Note: Descriptions are shown in the official language in which they were submitted.
2 1 ~3046
EN~ANCEMENT OF STAIN RESISTANCE OR ACID
DYE FIXATION, IMPROVED LIG~T FASTNESS AND
DURABILITY OF FIBROUS POLYAMIDE AND WOOL SUBSTRATES
This invention relates to a fibrous substrate,
more especially a polyamide or wool substrate having
stain resistance or enhanced fixation of acid dyes, light
fastness and wash fastness; to a process for imparting
stain resistance or enhanced fixation of acid dyes, light
fastness and wash fastness to such a fibrous substrate;
to a formulation for enhancing stain resistance or
fixation of acid dyes, light fastness and wash fastness
of such a fibrous substrate.
Fibrous polyamides and wool are employed in the
manufacture of textile products such as carpets which are
dyed in a variety of colours or in a pattern defined by
colours. Polyamides, notably nylons are in particular
widely employed in carpet manufacture.
Such products are frequently exposed to
staining by natural and artificial colourants which are
commonly found in many foods and beverages
A number of treatments are available to provide
stain resistance in such textile products, for example,
carpets, so that the products are resistant to staining
by such colourants.
The most efficient stain resisting agents known
are resins, in particular, novolak resins, resol resins
and condensation products of formaldehyde with
dihydroxydiphenyl sulfone and naphthalene sulfonic acid.
A major problem with these resins is that when
they are used alone as a stain resist, they have a
reverse effect on the light fastness and cause yellowing
problems on the treated fibers. Much research has been
done in an attempt to overcome this problem.
It has been proposed to reduce the amount of
dihydroxydiphenolsulfone and increase the amount of
- 2 - 2 1 93~4~
phenol sulfonic acid or naphthalene sulfonic acid,
however, the improvement in the yellowing problem and the
light fastness was not significant. The addition of
products having a high resistance to oxidation or light,
to the stain resist has also been proposed but this
improved only slightly the yellowing problem and the
light fastness.
It has been proposed to reduce the amount of
phenolic resins and replace them with other stain
blockers, for example, polymeric methacrylic acid resins,
which improved the light fastness and also solved to a
great extent the yellowing problem. The disadvantage
with these products is the poor wash fastness because the
polymeric methacrylic acid resins have poor wash fastness
and the low amount of phenolic resin in the product is
not sufficient to provide acceptable wash fastness, and
light fastness, at the same time.
It has also been proposed to use a small amount
of magnesium sulfate with the stain blocker in the same
bath, this did not improve the light fastness at all, but
slightly improved the exhaustion of the stain blocker and
did not have any effect on the wash fastness or the
durability of the carpet to shampooing.
The most popular acid used for application with
stain blockers is sulfamic acid because it is a strong
acid and economical, however, it causes noticeable
yellowing of polyamide fibers. Some manufacturers have
employed citric acid which produces a better quality and
does not cause yellowing of the polyamide fibers, but
this is expensive, especially if the pH required is under
2.5 where larger quantities of this acid are required.
There remains a need to provide stain
resistance in conjunction with light fastness and wash
fastness on polyamide and wool substrates, such as
carpet.
_ 3 _ 2 1 93346
Thus, U.S. Patent 4,592,940 describes the use
of a condensation product of formaldehyde, dihydroxy
diphenylsulfone and phenosulfonic acid to provide stain
resistance on nylon carpets. U.S. Patent 4,501,591
describes a process for continuously dyeing polyamide
carpets in which stain resistance is imparted to the
carpet during the dyeing by adding an alkali metal
silicate and a sulfonated phenol-formaldehyde
condensation product to the dye liquor used in the
dyeing.
U.S. Patent 5,3Z8,766 describes the use of a
combination of a partially sulfonated novolak resin and a
soluble aluminum salt optionally with a methacrylate
polymer to impart stain resistance, light fastness and
durability to alkaline wash, to fibrous polyamide and
wool substrates.
U.S. Patent 4,822,373 describes the use of a
partially sulfonated novolak resin and homopolymers or
copolymers of methacrylic acid, to provide resistance to
staining by acid colourants in fibrous polyamide
materials.
U.S. Patent 4,937,123 describes the use of
homopolymers or copolymers of methacrylic acid to provide
stain resistance to acid colourants in fibrous polyamide
materials.
