Note: Descriptions are shown in the official language in which they were submitted.
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DURABLE PRESSNVRINKLE-FREE PROCESS
CROSS REFERENCE TO RELATED APPLICATION
This application claims benefit under 35 USC 119(e) of prior pending
application 60/046,298 filed May 13, 1997.
BACKGROUND OF THE INVENTION
Field of invention
This invention relates to a durable press/wrinkle-free process for
cellulosic fiber-containing fabrics and more particularly to a process which
permits high treatment level amounts of formaldehyde and catalysts to impart
wrinkle resistance to the cellulosic fiber-containing fabrics while reducing
the
loss in both tensile and tear strength normally associated with such treatment
processes.
Description of related art
There are a number of known process for treating cellulosic fiber-
containing fabrics, such as cotton-containing fabrics, to make them wrinkle-
free. These treatment processes include resin or polymer treatment of the
fabric, but these are costly and unsatisfactory. Another process for treating
cellulosic fiber-containing products relies on formaldehyde to provide durable
crosslinking of the cellulose molecules and to thereby impart durable crease
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resistant and smooth drying characteristics to these products. However,
problems have been encountered with the known processes. A simple,
reproducible, completely satisfactory low-cost formaldehyde durable press
process has not yet been achieved.
It has long been known to treat celluiosic materials with formaldehyde,
as is evidenced by U.S. Patent Number 2,243,765. This patent describes a
process for treating cellulose with an aqueous solution of formaldehyde
containing a small proportion of an acid catalyst under such conditions of
time and temperature that the reaction is allowed to approach its equilibrium.
It is further stated that, in carrying out this process, the proportion of the
solution of formaldehyde to the cellulose must be at least such that the
.cellulose is always in a fully swollen state. It is also stated that the time
and
temperature of the treatment with the solution of formaldehyde and acid
catalyst will vary with one another, the time required increasing rapidly as
the
temperature diminishes. When it is desired, the product may be isolated by
washing and drying; preferably at a temperature of about 212°F. The
products obtained according to this process are said to show no increase in
wet strength and possess a high water imbibition, an increased resistance to
creasing and a slight increase in affinity to some direct dyes.
In recent years additional methods have been devised for treating
cellulosic fiber-containing products in order to impart durable crease
retention, wrinkle resistance and smooth drying characteristics to these
products. As discussed, formaldehyde has been crosslinked with cellulose
materials to produce these products. It is also known to treat cellulose
.materials with resins or precondensates of the urea-formaldehyde or
substituted urea-formaldehyde type to produce a resin treated durable press
product. As noted in U.S. patent Number 3,841,832, while formaldehyde has
made a sign~cant contribution to the cotton finishing art, the result has been
far from pertect. For instance, in some cases the formaldehyde crosslinking
treatment has tended to lack reproducibility, since control of the
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formaldehyde cross-linking reaction has been difficult. As noted in United
States patent 4, 396,390, lack of reproducibility is especially true on a
commercial scale.
Moreover, unacceptable loss of fabric strength has also been
observed in many of the proposed aqueous formaldehyde treatment
processes. When high curing temperatures were used with an acid or
potential acid catalyst, excess reaction and degradation of the cotton often
happened which considerably impaired its strength. On the other hand,
when attempts were made to achieve reproducibility at temperatures of
106°F or less, much longer reaction or finishing times were usually
required,
rendering the process economically relatively unattractive. A solution to this
is set forth in United States Patent 4,108,598, the entire disclosure of which
is herein incorporated by reference.
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SUMMARY OF THE INVENTION
In accordance with the present invention it is possible to obtain good
durable press properties in a cellulosic fiber-containing fabric with good
strength retention with a process that produces consistent results. This
invention relates to a durable press/wrinkle-free process for cetlulosic fiber-
containing fabrics and more particularly to a process which utilizes
formaldehyde and catalysts with silicone elastomers to impart wrinkle
.resistance to the cellulosic fiber-containing fabrics while reducing loss in
both
tensile and tear strength. This process is particularly effective on 100%
cotton fabric.
