Note: Descriptions are shown in the official language in which they were submitted.
2116299 -
.:~
. cuc~sl8l4
.`'. 5 ll~OD l?OR lMPRO~IllG q!l~lS BI.~5aC~1 R~ 18TAJI~
OF DY~D q~D~T~L~ FIBBR AND PRODUCT ~Dl~ T~B~UlBlr
R~5~ArED APPI.~CATIONS
J.'' This application is a continuation-in-part of Serial Number
07/876,493 filed April 30, 1992, specific mention being made
~' 10 herein to obtain tne benefit of its earlier filing date.
"
BAC~RO~D OF ~ INVENT~ON
. 3. This invention relates to formation of a non-volatile
polymeric salt film derived from polyamines and polycarS~oxylic
acids on a dyed textile fiber to prevent color loss, eapecially
`~ 15 by chemical attack from solutions of chlorine blcach, and to
improve colorfastn~ss.
Polymeric coal:ings have been applied to textile fiber~ to
solve a wide range of probleSms. It is well known that ~ela~ine-
~ formaldehyde, urea-formaldehyde, thiourea-formaldehyde and
;~ 20 phenyl-formaldehyde resins may be applied to cellulosic fibers to
impart anti-creasing properties, prevent shrinking and for
fixation of dyestuffs. Additionally, these resins have been
found to protect dyed cellulose textiles from color 108~ when
they are exposed to chlorine solutions. In Landolt, U.S. Patent
Number 2,373,191, a process is disclosed for combining a dyed
fiber, such as cotton, which has been treated with one of the
aforementioned resins and cured, with a fiber, such as wool,
which is to be treated in a chlorine solution to prevent
.,1
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2116299
'
: Cuc ND. 1814
shrinkage. Subsequent application of a chlorine solu~ion to ~he
fiber mixture should not discolor the dyed cotton fiber.
Recently, formaldehyde has been targeted as a hazardous chemical
in the work place and its use has become severely restricted.
Other drawbacks of the urea-formaldehyde type resins include
yellowing and stiffness imparted to the treated fiber.
A number of known procasses ar~ directed to providing
permanent press or anti shrink properties to wool and blend3 of
~; wool fibers with some type of polymeric film. For exampl~,
10 Intermacom A.G.'s British Patent 1,259,082 discloses in situ
formation of a polyamide film on a textile fiber. In i~i~u film
formation may be achieved by interfacial poly~erization u~ing a
diamine and diacid chloride or diacid ecter. Alternatively, a
polyamide emulsion or solution may be applied to a textlle ~iber
1~ and cured, such as in Coe, U.S. Patent 2,890,097. Th~
processes have limited applications to the treatment of carpet,
~ince thQy tend to impart a harsh hand to the finished product
.'J and have not been demonstrated ~o impart bleach resistance to
dyed textile fibers.
Textile floor coverings, particularly polyamide pile carpet,
have been the focus of a variety of protective treatments.
Sulfonated phenol-formaldehyde condensation products, styrene-
maleic anhydride copolymer and polymers and copol~mers of
methacrylic acid have been applied to polyamide fibers to prevent
staining, and represent the "stain blocker" technology. Ozone
;-`
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211fi299
Cll~e No. 1814
protection has been sought by coating polyaMide fiberis with one
or more of N,N'-disubstituted thioureas, polythioureas, tertiary
amines formed by the reaction of epoxides and amines and organic
phosphites. Also, a combination of film-forming polyvinyl
chloride and water insoluble organic phosphate ester has been
applied to polyamide fiber to provide flame retardancy.
Despite the availability of the aforementioned treatments,
serious shortcomings remain in protecting floor covering ~rom
discoloratio~ by bleach. This problem is especially pr~vnlent at
health care installations where bleach solutions are routinely
used to disinfect furniture, equipment, fixtures, and the
interior of the building. Even a spill of a dilute bleach
solution, as low as O.05 wt.% solution of sodium hypochlorite,
can ruin a section of carpet.
