Classifications

• • 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
  • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
  • D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
  • D06M15/29—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides containing a N-methylol group or an etherified N-methylol group; containing a N-aminomethylene group; containing a N-sulfidomethylene group
• • 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
  • Y10T442/2164—Coating or impregnation specified as water repellent
  • Y10T442/2172—Also specified as oil repellent
• • 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
  • Y10T442/2262—Coating or impregnation is oil repellent but not oil or stain release
  • Y10T442/227—Fluorocarbon containing

Definitions

• the precured fabrics are those for which the crosslinking reaction has occurred prior to transformation of the fabric into a garment or other article of commerce.
• Post cured fabrics are those fabrics which are subjected to the crosslinking reaction subsequent to the transformation of the fabric into a garment or other article of commerce.
• the precured and post cured fabrics may contain any of a number of natural or synthetic materials.
• these fabrics include synthetic, man-made fibers.
• These synthetic fibers offer tremendous advantages to the fabrics as opposed to fabrics containing only the natural materials.
• One drawback, however, is the fact that the synthetic fibers have a propensity to soiling and as such, the garment during normal wear may come into contact with oily type materials which are accepted due to the oleophilicity of the synthetic fibers. These oily type materials, however, are very hard to remove due to the hydrophobic properties of the synthetic fibers.
• soil release does not infer soil resistance, but only the characteristic that once a fabric is soiled, it may then be successfully cleaned via the normal wash cycle.
• fabrics, and/or garments that are treated to have soil release characteristics also have the characteristic of not taking up soil from the wash water, i.e., soil in the wash water will not be redeposited onto the garment being washed.
• the fluorochemical type water repellents are probably the most commonly used water repellent today.
• Two commercially available fluorochemical compositions are FC- 208, the fluorocarbon ingredient of Scotchgard treated fabrics, sold by Minnesota Mining and Manufacturing Company and Zepel, a water repellent fiuorochemical sold by E. I. du Pont de Nemours & Co.
• a certain degree of oil repellency is generally achieved with the water repellency imparted to the fabrics treated with the fluorocarbons.
• An object of the present invention is to provide textile material with the heretofore unattainable combination of soil and water repellency characteristics together with soil release characteristics.
• a further object of the invention is to provide a fabric including synthetic polymeric fibers which has soil and water repellency and soil release characteristics.
• Another object of the invention is to provide a fabric from which stains can be removed by laundering without destroying the water and oil repellency characteristics of the fabric.
• An additional object of the invention is to provide a fabric including synthetic polymeric fibers which not only has the combination of water and oil repellency and soil release characteristics but also possesses durable press and/ or wash and wear characteristics.
• water repellency, oil repellency and soil release characteristics are imparted to a textile material by a process which comprises applying to the textile material a soil release polymer and a water and oil repellent material.
• the textile material is subjected to textile resin curing conditions.
• a textile resin and a textile resin catalyst also are applied to the textile material.
• the process of the present invention may be used to treat a Wide variety of textile materials, i.e., fabrics made exclusively from naturally occurring fibers, fabrics made exclusively from synthetic polymeric fibers, as well as blends of natural and synthetic fibers.
• the process of the present invention may be utilized on fabrics containing cellulosic fibers, for example, cotton, viscose, regenerated cellulose, etc.
• fabrics of synthetic fibers which may be successfully employed in the practice of the present invention include those made with polyamide, acrylic and particularly polyester fibers, i.e., various types of Dacron, a registered trademark of E. I. du Pont; Fortrel, a registered trademark of Celanese; Kodel, a registered trademark of Eastman Kodak, etc.
• Blends of natural and synthetic fibers which may be utilized to prepare fabrics according to the present process include fabrics comprising 50% polyester and 50% cotton; 65% polyester and 35% cotton; etc.
• the proportion of the water repellent compound utilized to treat the fabric according to the process of the invention is generally in the same range as that commonly used for imparting water repellency to fabrics.