The problem of the yellowing and loss of stain
resistance in nylon carpets treated with sulfonated
phenol or naphthol condensates with aldehydes is
described in American Dyestuffs Report, Vol. 25, No. 11,
November 1993, by X. X. Huang et al of The Textile
Research Institute, Princeton, New Jersey, U.S.A.
Canadian Patent 1,258,365 describes a low pH
liquid buffer obtained by a combination of phosphoric
acid and sodium phosphate monobasic.
- 4 - 2 1 93046
U.S. Patent 5,328,766 describes the use of
aluminum sulfate as a catalyst with a stain blocker.
This invention seeks to provide a fibrous
polyamide or wool substrate having improved
characteristics of stain resistance, light fastness and
wash fastness.
This invention also seeks to provide a process
for imparting stain resistance, light fastness and wash
fastness to a fibrous polyamide or wool substrate.
Still further this invention seeks to provide a
formulation for enhancing stain resistance, light
fastness and wash fastness.
In accordance with one aspect of the invention
there is provided a fibrous substrate having improved
stain resistance, light and wash fastness comprising a
fibrous polyamide or wool substrate bearing a formulation
comprising:
i) a water soluble sulfonated aromatic aldehyde
condensation resin, a hydrolyzed aromatic-
containing vinyl ether maleic anhydride co-
polymer or a half ester of an aromatic-
containing vinyl ether maleic anhydride co-
polymer,
ii) a mixture of an acid selected from the group
consisting of citric acid, sulfuric acid,
phosphoric acid and polyphosphoric acid
and at least one metal compound selected from
the group consisting of magnesium salts,
magnesium hydroxide, magnesium oxide copper
salts, copper hydroxide, copper oxide,
aluminum salts, aluminum hydroxide and
aluminum oxide.
In accordance with another aspect of the
invention there is provided a process for imparting stain
2 1 93~46
resistance, light and wash fastness to a fibrous
substrate comprising:
a) contacting a fibrous polyamide or wool sub-
strate with an aqueous vehicle or medium
containing:
i) a water soluble sulfonated aromatic
aldehyde condensation product, a
hydrolyzed aromatic-containing vinyl
ether maleic anhydride copolymer or
a half ester of an aromatic-containing
vinyl ether maleic anhydride copolymer;
ii) a mixture of an acid selected from the
group consisting of citric acid,
sulfuric acid, phosphoric acid and
polyphosphoric acid and at least one metal
compound selected from the group con-
sisting of magnesium salts, magnesium
hydroxide, magnesium oxide, copper salts,
copper hydroxide, copper oxide, aluminum
salts, aluminum hydroxide and aluminum
oxide;
b) allowing components i) and ii) to transfer
from said aqueous vehicle or medium to said
substrate; and
c) drying said substrate.
In accordance with the invention there is
employed a sulfonated aromatic-aldehyde condensation
resin, a hydrolyzed aromatic-containing vinyl ether
maleic anhydride copolymer or a half ester of an
aromatic-containing vinyl ether maleic anhydride
copolymer in conjunction with a mixture of one or more of
phosphoric acid, polyphosphoric acid, citric acid and
sulfuric acid; and one or more of the metal compounds
identified hereinbefore.
2 7 9304G
In particular embodiments there may
additionally be employed a polymeric methacrylic acid,
namely, a homopolymer or copolymer of methacrylic acid.
i) Sulfonated Aromatic-Aldehyde Conden8ation Resin
The condensation product or resin may be a
sulfonated resol resin, a sulfonated novolak resin or a
condensation product of an aldehyde with
dihydroxydiphenyl sulfone and naphthalene sulfonic acid.
In these condensation products or resins, the
aldehyde is, in particular a lower aliphatic aldehyde,
for example, formaldehyde or acetaldehyde, usually
formaldehyde.
The sulfonated resol resin may be produced as
the sulfonated condensation product of at least one
phenol and at least one aliphatic aldehyde, the
condensation being carried out at a pH higher than 7.
Suitable sulfonated resol resins are produced
by condensing formaldehyde and phenol in alkaline media
at pH of about 9 for about 60 minutes, at about 90~ to
110~C, followed by approximately 40% sulfonation of the
phenol formaldehyde condensation product with sodium
metabisulfite at a pH between 4 and 6 at 90~ to 110~C for
about 60 to 90 minutes followed by neutralizing and
maintaining at acid pH after the treatment.
