US3617188A

US3617188A - Soil release fabrics and method for producing same

Info

Publication number: US3617188A
Application number: US779250A
Authority: US
Inventors: Duane W Snyder
Original assignee: Crompton-Shenandoah Co
Current assignee: Crompton-Shenandoah Co
Priority date: 1968-11-26
Filing date: 1968-11-26
Publication date: 1971-11-02
Anticipated expiration: 1988-11-02

Abstract

A process for treating textile materials to impart soil-release and stain-release characteristics thereto and the products produced thereby are described which comprises treating textile materials, preferably fabrics containing cellulosic fibers or a blend of cellulosic fibers and synthetic fibers such as polyesters, with an oil, preferably refined mineral oil, to substantially saturate the fabric fibers with the oil thereby attaining a textile material having improved soil and stain release characteristics. The mineral oil composition may be used alone or in conjunction with other compositions such as those which impart permanent-press and water-repellency characteristics to a textile material.

Description

United States Patent Inventor Duane W. Snyder Waynesboro, Va.

App]. No. 779,250

Filed Nov. 26, 1968 Patented Nov. 2, 1971 Assignee Cmmpton-Shenandoah Co.

Waynesboro, Va.

SOIL RELEASE FABRICS AND METHOD FOR PRODUCING SAME 16 Claims, No Drawings U.S.Cl 8/115.5, 8/1 15.6, 8/115.7, 8/116.3, 117/1355, 117/1385, 117/139.4,11'/ '/139.5 F, 117/161 LN, 38/144,

Int. Cl .5... .EDfltSrn 113/9 2,

v D06m 13/54 Field of Search 8/115.5,

1157,1163;1l7/138.5,139.5 F, 161 LN;

Primary Examiner-George F. Lesmes Assistant ExaminerJ Cannon Att0rney-Darby and Darby ABSTRACT: A process for treating textile materials to impart soil-release and stain-release characteristics thereto and the products produced thereby are described which comprises treating textile materials, preferably fabrics containing cellulosic fibers or a blend of cellulosic fibers and synthetic fibers such as polyesters, with an oil, preferably refined mineral oil,

to substantially saturate the fabric fibers with the oil thereby attaining a textile material having improved soil and stain release characteristics. The mineral oil composition may be used alone or in conjunction with other compositions such as those which impart permanent-press and water-repellency 252/8.8 L gharacteristicstgatextile materig SOIL RELEASE FABRICS AND METHOD FOR PRODUCING SAME This invention relates to a process of imparting improved soil-release and stain-release characteristics to a textile material by treating the material with an oil and to the products produced thereby.

In the years since the early days of permanent press garments much research has gone into the development of improved permanent press resins and compatible catalysts, so that today creases in garments containing synthetic and naturally occurring fibers are very durable and are not appreciably affected by wear or cleaning procedures. Likewise, much effort has been expended toward the attainment of good wash and-wear fabrics. I

Additionally, since the advent of resin-treated textiles of natural fibers and blends of natural and synthetic fibers much research has gone into developing various organic and inorganic systems for treating fabrics to allow them to be resistant to soiling and to facilitate the removal, during normalhome or commercial laundering, or particulatesoils and oil-borne or water-bome stains on the fabric.

The work by others up to know has been essentially confined to chemical systems which when applied to the fibers, encapsulate the fibers with aprotective coating which repels oil and water-home stains. To date such systems havebeen principally based on fluorocarbon chemistry or on an acrylic polymer emulsion containing high percentages of acid, calculated as acrylic acid, which renders the fiberhydrophilic and thus allows the removal of the soils or stains in laundering. To achieve resistance to soil redeposition during the laundering operation of the garment, the work up to now has been directed toward modifying the fiber surface with certain polyester emulsion polymers which change the surface,-thus tending to repel particulate soil in the wash water in launder- None of these treatments is completely satisfactory'in that they do not release a wide varietyof stains. While some are effective as antisoil redeposition finishes, they are poor soilrelease and stain-release agents'.0n the other hand,-those that are satisfactory soil-release and stain-release agents may'not be good against soil redeposition. Moreover, none of the finishes allows free use of adjuncts in the formulation which tend to improve wear properties, which is so important in blends containing resins used to impart permanent-press and permanent-crease properties. For example, the above mentioned systems do not allow the production of satisfactory water-repellent finishes in conjunction with them because such finishes depend upon making the surface of the fiber highly hydrophilic. ln the case of fluorocarbon polymers, addition of sufficient levels to the fibers to produce both Accordingly, an object of the-present invention is to provide a textile material having improved soil-release and stainrelease characteristics.

A further object of the present invention is to provide a process for treating a textile material with an oil (preferably mineral oil) to impart soil-release and stain-release'properties to the textile.

Still another object of the present invention is toprovide a process for treating a fabric with a mineral oilcomposition and permanent'press resin either simultaneously orseparately in such a manner that the fabric has both outstandin'gsoilrelease and stain-release properties as well as permanent-press characteristics.

Yet another object of the invention is to provide a textile material substantially saturated with a refined mineral oil which does not adversely affect the physical characteristics and/or endurance properties of the garment which are desired by the consumer, e.g. permanent'press, water-repellency, hand, etc.

Yet a further object of the invention relates to compositions suitable for imparting soil-release and stain-release properties, permanent-press characteristics and water-repellency, to a fabric.

An additional object of the invention is to provide garments made from pile fabrics such as corduroys treated with a mineral oil composition to obtain soil-release and stain-release characteristics superior to those heretofore available with such fabrics.

These and other objects of the present invention will become apparent from the following description.

