U.S. patent number RE28,914 [Application Number 05/270,784] was granted by the patent office on 1976-07-20 for treatment of a cellulosic-containing textile with a fluorocarbon, an aminoplast, and a synthetic acid copolymer, and textile obtained therefrom.
This patent grant is currently assigned to Deering Milliken Research Corporation. Invention is credited to Francis W. Marco.
United States Patent |
RE28,914 |
Marco |
* July 20, 1976 |
Treatment of a cellulosic-containing textile with a fluorocarbon,
an aminoplast, and a synthetic acid copolymer, and textile obtained
therefrom
Abstract
A process for imparting oil and water repellency, soil release,
and durable press characteristics to a celluosic-containing textile
material and product produced by this process, comprising applying
thereto an aminoplast textile resin, a textile resin catalyst, a
fluorocarbon, and a synthetic acid copolymer, and curing at a
temperature of 100-200.degree.C.
Inventors: |
Marco; Francis W. (Spartanburg,
SC) |
Assignee: |
Deering Milliken Research
Corporation (Spartanburg, SC)
|
[*] Notice: |
The portion of the term of this patent
subsequent to April 9, 1985 has been disclaimed. |
Family
ID: |
26954496 |
Appl.
No.: |
05/270,784 |
Filed: |
July 11, 1972 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
|
Reissue of: |
622086 |
Mar 10, 1967 |
03597145 |
Aug 3, 1971 |
|
|
Current U.S.
Class: |
442/80; 442/94;
8/115.6; 38/144; 427/392; 427/393.2; 427/498; 427/501; 427/506;
427/512; 427/513; 427/520; 522/65; 522/66; 522/74; 522/116;
524/462; 524/512 |
Current CPC
Class: |
D06M
15/263 (20130101); D06M 15/277 (20130101); D06M
15/29 (20130101); D06M 15/423 (20130101); Y10T
442/2172 (20150401); Y10T 442/2287 (20150401) |
Current International
Class: |
D06M
15/21 (20060101); D06M 15/37 (20060101); D06M
15/277 (20060101); D06M 15/29 (20060101); D06M
15/423 (20060101); D06M 15/263 (20060101); D06M
015/58 (); D06M 015/54 () |
Field of
Search: |
;117/161UT,143A,138.8F,139.4,161LN,161UZ,161UC,161UF ;8/116.3,115.6
;427/36,44,390,392 ;428/272,274,275,278,279 |
References Cited
[Referenced By]
U.S. Patent Documents
Other References
J Berch and H. Peper: "Wet Soiling of Cotton," Textile Research
Journal, vol. 34, No. 1, Jan. 1964, pp. 29-34. .
"A Study of Fluorocarbon Finishes and Their Effect on Dyestuffs,"
American Dyestuff Reporter, Oct. 31, 1960, p. 33-38..
|
Primary Examiner: Gwinnell; Harry J.
Assistant Examiner: Schmidt; William H.
Attorney, Agent or Firm: Petry; H. William Urban; Arthur
L.
Claims
Having thus disclosed the invention, what is claimed is:
1. A process for imparting oil and water repellency, soil release
and durable press characteristics to a cellulosic-containing
textile material which comprises applying thereto an aminoplast
textile resin; a textile resin catalyst, a fluorocarbon oil and
water repellent material, and a synthetic acid soil release
copolymer derived from an ethylenically unsaturated carboxylic
acid, said acid polymer comprising at least about 20 weight percent
acid calculated as acrylic acid; and subjecting said textile
material to textile resin curing conditions at a temperature
between about 100.degree. and 200.degree. C., whereby the textile
resin is crosslinked to the textile material, the proportion of
said fluorocarbon oil and water repellent material on said textile
material being between about 0.01% and 5% by weight based on the
dry weight of the textile material and the proportion of said acid
polymer on said textile material being between about 0.25% and 5%
by weight based on the dry weight of the textile material.
2. A process for imparting oil and water repellency, soil release
and durable press characteristics to a cellulosic containing
textile material which comprises applying thereto an unsaturated
aminoplast textile resin, a textile resin catalyst, a fluorocarbon
oil and water repellent material and a synthetic acid soil release
copolymer derived from an ethylenically unsaturated carboxylic
acid, said acid polymer comprising at least about 20 weight percent
acid calculated as acrylic acid; drying said textile material at a
temperature in the range of about 225.degree. F. to 300.degree. F.;
subjecting said textile material to between about 1000 rads and 100
megarads irradiation; and subsequently curing the textile resin at
a temperature between about 100.degree. and 300.degree. C., the
proportion of said fluorocarbon oil and water repellent material on
said textile material being between about 0.01% and 5% by weight
based on the dry weight of the textile material and the proportion
of said acid polymer on said textile material being between about
0.25% and 5% by weight based on the dry weight of the textile
material.
3. A process for imparting oil and water repellency, soil release
and durable press characteristics to a polyethylene
terephthalate/cotton (65/35) textile material which comprises:
(a) applying thereto an aqueous system consisting essentially of
about 2 to 30% of an aqueous solution of N-methylol acrylamide,
about 1 to 15% of an aqueous solution of a catalyst selected from
the group consisting of zinc nitrate and magnesium chloride, at
least about 0.1% of an organic fluorocarbon oil and water repellent
material, about 2.5 to 40% of an aqueous dispersion of a synthetic
acid polymer prepared by polymerizing a monomeric mixture of about
10 to 80 parts ethyl acrylate and about 20 to 90 parts acrylic
acid, and water; said aqueous dispersion being applied to the
textile material in the range of 30 to 100 weight percent of the
textile material;
(b) drying the textile material at a temperature in the range of
about 225.degree. F. to 300.degree. F.;
(c) subjecting the textile material to irradiation such that said
material is exposed to a dosage of about 1000 rads to 100 megarads;
and
(d) heating the textile material at a temperature in the range of
about 100.degree. C. to 300.degree. C. to cure the textile resin;
the proportion of said fluorocarbon oil and water repellent
material on said textile material being between about 0.01% and 5%
by weight based on the dry weight of the textile material and the
proportion of said acid polymer on said textile material being
between about 0.25% and 5% by weight based on the dry weight of the
textile material.
4. The process as defined in claim 1 wherein the synthetic acid
polymer is prepared by polymerizing a monomeric mixture comprising
an acrylic ester and an acrylic acid.
5. A textile material having improved oil and water repellency,
soil release and durable press characteristics produced according
to the process of claim 1.
6. A textile material having improved oil and water repellency,
soil release and durable press characteristics produced according
to the process of claim 2.
7. A textile material having improved oil and water repellency,
soil release and durable press characteristics produced according
to the process of claim 3.
8. The process as defined in claim 1 wherein the soil release
polymer and the oil and water repellent material are applied
sequentially.
9. A process as defined in claim 1 wherein the textile resin
catalyst is selected from the group consisting of metal salts and
amino salts.
