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Патент USA US3043723

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July 10, 1962
R. J. BOYER
3,043,713
PROCESS FOR COATING NON-FIBROUS ORGANIC SHEET MATERIAL
Filed May 1:5, 19:58
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INVENTOR
ROBERT JAY BOYER
BY %%%
ATTORNEY
United States Patent 0 " ICC
3,043,713
Patented July 10, 1962
1
2
3,043,713
remaining on the ?lm is made smooth, the [?lm passes
through an adjustable slot 21 into the dryer section 20.
Hot air heated by the heater 23 to a temperature of at
PROCESS FQR COATING NON-FIBROUS
ORGANIC SHEET MATERIAL
Robert Jay Boyer, Clinton, Iowa, assignor to E. I. du
Pont de Nemours and Company, Wilmington, DeL, a
corporation of Delaware
‘
Filed May 13, 1958, Ser. No. 734,903
5 Claims. (Cl. 117-62)
This invention relates to coating non-?brous, organic 10
sheet materials and has as its primary object, a continuous
process for coating ?lms, webs or sheets of regenerated
cellulose with a moisture-proo?ng composition at rela
tively high speeds. Other objects willappear hereinafter.
least 190° F., but which may be as high as 350° F., is
circulated through this section by means of a blower 22.
The air serves to dry the coated ?lm and to carry the
solvent vapor through the opening 24. The solvent vapor
may be recovered from the solvent-air mixture in a sep
arate operation.
After being dried in the dryer section 20, the coated
?lm passes into the cooling section ‘33 through the slot
34. In the cooling section the ?lm is cooled to a temper
ature of not lower than 60° F., but below 100° F. This
range of temperature is critical to the operation of the
The objects are accomplished by a continuous process 15 present process and its importance will be discussed in
greater detailsubsequently. Cooling is accomplished by
comprising the steps, in sequence, of passing the sheet
passing cold water through the roll 26 by feeding the cold
material through a bath containing a liquid coating com
water through inlet 36 and removing the water through
position; removing excess coating liquid from the surface
outlet 37. The ?lm passes over the cooled roll 26 and
of the sheet material; drying the coated sheet material at
then downwardly through the slot 27 into the condition
a temperature of at least 190° F. ; cooling the‘coated sheet
material to a temperature of not lower than 60° F. but
below 100° F.; and humidifying the dried coated sheet
material by exposure to a moist atmosphere, preferably
an atmosphere at a temperature of l58°—185° F. having
ing or humidifying section 25 of the coating tower.
In the conditioning section moisture is added to the base
?lm. The amount added serves to replace the amount
lost by the base ?lm during ‘drying, and to bring the mois
a relative humidity of 85-99%. The process as described 25 ture content of the ?lm up to the desired level. This is
has been found most useful when coating at speeds of
at least 250 yards/minute.
The FIGURE is a side elevation of one form of appara
accomplished by circulating moist air (air having a rela
tive humidity of at least 85%) at a temperature of 158°
185° F. into the section at 28 and out at 29.
The con
generated cellulose ?lm 10, the so-called :base ?lm, is un
wound from the roll 11 and enters the coating tower 12
ditioned coated ?lm passes under roll 31, out through
opening 35, and is collected on roll 32.
It may be desirable to apply the moisture-proo?ng coat
ing composition to one side only of the sheet material.
vent. The coating composition, in general, comprises a
mil, pliability is obtained with moisture contents of at
tus suitable for carrying out the process of the invention.
In the embodiment shown in the ?gure, uncoated re
This is easily accomplished by merely raising the dip roll
through an opening 13. It will be noted that the ?lm
18 so that only a portion of the roll is below the level
enters at the lower portion of the dryer section 20 of the
tower although this is not essential to the present inven 35 of the coating composition in dip tank 17. In addition, a
doctor roll would replace the doctor knife contacting the
tion. Here the ?lm receives preliminary heating by the
uncoated side of the sheet material.
circulating hot air.
