (CMP), the chemithermomechanical process (CT-MP) and the neutral
sulfite semichemical (NSSC) processes. Such pulps are normally considered to be more
brittle and of inferior strength when compared to lower lignin pulps produced by the
kraft, sulfite, kraft-anthraquinone (AQ), soda-AQ or alkaline sulfite AQ processes.
However, properties are adequate for many end-uses, including corrugated medium and
even as a linerboard component.
[0009] In the sulfite process, sulfite or bisulfite ion is the nucleophilic agent. The sulfite
or bisulfite ions cause the lignin molecules to break into small fragments. During
this chemical reaction, the sulfite or bisulfite ions become chemically bonded to
the lignin fragments thereby providing water solubility. A variation of the sulfite
process involves the use of anthraquinone (AQ) or substituted anthraquinones as a
second nucleophile. AQ is reduced in situ during the earliest stages of the cook to
anthrahydroquinone (AHQ). As AQ is insoluble and only the salt from of AHQ is soluble,
alkali presence is necessary for solution formation and uniform penetration of AQ
into the wood chip, grass stem or any other fiber-containing vegetative matter. Such
a cooking process is known as an alkaline sulfite-AQ process. Both the sulfite process
and the alkaline sulfite-AQ variation of the sulfite process are well known to the
industry and pulps thus prepared can be used to give the benefit of our invention.
[0010] There is currently considerable interest in treatments involving heat and pressure,
or heat alone, during or after the production process, to improve various qualities
of paper products. Quantifiable paper qualities include dry tensile strength, wet
tensile strength, reverse folding endurance, compressive strength and stiffness, among
others. Which qualities should desirably be enhanced depends upon the intended application
of the products. For paper and TMP paperboard to be used in humid or wet environments,
two qualities of particular interest are wet strength and folding endurance, both
of which can be measured by well-known standard tests. As used herein, then, "wet
strength" means wet tsneile strength as measured by American Society for Testing and
Materials (ASTM) Standard D829-48. "Folding endurance" is defined as the number of
times a board can be folded in two directions without breaking, under conditions specified
in Standard D2176-69. "Basic weight" is the weight per unit area of the dried end
product.
[0011] For linerboard to be used in manufacturing corrugated cartons for use in humid or
wet environments, three qualities of particular interest are wet strength, folding
endurance and high humidity compression strength. "Compression strength" is edgewise
linear compression strength as measured by a standard STFI (Swedish Forest Research
Institute) Tester.
[0012] Prior workers in this field have recognized that high-temperature treatment of linerboard
can improve its wet strength. See, for example E. Back, "Wet stiffness by heat treatment
of the running web",
Pulp & Paper Canada, vol. 77, No. 12, pp. 97-106 (Dec. 1976). This increase has been attributed to the
development and cross-linking of naturally occurring polysaccharides and other polymers,
which phenomenon may be sufficient to preserve product wet strength even where conventional
synthetic formaldehyde resins or other binders are entirely omitted.
[0013] It is important to note that wet strength improvement by heat curing has previously
been thought attainable only at the price of increased brittleness (i.e., reduced
folding endurance). Therefore, most prior high-temperature treatments have been performed
on particle board, wallboard, and other products not to be subjected to flexure. The
known processes, if applied to bleached kraft paper, TMP paperboard and SCMP paperboard,
would produce a brittle product. Embrittled paper and paperboard are not acceptable
for many applications involving subsequent deformation such as the converting operation
on a corrugating machine to make corrugated boxes out of linerboard, and therefore
heat treatment alone, to develop wet strength of linerboard, has not gained widespread
acceptance, and is not viable for TMP paperboard. As Dr. Back has pointed out in the
article cited above, "The heat treatment conditions must be selected to balance the
desirable increase in wet stiffness against the simultaneous embrittlement in dry
climates." Significantly, in U. S. Patent 3,875,680, Dr. Back has disclosed a process
for heat treating already manufactured corrugated board to set previously placed resins,
the specific purpose being to avoid running embrittled material through a corrugator.
[0014] It is plain that added wet strength and improved folding endurance were previously
thought incompatible results.
[0015] It is therefore an object of the invention to produce paper products and TMP paperboard
and linerboard having both greatly improved wet strength and good folding endurance.
Another goal is to achieve that objective without resorting to synthetic resins or
other added binders and wet strength agents.
[0016] With a view of the foregoing, a process has been developed which dramatically and
