CA1327856C - Method of enhancing the soil- and stain-resistance characteristics of polyamide and wool fabrics, the fabrics so treated, and treating composition - Google Patents
Method of enhancing the soil- and stain-resistance characteristics of polyamide and wool fabrics, the fabrics so treated, and treating compositionInfo
- Publication number
- CA1327856C CA1327856C CA 610371 CA610371A CA1327856C CA 1327856 C CA1327856 C CA 1327856C CA 610371 CA610371 CA 610371 CA 610371 A CA610371 A CA 610371A CA 1327856 C CA1327856 C CA 1327856C
- Authority
- CA
- Canada
- Prior art keywords
- aqueous solution
- solution
- stain
- fabric
- fluorochemical
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/004—Surface-active compounds containing F
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/24—Organic compounds containing halogen
- C11D3/245—Organic compounds containing halogen containing fluorine
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/3757—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
- D06M15/256—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
- D06M15/277—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof containing fluorine
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
- D06M15/41—Phenol-aldehyde or phenol-ketone resins
- D06M15/412—Phenol-aldehyde or phenol-ketone resins sulfonated
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/23907—Pile or nap type surface or component
- Y10T428/23986—With coating, impregnation, or bond
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
- Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
- Y10T442/2279—Coating or impregnation improves soil repellency, soil release, or anti- soil redeposition qualities of fabric
- Y10T442/2287—Fluorocarbon containing
Abstract
ABSTRACT OF THE DISCLOSURE
A method for enhancing the soil- and/or stain-resistant characteristics of polyamide and wool fabrics is provided. A
variety of combinations of sulfonated resins, sulfonated phenolic compounds, compounds of sulfonated phenolics and aldehydes, fluorochemicals, modified wax emulsions, acrylics and organic acids of low molecular weight provide enhanced soil release and anti-stain properties.
A method for enhancing the soil- and/or stain-resistant characteristics of polyamide and wool fabrics is provided. A
variety of combinations of sulfonated resins, sulfonated phenolic compounds, compounds of sulfonated phenolics and aldehydes, fluorochemicals, modified wax emulsions, acrylics and organic acids of low molecular weight provide enhanced soil release and anti-stain properties.
Description
--1 .... .
The object of the invention is to provide a method for enhancing the soil- and/or stain-resistant characteristics of polyamide and wool fabrics; to provide compositions useful in -providing stain-resistance characteristics to treated fabrics, as well as to the treated fabrics. The fabrics may be treated during manufacture, or during cleaning or reconditioning, and may be treated in whole or in part~ that is to say, the surface only of the fabric will be treated. ~
A particular object of the invention is to provide a method of enhancing soil- and stain-resisting properties of polyamide and wool fabrics comprising applying to the fabric a - -solution containing a condensation product of formaldehyde with one of the group; bis (hydroxyphenyl) sulfone: phenylsulfonic `-~
acid; dihydroxy diphenyl sulfone; benzene sulfonic acid; together :
with a fluorochemical plus an acrylic polymer or copolymer. ~;
It is a particular object of the invention to provide ~ -compositions containing in a variety of combinations, sulfonated ~;
phenolic resins; sulfonated aromatic compounds; compounds of sulfonated phenolics and aldehydes; modified wax emulsions;
fluorochemicals; acrylics; organic acids of low molecular weight. ;
Generally the treating compositions according to the invention are formulated from the following: Condensation products of aldehydes with aromatic sulfonic acids or sulfones;
non-ionic and anionic water-based fluorocarbon; acrylic copolymers; modified wax emulsions; citric or Sulfamic acid;
condensation products of formaldehyde with either bis (hydroxyphenyl) sulfone or phenyl sulfonic acid;
9~
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'. .
The object of the invention is to provide a method for enhancing the soil- and/or stain-resistant characteristics of polyamide and wool fabrics; to provide compositions useful in -providing stain-resistance characteristics to treated fabrics, as well as to the treated fabrics. The fabrics may be treated during manufacture, or during cleaning or reconditioning, and may be treated in whole or in part~ that is to say, the surface only of the fabric will be treated. ~
A particular object of the invention is to provide a method of enhancing soil- and stain-resisting properties of polyamide and wool fabrics comprising applying to the fabric a - -solution containing a condensation product of formaldehyde with one of the group; bis (hydroxyphenyl) sulfone: phenylsulfonic `-~
acid; dihydroxy diphenyl sulfone; benzene sulfonic acid; together :
with a fluorochemical plus an acrylic polymer or copolymer. ~;
It is a particular object of the invention to provide ~ -compositions containing in a variety of combinations, sulfonated ~;
phenolic resins; sulfonated aromatic compounds; compounds of sulfonated phenolics and aldehydes; modified wax emulsions;
fluorochemicals; acrylics; organic acids of low molecular weight. ;
Generally the treating compositions according to the invention are formulated from the following: Condensation products of aldehydes with aromatic sulfonic acids or sulfones;
non-ionic and anionic water-based fluorocarbon; acrylic copolymers; modified wax emulsions; citric or Sulfamic acid;
condensation products of formaldehyde with either bis (hydroxyphenyl) sulfone or phenyl sulfonic acid;
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-2- ~ 327856 fluorochemical with acrylic polymers or copolymers, for example a product sold by Dupont under the trade mark TEFLON MF; bis hydroxphenyl sulfone.
Preferred phenolic resins; fluorochemicals; acrylic resins, polymers and copolymers; as well as water-repellent materials have been selected from the following:
Phenolic Resins:
-Condensation products of formaldehyde with one of the followingbis (hydroxyphenyl) sulfone, Phenyl sulfonic acid, 2.2 bis (hydroxyphenyl) propane, bis (hydroxyphenyl ether, dihydroxy diphenyl sulfone or benzene sulfonic acid, the foregoing being in general, novolac resins.
Fluoro Chemicals:
polyvinylidene fluoride, 2-perfluora-octylacrylate, 2-perfluoro-ethylacrylate, poly tetra fluoro ethylene, and blends thereof -^
with: methyl methacrylate, butyl methylacrylate, modified wax emulsions, polyvinylidene chloride, ethyl methyl acrylate.
Acrylic Resin:
methyl acrylate polymer, methyl acrylate copolymer, or blends of tne foregoing two products with butyl methyl acrylate, methyl methacrylate, butyl acrylate, methyl acrylate, and ethyl acrylate.
TEFLON MF:
an anionic blend of fluorochemical and polyacrylic.
Wax Emulsions: -paraffinic wax emulsion, microcrystaline wax emulsion, metalized wax emulsion such as aluminum salt/wax emulsion or zirconium salt/wax emulsion, modified fatty amide dispersion~ anionic resinous wax emulsion such as melamine wax emulsion.
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Both nylon (polyamide) fabrics and wool fabrics are susceptible to staining by both natural and artificial acid colorants of the sort found in frui-t juices, non-alcoholic - -~
beverages, tea, coffee, common oolorants used in household products, and so on.
Products such as water and/or oil repellents have long been used as fabric protectants to keep liquid spills from penetrating fabrics so as to prevent colorants ~taining the -fibers. Repellents of that sort protect the fabric only as long as the spill remains suspended on the surface of the repellent coating. If the spill is dropped from a height or forced into the fabric by any means, acid colorants will stain the fabric.
Repellent and antisoil finishes may contain -fluorocarbons, waxes, silicones, acrylic polymers or combinations of such products, but chemical finishes of that nature offer little or no protection against warm to hot liquids. Spills of `
that kind penetrate into the fibre and staining commences immediately.
Other disadvantages inherent in known repellent finishes are that they tend to wear off quickly or become contaminated with air borne and/or trafficked soil which tends to ;
reduce their effectiveness as repellents - a particular problem in carpeted areas subject to heavy foot traffic, such as hallways and shopping mall corridors.
Products known as resist chemicals are used in the textile industry to prevent the dyeing of polyamide and wool fibers during special types of printing processes. The same type ,". ''..':
~ 1 327856 of chemical products have been used for many years to improve the wash fastness of acid dyestuff and to prevent colour bleeding.
Such products incl~lde the phenolic resins which in all known processes require temperatures in excess of room te~perature to bond them with the fabric, but we have found that when an aqueous solution of a condensation product of an aromatic sulfonic acid or a sulfone with an aldehyde (i.e. a phenolic resin) is applied to polyamide or wool fibers at a slightly acidic pH e.g. 6.5, and in fact at alkaline pH levels as high as 10, and allowed to dry, the resultant fibers will resist acid colorants without any heat fixation. The stain-resistant material need only penetrate into the fabric to a depth below which the stainin~ substance would not normally be detected when viewed from the fabric surface, for example to a depth of approximately 30% of pile height.
The said condensation products are normally dark in colour and tend to discolour fabrics, particularly those fabrics that are light in colour, and furthermore, treatment with such condensation products tends to reduce the lightfastness of many acid dyestuffs used to colour both polyamide and wool fabric~ and to leave a harsh hand, i.e. a hard or matted surface on the treated fabric. Such a surface on the fabric soils more readily and is more difficult to cleanse and rejuvenate.
Phenolic resins commercially available are all anionically charged and are incompatible with many nonionic -surfectsDts snd/or cstionic products. When phenolic resins sre ; ;' ~ ~
:~
. :':
: ~
1 3~7856 -mixed with nonionic surfactant products in an aqueous solution the ability of the phenolic resins to prevent acid dye staining is materially reduced within a short period of time, and when ~
phenolic resins are mixed with cationic products in an aqueous -solution immediate precipitation of the products is the result.
To achieve satisfactory resistance to acid dye colorants it is therefore necessary to reduce certain adverse effects that the condensation products we prefer happen to share wit~ the phenolic resins, namely, poor lightfastness, discoloration of the fiber and the harsh, soil-retaining hand.