011 011 ~)11 011
2 1 93~46
011. ~ )11 011
5 ~ CII,-- ?-J~
3ll '~3l~
It will be understood that the degree of
sulfonation may be varied but will generally be 30 to
50%, preferably 40%.
Suitably sulfonated novolak resins include but
are not limited to condensation products of formaldehyde
with bis(hydroxyphenyl)sulfone and phenol sulfonic acid.
The mole ratio of the bis(hydroxyphenyl)sulfone
and the phenol sulfonic acid is generally 30 to 50:70 to
50, for example, 50:50, preferably 40:60 and more
preferably 30:70.
A typical sulfonated novolak resin is a
condensation product of phenolsulfonic acid and
dihydroxydiphenyl sulfone with formaldehyde having a
repeating unit as illustrated below:
01~ 01
~/C112 ~12 -
\~ ~.~, /f
~~3l~ \
SO2
Ol~
- 8 - 2 1 93046
A suitable condensation product of an aldehyde
with dihydroxydiphenylsulfone and naphthalene sulfonic
acid, is one in which the aldehyde is formaldehyde.
The mole ratio of the dihydroxydiphenylsulfone
to the naphthalene sulfonic acid is suitably about Z5 to
40:75 to 60, for example, 40:60, 50:50, preferably 30:70
and more preferably 25:75.
A typical condensation product of naphthalene
sulfonic acid and dihydroxydiphenylsulfone with
formaldehyde has a repeating unit illustrated below:
~ , ~ - C112 - ~ ---Cll~
~ ~2
_ ~
1~ _
These condensation products are, in particular,
water soluble and form aqueous solutions in water.
2i q3~46
ii) Maleic Anhydride Copolymer Resin
A class of maleic anhydride copolymer resin
useful in the invention comprises a copolymer selected
from the group consisting of a hydrolyzed aromatic-
containing vinyl ether maleic anhydride copolymer, a halfester of an aromatic-containing vinyl ether maleic
anhydride copolymer, and mixtures thereof. By the
hydrolyzed copolymer, or hydrolysis product, is meant the
hydrolyzed copolymer in which some, preferably less than
about 20 to 50 percent, of the original anhydride units
remain as anhydride. By the half ester is meant the
esterification product of the copolymer with a lower
alcohol, preferably a Cl-Cs alcohol, most preferably
isopropyl alcohol, in which some, preferably about 25 to
50 percent, of the original anhydride units remain as
anhydride and in which the reacted anhydride units are
monoesterified. The copolymer has a weight average
molecular weight between about 1,200 and 23,000
preferably between about 1,200 and 15,000, more
preferably between about 2,000 and 10,000 and most
preferably between about 2,000 and 4,000.
Particular copolymers include phenylvinyl-
ether/maleic diacid copolymer.
One suitable resin is that available under the
Trade Mark SR400 of E. I. DuPont de Nemours.
iii) The Mixture of the Acid and Metal Compound
The sulfonated resin is employed in conjunction
with a mixture of one or more acids selected from the
group of phosphoric acid, citric acid or sulfuric acid,
and at least one metal compound from Groups A, B and C
below:
Group A): Magnesium phosphate
Magnesium citrate
Magnesium lactate
Magnesium carbonate
2 1 93046
-- 10 --
Magnesium sulfate
Magnesium silico fluoride
Magnesium hydroxide
Magnesium oxide
Group B): Copper phosphate
Copper carbonate
Copper sulfate
Copper hydroxide
Copper lactate
Copper acetate
Copper silico fluoride
Copper hydroxide
Copper oxide
Group C): Aluminum silico fluoride
Aluminum potassium phosphate
Aluminum potassium sulfate
Aluminum magnesium sulfate
Aluminum magnesium phosphate
Aluminum sodium silicate
Aluminum lactate
Aluminum phosphate
Aluminum sulfate
Aluminum carbonate
Aluminum hydroxide
Aluminum oxide
Sodium aluminate
This mixture or combination imparts a superior
stain resistance to the fibrous polyamide or wool
substrate when employed in conjunction with the
sulfonated resin. The mixture of acid and metal compound
is soluble in cold or hot water.