10. The process as defined in claim 1 wherein the textile resin is
selected from the group consisting of acrylamides and ethylene
ureas.
11. The process as defined in claim 1 wherein the textile resin is
selected from the group consisting of N-methylol acrylamide and
dihydroxydimethylol ethylene urea.
12. The process as defined in claim 1 wherein the textile material
is a polyester/cotton blend.
13. The process as defined in claim 1 wherein the soil release
polymer is prepared by polymerizing a monomeric mixture comprising
about 10 to 80 parts of an acrylic ester and about 20 to 90 parts
of an acrylic acid.
14. The process as defined in claim 2 wherein the textile resin is
N-methylol acrylamide.
15. The process as defined in claim 2 wherein the textile material
is subjected to an irradiation dosage of about 0.5 to 5
megarads.
16. The textile material as defined in claim 1 wherein said textile
material is a polyethylene terephthalate/cotton blend. .Iadd.17. In
a process for improving the soil release properties of a textile
material wherein the textile material is impregnated with a
composition including a durable press textile reactant selected
from water-soluble precondensates of formaldehyde with amino
compounds and a water-insoluble acrylic hydrophilic polymer which
absorbs about seven times its weight of water when immersed in an
aqueous detergent solution for 2 minutes at 140.degree. F., said
polymer being an addition polymer of at least one ethylenically
unsaturated monomer having one or more acid groups, and then drying
and curing, the improvement which comprises applying said durable
press reactant and hydrophilic polymer to said textile in a stable
aqueous mixture with an oil and water repellent fluoro-acrylic
polymer characterized by (CF.sub.2) groups and a terminal CF.sub.3
group, the amount of fluoro-acrylic polymer being in the range of
4-100% based on the weight of said hydrophilic polymer, the
proportion of said fluoro-acrylic polymer on said textile material
being between about 0.01% and 5% by weight based on the dry weight
of the textile material and the proportion of said acrylic
hydrophilic polymer on said textile material being between about
0.25% and 5% by weight based on the dry weight of the textile
material. .Iaddend. .Iadd. 18. The process of claim 17 wherein said
material is cellulosic, polyester, or a mixture thereof.
.Iaddend..Iadd. 19. The process of claim 17 wherein said mixture is
applied as an aqueous emulsion including an ethylene oxide
emulsifying agent. .Iaddend..Iadd. 20. A process according to claim
17 wherein said acrylic hydrophilic polymer is a methacrylic
acid/ethyl acrylate copolymer. .Iaddend. .Iadd. 21. The process of
claim 17 wherein said polymer is one selected from the group
consisting of polyacrylic acid; acrylic acid and methacrylic acid
copolymers with styrene; copolymers of itaconic acid and acrylic
acid; copolymers of ethyl acrylate and methacrylic acid;
terpolymers of methacrylic acid, butadiene and styrene; and
terpolymers of monomethyl
itaconate, acrylic acid and itaconic acid. .Iaddend..Iadd. 22. A
durable press textile having improved soil release properties, said
textile being finished with a cured durable press and soil release
finish consisting essentially of a mixture of durable press
reactant selected from water-soluble precondensates of formaldehyde
with amino compounds and a water-insoluble acrylic hydrophilic
polymer which absorbs about seven times its weight of water when
immersed in an aqueous detergent solution for 2 minutes at
140.degree. F., said polymer being an addition polymer of at least
one ethylenically unsaturated monomer having one or more acid
groups, and oil and water repellent fluoro-acrylic polymer
characterized by (CF.sub.2) groups and a terminal CF.sub.3 group,
the amount of fluoro-acrylic polymer being in the range of 4-100%
based on the weight of hydrophilic polymer, the proportion of said
fluoro-acrylic polymer on said textile material being between about
0.01% and 5% by weight based on the dry weight of the textile
material and the proportion of said acrylic hydrophilic polymer on
said textile material being between about 0.25% and 5% by weight
based on the dry weight of the textile material.
Description
BACKGROUND OF THE INVENTION
The textile industry during the past decade has, as a whole, made
important technological advances in the chemical finishing of
textile fabrics. Numerous processes have been developed for
imparting minimum care characteristics to garments and articles
prepared from specially treated textile fabrics. Exemplary of such
advances are the wash and wear fabrics, hereinafter referred to as
precured fabrics, and the durable press fabrics, hereinafter
referred to as post cured fabrics. These characteristics generally
have been imparted to textile fabrics by the application of
resinous materials. The resinous materials are applied to the
fabric and are later crosslinked to the fabric by the action of a
suitable catalyst. Depending upon the time at which the
crosslinking reaction occurs, either a wash and wear fabric or a
durable press fabric is produced. The precured fabrics are those
for which the crosslinking reaction has occurred prior to
transformation of the fabric into a garment or other article of
commerce. Post cured fabrics are those fabrics which are subjected
to the crosslinking reaction subsequent to the transformation of
the fabric into a garment or other article of commerce.
The precured and post cured fabrics, by way of fiber content, may
contain any of a number of natural or synthetic materials.
Presently, however, the majority of these fabrics include
synthetic, man-made fibers. These synthetic fibers offer tremendous
advantages to the fabrics as opposed to fabrics containing only the
natural materials. One drawback, however, is the fact that the
synthetic fibers have a propensity to soiling and as such, the
garment during normal wear may come into contact with oily type
materials which are accepted due to the oleophilicity of the
synthetic fibers. These oily type materials, however, are very hard
to remove due to the hydrophobic properties of the synthetic
fibers. Accordingly, once the garment comes into contact with these
stain-producing materials, it cannot be cleaned by wash and wear
laundering procedures, but must be dry cleaned to successfully
remove the stains from the garment. Furthermore, even in the
absence of the stain-producing material, repeated washing of a
garment including synthetic fibers causes the garment to assume a
dingy gray color due to soil that is picked up in the wash water.
Such soil pickup is referred to as "soil redeposition."
The soiling problem previously mentioned brought about a still
further technological innovation in the textile industry--a wash
and wear or durable press fabric having soil release
characteristics. The term "soil release" does not infer soil
resistance, but only the characteristic that once a fabric is
soiled, it may then be successfully cleaned via the normal wash
cycle. Furthermore, the fabrics, and/or garments that are treated
to have soil release characteristics also have the characteristic
of not taking up soil from the wash water, i.e., soil in the wash
water will not be redeposited onto the garment being washed.
Paralleling the development of durable press and wash and wear
fabrics has been the work in imparting oil and water repellency to
fabrics. Numerous means have been developed for imparting water
repellency to fabrics including the following types of water
repellent substances; (1) wax emulsions; (2) water repellents based
on pyridinium compounds, long chain fatty amides, resin-wax
mixtures; (3) silicones; (4) organo-chromium compounds; and (5)
fluorochemicals.