Acrylic polymers have long been used to provide both soil-release and hand-modifying characteristics in textile fabrics, as well as to provide good water repellency.
It has been found that the addition of a white acrylic polymer dispersion (anionic) to a phenolic resin ~reatly reduces the discoloration effect on the treated fabric, and also leaves a much softer hand in addition to providing enhanced soil-release properties. It has been discovered as well that the addition of a fluorochemical improves oil and water repellency and improves antisoiling properties.
TEFLON MF (trade mark), a carpet protection product, is an anionic blend of fluoroche~ical and polyacrylic resin and has -been found to be compatible with both phenolic resins, according to the invention.
Laboratory tests have demonstrated that the combination of one of our aldehyde condensation products i.e. a phenolic resin, with TEFLON ~F (fluorochemical plus an acrylic resin~ when applied to a fabric will enhance resistance to acid colorant ': ' . ~".
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- -6- l 327856 stains, will cause lîttle or no change in fabric hand, will have less effect on lightfastness -than straight phenolic resin, will provide antisoil properties, and will cause little or no colour change as compared to the phenolic resin by itself. In addition the product is applied at room temperature since it does not require heat fixation to bring about the improved properties.
This blended product, merchandised in association with the trade mark BARTEX, when simply diluted in water to a pH not to exceed 7 and sprayed on the polyamide or wool fabric will provide a fabric product that resists acid colorant stains1 is resistant to soiling, and displays good water and oil repellency.
There is also available a product sold under the trade mark ALGUARD NS, which is a condensation product of form~ldehyde with aromatic sulfonic acids which is compatible with both nonionic and anionic products and which does not lose its antistain properties when held in solution with nonionic surfactant products for prolonged periods of time. ALGUARD NS ~. :
enables us to use fluorochemicals other than TEFLON MF which heretofore was to our knowledge the only anionic fluorochemical on the market compatible with a phenolic resin. Accordingly TEFLON MF' was replaced with a commercially available nonionic fluorochemical. This product, '-;;~
identified by our trade mark BARTEX A-200, is made up as follows:
Fluorochemical - 10-20% ~-Acr~lic copolymer - 3.0-10% -Aromatic sulfonic acid condensation products - 3~10%
Citric Acid - to pH 5 to 6 Water - Balance .',,' ~"
_7_ 1 327~ :
BARTEX A-200 is a concentrate to be diluted in water at a ratio of from 1:20 to 1:32~ and is -topically applied to -fabric.
BARTEX A-200 is a fabric protectant that possesses antistain and anti-soil characteristics, and that demonstrates oil and water repellency as well. It also demonstrates good durability to wet cleaning when simply sprayed over the surface of nylon or wool fabrics and allowed to air dry. Those characteristics are imparted only to that portion of the fabric which has been contacted by the treating solution.
With some manufacturers and cleaners there is a market for a less expensive anti-stain and soil-release product that ~:
does not contain fluorochemicals, though it is not as durable as BARTEX A-200. It would be applied to nylon and wool fabrics during the cleaning process and its application would not require additional ]abour. This product, BARTEX SA (shampoo additive), is formulated as follows:
Acrylic copolymer - 10-20%
Aromatic sulfonic acid/aldehyde ~ :
condensation product - 6-20%
Citric Acid - To pH 6.5 to 7.0 Water - Balance ~........................................... ................................. .'-BARTEX SA is a concentrated product and when added to cleaning solutions will impart antistain and soil-release properties to nylon and wool fabrics during the cleaning process at an ~;
application pH of 10 or lower. The product is normally applied in ~ ran~e from 0.2 to 0.7X b~ed on weight of the portion of the : ';:
..
l- ~327856 fibres being treated. The wide variations in application rates are due to the variations in the depth of penetration into the fabric. (e.g. 20% to 100%) Also the level of antistain and soil-release protection can vary considerably outsi~e that range and still yield fair to excellent results. We have discovered too that it is possible to provide fabrics with antistain, antisoil and water-repellent characteristics without using either acrylic resin or fluorochemical. A typical formulation of our product BARTE~ WX would be as follows:
Aromatic sulfonic acid/aldehyde condensation product 5-20~
Modified wax emulsion 15-40%
pH 5-6 Water Balance The level of antistain and antisoil protection required to yield acceptable results may also vary considerably due to the type of nylon (6 or 66), heat-set or non-heat-set or if the fabric is wool. Generally speaking nylon 6 will reguire 1.5 times the amount of product used for nylon 66 whereas wool can require up to twice the amount of product required for nylon 66.
But where the fabrics have had antistain and antisoil treatments applied to them during manufacture they will require during subsequent treatment only small amounts of additional antistain and antisoil or soil-release to replace the original treatment products which have been removed by cleaning and normal use.
The products of the invention are in the main intended to be used to augment or supplement the anitstain, antisoil ~9~ 1 327 ~ 56 and/or soil-release properties of fabric~ which have been treated in that way during manufacture, and will be accompliRhed for example during cleaning processes or as a separate topical sprayed finish following installation of the fabric product.
Specifically antisoil substances reduce the affinity of fabrics to soil whereas soil-release substances facilitate soil removal.
Alternatively, BA~TEX SA can be applied to nylon fibres during the manufacturing process at levels of from 1% to 6% on weight of fibres and will yield excellent antistain and soil-release properties. In this case the fabric is immersed in an a~ueous solution containing BARTEX SA and may or may not be subsequently oversprayed with a fluorochemical.
It is to be noted that in general colorant materials ~ :;
used as food additives utilize anionic dyestuf~s as the substances providing the colour, and it is those substances that bond with nylon and wool fibers, either chemically or electrostatically.
The following specific examples will serve to illustrate the invention: ;
Example 1 - TEFLON MF vs. TEFLON MF ~ phenolic resin vs Untreated (Nylon 66).
Example 2 - TEFLON MF + phenolic resin vs pheDolic resin (Nylon 66).
Example 3 - phenolic resin vs phenolic resin ~ Acrylic ;~
vs Acrylic (Nylon 66).
Example 4 - TEFLON MF VR fluorochemical ~ phenolic resin vs Untreated (Nylon 6).
ExamPle 5 - TEFLON MF + phenolic resin vs phenolic resin (Nylon 6).
ExamPle 6 - Phenolic resin vs phenolic resin ~ Acrylic vs Acrylic (Nylon 6) Example 7 - TEFLON MF + phenolic resin vs TEFLON MF vs Untreated (Wool~
Example 8 - Phenolic resin t Acrylic vs phenolic resin -vs Control (Nylon 66) Example 9 - Phenolic resin + Acrylic vs phenolic resin vs Control (Nylon 6) ExamPle 10 - Phenolic resin + Acrylic pH 10 vs phenolic resin t Acrylic pH 6.5 (Nylon 66) Example 11 - TEFLON MF + phenolic resin vs Bartex A 200 (Nylon 66).
xample 12 - Modified wax emulsion + phenolic resin vs -phenolic resin vs acrylic vs control (Nylon 6). ; -Example 13 - Modified wax emulsivn + phenolic resin vs phenolic resin vs acrylic vs control ;
(Nylon 66).
In each of the examples the fabric samples, having first been treated with antistain/soil-release solutions and dried, were exposed to a staining test. In certain examples an untreated fabric sample was used as a control.
In the examples 1 to 7, 10, 11, 12, and 13, the following staining test was used: 20 ml. a solution of sugar-sweet cherry flavoured KOOL-AID (trade mark) is poured into a 2 1/4" diameter ring placed on the carpet surface. The solution is pres~ed into the carpet and allowed to remain there for one hour at room temperature. The sample is rinsed under cold running water, dried and evaluated against a scale which ranges from 1 to 5 where 5 represents complete stain removal. The treated portion of the pile height only (approx. 30% of pile height) was ~`~
evaluated for stain resistance.
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.~ ",' In the examples a graduated ~cale ~rom l -to 5 was used to evaluate yellowing where 5 represents no yellowing and 4 represents acceptable yellowing.
In the examples, discoloration due to exposure to light was determined using AATCC test method with an exposure time of 40 hours. The exposed samples were graded using a graduated rating scale which ranges from l to 5, where 5 represents no discoloration and a rating of 4 is acceptable.
In examples 8 and 9 the following stain test was used:
20 ml. o~ an aqueous solution of sugar-sweet cherry ~lavoured KOOL-AID is poured into a 2 l/4" diameter ring placed on a carpet - -surface. The solution is pressed into the carpet and allowed to remain there for 8 hrs. at room temperature (22 degrees C.). The sample is rinsed under cold running water, dried and evaluated against a scale which ranges from l to 5 where 5 represents complete stain removal.
EXAMPLE l AND COMPARATIVE EXAMPLES A-l AND B-l In example l an aqueous solution o~ TEFLON MF was ;
prepared according to manufacturer's instructions at room temperature yielding a 6.25% solution. To this solution was added 1% of a 30% by weight phenolic resin pH adjusted to 6.5.
This solution was then topically sprayed onto undyed nylon 56 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approx 30% penetration of pile height) and allowed -to air dry for 12 hrs. at room temperature.
In comparative example A-l, an aqùeous solution o~ ~;
TE~LON MF was prepared according to manu~acturer's instructions and at 20~C yielding a 6.25% solution. This solution was then -12- ~ 327856 topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft, brushed into the pile (approx. 30% pene-tration of pile height) and allowed to air dry for 12 hrs. at room temperature (22 C.). .