DESCRIPTION OF PREFERRED EMBODIMENTS
Such cellulosic fiber-containing fabrics include cloth made of cotton or
cotton blends. There is a constant consumer demand for better treatment,
that is, a more wrinkle-free product and for higher amounts of cotton in the
blended fabric, or preferably, a 100% cotton fabric. There is a great demand
for a wrinkle-free fabric made entirely of cotton and having good tensile and
tear strength. This has been achieved and 100% cotton fabrics are treated
today, but only in heavier weight pants or bottom weight fabrics.
Unfortunately, the more wrinkle-free the cellulosic containing fabric is made
by treatment in a formaldehyde system, the greater the loss in tear and
tensile strength.
That is, as the amount of chemicals used in the treating process are
increased to obtain an acceptable wrinkle resistance in the treated fabric,
the
loss in tear and tensile strength fall to unacceptable levels. Polyester
fibers
are most often blended into the cotton to form a polyester cotton blend fabric
to compensate for the loss in strength of the treated cotton. Polyester in
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amounts of up to 65% are commonly used. Because of the presence of
polyester fibers or other synthetic fibers in the blend, these blended fabrics
are sufficiently strong but do not have the comfort or feel of fabrics
containing
a higher amount of cotton, or most desirably, 100% cotton. The process of
the present invention overcomes the disadvantages of the prior art processes
and permits the presence of higher percentages of cotton in the blend and
even the treatment of lighter weight or shirting weight 100% cotton fabrics to
a commercially acceptable wrinkle free standard while retaining adequate
strength in the fabric to also make it commercially acceptable. Commercial
acceptability of the treated fabric is the ultimate goal of the process.
The durable press process of the present invention for treating cotton
containing fabrics and 100% cotton fabric, comprises treating a cellulosic
fiber-containing fabric with aqueous formaldehyde and a catalyst capable of
catalyzing the crosslinking reaction between formaldehyde and cellulose in
the presence of a silicone elastomer, heat curing the treated cellulosic fiber-
containing fabric, preferably having a moisture content of more than 20% by
weight, under conditions at which formaldehyde reacts with the cellulose in
the presence of a catalyst and without the substantial loss of formaldehyde
before the reaction of formaldehyde with cellulose to improve the wrinkle
resistance of the fabric while reducing the loss in both tensile and tear
strength. It is preferable that the cellulose containing fabric is in the
fully
swollen state.
Any silicone eslastomer may be used in the present invention.
Silicone elastomers are known materials. Silicone elastomers have a
backbone made of silicon and oxygen with organic substituents attached to
silicon atoms comprising n repeating units of the general formula:
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The groups R and R' may be the same or different and includes for
example, lower alkyl, such as methyl, ethyl, propyl, phenyl or any of these
groups substituted by hydroxy groups, fluoride atoms or amino groups; in
other words, reactive groups to cellulose.
The silicones used to make the silicone elastomers in the present
.invention are made by conventional processes which may include the
condensation of hydroxy organosilicon compounds formed by hydrolysis of
organosiiicon halides. The required halide can be prepared by a direct
reaction between a silicon halide and a Grignard reagent . Alternate
methods may be based on the reaction of a silane with unsatutrated
compounds such as ethylene or acetylene. After separation of the reaction
products by distillation, organosilicon halides may be polymerized by
carefully
controlled hydrolysis to provide the silicone polymers useful in the present
invention.
For example, elastomers may be made by polymerization of the purified
tertramer using alkaline catalysts at 212-302 degrees F., the molecular
weight being controled by using a monofunctional silane. Curing
characteristics and properties may be varied over a wide range by replacing
.some methyl groups by -H, -OH, fluoroalkly, alkoxy or vinyl groups and by
2o compounding with fillers as would be appreciated by one of ordinary skill
in
the art.
