U.S. patent application number 15/764914 was filed with the patent office on 2018-11-08 for carpet with hydrophobic surface finish.
The applicant listed for this patent is THE CHEMOURS COMPANY FC, LLC. Invention is credited to Gerald Oronde BROWN, Edward Patrick CAREY, John Christopher SWOREN.
Application Number | 20180320309 15/764914 |
Document ID | / |
Family ID | 57133441 |
Filed Date | 2018-11-08 |
United States Patent
Application |
20180320309 |
Kind Code |
A1 |
BROWN; Gerald Oronde ; et
al. |
November 8, 2018 |
CARPET WITH HYDROPHOBIC SURFACE FINISH
Abstract
The present invention relates to a treated carpet comprising a
partial or complete coating on a carpet surface, wherein the
coating comprises 5 to 100% by weight of a hydrophobic compound,
based on the total weight of the coating, selected from a cyclic or
acyclic alcohol which is substituted with at least two hydrophobic
groups.
Inventors: |
BROWN; Gerald Oronde;
(Swedesboro, NJ) ; SWOREN; John Christopher;
(Lincoln University, PA) ; CAREY; Edward Patrick;
(Atglen, PA) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
THE CHEMOURS COMPANY FC, LLC |
Wilmington |
DE |
US |
|
|
Family ID: |
57133441 |
Appl. No.: |
15/764914 |
Filed: |
September 30, 2016 |
PCT Filed: |
September 30, 2016 |
PCT NO: |
PCT/US2016/054581 |
371 Date: |
March 30, 2018 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
|
62236357 |
Oct 2, 2015 |
|
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|
Current U.S.
Class: |
1/1 |
Current CPC
Class: |
D06M 2200/01 20130101;
D06M 23/08 20130101; D06M 23/10 20130101; D06M 2101/34 20130101;
D06M 2200/12 20130101; D06M 15/564 20130101; D06M 13/17 20130101;
D06M 13/224 20130101 |
International
Class: |
D06M 13/224 20060101
D06M013/224; D06M 13/17 20060101 D06M013/17; D06M 23/08 20060101
D06M023/08; D06M 15/564 20060101 D06M015/564; D06M 23/10 20060101
D06M023/10 |
Claims
1. A treated carpet comprising a partial or complete coating on a
carpet surface, wherein the carpet is made of natural fiber, nylon,
acrylic, aromatic polyamide, polyester, polyacrylonitrile, or
polyacrylonitrile copolymer, wherein the coating comprises 5 to
100% by weight of a hydrophobic compound, based on the total solids
weight of the coating, selected from a cyclic or acyclic alcohol
which is substituted with at least two --R.sup.1, --C(O)R.sup.1,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1,
or mixtures thereof; where the cyclic or acyclic alcohol is
selected from a pentaerythritol, a saccharide, reduced sugar,
aminosaccharide, citric acid, aldonic acid, or aldonic acid
lactone; wherein each n is independently 0 to 20; each m is
independently 0 to 20; m+n is greater than 0; each R.sup.1 is
independently a linear or branched alkyl group having 5 to 29
carbons optionally comprising at least 1 unsaturated bond; and each
R.sup.2 is independently --H, a linear or branched alkyl group
having 6 to 30 carbons optionally comprising at least 1 unsaturated
bond.
2. The treated carpet of claim 1, where the hydrophobic compound is
selected from Formulas (Ia), (Ib), or (Ic): ##STR00003## wherein
each R is independently --H; --R.sup.1; --C(O)R.sup.1;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
each n is independently 0 to 20; each m is independently 0 to 20;
m+n is greater than 0; r is 1 to 3; a is 0 or 1; p is independently
0 to 2; provided that a is 0 when r is 3; each R.sup.1 is
independently a linear or branched alkyl group having 5 to 29
carbons optionally comprising at least 1 unsaturated bond; each
R.sup.2 is independently --H, or a linear or branched alkyl group
having 6 to 30 carbons optionally comprising at least 1 unsaturated
bond; provided when Formula (Ia) is chosen, then at least one R is
--H and at least two R groups are a --R.sup.1; --C(O)R.sup.1;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
each R.sup.4 is independently --H, a linear or branched alkyl group
having 6 to 30 carbons optionally comprising at least 1 unsaturated
bond, or combinations thereof;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
provided when Formula (Ib) is chosen, then at least one R or
R.sup.4 is --H; and at least two of R or R.sup.4 are a linear or
branched alkyl group optionally comprising at least 1 unsaturated
bond, or combinations thereof;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
and each R.sup.19 is --H, --C(O)R.sup.1, or
--CH.sub.2C[CH.sub.2OR].sub.3, provided when Formula (Ic) is
chosen, then at least one R.sup.19 or R is --H; and at least two of
R.sup.19 or R are --C(O)R.sup.1,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1.
3. The treated carpet of claim 2, where the hydrophobic compound is
selected from Formula (Ia) to be Formula (Ia'): ##STR00004##
wherein R is further limited to independently --H; --R.sup.1; or
--C(O)R.sup.1.
4. The treated carpet of claim 2, where the hydrophobic compound is
selected from Formula (Ia) to be Formula (Ia'): ##STR00005##
wherein R is further limited to independently --H;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1.
5. The treated carpet of claim 2, where the hydrophobic compound is
selected from Formula (Ib).
6. The treated carpet of claim 1, where the coating further
comprises a hydrophobic surface effect agent.
7. The treated carpet of claim 6, wherein the surface effect is
shrinkage control, moisture control, softness, strength, anti-slip,
anti-static, anti-snag, anti-pill, stain repellency, stain release,
soil repellency, soil release, water repellency, oil repellency,
odor control, antimicrobial, sun protection, or acid
resistance.
8. The treated carpet of claim 6 wherein the hydrophobic surface
effect agent is selected from the group consisting of
non-fluorinated or fluorinated cationic acrylic polymers,
non-fluorinated or fluorinated anionic acrylic polymers,
non-fluorinated or fluorinated nonionic acrylic polymers, partially
fluorinated urethanes, hydrophobic non-fluorinated urethanes,
silicones, and waxes.