unexpectedly increases not only the wet strength of paper products, TMP Paperboard,
SCMP paperboard and linerboard, but also preserves its folding endurance. In its
broadest sense, the invention comprises steps of 1) subjecting paper or linerboard,
produced from bleached or unbleached kraft pulp or paperboard produced from thermomechanically
produced pulp or SCMP paper pulp, to high pressure densification, and 2) heating the
product to an internal temperature of at least 420°F (216°C) for a period of time
sufficient to increase the wet strength of the product.
[0017] This method produces a product having folding endurance greatly exceeding that of
similar products whose wet strength has been increased by heat alone. This is clearly
shown by our tests exemplified below.
[0018] While the tests set out in the Examples have carried out the invention in a static
press, it is preferred that the heat and pressure be applied to continuously running
paper and board by hot pressure rolls, inasmuch as much higher production rates can
be attained.
[0019] In the case of linerboard from unbleached kraft, we prefer to raise the internal
temperature of the board to at least 550°F (289°C), as greater wet strength is then
achieved. This may be because at higher temperatures, shorter step duration is necessary
to develop bonding, and there is consequently less time for fiber degradation to occur.
Also, shorter duration enables one to achieve higher production speeds.
[0020] In the case of other paper products from kraft pulp, and TMP boards, we prefer to
raise the internal temperature of the paper to at least 465°F (240°C), as greater
wet strength is then achieved. In the case of SCMP paperboard, it is preferred to
raise the internal temperature of the board to at least 450°F (232°C).
[0021] It should be noted that the heating rate, and thus the required heating duration
at a particular temperature, depends on method of heat transfer chosen. Furthermore,
it is desirable to raise the web temperature as rapidly as possible to the chosen
treating temperature. Improved heating rates can be achieved by using high roll temperatures
and/or by applying high nip forces to the press roll against the sheet on the hot
rolls. That high pressure dramatically improves heat transfer rates has previously
been disclosed. One worker has attributed this to the prevention of vapor formation
at the web-roll interface.
[0022] While the invention may be practiced over a range of temperatures, pressures and
durations, these factors are interrelated. For example, the use of higher temperatures
requires a heating step of shorter duration, and vice-versa. At 550°F, in the case
of linerboard, a duration of 2 seconds has been found sufficient to obtain the desired
improvements, while at 420°F, considerably longer time is required. At 465°F, a duration
of 60 seconds has been found sufficient to obtain the desired improvements, while
at 420°F, considerably longer time is required. In the case of SCMP board, at 450°F,
a duration of 5 seconds has been found sufficient to obtain substantial improvement.
[0023] It is presently preferred that, for safety reasons, the roll temperature be not greater
than the web ignition temperature (572°F, 300°C); however, even higher roll temperatures
may be used if suitable precautions, such as the provision of an inert atmosphere,
or rapid removal of paper from the hot environment, are taken.
BRIEF DESCRIPTION OF THE DRAWINGS
[0024]
Figure 1 shows, in greatly simplified diagrammatic form, a conventional apparatus
for producing linerboard.
Figure 2 shows, in like diagrammatic form, an apparatus for practicing the present
invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0025] Figure 2 illustrates a preferred apparatus for carrying out the inventive process,
although it should be understood that other devices, such as platen presses, can be
used and in fact the data below was obtained from platen press tests. In the machine
depicted, bleached or unbleached kraft paper fibers or unbleached TMP pulp fibers
or SCMP or sulfite pulp fibers in aqueous suspension are deposited on a web former
screen 10,producing a wet mat or fibers. The mat is then passed through a series of
wet press nip rolls 12, 13, 14, 15, 16 and 17 which develop a consolidated web. Suitable
wet presses known today include long nip presses and shoe-type presses capable of
developing high unit press pressures on the wet fiber web. This step is known as "high
pressure wet pressing". The web is then passed over pre-drying rolls 18, 19 to remove
water from the wet web. Once the moisture content of the web has been reduced to less
than 70% by weight, steps of the high pressure densification and high temperature
treatment are applied according to the invention.
[0026] To densify the web, a series of drying rolls 20, 21, 22, 23 are provided with respective
pressure rollers 25, 26, 27, 28 which are loaded sufficiently to produce a web density
of at least 700 kg/m³. We define this step as "press drying" or "high pressure densification".
In the preferred embodiment, the high pressure densification step of the invention
is carried out both at normal drying temperatures (substantially below 400°F) in the
press drying section, and also in the high temperature heat treatment section described