Silicone elastomers used in the present invention are high weight
materials, generally composed of dimethyl silicone units (monomers) linked
together in a linear chain. These materials usually contain a peroxide type
catalyst which causes a linking between adjacent methyl groups in the form
of methylene bridges. The presence of crosslinking greatly improves the
durability of the silicone elastomer on cellulose by producing larger
molecules.
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It is also possible to produce a reactive silicone elastomer, which is
one where reactive groups capable of reacting with the substrate have been
added to the linear dimethyl silicone polymer. These silicones are capable
of reacting both with cellulose substrates as well as with most protein
fibers,
and are characterized by much greater durability of the silicone polymer on
the substrate, even approaching the life of the substrate.
Therefore silicone elastomers which give off reaction gases or
chemicals indicating chemical reaction with the substrate are much preferred
over non reactive silicone elastomer, but this is not to say that non reactive
silicone elastomers cannot be used in the process. Different elastomers, by
different manufacturers have all shown increases in tensile as well as tear
strength, as shown in Tables I and II included herein. Elastomeric silicone
polymers have been found to increase strength whereas simple emulsified
silicone oils (or lubricants) do not give increases in tensile strength.
The aqueous system containing formaldehyde, an acid catalyst,
silicone elastorner and a wetting agent may be padded on the fabric to be
treated, preferably to insure a moisture content of more than 20% by weight
on the fabric, and then the fabric cured. The padding technique is
conventional to the art and generally comprises running the fabric through
the aqueous solution which is then passed through squeezing rollers to
provide a wet pick-up of about 66%. As is conventional in the art, the
concentration of the reactants in the aqueous solution are adjusted to provide
.the desired amount of reactants on the weight of the fabric (OWF).
It is possible to use unexpected high temperatures which allow the
crosslinking reaction to take place before the loss of formaldehyde is great
enough to affect the process and provide inadequate treatment. In
accordance with this aspect of the invention, the padded fabric may be
immediately plunged into a heating chamber at from about 300 to about
325°F. This is an important commercial aspect of the invention as it
enables
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continuous processing on a commercial scale at speeds of 100-200 yards
per minute. It must be appreciated, that this process is designed for
commercial applications which are demanding in that the process must be
commercially viable.
This may also be accomplished by curing at a low temperature with an
active catalyst. It is also possible to use any combination of techniques
which prevent the substantial loss of formaldehyde during the curing. For
example, a low temperature may be used in combination with an aqueous
formaldehyde solution. It would also be possible to use a pressurized system
wherein the pressure is greater than atmospheric, thereby preventing the
substantial loss of formaldehyde before the formaldehyde crosslinks with the
ceHulosic fiber-containing fabric being treated.
In addition the process of the present invention uses less
formaldehyde than other known processes. Shirting fabrics treated in
accordance with the process of the present invention contain approximately
1000 ppm after treatment before steaming on a shirting fabric as compared
.to 3000 ppm+ by another crosslinking process on a similar shirting fabric.
Tests have shown that continuously running steaming chambers to which the
treated fabric is exposed should effectively remove residual formaldehyde to
concentrations as low as 200 ppm. This is also an important aspect of the
present invention in view of consumers concern about the presence of
formaldehyde in their purchased garments. It is also possible to wash fabrics
either continuously or in batch washers. Both approaches remove essentially
all of the formaldehyde.
It is known to add t~o the fabric a polymeric resinous additive that is
capable of forming soft film. For example, such additives may be a latex or
fine aqueous dispersion of polyethylene, various alkyl acrylate polymers,
acrylonitrile-butadiene copolymers, deacetylated ethylene-vinyl acetate
copolymers, polyurethanes and the like. Such additives are well known to
3o the art and are generally commercially available in concentrated aqueous
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latex form. Such a latex is diluted to provide about 1 to 3% polymer solids
in the aqueous catalyst-containing padding bath before the fabric is treated
therewith. One known softener which was virtually the softener of choice in
the durable press process using resin treatment or formaldehyde crosslinking
was high density polyethylene, Mykon HD. It has been unexpectedly
discovered that the substitution of a silicone elastomer for high density
polyethylene significantly reduces the loss in tear strength of the treated
fabric after washing as well as providing better control of the process as may
be seen from the examples. The importance of good control of the process
is essential to a commercially viable process to provide a consistent product
from run to run which is not adversely affected by variations in atmospheric
pressure, humidity and the like.