9. The treated carpet of claim 1, where the coating comprises 20 to
100% by weight of the hydrophobic compound, based on the total
solids weight of the coating.
10. The treated carpet of claim 1, where the coating comprises 50
to 100% of the hydrophobic compound, based on the total solids
weight of the coating.
11. The treated carpet of claim 10, where the coating comprises
100% of the hydrophobic compound, based on the total weight of the
coating.
12. A method of imparting a surface effect to a carpet comprising
contacting a carpet surface with a coating to form a partially or
completely treated carpet, wherein the carpet is made of natural
fiber, nylon, acrylic, aromatic polyamide, polyester,
polyacrylonitrile, or polyacrylonitrile copolymer, wherein the
coating comprises 5 to 100% by weight of a hydrophobic compound,
based on the total solids weight of the coating, selected from a
cyclic or acyclic alcohol which is substituted with at least two
--R.sup.1, --C(O)R.sup.1,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1,
or mixtures thereof; where the cyclic or acyclic alcohol is
selected from a pentaerythritol, saccharide, reduced sugar,
aminosaccharide, citric acid, aldonic acid, or aldonic acid
lactone; wherein each n is independently 0 to 20; each m is
independently 0 to 20; m+n is greater than 0; each R.sup.1 is
independently a linear or branched alkyl group having 5 to 29
carbons optionally comprising at least 1 unsaturated bond; and each
R.sup.2 is independently --H, a linear or branched alkyl group
having 6 to 30 carbons optionally comprising at least 1 unsaturated
bond.
13. The method of claim 12, where the hydrophobic compound is
selected from Formulas (Ia), (Ib), or (Ic): ##STR00006## wherein
each R is independently --H; --R.sup.1; --C(O)R.sup.1;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
each n is independently 0 to 20; each m is independently 0 to 20;
m+n is greater than 0; r is 1 to 3; a is 0 or 1; p is independently
0 to 2; provided that a is 0 when r is 3; each R.sup.1 is
independently a linear or branched alkyl group having 5 to 29
carbons optionally comprising at least 1 unsaturated bond; each
R.sup.2 is independently --H, or a linear or branched alkyl group
having 6 to 30 carbons optionally comprising at least 1 unsaturated
bond; provided when Formula (Ia) is chosen, then at least one R is
--H and at least two R groups are a --R.sup.1; --C(O)R.sup.1;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
each R.sup.4 is independently --H, a linear or branched alkyl group
having 6 to 30 carbons optionally comprising at least 1 unsaturated
bond, or combinations thereof;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
provided when Formula (Ib) is chosen, then at least one R or
R.sup.4 is --H; and at least two of R or R.sup.4 are a linear or
branched alkyl group optionally comprising at least 1 unsaturated
bond, or combinations thereof;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
and each R.sup.19 is --H, --C(O)R.sup.1, or
--CH.sub.2C[CH.sub.2OR].sub.3, provided when Formula (Ic) is
chosen, then at least one R.sup.19 or R is --H; and at least two of
R.sup.19 or R are --C(O)R.sup.1,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1.
14. The method of claim 12, further comprising the step of heating
the partially or completely treated carpet.
15. The method of claim 12, further comprising the step of
solidifying the coating by drying, cooling, or allowing to
cool.
16. The method of claim 12, where the contacting step occurs by
spraying, rolling, padding, brushing, sprinkling, dipping,
dripping, tumbling, or screen printing.
Description
FIELD OF THE INVENTION
[0001] Hydrophobic substituted alcohols are employed in surface
finish coatings to provide surface effects to carpet articles.
BACKGROUND OF THE INVENTION
[0002] Various compositions are known to be useful as treating
agents to provide surface effects to substrates. Surface effects
include repellency to moisture, soil and stain resistance, and
other effects which are particularly useful for fibrous substrates
such as fibers, fabrics, textiles, carpets, paper, leather and
other such substrates. Many such treating agents are partially
fluorinated polymers or copolymers.
[0003] Fluorinated polymer compositions having utility as fibrous
substrate treating agents generally contain pendant perfluoroalkyl
groups of three or more carbon atoms, which provide oil- and
water-repellency when the compositions are applied to fibrous
substrate surfaces. The perfluoroalkyl groups are generally
attached by various connecting groups to polymerizable groups not
containing fluorine. The resulting monomer is then generally
copolymerized with other monomers which confer additional favorable
properties to the substrates. Various specialized monomers may be
incorporated to impart improved cross-linking, latex stability and
substantivity. Since each ingredient may impart some potentially
undesirable properties in addition to its desirable ones, the
specific combination is directed to the desired use. These polymers
are generally marketed as aqueous emulsions for easy application to
the fibrous substrates.
[0004] Various attempts have been made to increase the oil- and
water-repellency imparted to the substrate and its durability while
reducing the amount of fluorinated polymer required, i.e., boost
the efficiency or performance of the treating agent. One method is
to incorporate blocked isocyanates or melamine resins. However,
only limited amounts can be used because these ingredients tend to
adversely affect the handle (the feel) of the fibrous substrate.
Another approach employs use of various extender polymers. These
are typically hydrocarbon polymers in aqueous emulsions, which are
blended with the fluorinated polymer emulsion before application to
the substrate.
[0005] U.S. Pat. No. 7,820,745 discloses aqueous water- and
oil-repellent compositions containing a fluorinated copolymer in
aqueous medium and a sorbitan ester used in small amounts to act as
a surfactant. The reference does not, however, show the surface
effect benefits of using hydrophobic sorbitan esters or other
hydrophobic ester alcohol compounds on carpet substrates.
BRIEF SUMMARY OF THE INVENTION
[0006] There is a need for surface effect compositions which
provide hydrophobicity performance to carpet with improved fluorine
efficiency. The present invention provides such a composition.