2 1 93~46
The metal compounds of Groups B) and C) are all
salts and the compounds of Group A are salts with the
exception of magnesium oxide and magnesium hydroxide.
The metal compound is employed in an amount of
at least 0.1%, by weight, based on the weight of the acid
and the metal compound. The acid is employed in an
amount such that the formulation of resin, acid and metal
compound in a vehicle such as water has a pH below 7,
preferably 1.5 to 5 and more preferably 2 to 3.
iv) Polymers of Methacrylic Acid
In preferred embodiments, especially when the
fibrous substrate is a polyamide substrate, the
sulfonated resin and the mixture of acid and metal
compound are employed in conjunction with a
polymethacrylic acid, namely, methacrylic acid
homopolymer or copolymers of methacrylic acid or
combinations of methacrylic acid, homopolymer and
copolymers of methacrylic acid.
In case of the copolymers, the comonomer may be
a monocarboxylic acid, a polycarboxylic acid, an
anhydride, an unsubstituted or substituted ester or amide
of a carboxylic acid, an unsubstituted or substituted
ester or amide of an anhydride, a nitrile, a vinyl
monomer, a vinylidene monomer, a monoolefinic or
polyolefinic monomer or a combination thereof.
Representative comonomers include alkyl
acrylates wherein the alkyl group has 1 to 5, preferably
1 to 4 carbon atoms, itaconic acid, acrylic acid, styrene
and sodium sulfostyrene. The copolymers may contain one
or more comonomers for methacrylic acid.
Representative copolymers of methacrylic acid
also include terpolymers of methacrylic acid, sodium
sulfostyrene and styrene; methacrylic acid, and acrylic
- 12 - 2~93046
acid and methacrylic acid, acrylic acid and sulfated
castor oil.
Preferably, the polymeric methacrylic acid
comprise about 30 to 100 weight percent of the
methacrylic acid. Homopolymers contain 100 weight
percent of the methacrylic acid. Copolymers contain
about 30 to less than 100, preferably 60 to 90 weight
percent of methacrylic acid.
The weight average molecular weight and the
number average molecular weight of the methacrylic
polymer should be such that satisfactory stain resistance
is provided by the polymer in combination with the
sulfonated resin and the mixture of acid and metal
compound. Generally, the lower 90 weight percent of the
methacrylic acid homopolymer or copolymer has a number
average molecular weight in the range of about 2,500 to
500,000.
v) Formulation8
The active agents of the invention, namely
sulfonated resin, the mixture of acid and metal compound,
for example, salts and the optional polymeric methacrylic
acid are employed together in a vehicle or medium for
their application to the fibrous substrate. Preferably
they are employed in an aqueous vehicle or medium.
The active agents may also be employed in a
vehicle comprising a resist printing paste. In this way
the resist printing paste may be employed to print a
printed area on a polyamide or wool substrate, for
example, a carpet, and the combination of active agents
of the invention prevent staining of the printed area
with acid dyes during dyeing.
The relative amounts of the resin, the mixture
and the optional polymeric methacrylic acid in this
invention should be sufficient to provide commercially
acceptable stain resistance or light fastness and also
- - 13 - 2 ! S3046
wash fastness to fibrous polyamide or wool substrates, to
the desired degree of durability and resistance.
Optimum amounts of the active agents will vary
depending on the nature of the substrate.
In general an improvement in stain resistance,
light fastness and durability or wash fastness is
achieved when the water soluble sulfonated aromatic
aldehyde condensation product is present on the substrate
in an amount of at least 0.008, preferably at least 0.01,
and more preferably at least 0.02 weight percent based on
the weight of the substrate; and the mixture of acid and
metal compound is present in an amount of at least 0.10,
preferably at least 0.2 weight percent based on the
weight of the substrate.
By way of example, when the substrate is nylon
66 and a sulfonated resol resin is employed, the resol
resin is preferably in an amount of at least 0.008 weight
percent, the amount of methacrylic acid polymer, if
present, is at least about 0.06 weight percent; and the
amount of acid and metal compound mixture is preferably
at least about 0.1 weight percent, based on the weight of
the substrate.