In general, the present invention is directed to an economical and simple process for imparting soil-release and stainrelease characteristics to a fabric by impregnating the fabric with either a nonaqueous oil solution or an oil emulsion used alone or as an adjunct to other standard compositions employed to impart desired physical and endurance characteristics to afabric, e.g. permanent-press, water-repellency, etc. The term permanent-press" used throughout this application is intended to have the same meaning as and be interchangeable with the term durable press.

The term soil-release" as used herein refers to the ease with which a fabric releases in the laundering process dirtiness that arises from dirty air or body lipids.

The term stain release means the ease with which a fabric gives up stains in water.

The term soil redeposition" means "the tendency of soil removed during'laundering to redeposit on the fabric during the washing cycle.

The terms textile resin as used herein includes monomers, polymers (homopolymers and copolymers) which when applied to a textile material and reacted under proper conditions undergo polymerization and/or condensation and are transformed to the thermoset state.

The preferred oil used in the process of the presentinvention is a refined mineral oilwhich may be of either paraffin or naphthene base. Unrefined mineral oils which contain sulfur and the like are operative but among other things have the drawback that they are likely to discolor the fabric and impart undesirable odors thereto. :In order to achieve good soilrelease and stain-release properties, it has been found that the mineral oils should'have the following properties particularly when used in conjunction with a textileresin: (l) a saybolt ,viscosity 0 "1 00F. of at least about 200 and preferably above form a water-in-oil or oil-in-water emulsion concentrate so that it will be compatible with other chemicals used in the water system. The emulsion concentrate is preferablya waterin-oil emulsiomHowever, the mineral oil need not be emulsified if it is used ina solvent system.

The selection of a-suitable emulsifying agent for forming the mineral oil emulsion concentrate is controlled by therequirements of the method by which the mineral oil is applied to the textile material. Thus, when applying the mineral oil 'from a pad bath, it is essential that the emulsion be sufficiently stable so as not to break down during the padding operation. lf the latter occurs, uneven-impregnation of the textile material occurs. In general, the preferred emulsifiers are nonionic and have a hydrophilic-lipophilic balance (l-lLB" value) between 'i 1 and 14 as determined inaccordance with the Atlas Chemical Industries HLB System. It has also been found that the desired stability can be achieved by using a blend of different nonionic emulsifiers. The stability of themineral oil emulsion can be further increased by incorporating a stabilizing additive, e.g. sodium-carboxymethyl cellulose of the like, in the emulsion. Illustrative of suitable emuis'ifying systems are: blends of mono and diglycerides, blends of sorbitan fatty acid esters, blends of polyoxyethylene sorbitan fatty acid esters, polyoxyethylene alcohols and blends thereof, etc.

The balance of mineral oil and water used in the makeup of an emulsion concentrate is not important, provided the required ultimate concentration of oil in the total pad bath is maintained. ln general, a 50/50% balance in the concentrate has been found quite satisfactory. However, the emulsion concentrate can, if desired, contain more mineral oil than water or visa versa. Ultimately, the emulsion concentrate is further diluted with water when added to the pad bath so that the concentration of mineral oil is substantially reduced in the bath to required values.

In preparing mineral oil emulsion concentrate, the ratio of mineral oil to emulsifying agent may be varied depending on numerous factors including whether a stabilizer is present, the nature of the emulsifier and the degree of stability desired. Obviously, if mineral oil emulsions are prepared well in advance of their use in the bath, they also need to have the requisite storage stability. Good results have been obtained in the process of the present invention where the emulsion concentrate contains at least 2% by weight and preferably 6% by weight, of the emulsifying agent.

Where the mineral oil is impregnated into a textile material from a nonaqueous solvent system, any conventional solvent may be employed which is miscible with the oil and is easily and rapidly volatilized or evaporated and does not adversely affect the fibers of the textile material being treated. Illustrative of suitable solvents are: chlorinated hydrocarbons, e.g. perchloroethylene, carbon tetrachloride, trichloroethylene; petroleum distillates, e.g. Stoddard solvent, etc., fluorinated hydrocarbon solvents, etc.

The textile materials which can be treated according to the process of the present invention to impart soil-release and stain-release properties thereto may be composed of natural fibers, synthetic fibers or mixtures of these fibers. The preferred type of textile which can be treated with the process of this invention is one which contains cellulosic fibers, (e.g. cotton), regenerated cellulosic fibers (rayon), polyester fibers (e.g. polyhexamethylene terephthalate), or combination of such fibers. Fabrics made from such fibers may be knitted, woven, matted or otherwise nonwoven. The fabrics employed in the invention may also be formed from a mixture of polyester fibers and polyamide fibers (e.g. nylon) or with acrylic fibers (e.g. polyacrylonitrile and copolymers containing acrylonitrile) and cellulosic fibers, and the like. It should also be understood that textile materials containing only noncellulosic fibers other than polyesters are within the scope of the present invention.

The advantages of the present invention are best achieved when the process is carried out using a textile fabric or the ultimate product, e.g. a garment, etc. as the textile material. However, the material may also be in the form of yarns and the like which have been previously dyed, if dyeing is required. The fabric may be in any form such as a pile or flat fabric. Very unexpectedly, good soilrelease and stain-release properties have been obtained with pile fabrics such as corduroys, which are not attainable with such fabrics using the present commercially available soil-release chemicals even though such chemicals are adequate on flat fabrics.

The textile materials treated in accordance with the present invention may be formed into a variety of products, such as clothing, e.g. shirts, slacks'outerwear, including raincoats; apparel accessories, e.g. ties, scarves, fabric belts, etc., household furnishings, e.g. draperies, upholstery for furniture, etc.