In comparative example B~1 the undyed nylon 66 carpet was left untreated. -~
Each sample was tested for initial stain resistance characteristics and stain resistance after hot water extraction cleaning using 10 gm/L. of a commercial carpet cleaning solution TABLE 1 ~
EXAMPLE STAIN RESISTANCE AFTER CLEANIN~ STAIN .~
RESISTANCE .-A-l 1 1 B-l As can be seen ~rom the results in table 1 the treatment of the nylon 66 carpet with TEFLON NF together with a ~.
phenolic resin provides sta.in resistance before and after .,.
cleaning on the treated portion o~ the fibres and that TEFLON NF . .;
by itself offer~ negligible stain resistance initially and after ~:
cleaning. : ^
EXANPLE 2 AND COMPARATIVE EXAMPLES A-2 AND B-2 :~
In example 2 an aqueous solution of TEFLON MF was :~.
... . ..
prepared accordingly to manufacturer's instructions and at 20C
yielding a 6.25% solution. To this solution was added 1% of a ..
30% weight percent phenolic resin solution, pH to 6.5. This solution was then topically sprayed onto undyed nylon 66 . ': : .' "~
~ ... ..
~ -13- l 327 8 5 6 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approx 30% pene-tration of pile height) and allowed to air dry for 12 hrs. at room temperature. -In comparative example A-2, an aqueous solution of 1%
phenolic resin was prepared at 20C and the pH adjusted to 6.5.
This solution was then topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approx. 30% penetration of pile height) and allowed to air dry for 12 hrs at room temperature (220C.).
Each sample was tested for initial stain resistance characteristics and yellowing.
Example Stain Resistance Yellowin~
2 5 4.5 As can be seen from the results in table 2 the treatment of the nylon 66 carpet with TEFLON MF together with a phenolic resin causes substantially less yellowing on the treated portion of the fibre than the sulfonated phenolic resin by itself, while still exhibiting excellent stain resistance.
Furthermore the yellowing in example A-2 is unacceptable whereas the yellowing in example 2 is acceptable.
In example 3 a 1.0~ aqueous solution of a 30 percent by ~;
weight solution of a phenolic resin was prepared at 20 C and the pH adjusted to 6.5. This solution was then topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft., -14- l 3~7856 brushed into the pile ~nd allowed to air dry for 12 hrs. at room temperature.
In example A-3 a 1.0% aqueous solution of a 30 percent by weight solution of phenolic resin was prepared and to this solution was a~ded 2% of a 25 weight percent aqueous polyacrylic solution and the pH adjusted to 6.5. This solution was then topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft., brushed into the pile approx 30% penetration of pile height and allowed to air dry for 12 hrs at room temperature.
In example B-3 an aqueous solution of 2% of a 25 weight percent aqueous polyacrylic solution was prepared and the pH
adjusted to 6.5. This solution was then topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approx 30% penetration of pile height) and allowed to air dry for 12 hrs. at room temperature Each sample was tested for initial stain resistance characteristics and yellowing and stain resistance after hot water extraction cleaning using 10 gm/L. of a commercial carpet cleaning solution.
TABLE 3 ~ -Example Stain Resist Stain Resist After Yellowing Cleanin~ _ A-3 6 4 4.5 As can be seen from the results in table 3 the treatment of nylon 66 with phenolic resin in combination with polyacrylic yielding over-all superior results to either phenolic resin or polyacrylics by themselves. This comparison was done on the treated portion of the pile height or approximately 30% o~ pile height.
EXAMPLE 4 AND COMPA~ATIVE EXAMPLES A-4 AND B-4 In example 4 an aqueous solution of TEFLON MF was prepared according to manufacturer's instructions and at room temperature yielding a 6.5% solution. To this solution was added 1.5% of a 30% by weight phenolic resin solution, pH adjusted to 6.5. This solution was then topically sprayed onto the undyed nylon 6 carpeting at a rate of 20 ml/sq.ft., brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at room temperature.
In comparative example A-4, an aqueous solution of TEFLON MF was prepared according to manufacturer's instructions and at 20 C. yielding a 6.5X solution. This solution was then .
tôpically sprayed onto undyed nylon 6 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at room temperature. ;
In comparative example B-4 the undyed nylon 6 carpet was left untreated.
.
Each sample was tested for initial stain resistance characteristic~ and stain resistance after hot water extraction --cleaning usinq 10 gmJL. Or commercial carpet clesning solution.
: -,. :-, ,:' Example Stain ~esistance After Cleaning Stain ~esistance ~-4 As can be seen from the results in table 4 the treatment of the nylon 6 carpet with TEFLON MF together with a phenolic resin provides stain resistance before and after ~-cleaning on the treated portion of the fabric and the TEFLON NF :-by itself offers negligible stain resistance initially and after ~
cleaning. ;
EXAMPLE 5 AND COMPARATIVE EXAMPLES A-5 AND B-6 ;
In example 5 an aqueous solution of TEFLON MF was I prepared according to manufacturer'~ instructions and at a 20C -~
yielding a 6.25% ~olution. To this olution w~s added 1.5% of a 30% by weight phenolic resin solution pH adjusted to 6.5. This solution was then topically sprayed onto undyed nylon 6 carpeting -at the rate of 20 ml/sq.ft., brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at room temperature.
In comparative example A-5, an aqueous solution o~ 1.5% ;
phenolic resin was prepared at 20C. and the pH adjusted to 6.5. ~-This solution was then topically sprayed onto undyed nylon 6 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approximately 30% penetration of pile height) and allowed to air ~- dry for 12 hrs at room temperature. ; ~;
Each sample was tested for initial stain resistance ' '~
characteristics and yellowing.
. " ".
'''`''''~.'',' . . .; ~.
: . .
Example Stain Resistance Yellowin~
4.5 As can be seen from the results in table 5 the treatment of the nylon 6 carpet with TEFLON MF together with a phenolic resin caused substantially less yellowing on the treated portion of the fabric than the phenolic resin by itself, while still exhibiting excellent stain resistance. Furthermore the yellowing in example A-5 is unacceptable whereas the yellowing in example 5 is acceptable.
EXAMPLE 6 AND COMPARATIVE EXAMPLES A-6 AMD B-6 `
In example 6 an aqueous solution o~ 1.5% phenolic resin solution which was 30% by weight was prepared at 20C. and the pH ;
adjusted to 6.5. This solution was then topically sprayed onto undyed nylon 6 carpeting at the rate of 20 ml/sq.ft., brushed into the pile ~approximately 30% penetration of pile height~ and allowed to air dry for 12 hrs. at room temperature.
In example A-6 an aqueous solution of 1.5% phenolic resin was prepared and to this solution was added 2% of a 25 weight percent aqueous polyacrylic solution and the pH adjusted to 6.5. This solution was then topically sprayed onto the pile, brushed in the pile (approx. 30% penetration of pile height) and allowed to air dry for 12 hrs at room temperature.
In example B-6 an aqueous solution of 2% of a 25 weight percent aqueous polyacrylic solution was prepared and the pH ~-adjusted to 6.5. This solution was then topically sprayed onto ~;
undyed nylon 6 carpeting at the rate of 20 ml/sq.ft., brushed :
: ' - :
. ',.',,',''.
-18- l 327 ~ 5 6 into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at room -temperature.
Each sample was tested for initial stain resistance characteristics and yellowing, and stain resistance after hot water extraction cleaning using 10 gm/L of a commercial carpet cleaning solution.
Example Stain Resist Stain Resist After Yellowing CleaninR ~
4 3 `
As can be seen from the results in table 6 the ~`
treatment of nylon 66 with phenolic resin in combination with `
polyacrylic yields superior results to either phenolic resin OI' ... `
polyacrylics by themselves. This comparison was made base on the treated portion of the pile height or approximately 30% pile ~ -height.
In example 7 an aqueous solution of TEFLON MF was prepared according to manufacturer's instructions and at ;
200C yielding a 6.5% solution. To this solution was added 2% of a 30 weight percent solution of a phenolic resln solution and the pH adjusted to 6.5 with citric acid. This solution was then topically sprayed onto 100% wool carpeting at the rate of 20 `
ml/~q.ft. brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at roo~;;
temperature.
,.
. ....
~.
In comparative example A-7, an aqueous solution of TEFLON MF was prepared according to manufacturer's instruc-tions at a 20C yielding a 6.5% solution. This solution was then topically sprayed onto 100% wool carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approx. 30% penetra-tion of pile height) and allowed to air dry for 12 hrs at room temperature.
In comparative example B-7 the 100% wool carpeting was left untreated.
Each example was tested for initial stain resistance characteristics and stain resistance after hot water extraction using 10 gm/L of a commercial carpet cleaning solution.
Example Stain Resistance After Cleaning Stain Resistance As can be seen from the results in table 7 the treatment of the 100% wool carpet with TEFLON M~ together with a phenolic resin provides stain resistance before and after the cleaning and the TEFLON MF by itself ofers negligible stain resistance initially and after cleaning. -EXAMPLE 8 AND COMPARATIVE EXAMPLES A-8. B-8 AND C-8 In example 8, into a bath containing 0.5 gm. of BARTEX -SA, 300 gm. of water, and the pH adjusted to 2.3 with sulfam~ic acid, was placed a 20 gm. sample of undyed nylon 66 carpe-ting.
The temperature was raised to about 85C and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example A-8 into a bath con-taining 0.5 gm of a 30% by weight phenolic resin solution, 300 gm of wa-ter and a pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 66 carpeting. The temperature was raised to about 850C and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example B-8 into a bath containing 0.5 ~-gm of an alternative 30% by weight phenolic resin, 300 gms of water and the pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 66 carpeting. The temperature was raised to about 85C and maintained for 20 minutes, and then the sample was rinsed and dried at 110C for 15 minutes.
In comparative example C-8 into a bath containing 300 -gms of water and the pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of nylon 66 carpeting. The temperature was raised to about 850C and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes. `
Each example was tested for initial stain resistance ^
characteristics, yellowing and discoloration due to light.