When the substrate is nylon 6 the amount of the
sulfonated resol resin is suitably in an amount of at
least 0.02, preferably at least 0.03 weight percent, the
amount -of methacrylic acid polymer, if present, is
suitably at least 0.12 weight percent and the acid and
metal compound mixture is suitably in an amount of at
least 0.2 weight percent, based on the weight of
substrate.
When the substrate is wool the sulfonated resol
resin is suitably used in an amount of at least 0.02,
preferably at least 0.03 weight percent and the amount of
the acid and metal compound mixture is suitably at least
0.2, preferably at least 0.3 weight percent, based on the
- - 14 - 2 1 9304 6
weight of the substrate; it is found that methacrylic
acid polymers provide no significant improvement in the
stain resistance of the wool substrates, in the present
invention.
When using sulfonated novolak resin on nylon 66
substrate the amount of resin is preferably at least 0.01
weight percent, the amount of the methacrylic acid
polymer, if employed, is about at least 0.06 weight
percent, and the amount of the mixture of acid and metal
compound is at least 0.10 weight percent, based on the
weight of substrate.
When the substrate is nylon 6, the sulfonated
novolak resin is suitably in an amount of at least 0.02
weight percent, the amount of the methacrylic acid
polymer, if employed, is at least 0.12 weight percent,
and the amount of the mixture of acid and metal compound
is at least 0.02 weight percent, based on the weight of
the substrate.
vi) Application
The treatment of the fibrous polyamide or wool
substrate can be by different known methods to achieve
higher stain resistance, durability or wash fastness and
improved light fastness. The results may vary depending
upon the method of application. Usually the stain resist
can be applied to carpet by the following methods:
1. Exhaust method at a fiber to water ratio
between 1:10 and 1:50, preferably between
1:10 and 1:30; the carpet is usually treated
for between 20 to 30 minutes at 160 to 170~F,
2. Spray method in which the stain resist is
sprayed in combination with fluorochemicals
and other agents, for example, as soil
release or soil resist agents or antistatic
agents.
In this case, the substrate usually contains
- 15 - 2 1 5 30 4 6
between 30 to 50% humidity, and, the stain
resist and the other additives are sprayed
on the carpet, the carpet is dried and then
cured without steaming.
3. Continuous Method:
This can be carried out in two different
techniques:
a) Pad with 200 to 400%, by weight, pick
up, steam for 2 to 3 minutes, light
rinse then normal dry.
b) The solution of the stain resist is
passed through the carpet to improve
the penetration with a pick-up between
200 and 400%, by weight, the carpet is
steamed for about 3 minutes, followed
by a light rinse and drying.
In all methods the solution of stain resist can
be applied at cold or hot temperatures preferably hot.
vii) Substrate
The substrates employed in the invention are
fibrous polyamide or wool substrates. The substrate may
be in the form of fibers, yarns or fabrics; the invention
has particular value for the case in which the substrate
is a carpet, for example, household carpet, commercial
and industrial carpet or automotive carpet.
The following Examples illustrate the invention
employing stain resist and different formulations,
combinations or acid and metal compound mixtures and
other common products used in the industry.
EXAMPLES
The carpet samples used in this illustration
are of untreated white nylon 6 or nylon 66. The first
evaluation method was done by padding where the carpet
sample was immersed in a solution of the stain resist at
a pH 2. The pad pick-up on the carpet was 350%, by
- 16 - 2193046
weight, of the untreated carpet. The carpet was steamed
for 3 minutes at 110~C or higher without any pressure,
washed lightly, squeezed then dried.
The second evaluation method was done by the
exhaust method in which the carpet sample was weighed,
immersed in a solution of the stain resist with a fiber
to water ratio of 1:20, the carpet sample was treated for
20 minutes at a temperature of 170~F and at a pH of 2,
the carpet sample was then rinsed, squeezed and dried.
I 0 StA ~ n ~ ng Test:
The first staining test employs a staining test
solution of the sweetened cherry soft drink KOOLAID
(Trade Mark). The solution was made by diluting 100g of
KOOLAID in one liter of water. The treated carpet
samples were stained with 20 g of the prepared test
solution and kept for 16 hours at room temperature, then
rinsed for evaluation. The samples were evaluated for
staining on a graduated scale from 1 to 8 wherein 1
represents complete staining and 8 represents complete
non-staining of the carpeti usually a stain resistance
rating of 5 is considered acceptable, 7 is very good, 8
is excellent resistance to staining.