• the fluorocarbon concentration is at least about 0.1% by weight of the pad bath or treating solution with the upper limit being dependent upon the degree of water repellency desired. Amounts greater than about 1% generally meet the water and oil repellency standards for rainwear recognized by the industry. When the proportion of the fluorocarbon is less than about 1%, a significant degree of oil repellency is still achieved although the water repellency level may be reduced.
• between about 0.01% and 5% by weight of the water repellent shall be present on the textile material on a dry weight basis and preferably between about 0.1% and 2%.
• textile resin includes both monomers and polymers which when applied to a textile material and reacted under proper conditions undergo polymerization and/or condensation and are transformed to the thermoset state.
• Textile resins that may be employed when practicing the present invention include epoxy, acetal, aminoplast resins, etc., with the aminoplast resins being preferred. These nitrogen containing resins when applied to a textile material in the presence of a catalyst at temperatures of from C. to about 300 C. are transformed into the thermoset state.
• the aminoplast resin condenses with the cellulose molecules and when vinyl groups are present in the aminoplast resin, it undergoes adidtion polymerization with itself and also with the cellulose molecule if irradiated.
• the cured textile resin on the textile material affords the textile material a durable press and/ or wrinkle resistant characteristic.
• aminoplast resins that may be employed according to the present invention are the urea formaldehydes, e.g., propylene urea formaldehdye, dimethylol urea formaldehyde, etc.; melamine formaldehydes, e.g., tetramethylol melamines, pentamethylol melamines, etc.; ethylene ureas, e.g., dimethylol ethylene urea, dihydroxy dimethylol ethylene urea, ethylene urea formaldehyde, hydroxy ethylene urea formaldehyde, etc., carbamates, e.g., alkyl carbamate formaldehydes, etc.; formaldehyde-acrolein condensation products; formaldehyde-acetone condensation products; alkylol amides, e.g., methylol formamide, methylol acetamide, etc.; acrylarnides, urea formal
• R hydrogen, lower alkyl or CX-CR CHR
• R hydrogen or methyl hydrogen or lower alkyl
• R" hydrogen, hydroxyl or lower alkyl
• R hydrogen, lower alkyl, alkylol or alkenol X sulfur or oxygen and where may have substituted therefor or sulfonium if desired.
• the amount of the textile resin employed is primarily determined by the ultimate use of garments or articles prepared from the fabric. Very small amounts of the resin will afford some improvement and large amounts even greater improvements, but the larger amounts of resin generally adversely affect the hand of the fabric. Hence, the amount of resin employed is preferably that which will afford good crease retention and flat dry properties while not adversely affecting the hand.
• the amount of textile resin in the pad bath may vary between about 2 and 30% by weight. Resin applied to the fabric should be in the range of about 2 to 20% based on the dry Weight of the fabric and preferably in the range of about 4 to 9%.
• Catalysts employed within the scope of the present in vention depend upon the specific textile resin that is applied to the textile material. For instance, if the textile resin has a functional group that is reactive under acidic conditions, then an acid catalyst is used. Likewise, when a functional group is present that is reactive under alkaline conditions, then a base catalyst is used. Furthermore, both acid and base catalysts may be used when both types of functional groups are present in the textile resin. In this instance, the catalyst may be added separately or together. When they are added together, one must be a latent catalyst, i.e., one that will not initiate its reaction during the opposite type reaction, but may be activated subsequently under proper catalytic conditions.
• the catalysts useful in activating the acid or base reactive groups are those conventionally used to activate the reaction of textile resins containing the same group for reaction with hydroxy groups of cellulose.
• latent acid or base acting catalysts are utilized, that is, compounds which are acidic or basic in character under the curing conditions.
• the most common acid acting catalysts are the metal salts, for example, magnesium chloride, zinc nitrate and zinc fluoroborate and the amino salts, for example, monoethanolarnine hydrochloride and 2-amino-2-methylpropanol nitrate.