below. It should be understood, however, that the two steps may be performed sequentially
or simultaneously.
[0027] In the heat treatment section, one or more drying rolls (e.g. 30, 31, 32, 33) is
heated to or slightly above the desired maximum internal web temperature. Pressure
rolls 35, 36, 37, 38 are used to improve heat transfer between the drying rolls and
the web, and preferably, these pressure rolls are also highly loaded to continue the
high pressure densification step during heat treatment. The drying roll temperature
necessary to achieve target web temperature is a function of several factors including
web thickness, web moisture, web entering temperature, web speed, nip pressure, and
roll diameter; its calculation is within the skill of the art. It is presently believed
optimum in the case of linerboard from unbleached kraft pulp to achieve an internal
web temperature of 550°F (289°C) and to maintain such temperature for two seconds
or 465°F (240°C) in the case of paperboard from bleached kraft pulp or TMP board and
to maintain this temperature for 60 seconds or 450°F (232°C) in the case of paperboard
from SCMP and other sulfite pulp and to maintain this temperature for 5 seconds. In
any event, the roll temperature must be at least 420°F (221°C) which is well in excess
of the temperature of normal drying rolls. The heat treatment rollers are contained
within an envelope 40, and air caps 41, 42, 43, 44 may be used to heat the web further
as it passes over the rolls. An inert gas, steam or superheated steam atmosphere may
be used for this purpose and to prevent oxidation or combustion at high temperatures.
[0028] Following heat treatment, the web may be passed over final rolls 50, 51 having air
caps 60, 61 to condition the web, which is then calendered and reeled in a conventional
manner.
[0029] The combined effect of high pressure densification and high temperature produce an
unexpected combination of good wet strength and good folding endurance in the finished
product.
[0030] The invention has been practiced as described in the following examples. The improvement
in board quality will be apparent from an examination of the test results listed in
the tables below.
EXAMPLE 1
[0031] Pine wood chips from the southeastern United States were cooked by the kraft process
to an extent typical of pulp used in linerboard production. The cooked chips were
converted to a pulp by passage through a disk refiner. The pulp was thoroughly washed
with water to remove residual black liquor and was stored in the wet state at 38-42°F
(3°-6°C) in a refrigerator until sheets were prepared. The cooked, washed pulp had
a kappa number of 98, indicating presence of 15% residual lignin and had a freeness
of 720 ml by the Canadian Standard Freeness test, which values are typical of a pine
linerboard pulp prior to beating.
[0032] A dispersion of the pulp in distilled water was converted to handsheets using a TAPPI
sheet mold. The quantity of fiber in the dispersion was adjusted to give a TAPPI sheet
weight of 3.6 g in the oven dried state, said weight being close to that of an air
dried, 42 lb/1000 ft² (205 g/m²) commercial linerboard sheet. The sheets were wet
pressed with blotters at 60 psi (415 kPa) prior to drying.
[0033] Three sets of sheets were prepared. Sheets from the first set were dried on TAPPI
rings at room temperature according to TAPPI standard T205 om-81. This is a conventional
(C) drying procedure. Sheets from the second set were also dried by the conventional
procedure but this procedure was followed by a heat treatment (HT). The paper sheet
was placed between two 150 mesh stainless steel screens, which assembly was placed
in the platen press. Heat treatment was in accordance with the conditions found optimum
for this invention, namely 2 seconds at 550°F (289°C) sheet internal temperature.
To do this, single sheets were placed in a 550°F (289°C) Carver platen press for 4
seconds with 15 psi (105 KPa) as applied pressure. Previous experiments using a thermocouple
buried in the sheet had shown that the sheet required 2 seconds to reach the target
550°F (289°C) temperature. Individual sheets from the third set were inserted in the
wet state in a different platen press at 280°F (138°C). A pressure of 15 psi (105
KPa) was maintained for 5 seconds to dry surface fibers, after which the pressure
was increased to 790 psi (5450 KPa) for 20 seconds. On completion of this press densification
process (PD) sheet moisture was about 10%. Each sheet was removed from the PD press
and immediately placed in the other, HT press for 4 seconds at 550°F (289°C). All
three sets of sheets were conditioned at 73°F (23°C) and 50% humidity for at least
24 hours before testing.
[0034] Fold, wet and conditioned tensile strength and conditioned compressive strength were
the tests that were carried out. Wet tensile tests were carried out immediately after
excess water was blotted from test sheets which had been removed after 4 hours immersion
in distilled water. Otherwise, this test was the same as the ASTM standard wet tensile
test.
[0035] The results summarized in Table I show superior folding endurance and wet strength
for the densified and heat treated sheets.