The mineral oil emulsion or the nonaqueous mineral oil solution previously described may be used alone to treat the selected textile materials or as an adjunct with other finishing systems such as textile resin compositions, water-proofing compositions, softeners, antistatic agents, bacteriostats, compositions for improving abrasion resistance, etc., without adversely affecting the physical and endurance properties of the fabric. This provides a garment that more nearly supplies utopian requirements of the consumer and the housewife than previous treatments.

It has surprisingly been found that the combination of mineral oil and a textile resin in treating a fabric containing 75 L polyester fibers gives substantially superior soil-release and stain-release characteristics than when such a fabric is treated only with a mineral oil.

The textile resins that may be employed in conjunction with the practice of the present invention are the well-known aminoplast resins. These nitrogen-containing resins when applied to a textile material in the presence/of a textile resin catalyst at elevated temperatures of between about 260 F. to about 390 F. are transformed into the thermoset state. Where the textile material contains cellulosic fibers the aminoplast resin condenses with the cellulose molecules, and when vinyl groups are present in the aminoplast resin, it undergoes additional polymerization with itself. The cured textile resin imparts to the textile substrate a permanent-press and/or wrinkle-resistant finish.

Exemplary of the textile resins that may be employed according to the present invention are the following:

Urea formaldehydes, e.g., propylene urea formaldehyde, 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 fonnaldehydes, etc., formaldehyde-acrolein condensation products; formaldehyde-acetone condensation products; alkylol amides, e.g., methylol formamide, methylol acetamide, etc., acrylamides, e.g., N-methylol acrylamide, N- methylol methacrylamide, N-methylol-N-methacrylamide, N- methylmethylolacrylamide, Nmethylol methylene-bis(acrylamide), methylene-bis(N-methylol acrylamide), etc., haloethylene acrylamide; diureas, e.g., trimethylol acetylene diurea, tetramethylol-acetylene diurea, etc., triazones, e.g., dimethylol-N-ethyl triazone, N-N'-ethylene-bis dimethylol triazone, halotriazones, etc., haloacetamides, e.g.,, N- methylol-N-methylchloroacetamide, etc.; urons, "e.g., dimethylol uron, dihydroxy dimethylol uron, etc., and the like. Mixtures of aminoplast textile resins are also within the scope of the present invention.

Further exemplary of the textile resins within the scope of the present invention are those which conform to the following structural formulas. in each of the following formulas the variables may be selected as follows:

R: hydrogen, lower alkyl or residue of saturated or unsaturated aldehyde R: hydrogen, lower alkyl or CX-CR CHR R": hydrogen or methyl R: hydrogen or lower alkyl R: hydrogen, lower alkyl, or CHR'OR, at least one R being CHROR R: lower alkyl or hydroxy alkyl R": hydrogen, hydroxyl or lower alkyl R: hydrogen, lower alkyl,'alkylol or alkenol 5 5 X: sulfur or oxygen catalysts may be used when. both types of functional groups are present in the textile resin. in this instance, the catalysts, may be added separately or together. When they are added together, one must be a latent catalyst, i.e., one that willnot initiate its reaction during the opposite type reaction, butmay be activated subsequently under proper catalytic conditions.

The catalysts useful in activatingthe acid-[or base-reactive .groups are thosecpnventiorrail usedtg activate thergction of textile resins containing the same reactive group for reaction with hydroxy groups of a cellulose-containing material. Preferably, latent acid or baseacting 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, mnc nitrate and zinc fluoroborate and .the amino salts, for example, monoethanolamine hydrochloride and 2-amino- Zrnethyl-propanol 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 reactionunder prescribed conditions, such as elevated temperature or. some otheractivating means, as through use of another chemical-5 compound. For example, an alkali-metal sulfite canbe padded onto a 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 hav- 65 ing, for example, apt-l of about 8.5 on the fabric, but which decomposes at temperatures in excess of about 80 C. to form the more alkaline 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 j the fabric produced by this compound in normal conditions is generally insufficient to initiate the desired degree of reaction under normal-temperature conditions.

if fabrics containing a base-reactive group are maintained at )pH levels above about [0, however, degradation occurs. so

j material.

15% by weight of an acid-acting catalyst in the application; bath with the preferred range being from about 19? 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 l6%, 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, whenbase catalystsare utilized and if a highly acidic group is released during the reaction, the amount of base catalyst 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. L

The selected textile resin may be used in the same bath as the mineral'oil emulsion or solution or applied separately to the textile material from a different bath. When employing a single bath containing the mineral oil aswell asthe other materials, e.g. textile resin, resin catalyst, water-proofing agent and the like, the amount of each material employed is determined'by the ultimate use ofthe garments orother articles prepared from the treated fabric. Preferably all the ichemicals are applied to the textile material from a single bath.

The bath; used, to impregnate the textile material in accordance with the present invention (which may contain any number of ingredients in addition to the selected mineral oil) may be appliedto the textile material in any suitable manner. For example, when employing a mineral oil emulsion, padding of the bath onto a textile fabric is a simple and economical ffoperation to perform On the other hand, where the-mineral oil is in a nonaquebus system this composition may be sprayed onto thefabric. Other conventional techniques for applying a composition can be employed for impregnating the textile.

ln generaL'when using a pad bath the applicator system is adjusted to provide preferably from 30 to about 70% weight wet pickup by the fabric from the bath. However, this pickup can be varied within the skill of the art. The most important ?factor is to saturate the textile material to the extent that it will contain a minimum of about 5% by weight and preferably at least about 7% by weight of mineral oil based on the dry weight of'the fabric after the fabric has dried and cured,.if a textile resin is present. The minimum amount required is a variable of the type of fibers in the material being treated.