The fluorochemical type water repellents are probably the most
commonly used water repellent today. Two commercially available
fluorochemical compositions are FC-208, the fluorocarbon ingredient
of Scotchgard treated fabrics, sold by Minnesota Mining and
Manufacturing Company and Zepel, a water repellent fluorochemical
sold by E. I. du Pont de Nemours & Co. A certain degree of oil
repellency is generally achieved with the water repellency imparted
to the fabrics treated with the fluorocarbons.
One drawback of water and oil repellent fabrics is the difficulty
in removing stains by laundering. The water and oil repellency
characteristics, of course, render a fabric both hydrophobic and
oleophobic and presumably resistant to any water or oil. Under
normal circumstances, this resistance provides a degree of
protection from soiling. However, when oil, for instance, is forced
into the fabric by rubbing and/or pressure, it cannot be removed by
laundering due to the fact that the fabric is hydrophobic and will
not accept water that is necessary for removal of the oil. For
example, while rainwear garments repel falling rain, etc., in use
these garments are stained with oils from the body of the wearer
particularly at the collar and the cuffs. These stains may be
partially removed during dry cleaning, but the dry cleaning process
adversely affects the water repellency characteristic of the
garment. On the other hand, these oil stains will not be removed in
normal laundering.
Heretofore, it was not considered possible for a fabric to have oil
and water repellency and also soil release characteristics. This
was because the oil and water repellency were believed to be
achieved due to hydrophobicity and oleophobicity of the fibers
making up the fabric or treatments increasing the hydrophobicity
and oleophobicity. On the other hand, soil release was considered
to be achieved with fibers which were hydrophilic in nature or by
treatments to increase the hydrophobicity of the fibers. Thus, oil
and water repellency were considered to be directly opposite to the
characteristics required for soil release.
An object of the present invention is to provide textile material
with the heretofore unattainable combination of soil and water
repellency characteristics together with soil release
characteristics.
A further object of the invention is to provide a fabric including
synthetic polymeric fibers which has soil and water repellency and
soil release characteristics.
Another object of the invention is to provide a fabric from which
stains can be removed by laundering without destroying the water
and oil repellency characteristics of the fabric.
An additional object of the invention is to provide a fabric
including synthetic polymeric fibers which not only has the
combination of water and oil repellency and soil release
characteristics but also possesses durable press and/or wash and
wear characteristics.
SUMMARY OF THE INVENTION
In accordance with the present invention, water repellency, oil
repellency and soil release characteristics are imparted to a
textile material by a process which comprises applying to the
textile material a soil release polymer and a water and oil
repellent material. Preferably, the textile material is subjected
to textile resin curing conditions. Advantageously, a textile resin
and a textile resin catalyst also are applied to the textile
material.
The process of the present invention may be used to treat a wide
variety of textile materials, i.e., fabrics made exclusively from
naturally occurring fibers, fabrics made exclusively from synthetic
polymeric fibers, as well as blends of natural and synthetic
fibers. The process of the present invention may be utilized on
fabrics containing cellulosic fibers, for example, cotton, viscose,
regenerated cellulose, etc. Examples of fabrics of synthetic fibers
which may be successfully employed in the practice of the present
invention include those made with polyamide, acrylic and
particularly polyester fibers, i.e., various types of Dacron, a
registered trademark of E. I. du Pont; Fortrel, a registered
trademark of Celanese; Kodel, a registered trademark of Eastman
Kodak, etc. Blends of natural and synthetic fibers which may be
utilized to prepare fabrics according to the present process
include fabrics comprising 50% polyester and 50% cotton; 65%
polyester and 35% cotton; etc.
Several theories have been advanced as to proper fabric
construction for obtaining optimum water repellency properties. One
such theory states that the fabric should be woven in such a manner
that the warp and filling elements are very tightly woven together,
whereas the other theory states that a normal or loosely woven
fabric is best treated to obtain water repellency properties. The
present invention, however, is not directed to any particular
fabric construction but to the process for treating a textile
material in such a manner that the combination of water repellency,
oil repellency and soil release characteristics are obtained.
While various water and oil repellent materials may be utilized in
the process of the invention, the use of fluorocarbons is
preferred. Examples of the different types of such materials are
set forth in an article by E. G. Higgins entitled "Finishing for
Water Repellency," Textile Institute and Industry, September 1966,
pages 255-257. Types tested included those set forth on page 3. Two
specific systems of the preferred fluorocarbon treatment are the
Scotchgard treatment, a registered trademark for a finishing
process by Minnesota Mining and Manufacturing Company and a Du Pont
process employing their registered product Zepel. Generally, the
Scotchgard process employs a minor amount of a textile resin, a
fluorocarbon sold under the 3M trademark FC-208 and an extender,
Nalan W, sold by Du Pont.
The proportion of the water repellent compound utilized to treat
the fabric according to the process of the invention is generally
in the same range as that commonly used for imparting water
repellency to fabrics. Advantageously, the fluorocarbon
concentration is at least about 0.1% by weight of the pad bath or
treating solution with the upper limit being dependent upon the
degree of water repellency desired. Amounts greater than about 1%
generally meet the water and oil repellency standards for rainwear
recognized by the industry. When the proportion of the fluorocarbon
is less than about 1%, a significant degree of oil repellency is
still achieved although the water repellency level may be reduced.
Advantageously, between about 0.1% and 5% by weight of the water
repellent shall be present on the textile material on a dry weight
basis and preferably between about 0.1% and 2%.
The term "textile resin" according to the present invention
includes both monomers and polymers which when applied to a textile
material and reacted under proper conditions undergo polymerization
and/or condensation and are transformed to the thermoset state.
Textile resins that may be employed when practicing the present
invention include epoxy, acetal, aminoplast resins, etc., with the
aminoplast resins being preferred. These nitrogen containing resins
when applied to a textile material in the presence of a catalyst at
temperatures of from 100.degree. C. to about 300.degree. C. are
transformed into the thermoset state. The aminoplast resin
condenses with the cellulose molecules and when vinyl groups are
present in the aminoplast resin, it undergoes addition
polymerization with itself and also with the cellulose molecule if
irradiated. The cured textile resin on the textile material affords
the textile material a durable press and/or wrinkle resistant
characteristic.
Exemplary of the aminoplast resins that may be employed according
to the present invention are the urea formaldehydes, e.g.,
propylene urea formaldehyde, dimethylol urea formaldehyde, etc.;
melamine formaldehydes, e.g., tetramethylol melamines,
pentamethylol melamines, etc.; ethylene ureas, e.g., dimethylol
ethylene urea, dihydroxy dimethylol ethylene urea, ethylene urea
formaldehyde, hydroxy ethylene urea formaldehyde, etc., carbamates,
e.g., alkyl carabamate formaldehydes, etc.; formaldehyde-acrolein
condensation products; formaldehyde-acetone condensation products;
alkylol amides, e.g., methylol formamide, methylol acetamide, etc.;
acrylamides, e.g., N-methylol acrylamide, N-methylol
methacrylamide, N-methylol-N-methacrylamide,
N-methyl-methylolacrylamide, N-methylol methylene-bis-(acrylamide),
methylene-bis-(N)-methyl acrylamide), etc.; haloethylene
acrylamide; diureas, e.g., trimethylol acetylene diurea,
tetramethylol-acetylene diurea, etc.; triazones, e.g.,
dimethylol-N-ethyl triazone, N,N'-ethylene-bis-dimethylol triazone,
halotriazones, etc.; haloacetamides, e.g.,
N-methylol-N-methylchloroacetamide, etc.; urons, e.g., dimethylol
uron, dihydroxy dimethylol uron, etc., and the like. Mixtures of
aminoplast textile resins are also with the scope of the present
invention.
