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Publication numberUS3909861 A
Publication typeGrant
Publication dateOct 7, 1975
Filing dateOct 5, 1973
Priority dateOct 5, 1973
Publication numberUS 3909861 A, US 3909861A, US-A-3909861, US3909861 A, US3909861A
InventorsRobert M Reinhardt, Norton A Cashen, Wilson A Reeves
Original AssigneeUs Agriculture
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Aluminum chlorhydroxide catalyst systems for treatments to give wrinkle resistant textiles
US 3909861 A
Abstract
Aluminum chlorhydroxide catalyst systems are applicable in a broad variety of finishing techniques for producing wrinkle resistant textile materials. Al2(OH)5Cl is unique in its versatile effectiveness in the catalysis of formaldehyde and formaldehyde-amide treatments of cellulose-containing textiles. It can function alone as catalyst, with strong acids to attenuate their catalytic activity, or with weak acids and salts to give synergistically activated catalysis.
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Tlimited States Patent [191 Reinhardt et a1. 9

[ Oct. 7, 1975 ALUMINUM CHLORHYDROXIDE CATALYST SYSTEMS FOR TREATMENTS TO GIVE WRINKLE RESISTANT TEXTILES [75] Inventors: Robert M. Reinhardt, New Orleans;

Norton A. Cashen; Wilson A. Reeves, both of Metairie, all of La.

[73] Assignee: The United States of America as represented by the Secretary of Agriculture, Washington, DC.

22 Filed: Oct. 5, 1973 21 Appl. No.1 404,042

7,300,600 1/1973 Japan 1,767,934 6/1971 Gennany 1,511,388 1/1968 France OTHER PUBLICATIONS Chemcon Database Reference Catalyst System for Creasing Fully Cured Durable Press Goods U.S.D.A. ARS 7298, 43-45, (1972).

Primary Examiner-Benjamin R. Padgett Assistant Examiner-Donald P. Walsh Attorney, Agent, or Firm-M. Howard Silverstein; Max D. Hensley [5 7] ABSTRACT Aluminum chlorhydroxide catalyst systems are applicable in a broad variety of finishing techniques for producing wrinkle resistant textile materials. A1 (OH) Cl is unique in its versatile effectiveness in the catalysis of formaldehyde and formaldehyde-amide treatments of cellulose-containing textiles. It can function alone as catalyst, with strong acids to attenuate their catalytic activity, or with weak acids and salts to give synergistically activated catalysis.

114 Claims, No Drawings 1 ALUMINUM CHLORHYDROXIDE CATALYST SYSTEMS FOR TREATMENTS TO GIVE WRINKLE RESISTANT TEXTILES FIELD TO WHICH INVENTION RELATES This invention relates to wrinkle resistant fabrics. More specifically, it relates to catalyst systems that are useful in the treatment of cellulose-containing textile materials with formaldehyde and certain formaldehyde-amide adduct finishing agents to give wrinkle resistant textile products.

OBJECTS OF THE INVENTION It is an object of the present invention to obtain fabrics with levels of wrinkle resistance that make them valuable for durable press clothing and household items.

It is a further object to provide catalyst systems that are efficient and practical for use in conventional as well as in specialized and unusual finishing treatments for cellulose-containing textiles.

A still further object is to provide a material that can be used with strong acid catalysts to dimish the undesirable effects of these acids without eliminating the excellent catalysis they produce.

A still further object is to provide a material that can be used with weak acids and salts to give catalytic effects greater than those of either component employed separately.

A still further object is also to provide catalyst systems which give durable press fabrics which though fully cured can be creased by simple processing methods so that the creases as well as the smoothness and wrinkle resistance are durable to repeated laundering.

Other objects will become apparent to those of ordinary skill in the art upon studying the specification and examples of the invention.

HOW THE OBJECTS OF THE INVENTION ARE ACHIEVED The objects of the present invention are achieved by the use of catalyst systems based upon aluminum chlorhydroxide in treatments for cellulose-containing textiles with formaldehyde or foramldehyde-amide adduct finishing agents. These systems in which aluminum chlorhydroxide are used either alone or in combination with other materials provide efficient catalysis in conventional processing as well as in specialized and unusual treatments. Unexpectedly, aluminum chlorhydroxide functions in various roles depending upon the finishing treatment in which it is used. It acts alone as catalyst in many treatments, as a moderator with strong acids, and as an activator with Weak acids and certain salts. Furthermore, fully cured, wrinkle resistant fabrics from treatments with aluminum chlorhydroxide catalysis can be durably creased by simple processing methods--methods so simple that they are applicable in the home.