One approach to eliminating the risk of discoloration caused
by bleach has been to provide solution dyed fibers. Thus, the
dye is incorporated into the polymer melt prior to spinning. The
colorant is evenly distributed throughout the cross-section of
;3 the fiber. If the fiber is later exposed to bleach, only the dyé
at the surface will be affected and the overall color of the
~ fiber will not be significantly diminished.
i Nevertheless, solution dyed fibers have several drawbacks,
not the least of which is that they are more expensive to
, produce. Further, solution dyed fibers introduce additional
complications to the manufacturing process. Large inventories of
~.1
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~J
- ~ 2116299
~ ~ 1814
each color of fiber must be maintained rather than a single
inventory of undyed fibers, which can later be dyed to the
desired color. If patterning is desired, one must either tuft ~-
the carpet with two or more different colored yarns or print the
pattern over the base color. The first alternative is very
~2'~, expensive. Overprinted patterns, which are only applied to the2~2 surface of the fiber, are typically used, but the patterns are subject to bleach attack.
In addition to the problems encountered from bleach attack,
~ l0 many dyed textile fibers, especially those incorporated into
'.:f floor coverings, are susceptible to wet crocking. The problem is
frequently encountered during shampooing, where the combination
of mechanical agitation and detergents particularly is severe.
~M~A~Y OF T~ INV~NTION
Therefore, one of the objects of this invention is to
provide an economical dyed textile fiber which is resistant to
discoloration by chlorine bleach.
Another object of this invention is to provide a treatment
, to impart bleach resistance which can be applied after the fiber
-i' 20 is dyed or to textiles having a pattern printed thereon.
. Yet another object of this invention i~ to provide a
treatment for imparting bleach resistance which does not contain
formaldehyde, discolor or adversely impact on the hand of the
textile f iber.
"',
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. .~, .
211~299
C~ 1814
A further object of this invention is to provide a treatment
which will improve the colorfastness of dyed textile fiber,
especially with regard to wet crocking and shampooing.
Accordingly, a method for treating a dyed textile fiber is
provided having the steps of applying solutions of non-volatile,
polymeric ~alt formin;~, poly-functional monomers to the dyed
t~xtile fiber, drying the textile fiber at a temperature
sufficient to polymerize the monomers and below a softening
te~perature of the textile fiber, to form a water insoluble, non-
volatile polymeric salt film on the textile fiber. A textileproduct made according to the above method is also included
within the scope of th invention.
The invention features application of the treatment solution
by conventional techniques, such as padding, baths or spraying.
The solution may be a~ueous, thereby avoiding the emission of
organic solvents. The treatment ~olution may be applied to
carpet which has already been installed and the non-volatile
polymeric salt allowed to equilibrate at ambient temperature.
DE~CRIPTION OF T~E PREFERRED EMBODIM~NT OF TH~ INV~NTION
Without limiting the scope of the invention, the preferred
features and embodiment of the invention is hereinafter set
forth. The object of the invention is to provide dyed textile
fiber with protection from chemical attack by chlorine bleach,
~ which is known to discolor the dye, and improved colorfastness.
`~, 5
, '
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5~ , ' ' "''''`' ~`'~
2116299
':
` Cuet~ 1814
The most common route of exposure to damage occurs when cleaning
solutions or disinfectants containing sodium hypo~hlorite are
spilled on carpet. Nylon or polyamide fiber is used
predominantly as the face material for floor covering and is the
focus of the present invention.
Of course, an important criteria in evaluating the treatment
is the degree to which the textile fiber is protected from
discoloration when exposed to a chlorine bleach solution. For
disinfecting purposes, the Center for Disease Control recommends
a 0.05 % solution of sodium hypochlorite for non-porous sur~aces,
such as counter tops, and a 0.5% solution for porous sur~aces,
such as grout. Sodium hypochlorite is referred to gener~lly
herein as chlorine bleach or bleach. Spills of bleach solution
may remain unattended on the carpet for hours or even day~, which
i~ 15 adds to the strain placed on any protective treatment.
Additionally, the protective treatment should be durable, be
able to withstand foot traffic and multiple washings, and improve
colorfastness. With regard to cleaning the carpet with "wetS'
techniques, such as hot water extraction, it is important that
the treatment be water insoluble. The protective treatment
should have a minimum impact on the physical characteristics of
the textile fiber. Therefore, the treatment should not impart a
i~ harsh hand to the fiber, cause matting or yellowing.
Heightened environmental awareness has limited the
acceptable monomers, polymers and solvents which may be use~ in a
.,i
~ ~,
:;,r ~ ;:
11 21162~9
~ N~1814
protective treatment. For example, resins containing
formaldehyde and organic solvents, especially those containing
aromatics, are undesirable. Even treatments employing less toxic
organic solvents can substantially increase manufacturing costs
when emission controls are required.