Further exemplary of the textile resins within the scope of the
present invention are those which conform to the following
structural formulae. In each of the following formulae the
variables may be selected as follows:
R.sup.1 : hydrogen, lower alkyl or residue of saturated or
unsaturated aldehyde
R.sup.2 : hydrogen, lower alkyl or --CX--CR.sup.3 =CHR.sup.4
R.sup.3 : hydrogen or methyl
R.sup.4 : hydrogen or lower alkyl
R.sup.5 : hydrogen, lower alkyl, or CHR.sup. 1 OR.sup.4, at least
one R.sup.5 being CHR.sup.1 OR.sup.4
R.sup.6 : lower alkyl or hydroxy alkyl
R.sup.7 : hydrogen, hydroxyl or lower alkyl
R.sup.8 : hydrogen, lower alkyl, alkylol or alkenol
X: sulfur or oxygen and where ##EQU1## may have substituted
therefor ##EQU2## or sulfonium if desired. ##EQU3## where a is a
whole integer from 1 to 6 ##EQU4##
The amount of the textile resin employed is primarily determined by
the ultimate use of garments or articles prepared from the fabric.
Very small amounts of the resin will afford some improvement and
large amounts even greater improvements, but the larger amounts of
resin generally adversely affect the hand of the fabric. Hence, the
amount of resin employed is preferably that which will afford good
crease retention and flat dry properties while not adversely
affecting the hand. For the purposes of the present invention, the
amount of textile resin in the pad bath may vary between about 2
and 30% by weight. Resin applied to the fabric should be in the
range of about 2 to 20% based on the dry weight of the fabric and
preferably in the range of about 4 to 9%.
Catalysts employed within the scope of the present invention depend
upon the specific textile resin that is applied to the textile
material. For instance, if the textile resin has a functional group
that is reactive under acidic conditions, then an acid catalyst is
used. Likewise, when a functional group is present that is reactive
under alkaline conditions, then a base catalyst is used.
Furthermore, both acid and base catalysts may be used when both
types of functional groups are present in the textile resin. In
this instance, the catalyst may be added separately or together.
When they are added together, one must be a latent catalyst, i.e.,
one that will not initiate its reaction during the opposite type
reaction, but may be activated subsequently under proper catalytic
conditions.
The catalysts useful in activating the acid or base reactive groups
are those conventionally used to activate the reaction textile
resins containing the same group for reaction with hydroxy groups
of cellulose. Preferably, latent acid or base acting catalysts are
utilized, that is, compounds which are acidic or basic in character
under the curing conditions. The most common acid acting catalysts
are the metal salts, for example, magnesium chloride, zinc nitrate
and zinc fluoroborate and the amino salts, for example,
monoethanolamine hydrochloride and 2-amino-2-methylpropanol
nitrate.
The base acting catalyst preferably is a compound which does not
initiate substantial reaction between the base reactive group and
hydroxy groups of cellulose under normal acid conditions, but does
initiate substantial reaction under prescribed conditions, such as
elevated temperature or some other activating means, as through use
of another chemical compound. For example, an alkali metal sulfite
can be padded onto the fabric and be decomposed into strongly basic
alkali metal hydroxide by including small amounts of formaldehyde
in the steam used for curing.
The latent base acting catalyst utilized herein preferably
comprises alkali-metal salts, such as alkali-metal carbonates like
sodium carbonate, which is neutral to mildly alkaline, for example,
pH of about 8.5 on the fabric but decomposes at temperatures in
excess of about 80.degree. C. to form the stronger base sodium
oxide which will initiate substantial reaction at the elevated
temperatures utilized during curing. Sodium carbonate may be
utilized if desired since the pH in the fabric produced by this
compound in normal conditions is generally insufficient to initiate
the desired degree of reaction under the normal temperature
conditions.
If fabrics containing a base reactive group are maintained at pH
levels above about 10, however, degradation occurs, so that
essentially neutral or mildly alkaline catalysts are preferred when
base reactive compounds are utilized.
Additional base acting catalysts include potassium bicarbonate,
potassium carbonate, sodium silicate, alkali metal phosphates, such
as sodium or potassium phosphates, barium carbonate quaternary
ammonium hydroxides and carbonates, for example, lauryl trimethyl
ammonium hydroxides and carbonates and the like.
The amount of catalyst to be utilized is that conventionally used
in activating the reaction between textile resins and hydroxy
groups of cellulose, for example, up to about 15% by weight of an
acid acting catalyst in the application bath with the preferred
range being from about 1% to about 7%. A preferred range for the
base acting catalyst is again the conventional amount and is
generally between about 0.2% to about 16%, preferably about 2 to
16%. The amount of catalyst to be utilized will further depend in
part on the temperature at which the reaction is conducted and the
amount of catalyst consumed in the reaction. For example, when base
catalysts are utilized and if a highly acidic group is released
during the reaction, the amount of base applied to the textile
material should be at least sufficient to provide an excess of base
in addition to that which is consumed by the highly acidic
group.
The term "soil release" in accordance with the present invention
refers to the ability of the fabric to be washed or otherwise
treated to remove soil and/or oily materials that have come into
contact with said material. The present invention does not per se
prevent the attachment of soil or oily materials to the fabric, but
hinders such attachment and renders the heretofore uncleanable
fabric now susceptible to a successful cleaning operation. While
the theory is still somewhat of a mystery, soiled, treated fabric
when immersed in the detergent containing wash water experiences an
agglomeration of the oil at the fabric surface. This water is basic
in nature and it has been determined that soil release is best
realized in wash water that is basic in nature. These globules of
oil are then removed from the fabric and rise to the surface of the
wash water. This phenomenon takes place in the home washer during
continued agitation, but the same effect has been observed even
under static conditions. In other words, a strip of
polyester/cotton fabric treated according to the process of the
present invention and soiled with crude oil, when simply immersed
in a detergent solution will lose the oil without agitation. The
oil just balls up on the fabric, dislodges therefrom, and rises to
the surface of the solution.