EXAMPLE 2
[0036] Hardwood chips from the southeastern United States were cooked by the kraft process
to yield, after disk refining and washing, a 98 kappa pulp of 618 ml Canadian Standard
Freeness. This pulp was mixed with the softwood of example 1 to give a mixture containing
60% softwood and 40% hardwood fiber. Sheets were prepared and tested following the
procedure in Example 1. The superior fold and strength properties that were obtained
are given in Table II.

EXAMPLE 2A
[0037] Pine wood chips were processed into a pulp as in Example 1, first paragraph. A dispersion
of the pulp in distilled water was converted to handsheets using a Noble & Wood sheet
mold. The quantity of fiber in the dispersion was adjusted to give a sheet weight
of 7.9 g in the oven dried state. The sheets were wet pressed with blotters at 50
psi (346 kPa) prior to drying.
[0038] Three sets of sheets were prepared. Sheets from the first set were dried on a rotary
drum dryer in a conventional (C) manner. Sheets from the second set were heat treated
(HT) as in Example 1, and sheets from the third set were densified and then heat treated
(PD & HT) as in Example 1. One sample from each set was conditioned at 73°F, 50% relative
humidity ("dry"); another sample was conditioned at 90°F, 90% relative humidity ("moist").
Folding endurance, wet tensile strength and compressive strength tests were then carried
out as in Example 1. The results, summarized below, show a marked improvement in both
folding endurance and in tensile and compressive strength in high moisture conditions.