TABLE 8 --;
ExampleStain Resistance YellowingDiscoloration Due to li~ht ~ . .
As can be seen from the test results in table 8, example 8 (acrylic polymer with phenolic resin) yields average ,., :~,'',,' ~ 327856 stain resis-tance when compared to both of the two comparative phenolic resin samples, negligible yellowing and acceptable discoloration due to light. Conversely examples A-8 and B-8 demonstrate good stain resistance but only acceptable yellowing and only unacceptable discoloration due to ligh-t.
EXANPLE 9 AND COMPARATIVE EXAMPLES A-9~ B-9 AND C-9 In example 9, into a bath containing 0.9 gm of BARTEX
SA, 300 gm of water and the pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 6 carpeting. The temperature was raised to 85OC and maintained for 20 minutes.
The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example A-9 into a bath containing 0.9 gm of a 30% by weight phenolic resin, 300 gm of water and pH
adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 6 carpeting. The temperature was raised to 85C and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example B-9 into a bath containing 0.5 gm of an alternate 30% weight phenolic reqin, 300 gm o~ water and the pH adiusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 6 carpeting. The temperature was raised ~ ;
to 85~C and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example C-9 into a bath containing 30G
gms of wat~r and the pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 6 carpeting. The te~perature was raised to 85OC and maintained for 20 minutes.
The sample was rinsed and then dried at 110~C for 15 minutes.
-22- ~ 327 8 5 6 Each example was -tested for initial stain resistance characteristics, yellowing and discolora-tion due to light.
Example Stain resistanceYellowing Discoloration Due to li~ht -As can be seen from the test results in table 9, example 9 ~acrylic polymer with phenolic resin) yields above average stain resistance when compared to both of the two -comparative phenolic resin samples, negligible yellowing and acceptable discoloration to light. Conversely example A-9 and B- -: -:
9 demonstrate marginal stain resistance and unacceptable discoloration due to light and marginal to unacceptable~^
yellowing.
In example 10, a 1.0% aqueous solution of a 30% by weight phenolic resin solution was prepared and to this solution was added 2% of a 25 weight percent aqueous polyacrylic solution, 0.1% of a commercial carpet cleaning solution and the pH adjusted `
to 10. This solution was then sprayed onto the pile of undyed nylon 66 carpeting, at the rate of 10 ml/sq.ft. brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at room temperature.
In comparative example A-10, a 1.0% aqueous solution of a 30X by weight phenolic resin was prepared and to this solution was added 2% of a 25 weight percent aqueous polyacrylic solution, 0.1% of a commercial carpet cleaning solution and the pH adjusted .
I ., -23- l 327 8 5 6 $o 10. This solution was -then sprayed onto the pile of undyed nylon 66 carpeting at the rate of 10 ml/sq.ft., brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at room temperature.
Each example was tested for initial stain resistance characteristics and stain resistance after hot water extraction cleaning using 10 gm/L of commercial carpet cleaning solution.
ExampleStain Resist Stain Resist After _ _ Cleanin~
~-5 3-4 As can be seen from the results in table 10 the treatment of nylon 66 carpeting at a pH level of 10 shows only slightly inferior stain resistance to A-10 treated at a pH level of 6.5. The presence of a carpet cleaning solution had no effect on the antistain characteristics.
In example 11 an aqueous solution of TEFLON MF, was prepared according to manufacturer's instructions at room temperature yielding a 6.25% solution. To this solution was added 1% of a 30% by weight phenolic resin solution, Ph adjusted to 6.5. This solution was then topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry at room temperature for 12 hrs.
In comparative example A-ll a 1.5% a~ueous solution of BA~TEX A200 was prepared at room temperature with a resultant pH
of 6.5. This solution was then topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft., brushed into the :, ..
~ '`.',"
-2~ 2 7 8 5 6 pile (approximately 30% pene-tration of pile height~ and allowed to air dry at room temperature for 12 hrs.
Each sample was tested for initial s-tain resis-tance characteristics, s-tain resistance after hot water extraction ~ -cleanin~ using 10 ~m/L of a commercial carpet cleaning solution, -yellowing and discoloration due to light.
:, .
TABLE 11 ~-Example Stain After Cleaning Yellowing Discoloration Resistance stain resistance due to li~ht 11 5 4 4.5 4 ;
A-11 5 4.5 4.5 4-5 --As can bee seen from the results in table 11 the treatment of nylon 66 carpeting with either of the antistain combinations yields excellent results in all tests. -Example 12 and comparative Examples A-12. B-12 and C-12 In example 12, into a bath containing 0.9 gm of Bartex WX, 300 gm of water and pH adju~ted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 6 carpeting. The temperature was raised to 85C and maintained for 20 minutes.
The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example A-12 into a bath containing 0.9 gm of a 30% by weight phenolic resin, 300 gm of water an pH
adjusted to 2.3 with sulfamic acid was placed a 20 ~m sample of :
undyed nylon 6 carpeting. The temperature was raised to 85C and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes. ;
In comparative example B-12 into a bath containing 2%
of a 25% wei~ht acrylic resin, 300 gm of water and pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon I . ' ';
.~.
,'....
-25~ l 327856 6 carpeting. The temperature was raised to 85OC and maintained for 20 minutes. The sample was rinsed and then dried at 1104C
for 15 minutes.
In compara-tive example C-12 into a bath containing 300 gm of wa-ter and the pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 6 carpeting. The temperature was raised to 85C and maintained for 20 minutes. ~ ;
The sample was rinsed and then dried at llO~C for 15 minutes.
Each example was tested for initial stain resistance characteristics, yellowing and discoloration due to light.
Example Stain ResistanceYellowingDiscoloration Due to Li~ht -As can be seen form the test results in table 12, example 12 Bartex WX (wax emulsion and phenolic resin~ yields excellent stain resistance when compared to phenolic resin alone or acrylic resin alone.
Conversely example A-12 demonstrates acceptable stain resist&nce and yellowing, and unacceptable discoloration due to light. ;
Example B-12 demonstrates unacceptable stain resistance, acceptable yeIlowing, and discoloration due to light.
It is clearly evident that example 12 shows that Bartex -WX, is superior to all other examples.
. , .,.".,;~
,., -26- l 327856 ~:
Example 13 and comparative Examples A-13, B-13 and C-13 In example 13, into a bath containing 0.9 gm of Bartex WX, 300 gm of water and pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 66 carpetingr. The temperature was raised to 85~C and maintained for 20 minutes~ ~
The sample was rinsed and then dried at 110C for 15 minutes. -In comparative example A-13 into a bath containing 0.9 gm of a 30% by weight phenolic resin, 300 gm of water an pH
adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 66 carpeting. The temperature was raised to 85C
and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example B-13 into a bath containing 2%
of a 25% weight acrylic resin, 300 gm of water alld pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 66 carpeting. The temperature was raised to 85C and maintained for 20 minutes. The sample was rinsed and then dried at 110C
for 15 minutes.
In comparative example C-13 into a bath containing 300 gm of water and the pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 66 carpeting. The temperature was raised to 85C and maintained for 20 minutes.
The sample was rinsed and then dried at 110C for 15 minutes.
Each example was tested for initial stain resistance characteristics, yellowing and discoloration due to light.
' ~
.
-27- l 327856 Example Stain ResistanceYellowing~iscoloration _ ~ue to Li~ht 13 5 5 . :
A-13 4 4 3 .~.
B-13 3 4~5 5 C-13 1 5 5 .
As can be seen form the test results in table 13, example 13 Bartex WX (wax emulsion and phenolic resin) yields excellent stain resistance when compared to phenolic resin alone or acrylic resin alone.
Conversely example A-13 demonstrates acceptable stain resistance and yellowing, and unacceptable d.iscoloration due to ~.-light. ~.
Example B-13 demonstrates unacceptable stain resistance, acceptable yellowing, and discoloration due to light.
It is clearly evident that example 13 shows that Bartex WX, is superior to all other examples.
''' ;-The foregoing is by way of example only and the invention should be limited only be the scope of the appended .
claims.
'''~"''",.'~' , "
Preferred phenolic resins; fluorochemicals; acrylic resins, polymers and copolymers; as well as water-repellent materials have been selected from the following:
Phenolic Resins:
-Condensation products of formaldehyde with one of the followingbis (hydroxyphenyl) sulfone, Phenyl sulfonic acid, 2.2 bis (hydroxyphenyl) propane, bis (hydroxyphenyl ether, dihydroxy diphenyl sulfone or benzene sulfonic acid, the foregoing being in general, novolac resins.
Fluoro Chemicals:
polyvinylidene fluoride, 2-perfluora-octylacrylate, 2-perfluoro-ethylacrylate, poly tetra fluoro ethylene, and blends thereof -^
with: methyl methacrylate, butyl methylacrylate, modified wax emulsions, polyvinylidene chloride, ethyl methyl acrylate.
Acrylic Resin:
methyl acrylate polymer, methyl acrylate copolymer, or blends of tne foregoing two products with butyl methyl acrylate, methyl methacrylate, butyl acrylate, methyl acrylate, and ethyl acrylate.
TEFLON MF:
an anionic blend of fluorochemical and polyacrylic.
Wax Emulsions: -paraffinic wax emulsion, microcrystaline wax emulsion, metalized wax emulsion such as aluminum salt/wax emulsion or zirconium salt/wax emulsion, modified fatty amide dispersion~ anionic resinous wax emulsion such as melamine wax emulsion.
~ B `:
. :
",.,,~",,,,,,,",,~",,,~...",,.~
..
Both nylon (polyamide) fabrics and wool fabrics are susceptible to staining by both natural and artificial acid colorants of the sort found in frui-t juices, non-alcoholic - -~
beverages, tea, coffee, common oolorants used in household products, and so on.