An added feature of the present invention is the prevention of soil
redeposition from the wash water. One of the greatest disadvantages
of the synthetic polymers is the feature that even after removing
the soil by washing, there is the continued danger that the soil
will be redeposited onto the fibers from the wash water before the
garment is removed therefrom. It has been observed that the soil
releasability of the presently treated fabric diminishes after
repeated washings. Even after the ability to remove soil from the
fabric has diminished, however, the observation has been made that
the prevention of redeposition of soil from the wash water remains
potent. This phenomenon likewise is unexplainable, but it has been
established that the troublesome soil is negatively charged and
presumably there remains enough acid on the fabric to repel the
negatively charged soil.
Some of the textile materials that may be treated according to the
process of the present invention may not be feasily removed from
their environment and washed in a washing machine, e.g., upholstery
fabrics. Further, there are also materials that may be treated
which when subjected to the action of a washing machine are
adversely affected either in structure or in looks. Articles within
these classes may still be easily cleaned in place or otherwise by
scrubbing the soiled area lightly with a solution of a commercial
detergent and water.
The soil release polymer of the present invention may be selected
from a large number of different compounds, for example, acid
polymers, low molecular weight polyesters, etc. The polymer
employed advantageously is capable of forming a film around the
fibers that constitute the textile material. Softness of the film
is desirable for if the film is too hard, the hand of the textile
material may be adversely affected. Further the film preferably has
hydrophilic properties and is at least partially insoluble in
water. The film, if water soluble, would, of course, be easily
washed from the fabric. The polymer from which the film is formed
may, however, be water soluble if applied with a textile resin, for
during the curing process, the polymer if water soluble, is
transformed to a water insoluble film. Furthermore, when the
polymer is applied to a substrate without a textile resin, it may
likewise be water soluble if the substrate is such that the soil
removal is only required once. An acid content of at least 10
weight percent acid calculated as acrylic acid in the soil release
polymer from which the film is formed is desirable, and preferably
at least 20 weight percent. It has further been observed that acid
polymers that afford soil release have a carbon atom to acid group
ratio in the repeat group in the range of 2:1 to 30:1, and that an
air dried film cast therefrom has a water of imbibition of at least
89%.
Synthetically produced acid polymers within the scope of the
present invention may be prepared from any of the polymerizable
organic acids, i.e., those having reactive points of unsaturation,
e.g., one of the acrylic acids. These polymers may be homopolymers
of the acids, or interpolymers of an acid and other monomers
copolymerizable therewith so long as at least 10 weight percent
acid monomer is present in the polymer. Exemplary of polymerizable
acids that may be used, are acrylic acid, methacrylic acid, maleic
acid, fumaric acid, itaconic acid, crotonic acid, cinnamic acid,
polymerizable sulfonic acids, polymerizable phosphoric acids, etc.
Monomers that may be interpolymerized with the acids include any
monomers capable of copolymerizing with the acids and which will
not detrimentally affect the film-forming properties of the
polymer. Suitable monomers include, esters of the above acids
prepared by reacting the particular acid with an alkyl alcohol,
e.g., acrylic esters such as ethyl acrylate, methyl acrylate,
propyl acrylate, isopropyl acrylate, methyl methacrylate, ethyl
methacrylate, 2-ethylhexyl acrylate, butyl acrylate, etc.; alkyl
fumarates, maleates, crotonates, cinnamates, etc.; vinyl halides;
monomers having vinylidene groups; e.g., styrene, acrylonitrile,
methylstyrene; substituted vinyl monomers, e.g., chlorostyrene;
butadiene, etc. In all of the polymers prepared from the above
listed monomers, there must be at least 10 weight percent acid
calculated as acrylic acid. It should be noted that various
mixtures of the above polymers will work according to the process
of the present invention and hence should be considered within the
scope of the present invention. Furthermore, salts of the acid
polymers, e.g., sodium, potassium, lithium, ammonium, etc., will
afford the desired soil release characteristics.
Examples of some of the synthetic acid polymers that may be used
according to the present invention are polymerization products
of:
ethyl acrylate:acrylic acid
ethyl acrylate:acrylic acid:acrylamide
butyl acrylate:acrylic acid
ethyl acrylate:methacrylic acid
ethyl acrylate:itaconic acid
methyl methacrylate:acrylic acid
2-ethyl hexyl acrylate:acrylic acid
acrylamide:acrylic acid
butyl acrylate:acrylic acid:acrylamide
ethyl acrylate:acrylic acid:N-methylol acrylamide
ethyl acrylate:acrylic acid:styrene
ethyl acrylate:acrylic acid:hydroxy propyl methacrylate
ethyl acrylate:acrylic acid:divinyl benzene
ethyl lacrylate:acrylic acid:allyl acrylamide
ethyl acrylate:acrylic acid: glycidyl acrylate
ethyl acrylate: itaconic acid
ethyl acrylate:sodium styrene sulfonate
ethyl acrylate:crotonic acid
styrene:acrylic acid
ethyl acrylate:acrylic acid:hydroxy ethyl methacrylate
hydroxy ethyl:acrylic:hydroxy ethyl methacrylate
hydroxy ethyl methacrylate:acrylic acid:acrylamide
butyl acrylate:ethyl acrylate:acrylic acid
and the like.
Some acid polymers work better than others, however, and these are
preferred. Examples of the preferred acid polymers include (1)
copolymers of an acrylic ester such as ethyl acrylate and an
acrylic acid that are prepared by polymerizing a co-monomer mixture
of from about 10 to 80 parts of the acrylate and about 20 to 90
parts of the acrylic acid and advantageously from about 50 to 80
parts of the acrylate and 20 to 50 parts of the acrylic acid; (2)
copolymers of propyl or isopropyl acrylate and acrylic acid wherein
the copolymers are prepared by polymerizing a monomer mixture of
from about 40 to 57 parts propyl or isopropyl acrylate and about 43
to 60 parts of acrylic acid; (3) copolymers of butyl acrylate and
acrylic acid prepared by polymerizing a co-monomer mixture of from
about 30 to 70 parts butyl acrylate and about 70 to 30 parts of
acrylic acid; (4) copolymers of 2-ethyl-hexyl-acrylate and acrylic
acid prepared by polymerizing a co-monomer mixture of from about 10
to 40 parts of 2-ethyl hexyl acrylate and about 60 to 90 parts of
acrylic acid; (5) copolymers substantially identical to the ones
listed above with the exception that methacrylic acid is
substituted for acrylic acid and the esters are methacrylates
instead of acrylates; (6) a copolymer of ethyl acrylate and
itaconic acid prepared by polymerizing a monomer mixture comprising
about 70 parts ethyl acrylate and about 30 parts itaconic acid; (7)
copolymers of the acrylic acid set forth above wherein the
acrylates are replaced by methacrylates; (8) a copolymer of
acrylamide and acrylic acid prepared by polymerizing a monomer
mixture comprising about 10 parts acrylamide and about 90 parts
acrylic acid; and (9) terpolymers comprising ethylacrylate, acrylic
acid and acrylamide prepared from monomer mixtures of ethyl
acrylate, at least 10 parts acrylic acid and up to 20 parts
acrylamide. One commercial polymer that has performed very
satisfactorily and therefore is among the preferred acid polymers
is Acrysol ASE-75, an acrylic emulsion polymer sold by Rohm &
Haas, Philadelphia, Pa. .Iadd.which absorbs about seven times its
weight of water when immersed in an aqueous detergent solution for
2 minutes at 140.degree. F. .Iaddend.