• the base acting catalyst preferably is a compound which does not initiate substantial reaction between the base reactive group and hydroxy groups of cellulose under normal acid conditions, but does initiate substantial reaction under prescribed conditions, such as elevated temperature or some other activating means, as through use of another chemical compound.
• an alkali metal sulfite can be padded ontothe fabric and be decomposed into strongly basic alkali metal hydroxide by including small amounts of formaldehyde in the steam used for curing.
• the latent base acting catalyst utilized herein preferably comprises alkali-metal salts, such as alkali-metal carbonates like sodium carbonate, which is neutral to mildly alkaline, for example, pH of about 8.5 on the fabric but decomposes at temperatures in excess of about C. to form the stronger base sodium oxide which will initiate substantial reaction at the elevated temperatures utilized during curing.
• alkali-metal salts such as alkali-metal carbonates like sodium carbonate, which is neutral to mildly alkaline, for example, pH of about 8.5 on the fabric but decomposes at temperatures in excess of about C. to form the stronger base sodium oxide which will initiate substantial reaction at the elevated temperatures utilized during curing.
• Sodium carbonate may be utilized if desired since the pH in the fabric produced by this compound in normal conditions is generally insufficient to initiate the desired degree of reaction under normal temperature conditions.
• Additional base acting catalysts include potassium bicarbonate, potassium carbonate, sodium silicate, alkali metal phosphates, such as sodium or potassium phosphates, barium carbonate quaternary ammonium hydroxides and carbonates, for example, lauryl trimethyl ammonium hydroxides and carbonates and the like.
• the amount of catalyst to be utilized is that conventionally used in activating the reaction between textile resins and hydroxy groups of cellulose, for example, up to about 15% by weight of an acid acting catalyst in the application bath with the preferred range being from about 1% to about 7%.
• a preferred range for the base acting catalyst is again the conventional amount and is generally between about 0 .2% to about 16 preferably about 2 to 16%.
• the amount of catalyst to be utilized will further depend in part on the temperature at which the reaction is conducted and the amount of catalyst consumed in the reaction. For example, when base catalysts are utilized and if a highly acidic group is released during the reaction, the amount of base applied to the textile material should be at least sufficient to provide an excess of base in addition to that which is consumed by the highly acidic group.
• soil release in accordance with the present invention refers to the ability of the fabric to be washed or otherwise treated to remove soil and/or oily materials that have come into contact with said material.
• the present invention does not per se prevent the attachment of soil or oily materials to the fabric, but hinders such attachment and renders the heretofore uncleanable fabric now susceptible to a successful cleaning operation. While the theory is still somewhat of a mystery, soiled, treated fabric when immersed in the detergent containing wash water experiences an agglomeration of the oil at the fabric surface. This water is basic in nature and it has been determined that soil release is best realized in wash water that is basic in nature. These globules of oil are then removed from the fabric and rise to the surface of the wash water.
• An added feature of the present invention is the prevention of soil redeposition from the wash water.
• One of the greatest disadvantages of the synthetic polymers is the feature that even after removing the soil by washing, there is the continued danger that the soil will be redeposited onto the fibers from the wash water before the garment is removed therefrom. It has been observed that the soil releasability of the presently treated fabric diminishes after repeated washings. Even after the ability to remove soil from the fabric has diminished, however, the observation has been made that the prevention of redeposition of soil from the wash water remains potent. This phenomenon likewise is unexplainable, but it has been established that the troublesome soil is negatively charged and presumably there remains enough acid on the fabric to repel the negatively charged soil.
• the soil release polymer of the present invention may be selected from a large number of different compounds, for example, acid polymers, low molecular weight polyesters, etc.
• the polymer employed advantageously is capable of forming a film around the fibers that constitute the textile material. Softness of the film is desirable for if the film is too hard, the hand of the textile material may be adversely affected.
• the film preferably has hydrophilic properties and is at least partially insoluble in water. The film, if water soluble, would, of course, be easily washed from the fabric.
• the polymer from which the film is formed may, however, be water soluble if applied with a textile resin, for during the curing process, the polymer if water soluble, is transformed to a water insoluble film.