EXAMPLE 3
[0039] The pine pulp used in Example 1 was subjected to three levels of beating by multiple
passes through an Escher Wyss refiner to decrease the freeness of the pulp. Sheets
were prepared and tested at each process level following the procedure in Example
1. The results in Table 3 again clearly demonstrate the lack of brittleness of the
PD + HT sheets in comparison with sheets treated by the C + HT procedure.

[0040] These values may be compared to those shown in Table I, for unbeaten pulp (720 Canadian
Standard Freeness).
EXAMPLE 4
[0041] On a conventional linerboard machine, three hard covered 12" diameter press nip rolls
were located on drier cans #43, 45 and 47. Furnish of 100% softwood kraft pulp was
run on the machine and a 42 lb/1000 ft² (205g/m²) basis weight linerboard was obtained
at a speed of 1550 ft/min. (473 m/min.). No nip pressure was applied to the nip rolls
mentioned during the first stage of the trial and with conventional drying temperature,
properties outlined below in Table IV were obtained. In the table, "MD" denotes testing
along the machine length; "CD" denotes testing across the machine width.

[0042] When this board was subject to high temperature treatment of 464°F for 30 seconds,
properties shown in Table V were obtained.

[0043] The increase in wet strength, coupled with the very great reduction in folding endurance,
conform to prior art experience. To test the effect of densification, the press nip
rolls were then activated. A force of 230 pli (41 kg/cm) gave a nip pressure of 1225
psi (8445 KPa) and when three pressure nips were applied, the densified board gave
test results as follows:

[0044] The densified board was then heat treated at 464°F for 20 seconds. The following
results were obtained.

[0045] The unexpected lack of brittleness (as measured by the folding endurance test) of
the densified and heat treated product (Table VII) when compared with the other high
wet strength paperboard (Table V) can be identified as a direct result of the sequence
of densification and high temperature treatment.
EXAMPLE 5
[0046] To illustrate the effect of densification prior to conventional or dynamic press
drying, handsheets were prepared from a 60% softwood, 40% hardwood high yield pulp
blend of the linerboard type. The sheets were divided into two main groups. The first
group of sheets were wet pressed at an intensity level approximating that in a conventionally
equipped production machine wet press (CWP). The second group were pressed at an intensity
level approximating that of a modern production machine equipped with a shoe press
(SP).
[0047] Each group of sheets was further subdivided into individual sheets which were retained
for testing after drying on a steam-heated rotating drum, or press drying by passage
through the nip between a press roll and the rotating drum, or by static press drying
between 150 mesh stainless steel screens at 465°F for 30 seconds with 15 psi pressure
applied by means of a suitable press.
[0048] Heat treated control sheets which had been subjected to conventional wet pressing
(CWP) and drying on the rotating drum had high caliper. Such thick sheets have minimal
fiber-fiber contacting points. As adhesive forces develop at such points during drying,
minimal contacting points result in poor folding endurance and wet tensile strength
properties after heat treatment. Densification by use of the shoe press gave lower
caliper and improved contact between fibers, and wet strength also increased. Dynamic
press drying gave somewhat more efficient densification and provided a further improvement
in wet tensile strength. The combination of shoe wet pressing and dynamic press drying
provided further improvements after heat treatment. The final data in the table show
what can be obtained by application of static press drying followed by heat treatment
of sheets which had been subjected to the shoe pressing procedure.

EXAMPLE 6
[0049] Pine wood chips from the southeastern United States were cooked by the kraft process
to an extent typical of pulp used in linerboard production. The cooked chips were
converted to a pulp by passage through a disk refiner. The pulp was bleached and washed
with water to remove residual black liquor and was stored in the wet state at 38-42°F
(3°-6°C) in a refrigerator until sheets were prepared. The cooked, bleached pulp contained
substantially no lignin and had a freeness of 720 ml by the Canadian Standard Freeness
test, which values are typical of a bleached pine pulp prior to beating.
[0050] A dispersion of the pulp in distilled water was converted to handsheets using a TAPPI
sheet mold. The quantity of fiber in the dispersion was adjusted to give a TAPPI sheet
weight of 3.6 g in the oven dried state, said weight being close to that of an air
dried, 42 lb/1000 ft² (205 g/m²) commercial sheet. The sheets were wet pressed with
blotters at 60 psi (415 kPa) prior to drying.
[0051] Three sets of sheets were prepared. Sheets from the first set were dried on TAPPI
rings at room temperature according to TAPPI standard T205 om-81. This is a conventional
(C) drying procedure. Sheets from the second set were also dried by the conventional
procedure but this procedure was followed by a heat treatment (HT). The paper sheet
was placed between two 150 mesh stainless steel screens, which assembly was placed
in the platen press. Heat treatment was in accordance with the conditions found optimum
for this invention, namely 60 seconds at 465°F (240°C) sheet internal temperature.
To do this, single sheets were placed in a 465°F (240°C) Carver platen press for 60
seconds with 15 psi (105 KPa) as applied pressure. Individual sheets from the third
set were inserted in the wet state in a different platen press at 280°F (138°C). A
pressure of 15 psi (105 KPa) was maintained for 5 seconds to dry surface fibers, after
which the pressure was increased to 790 psi (5450 KPa) for 20 seconds. On completion
of this press densification process (PD) sheet moisture was about 10%. Each sheet
was removed from the PD press and immediately placed in the other, HT press for 4
seconds at 465°F (240°C). All three sets of sheets were conditioned at 73°F (23°C)
and 50% humidity for at least 24 hours before testing.
[0052] Folding endurance and wet tensile strength were the tests that were carried out.
Wet tensile tests were carried out immediately after excess water was blotted from
test sheets which had been removed after 4 hours immersion in distilled water. Otherwise,
this test was the same as the ASTM standard wet tensile test.
[0053] The results summarized in Table IX show superior folding endurance and wet strength
for the density and heat treated sheets.