As the cellulosic fiber-containing fabric which may be treated by the
present process there can be employed various natural cellulosic fibers and
mixtures thereof, such as cotton and jute, Other fibers which may be used
in blends with one or more of the above-mentioned cellulosic fibers are, for
example, polyamides (e.g., nylons), polyesters, acrylics (e.g.,
polyacrylonitrile), polyolefins, polyvinyl chloride, and polyvinylidene
chloride.
Such blends preferably include at least 35 to 40% by weight, and most
preferably at least 50 to 60% by weight, of cotton or natural cellulose
frbers.
The fabric may be a resinated material but preferably it is unresinated;
.it may be knit, woven, non-woven, or otherwise constructed. After
processing, the formed wrinkle resistant fabric will maintain the desired
configuration substantially for the life of the fabric. In addition, the
fabric will
have an excellent wash appearance even after repeated washings.
This invention is not dependent upon the limited amounts of moisture
to control the crossfinking reaction since the crosslinking reaction is most
efficient in the most highly swollen state of the cellulose fiber. Lesser
amounts of moisture may be used but are less preferred.
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However, the silicone elastomer must be present in a sufficient
amount to reduce the loss of tensile and tear strength in the fabric normally
associated with the treatment of the same fabric in a prior art treatment
process which may include the use of softeners such as Mykon HD. The
formulation and process of the present invention may be adjusted to meet
specific commercial requirements for the treated fabric. For example,
formaldehyde and the catalyst concentration may be increased to provide
better treatment; then the concentration of the softener is also increased to
combat the loss of tear strength caused by the increased amount of catalyst
used in the process. This lends itself to computerized control of the systems
for treating various fabrics and allows variation in the treatment of
different
fabrics, which is another advantage of the process of the present invention.
While silicone oils are known as silicone softeners and have found
some use in fabric treatment, they suffer serious disadvantages in having a
strong tendency to produce non-removable spots. However, the particular
silicone elastomer used in the process of the present invention completely
overcomes these problems.
Blended fabrics to be treated in accordance with the present invention
are immersed in a solution to provide a pick up or on the weight of fabric
(OWF) of about 3 % formaldehyde, 1 % of catalyst, 1 % of the silicone
elastomer. This requires a pickup of about 66% by weight of the aqueous
formulation to achieve the above stated percentage of reactants on the
fabric. However, when treating 100% cotton fabric chemical concentrations
must be increased so that 5% formaldehyde OWF, about 2% catalyst and
about 2% elastomer padded onto the fabric. This is contrary to the prior art
attempts to treat 100% cotton where the concentration of reactants were
decreased because of the loss of strength due to the treatment process. The
curing temperature may be about 300° F. In fact, the padded fabric may
be
plunged into a oven or heating chamber at 300°F.
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The formaldehyde concentration rnay be varied as would be
appreciated by one of ordinary skill in the art. The process inlcudes the use
of formaldehyde in the form of an aqueous solution having a concentration
of 0.5% to 10%, by weight.
The preferred formaldehyde concentration on the fabric is from 1.5% to 7%
based on the weight of the fabric.
The catalyst used in the process includes fluorosilicic acid for mild
reactions and is applicable to blend fabrics. On heavyweight, all-cotton
fabrics, or shirting fabrics, a catalyst such as magnesium chloride spiked
with
citric acid can be used, which is a commercially available catalyst Freecat
No. 9, as is a similar catalyst which contains aluminum/magnesium chloride.