Products such as water and/or oil repellents have long been used as fabric protectants to keep liquid spills from penetrating fabrics so as to prevent colorants ~taining the -fibers. Repellents of that sort protect the fabric only as long as the spill remains suspended on the surface of the repellent coating. If the spill is dropped from a height or forced into the fabric by any means, acid colorants will stain the fabric.
Repellent and antisoil finishes may contain -fluorocarbons, waxes, silicones, acrylic polymers or combinations of such products, but chemical finishes of that nature offer little or no protection against warm to hot liquids. Spills of `
that kind penetrate into the fibre and staining commences immediately.
Other disadvantages inherent in known repellent finishes are that they tend to wear off quickly or become contaminated with air borne and/or trafficked soil which tends to ;
reduce their effectiveness as repellents - a particular problem in carpeted areas subject to heavy foot traffic, such as hallways and shopping mall corridors.
Products known as resist chemicals are used in the textile industry to prevent the dyeing of polyamide and wool fibers during special types of printing processes. The same type ,". ''..':
~ 1 327856 of chemical products have been used for many years to improve the wash fastness of acid dyestuff and to prevent colour bleeding.
Such products incl~lde the phenolic resins which in all known processes require temperatures in excess of room te~perature to bond them with the fabric, but we have found that when an aqueous solution of a condensation product of an aromatic sulfonic acid or a sulfone with an aldehyde (i.e. a phenolic resin) is applied to polyamide or wool fibers at a slightly acidic pH e.g. 6.5, and in fact at alkaline pH levels as high as 10, and allowed to dry, the resultant fibers will resist acid colorants without any heat fixation. The stain-resistant material need only penetrate into the fabric to a depth below which the stainin~ substance would not normally be detected when viewed from the fabric surface, for example to a depth of approximately 30% of pile height.
The said condensation products are normally dark in colour and tend to discolour fabrics, particularly those fabrics that are light in colour, and furthermore, treatment with such condensation products tends to reduce the lightfastness of many acid dyestuffs used to colour both polyamide and wool fabric~ and to leave a harsh hand, i.e. a hard or matted surface on the treated fabric. Such a surface on the fabric soils more readily and is more difficult to cleanse and rejuvenate.
Phenolic resins commercially available are all anionically charged and are incompatible with many nonionic -surfectsDts snd/or cstionic products. When phenolic resins sre ; ;' ~ ~
:~
. :':
: ~
1 3~7856 -mixed with nonionic surfactant products in an aqueous solution the ability of the phenolic resins to prevent acid dye staining is materially reduced within a short period of time, and when ~
phenolic resins are mixed with cationic products in an aqueous -solution immediate precipitation of the products is the result.
To achieve satisfactory resistance to acid dye colorants it is therefore necessary to reduce certain adverse effects that the condensation products we prefer happen to share wit~ the phenolic resins, namely, poor lightfastness, discoloration of the fiber and the harsh, soil-retaining hand.
Acrylic polymers have long been used to provide both soil-release and hand-modifying characteristics in textile fabrics, as well as to provide good water repellency.
It has been found that the addition of a white acrylic polymer dispersion (anionic) to a phenolic resin ~reatly reduces the discoloration effect on the treated fabric, and also leaves a much softer hand in addition to providing enhanced soil-release properties. It has been discovered as well that the addition of a fluorochemical improves oil and water repellency and improves antisoiling properties.
TEFLON MF (trade mark), a carpet protection product, is an anionic blend of fluoroche~ical and polyacrylic resin and has -been found to be compatible with both phenolic resins, according to the invention.
Laboratory tests have demonstrated that the combination of one of our aldehyde condensation products i.e. a phenolic resin, with TEFLON ~F (fluorochemical plus an acrylic resin~ when applied to a fabric will enhance resistance to acid colorant ': ' . ~".
: ~. .
; r~ `
- -6- l 327856 stains, will cause lîttle or no change in fabric hand, will have less effect on lightfastness -than straight phenolic resin, will provide antisoil properties, and will cause little or no colour change as compared to the phenolic resin by itself. In addition the product is applied at room temperature since it does not require heat fixation to bring about the improved properties.
This blended product, merchandised in association with the trade mark BARTEX, when simply diluted in water to a pH not to exceed 7 and sprayed on the polyamide or wool fabric will provide a fabric product that resists acid colorant stains1 is resistant to soiling, and displays good water and oil repellency.
There is also available a product sold under the trade mark ALGUARD NS, which is a condensation product of form~ldehyde with aromatic sulfonic acids which is compatible with both nonionic and anionic products and which does not lose its antistain properties when held in solution with nonionic surfactant products for prolonged periods of time. ALGUARD NS ~. :
enables us to use fluorochemicals other than TEFLON MF which heretofore was to our knowledge the only anionic fluorochemical on the market compatible with a phenolic resin. Accordingly TEFLON MF' was replaced with a commercially available nonionic fluorochemical. This product, '-;;~
identified by our trade mark BARTEX A-200, is made up as follows:
Fluorochemical - 10-20% ~-Acr~lic copolymer - 3.0-10% -Aromatic sulfonic acid condensation products - 3~10%
Citric Acid - to pH 5 to 6 Water - Balance .',,' ~"
_7_ 1 327~ :
BARTEX A-200 is a concentrate to be diluted in water at a ratio of from 1:20 to 1:32~ and is -topically applied to -fabric.
BARTEX A-200 is a fabric protectant that possesses antistain and anti-soil characteristics, and that demonstrates oil and water repellency as well. It also demonstrates good durability to wet cleaning when simply sprayed over the surface of nylon or wool fabrics and allowed to air dry. Those characteristics are imparted only to that portion of the fabric which has been contacted by the treating solution.
With some manufacturers and cleaners there is a market for a less expensive anti-stain and soil-release product that ~:
does not contain fluorochemicals, though it is not as durable as BARTEX A-200. It would be applied to nylon and wool fabrics during the cleaning process and its application would not require additional ]abour. This product, BARTEX SA (shampoo additive), is formulated as follows:
Acrylic copolymer - 10-20%
Aromatic sulfonic acid/aldehyde ~ :
condensation product - 6-20%
Citric Acid - To pH 6.5 to 7.0 Water - Balance ~........................................... ................................. .'-BARTEX SA is a concentrated product and when added to cleaning solutions will impart antistain and soil-release properties to nylon and wool fabrics during the cleaning process at an ~;
application pH of 10 or lower. The product is normally applied in ~ ran~e from 0.2 to 0.7X b~ed on weight of the portion of the : ';:
..
l- ~327856 fibres being treated. The wide variations in application rates are due to the variations in the depth of penetration into the fabric. (e.g. 20% to 100%) Also the level of antistain and soil-release protection can vary considerably outsi~e that range and still yield fair to excellent results. We have discovered too that it is possible to provide fabrics with antistain, antisoil and water-repellent characteristics without using either acrylic resin or fluorochemical. A typical formulation of our product BARTE~ WX would be as follows:
Aromatic sulfonic acid/aldehyde condensation product 5-20~
Modified wax emulsion 15-40%
pH 5-6 Water Balance The level of antistain and antisoil protection required to yield acceptable results may also vary considerably due to the type of nylon (6 or 66), heat-set or non-heat-set or if the fabric is wool. Generally speaking nylon 6 will reguire 1.5 times the amount of product used for nylon 66 whereas wool can require up to twice the amount of product required for nylon 66.
But where the fabrics have had antistain and antisoil treatments applied to them during manufacture they will require during subsequent treatment only small amounts of additional antistain and antisoil or soil-release to replace the original treatment products which have been removed by cleaning and normal use.
The products of the invention are in the main intended to be used to augment or supplement the anitstain, antisoil ~9~ 1 327 ~ 56 and/or soil-release properties of fabric~ which have been treated in that way during manufacture, and will be accompliRhed for example during cleaning processes or as a separate topical sprayed finish following installation of the fabric product.
Specifically antisoil substances reduce the affinity of fabrics to soil whereas soil-release substances facilitate soil removal.
Alternatively, BA~TEX SA can be applied to nylon fibres during the manufacturing process at levels of from 1% to 6% on weight of fibres and will yield excellent antistain and soil-release properties. In this case the fabric is immersed in an a~ueous solution containing BARTEX SA and may or may not be subsequently oversprayed with a fluorochemical.
It is to be noted that in general colorant materials ~ :;
used as food additives utilize anionic dyestuf~s as the substances providing the colour, and it is those substances that bond with nylon and wool fibers, either chemically or electrostatically.
The following specific examples will serve to illustrate the invention: ;
Example 1 - TEFLON MF vs. TEFLON MF ~ phenolic resin vs Untreated (Nylon 66).
Example 2 - TEFLON MF + phenolic resin vs pheDolic resin (Nylon 66).
Example 3 - phenolic resin vs phenolic resin ~ Acrylic ;~
vs Acrylic (Nylon 66).
Example 4 - TEFLON MF VR fluorochemical ~ phenolic resin vs Untreated (Nylon 6).
ExamPle 5 - TEFLON MF + phenolic resin vs phenolic resin (Nylon 6).
ExamPle 6 - Phenolic resin vs phenolic resin ~ Acrylic vs Acrylic (Nylon 6) Example 7 - TEFLON MF + phenolic resin vs TEFLON MF vs Untreated (Wool~
Example 8 - Phenolic resin t Acrylic vs phenolic resin -vs Control (Nylon 66) Example 9 - Phenolic resin + Acrylic vs phenolic resin vs Control (Nylon 6) ExamPle 10 - Phenolic resin + Acrylic pH 10 vs phenolic resin t Acrylic pH 6.5 (Nylon 66) Example 11 - TEFLON MF + phenolic resin vs Bartex A 200 (Nylon 66).
xample 12 - Modified wax emulsion + phenolic resin vs -phenolic resin vs acrylic vs control (Nylon 6). ; -Example 13 - Modified wax emulsivn + phenolic resin vs phenolic resin vs acrylic vs control ;
(Nylon 66).