The bleach resistance treatment is applicable to both
natuxal and synthetic textile fibers. Thus, by way of example,
fibers made from the following materials may be effectively
treated according to the methods disclosed herein: polyamides,
polyesters, polyolefins, acrylics, and cellulosic fibers such as
cotton and rayon. The treatment method is especially useful ~n
polyamide fibers, particularly Nylon 6 and Nylon 6,6. The term
"fiber" is used in a broad sense and is intended to include both
staple fibers and filaments. It is not material to the praCtice
l 15 of ths invention whether the fibers are treated prior to or after
, being formed into a textile product as long as the fiber has
.,. f irst been dyed. Accordingly, the fiber may be treated in the
form of a staple fiber, filament, yarn, woven, knitted, or
nonwoven fabric, or adhered to a substrate as by tufting or
adhesion. From a manufacturing point of view, since most fibers
are dyed after being formed into a textile product, the bleach
resistance treatment will usually be applied to a fabric or floor
covering product.
The present treatment method has applications when any dye
which is susceptible to discoloration by chlorine bleach, is used
. .
s,
,,,~ , ~ . '
21162~9
~i ~JO. 1814
to color textile fibers. The dye may be fixed to the sur~ace, of
the textile fiber by, for example, chemical reaction, ionic
association or with a binder. Representative examples of types
of dyes which may be protected by the instant treatment include
5 acid dyes, basic dyes, cationic dyes, direct dyes, dispersed
dyes, fiber-reactive dyes, metalized dyes, pre-metalized dyes,
and vat dyes. Classes of dyes within each o~ these categories
which are particularly susceptible to attack by hypochlorite ions
are acid dyes and fiber reactive dyes. Selection of an
10 appropriate dye for a particular type of fiber is well within the
knowledge of those with skill in the art,. Likewise, applica~ion
~ of the dye to a particular textile product such as by yarn
; dyeing, range dyeing, jet dyeing, solution dyeing or other
, conventional techniques, is a routine matter. Textile pr~ducts
!3 15 containing a base color, including those made of solution dyed
i synthetic fibers, which have been overprinted with a pattern,
such a~ by ink jet printing, screen printing, or gravure
printing, may be treated to provide bleach resistance. Since the
~;` method of imparting bleach resistance to the textile fiber
20 comprises forming a non-volatile, polymeric salt film on the
~ fiber surface, the particular dye or dyeing technique is not
3 considered critical.
Generally, bleach resistance is imparted to a textile fiber
by applying solutions of monomers and allowing the monomers to
25 react to form a protective film on the fiber. The monomers may
;d
'.'i
`: ` ` 2116299
~ ~.1814
include oligomers or relatively low molecular weight "polymers"
containing functional end groups, which may be reacted to form a
,'.7, non-volatile salt film. The monomers are characterized by
3, compounds which form polymeric, non-volatile salt films,
~ 5 requiring that thev are at least bifunctional. Higher
j.7 functionality monoJ,ers, such as a combination of butane
tetracarboxylic acid and a diamine may be used effectively.
~i In a preferred embodiment the diamine used in the reaction
to form a polymeric salt is a low molecular weight "polymeric~
diamine made by reacting one mole of an ester of a diacid or
diacid chloride wit~ two moles of a diamine. For example, one
mole of a methyl ester of adipic acid, glutaric acid or succ$nic
acid, may be reacted with 2 moles of hexamethylene diamine to
;! for~ a low molecula- weight polyamide, diamine. The "polymeric"
;~ 15 diamine is substantially less volatile than hexamethylen~
diamine, and thus, does not pose a health risk. The "polymeric"
diamine contains a diamine covalen~ly bonded to the diacid ester
to form an amide linkage and is distinguished from the polymeric
salt film formed on the fiber by the reaction of a diamine and
diacid under conditions which do not form a polyamide.
The monomers used to form the polymeric salt are preferably
water soluble or easily emulsified or dispersed in an aqueous
solution. Monomers having molecular weights less than l,000 are
preferred, those with molecular weights less than 750 are most
~', 25 preferred.