During the crosslinking reaction at the curing stage, moisture is given up
from the fabric as the crosslinking occurs, resulting in a decrease in the
moisture content of the fabric. In fabrics having a moisture content of 20%
or less, this tends to lower the effectiveness of the crosslinking reaction
requiring higher concentrations of formaldehyde. In a preferred aspect of the
present invention, moisture is given up from a high level, that is, greater
than
20%, preferably greater than 30%, e.g., from 60-100% or more, and the
crosslinking is optimized. Moisture, which is so difficult to control, is not
a
problem in the present invention. Of course, water is not allowed to be
present in so much of an excess as to cause the catalyst to migrate on the
fabric.
All results reported in the following examples were obtained by the
foNowing standard methods:
1. Appearance of Fabrics after Repeated Home Launderings:
AATCC Test Method 124-1992
2. Tensile Strength: ASTM :Test Method D-1682-64 (Test 1 C)
3. Tear Strength: ASTM : Test Method D-1424-83 Falling
Pendulum Method
4. Shrinkage: AATCC Test Method 150-1995
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5. Wrinkle Recovery of Fabrics: Recovery Angle Method:
AATCC Test Method 66-1990 which provides the DP value.
In determining the DP value for the fabrics, a visual comparative test
is performed under controlled lighting conditions in which the amount of
wrinkles in the treated fabric is compared with the amount of wrinkles present
on pre-wrinkled plastic replicas. The plastic replicas have various degrees
of wrinkles and range from a value of 1 DP for a very wrinkled fabric to 5.0
DP for a flat wrinkle free fabric. The higher the DP value, the better. For a
commercially acceptable wrinkle free fabric, a DP value of 3.5 is desired but
1 o rarely achieved. As would be appreciated by one of ordinary skill in the
art,
the difference between a DP of 3.50 and 3.25 is significant. At DP 3.50 all
.wrinkles are rounded and disappearing. At DP 3.25 all wrinkles are still
visible and show sharp creases. The goal for commercial acceptance is a
DP of 3.50 with a filling tensile strength 25 pounds and a filling tear
strength
of 24 ounces. Of equal or even greater importance to these properties is that
the process must be consistently reproducible on an industrial scale.
In all of the following examples a non-ionic wetting agent was used as
is conventional to the art. The wetting agent was used in an amount of about
0.1% by weight. The wetting agent used in all of the examples was an alkyl
aryl polyether alcohol such as Triton X-100. The wetting agent is used to
cause complete wetting by the aqueous treating solution of the fibers in the
fabric.
All of the samples were run on all-cotton fabrics which are the most
difficult to treat because of the severe loss in tensile and tear strength,
which
.causes the treated fabric to be commercially unacceptable. The normal
industry standard for tear and tensile strength for an all cotton shirting
fabric
is characterized by having a filling tensile strength of 25 pounds and a
filling
tear strength of 24 ounces. The cotton fabric must meet and/or exceed this
standard. The test conditions are set forth in the table.
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The silicone elastomer was the commercially available softener
Sedgefield Elastomer Softener ELS, which is added as an opaque white
liquid which contains from 24-26% silicone, has a pH of from 5.0-7.0 and is
readily dilutable with water. When used in the present invention, this product
produced DP values at catalyst concentrations of 0.8%, whereas with the
Mykon HD, a catalyst concentration of 2.0% was required to give a DP value
of 3.50 after 1 washing and 3.25 after 5 washings.
The tensile strength with a catalyst concentration of 0.8% and tear
strength are significantly and unexpectedly higher than the 2.0% catalyst
required with Mykon HD to give equal DP results. Catalyst concentration of
1.0% ELS is recommended to ensure a margin of safety, such that any
variation in treatment will be well within accepted specifications.
The following examples are being presented not as limitations but to
illustrate and provide a better understanding of the invention. In order to
confirm the fact that formaldehyde was being lost from the conventional
processes, experiments were conducted in which the fabric was heated very
quickly by very hot air as in the conventional processes as well as in
accordance with the present invention.