ALUMINUM 'CHLORHYDROXIDE Aluminum chlorhydroxide is widely used in cosmetics, deodorants, shaving lotions, and other personal products. Because of the large amounts consumed, the price is relatively low even in the purity required for these uses. Although various aluminum chlorhydroxide complexes are known, that commonly used and, thus readily available, has the empirical formula: A1 (OH) Cl. It is sometimes called aluminum hydroxy- 2 chloride or, the 5/6 basic aluminum chloride complex, as it may be considered to be aluminum chloride with '5/6 of the chlorine replaced with hydroxyl groups. De-

velopment ofa grade suitable for textile processing, but not necessarily as pure as needed for cosmetics, could afford a further decrease in the cost of aluminum chlorhydroxide.

Specifications for the present commercial product indicate the presence of about two molecules of water of hydration per complex unit. Furthermore, there are indications that aluminum chlorhydroxide exists, particularly in aqueous solutions, as oligomers of the simple empirical formula which may be represented as: [Al (OH),-,Cl.2H O]x wherein x may be I or an integer of low value.

Solutions of Al (OH) Cl are mildly acidic and have excellent buffering capacity. Solutions ranging to percent concentration exhibit a pH of about 4-4.5. By its usage for many years in cosmetic applications, aluminum chlorhydroxide has been demonstrated to be safe even for direct application to human skin.

Although Al (OH) -,Cl is the most common of the aluminum chlorhydroxide complexes, other are known.

They all may be represented by the simple formula:'

Al (OH),,Cl,, wherein n is an integer below 6. Often the complexes exist in mixtures in which the overall composition is, for simplicity, expressed as the average formula rather than that indicative of the true structure. Thus, the formulae are sometimes expressed such that the value of n is not a whole number. For example, we have used a complex in which the empirical formula was AI (OH)., CI, although this probably was, in reality, a mixture with a ratio of two Al (OH) Cl complexes to one Al (OH) Cl complex.

The lower the value of n in the general formula for the aluminum chlorhydroxide complexes, the greater is the acidity of the complex and the greater is the catalytic power of the complex. However, as acidity and catalytic power become greater, the greater is the need for control of the finishing treatment to preclude degradation and other undesirable side effects to fabric.

SCOPE OF THE INVENTION With suitable adjustment, all of the various aluminum chlorhydroxides can be used in the catalysis of wrinkle resistance finishing treatments. However, the most versatile is Al (OH) Cl. Those complexes in which the ratio of OH to Cl is lower are more acidic and thus less applicable in some embodiments of the invention. A1 (OH) =,Cl is the preferred complex for use in the catalyst systems of this invention.

Concentrations of Al (OH) =,Cl that can be used are 0.1 to about 5 percent by weight of the treatment bath. Preferred concentration is from about 0.25 to 3 percent.

Aluminum chlorhydroxide can be employed alone as catalyst for wrinkle resistance treatments but in certain embodiments of the invention, Al (OH) Cl is used in conjunction with other materials to produce specific catalytic effects. It has been found that when used in conjunction with strong acid catalysts, Al (OH) Cl serves to buffer the treatment solution and attenuate the catalytic activity of the strong acid. On the other hand, when Al (OII) Cl is used with weak acids and certain salts, a synergistic effect results to give catalyst systems with greater activity than that of either of the components individually. This ambivalent behavior in diverse catalyst systems is unexpected and surprising. It

3 makes aluminum chlorhydride a valuable chemical for broad application and utility in the catalysis of a wide range of wrinkle resistance treatments.

Among strong acids with which Al (OH) Cl can be used to moderate their catalytic activity are the mineral acids, hydrochloric acid and nitric acid but not sulfuric acid (immediate precipitation occurs when Al OH );,Cl is used with sulfuric acid) and sulfonic acids such as hydroxymethanesulfonic acid and the like. Concentrations operative in strong acid/Al (OH) Cl catalyst systems include from about 0.1-1.2 percent acid and l-3% Al (Ol-l) ,Cl.