,.,; 9
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~,
2116299
CueNo.1814
Thus, one important group of monomers useful herein are
combinations of C2_20 polyamines and polycarboxylic acid~. By
way of example, suitable polyamines include: ethylenediamine,
hexamethylenediamine, 1,8-octanediamine and piperazine. And,
examples of suitable polycarboxylic acids include: carbonic
acid, cxalic acid, glutaric acid, adipic acid, pimelic acid,
suberic acid, azelaic acid, sebacic acid, dodecanedioic acid,
i`i isophthalic acid, butane tetracarboxylic acid and terephthalic
'i~ acid. Especially useful are combinations of diami~es and
r~ 10 diacids, most preferable are hexamethylene diamine and adipic
acid. Polymers formed from the reaction of diamines and dibasic
acid will be referred to as AABB type polymeric salts.
Another class of monomers are C2_20 amino acids which ~orm
~i AB type polymeric salts. Examples of these type monomers include
6-aminohexanoic acid, aminoundeconoic acid, 2-
pyrrolidinecarboxylic acid, glycine, cystine, asparagine,
glutamine, lysine, arginine, tyrosine, and aminododeconoic acid.
~, Al~o included within the scope of useful monomers are lactams
formed from the aforementioned amino acids, where possible,
especially ~-caprolactam, provided t~e lactam is heated in the
presence of water to form an amino acid salt.
l The treatment solution has a total monomer concentration of
- from 2 to 30 wt.%, preferably from 5 to 20 wt.~. The solvent
itself is selected on the basis of its ability to form a solution
i 25 with the monomers, preferably at ambient temperatures. However,
:.:.,s ..
11 10
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: , . -: , : : : ~ : : . .:
2116299
Ca~ No. 1814
it is i~portant that the textile fiber itself is not isoluble in
~` or plasticized by the solvent. The solvent is preferably aqueous
or a Cl-C8 alcohol. Other polar solvents and organic solvents
may be employed, however, due to problems with toxicity or other
limitations on emissions, their use is less desirable.
~; The treatment solution is applied to a dyed textile fiber,
; which may be in the form of a staple fiber, filament, yarn,
~ fabric, or adhered to a substrate. Any of a number of
G,1, conven~ional techniques for wetting a textile fiber with a liquid
!,'. 10 solution may be used. For example, the treatment solution may be
applied to pile carpet by padding, spraying, or immersion in a
bath. The traatment solution can be applied to carpe~ which ha~
already been installed, and may even be accompanied by mechanical
agitation to ensure thorough wetting. The wet pick up ii~
typically from 5 to about 50 wt.% treatment solution based on the
dry weight of the textile fiber, not including a substrate. A
~t, wet pick up of approximately 25% of the weight of the textile
fiber is typical.
The amount of treatment solution applied to the textile
~' 20 fiber may conveniently be gauged in terms of the weight percent
of monomer solids per weight of fiber, which when reacted, will
represent the weight percent of polymeric salt film on the fiber.
The lower limit of application believed to provide at least a
. modicum of protection is about one weight percent solids per
~: 25 weight of fiber. The amount of monomer applied may be increased
,. 11
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- 2116299
~'s
C~: No. 1814
-~ up until the point that an adverse effect on the hand and matting
of the textile fibers is observed. As a practical matter,
diminishing returns of increased protection versus cost will be
seen after approximatel-~ 10 wt.% monomer solids per weight of
5 fiber is reached. Preferably, from 2 to 7 wt.% monomer solids
per textile fiber is achieved by application of the treatment
solution.
The next step of the process is to allow the monomers to
react to form a protective, non-volatile, polymeric salt film on
the textile fibers. The treatment solution will react at ambient
conditions, at least 20 C~ However, in the case of applica~ion
of the treatment solution to installed carpet, that is a vlable
method of achieving protection. ~dditionally, when treating
installed carpet, it~is important to consider the solvent ~
selected for the treatment solution. Aqueous solution~ are
preferred for health, safety, and environmental concerns, since
the solvent evaporates after application as the monomers begin to ~;
.~ react.
Those with skill in the art will recognize that the pH of
the treatment solution may need to be adjusted to dissolve,
emulsify or disperse the monomers. For example, amino acids such
as cystine, arginine and asparagine are more readily dispersed at
~ a pH of 11-12 in an aqueous solvent. After application of the
,1 treatment solution to the textile fiber, an acid, such as citric
acid, may be applied to lower the pH and precipitate the
;,
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, 2116299
C~ ND. 1814
monomers. Preferably, the pH of the treatment solution i~
returned to neutral, since the treatment is found to be most
effective in protecting against bleach attack at a pH of 6-8,
preferably 7. In that regard, a buffer, such as sodium citrate,
may be useful in maintaining a neutral pH and may be added with
~! the citric acid.