The amount of mineral oil that is required in the pad bath in mineral oil emulsion but no textile resin andcatalyshit-has been found that the bathshould contain at least- 10% by weight mineral oil and'preferably at least l5% by weight in treating a cotton fabric, based on about a 40 weight percent wet pickup by the fabric, in order to obtain good soilrelease and stain-release properties. Where the fabric is a blend of cellulose and polyester fibers the minimum quantity of mineral oil needed is somewhat reduced. Similarly, when the weight percent of wet pickup by the fabric is increased the minimum quantity of mineral oil can be somewhat reduced without adversely affecting-the soil-release and stain-release properties. The inclusion of a pennanent-press chemical system in the pad bath requires somewhat larger quantities of iiii ne r l dil in the batfl'ihaii'when QEZEEEriiial syStem E not present.

As previously indicated, if a textile resin is employed, it is preferably simultaneously applied from the same bath containing the mineral oil composition. Simultaneous application is not required and the same result may be realized by first applying the mineral oil composition followed by separate application of the textile resin and curing of the resin. However, where the textile resin is applied first and cured followed by treatment with the mineral oil composition, the soil-release and stain-release properties are not as good as in the case of simultaneous application.

The fabrics treated with the mineral oil and any additional chemical s employed to modify the physical and endurance characteristics of the fabric, can be processed in any number of ways after the bath treatment. In the case where no textile resin or other chemical is employed, the fabric is simply dried by conventional techniques at a temperature which will not result in volatilization of the mineral oil to such an extent that the remaining mineral oil content will be below the quantity necessary to obtain good soil-release and stain-release properties. After drying, the fabric can be processed in the normal manner into a garment or other article. In general, when employing a pad bath containing no textile resin the fabric is dried at a temperature of about 270 F. to 300 F. for about minutes.

1f the mineral oil is used in conjunction with a textile resin and curing catalyst the fabric after treatment in the bath may be processed in accordance with any number of well-known prior art techniques which require no additional step other than those normally used for the preparation of the conventional permanencpress articles. For example, the fabric may be folded and pressed on conventional equipment for a short period of time followed by a curing operation in an oven. The curing should preferably be performed at a temperature between about 310 F. and about 325 F. The selected curing temperature should be below the temperature at which substantial volatilization of the mineral oil would occur. Depending on the selection of the textile resin and catalyst, the following are exemplary of the types of processes that may be employed following the treatment of the fabric with the mineraloil-containing composition.

PROCESS TYPE i l. Apply to fabric mineral-oil-containing composition and textile resin having one functional group and textile resin catalyst.

2. Dry fabric at temperature that is insufficient to substantially volatilize the mineral oil and to initiate catalysis of the textile resin.

3. Convert the fabric into a garment.

4. Press the garment to produce the desired creases.

5. Subject the garment during and/or after pressing to a sufficient temperature to catalyze and cure the textile resin but not substantially volatilize the mineral oil.

PROCESS TYPE [I 1. Apply to fabric mineral-oil-containing composition, textile resin having more than one type of functional group, and textile resin catalyst for each type of functional group. I 2. Dry fabric below temperature at which substantial volatilization of mineral oil takes place and subject fabric to condition whereby one type of functional group reacts and the remaining functional group remains uureacted.

3. Convert the fabric into a garment.

4. Press the fabric to produce the desired creases.

5. Subject fabric during and/or after pressing to curing conditions whereby the remaining functional groups are reacted with the fibers in the garment (e.g. cellulose fibers) but below the temperature at which substantial volatilization of the ,mineral oil takes place.

PROCESS TYPE ill 1. Apply to the fabric mineral oil composition, textile resin having more than one type of functional group, (one type being sites of ethylenic unsaturation), and a textile resin catalyst.

2. Dry the fabric below the temperature at which substantial volatilization of the mineral oil takes place and below the catalysis temperature of the catalyst.

3. Subject the fabric to irradiation as described in U.S. Pat. No. 3,377,249, for example.

4. Convert the fabric into a garment.

5. Make the desired creases in the garment.

6. Subject the garment to textile-resin-curing conditions at a temperature at which substantial volatilization of the mineral oil does not take place.

When a permanent-press resin is employed in conjunction with the mineral oil, in any of the above processes, drying temperatures are employed which are not only below the temperature at which substantial volatilization of the mineral oil would take place but also below the temperature that would initiate a catalysis reaction, although in some cases a partial catalysis or curing is acceptable.

The following examples are given by way of illustration and not by way of limitation. lt is readily apparent that variations from the specific conditions and reactants may be made without departing from the scope of the invention.

EXAMPLE A (EMULSION CONCENTRATE) An emulsifier blend was prepared by mixing 60% by weight polyoxyethylene (10) oleyl ether having a hydrophilic-lipophilic balance of 12.4 with 40% by weight polyoxyethylene (2) oleyl ether having a hydrophilic-lipophilic balance of 4.9.

A stock emulsion concentrate was prepared by adding 6% by weight of the above blended emulsifiers to 50% by weight of refined mineral oil (available as Nujo1" from Plough, lnc.) having a specific gravity at 60 F. of 0.88 to 0.90; a saybolt viscosity in the range of 360 to 390 at F.; a paraffin/naphthene ratio of 1.4/1.0; and a refractive index of about 1.48. After mixing of the mineral oil and blended emulsifiers is completed, 44% by weight of water is added slowly while stirring. A water-in-oil emulsion will be formed first and the viscosity will increase until sufficient of the water has been added at which time inversion of the emulsion will take place with a s ubsequent i educt?n in viscosity, resulting in an oil-inwater system. The resulting emulsion is about a 50% oil emulsion concentrate.