[0007] The present invention comprises a treated carpet comprising
a partial or complete coating on a carpet surface, wherein the
carpet is made of natural fibers, nylon, acrylics, aromatic
polyamides, polyesters, polyacrylonitrile, or polyacrylonitrile
copolymers, wherein the coating comprises 5 to 100% by weight of a
hydrophobic compound, based on the total solids weight of the
coating, selected from a cyclic or acyclic alcohol which is
substituted with at least two --R.sup.1, --C(O)R.sup.1,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1,
or mixtures thereof; where the cyclic or acyclic alcohol is
selected from a pentaerythritol, a saccharide, reduced sugar,
aminosaccharide, citric acid, aldonic acid, or aldonic acid
lactone; wherein each n is independently 0 to 20; each m is
independently 0 to 20; m+n is greater than 0; each R.sup.1 is
independently a linear or branched alkyl group having 5 to 29
carbons optionally comprising at least 1 unsaturated bond; and each
R.sup.2 is independently --H, a linear or branched alkyl group
having 6 to 30 carbons optionally comprising at least 1 unsaturated
bond.
[0008] The present invention further comprises a method of
imparting a surface effect to a carpet comprising contacting a
carpet surface with a coating to form a partially or completely
treated carpet, wherein the carpet is made of natural fibers,
nylon, acrylics, aromatic polyamides, polyesters,
polyacrylonitrile, or polyacrylonitrile copolymers, wherein the
coating comprises 5 to 100% by weight of a hydrophobic compound,
based on the total solids weight of the coating, selected from a
cyclic or acyclic alcohol which is substituted with at least two
--R.sup.1, --C(O)R.sup.1,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1,
or mixtures thereof; where the cyclic or acyclic alcohol is
selected from a pentaerythritol, saccharide, reduced sugar,
aminosaccharide, citric acid, aldonic acid, or aldonic acid
lactone; wherein each n is independently 0 to 20; each m is
independently 0 to 20; m+n is greater than 0; each R.sup.1 is
independently a linear or branched alkyl group having 5 to 29
carbons optionally comprising at least 1 unsaturated bond; each
R.sup.2 is independently --H, a linear or branched alkyl group
having 6 to 30 carbons optionally comprising at least 1 unsaturated
bond.
DETAILED DESCRIPTION OF THE INVENTION
[0009] Trademarks are indicated herein by capitalization.
[0010] The present invention provides treated carpet articles
having improved water repellency, oil or stain repellency, and/or
other surface effects. The treated articles provide enhanced
performance compared to traditional non-fluorinated commercially
available treatment agents. The coating materials of the present
invention can be derived from bio-sourced materials. The coatings
formed are durable, by which is meant that the coatings are lasting
films that are not readily removed by water or cleaning agents. In
one aspect, the coatings are not soluble or dispersable in water or
cleaning agents once they are dry, and in another aspect, the
coatings withstand multiple cleanings without loss of
performance.
[0011] The present invention comprises a treated carpet comprising
a partial or complete coating on a carpet surface, wherein the
carpet is made of natural fibers, nylon, acrylics, aromatic
polyamides, polyesters, polyacrylonitrile, or polyacrylonitrile
copolymers, wherein the coating comprises 5 to 100% by weight of a
hydrophobic compound, based on the total solids weight of the
coating, selected from a cyclic or acyclic alcohol which is
substituted with at least two --R.sup.1, --C(O)R.sup.1,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1,
or mixtures thereof; where the cyclic or acyclic alcohol is
selected from a pentaerythritol, a saccharide, reduced sugar,
aminosaccharide, citric acid, aldonic acid, or aldonic acid
lactone; wherein each n is independently 0 to 20; each m is
independently 0 to 20; m+n is greater than 0; each R.sup.1 is
independently a linear or branched alkyl group having 5 to 29
carbons optionally comprising at least 1 unsaturated bond; and each
R.sup.2 is independently --H, a linear or branched alkyl group
having 6 to 30 carbons optionally comprising at least 1 unsaturated
bond. These hydrophobic compounds can contain only EO groups, only
PO groups, or mixtures thereof. These compounds can also be present
as a tri-block copolymer designated PEG-PPG-PEG (polyethylene
glycol-polypropylene glycol-polyethylene glycol), for example. In
one embodiment, n+m is 1 to 20; in another embodiment, n and m are
independently 0 to 15 and n+m is 1 to 15; and in a third
embodiment, n and m are independently 0 to 12 and n+m is 1 to
12.
[0012] The hydrophobic compound may be a multi-ester alcohol having
at least two hydrophobic substitutions, which originates from a
polyol or polycarboxylic acid compound. Examples of suitable
polyols include but are not limited to cyclic or acyclic sugar
alcohols, or pentaerythritols including dipentaerythritol. Suitable
polycarboxylic acid compounds include citric acid. The cyclic or
acyclic sugar alcohol is selected from a saccharide, reduced sugar,
aminosaccharide, aldonic acid, aldonic acid lactone. Mixtures of
these compounds may also be used. The hydrophobic compounds are
substituted with at least two --R.sup.1; --C(O)R.sup.1;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
or mixtures thereof. Such a substitution lends hydrophobic
character to the monomer, and to the polymer molecules. In one
embodiment, the hydrophobic compound is substituted with at least
three --R.sup.1; --C(O)R.sup.1;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
or mixtures thereof.
[0013] These substituted compounds can be made by the reaction of a
sugar alcohol with at least one fatty acid or alkoxylated fatty
acid, such as by esterification of a fatty acid; or by
esterification of a polycarboxylic acid with a long-chain alcohol.
Examples of such sugar alcohols include but are not limited to
aldoses and ketoses such as those compounds derived from tetroses,
pentoses, hexoses, and heptoses. Specific examples include glucose,
1,4-anhydro-D-glucitol, 2,5-anhydro-D-mannitol,
2,5-anhydro-L-iditol, isosorbide, sorbitan, glyceraldehyde,
erythrose, threitol, glucopyranose, mannopyranose, talopyranose,
allopyranose, altropyranose, idopyranose, gulopyranose, glucitol,
mannitol, erythritol, sorbitol, arabitol, xylitol, ribitol,
galactitol, fucitol, iditol, inositol, pentaerythritol,
dipentaerythritol, volemitol, gluconic acid, glyceric acid, xylonic
acid, galactaric acid, ascorbic acid, citric acid, gluconic acid
lactone, glyceric acid lactone, xylonic acid lactone, glucosamine,
galactosamine, or mixtures thereof.