~ In a preferred embodiment, salicylic acid is added to the
,~, treatment solution and has been found to enhance the bl~ach
resistance of the treated textile. Without being bound to a
particular theory, it is believed that the -O~ group of the acid
participates in the reaction with the hypochlorite ion. Unllk~
other phenolic comE~ounds, the salicylic acid does not appear to
cause yellowing of the textile fiber. The pH of the treatment
~, solution may be adjusted to 11-12 to dissolve the salicylic acid
prior to application. From 0.1 to 7 wt.% of salicylic acid per
weight of textile Ciber ~ay be applied, preferably from 0.5 to
5.O wt.% of salicylic acid.
It has been found that some monomers, such as the
"polymeric" diamine containing two moles of hexamethylene diamine
and one mole of a dibasic ester described above may act as an
~, emulsifier to disperse salicylic acid at neutral pH.
Consequently, a treatment solution containing a "polymeric"
~; diamine, or other emulsifier, and salicylic acid could be
neutralized prior to application of the solution to a textile
fiber.
.
13
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~ ' ~ ' ' . ' - ,, A ~ , . ' '
21162~9
:
.,, C~eNQ 1814
While it is preferable to apply all of the monomers to the
~; textile fiber in a single treatment solution, the invention is
-~ not so limited. For example, a solution of the diamine could be
~, applied first to the textile fiber followed by application of a
second solution containing the diacid, or vice versa. As
~ discuss2d above, the pH of the treatment solution containing one
or more monomers may be adjusted after the treatment solution i~
applied to a textile fiber.
The durability of the protective non-volatile polymeric salt
film may be enhanced by reacting the treatment solution at higher
temperatures. For example, polyamide fiber in the form of a
. tufted pile carpet, may be heated in an oven to temperatures up
!~ to the softening point of the fiber. Thus, reaction temperatures
of from 100 C to the softening temperature of the fiber m~y be
used. Typically, the textile fiber is exposed to temperatures o~
from 100 to 200 C, preferably 120 to 160 C. The length of
exposure will be determined by the time required to evaporate the
sol~ent and to drive the reaction to completion.
Catalysts may be employed in the treatment solution to
improve the configuration of the non-volatile, polymeric salt on
the surface of the fiber when the treatment is performed at l~wer
temperatures, especially when reac~ion occurs at ambient
conditions. Since bleach resistance may be lost if the
protective film is washed off during normal carpet cleaning, it
is preferable that the reaction proceed to the extent that a
14
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;: , - -~ ~:: .,,
. "-' ' ' ., - :, -~ :
,~
",,. ':
2~16299
Ca~e No. 181~.
; water-insoluble film is formed on the textile fiber.
Without being bound to a particular theory, it is
hypothesized that the non-volatile, polymeric salt film formed on
the textile fiber provides a primary amine functionality which is
sacrificed to the bleach solution. In particular, the amino
nitrogen of the non-volatile polymeric salt film reacts with the
hypochlorite ion of the bleach solution.
Additional compounds used to improve the characteristics of
textile fibers may be incorporated into the treatment solution so
long as they do not interfere with the non-volatile polym~ric
salt formation. For example, fluorocarbon polymers which provide
~ anti-soiling and water repellency, and stain blockers ~uch as
.9 condensation products containin~ sulfonated phenols may be
employed.
The invention may be further understood by re~erences to the
following examples, but the invention is not to be construed to
be unduly limited thereby. Unless otherwise indicated, all parts
and percentages are by weight.
, E~ANP~ 1
,~, 20 A 26 oz/yd2, stock dyed with premetalized and standard acid
s, dyes, loop pile, nylon 6,6 carpet is pretreated by spraying onto
, the pile a homogeneous aqueous solution containing 8 percent by ~-
~, weight of hexamethylenediamine and 8 percent by weight of adipic
acid. The wet pickup is about 25 percent based on the dry weight
'''s
` 211629~
.,
., C~cNo.1814
of the nylon face fiber. The carpet is then submitted to a
drying temperature of 275F for a period of 7 minutes. The
treated carpet shows no appreciable change in appearance. The
.i treated carpet and an untreated control are then subjected to a
~, 5 0.5 percent solution of sodium hypochlorite (the recommended
r.J Center for Disease Control concentration for disinfecting
,,AIj purposes for porous surfaces) for a period of 24 hours, a~ter
which the carpet is washed with water and dried. Visual
comparison of the treated carpet to an untreated control sample
10 clearly reveals that the treated carpet has superior re~istance
to color loss.