• the polymer when applied to a substrate without a textile resin, it may likewise be water soluble if the substrate is such that the soil removal is only required once.
• An acid content of at least weight percent acid calculated as acrylic acid in the soil release polymer from which the film is formed is desirable, and preferably at least weight percent. It has further been observed that acid polymers that afford soil release have a carbon atom to acid group ratio in the repeat group in the range of 2:1 to :1, and that an air dried film cast therefrom has a water of imbibition of at least 89%.
• synthetically produced acid polymers within the scope of the present invention may be prepared from any of the polymerizable organic acids, i.e., those having reactive points of unsaturation, e.g., one of the acrylic acids. These polymers may be homopolymers of the acids, or interpolymers of an acid and other monomers copolymerizable therewith so long as at least 10' weight percent acid monomer is present in the polymer.
• Exemplary of polymerizable acids that may be used are acrylic acid, methacrylic acid, maleic acid, fumaric acid, itaconic acid, crotonic acid, cinnamic acid, polymerizable sulfonic acids, polymerizable phosphoric acids, etc.
• Monomers that may be interpolymerized 'With the acids include any monomers capable of copolymerizing with the acids and which Will not detrimentally affect the film-forming properties of the polymer.
• Suitable monomers include, esters of the above acids prepared by reacting the particular acid with an alkyl alcohol, e.g., acrylic esters such as ethyl acrylate, methyl acrylate, propyl acrylate, isopropyl acrylate, methyl methacrylate, ethyl methacrylate, 2-ethylhexyl acrylate, butyl acrylate, etc.; alkyl fumarates, maleates, crotonates, ciunamates, etc.
• Examples of some of the synthetic acid polymers that may be used according to the present invention are polymerization products of:
• ethyl acrylatezacrylic acid ethyl acrylate acrylic acid: acrylamide butyl acrylatezacrylic acid ethyl acrylatezmethacrylic acid ethyl acrylate: itaconic acid methyl methacrylateracrylic acid Z-cthyl hexyl acrylatezacrylic acid acrylamide acrylic acid butyl acrylate acrylic acid: acrylamide ethyl acrylatezacrylic acid:Nmethylol acrylamide ethyl acrylate acrylic acid: styrene ethyl acrylatezacrylic acidzhydroxy propyl methacrylate ethyl acrylate:acrylic acidzdivinyl benzene ethy lacrylate:acrylic acidzallyl acrylamide ethyl acrylate:acrylic acid: glycidyl acrylate ethyl acrylate: itaconic acid ethyl acrylatezsod
• the preferred acid polymers include (1) copolymers of an acrylic ester such as ethyl acrylate and an acrylic acid that are prepared by polymerizing a co-monorner mixture of from about 10 to parts of the acrylate and about 20 to parts of the acrylic acid and advantageously from about 50 to 80 parts of the acrylate and 20 to 50 parts of the acrylic acid; (2) copolymers of propyl or isopropyl acrylate and acrylic acid wherein the copolymers are prepared by po lymerizing a monomer mixture of from about 40 to 57 parts propyl or isopropyl acrylate and about 43 to 60 parts of acrylic acid; (3) copolymers of butyl acrylate and acrylic acid prepared by polymerizing a co-monomer mixture of from about 30 to 70' parts butyl acrylate and about 70 to 30 parts of acrylic acid; (4) copolymers of Z-ethyl-hexyl-acrylate and acrylic acid prepared
• the acid polymers suitable for use in practicing the present invention form a hydrophilic film upon drying and afford soil release ability at that point. For unknown reasons, further treatments and/or ingredients will enhance the soil release ability of the substrate. If the substrate having the acid polymer thereon is subjected to textile resin curing conditions, the durability of the soil release ability is enhanced. Likewise the presence of a textile resin catalyst during the textile resin curing conditions further improves soil release ability. Still further, the soil release finish is much more lasting on a substrate when the acid polymer is subjected to textile resin curing conditions in the presence of an aminoplast textile resin. It is known that the film covers the hydrophobic synthetic fiber contents of the textile material without any reaction therewith. What is not understood, however, is the durability of the soil release characteristic.