EXAMPLE B (EMULSION CONCENTRATE) Another emulsion concentrate was prepared as described in example A using 50% by weight "Nujol, 2% by weight Dexapol" (available from Dexter Chemical) as the emulsifier, 1% by weight sodium carboxylmethyl cellulose as a stabilizer, and 47% by weight of water. The resulting emulsion is about a 50% oil emulsion concentrate.

EXAMPLE 1 (PAD BATH) A pad bath solution was prepared having a temperature between about 70 and 100 F. by adding to 70% by weight of water 30% by weight of the emulsion concentrate described in example A. This composition was padded onto a 100% corduroy fabric to 56% wet pickup and thereafter the fabric was dried at 295 F. on a tented frame for about 5 minutes.

The dried fabric was stained with mustard, peanut butter, French dressing, butter, ketchup, mayonnaise, corn oil, shortening, motor oil, used motor oil and U.S.P. white mineral oil. The stained fabric material was subjected to one standard F. home wash for 10 minutes (AATCC Test Method 88A-l964T, 111) using one cup of Tide detergent and tumble-dried. The stains were then rated using the Deering Milliken Soil Release Replica showing five degrees of staining, 1.0 being the heaviest stain and 5.0 showing virtually no stain. After one wash all stains were removed and classed 5.0. The

sample was then laundered four additional times and again EXAMPLE 2 (PAD BATH) A pad bath solution was prepared in the manner described in example 1 by adding to 60% by weight of water, 40% by weight of the emulsion described in example A. This composition was padded onto a 100% cotton corduroy fabric under the same conditions described in example 1 and dried as described in that example.

The dried fabric was stained with the same stains as in the previous example. The stains were completely removed after the first wash, with a rating of 5.0. The stains applied after the fifth wash and prior to the sixth wash were also completely removed and were rated at .0.

The same 100% cotton fabric untreated, serving as a control, was stained with the same stains as the mineral-oil-treated ;fabric and washed one time under the same conditions. All

. stains remained plainly visible except the ketchup which was completely removed. The stains remaining were classed 1.0 to l .5 using the Deering Milliken Soil Release Replica.

EXAMPLE 3 (PAD BATH) A pad 'bath solution was prepared by dispersing 12% by weight of Nujol" (previously described in example A) in 88% by weight perchloroethylene. The solution was padded onto a. 100% cotton corduroy fabric at a wet pickup of 70%. The fabric was dried as previously described to volatilize the sol- .vent.

The dried fabric was stained with the same stains listed in the previous examples and subjected to the same washing described in example 1. The stains were completely removed after the first wash and were rated 5.0. The stains applied after the fifth wash and prior to the sixth wash were also completely removed and were rated 5.0.

EXAMPLE 4 (PAD BATH) A pad bath solution was prepared containing the following:

A 100% cotton fabric was padded with this solution at a wet pickup of 56%. The fabric was dried at 295 F. as previously described. The fabric was then creased by using a hot-head press at 350 F. with steam 3 seconds, press seconds and vacuum 7 seconds. Thereafter the fabric was cured at 315 F. for 10 minutes.

The cured fabric was stained and washed as described in ex- :ample 1. All stains were removed completely after the first wash and were rated 5.0. After the sixth wash the only stain visible was the used motor oil which was classed 4.5.

The fabric was rated for crease retention by the AATCC method 88C-l964T with an initial rating of 5. After six m'iiiifioiiemulsimi Er Example A 30 I Water 57.5

A fabric of a blend of 50% polyester/50% cotton was padded with this solution in the manner described in example 4. The fabric was dried at about 280 F. as previously described.

The dried fabric was made into pants legs and pressed in a conventional hot-head press for 20 seconds with steam and vacuum. The pants legs were then cured at 315 F. for 10 minutes in a conventional curing oven.

The pants legs were then stained, washed and evaluated for both stain removal, appearance, retention and crease retention as previously described in example 4.

For a control, the same fabric of a blend of 50% polyester/50% cotton was padded with the following formulation:

Ingredient I: By Weight KaraseF 4 Reactant Resin 5 "Karaset" l Metallic Catalyst 2.5 I Polycryl 7Fl2 Nonionionic Acrylic Emulsion s Polyson ABR" Nonionic High Density Polyolefin Emulsion B "Dexapal 555 Nonionic Wetting Agent 0.2 Water 79.3

The control fabric was processed as described hereinabove a in this example and made into pants legs.

Upon washing, ,the pants legs containing the mineral oil had iall stains removed and were classed 5 using the Deering Mil- "liken Soil Release Replica. In contrast all stains remained in the control fabric containing no mineral oil, except ketchup which was completely removed. The remaining stains were classed L5 to 2.

The pants legs made from the control and mineral-oiltreated fabric were laundered four additional times and restained with each of the materials identified in example I and washed a sixth time. In the case of the pants legs made from the fabric treated with mineral oil, all stains were completelyr eiiovedand were rated 5Twhereas the stains were' quite visible on the pants legs made from the control fabric and were rated 2.0-2.5.

The crease retentions of the pants legs made from both fabrics were equivalent, with a 4 rating after six launderings and the appearance rating was virtually the same at 4.5. Therefore, it was found that the mineral oil processing does not detract from the permanent-press properties of the fabric or garment.