,
The result of the process is a smooth, adherent, mois
The ?lm then passes over roll 14 and enters the coating
ture-proof coating on the regenerated cellulose ?lm. The
section 30 of the tower through the slot 15. The ?lm
passes into the dip tank 17; around roll 18; and upwardly 40 coated ?lm is very pliable and free of appearance de
fects. The pliability of the ?lm is due to its high mois
between doctor knives 19. The dip tank 17 contains a
ture content. For ?lms having a thickness of up to 1
moisture-proo?ng coating composition dissolved in a sol
least 7.5%. For thicker ?lms, i.e. about 1.2-1.5 mils,
cellulose derivative, a resin, a wax and a plasticizer. The
cellulose derivative may be a cellulose ester or cellulose 45 a minimum moisture content of 7.0% has been found to
ether, but is preferably nitrocellulose and represents 30
be satisfactory. Sheet materials coated according to the
70% of the composition. The resin may be a gum or a
resin, either natural or synthetic, such as ester gum, rosin,
present invention are suitable ‘for use as packaging for
gum mastic, a copal resin, etc. and represents 10-60% of
the coating composition. The wax is preferably a color 50
as tank linings, etc.
less, odorless, high melting paraf?n wax (i.e., having a
tinguish it from prior art processes are:
food stuffs, textiles, hardware, etc., as bottle cap seals,
'
The critical features of the process which serve to dis
'
melting point above about 140° F.) but may also be
ceresin or beeswax and represents 1-10% of the coating
(1) Cooling the sheet material coated with a compo
sition containing at least 1% parai?n wax to a tempera
composition. As a plasticizer, 540% of one or more of
ture of 60°-100° F. prior to humidi?cation.
the following compounds may be used: tricresyl phos 55
(2) ‘Humidifying the coated sheet material at a tem
phate, triphenyl phosphate, diamyl phthalate, dibutyl
perature of 158°—185° ‘F. in a moist atmosphere, i.e., an
phthalate, dicyclohexyl phthalate or castor oil. While the
atmosphere having ‘a relative humidity of at least 85%.
particular solvent must be determined for the particular
The following theory is offered to explain the surpris
composition used, the following provide a basic group
ingly effective results of the present invention but the
from which selection of an appropriate solvent can be 60 theory should not be construed to limit the scope of the
made: alcohol, ether, toluene, ethyl acetate and butyl
invention. In the operation of the process, the heated
acetate. The coating liquid is maintained at a tempera
coated ?lm emerging from the top of the drying section
ture of 100°-125° F.
of the coating tower is cooled to a temperature within
To prevent premature gelation of the coating on the
the above mentioned critical limits. When the cooled
surface of the ?lm, the doctor knives 19 should be located 65 ?lm enters the humidifying section of the tower, moisture
close to the coating bath in dip tank 17. The gap‘ between
immediately condenses on the coated surface or surfaces
knife blades should be about 11/: inches with the edges
of the ?lm. Condensation ‘of moisture serves to release
overlapping slightly. The overlap is adjusted to provide
heat. The amount of heat released, it is believed, must
the desired coating thickness. As an alternative to doctor
be suf?cient to raise the temperature of the coating above
knives, doctor rolls may be used in a similar manner. 70
the-softening temperature of the wax in the coating, i.e.,
After passing between the doctor knives 19‘ where excess
above about 140° F., in order to permit the penetration of
coating is removed from the ?lm surface and the coating
3,043,713
r,
K)
o
moisture. It the ?lm is cooled in the cooling section
4
maintained between 165 ° F. and 175° F. and at a rela
tive humidity of about 90%.
The moisture content of the resulting coated regenerated
cellulose ?lm averaged 7.8% and the coated ?lm was
ing above 140° F.; the wax layer, therefore, remains (as 01 smooth and clear.
of the tower to a temperature below 60° F., then the
amount of moisture condensed and the accompanying
heat released does not raise the temperature of the coat
it is ‘in the ?nal product) {substantially impermeable to
moisture; and the resulting moisture content in the prod
Example III
uct is not as high as ‘necessary to provide the desired pli
able product. If the ?lm is cooled to a temperature above
100° F., then the surface is too warm and not enough
The speed of the ?lm through the coating tower was
420 yards/minute. The temperature in the cooling sec
tion was about 68° F.
The humidifying section was
that 'penetratesthe wax layer is not as high as necessary
maintained between 165 ° F. and 175 ° F. and at a rela
tive humidity of about 90%. ‘
to provide the desired pliable product.
Although cooling has been accomplished in the ‘fore
The moisture content of the resulting coated regenera
ted cellulose ?lm averaged ‘above 7.5% and the coated
'moisture condenses initially; and, hence, the moisture
going description by passing the ?lm over a cooled roll, 15 ?lm was smooth and clear.