[0014] Suitable fatty acids include, but are not limited to,
caprylic acid, capric acid, lauric acid, mysteric acid, palmitic
acid, stearic acid, arachidic acid, behenic acid, lignoceric acid,
palmitoleic acid, lineolic acid, oleic acid, erucic acid,
alkoxylated versions of these acids, and mixtures thereof.
[0015] In one embodiment, R.sup.1 is a linear or branched alkyl
group having 11 to 29 carbons, and in another embodiment, R.sup.1
is a linear or branched alkyl group having 17 to 21 carbons. In one
embodiment, R.sup.2 is a linear or branched alkyl group having 12
to 30 carbons, in another embodiment, R.sup.2 is a linear or
branched alkyl group having 18 to 30 carbons, and in another
embodiment, R.sup.2 is a linear or branched alkyl group having 18
to 22 carbons. In one embodiment, the fatty acid or long-chain
alcohol substitution of the cyclic or acyclic sugar alcohols has a
melting point of at least -59.degree. C. In another embodiment, it
has a melting point of at least 0.degree. C., and in a third
embodiment, it has a melting point of at least 40.degree. C.
[0016] In one embodiment, the hydrophobic compound is selected from
Formulas (Ia), (Ib), or (Ic):
##STR00001##
wherein each R is independently --H; --R.sup.1; --C(O)R.sup.1;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
each n is independently 0 to 20; each m is independently 0 to 20;
m+n is greater than 0; r is 1 to 3; a is 0 or 1; p is independently
0 to 2; provided that a is 0 when r is 3; each R.sup.1 is
independently a linear or branched alkyl group having 5 to 29
carbons optionally comprising at least 1 unsaturated bond; each
R.sup.2 is independently --H, or a linear or branched alkyl group
having 6 to 30 carbons optionally comprising at least 1 unsaturated
bond; provided when Formula (Ia) is chosen, then at least one R is
--H and at least one R is a --R.sup.1; --C(O)R.sup.1;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
each R.sup.4 is independently --H, a linear or branched alkyl group
having 6 to 30 carbons optionally comprising at least 1 unsaturated
bond, or combinations thereof;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
provided when Formula (Ib) is chosen, then at least one R or
R.sup.4 is --H; and at least two of R or R.sup.4 are a linear or
branched alkyl group optionally comprising at least 1 unsaturated
bond, or combinations thereof;
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1;
and each R.sup.19 is --H, --C(O)R.sup.1, or
--CH.sub.2C[CH.sub.2OR].sub.3, provided when Formula (Ic) is
chosen, then at least one R.sup.19 or R is --H; and at least two of
R.sup.19 or R are --C(O)R.sup.1,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1.
[0017] Where the hydrophobic compound is Formula (Ia), any suitable
substituted reduced sugar alcohol may be employed, including esters
of 1,4-sorbitan, esters of 2,5-sorbitan, and esters of
3,6-sorbitan. In one embodiment, the hydrophobic compound is
selected from Formula (a) to be Formula (Ia'):
##STR00002##
wherein R is further limited to --H; --R.sup.1; or --C(O)R.sup.1
and at least two R groups are --C(O)R.sup.1 or R.sup.1. Compounds
used to form residues of Formula (Ia'), having at least one of R is
--H and at least one R is selected from --C(O)R.sup.1, are commonly
known as alkyl sorbitans. These sorbitans can be di-substituted or
tri-substituted with --C(O)R.sup.1. It is known that commercially
available sorbitans, such as SPAN, contain a mixture of the various
sorbitans ranging from where each R is H (un-substituted), and
sorbitans where each R is --C(O)R.sup.1 (fully substituted);
wherein R.sup.1 is a linear or branched alkyl group having 5 to 29
carbons; and mixtures of various substitutions thereof. The
commercially available sorbitans may also include amounts of
sorbitol, isosorbide, or other intermediates or byproducts.
[0018] In one embodiment, at least two R groups are --C(O)R.sup.1,
and R.sup.1 is a linear branched alkyl group having 5 to 29
carbons. In another embodiment, R.sup.1 is a linear or branched
alkyl group having 7 to 21 carbons, and in a third embodiment,
R.sup.1 is a linear or branched alkyl group having 11 to 21
carbons. Preferred compounds used to form these residues include
mono-, di-, and tri-substituted sorbitans derived from caprylic
acid, capric acid, lauric acid, mysteric acid, palmitic acid,
stearic acid, arachidic acid, behenic acid, lignoceric acid, and
mixtures thereof. Particularly preferred compounds include di- and
tri-substituted sorbitan stearates or sorbitan behenins.
[0019] Optionally, R.sup.1 is a linear or branched alkyl group
having 5 to 29 carbons comprising at least 1 unsaturated bond.
Examples of compounds of Formula (Ia) wherein at least two R groups
are selected from --C(O)R.sup.1; and R.sup.1 contains least 1
unsaturated bond, include, but are not limited to, sorbitan
trioleate (i.e., wherein R.sup.1 is
--C.sub.7H.sub.14CH.dbd.CHC.sub.8H.sub.17). Other examples but are
not limited to include di- and tri-substituted sorbitans derived
from palmitoleic acid, lineolic acid, arachidonic acid, and erucic
acid.
[0020] In one embodiment, a compound of Formula (Ia) is employed,
wherein at least two R groups are independently
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2 or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1.
Compounds of Formula (Ia), wherein at least two R groups are
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2 or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1,
wherein each m is independently 0 to 20, each n is independently 0
to 20, and n+m is greater than 0 are known as polysorbates and are
commercially available under the tradename TWEEN. These
polysorbates can be di-substituted or tri-substituted with alkyl
groups R.sup.1 or R.sup.2. It is known that commercially available
polysorbates contain a mixture of the various polysorbates ranging
from where each R.sup.2 is H (unsubstituted), and polysorbates
where each R.sup.1 is a linear or branched alkyl group having 5 to
29 carbons (fully substituted); and mixtures of various
substitutions thereof. Examples of compounds of Formula (Ia)
include polysorbates such as polysorbate tristearate and
polysorbate monostearate. Examples of compounds of Formula (Ia)
wherein m+n is greater than 0, and wherein R.sup.1 comprises at
least 1 unsaturated bond, but not limited to, polysorbate trioleate
(wherein R.sup.1 is C.sub.7H.sub.14CH.dbd.CHC.sub.8H.sub.17) and
are sold commercially under the name Polysorbate 80. Reagents may
include mixtures of compounds having various values for R, R.sup.1,
and R.sup.2, and may also include mixtures of compounds where
R.sup.1 comprises at least one unsaturated bond with compounds
where R.sup.1 is fully saturated.