• Soil release polymers like the textile resins, give some improvement at very low levels on the fabric. Accordingly, as the amount of soil release polymer is increased, the ability of the fabric to release soil increases. Thus, the upper limit on the amount of soil release polymer is determined by economics and resulting adverse effects on the fabric, e.g., the hand of the fabric. Furthermore, practically speaking there is a set range of soil release polymer dictated by commercial success.
• the acid polymers are emulsion polymers containing varying amounts of solids, normally 5 in the range of about to 50 weight percent.
• the polymer emulsion should be present in the pad bath or other application medium in the range of about 2.5 to weight percent. Otherwise stated, there should be from about 0.25 to 5 weight percent of acid polymer solids applied to the substrate, based on dry Weight, and preferably 1.0 to 1.5 weight percent.
• composition used to impregnate the textile material according to the present invention is not limited to including only the possible ingredients heretofore mentioned, e.g., textile resin, textile resin catalyst, soil release polymer and water repellent compound.
• other ingredients may be employed such as, for example, emulsifying agents, wetting agents, softeners, etc., and numerous other compounds that enhance the physical characteristics of the fabric.
• the composition may be applied to the substrate in any suitable manner. For instance, padding of the solution onto fabric is preferred because of ease of operation at that particular stage of the development.
• the composition may be sprayed on as a liquid; the substrate may be treated with vapors of the compounds if convenient; the substrate may be dipped, etc.
• the applicator system is adjusted to provide from 30 to weight percent wet pickup by the fabric from the pad bath.
• the aminoplast textile resin When the aminoplast textile resin is applied to the substrate, e.g., textile materials, along with the soil release polymer and a fluorocarbon water repellent compound, they may be simultaneously applied from the same pad bath. Simultaneous application is not required though and beneficial results may be realized by first applying the soil release polymer followed by separate applications of the textile resin and the water repellent compound and curing of the textile resin. Insofar as separate application is concerned, however, where the textile resin is applied first and cured and the soil release polymer and the water repellent compound are added separately thereafter, initial soil release abiilty is outstanding, but not nearly so durable as the simultaneous application or the separate addition where textile resin, soil release polymer and water repellent all are present during curing of the textile resin.
• the soil release polymer and the water repellent may be employed.
• the soil release polymer and the water repellent may be employed.
• the ultimate article of manufacture is not one that will be washed or cleaned on a weekly basis, for instance, the desirable property might possibly be to have a very superior initial soil release property.
• An example would be upholstery for automobiles, seat covers, wall coverings, etc.
• Garments made from the fabrics treated according to the process of the present invention require no additional steps than normal for the preparation of the conventional durable press garments.
• the garment may be folded and pressed on conventional equipment, for example, a Hoffman press.
• the pressing cycle utilized is standard in the. industry and generally involves pressing of the garment for a short period of time, followed by a curing operation in an oven.
• the garment may be set in a desired configuration under hot, dry conditions, such as by hot pressing without steaming, for example, at temperatures of up to about 300 C. for as long as necessary to cure the resin.
• the textile resin may be selected from several general types. According to the type resin selected, one of the following processes may be generally followed to achieve the novel garments produced by the present invention. In each type procedure, the methods of application and order of application of textile resin, soil release polymer, catalysts, -water repellent, etc., may be varied as described supra.
• Type I Apply textile resin having one type functional group, textile resin catalyst, soil release polymer and water repellent to fabric.
• Type II Apply textile resin having more than one type of functional group, textile resin catalysts for each type functional group, soil release polymer and water repellent to fabric.
• Type HI Apply textile resin having more than one type of functional group, one type being sites of ethylenic unsaturation, a textile resin catalyst, a soil release polymer and water repellent to the fabric.