The acid polymers suitable for use in practicing the present
invention form a hydrophilic film upon drying and afford soil
release ability at that point. For unknown reasons, further
treatments and/or ingredients will enhance the soil release ability
of the substrate. If the substrate having the acid polymer thereon
is subjected to textile resin curing conditions, the durability of
the soil release ability is enhanced. Likewise the presence of a
textile resin catalyst during the textile resin curing conditions
further improves soil release ability. Still further, the soil
release finish is much more lasting on a substrate when the acid
polymer is subjected to textile resin curing conditions in the
presence of an aminoplast textile resin. It is known that the film
covers the hydrophobic synthetic fiber contents of the textile
material without any reaction therewith. What is not understood,
however, is the durability of the soil release characteristic.
While it is known that there is some reaction between the acid
polymer and the textile resin, the reaction mechanism is very
speculative. Furthermore, there may be some crosslinking between
the cellulose molecules and the acid polymer or there may be just
an enhanced physical bond between the textile resin and the acid
polymer above and beyond their reactivity.
Soil release polymers, like the textile resins, give some
improvement at very low levels on the fabric. Accordingly, as the
amount of soil release polymer is increased, the ability of the
fabric to release soil increases. Thus, the upper limit on the
amount of soil release polymer is determined by economics and
resulting adverse effects on the fabric, e.g., the hand of the
fabric. Furthermore, practically speaking there is a set range of
soil release polymer dictated by commercial success.
The acid polymers, as a general rule, are emulsion polymers
containing varying amounts of solids, normally in the range of
about 25 to 50 weight percent. The polymer emulsion should be
present in the pad bath or other application medium in the range of
about 2.5 to 40 weight percent. Otherwise stated, there should be
from about 0.25 to 5 weight percent of acid polymer solids applied
to the substrate, based on dry weight, and preferably 1.0 to 1.5
weight percent.
The composition used to impregnate the textile material according
to the present invention is not limited to including only the
possible ingredients heretofore mentioned, e.g., textile resin,
textile resin catalyst, soil release polymer and water repellent
compound. In addition, other ingredients may be employed such as,
for example, emulsifying agents, wetting agents, softeners, etc.,
and numerous other compounds that enhance the physical
characteristics of the fabric. The composition may be applied to
the substrate in any suitable manner. For instance, padding of the
solution onto fabric is preferred because of ease of operation at
that particular stage of the development. The composition may be
sprayed on as a liquid; the substrate may be treated with vapors of
the compounds if convenient; the substrate may be dipped, etc.
In general, the applicator system is adjusted to provide from 30 to
100 weight percent wet pickup by the fabric from the pad bath.
Preferably, however, it has been determined that best results are
obtained by providing a wet pickup of from 40 to 60 weight percent
from the pad bath.
When the aminoplast textile resin is applied to the substrate,
e.g., textile materials, along with the soil release polymer and a
fluorocarbon water repellent compound, they may be simultaneously
applied from the same pad bath. Simultaneous application is not
required though and beneficial results may be realized by first
applying the soil release polymer followed by separate applications
of the textile resin and the water repellent compound and curing of
the textile resin. Insofar as separate application is concerned,
however, where the textile resin is applied first and cured and the
soil release polymer and the water repellent compound are added
separately thereafter, initial soil release ability is outstanding,
but not nearly so durable as the simultaneous application or the
separate addition where textile resin, soil release polymer and
water repellent all are present during curing of the textile
resin.
According to the desires of the individual, and the dictates of the
ultimate product, separate or simultaneous application of the
textile resin, the soil release polymer and the water repellent may
be employed. For instance, when treating a textile fabric which is
to be converted into work clothes, it would be desirable to have as
durable a finish as possible so that the soil release properties
will be as long lasting as possible. In this situation, either a
simultaneous addition or a separate addition where the soil release
polymer is added first would be desired. On the other hand, where
the ultimate article of manufacture is not one that will be washed
or cleaned on a weekly basis, for instance, the desirable property
might possibly be to have a very superior initial soil release
property. An example would be upholstery for automobiles, seat
covers, wall coverings, etc. For these items it may be more
desirable to first apply the textile resin and separately after
curing of the textile resin apply the soil release polymer and the
water repellent, or just apply the soil release polymer, and the
water repellent, etc., as described herein, if a textile resin is
not desired. It must be emphasized, however, that under such
conditions the water repellent and soil release properties are less
durable than those attained by the aforesaid simultaneous means of
application.
Advantages afforded by the process of the present invention are
available for textile materials treated in almost any form, e.g.,
fibers, yarns, threads, fabrics or the ultimate product, e.g., a
garment, etc.
Garments made from the fabrics treated according to the process of
the present invention require no additional steps than normal for
the preparation of the conventional durable press garments. In
other words, the garment may be folded and pressed on conventional
equipment, for example, a Hoffman press. The pressing cycle
utilized is standard in the industry and generally involves
pressing of the garment for a short period of time, followed by a
curing operation in an oven. Alternatively, the garment may be set
in a desired configuration under hot, dry conditions, such as by
hot pressing without steaming, for example, at temperatures of up
to about 300.degree. C. for as long as necessary to cure the
resin.
In general, the textile resin may be selected from several general
types. According to the type resin selected, one of the following
processes may be generally followed to achieve the novel garments
produced by the present invention. In each type procedure, the
methods of application and order of application of textile resin,
soil release polymer, catalysts, water repellent, etc., may be
varied as described supra.
Type I
(1) Apply textile resin having one type functional group, textile
resin catalyst, soil release polymer and water repellent to
fabric.
(2) Dry fabric at temperature that is insufficient to initiate
catalysis of the textile resin.
(3) Make garment from fabric.
(4) Press garment to produce creases where desired.
(5) Subject garment to temperature sufficient to catalyze and cure
the textile resin.
Type II
(1) Apply textile resin having more than one type of functional
group, textile resin catalysts for each type functional group, soil
release polymer and water repellent to fabric.
(2) Subject fabric to conditions whereby one type of functional
group reacts and remaining functional groups remain dormant.
(3) Prepare garment from the fabric.
(4) Press creases where desired in garment.
(5) Subject garment to conditions whereby the remaining functional
groups are reacted with the cellulose.
Type III
(1) Apply textile resin having more than one type of functional
group, one type being sites of ethylenic unsaturation, a textile
resin catalyst, a soil release polymer and water repellent to the
fabric.
(2) Dry the fabric at temperatures such that the textile resin
catalyst remains dormant.
(3) Subject the fabric to irradiation.