[0021] Compounds of Formula (Ib) are known as alkyl citrates. These
citrates can be present as a di-substituted or tri-substituted with
alkyl groups. It is known that commercially available citrates
contain a mixture of the various citrates as well as citric acids
from where R and each R.sup.4 is --H, ranging to citrates where
each R.sup.4 is a linear or branched alkyl group having 6 to 30
carbons optionally comprising at least 1 unsaturated bond; and
mixtures of various substitutions thereof. Mixtures of citrates
having various values for R.sup.1, R.sup.2, and R.sup.4 may be
used, and may also include mixtures of compounds where R.sup.1
comprises at least one unsaturated bond with compounds where
R.sup.1 is fully saturated. Alkyl citrates are also commercially
available wherein m+n is greater than 0, R.sup.4 is
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2; or
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1
and are present in the various substitutions from wherein R and
each R.sup.2 is H to wherein each R.sup.1 and/or R.sup.2 is a
linear or branched alkyl group having 5 to 30 carbons optionally
comprising at least 1 unsaturated bond. Examples of compounds of
Formula (Ib) include, but are not limited to, trialkyl
citrates.
[0022] Compounds of Formula (Ic) are known as pentaerythriol
esters. These pentaerythriol esters can be present as a
di-substituted or tri-substituted with alkyl groups. Preferred
compounds used to form X of Formula (Ic) are dipentaerythriol
esters, where R.sup.19 is --CH.sub.2C[CH.sub.2OR].sub.3. It is
known that commercially available pentaerythriol esters contain a
mixture of the various pentaerythriol esters where R.sup.19 and
each R is --H, ranging to pentaerythriol esters where each R is
--C(O)R.sup.1, and R.sup.1 is a linear or branched alkyl group
having 5 to 29 carbons optionally comprising at least 1 unsaturated
bond; and mixtures of various substitutions thereof. The
pentaerythriol esters also may contain compounds with mixtures of
different chain lengths for R, or mixtures of compounds where
R.sup.1 comprises at least one unsaturated bond with compounds
where R.sup.1 is fully saturated.
[0023] Compounds of Formulas (Ia), (Ib), and (Ic) can all be
bio-based derived. By "bio-based derived", it is meant that at
least 10% of the material can be produced from non-crude oil
sources, such as plants, other vegetation, and tallow. In one
embodiment, the hydrophobic compound is from about 10% to 100%
bio-based derived. In one embodiment, hydrophobic compound is from
about 35% to 100% bio-based derived. In another embodiment,
hydrophobic compound is from about 50% to 100% bio-based derived.
In one embodiment, hydrophobic compound is from about 75% to 100%
bio-based derived. In one embodiment, hydrophobic compound is 100%
bio-based derived. The average OH value of the hydrophobic
compounds can range from just greater than 0 to about 230. In one
embodiment, the average OH value is from about 10 to about 175, and
in another embodiment, the average OH value is from about 25 to
about 140.
[0024] The coating on the carpet surface comprises 5 to 100% by
weight of the hydrophobic compound, based on the total solids
weight of the coating. In a second aspect, the coating on the
carpet surface comprises 20 to 100% by weight of the hydrophobic
compound; and in a third aspect, 50 to 100% by weight of the
hydrophobic compound based on the total solids weight of the
coating. The term "solids weight of the coating", is used to mean
the sum of the coating components that would remain once the
aqueous, solvent, or other liquid components evaporated. In other
words, it is the sum of the non-aqueous, non-solvent, and
non-volatile components of the coating. The coating may further
comprise aqueous or organic solvents, polymer resins, coating bases
that contain polymer resins, pigments, functional additives,
surfactants, and hydrophobic surface effect agents.
[0025] In one embodiment, the hydrophobic compound is combined with
a hydrophobic surface effect agent to extend or improve the
performance of the surface effect agent. In this case, the
hydrophobic surface effect agents may be used from about 5:95 to
about 95:5 in one aspect; from about 10:90 to 90:10 in a second
aspect; and from about 20:80 to 80:10 in a third aspect, based on
the total solids weight of the coating. Hydrophobic surface effect
agents provide surface effects such as no iron, easy to iron,
shrinkage control, wrinkle free, permanent press, moisture control,
softness, strength, anti-slip, anti-static, anti-snag, anti-pill,
stain repellency, stain release, soil repellency, soil release,
water repellency, oil repellency, odor control, antimicrobial, sun
protection, and similar effects. Such materials can be in the form
of hydrophobic non-fluorinated cationic acrylic polymers,
hydrophobic non-fluorinated anionic acrylic polymers, hydrophobic
non-fluorinated nonionic acrylic polymers, partially fluorinated
urethanes, hydrophobic non-fluorinated urethanes, cationic
partially fluorinated acrylic polymers or copolymers, nonionic
partially fluorinated acrylic polymers or copolymers, partially
fluorinated acrylamide polymers or copolymers, fluorinated
phosphates, fluorinated or non-fluorinated organosilanes,
silicones, waxes, including parafins, and mixtures thereof. Some
stain release and soil release agents are hydrophilic and include
compounds such as polymethyl acrylates. These compounds may also be
combined with the hydrophobic compounds, in the ratios stated
above, as surface effect agents.
[0026] Superior properties, along with desirable properties of low
yellowing and good durability, are imparted to articles by the
combination of the hydrophobic compounds to hydrophobic surface
effect agents before application to the articles. These combined
blends are applied to the articles in the form of a dispersion in
water or other solvent either before, after or during the
application of other treatment chemicals.