EXAMPLE 7
[0054] A southern hardwood bleached kraft pulp in the never-dried state was processed in
accordance with the procedure in Example 6. The test results illustrate the lack of
wet pulp strength and the somewhat brittle nature of conventionally dried hardwood
pulp sheets. Heat treatment of the conventionally dried sheets produced rather mediocre
wet strength accompanied by increased brittleness. However, sheets processed in accordance
with this invention gave fold values improved by a factor of almost four, thereby
demonstrating a pronounced lowering or brittleness in the sheets, which also had significantly
improved wet strength.

Example 8 illustrates the process of this invention when applied to TMP board.
EXAMPLE 8
[0055] Pine wood chips from the southeastern United States were converted to a pulp by passage
through a 250°F (121°C) disk refiner. The pulp was stored in the wet state at 38-42°F
(3°-6°C) in a refrigerator until sheets were prepared.
[0056] A dispersion of the pulp in distilled water was converted to handsheets using a TAPPI
sheet mold. The quanity of fiber in the dispersion was adjusted to give a TAPPI sheet
weight of 3.6 g in the oven dried state, said weight being close to that of an air
dried, 42 lb/1000 ft² (205 g/m²) commercial linerboard sheet. The sheets were wet
pressed with blotters at 60 psi (415 kPa) prior to drying.
[0057] Three sets of sheets were prepared. Sheets from the first set were dried on TAPPI
rings at room temperature according to TAPPI standard T205 om-81. This is a conventional
(C) drying procedure. Sheets from the second set were also dried by the conventional
procedure but this procedure was followed by a heat treatment (HT). The paper sheet
was placed in a 465°F (240°C) Carver platen press for 60 seconds with 15 psi (105
KPa) as applied pressure. Individual sheets from the third set were inserted in the
wet state in a different platen press at 280°F (138°C). A pressure of 15 psi (105
KPa) was maintained for 5 seconds to dry surface fibers, after which the pressure
was increased to 790 psi (5450 KPa) for 20 seconds. On completion of this press densification
process (PD) sheet moisture was about 10%. Each sheet was removed from the PD press
and immediately placed in the other, HT press for 60 seconds at 465°F (240°C). All
three sets of sheets were conditioned at 73°F (23°C) and 50% humidity for at least
24 hours before testing.
[0058] Folding endurance and wet tensile strength were the tests that were carried out.
Wet tensile tests were carried out immediately after excess water was blotted from
test sheets which had been removed after 4 hours immersion in distilled water. Otherwise,
this test was the same as the ASTM standard wet tensile test.
[0059] The results summarized in Table X show superior folding endurance and wet strength
for the densified and heat treated sheets.