Insofar as physical properties are concerned, the mineraloil-treated fabric showed an improvement in tear value over the control sample. Crease recovery as measured by the ;AATCC Wrinkle Recovery test method 66-l959T showed 296 recovery on the warp plus weft direction for the oil- I treated fabric and 293 for the control fabric, a rating of 180 in each of the warp and weft direction representing a complete recover E washes the rating was 4. Fabric appearance was rated accordy ing to the AATCC method SBA-19641 with an initial rating of EXAMPLE 6 (PAD BATH) 5, which became 4.5 after six washes.

I A pad bath solution was prepared with the following: EXAMPLE 5 (PAD BATH) A pad bath solution was prepared containing the following:

Ingredient I: By Weight Ingredient y Weight Fixapret C P 40-Resin 17 l cunte" Mg-Catalyst 4.25

n 4 Remnant Resin :5 Mineral oil emulsion Concentrate of Example B 30 Karaset" 1 Metallic Catalyst 2.5 7 5 43-75 "Polycryl 7Fl2" Nonionic Acrylic Emulsion 5 svrsriiat fabrics of 36% polyester/50% Edda; dyed in various shades (light to dark) were padded with this composition at a 55% wet pickup. The fabrics were dried at 295 F., pressed as previously described, and cured at 325 F. for 15 minutes.

The fabrics were stained and washed as described in example 1. Examination of the fabrics after one wash showed complete removal of all stains except used motor oil which was still visible in the lighter shade. The same effect was noted after a sixth wash following restaining between the fifth and sixth wash.

EXAMPLE 7 (PAD BATH) A corduroy fabric of 50% polyester/50% cotton dyed to the shade of burnt green was treated with the following composition which included a water-proofing resin.

The fabric was padded, dried, pressed and cured and stained in the same manner as example 6. Examination showed no stains remaining after the first wash. The fabric was restained after the fifth wash and washed a sixth time. No stains remained after the sixth wash.

The sample was tested before the first wash for water repellency and the spray rating was 100, which is excellent for a water-repellent corduroy finish. After the fifth wash, a spray rating of 70 was maintained which is A normal for a durable water-repellent finish.

EXAMPLE 8 (PAD BATH) A whiskey shade corduroy fabric of a blend of 50% polyester/50% cotton was padded in the manner described in example with the following fonnulation:

Ingredient X7 By Weight Karnset" 4 Rcactant Resin 4.5 Karaset lMetallic Catalyst 2.25 "Polycryl 7Fl2 590 "Polyson ABR" 5.00 Water 83.25

The padded fabric was dried at 275 F. for 5 minutes as previously described and then pressed and cured at 315 F. for 10 minutes following the procedure indicated in the previous examples. The cured fabric was repadded with the mineral oil concentrate of example A and again dried at 275 F. for 5 minutes. Thereafter the fabric was stained and washed as described in example 1. The stain removal was found not to be as good as when the textile resin and mineral oil are padded onto the fabric from the same bath and a number of stains were visible which were rated at 3.5 to 4.

EXAMPLE 9 (PAD BATH) Refining Co.) are identified as follows:

Mineral Oil A: A side draw heavy cylinder type lubricating oil having a saybolt viscosity at 210 of 87 F.; a specific gravity at 60 F. of0.887; a flash point (Cleveland open cup F.) of

510 F. and an average molecular weight of 600.

5 Mineral oil 8": A neutral oil; nonacid paraffin base oil having a saybolt viscosity at 100 F. of 650; a specific gravity at 60 F. of 0.876; a flash point (Cleveland open cup F.) of 520 F.; and an average molecular weight of 570.

Mineral Oil C": A mineral oil containing less than 30% naphthene hydrocarbons having a saybolt viscosity at 100 F. of 470; a specific gravity at 60 F. of 0.877; and a flash point (Cleveland open cup F.) of 485 F.

Mineral Oil D": A refined mineral oil having a saybolt viscosity at 100 F. of 350; a specific gravity at 60 F. of 0.870; a flash point (Cleveland open cup F.) of 455 F. and an average molecular weight of 455.

Mineral Oil E: A naphthene base mineral oil having a saybolt viscosity at 100 F. of 556; a specific gravity 0 60 F. of 0.901; and a flash point (Cleveland open cup F.) of 440 F. Mineral Oil "F": A refined mineral oil having a saybolt viscosity 0 100 F. of 360-385; a specific gravity 0 60 F of 0.88l-0.890; a flash point (Cleveland open cup F.) of 435 F.; and an average molecular weight of 475.

In each case the mineral oil emulsion concentrate was a 50% solution prepared with the same emulsifiers used in example A and differing only in the oil used.

Six separate pad bath solutions were prepared each containing a different one of the six mineral oil emulsions. The other components of each pad bath were as follows:

Ingredient I; By Weight Karaset" (4) Rcactant Resin "Karasct" l) Metallic Catalyst Water Each of the six pad solutions was padded onto (1) a white 50% polyester/50% cotton fabric (2) a dyed 50%- polyester/50% cotton fabric, and (3) a [00% polyester fabric, at a wet pickup ofabout 37% in each case.

After padding, each of the fabrics wmried at 275 F .Tof5 minutes and cured at 315 F. for 10 minutes. Each of the fabrics was then stained with the materials described in example 1.

In addition an untreated control fabric and a resin-treated and cured control fabric (without oil emulsion) were stained with the same materials. The resin and catalyst were the same as in the case of the mineral-oil-treated samples.

All of the fabrics including the controls were subjected to one IO-minute wash cycle at 140 F. in a home washing machine and tumble-dried.