[0027] Of particular interest are fluorinated polymers useful as
hydrophobic surface effect agents to provide repellency properties
to the surface of treated substrates. These include fluorochemical
compounds or polymers containing one or more fluoroaliphatic groups
(designated here as R.sub.f groups) which are fluorinated, stable,
inert, and non-polar, preferably saturated, monovalent, and both
oleophobic and hydrophobic. The R.sub.f groups contain at least 3
carbon atoms, preferably 3 to 20 carbon atoms, more preferably 4 to
12 carbon atoms, and most preferably about 4 to about 6 carbon
atoms. The R.sub.f groups may contain straight or branched chain or
cyclic fluorinated alkylene groups or combinations thereof. The
terminal portion of the R.sub.f groups is preferably a
perfluorinated aliphatic group of the formula C.sub.nF.sub.2n+1
wherein n is from about 3 to about 20. Examples of fluorinated
polymer treating agents are CAPSTONE and ZONYL available from The
Chemours Company, Wilmington, Del.; ASAHI GARD from Asahi Glass
Company, Ltd., Tokyo, Japan; UNIDYNE from Daikin America, Inc.,
Orangeburg, N.Y.; SCOTCHGARD from 3M Company, St. Paul, Minn.; and
NANO TEX from Nanotex, Emeryville, Calif.
[0028] Examples of such fluorinated polymers include
R.sub.f-containing polyurethanes and poly(meth)acrylates.
Especially preferred are copolymers of fluorochemical
(meth)acrylate monomers with a co-polymerizable monovinyl compound
or a conjugated diene. The co-polymerizable monovinyl compounds
include alkyl (meth)acrylates, vinyl esters of aliphatic acids,
styrene and alkyl styrene, vinyl halides, vinylidene halides, alkyl
esters, vinyl alkyl ketones, and acrylamides. The conjugated dienes
are preferably 1,3-butadienes. Representative compounds within the
preceding classes include the methyl, propyl, butyl,
2-hydroxypropyl, 2-hydroxyethyl, isoamyl, 2-ethylhexyl, octyl,
decyl, lauryl, cetyl, and octadecyl acrylates and methacrylates;
vinyl acetate, vinyl propionate, vinyl caprylate, vinyl laurate,
vinyl stearate, styrene, alpha methyl styrene, p-methylstyene,
vinyl fluoride, vinyl chloride, vinyl bromide, vinylidene fluoride,
vinylidene chloride, allyl heptanoate, allyl acetate, allyl
caprylate, allyl caproate, vinyl methyl ketone, vinyl ethyl ketone,
1,3-butadiene, 2-chloro-1,3-butadiene, 2,3-dichloro-1,3-butadiene,
isoprene, N-methylolacrylamide, N-methylolmethacrylamide, glycidyl
acrylate, glycidyl methacrylate, amine-terminated (meth)acrylates,
and polyoxy(meth)acrylates.
[0029] Hydrophobic non-fluorinated acrylic polymers include
copolymers of monovinyl compounds, including alkyl (meth)acrylates,
vinyl esters of aliphatic acids, styrene and alkyl styrene, vinyl
halides, vinylidene halides, alkyl esters, vinyl alkyl ketones, and
acrylamides. The conjugated dienes are preferably 1,3-butadienes.
Representative compounds within the preceding classes include the
methyl, propyl, butyl, 2-hydroxypropyl, 2-hydroxyethyl, isoamyl,
2-ethylhexyl, octyl, decyl, lauryl, cetyl, and octadecyl acrylates
and methacrylates; vinyl acetate, vinyl propionate, vinyl
caprylate, vinyl laurate, vinyl stearate, styrene, alpha methyl
styrene, p-methylstyene, vinyl fluoride, vinyl chloride, vinyl
bromide, vinylidene fluoride, vinylidene chloride, allyl
heptanoate, allyl acetate, allyl caprylate, allyl caproate, vinyl
methyl ketone, vinyl ethyl ketone, 1,3-butadiene,
2-chloro-1,3-butadiene, 2,3-dichloro-1,3-butadiene, isoprene,
N-methylolacrylamide, N-methylolmethacrylamide, glycidyl acrylate,
glycidyl methacrylate, amine-terminated (meth)acrylates, and
polyoxy(meth)acrylates.
[0030] Hydrophobic non-fluorinated urethanes include, for example,
urethanes synthesized by reacting an isocyanate compound with the
hydrophobic compounds described above as an alcohol reagent. These
compounds are described in US2014/0295724 and US2016/0090508.
Hydrophobic non-fluorinated nonionic acrylic polymers include, for
example, polymers made by polymerizing or copolymerizing an acrylic
ester of the hydrophobic compounds described above. Such compounds
are described in US2016/0090686.
[0031] The coatings of the present invention applied to the carpet
surface optionally further comprise a blocked isocyanate to promote
durability, added after copolymerization (i.e., as a blended
isocyanate). An example of a suitable blocked isocyanate is PHOBOL
XAN available from Huntsman Corp, Salt Lake City, Utah Other
commercially available blocked isocyanates are also suitable for
use herein. The desirability of adding a blocked isocyanate depends
on the particular application for the copolymer. For most of the
presently envisioned applications, it does not need to be present
to achieve satisfactory cross-linking between chains or bonding to
fibers. When added as a blended isocyanate, amounts up to about 20%
by weight are added.
[0032] The coating composition of the present invention optionally
further comprises additional components such as additional treating
agents or finishes to achieve additional surface effects, or
additives commonly used with such agents or finishes. Such
additional components comprise compounds or compositions that
provide surface effects such as no iron, easy to iron, shrinkage
control, wrinkle free, permanent press, moisture control, softness,
strength, anti-slip, anti-static, anti-snag, anti-pill, stain
repellency, stain release, soil repellency, soil release, water
repellency, oil repellency, odor control, antimicrobial, sun
protection, and similar effects. One or more such treating agents
or finishes can be combined with the blended composition and
applied to the fibrous substrate. Other additives commonly used
with such treating agents or finishes may also be present such as
surfactants, pH adjusters, cross linkers, wetting agents, and other
additives known by those skilled in the art. Further, other
extender compositions are optionally included to obtain a
combination of benefits.