[0060] surface fibers, after which the pressure was increased to 790 psi (5450 KPa) for
20 seconds. On completion of this press densification process (PD) sheet moisture
was about 10%. Each sheet was removed from the PD press and immediately placed in
the other, HT press for 60 seconds at 465°F (240°C). All three sets of sheets were
conditioned at 73°F (23°C) and 50% humidity for at least 24 hours before testing.
[0061] Folding endurance and wet tensile strength were the tests that were carried out.
Wet tensile tests were carried out immediately after excess water was blotted from
test sheets which had been removed after 4 hours immersion in distilled water. Otherwise,
this test was the same as the ASTM standard wet tensile test.
[0062] The results summarized in Table X show superior folding endurance and wet strength
for the densified and heat treated sheets.

Example 9
[0063] A mixture of spruce and fir wood chips was cooked by the SCMP process to a yield
of 92% by weight of dry chips. The cooked chips were converted to a pulp by passage
through a disk refiner. The pulp was washed with water to remove residual cooking
chemical and solubilized material. Latency removal was accomplished by stirring at
4% consistency for 20 minutes at 85-90°C. Pulp freeness was 705 ml by the Canadian
Standard Freeness Test.
[0064] A dispersion of the pulp in distilled water was converted to handsheets using a TAPPI
sheet mold. The quantity of fiber in the slurry fed to the mold was adjusted to give
a basis weight of 42 lb/1000 ft² (205 g/m²) in the oven dried state.
[0065] Two sets of sheets were prepared. Sheets from the first set were dried on TAPPI rings
at room temperature after wet pressing. Wet pressing and drying were in accordance
with the procedure in TAPPI T-205 om-81. Sheets from the second set were placed between
two 150 mesh stainless steel screens and pressed in a platen press at 300 psi (2067)
kPa) and 450°F (232°C) platen temperature for different times between 5 and 60 seconds.
This drying procedure effectively combines the densification and heat treatment stages
and is known as high temperature press drying (HTPD). All sheets were conditioned
at 73°F (22.5°C) and 50% humidity for at least 48 hours before testing.
[0066] Folding endurance, wet tensile and conditioned tensile strengths were the tests that
were carried out. Wet tensile tests were run immediately after excess water was blotted
from test sheets which had been removed after four hours immersion in distilled water.
Otherwise, this test was the same as the ASTM standard tensile test for a conditioned
sheet.

[0067] The improved tensile properties, both wet and conditioned, and the lowered brittleness
as illustrated by the increased number of double folds, are in accordance with the
invention.
Example 10
[0068] A sample of a commercial low yield sulfite pulp in the never dried state, prepared
from northern softwood chips, was obtained and converted to handsheets using a TAPPI
mold. The quantity of fiber in the slurry fed to the mold was adjusted to give a basis
weight of 42 lbs/1000ft² (205.5 kg/M²) in the oven dried state. Four sets of sheets
were prepared and wet pressed as specified in accordance with the procedure in TAPPI
T-205 om-81. Two of the four sets of sheet were dried on rings as required by the
procedure. These sheets were considered to be dried by a conventional (C) method.
One of the two sets of dry sheets was then subjected to heat treatment. For heat treatment,
each sheet was placed between two 150 mesh stainless steel screens and inserted between
the platens of a preheated platen press. Press temperatures of 392, 428, 454°F (200,
220 and 240°C) were studied. The platens were immediately closed and 15 psi (103.4
kPa) pressure was applied for 5 seconds. Sheets were immediately removed from screens
and allowed to cool after pressing.
[0069] Preliminary experiments using a thermocouple wire buried in the sheet showed the
sheet internal temperature after 2 seconds is only 1-2°C lower than the platens temperature.
[0070] The third and fourth sets of sheets were placed between the 150 mesh screens and
densified by a press densification (PD) procedure during the process of drying. To
carry out the PD procedure, the wet sheets and the screens were placed between the
platens of a second press and subjected to 15 psi (103.4 kPa) pressure at 138°C for
5 seconds to dry surface fibers, after which the pressure was increased to 790 psi
(5443 kPa) for 20 seconds. On completion of this PD process, sheet moisture was about
10%. One set of sheets was retained for testing. EAch individual sheet and screens
from the second set were removed from the PD press and immediately placed in the other,
HT press for 5 seconds. HT press temperatures of 200, 220 and 240°C were studied.
HT pressure was 15 psi (103.4 kPa). All sheets were conditioned at 22.5°C for at least
48 hours before testing.
[0071] Fold and wet tensile strengths were determined as specified in Example 8