In each of the examples the fabric samples, having first been treated with antistain/soil-release solutions and dried, were exposed to a staining test. In certain examples an untreated fabric sample was used as a control.
In the examples 1 to 7, 10, 11, 12, and 13, the following staining test was used: 20 ml. a solution of sugar-sweet cherry flavoured KOOL-AID (trade mark) is poured into a 2 1/4" diameter ring placed on the carpet surface. The solution is pres~ed into the carpet and allowed to remain there for one hour at room temperature. The sample is rinsed under cold running water, dried and evaluated against a scale which ranges from 1 to 5 where 5 represents complete stain removal. The treated portion of the pile height only (approx. 30% of pile height) was ~`~
evaluated for stain resistance.
''' ''~
'~
,,.,.,",~
.~ ",' In the examples a graduated ~cale ~rom l -to 5 was used to evaluate yellowing where 5 represents no yellowing and 4 represents acceptable yellowing.
In the examples, discoloration due to exposure to light was determined using AATCC test method with an exposure time of 40 hours. The exposed samples were graded using a graduated rating scale which ranges from l to 5, where 5 represents no discoloration and a rating of 4 is acceptable.
In examples 8 and 9 the following stain test was used:
20 ml. o~ an aqueous solution of sugar-sweet cherry ~lavoured KOOL-AID is poured into a 2 l/4" diameter ring placed on a carpet - -surface. The solution is pressed into the carpet and allowed to remain there for 8 hrs. at room temperature (22 degrees C.). The sample is rinsed under cold running water, dried and evaluated against a scale which ranges from l to 5 where 5 represents complete stain removal.
EXAMPLE l AND COMPARATIVE EXAMPLES A-l AND B-l In example l an aqueous solution o~ TEFLON MF was ;
prepared according to manufacturer's instructions at room temperature yielding a 6.25% solution. To this solution was added 1% of a 30% by weight phenolic resin pH adjusted to 6.5.
This solution was then topically sprayed onto undyed nylon 56 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approx 30% penetration of pile height) and allowed -to air dry for 12 hrs. at room temperature.
In comparative example A-l, an aqùeous solution o~ ~;
TE~LON MF was prepared according to manu~acturer's instructions and at 20~C yielding a 6.25% solution. This solution was then -12- ~ 327856 topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft, brushed into the pile (approx. 30% pene-tration of pile height) and allowed to air dry for 12 hrs. at room temperature (22 C.). .
In comparative example B~1 the undyed nylon 66 carpet was left untreated. -~
Each sample was tested for initial stain resistance characteristics and stain resistance after hot water extraction cleaning using 10 gm/L. of a commercial carpet cleaning solution TABLE 1 ~
EXAMPLE STAIN RESISTANCE AFTER CLEANIN~ STAIN .~
RESISTANCE .-A-l 1 1 B-l As can be seen ~rom the results in table 1 the treatment of the nylon 66 carpet with TEFLON NF together with a ~.
phenolic resin provides sta.in resistance before and after .,.
cleaning on the treated portion o~ the fibres and that TEFLON NF . .;
by itself offer~ negligible stain resistance initially and after ~:
cleaning. : ^
EXANPLE 2 AND COMPARATIVE EXAMPLES A-2 AND B-2 :~
In example 2 an aqueous solution of TEFLON MF was :~.
... . ..
prepared accordingly to manufacturer's instructions and at 20C
yielding a 6.25% solution. To this solution was added 1% of a ..
30% weight percent phenolic resin solution, pH to 6.5. This solution was then topically sprayed onto undyed nylon 66 . ': : .' "~
~ ... ..
~ -13- l 327 8 5 6 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approx 30% pene-tration of pile height) and allowed to air dry for 12 hrs. at room temperature. -In comparative example A-2, an aqueous solution of 1%
phenolic resin was prepared at 20C and the pH adjusted to 6.5.
This solution was then topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approx. 30% penetration of pile height) and allowed to air dry for 12 hrs at room temperature (220C.).
Each sample was tested for initial stain resistance characteristics and yellowing.
Example Stain Resistance Yellowin~
2 5 4.5 As can be seen from the results in table 2 the treatment of the nylon 66 carpet with TEFLON MF together with a phenolic resin causes substantially less yellowing on the treated portion of the fibre than the sulfonated phenolic resin by itself, while still exhibiting excellent stain resistance.
Furthermore the yellowing in example A-2 is unacceptable whereas the yellowing in example 2 is acceptable.
In example 3 a 1.0~ aqueous solution of a 30 percent by ~;
weight solution of a phenolic resin was prepared at 20 C and the pH adjusted to 6.5. This solution was then topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft., -14- l 3~7856 brushed into the pile ~nd allowed to air dry for 12 hrs. at room temperature.
In example A-3 a 1.0% aqueous solution of a 30 percent by weight solution of phenolic resin was prepared and to this solution was a~ded 2% of a 25 weight percent aqueous polyacrylic solution and the pH adjusted to 6.5. This solution was then topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft., brushed into the pile approx 30% penetration of pile height and allowed to air dry for 12 hrs at room temperature.
In example B-3 an aqueous solution of 2% of a 25 weight percent aqueous polyacrylic solution was prepared and the pH
adjusted to 6.5. This solution was then topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approx 30% penetration of pile height) and allowed to air dry for 12 hrs. at room temperature Each sample was tested for initial stain resistance characteristics and yellowing and stain resistance after hot water extraction cleaning using 10 gm/L. of a commercial carpet cleaning solution.
TABLE 3 ~ -Example Stain Resist Stain Resist After Yellowing Cleanin~ _ A-3 6 4 4.5 As can be seen from the results in table 3 the treatment of nylon 66 with phenolic resin in combination with polyacrylic yielding over-all superior results to either phenolic resin or polyacrylics by themselves. This comparison was done on the treated portion of the pile height or approximately 30% o~ pile height.
EXAMPLE 4 AND COMPA~ATIVE EXAMPLES A-4 AND B-4 In example 4 an aqueous solution of TEFLON MF was prepared according to manufacturer's instructions and at room temperature yielding a 6.5% solution. To this solution was added 1.5% of a 30% by weight phenolic resin solution, pH adjusted to 6.5. This solution was then topically sprayed onto the undyed nylon 6 carpeting at a rate of 20 ml/sq.ft., brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at room temperature.
In comparative example A-4, an aqueous solution of TEFLON MF was prepared according to manufacturer's instructions and at 20 C. yielding a 6.5X solution. This solution was then .
tôpically sprayed onto undyed nylon 6 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at room temperature. ;
In comparative example B-4 the undyed nylon 6 carpet was left untreated.
.
Each sample was tested for initial stain resistance characteristic~ and stain resistance after hot water extraction --cleaning usinq 10 gmJL. Or commercial carpet clesning solution.
: -,. :-, ,:' Example Stain ~esistance After Cleaning Stain ~esistance ~-4 As can be seen from the results in table 4 the treatment of the nylon 6 carpet with TEFLON MF together with a phenolic resin provides stain resistance before and after ~-cleaning on the treated portion of the fabric and the TEFLON NF :-by itself offers negligible stain resistance initially and after ~
cleaning. ;
EXAMPLE 5 AND COMPARATIVE EXAMPLES A-5 AND B-6 ;
In example 5 an aqueous solution of TEFLON MF was I prepared according to manufacturer'~ instructions and at a 20C -~
yielding a 6.25% ~olution. To this olution w~s added 1.5% of a 30% by weight phenolic resin solution pH adjusted to 6.5. This solution was then topically sprayed onto undyed nylon 6 carpeting -at the rate of 20 ml/sq.ft., brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at room temperature.
In comparative example A-5, an aqueous solution o~ 1.5% ;
phenolic resin was prepared at 20C. and the pH adjusted to 6.5. ~-This solution was then topically sprayed onto undyed nylon 6 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approximately 30% penetration of pile height) and allowed to air ~- dry for 12 hrs at room temperature. ; ~;
Each sample was tested for initial stain resistance ' '~
characteristics and yellowing.
. " ".
'''`''''~.'',' . . .; ~.
: . .
Example Stain Resistance Yellowin~
4.5 As can be seen from the results in table 5 the treatment of the nylon 6 carpet with TEFLON MF together with a phenolic resin caused substantially less yellowing on the treated portion of the fabric than the phenolic resin by itself, while still exhibiting excellent stain resistance. Furthermore the yellowing in example A-5 is unacceptable whereas the yellowing in example 5 is acceptable.
EXAMPLE 6 AND COMPARATIVE EXAMPLES A-6 AMD B-6 `
In example 6 an aqueous solution o~ 1.5% phenolic resin solution which was 30% by weight was prepared at 20C. and the pH ;
adjusted to 6.5. This solution was then topically sprayed onto undyed nylon 6 carpeting at the rate of 20 ml/sq.ft., brushed into the pile ~approximately 30% penetration of pile height~ and allowed to air dry for 12 hrs. at room temperature.
In example A-6 an aqueous solution of 1.5% phenolic resin was prepared and to this solution was added 2% of a 25 weight percent aqueous polyacrylic solution and the pH adjusted to 6.5. This solution was then topically sprayed onto the pile, brushed in the pile (approx. 30% penetration of pile height) and allowed to air dry for 12 hrs at room temperature.
In example B-6 an aqueous solution of 2% of a 25 weight percent aqueous polyacrylic solution was prepared and the pH ~-adjusted to 6.5. This solution was then topically sprayed onto ~;
undyed nylon 6 carpeting at the rate of 20 ml/sq.ft., brushed :
: ' - :
. ',.',,',''.