Upon examination of the dyed polyester/cotton samples, there was no indication of stains remaining on any fabric treated with any of the mineral-oil-containing formulations A through F. In the case of the undyed white 100% polyester only a slight stain remained as a result of the used motor oil. It was noted that the fabric treated with mineral oil A was left with a yellow tinge. In the case of the white polyester/cotton blend all stains were removed except that there was a slight red tint where the French dressing and ketchup stains were applied, and the used motor oil was not completely removed.

By comparison all stains remained visible on the resinated and cured control and on the untreated control.

To each of the mineral-oil-containing pad .bath solutions described in this example there was added 5 by weight Polycryl 7Fl2" to improve abrasion resistance. The addition of this product was found not to adversely affect the soilrelease and stain-release properties.

EXAMPLE 10 Several whiskey shade corduroy fabrics of a blend of 50% Proctor Chemical Co.

EXAMPLE 1 1 A series of fabrics of 100% polyester white taffeta were padded with different formulations as follows (all percentages in the formulations are by weight):

1 4 l. A method of imparting soil-release and stainreleasecharacteristics to a fibrous textile material which comprises impregnating said material with a composition containing a grefined mineral oil so as to provide said textile material with at; :least 5% by weight of said refined mineral oil based on the dry weight of said fabric and drying said impregnated material} Formulation A Formulation B 5% Karaset" 4 Mineral Oil Emulsion of Example A 2.5% l(araset" i 92.5 Water 70% Water Fonnulation C l 5% Karasct" 4 2.5% "Karaset" l 30% Mineral Oil Emulsion of Example A 62.5% Water The fabrics treated with formulations A and C'- were dried and cured as previously described whereas the fabricpadded with formulation 5" was dried only. The fabrics treated with formulations A, B and C as well as a control fabric (untreated were stained with the stains listedin exam-;

pie 1 except used motor oil, and washed one time. i

The untreated fabric and the fabric treated with formulatioru A both showed all stains remaining visible each having a rating of 3 to 3.5. The fabrics treated'with formulation 8 showed; only slight stains remaining and were rated 4.5 to 5. in thecase, of the fabrics treated with fonnulation 0 allstains werei removed completelyarid 'ratgd5 The foregoing tests indicate that the use of the mineral 'oil in conjunction with a textile resin improves the soil-release and available from Diaperm 500": A cyclic nitrogenous steal-amide condensate available from Quaker Chemical Co. Fixapret CF. 40.": Dimethylol dihydroxy ethyleneurea available from B.A.S.F. Corp.

Karaset 4": Available froin Refined-Onyx Division, Millmaster-onyx Corp.

Karaset 1: Available from'Refined-Onyx Division, Mill-I master-Onyx Corp.

Polycryl 7H2: Nonionic self-crosslinking acrylic emulsion available from Polymer'lndustries, inc.

Polyson A.B.R.: Nonionic :high density polyethylene emulsion available from Refined-Onyx Division of Millmaster- Onyx Corp.

Catalyst LT: hydroxyacetic acid available from Quaker Chemical Co.

The above examples are illustrative of the preferred embodiments of the invention. However, other modifications can be made without departing from the'scope of the present invention. it is therefore to be understood that changes may be made in the embodiment of the invention which are within the full intended scope of the invention as defined by the appended claims.

What is Claimed is:

below a temperature at which substantial volatilization of said. mineral oil occurs wherein said refined mineral oil has a' saybolt viscosity at 100 F. of at least about 200, a-flash point of at least about 400 F., an average molecular weight of at least about 440 and a specific gravity at 60 F. of at least about 0.80.

2. A method as defined in claim 1 wherein the fibrous textile material contains fibers selected from the class consisting of, cellulosic fibers, polyester fibers and blends thereof.

3. A method as" defined in claim 2-wherein said textilej material is in the form of a fabric.

3 4. A method according to claim 3 wherein said fabric is 100. percent cotton. 1 5. A method as defined in claim 1 wherein said material also treated with an aminoplast resin forimparting'permanent-i press properties to an article manufactured from said textile; material. 6. A method as defined in claim 5 wherein said textilei material is dried at a temperature below that at which curingi of said textile resin takes place. 1

7. A method as defined in claim 6 which includesthe addi- 'tional step of curing said textile resin at a temperature no greater than about 325 F. after dryinggf said textile material.

8. A method of imparting soil-release and stain-release characteristics to a textile article of manufacture composed of a textile fabric containing substantially cellulosic fibers which comprises impregnating said fabric with a composition c ontaining refined mineral oil to substantially saturate said textile 7 material with said refined mineral oil and drying said fabric below a temperature at which substantial volatilization of said mineral occurs, said dried fabric containing at least about 5% by weightof said mineral oil based on the dried weightof said fabric and said mineral oil impregnated into said fabric'has a.

*least 400 F.-,'an average molecular weight of at least about;

440 and as 'cific' avity at F. of at least 0.80. i 9. A me odas' efined in claim 8 wherein said mineral oil is impregnated into said fabric from an aqueous bath containing at least one nonionic emulsifying agent for said mineral oil, said aqueous-bath containing at least 10% by weight of-said mineral oil.

10. A method of imparting soil-release and stain-release and permanenbpress characteristics to a textile article of nianu 'facture composedof a textile fabric containing fibers-select'ed from the class consisting of cellulosic fibers, polyester fibers; and blends'thereof which comprises treating said fabric with? (l) a refined mineral oil, and (2) an aminoplast resin, substan-; tially drying said fabric and converting'said resin" to. a thermoset state, said dried fabric containing at least 7% by weighti of said refined mineral oil based on the dried weight of said fabric, and saidmineral oil having a saybolt viscosity at 100 F. i

of at least about 350, a flash point of at least about 400' F., an average molecular weight of at least about 440 anda specific. gravity at 60 F. of at least about 0.88.