[0072] The results show that wet strength improves as heat treatment temperature is increased.
Fold decreases as heat treatment temperature is increased, but the decrease is much
less pronounced for the densified, heat treated sheets. This shows that the densified
sheets are much less brittle than the conventional sheets, even after heat treatment
to yield enhancement of wet strength.
1. A method of producing paper products with improved wet strength from bleached or
unbleached kraft pulp, thermomechanical pulp, SCMP or sulfite pulp, while preserving
its folding endurance, comprising steps of
subjecting paper to high pressure densification during its production, and
heating the paper so as to raise its internal temperature to at least 420°F (216°C)
for a period of time sufficient to increase the wet strength thereof.
2. The method of claim 1, wherein said densification and heating steps are carried
out simultaneously.
3. The method of claim 1, wherein said densification step precedes said heating step.
4. The method of claims 1 to 3, wherein said internal temperature is in the range
of 420°F (216°C) to 572°F (300°C).
5. The method of claims 1 to 4, wherein the kraft pulp is unbleached and the internal
temperature is about 550°F (289°C), and when the pulp is bleached, or when the pulp
is thermomechanical pulp, the internal temperature is about 465°F (240°C) and when
the pulp is SCMP or sulfite pulp, the internal temperature is about 450°F (232°C).
6. The method of claims 1 to 5, wherein in said densification step the paperboard
is compressed to a density of 600 to 1200 kg/m³.
7. The method of claims 1 to 6, wherein said densification includes applying sufficient
pressure to the paper to produce density in range of 700-900 kg/m³ prior to said heating
step.
8. The method of claims 1 to 7, wherein said paper prior to said densification step,
has a moisture content in the range of 10% to 70% by weight.
9. The method of claims 1 to 8, wherein said paper product is linerboard or paperboard.
10. The method of claim 9, wherein said paper product is linerboard and has a basis
weight in the range of 125 to 464 g/m².
11. The method of claims 1 to 9, wherein said paper product is paperboard and has
a basis weight in the range of 30 to 464 g/m² and when the paperboard is produced
from thermomechanical pulp, the basis weight is 60-464 g/m².
12. A linerboard of high wet strength and high folding endurance, producible with
the method according to any of claims 1 to 11.
13. A linerboard as in claim 12, having a wet strength of at least 15 lb/in, and satisfying
a folding endurance test of at least 300 cycles, preferably at least 1000 cycles.
14. A linerboard as in claim 12, from SCMP or sulfite pulp, having a wet strength
of at least 6 lb/in, and satisfying a folding endurance test of at least 10 cycles.
15. A bleached kraft paperboard of high wet strength and high folding endurance, producible
with the method according to any of claims 1 to 9 and 11.
16. A bleached kraft paperboard as in claim 15, having a wet strength of at least
5 lb/in, and satisfying a folding endurance test of at least 50 cycles.
17. A bleached kraft paperboard as in claim 15, having a wet strength of at least
15 lb/in, and satisfying a folding endurance test of at least 300 cycles.
18. A paperboard of high wet strength and high folding endurance, producible from
thermomechanical pulp with the method according to any of claims 1 - 9 and 11.
19. A paperboard as in claim 18, having a wet strength of at least 10 lb/in, and satisfying
a folding endurance test of at least one cycle.
20. An apparatus for carrying out the method according to any of claims 1 to 11.