• the ultimate curing of the textile resin may be accomplished prior to the manufacture of the garment whereby a good Washand-wear fabric having water and oil repellency and soil release properties is produced.
• Procedures of Types I, II and III relate to the process of the present invention being applied to a textile material to afford said textile material water and oil repellency, soil release and durable press or wash and wear characteristics. Otherwise than above shown, the various materials are applied and dried, subjected to textile resin curing conditions, etc., according to the specifications described herein.
• the drying temperatures that are insuflicient to initiate the catalysis are, of course, dependent upon the particular catalyst being employed. In general, however, the drying step is conducted at a rate of approximately 10 to 70 yards per minute at temperatures ranging from about 225 to 300 F. preferably in a tenter frame.
• the drying temperature range overlaps to some degree with the curing temperature range set forth below. When drying in the overlapping portion of the drying and curing ranges, it is important that there be no premature curing of the textile resin. Time is the prime variable and when drying the substrate in the higher end of the drying temperature range, care must be taken to avoid heating the substrate for a time sufficient to initiate catalysis that would at least partially cure the textile resin.
• Irradiation techniques may be employed according to the process of the present invention when a textile resin having ethylenic unsaturation is applied to the textile material.
• An insulating core transformer operated at a potential varying between one hundred thousand electron volts and five hundred thousand electron volts may be successfully used to irradiate the textile material.
• Such a transformer is commercially available from High Voltage Engineering Corporation, Burlington, Mass.
• the amount of ionizing irradiation necessary according to the present invention is at least 32 electron volts for each ion pair formed. Thus irradiation of 32 volts and above is effective. Both high energy particle and ionizing irradiation are useful according to the present invention.
• the preferred dosage of irradiation according to thepresent invention is in the range of one thousand rads to one hundred megarads, a rad being the amount of high energy irradiation of the type which results in energy absorption of one hundred ergs per gram of absorbing material. More preferably, however, the irradiation dosage ranges from 0.5 to 5 megarads.
• Curing of the textile resin is accomplished by subjecting the textile material having the textile resin thereon to conditions such that the catalyst initiates a crosslinkiug reaction between functional groups of the resin and hydroxyl groups of the cellulose in the textile material and converts the resin to the thermoset state.
• the catalyst initiates a crosslinkiug reaction between functional groups of the resin and hydroxyl groups of the cellulose in the textile material and converts the resin to the thermoset state.
• the resin adheres to the material and is converted to a thermoset state.
• Temperature is the prime mover and generally a temperature in the range of 100 C. to about 300 C. is sufficient.
• the curing medium that supports the necessary temperature may be any substance that is inert to both the fabric and the ingredients applied thereto, e.g., hot air, steam, etc.
• the first being conducted at a temperature lower than the second and insufficient to initiate the second type of catalysis, e.g., a first partial curing step to initiate alkaline catalysis and a subsequent curing step to initiate acid catalysis and also convert the resin to the thermoset state.
• the duration of the various processing steps varies diversely with the particular ingredients employed. In each situation, however, the treatment time is that necessary to sufliciently cause reaction of and/or curing of the textile resin, and preferably, between about 0.1 and 30 minutes.
• All soil release values are determined by comparison to a set of standards having numerical ratings from 1.0 to 5.0, with 1.0 representing very poor stain removal and 5.0 being virtually complete removal of the stain.
• the fabrics are stained with mineral oil. After staining the fabric is washed one time in a Kenmore automatic washer using one cup of Tide detergent (sold by Procter and Gamble) and a wash water temperature at about F. The fabric is dried for approximately 40 minutes at a temperature of about F. The stains in the dried fabric are compared with the set of standards.
• the values listed in the tables under the headings 5 and 10 washes represent staining after 5 or 10 normal washings and then a single wash to remove the stain.