[0033] In one embodiment, the present invention is method of
imparting a surface effect to a carpet comprising contacting a
carpet surface with a coating to form a partially or completely
treated carpet, wherein the carpet is made of natural fibers,
nylon, acrylics, aromatic polyamides, polyesters,
polyacrylonitrile, or polyacrylonitrile copolymers, wherein the
coating comprises 5 to 100% by weight of a hydrophobic compound,
based on the total solids weight of the coating, selected from a
cyclic or acyclic alcohol which is substituted with at least two
--R.sup.1, --C(O)R.sup.1,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mR.sup.2,
--(CH.sub.2CH.sub.2O).sub.n(CH(CH.sub.3)CH.sub.2O).sub.mC(O)R.sup.1,
or mixtures thereof; where the cyclic or acyclic alcohol is
selected from a pentaerythritol, saccharide, reduced sugar,
aminosaccharide, citric acid, aldonic acid, or aldonic acid
lactone; wherein each n is independently 0 to 20; each m is
independently 0 to 20; m+n is greater than 0; each R.sup.1 is
independently a linear or branched alkyl group having 5 to 29
carbons optionally comprising at least 1 unsaturated bond; each
R.sup.2 is independently --H, a linear or branched alkyl group
having 6 to 30 carbons optionally comprising at least 1 unsaturated
bond. Specific representative examples of carpet compositions
include but are not limited to natural fibers, such as cotton,
wool, silk, jute, sisal, and other cellulosics; nylon including
nylon 6, nylon 6,6 and aromatic polyamides; polyesters including
poly(ethyleneterephthalate) or poly(trimethyleneterephthalate) such
as Triexta; polyacrylonitrile or polyacrylonitrile copolymers. The
contacting step may occur by applying the hydrophobic compound as a
solid, or by liquid carrier. When applied by liquid carrier, the
hydrophobic compound may be in the form of an aqueous solution,
aqueous dispersion, organic solvent solution or dispersion, or
cosolvent solution or dispersion. The contacting step may occur by
any conventional method, including but not limited to spraying,
rolling, padding, brushing, sprinkling, dipping, dripping,
tumbling, screen printing, or other mechanical means known in the
technology to treat fibrous substrates.
[0034] In one aspect, the method further comprises the step of
heating the partially or completely coated carpet. For example, the
hydrophobic agent may be applied alone or in liquid carrier, and
the treated carpet may be heated to melt, flow, dry, or otherwise
fix the hydrophobic agent onto the carpet surface. The final
coating on the carpet surface will be a solidified, lasting,
permanent coating. In another aspect, the method further comprises
the step of solidifying the coating by drying, cooling, or allowing
to cool. In one embodiment, the solid hydrophobic compound is
sprinkled onto the carpet surface, and the treated carpet is heated
to fix the hydrophobic compound onto the surface. The liquid
carrier, if used, may be dried by heating or air drying to allow
for evaporation of the liquid carrier, thus leaving a permanent
solid coating.
[0035] Specifically, the treated carpets of the present invention
are useful for providing articles with enhanced surface properties,
especially durability of oil-, water- and soil-repellency, while
reducing or eliminating the amount of fluorinated compounds
employed. The repellency property is effective with a variety of
other surface effects.
TEST METHODS
[0036] All solvents and reagents, unless otherwise indicated, were
purchased from Sigma-Aldrich, St. Louis, Mo., and used directly as
supplied. Sorbitan tristearate was obtained from Croda, East
Yorkshire, England and DuPont Nutrition & Health, Copenhagen,
Denmark. WITCOLATE WAQE is available from Akzo Nobel, Chicago,
Ill.
[0037] The following tests were employed in evaluating the examples
herein.
Test Method 1--Accelerated Soiling Test
[0038] A drum mill (on rollers) was used to tumble synthetic soil
onto the carpet. Synthetic soil was prepared as described in AATCC
Test Method 123-2000, Section 8. Synthetic soil, 3 g, and 1 liter
of clean nylon resin beads ( 3/16 inch (0.32-0.48 cm) diameter
ZYTEL 101 nylon resin beads, commercially available from E. I. du
Pont de Nemours and Company, Wilmington, De., were placed into a
clean, empty canister. The canister lid was closed and sealed and
the canister rotated on rollers for 5 minutes. The soil-coated
beads were removed from the canister.
[0039] Total carpet sample size was 8.times.24 inch
(20.3.times.60.9 cm). One test item and one control item were
tested simultaneously. The carpet pile of all samples was laid in
the same direction. Strong adhesive tape was placed on the backside
of the carpet pieces to hold them together. The carpet samples were
placed in the clean, empty drum mill with the tufts facing toward
the center of the drum. The carpet was held in place in the drum
mill with rigid wires. Soil-coated resin beads, 250 ml, and 250 ml
of 5/16 in. diameter ball bearings (0.79 cm.), prepared as
described above, were placed into the drum mill. The drum mill lid
was closed and sealed. The drum was run on the rollers for 21/2
minutes at about 105 rpm. The rollers were stopped and the
direction of the drum mill reversed. The drum was run on the
rollers for an additional 21/2 minutes at about 105 rpm. The carpet
samples were removed and vacuumed uniformly with 5 passes in each
direction to remove excess dirt. The Delta (.DELTA.) E color
difference for the soiled carpet was measured for the test and
control items versus the unsoiled carpet for each item.
[0040] Color measurement of each carpet was conducted on the carpet
following the accelerated soiling test. For each test sample and
control sample the color of the carpet was measured, the sample was
soiled, and the color of the soiled carpet was measured. The
.DELTA. E was the difference between the color of the soiled and
unsoiled samples. Color difference was measured on each item, using
a Minolta Chroma Meter CR 410 (Minolta Corporation, Ramsey, N.J.).
Color readings were taken at three different areas on the carpet
sample, and the average .DELTA.E was recorded.
[0041] The control carpet for each test item was of the same color
and construction as the test item.
[0042] .DELTA. .DELTA. E was calculated by subtracting the .DELTA.
E of the control (untreated) carpet from the .DELTA. E of the test
item. A larger negative value for .DELTA. .DELTA. E indicated that
the test carpet had better performance and less soiling than the
control. A larger positive value for .DELTA. .DELTA. E indicated
that the test carpet had poorer performance and soiled more than
the control. Note that, although different untreated samples may
yield slightly different L ratings, the test samples are compared
to the untreated control sample that is tested simultaneously with
the test sample.