-18- l 327 ~ 5 6 into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at room -temperature.
Each sample was tested for initial stain resistance characteristics and yellowing, and stain resistance after hot water extraction cleaning using 10 gm/L of a commercial carpet cleaning solution.
Example Stain Resist Stain Resist After Yellowing CleaninR ~
4 3 `
As can be seen from the results in table 6 the ~`
treatment of nylon 66 with phenolic resin in combination with `
polyacrylic yields superior results to either phenolic resin OI' ... `
polyacrylics by themselves. This comparison was made base on the treated portion of the pile height or approximately 30% pile ~ -height.
In example 7 an aqueous solution of TEFLON MF was prepared according to manufacturer's instructions and at ;
200C yielding a 6.5% solution. To this solution was added 2% of a 30 weight percent solution of a phenolic resln solution and the pH adjusted to 6.5 with citric acid. This solution was then topically sprayed onto 100% wool carpeting at the rate of 20 `
ml/~q.ft. brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at roo~;;
temperature.
,.
. ....
~.
In comparative example A-7, an aqueous solution of TEFLON MF was prepared according to manufacturer's instruc-tions at a 20C yielding a 6.5% solution. This solution was then topically sprayed onto 100% wool carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approx. 30% penetra-tion of pile height) and allowed to air dry for 12 hrs at room temperature.
In comparative example B-7 the 100% wool carpeting was left untreated.
Each example was tested for initial stain resistance characteristics and stain resistance after hot water extraction using 10 gm/L of a commercial carpet cleaning solution.
Example Stain Resistance After Cleaning Stain Resistance As can be seen from the results in table 7 the treatment of the 100% wool carpet with TEFLON M~ together with a phenolic resin provides stain resistance before and after the cleaning and the TEFLON MF by itself ofers negligible stain resistance initially and after cleaning. -EXAMPLE 8 AND COMPARATIVE EXAMPLES A-8. B-8 AND C-8 In example 8, into a bath containing 0.5 gm. of BARTEX -SA, 300 gm. of water, and the pH adjusted to 2.3 with sulfam~ic acid, was placed a 20 gm. sample of undyed nylon 66 carpe-ting.
The temperature was raised to about 85C and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example A-8 into a bath con-taining 0.5 gm of a 30% by weight phenolic resin solution, 300 gm of wa-ter and a pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 66 carpeting. The temperature was raised to about 850C and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example B-8 into a bath containing 0.5 ~-gm of an alternative 30% by weight phenolic resin, 300 gms of water and the pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 66 carpeting. The temperature was raised to about 85C and maintained for 20 minutes, and then the sample was rinsed and dried at 110C for 15 minutes.
In comparative example C-8 into a bath containing 300 -gms of water and the pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of nylon 66 carpeting. The temperature was raised to about 850C and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes. `
Each example was tested for initial stain resistance ^
characteristics, yellowing and discoloration due to light.
TABLE 8 --;
ExampleStain Resistance YellowingDiscoloration Due to li~ht ~ . .
As can be seen from the test results in table 8, example 8 (acrylic polymer with phenolic resin) yields average ,., :~,'',,' ~ 327856 stain resis-tance when compared to both of the two comparative phenolic resin samples, negligible yellowing and acceptable discoloration due to light. Conversely examples A-8 and B-8 demonstrate good stain resistance but only acceptable yellowing and only unacceptable discoloration due to ligh-t.
EXANPLE 9 AND COMPARATIVE EXAMPLES A-9~ B-9 AND C-9 In example 9, into a bath containing 0.9 gm of BARTEX
SA, 300 gm of water and the pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 6 carpeting. The temperature was raised to 85OC and maintained for 20 minutes.
The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example A-9 into a bath containing 0.9 gm of a 30% by weight phenolic resin, 300 gm of water and pH
adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 6 carpeting. The temperature was raised to 85C and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example B-9 into a bath containing 0.5 gm of an alternate 30% weight phenolic reqin, 300 gm o~ water and the pH adiusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 6 carpeting. The temperature was raised ~ ;
to 85~C and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example C-9 into a bath containing 30G
gms of wat~r and the pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 6 carpeting. The te~perature was raised to 85OC and maintained for 20 minutes.
The sample was rinsed and then dried at 110~C for 15 minutes.
-22- ~ 327 8 5 6 Each example was -tested for initial stain resistance characteristics, yellowing and discolora-tion due to light.
Example Stain resistanceYellowing Discoloration Due to li~ht -As can be seen from the test results in table 9, example 9 ~acrylic polymer with phenolic resin) yields above average stain resistance when compared to both of the two -comparative phenolic resin samples, negligible yellowing and acceptable discoloration to light. Conversely example A-9 and B- -: -:
9 demonstrate marginal stain resistance and unacceptable discoloration due to light and marginal to unacceptable~^
yellowing.
In example 10, a 1.0% aqueous solution of a 30% by weight phenolic resin solution was prepared and to this solution was added 2% of a 25 weight percent aqueous polyacrylic solution, 0.1% of a commercial carpet cleaning solution and the pH adjusted `
to 10. This solution was then sprayed onto the pile of undyed nylon 66 carpeting, at the rate of 10 ml/sq.ft. brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at room temperature.
In comparative example A-10, a 1.0% aqueous solution of a 30X by weight phenolic resin was prepared and to this solution was added 2% of a 25 weight percent aqueous polyacrylic solution, 0.1% of a commercial carpet cleaning solution and the pH adjusted .
I ., -23- l 327 8 5 6 $o 10. This solution was -then sprayed onto the pile of undyed nylon 66 carpeting at the rate of 10 ml/sq.ft., brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry for 12 hrs. at room temperature.
Each example was tested for initial stain resistance characteristics and stain resistance after hot water extraction cleaning using 10 gm/L of commercial carpet cleaning solution.
ExampleStain Resist Stain Resist After _ _ Cleanin~
~-5 3-4 As can be seen from the results in table 10 the treatment of nylon 66 carpeting at a pH level of 10 shows only slightly inferior stain resistance to A-10 treated at a pH level of 6.5. The presence of a carpet cleaning solution had no effect on the antistain characteristics.
In example 11 an aqueous solution of TEFLON MF, was prepared according to manufacturer's instructions at room temperature yielding a 6.25% solution. To this solution was added 1% of a 30% by weight phenolic resin solution, Ph adjusted to 6.5. This solution was then topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft., brushed into the pile (approximately 30% penetration of pile height) and allowed to air dry at room temperature for 12 hrs.
In comparative example A-ll a 1.5% a~ueous solution of BA~TEX A200 was prepared at room temperature with a resultant pH
of 6.5. This solution was then topically sprayed onto undyed nylon 66 carpeting at the rate of 20 ml/sq.ft., brushed into the :, ..
~ '`.',"
-2~ 2 7 8 5 6 pile (approximately 30% pene-tration of pile height~ and allowed to air dry at room temperature for 12 hrs.
Each sample was tested for initial s-tain resis-tance characteristics, s-tain resistance after hot water extraction ~ -cleanin~ using 10 ~m/L of a commercial carpet cleaning solution, -yellowing and discoloration due to light.
:, .
TABLE 11 ~-Example Stain After Cleaning Yellowing Discoloration Resistance stain resistance due to li~ht 11 5 4 4.5 4 ;
A-11 5 4.5 4.5 4-5 --As can bee seen from the results in table 11 the treatment of nylon 66 carpeting with either of the antistain combinations yields excellent results in all tests. -Example 12 and comparative Examples A-12. B-12 and C-12 In example 12, into a bath containing 0.9 gm of Bartex WX, 300 gm of water and pH adju~ted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 6 carpeting. The temperature was raised to 85C and maintained for 20 minutes.
The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example A-12 into a bath containing 0.9 gm of a 30% by weight phenolic resin, 300 gm of water an pH
adjusted to 2.3 with sulfamic acid was placed a 20 ~m sample of :
undyed nylon 6 carpeting. The temperature was raised to 85C and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes. ;
In comparative example B-12 into a bath containing 2%
of a 25% wei~ht acrylic resin, 300 gm of water and pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon I . ' ';
.~.
,'....
-25~ l 327856 6 carpeting. The temperature was raised to 85OC and maintained for 20 minutes. The sample was rinsed and then dried at 1104C
for 15 minutes.
In compara-tive example C-12 into a bath containing 300 gm of wa-ter and the pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 6 carpeting. The temperature was raised to 85C and maintained for 20 minutes. ~ ;
The sample was rinsed and then dried at llO~C for 15 minutes.
Each example was tested for initial stain resistance characteristics, yellowing and discoloration due to light.
Example Stain ResistanceYellowingDiscoloration Due to Li~ht -As can be seen form the test results in table 12, example 12 Bartex WX (wax emulsion and phenolic resin~ yields excellent stain resistance when compared to phenolic resin alone or acrylic resin alone.
Conversely example A-12 demonstrates acceptable stain resist&nce and yellowing, and unacceptable discoloration due to light. ;
Example B-12 demonstrates unacceptable stain resistance, acceptable yeIlowing, and discoloration due to light.
It is clearly evident that example 12 shows that Bartex -WX, is superior to all other examples.
. , .,.".,;~
,., -26- l 327856 ~:
Example 13 and comparative Examples A-13, B-13 and C-13 In example 13, into a bath containing 0.9 gm of Bartex WX, 300 gm of water and pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 66 carpetingr. The temperature was raised to 85~C and maintained for 20 minutes~ ~
The sample was rinsed and then dried at 110C for 15 minutes. -In comparative example A-13 into a bath containing 0.9 gm of a 30% by weight phenolic resin, 300 gm of water an pH
adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 66 carpeting. The temperature was raised to 85C
and maintained for 20 minutes. The sample was rinsed and then dried at 110C for 15 minutes.