• Example I.--A pad bath solution is prepared by dispersing in water 24% dihydroxy dimethylol ethylene urea (50% aqueous solution); 4.3% zinc nitrate (50% aqueous solution of (Zn(NO;,) -6H O); 10% emulsion copolymer comprising 70% ethyl acrylate and 30% acrylic acid; 6% FC-208 (a fluorochemical resin emulsion-water repellent sold by 3M Co.), 6% Nalan W (a cationic modified resin Water repellent sold by du Font) and 2.3% ethoxylated alkyl phenol.
• the above composition is padded onto samples of Dacron/cotton (65/35) fabric to provide about 50% wet pickup. The fabric is then dried on a tenter frame at a speed of about 13 yards per minute and a temperature of about 250-280 F. until the moisture content of the fabric is reduced to approximately 5%.
• the slacks are tested to determine their soil release, oil repellency and water repellency both initially and after laundering a number of times. Even after the testing procedures, the pressed slacks retain creases satisfactorily. The results of the tests are reported in Table 1.
• Example II The procedure of this example is the same as that of Example I except that the 10% copolymer emulsion of 70% ethyl acrylate and 30% acrylic acid is omitted from the pad bath solution. Slacks tested show the results set forth in Table 1.
• Example III The procedure of this example is the same as that of Example I except that the 6% FC-208 and 6% Nalan W are omitted from the pad bath solution. Test results are set forth in Table I.
• Soil release 4. 1. 3 4. 3 Oil repellency 6 5 0 Water repellency- 70 100 0 After 5 washes:
• Example IV The procedure of this example is the same as Example I except that the dihydroxy dimethylol ethylene urea is replaced with 18% N-methylol acrylamide (50% aqueous solution). Also, the dried fabric is subjected to irradiation in an insulated core transformer manufactured by the High Voltage Engineering Corporation of Burlington, Mass. The fabric is passed through the irradiation equipment at a speed of about 40 yards per minute with a setting on the transformer of about 500 kilovolts and milliamps, the fabric being arranged in a 5 pass festoon during irradiation to produce a dosage of about 2 megarads. The results of tests are reported in Table II.
• Example V The procedure of this example is the same as Example IV except that the 10% copolymer emulsion of 70% ethyl acrylate and 30% acrylic acid is omitted from the pad bath solution. Slacks tested show the results as set forth in Table II.
• Example VI The procedure of this example is the same as Example V except that the 6% FC-208 and Nalan W are omitted from the pad bath solution. Slacks tested show the results set forth in Table II.
• Example VIII-The procedure of this example is the same as that of Example I except that the proportion of the FC208 is 0.25 the proportion of the ethyl acrylateacrylic acid copolymer is 8% and the curing temperature is 340 F. The results of testing are reported in Table III.
• Example IX The procedure of this example is the same as that of Example I except that the proportion of the FC-208 is 0.5 the proportion of the ethyl acrylateacrylic acid copolymer is 6% and the curing temperature is 340 F. The test results are reported in Table III.
• Example X The procedure of this example is the same as that of Example I except that the proportion of the FC-208 is 6%, the proportion of the ethyl acrylate-acrylic acid copolymer is 2% and the curing temperature is about 325 F.
• the test results are reported in Table IV.
• Example XI Soil release 3.0 Oil repellency 100 Water repellency 50
• Example XI The procedure of this example is the same as that of Example I except that 4.3% magnesium chloride (MgCl -6H O) is substituted for the Zinc nitrate. Results similar to those of Example I are achieved.
• Example XII The procedure of this example is the same as that of Example I except that the acrylic acidethyl acrylate copolymer is replaced with each of the following copolymers with results similar to those of Example I:
• Methyl methacrylate acrylic acid (70:30)
• Example XIII The procedure of this example is the same as that of Example I except that the dihydroxy dimethylol ethylene urea, the copolymer of ethyl acrylate and acrylic acid and the Nalan W are omitted from the pad bath solution. Instead, the ethyl acrylateacrylic acid copolymer is applied to the fabric and the fabric is dried TABLE V Example XIII XIV XV As received:
• the present invention provides novel textile materials having the heretofore unattainable combination of oil and water repellency and soil release characteristics. Furthermore, this combination of characteristics can be achieved with fabrics including synthetic polymeric fibers. As a result, the fabrics and garments of the invention can be laundered to remove stains without destroying the water and oil repellency characteristics. In addition, through the process of the invention, it is possible to achieve water and oil repellency and soil release in fabrics having durable press and/ or wash and wear characteristics.