Test Method 2--Oil Repellency
[0043] Oil repellency was measured according to AATCC Test Method
118. Higher values indicate increased oil repellency.
[0044] The treated samples were tested for oil repellency by a
modification of AATCC standard Test Method No. 118, conducted as
follows. A substrate treated with an aqueous dispersion of polymer
as previously described, is conditioned for a minimum of 2 hours at
23 C and 20% relative humidity and 65 C and 10% relative humidity.
A series of organic liquids, identified below in Table 1, are then
applied dropwise to the samples. Beginning with the lowest numbered
test liquid (Repellency Rating No. 1), one drop (approximately 5 mm
in diameter or 0.05 mL volume) is placed on each of three locations
at least 5 mm apart. The drops are observed for 30 seconds. If, at
the end of this period, two of the three drops are still spherical
in shape with no wicking around the drops, three drops of the next
highest numbered liquid are placed on adjacent sites and similarly
observed for 30 seconds. The procedure is continued until one of
the test liquids results in two of the three drops failing to
remain spherical to hemispherical, or wetting or wicking
occurs.
[0045] The oil repellency rating is the highest numbered test
liquid for which two of the three drops remained spherical to
hemispherical, with no wicking for 30 seconds. In general, treated
samples with a rating of 5 or more are considered good to
excellent; samples having a rating of one or greater can be used in
certain applications.
TABLE-US-00001 TABLE 1 Oil Repellency Test Liquids Oil Repellency
Rating Test Solution 1 NUJOL Purified Mineral Oil 2 65/35
Nujol/n-hexadecane by volume at 21 C. 3 n-hexadecane 4
n-tetradecane 5 n-dodecane 6 n-decane 7 n-octane 8 n-heptane Note:
NUJOL is a trademark of Plough, Inc., for a mineral oil having a
Saybolt viscosity of 360/390 at 38 C. and a specific gravity of
0.880/0.900 at 15 C.
Test Method 3--Water Repellency
[0046] The water repellency of a treated substrate was measured
according to AATCC standard Test Method No. 193 and the DuPont
Technical Laboratory Method as outlined in the TEFLON Global
Specifications and Quality Control Tests information packet. The
test determines the resistance of a treated substrate to wetting by
aqueous liquids. Drops of water-alcohol mixtures of varying surface
tensions are placed on the substrate and the extent of surface
wetting is determined visually. Place a test carpet sample on a
flat, non-absorbent surface. Beginning with the lowest numbered
test liquid, carefully place one drop in several locations on the
surface of the carpet sample. If no penetration or wetting of the
carpet at the liquid-carpet interface and no wicking around the
drop occurs, place drops of the next higher-numbered test liquid at
an adjacent site on the carpet sample. Repeat this procedure until
one of the higher number test liquids shows obvious wetting or
wicking of the carpet under or around the drop within 10 seconds.
The water repellency rating for a carpet sample is the numerical
value of the highest-numbered test liquid which will not wet the
carpet within 10 seconds. Higher ratings indicate greater
repellency. The composition of water repellency test liquids is
shown in Table 2.
TABLE-US-00002 TABLE 2 Water Repellency Test Liquids Composition,
Vol. % (Isopropyl Alcohol:Distilled Water Repellency Rating Water)
1 2:98 2 5:95 3 10:90 4 20:80 5 30:70 6 40:60
EXAMPLES
Example 1
[0047] Sorbitan tristearate, as a dry powder, is spread evenly over
a commercial level loop nylon-6,6 carpet with stain resist to
uniformly cover the carpet surface. Excess powder is removed by
shaking the carpet until only a fine powder coating remained. The
treated carpet is heated to 250.degree. F. (121.degree. C.) until
the surface temperature reaches 250.degree. F., cooled to room
temperature, allowed to equilibrate at room temperature for 24-48
hours, and the carpet sample is tested according to Test Methods
1-3.
Comparative Example A
[0048] An untreated sample of commercial level loop nylon-6,6
carpet with stain resist is tested according to Test Methods
1-3.
Example 2
[0049] Into a 4-neck round bottom flask equipped with an overhead
stirrer, thermocouple and condenser is added sorbitan tristearate
(60.1 g) and 4-methyl-2-pentanone (MIBK, 150 g). After the solution
is heated to 55.degree. C., an aqueous dispersion is prepared by
adding warm water (383 g), WITCOLATE WAQE (11.4 g) and dipropylene
glycol (14.8 g) at 65.degree. C. The mixture is immersion blended
(2 min), homogenized at 6000 psi, and the resulting dispersion is
distilled under reduced pressure to remove the solvent and yield a
non-flammable urethane dispersion at 12.91% solids after cooling
and filtering. The sample is applied as an aqueous composition by
spray application to a level loop nylon-6,6 carpet with stain
resist at 25% wet pick-up (wpu) and dried to a carpet face
temperature of 250.degree. F. (121.degree. C.). The treated carpet
is tested according to Test Methods 1-3.
TABLE-US-00003 TABLE 3 Performance on Level Loop Nylon Carpet
Samples Water .DELTA.E Before .DELTA.E After Repellency Example
Vacuum Vacuum .DELTA..DELTA.E Rating A 10.6 8.68 0 0 B -- 9.25 1.36
5 1 9.74 7.85 -0.83 4 2 -- 9.28 0.63 4
[0050] Results indicate that the carpet treated by sorbitan
tristearate compounds yields high water repellency performance when
compared with an untreated sample. Further, Example 1 indicates
that dry applications promote soil resistance in addition to water
repellency.
Example 3
[0051] Example 1 was repeated, except a commercial SORONA carpet
was used.
TABLE-US-00004 TABLE 4 Performance on SORONA Carpet Example
.DELTA..DELTA.E Water Repellency Rating 3 -5.5 1
[0052] Results indicate that the carpet treated by sorbitan
tristearate compounds yields water repellency performance and high
soil resistance performance when compared with an untreated
sample.
* * * * *