.~
i'. E~AMPLE 2
. '
The procedure of Example 1 is repeated in all respects
except the carpet is 28 oz/yd2 stock dyed nylon 6,6 cut pile.
Identical results as those of Example 1 are ohtai~ed.
~SA~PLE 3
,.~
The procedure of Example 1 is repeated in all respects
except the 26 oz/yd2 stock dyed nylon 6,6 carpet is also
overprinted with a pattern using similar acid dyes as in Example
1, prior to application o~ the treatment solution. Identical
¦¦ results as th e of ~xample l are obtained.
',,'
~l 16
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211fi299
~ ~.1814
EXA~PLE ~
The procedure of Example l is repeated in all respects
except the carpet is made from a solution dyed nylon 6,6 fiber
and is overprinted with a pattern prior to application of the
treatment solution. Identical results as those of Exa~ple l are
obtained on the overprinted pattern, the solution dyed color
being unaffected on both the treated and control carpet.
.,
~AMP~ 5
The procedure of Example l is repeated in all respects
except the carpet is treated with a homogenous solution of lO
percent by weight of caprolactam and lO percent by weight o~
urea. Identical results as those of Example l are obtained.
} EXAMPL~ 6
,~,j
The procedure of Example l is repeated in all respect~
15 except butanetetracarboxylic acid is substituted for the adipic
acid. Similar results as those of Example l are obtained. -~
EXANPLE 7
The procedure of Example 2 is repeated in all respects
except the treated carpet is subjected to simulated wear and
cleaning of 5 years before exposure to the hypochlorite solution.
Similar results as those of Example l are obtained.
17
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2116299
~!,
~j C~eNo.1814
.j, E~I.B 8
Example 2 was repeated in all respects except the treated
sample was air dried. A visual comparison of the treated sample
to the untreated control reveals a decrease in color 1088 in the
treated sample but not as significant as in the untreated
control.
~,
The following examples demonstrate the improved
' colorfastness of dyed textile ~ibers which have been treated
according to the present invention and subjected to commercial
, 10 cleaning solutions or water.
,i 1
-i E~AMPL~ 9
';~ Example 3 was repeated im all respects except that both the
treated and untreated control samples ere scrubbed with a 5%
solution of Fiber Fresh from Service Master Company. m e samples
were then covered by a multifiber test strip available from Test
Fabrics, Inc. The test strip was in turn covered by a l/4"
plexiglas and placed in an over at 100 F. A 5 pound cylindrical
~ weight was placed on the plexiglas. The samples remained in the
;, over for 18 hours, after which the dye bleeding into the
' 20 multifiber test strip was graded on a 5 point AATCC grey scale.
, The treated sample showed a passing rating of 4.0, whereas the
untreated control had a failing rating of 3Ø
, 18
~,
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` ~ 2~16299
;,
~ ~Nh1814
, E~AMPLB lO
,, Example 9 was repeated in all respects except that the
c carpet of Example 4 was used. Identical results were obtained on
, the overprinted pattern.
...
~, 5 B8AMPLB ll
Example 3 was repeated in all respects except that both the
''.J' untreated control and the treated samples were subjected to
i deionized water in a beaXer for 15 minutes. Next, the sample~
'.J~ were remov~d from the water and shaken until the amount o~ water
remaining was 2.5 to 3 times the original dry weight o~ the
-¦ carpet. The samples were covered with a multifiber test strip,
covered with l/4" plexiglass and placed in a 100 F oven. A 5
pound cylindrical weight was placed on the plexiglass. ~he
samples remained in the over ~or 18 hours after which the dye
bleeding into the multifiber test strip was graded on a 5 point
AATCC grey scale. The treated sample showed a passing 4.5
rating, whereas the untreated control had a failing 3.5 rating.
,i :
EXAMPLE 12
~ Example ll was repeated except that the carpet of ~xampl~ 4
;~ 20 was used. Similar results were obtained on the overprinted
pattern.
19 .,
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2116299
.,
.
Cu~ ND. 1814
There are, of course, many alternate embodiments and
/ modifications which are intended to be included wikhin the scope
:i of the following claims.
-:~
,~
~ 20