• a process for imparting oil and water repellency, soil release and durable press characteristics to a cellulosic-containing textile material which comprises applying thereto an aminoplast textile resin; a textile resin catalyst, a fluorocarbon oil and water repellent material, and a synthetic acid soil release copolymer derived from an ethylenically unsaturated carboxylic acid, said acid polymer comprising at least about 20 weight percent acid calculated as acrylic acid; and subjecting said textile material to textile resin curing conditions at a temperature between about 100 and 200 C., whereby the textile resin is crosslinked to the textile material, the proportion of said fluorocarbon oil and water repellent material on said textile material being between about 0.01% and 5% by weight based on the dry weight of the textile material and the proportion of said acid polymer on said textile material being between about 0.25% and 5% by Weight based on the dry weight of the textile material.
• a process for imparting oil and water repellency, soil release and durable press characteristics to a cellulosic containing textile material which comprises applying thereto an unsaturated aminoplast textile resin, a textile resin catalyst, a fluorocarbon oil and water repellent material and a synthetic acid soil release copolymer derived from an ethylenically unsaturated carboxylic acid, said acid polymer comprising at least about 20 Weight percent acid calculated as acrylic acid; drying said textile material at a temperature in the range of about 225 F.
• a process for imparting oil and water repellency, soil release and durable press characteristics to a polyethylene terephthalate/ cotton (65/35) textile material which comprises:
• an aqueous system consisting essentially of about 2 to 30% of an aqueous solution of N-methylol acrylamide, about 1 to 15% of an aqueous solution of a catalyst selected from the group consisting of zinc nitrate and magnesium chloride, at least about 0.1% of an organic fluorocarbon oil and water repellent material, about 2.5 to 40% of an aqueous dispersion of a synthetic acid polymer prepared by polymerizing a monomeric mixture of about 10 to parts ethyl acrylate and about 20 to parts acrylic acid, and water; said aqueous dispersion being applied to the textile material in the range of 30 to weight percent of the textile material;
• a textile material having improved oil and Water repellency, soil release and durable press characteristics produced according to the process of claim 1.
• a textile material having improved oil and water repellency, soil release and durable press characteristics produced according to the process of claim 2.
• a textile material having improved oil andwater repellency, soil release and durable press characteristics produced according to the process of claim 3.
• textile resin catalyst is selected from the group consisting of metal salts and amino salts.
• the textile resin is selected from the group consisting of N- methylol acrylamide and dihydroxydimethylol ethylene urea.
• soil release polymer is prepared by polymerizing a monomeric mixture comprising about 10 to 80 parts of an acrylic ester and about 20 to 90 parts of an acrylic acid.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

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• 1967
  • 1967-03-10 US US622086A patent/US3597145A/en not_active Expired - Lifetime
• 1968
  • 1968-03-07 LU LU55633D patent/LU55633A1/xx unknown
  • 1968-03-08 SE SE03096/68A patent/SE340611B/xx unknown
  • 1968-03-08 AT AT233968A patent/AT298406B/de not_active IP Right Cessation
  • 1968-03-08 BE BE711895A patent/BE711895A/xx unknown
  • 1968-03-08 CH CH349068D patent/CH349068A4/fr not_active IP Right Cessation
  • 1968-03-08 JP JP43014932A patent/JPS516276B1/ja active Pending
  • 1968-03-08 NL NL6803389A patent/NL6803389A/xx unknown
  • 1968-03-08 GB GB1225275D patent/GB1225275A/en not_active Expired
  • 1968-03-08 FR FR1564068D patent/FR1564068A/fr not_active Expired
  • 1968-03-08 DE DE19681719368 patent/DE1719368A1/de active Pending

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