2o Example 1
As indicated, it is possible to cure with a high enough temperature that
the crosslinking reaction is achieved before sufficient formaldehyde is lost
preventing good treatment. In this experiment, 100% cotton oxford shirting
was padded with formaldehyde (37%) at a concentration of 5.0% OWF, 0.8
% OWF of Freecat #9 Accelerator manufactured by Freedom Textile
Chemicals Co. and 1.5 % OWF of a silicone elastomeric softener, Sedgesoft
ELS manufactured by Sedgefield Specialties, to a pickup of approximately
60-70%. The sample was then dried and cured while under tension in an air
circulating oven set at 300°F. for 10 minutes.
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Example 2
Another sample of the same fabric as used in Example 1 was padded
with a similar solution differing only in that the catalyst Accelerator #9 was
1.0% OWF. Otherwise the sample was treated precisely the same.
Example 3
Another sample of the same fabric as used in Example 1 was padded
with a similar solution differing only in that the catalyst Accelerator #9 was
2.0% OWF. Otherwise the sample was treated precisely the same.
Example 4
Another sample of the same fabric as used in Example 1 was padded
with a similar solution differing only in that the catalyst Accelerator #9 was
0.4% OWF, and Mykon HD was substituted for the Sedgesoft ELS
elastomeric Softener. Otherwise the sample was treated precisely the same.
Example 5
Another sample of the same fabric as used in Example 1 was padded
with a similar solution differing only in that the catalyst Accelerator #9 was
0.8% OWF, and Mykon HD was substituted for the Sedgesoft ELS
elastomeric Softener. Otherwise the sample was treated precisely the same.
Example 6
Another sample of the same fabric as used in Example 1 was padded
with a similar solution differing only in that the catalyst Accelerator #9 was
1.0% OWF, and Mykon HD was substituted for the Sedgesoft ELS
elastomeric Softener. Otherwise the sample was treated precisely the same.
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Example 7
Another sample of the same fabric as used in Example 1 was padded
with a similar solution differing only in that the catalyst Accelerator #9 was
1.5% OWF, and Mykon HD was substituted for the Sedgesoft ELS
elastomeric Softener. Otherwise the sample was treated precisely the same.
Example 8
Another sample of the same fabric as used in Example 1 was padded
with a similar solution differing only in that the catalyst Accelerator #9 was
2.0% OWF, and Mykon HD was substituted for the Sedgesoft ELS
elastomer~c Softener. Otherwise the sample was treated precisely the same.
Example 9
A sample of the same fabric was washed in a home washer and
tumble tried, but not treated with any crosslinking process.
Example 10
Another sample of the same fabric served as an untreated, unwashed
control.
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WO 99/58758 PCTNS98/09367
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CA 02331646 2000-11-10
WO 99158758 PCT/US98/09367
It is clear in Table No. I that samples treated with the
elastomeric softener produced higher degrees of durable press than
any of the samples treated with Mykon HD. Tensile Strengths are
similar as is shrinkage for each degree of treatment.
In another experiment, the results shown in Table No. II,
samples of 100% cotton oxford shirting were padded with two
concentrations of formaldehyde 3.0 and 5.0% OWF, each
concentration also treated with three concentrations of Accelerator #9
Catalyst, 0.8, 1.0, and 2.0% . In one half of the samples, Sedgesoft
1 o ELS was applied and in the other half Mykon HD was used as the
softener. Both softeners were applied at 1.5% OWF. Each of the
samples were padded with the respective solutions shown in Table
No. II, then cured at 300°F. for 10 minutes under tension. All
samples were treated in precisely the same way, intervals were
timed.
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the control) that after 5 washes, the Sedgesoft ELS samples have
almost twice the tear strength of the Mykon HD samples without
exception. In addition, again seen, the DP values are higher
indicating better smoothness.
17
CA 02331646 2000-11-10
WO 99/58758 PC'f/IJS98/09367
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