Light Test:
The light test in this invention was made
according to the light test method in the AATCC Test Book
No. 1 GE 1978 for 40 hours under a xenon arc lamp. The
sample exposed to ultraviolet light is evaluated for
light fastness according to a graduated rating scale
which ranges from 1 to 5 where rate 5 represents non-
yellowing and 1 is very poor with severe yellowing, ingeneral 4.5 is excellent and 4 is acceptable.
Wash Test:
The wash test was carried out using 0.1 g/L
anionic soap, the solution was adjusted to pH 10 with
trisodium phosphate. The treated carpet sample was
- 17 - 2~93046
exposed to this solution for 5 minutes at 40~C, rinsed,
dried and stained as mentioned above.
The sulfonated resins used to treat the carpet
test samples were then as follows:
1. Sulfonated resol resin as described in this
invention.
2. FX-661 (Trade Mark) a commercially available
aqueous solution from Minnesota Mining Manu-
facturing Co., based on novolak resin and a
methacrylic acid copolymer.
3. A resin formed by condensing formaldehyde with
dihydroxydiphenyl sulfone and phenol sulfonic
acid, the ratio of dihydroxydiphenyl sulfone
to the phenol sulfonic acid is 30 to 70, the
concentration, in weight %, of the novolak
resin, the remainder being water, is 40%.
The methacrylic acid polymer used for
evaluation has a weight average molecular weight of
6,000, the concentration, in weight %, in water, of the
resin is 30%; the resin is available from Rohm & Haas
under the Trade Mark LEUKOTAN 970.
Evaluation is then made by the stain test
evaluation in which the stain is evaluated after washing
on the scale of 1 to 8 as described for the staining
test.
The additional agents used in the Examples
were:
1) Product A which consists of:
65% Phosphoric Acid 85%
15% Magnesium Phosphate
5% Aluminum Potassium Phosphate
15% Water.
- 18 - 2 1 9~04 6
All the ingredients are added and the
temperature of the mix is raised, the mix is stirred
until the salt is completely dissolved.
2) Product B which consists of:
65% Phosphoric Acid 85%
15% Magnesium Phosphate
3% Copper Sulfate
17% Water.
The ingredients are mixed as for product A.
3) Magnesium sulfate.
4) Magna Flo II (Trade Mark of Sybron Chemical)
5) Tanacid PC (Trade Mark of Sybron Chemical)
6) Sulfamic Acid.
7) Product C which consists of:
24% Water
10% Aluminum Potassium Sulfate
20% Magnesium Sulfate
1.0% Copper Sulfate
5% Polyphosphoric Acid
40% Sulfuric Acid 66 B.
The above % are in weight %.
Table #l shows the formulations of the
invention and comparison formulations.
Table #2 shows the test results for the
different formulations.
TABLE ~1
A ~plication cr. Nylon 6
Formulations g/L 1 3 4 ~ 6 7 S 9 10 11 1' 13 . 1~ 15
Sulfonated Resol Resin
6070 i.l l.l l.l l.l 1.1
~lethylmethacrylate
copolymer 40000mtv '~ ~c 10 . 5 10 . 5 10 . 5 10 . 5 10 . 5 10 . 5 10 . 510 . 5 10 . 5 10 . 5
ac~ive
FX 661 12 1212 12 12
SR~00
Sulfonated Novola}; resin
4oao 1 ~ 1.5 1.5 1.5 1.5 ~O
Sulfamic acid ~ ~ ,
~ oSil1m sulfate
Tan~cid PC ' 2 2
~Iagnaflo II 3 3
Product A
Product B
Produc~ C
Final pH of the padding
bath 2.1 2.1 2.2 2 2 _. ~ .~ 1.9-~.0 ~.0 2.0 2.0 1.9
- 20 - 2193046
U' CC~ V' ~
-rC,3 V~ ~
r
r ~ oc V, '~
V~
00
r
C ~ ~
r ~ ~ r~ t~)
o
~:1 r U C
- 21 - 2 ~ 93046
The results on Table 2 show that by applying
different additives the results of the stain resist, the
light fastness and the durability to wash behaves
differently. It is clear that by using Product A, B or
C, better light fastness is obtained, in addition to
superior stain resistance and durability to wash.