'11. A method as defined in claim "10 wherein the drying of said fabric is carried out prior to the curing of said aminoplast resin and at a temperature below the curing temperature of said resin'and said treating step comprises impregnating said mineral oil comprises at least l0% by weight of said composition. 7

16. A composition according to claim 14 said aminoplast resin is at least one member selected from the class consisting of dimethylol dihydroxy ethylene urea, carbamates, propylene urea, dimethylol ethylene urea and acrylamides.

* k t i UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTION Patent 3.617.188 Dated November 2, 1971 Inventor DUANE W SNYDER It is certified that error appears in the aboveidentified patent and that said Letters Patent are hereby corrected as shown below:

Col. 3, line 5, after "or" delete "visa" and insert vice Col. 3, line 42, before "acrylonitrile" insert both Col. 4, line 42, "formulas" (both occurrences) should be changed to read formulae Col. 4, lines 67 70, Formula III should read as follows:

R 0-cHR Col. 6, line 2, delete "reative" and insert reactive Col. 7, line 26, delete "270F" and insert 275F Col. 8, line 64, delete "tented' and insert tenter v1 PO-IOSO (10-69) USCOMM-DC scan-Pea e u c r: nnnnnnnnnnnnnnn nu: nnnr: "a. 0-);6-55t UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTION Patent No. 3,617,188 Dated November 2, 1971 Inventor(s) DUANE W. SNYDER It is certified that error appears in the above-identified patent and that said Letters Patent are hereby corrected as shown below:

Page 2 Col. 9, line 45, delete "44.6" in first line of table and insert 6 C line delete "1" before "5" in the first line of the table.

Col. 13, line 59, delete "onyx" and insert Onyx Signed and sealed this 27th day of August 1974.

(SEAL) Attest:

MCCOY M GIBSON, JR. C. MARSHALL DANN Attesting Officer Commissioner of Patents M $69) uscowwoc scan-Poo ".5. GOVERNMENT PIINTIIIG OFFICE: l9. O3li-3!4.

Claims

2. A method as defined in claim 1 wherein the fibrous textile material contaIns fibers selected from the class consisting of cellulosic fibers, polyester fibers and blends thereof.
3. A method as defined in claim 2 wherein said textile material is in the form of a fabric.
4. A method according to claim 3 wherein said fabric is 100 percent cotton.
5. A method as defined in claim 1 wherein said material is also treated with an aminoplast resin for imparting permanent-press properties to an article manufactured from said textile material.
6. A method as defined in claim 5 wherein said textile material is dried at a temperature below that at which curing of said textile resin takes place.
7. A method as defined in claim 6 which includes the additional step of curing said textile resin at a temperature no greater than about 325* F. after drying of said textile material.
8. A method of imparting soil-release and stain-release characteristics to a textile article of manufacture composed of a textile fabric containing substantially cellulosic fibers which comprises impregnating said fabric with a composition containing refined mineral oil to substantially saturate said textile material with said refined mineral oil and drying said fabric below a temperature at which substantial volatilization of said mineral occurs, said dried fabric containing at least about 5% by weight of said mineral oil based on the dried weight of said fabric and said mineral oil impregnated into said fabric has a saybolt viscosity at 100* F. of at least 200, a flash point of at least 400* F., an average molecular weight of at least about 440 and a specific gravity at 60* F. of at least 0.80.
9. A method as defined in claim 8 wherein said mineral oil is impregnated into said fabric from an aqueous bath containing at least one nonionic emulsifying agent for said mineral oil, said aqueous bath containing at least 10% by weight of said mineral oil.
10. A method of imparting soil-release and stain-release and permanent-press characteristics to a textile article of manufacture composed of a textile fabric containing fibers selected from the class consisting of cellulosic fibers, polyester fibers and blends thereof which comprises treating said fabric with (1) a refined mineral oil, and (2) an aminoplast resin, substantially drying said fabric and converting said resin to a thermoset state, said dried fabric containing at least 7% by weight of said refined mineral oil based on the dried weight of said fabric, and said mineral oil having a saybolt viscosity at 100* F. of at least about 350, a flash point of at least about 400* F., an average molecular weight of at least about 440 and a specific gravity at 60* F. of at least about 0.88.
11. A method as defined in claim 10 wherein the drying of said fabric is carried out prior to the curing of said aminoplast resin and at a temperature below the curing temperature of said resin and said treating step comprises impregnating said fabric with an aqueous solution containing said mineral oil in the form of an emulsion.
12. A method as defined in claim 11 wherein said aqueous solution also contains said aminoplast resin and a textile resin catalyst and said curing of said textile resin is carried out below about 325* F.
13. A method as defined in claim 12 wherein said textile resin is at least one member selected from the class consisting of dimethylol dihydroxy ethylene urea, carbamates, dimethylol ethylene urea, propylene urea and acrylamides.
14. A composition suitable for imparting soil-release, stain-release and permanent-press characteristics to a textile material which comprises (1) a refined mineral oil emulsion, (2) an aminoplast resin, (3) a textile resin catalyst suitable for polymerizing said aminoplast resin and wherein said mineral oil has a saybolt viscosity at 100* F. of at least about 200, a flash point of at least 400* F., and average molecular weight of at least about 440 and a specific gravity at 60* F. of at least about 0.80.
15. A composition according to claim 14 wherein said mineral oil comprises at least 10% by weight of said composition.
16. A composition according to claim 14 said aminoplast resin is at least one member selected from the class consisting of dimethylol dihydroxy ethylene urea, carbamates, propylene urea, dimethylol ethylene urea and acrylamides.