As many widely di?ferent embodiments can be made
numbered‘z? in the ?gure, through which cold water or
without departing from the scope of this invention, it is
cold brine is circulated, other means for cooling the ?lm
understood that the invention is not limited except as de
may be used. Cold air jets to pass cold air through the
?ned in the appended claims.
cooling. section 33‘ of the coating tower may be used with
Having fully described the invention, what is claimed is:
similar results.
1. A continuous process for coating regenerated cellu
In the cfollowing examples the importance of the pres
lose ?lm which comprises the steps, in sequence, of pass
ent invention will :be apparent, particularly for a process
ing a web of regenerated cellulose ?lm through a mois
operated at coating speeds above 250 yards/ minute. In
ture-proo?ng composition containing 30-70% nitrocellu
all the examples the procedure depicted in the ?gure was
used with a 300 gauge regenerated cellulose ?lm (ap
lose and 1-10% parai?n wax dissolved in a solvent, said
wax having a melting point of at least about 140° F.;
driving off the solvent ‘from the coated web at a tempera
ture of at least 190° F.; cooling the coated web to a tem
‘ proximately 0.9 mil thick) and the following moisture
proo?ng composition in dip tank 17:
perature of 60° F.-l00° F.; and, thereafter, humidifying
Parts By
_
Compound
Percent in
Weight
'
30 said dried coated web to a moisture content of at least
7.5% by exposing said web to a moist atmosphere at a
temperature of 158° F.-185° F.
Coating
Composition
Nitrocellulose (11.4% nitrogen) ______________ -_
56. 2
48
11.7 }
15
2. A process as in claim 1 wherein the moist atmos
phere during the humidifying step has a relative humidity
Resin:
“Petrex-7-H’I‘" 1 ..... --_
5.8
Crystalline para?'in (melting point 140° F.)__._
>
Polypale WB z _______ __
-_
3.5
Plasticizer:
‘ of at least 85%.
3
,.
Dibutyl phthalate _______________________ _.
19.9 }
34
3. A process as in claim 1 wherein the moist atmos
phere during the hurnidifying step has a relative humidity
of 85-99%.
4. A process 'as in claim 1 wherein the web is treated
40 at a speed of at least 250 yards/minute.
5. A continuous process for coating regenerated cellu
lose ?lm which comprises the steps, in sequence, of pass
1 A diethylene glycol ester of terpene-nialeic acid manufactured by
ing a web of regenerated cellulose ?lm through a mois~
Hercules Powder C0. in accordance with USP 2,236,546.
tureeproo?ng composition containing 30‘-70% of a cellu
1 A sulfuric acid-modi?ed wood rosin manufactured by Hercules
Powder Co. in accordance with USP 2,017,866.
lose derivative and .*1—10% of paraf?n wax dissolved in a
solvent, said wax having a melting point of at least about
Example I
140° F.; driving off the solvent from the coated web‘ at a
temperature of at least 190° F.; cooling the coated web to
The speed of the ?lm through the coating tower was 300
a temperature of 60° F.—-l00° F.; and, thereafter, expos
yards/minute. The temperature in the cooling section
ing said web to a moistv atmosphere at a temperature of
was 100° F. The humidi-fying section was maintained
158° F.—185° F.
between 165° (F. and 175° F. and at a relative humidity
Dicyclohexyl phthalate.__
19. 9
Solvent:
Ethyl acetate". _______ __
573. 9
Toluene . _ _ . . . . . . _ _ . . . _ . _ _
__________ __
_ . _ _ _ _ . ._
285. 0
__________ ._
Ethyl alcohol ___________________ __' ______ ._
24.1
__________ __
of about 90%.
.
'
Themoisture content of the resulting regenerated cellu
lose ?lm averaged 7.6% ‘and the coated ?lm was smooth 55
and clear.
Example II
The speed of the ?lm through the coating tower was
330yards/minute. The temperature in the cooling sec
tion was about 85‘? F.
The humidifying section was 60
References Cited in the ?le of this patent
UNITED STATES PATENTS
1,826,699
2,159,152
2,350,292
2,354,060
Charch et 'al ____________ __ Oct. 6,
Hershberger __________ __ May 23,
Sermattei et a1 _________ __ May 30,
Rhodes et a1. __________ __ July 18,
1931
1939
1944
1944
2,808,340
Learn _________ _; _____ .._ Oct. 1, 1957
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