Also it was observed that complete non-
yellowing of the fiber and better whiteness is obtained
by using Product A, B or C.
The above formulations show the importance of
having the Product A, B or C in the solution of stain
blocker to optimize the performance and the durability.
EXAMPLE #2
The following stain blocker formulations set
out in Table 3 were applied to untreated white polyamide
(Nylon 66) carpet samples using the padding method
explained hereinbefore; and Table 4 shows the test
results.
~AgLE ~3 .~lon 66
Formul~tions ~/L 13 1~ 1~ 16 17 IS 19 '0 ~1 77 ~3 ~ 6 ~7 ~S '9 30
Sulfonaled Resol Resin 60
0 50.50.5 0.5 0.
Meth~ Ime~hacr~ lale copol~ mer higher
stain 40000mw 4 5.5
F~ 661 3M stain blocker 5 5 5 5
SR~00 ~uPont stain blocker Io lo lo lo 5 10 5 10
Sulfamic acid 3 ; ; 3
!~far~nesium suifale Epsom Salt 3
Tanacid ; 3 3
~fa~naflo 11 3 3 3
Product A
Product B I ~ 1 1
Product C
Final pH of the paddin~ bathl.9 l.9 1.9 ~ .0 ~.1 '.0I.S5 1.85 3.0 '.0 1.S5 l.S5 '.0 '.0 1 9 1.95 1.9 C3
-23- 2793~46
t~ t
t~' t~o -t
' t ~~
7 'D
~'~ ~ t ~--
~,, ~ -r ~o
-t " ~
''~ t~ ~ In
~'
r '' '~ 't ~,
tx~vl
-- ~r 'J
V) y
-- ~-- --'t v )
t' ~ ~ r -t
t~ ", V)
~t C~ 't
t ~
C~ -- O
C r~ C L~ ~
Ot~
~~ - 24 - 2193046
In Table 4 the formulations 13 to 30 shows that
Products A, B and C improve the light fastness and the
durability to wash in addition to the improvement in
stain resistance after washing.
It is believed that the Products A, B or C in
combination with stain blocker will change many
conventional methods in the industry and will overcome
the light fastness and the yellowing problems of nylon
fibers. In addition these products provide improvement
of the stain resistance itself and the wash durability,
and also the handling of the product.
Example #3
Table 5 shows different formulations of the
invention employing a stain blocker available from Dupont
under the Trade Mark SR400.
Results are shown in Table 6.
TABLE # 5
Formul~tions g/L ~8 '9 30 31 3' 33 31 3~ 36 37 38 39 ~iO
SR400 l~ 1' I' 6 6 I' 6 l~ 6 6
SulfJmic acid 3 3
Magnesium sulfate 3
Epsom Salt
Tanacid 3 3 , ~"
Ma6naflo l~ 3
Product A ~ 6 G
Product B ~ 6 6
Product C 4 0 4 . 0
pH ofthe l.9 I.S5 1.9 1.~5 ~.0 1.91.~5'.0 1.9 1.~5 1.9 1.9 1.95 I'V
paddinl~ bath
C~
21 93346
- -- 26
o C')
-t
CO V~
Vl
t~ ~ V~ -t
'~
-t ~/1
~n ~ v~
~ --t ~"
--r ~ ,,,
t ~ )
~O ~ ~r '~I
P ~ 't 'r)
~ ~ --t
O 0~
~ ~ 't
O~ 00 ~ ~
~'J ~ t
0:, 0~ -r
~ ~ , ~
~ v~ ~ c~ 3
21 ~3~6
- 27 ~
By means of the invention it is possible to
obtain treated dyed fibrous polyamide or wool substrate,
especially carpets, having a stain resistance of at least
5, typically at least 7 on a scale of 1 to 8, a light
fastness as determined by non-yellowing of at least 4 on
a scale of 1 to 5, by the first staining test and the
light fastness test described hereinbefore. Furthermore,
the stain resistance of at least 5 is maintained after 1
to 5 washings of the substrate, demonstrating the
durability or wash fastness of the stain resistance
provided by the invention.
In this Specification % and ratios are by
weight unless otherwise indicated.