(4) Make a garment from the fabric.
(5) Produce desired creases in the garment.
(6) Subject the garment to textile resin curing conditions.
In each of the above types of procedures, the ultimate curing of
the textile resin may be accomplished prior to the manufacture of
the garment whereby a good wash-and-wear fabric having water and
oil repellency and soil release properties is produced.
Procedures of Types I, II and III, as is evident, relate to the
process of the present invention being applied to a textile
material to afford said textile material water and oil repellency,
soil release and durable press or wash and wear characteristics.
Otherwise than above shown, the various materials are applied and
dried, subjected to textile resin curing conditions, etc.,
according to the specifications described herein.
The drying temperatures that are insufficient to initiate the
catalysis are, of course, dependent upon the particular catalyst
being employed. In general, however, the drying step is conducted
at a rate of approximately 10 to 70 yards per minute at
temperatures ranging from about 225 to 300.degree. F. preferably in
a tenter frame. The drying temperature range overlaps to some
degree with the curing temperature range set forth below. When
drying in the overlapping portion of the drying and curing ranges,
it is important that there be no premature curing of the textile
resin. Time is the prime variable and when drying the substrate in
the higher end of the drying temperature range, care must be taken
to avoid heating the substrate for a time sufficient to initiate
catalysis that would at least partially cure the textile resin.
Irradiation techniques may be employed according to the process of
the present invention when a textile resin having ethylenic
unsaturation is applied to the textile material. An insulating core
transformer, operated at a potential varying between one hundered
thousand electron volts and five hundred thousand electron volts
may be successfully used to irradiate the textile material. Such a
transformer is commercially available from High Voltage Engineering
Corporation, Burlington, Mass. The amount of ionizing irradiation
necessary according to the present invention is at least 32
electron volts for each ion pair formed. Thus irradiation of 32
volts and above is effective. Both high energy particle and
ionizing irradiation are useful according to the present invention.
The preferred dosage of irradiation according to the present
invention is in the range of one thousand rads to one hundred
megarads, a rad being the amount of high energy irradiation of the
type which results in energy absorption of one hundred ergs per
gram of absorbing material. More preferably, however, the
irradiation dosage ranges from 0.5 to 5 megarads.
Curing of the textile resin is accomplished by subjecting the
textile material having the textile resin thereon to conditions
such that the catalyst initiates a crosslinking reaction between
functional groups of the resin and hydroxyl groups of the cellulose
in the textile material and converts the resin to the thermoset
state. When a 100 percent synthetic fabric is treated, the resin
adheres to the material and is converted to a thermoset state.
Temperature is the prime mover and generally a temperature in the
range of 100.degree. C. to about 300.degree. C. is sufficient. The
curing medium that supports the necessary temperature may be any
substance that is inert to both the fabric and the ingredients
applied thereto, e.g., hot air, steam, etc. In the instance where
the textile resin possesses two different types of functional
groups, there are actually two curing steps, the first being
conducted at a temperature lower than the second and insufficient
to initiate the second type of catalysis, e.g., a first partial
curing step to initiate alkaline catalysis and a subsequent curing
step to initiate acid catalysis and also convert the resin to the
thermoset state.
The duration of the various processing steps varies diversely with
the particular ingredients employed. In each situation, however,
the treatment time is that necessary to sufficiently cause reaction
of and/or curing of the textile resin, and preferably, between
about 0.1 and 30 minutes.
The following examples illustrate preferred embodiments of the
present invention but are not intended to restrict the scope of the
invention. In the examples, parts and percentages are by weight.
The fabrics prepared in accordance with the procedures set forth in
the examples are tested according to the following procedures. The
oil repellency test results as set forth in Tables I and II are
determined according to the procedure set forth in du Pont
Industrial Chemicals Information Bulletin 5C463Rev965. The oil
repellency test results in Tables III, IV and V are determined
according to the procedure of the 3M Company as set forth in
Appendix B of a brochure entitled "Textile Chemicals," dated Jan.
2, 1962, under the section "Test Methods--A. Oil Repellency." All
water repellency values are based on the AATCC Standard Test Method
22- 1952. All soil release values are determined by comparison to a
set of standards having numerical ratings from 1.0 to 5.0, with 1.0
representing very poor stain removal and 5.0 being virtually
complete removal of the stain. The fabrics are stained with mineral
oil. After staining the fabric is washed one time in a Kenmore
automatic washer using one cup of Tide detergent (sold by Procter
and Gamble) and a wash water temperature at about 140.degree. F.
The fabric is dried for approximately 40 minutes at a temperature
of about 160.degree. F. The stains in the dried fabric are compared
with the set of standards. The values listed in the tables under
the headings 5 and 10 washes represent staining after 5 or 10
normal washings and then a single wash to remove the stain.
Example I.--A pad bath solution is prepared by dispersing in water
24% dihydroxy dimethylol ethylene urea (50% aqueous solution); 4.3%
zinc nitrate (50% aqueous solution of (Zn(NO.sub.3).sub.2.sup..
6H.sub.2 O); 10% emulsion copolymer comprising 70% ethyl acrylate
and 30% acrylic acid; 6% FC-208 (a fluorochemical resin
emulsion-water repellent sold by 3M Co.), 6% Nalan W (a cationic
modified resin water repellent sold by du Pont) and 2.3%
ethoxylated alkyl phenol. The above composition is padded onto
samples of Dacron/cotton (65/35) fabric to provide about 50% wet
pickup. The fabric is then dried on a tenter frame at a speed of
about 13 yards per minute and a temperature of about
250.degree.-280.degree. F. until the moisture content of the fabric
is reduced to approximately 5%.
Several pairs of men's slacks are then prepared from the treated
fabric and pressed on a Hoffman press in the conventional manner
and then pressed on a hot-head press, at a cycle of 5 seconds
steam, 10 seconds bake and 5 seconds vacuum. The pressed slacks are
then suspended from a continuously moving conveyor in an oven and
cured for about 15 minutes at 305.degree. F.
The slacks are tested to determine their soil release, oil
repellency and water repellency both initially and after laundering
a number of times. Even after the testing procedures, the pressed
slacks retain creases satisfactorily. The results of the tests are
reported in Table I.
Example II.--The procedure of this example is the same as that of
Example I except that the 10% copolymer emulsion of 70% ethyl
acrylate and 30% acrylic acid is omitted from the pad bath
solution. Slacks tested show the results set forth in Table I.
Example III.--The procedure of this example is the same as that of
Example I except that the 6% FC-208 and 6% Nalan W are omitted from
the pad bath solution. Test results are set forth in Table I.