In comparative example B-13 into a bath containing 2%
of a 25% weight acrylic resin, 300 gm of water alld pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 66 carpeting. The temperature was raised to 85C and maintained for 20 minutes. The sample was rinsed and then dried at 110C
for 15 minutes.
In comparative example C-13 into a bath containing 300 gm of water and the pH adjusted to 2.3 with sulfamic acid was placed a 20 gm sample of undyed nylon 66 carpeting. The temperature was raised to 85C and maintained for 20 minutes.
The sample was rinsed and then dried at 110C for 15 minutes.
Each example was tested for initial stain resistance characteristics, yellowing and discoloration due to light.
' ~
.
-27- l 327856 Example Stain ResistanceYellowing~iscoloration _ ~ue to Li~ht 13 5 5 . :
A-13 4 4 3 .~.
B-13 3 4~5 5 C-13 1 5 5 .
As can be seen form the test results in table 13, example 13 Bartex WX (wax emulsion and phenolic resin) yields excellent stain resistance when compared to phenolic resin alone or acrylic resin alone.
Conversely example A-13 demonstrates acceptable stain resistance and yellowing, and unacceptable d.iscoloration due to ~.-light. ~.
Example B-13 demonstrates unacceptable stain resistance, acceptable yellowing, and discoloration due to light.
It is clearly evident that example 13 shows that Bartex WX, is superior to all other examples.
''' ;-The foregoing is by way of example only and the invention should be limited only be the scope of the appended .
claims.
'''~"''",.'~' , "
Claims (14)
1. The method of enhancing soil- and stain-resisting properties of polyamide and wool fabrics comprising applying to the fabric an aqueous solution containing the condensation products of formaldehyde with a compound selected from the group consisting of bis(hydroxyphenyl) sulfone, phenylsulfonic acid, dihydroxy diphenyl sulfone, and benzene sulfonic acid: and at least one material selected from the group consisting of a wax emulsion and a fluorochemical: and a polymer selected from the group consisting of acrylic polymer and copolymer.
2. The method according to claim 1 where the solution is an aqueous solution having a pH not exceeding 10.
3. The method according to claim 1 where the solution is an aqueous solution having a pH below 7 applied to the fabric by spraying at room temperature and in the absence of any heat fixation.
4. The method according to claim 1 wherein the condensation product is a polymer of benzene sulfonic acid and formaldehyde, the fluorochemical is a nonionic or anionic water based fluorochemical, the acrylic polymer is polymerized 2-methyl propenoic acid ethyl ester, and wherein the solution contains citric acid in an amount sufficient to provide a pH
below 7.
below 7.
5. The method according to claim 1 where the fluorochemical is present in the solution in an amount of between 0.1 percent and 20 percent.
6. The method according to claim 5 where the solution contains 0.1 percent fluorochemical.
7. An aqueous solution for enhancing the soil- and stain-resistant properties of polyamide and wool fabrics comprising in admixture a condensation product of an aromatic sulfonic acid and formaldehyde together with wax emulsion, a nonionic water based fluorochemical, and an acrylic polymer, said admixture having a pH below 10.
8. The aqueous solution according to claim 7 wherein the pH is below 7.
9. A fibrous material selected from the group consisting of polyamide and wool fibrous materials having applied thereto an aqueous solution containing a polymer of a phenolic compound selected from the group consisting of bis(hydroxyphenyl) sulfone and benzene sulfonic acid with an aldehyde: a fluorochemical and an acrylic polymer together with citric acid in an amount sufficient to provide a pH below 7.
10. The method of enhancing the soil- and stain-resistance of a polyamide fabric by immersing or totally wetting out said fabric with an aqueous solution containing a polymer of a phenolic compound selected from the group consisting of bis(hydroxyphenyl) sulfone, phenylsulfonic acid, dihydroxy diphenyl sulfone and benzene sulfonic acid with an aldehyde: a fluorochemical and an acrylic polymer: said solution having a pH
below 7.
below 7.
11. The method according to claim 10 where the fabric is subsequently sprayed with a fluorochemical water and oil repellent.
12. The method according to claim 10 where the fabric is subsequently sprayed with a fluorochemical water and oil repellent which also contains an acrylic polymer or copolymer and a phenolic resin.
13. The method of enhancing the soil- and stain-resistant properties of polyamide and wool fabrics comprising applying to the fabric an aqueous solution containing the condensation product of formaldehyde with a phenolic compound selected from the group consisting of bis(hydroxy phenyl) sulfone, phenylsulfonic acid, dihydroxy diphenyl sulfone, and benzene sulfonic acid: and at least one material selected from the group consisting of a wax emulsion and an acrylic polymer;
said aqueous solution having a pH below 10.
said aqueous solution having a pH below 10.
14. The method of enhancing the soil- and stain--resistant properties of polyamide and wool fabrics comprising applying to the fabric an aqueous solution containing the condensation product of formaldehyde with a phenolic compound selected from the group consisting of bis(hydroxyphenyl) sulfone, phenylsulfonic acid, dihydroxy diphenyl sulfone, and benzene sulfonic acid, and a wax emulsion: said aqueous solution having a pH below 10.
Priority Applications (8)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA 610371 CA1327856C (en) | 1989-09-05 | 1989-09-05 | Method of enhancing the soil- and stain-resistance characteristics of polyamide and wool fabrics, the fabrics so treated, and treating composition |
| US07/433,508 US5073442A (en) | 1989-09-05 | 1989-11-08 | Method of enhancing the soil- and stain-resistance characteristics of polyamide and wool fabrics, the fabrics so treated, and treating compositions |
| GB9122904A GB2260994B (en) | 1989-09-05 | 1991-10-29 | Soil and stain resistance of fabrics |
| GB9205004A GB2260995B (en) | 1989-09-05 | 1991-10-29 | Soil and stain resistance of fabrics |
| BE9101031A BE1007018A5 (en) | 1989-09-05 | 1991-11-08 | PROCESS FOR IMPROVING THE RESISTANCE TO SOILING AND TAMPERING OF WOOL AND POLYAMIDE TISSUES. |
| FR9114251A FR2683836B1 (en) | 1989-09-05 | 1991-11-19 | PROCESS FOR IMPROVING SOIL AND STAIN RESISTANCE PROPERTIES OF POLYAMIDE AND WOOL FABRICS; AQUEOUS SOLUTION FOR APPLYING THE PROCESS; POLYAMIDE OR WOOL FIBROUS MATERIAL, TREATED BY THE PROCESS. |
| CH03399/91A CH689367B5 (en) | 1989-09-05 | 1991-11-20 | A method for improving the resistance of polyamide fabrics and wool against dirt and stains, tissues treated with this method and compositions for its implementation. |
| DE4138382A DE4138382A1 (en) | 1989-09-05 | 1991-11-22 | METHOD FOR IMPROVING THE DIRT AND STAIN RESISTANCE OF POLYAMIDE AND WOOLEN SUBSTANCES, SO-TREATED SUBSTANCES, AND MEANS FOR IMPLEMENTING THE PROCESS |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA 610371 CA1327856C (en) | 1989-09-05 | 1989-09-05 | Method of enhancing the soil- and stain-resistance characteristics of polyamide and wool fabrics, the fabrics so treated, and treating composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1327856C true CA1327856C (en) | 1994-03-15 |
Family
ID=43807113
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA 610371 Expired - Lifetime CA1327856C (en) | 1989-09-05 | 1989-09-05 | Method of enhancing the soil- and stain-resistance characteristics of polyamide and wool fabrics, the fabrics so treated, and treating composition |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US5073442A (en) |
| BE (1) | BE1007018A5 (en) |
| CA (1) | CA1327856C (en) |
| CH (1) | CH689367B5 (en) |
| DE (1) | DE4138382A1 (en) |
| FR (1) | FR2683836B1 (en) |
| GB (2) | GB2260994B (en) |
Families Citing this family (76)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5310828A (en) * | 1989-04-20 | 1994-05-10 | Peach State Labs, Inc. | Superior stain resistant compositions |
| US5223340A (en) * | 1989-04-20 | 1993-06-29 | Peach State Labs, Inc. | Stain resistant polyamide fibers |
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-
1989
- 1989-09-05 CA CA 610371 patent/CA1327856C/en not_active Expired - Lifetime
- 1989-11-08 US US07/433,508 patent/US5073442A/en not_active Expired - Lifetime
-
1991
- 1991-10-29 GB GB9122904A patent/GB2260994B/en not_active Expired - Fee Related
- 1991-10-29 GB GB9205004A patent/GB2260995B/en not_active Revoked
- 1991-11-08 BE BE9101031A patent/BE1007018A5/en not_active IP Right Cessation
- 1991-11-19 FR FR9114251A patent/FR2683836B1/en not_active Expired - Fee Related
- 1991-11-20 CH CH03399/91A patent/CH689367B5/en not_active IP Right Cessation
- 1991-11-22 DE DE4138382A patent/DE4138382A1/en not_active Ceased
Also Published As
| Publication number | Publication date |
|---|---|
| GB9205004D0 (en) | 1992-04-22 |
| CH689367GA3 (en) | 1999-03-31 |
| GB2260995B (en) | 1995-11-01 |
| GB2260995A (en) | 1993-05-05 |
| FR2683836A1 (en) | 1993-05-21 |
| GB2260994A (en) | 1993-05-05 |
| GB2260994B (en) | 1995-11-01 |
| US5073442A (en) | 1991-12-17 |
| GB9122904D0 (en) | 1991-12-11 |
| CH689367B5 (en) | 1999-09-30 |
| BE1007018A5 (en) | 1995-02-21 |
| FR2683836B1 (en) | 1994-11-10 |
| DE4138382A1 (en) | 1993-05-27 |
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