TABLE I ______________________________________ Example I II III
______________________________________ As received: Oil repellency
6 5 0 Water repellency 93 100 0 After 1 wash: Soil release 4.5 1.3
4.3 Oil repellency 6 5 0 Water repellency 70 100 0 After 5 washes:
Soil release 3.5 1.0 2.8 Oil repellency 6 6 1 Water repellency 50
100 0 After 10 washes: Soil release 3.2 1.1 2.8 Oil repellency 4 6
1 Water repellency 50 92 0
______________________________________
Example IV.--The procedure of this example is the same as Example I
except that the dihydroxy dimethylol ethylene urea is replaced with
18% N-methylol acrylamide (50% aqueous solution). Also, the dried
fabric is subjected to irradiation in an insulated core transformer
manufactured by the High Voltage Engineering Corporation of
Burlington, Mass. The fabric is passed through the irradiation
equipment at a speed of about 40 yards per minute with a setting on
the transformer of about 500 kilovolts and 15 milliamps, the fabric
being arranged in a 5 pass festoon during irradiation to produce a
dosage of about 2 megarads. The results of tests are reported in
Table II.
Example V.--The procedure of this example is the same as Example IV
except that the 10% copolymer emulsion of 70% ethyl acrylate and
30% acrylic acid is omitted from the pad bath solution. Slacks
tested show the results as set forth in Table II.
Example VI.--The procedure of this example is the same as Example V
except that the 6% FC-208 and Nalan W are omitted from the pad bath
solution. Slacks tested show the results set forth in Table II.
TABLE II ______________________________________ Example IV V VI
______________________________________ As received: Oil repellency
7 5 0 Water repellency 100 100 0 After 1 wash: Soil release 3.9 1.3
3.9 Oil repellency 6 6 0 Water repellency 70 100 0 After 5 washes:
Soil release 2.9 1.4 2.4 Oil repellency 6 6 1 Water repellency 50
100 0 After 10 washes: Soil release 2.1 1.5 2.2 Oil repellency 4 6
1 Water repellency 50 93 0
______________________________________
Example VII.--The procedure of this example is the same as that of
Example I except that the proportion of FC-208 is 0.5% and the
proportion of the ethyl acrylate-acrylic acid copolymer is 8%. The
test results are reported in Table III.
Example VIII.--The procedure of this example is the same as that of
Example I except that the proportion of the FC-208 is 0.25%, the
proportion of the ethyl acrylate-acrylic acid copolymer is 8% and
the curing temperature is 340.degree. F. The results of testing are
reported in Table III.
Example IX.--The procedure of this example is the same as that of
Example I except that the proportion of the FC-208 is 0.5%, the
proportion of the ethyl acrylate-acrylic acid copolymer is 6% and
the curing temperature is 340.degree. F. The test results are
reported in Table III.
TABLE III ______________________________________ As received, Soil
release, oil repellency after 1 wash
______________________________________ Example: VII 90 3.8 VIII 70
3.0 IX 70 3.6 ______________________________________
While the oil repellency of the fabrics prepared in Examples VII,
VIII and IX is significantly reduced in laundering due to the same
amount of FC-208 employed, the fabrics do have a high level initial
oil repellency and good soil release and thus would be useful in
applications where laundering is infrequent, for example,
upholstery fabrics.
Example X.--The procedure of this example is the same as that of
Example I except that the proportion of the FC-208 is 6%, the
proportion of the ethyl acrylate-acrylic acid copolymer is 2% and
the curing temperature is about 325.degree. F. The test results are
reported in Table IV.
TABLE IV ______________________________________ As received: Oil
repellency 120 Water repellency 100 After 1 wash: Soil release 4.0
Oil repellency 120 Water repellency 100 After 5 washes: Soil
release 3.0 Oil repellency 100 Water repellency 50
______________________________________
Example XI--The procedure of this example is the same as that of
Example I except that 4.3% magnesium chloride (MgCl.sub.2.sup..
6H.sub.2 O) is substituted for the zinc nitrate. Results similar to
those of Example I are achieved.
Example XII.--The procedure of this example is the same as that of
Example I except that the acrylic acid-ethyl acrylate copolymer is
replaced with each of the following copolymers with results similar
to those of Example I:
Butyl acrylate:acrylic acid (12:88)
Butyl acrylate:acrylic acid (30:70)
Butyl acrylate:acrylic acid (80:20)
Butyl acrylate:acrylic acid (88:12)
Ethyl acrylate:methacrylic acid (70:30)
Ethyl acrylate:itaconic acid (70:30)
Methyl methacrylate:acrylic acid (70:30)
Acrylamide:acrylic acid (10:90)
Ethyl acrylate:acrylic acid:acrylamide (50:38:12)
Ethyl acrylate:acrylic acid:acrylamide (65:3: 5)
Example XIII.--The procedure of this example is the same as that of
Example I except that the dihydroxy dimethylol ethylene urea, the
copolymer of ethyl acrylate and acrylic acid and the Nalan W are
omitted from the pad bath solution. Instead, the ethyl
acrylate-acrylic acid copolymer is applied to the fabric and the
fabric is dried prior to the application of the pad bath solution.
The test results are reported in Table V.
Example XIV.--The procedure of this example is the same as that of
Example XIII except that the ethoxylated alkyl phenol is omitted
from the pad bath solution. The results of testing the fabrics are
reported in Table V.
Example XV.--The procedure of this example is the same as that of
Example XIII except that the zinc nitrate and the ethoxylated alkyl
phenol are omitted from the pad bath solution. The results of
testing the fabrics are reported in Table V.
TABLE V ______________________________________ Example XIII XIV XV
______________________________________ As received: Oil repellency
120 120 120 Water repellency 90 100 100 After 1 wash: Soil release
3.8 3.0 2.8 Oil repellency 110 50 90 Water repellency 50 50 50
After 3 washes: Soil release 3.0 2.0 2.0 Oil repellency 50 0 80
Water repellency 50 50 0 ______________________________________
Example XVI.--The procedure of the above examples is repeated
utilizing other fabrics including fabrics containing viscose rayon.
Orlon, Acrilan, acetate, polypropylene, etc., fibers with similar
improvements in oil and water repellency and soil release
characteristics.
While the durability of the oil and water repellency achieved
through the process of the present invention, in some cases, may be
somewhat below industry standards for rainwear, after repeated
laundering, the level of oil and water repellency which is retained
provides benefits and advantages in many non-rainwear applications.
For example, tablecloths or wearing apparel such as shirts or
slacks exhibit improved performance so that materials such as food
or drinks which are accidentally spilled thereon can be wiped from
the surface of the fabric without excessive amounts soaking into
the fabric. Furthermore, the balance can be removed in subsequent
laundering.
The above description and examples show that the present invention
provides novel textile materials having the heretofore unattainable
combination of oil and water repellency and soil release
characteristics. Furthermore, this combination of characteristics
can be achieved with fabrics including synthetic polymeric fibers.
As a result, the fabrics and garments of the invention can be
laundered to remove stains without destroying the water and oil
repellency characteristics. In addition, through the process of the
invention, it is possible to achieve water and oil repellency and
soil release in fabrics having durable press and/or wash and wear
characteristics.
* * * * *