An entirely different catalytic effect is produced in treatments in which Al (OH),,Cl is used with weaker inorganic acids such as phosphoric acid and many organic acids. A synergistic interaction occurs so that greater catalysis results from the use of such acids and Al (Ol-l). C1 than from either alone. Among organic acids which have been found to give synergistically activated catalyst systems with Al OH) Cl are fatty acids such as formic acid, acetic acid, propionic acid, and the like, unsaturated acids such as acrylic acid and the like, dicarboxylic acids such as oxalic acid, succinic acid and the like, hydroxy-substituted acids such as glycolic acid, lactic acid, malic acid, citric acid and the like, halo-substituted acids such as chloroacetic acid, trichloroacetic acid and the like, and cyanosubstituted acids such as cyanoacetic acid and the like. For catalyst systems based on these acids, concentrations of A1 (OH),,C1 of about 0.1-4% are used with about 0.1-5% of the acid.

Synergistic catalyst effects also are produced when Al (OH);,Cl is used in conjunction with certain salts such as magnesium chloride, zinc chloride, zinc nitrate, and the like. About 2% Al (OH) Cl is used with about 0.2-3 percent of the salt although other concentrations of the aluminum complex probably could be employed. Al (OH) Cl is not compatible with Mg(H PO nor with alkaline salts such as potassium carbonate, sodium bicarbonate, and the like.

The catalyst systems of this invention can be used in treatments of textiles with formaldehyde and formaldehyde-amide adduct finishing agents. There are advantages in the use of these catalyst systems with formaldehyde and with certain, but not all, formaldehyde-amide adduct agents. The catalyst systems of this invention operate well with urea, cyclic urea, uron, and carbamate type finishing agents. Typical of these agents are dimethylol urea, partially methylolated urea,

methylated urea-formaldehyde, dimethylol ethyleneurea, dimethylol dihydroxyethyleneurea, dimethylol propyleneurea, dimethylol substituted propyleneurea, tetramethylol acetylenediurea,

bis(methoxymethyl)uron, dimethylol methyl carbamate, dimethylol ethyl carbamate and the like. However, with melamine type finishing agents such as trimethylol melamine, methylated trimethylol melamine and the like,,the catalysis provided by Al (OH) Cl is less effective than that provided by magnesium chloride, a relatively mild, common catalyst.

-Additives, softeners, modifiers, and other components customarily used in textile finishing pad baths can be used with the catalyst systems of this invention. The composition of the bath is limited only by the compatibility of these ingredients with the catalyst.

The textile materials treated with the catalyst systems of this invention may be in form of fibers, yarns and fabrics. The latter may be woven, knitted, or nonwoven structures. The material may be composed entirely of cellulosic fibers, either natural or regenerated, or may be composed of said cellulosics as components of the textile structure with other cellulosic, noncellulosic natural or synthetic fibers.

Finishing treatments in which the aluminum chlorhydroxide catalyst systems of this invention can be employed include conventional methods such as pad-dry-cure finishing, post-cure finishing, and the like, as well as unusual and specialized finishing treatments such as mild cure finishing, moist cure finishing (damp crosslinking), one-step dry-cure finishing, solvent vapor cure finishing, superheated steam cure finishing, and the like.

Pad-dry-cure finishing is the most common ofthe treatment methods for producing wrinkle resistant textile fabrics. As the name denotes, the sequence of steps consists of impregnating the textile material by immersing it in the treatment solution (pad bath), squeezing free of excess solution by passing through pad rolls, drying at a moderately elevated temperature (usually so that the temperature of the fabric does not exceed about 100C), and curing at a higher temperature, generally in the range of l50-l C. This type of treatment is sometimes referred to as precure finishing.

Post-cure finishing is a modification of pad-dry-cure finishing in which there is a delay period, often quite extended, between the drying step and the curing step. The fabric, impregnated with finishing agent and catalyst and dried but not cured, is called sensitized fabric. It can be shipped, held in warehouses, and fabricated (cut, sewn, and trimmed) into garments in this state and then creased and shaped prior to the final curing step.

Mild cure finishing is a process for producing wrinkle resistant goods in which cotton or polyester/cotton fabric, impregnated with a solution containing a suitable crosslinking agent and a strong catalyst, is heated at about 60-l00C for a relatively short period of time without prior drying. During the heat treatment, moisture content of the cotton fibers is reduced to about 3-5 percent and the strong catalyst promotes crosslinking of the cellulose chains with the fibers in a slightly swollen state. This type of treatment gives a finished fabric with a high level of wet wrinkle resistance together with a high level of dry wrinkle resistance. Detailed descriptions of mild cure finishing are given in the Textile Chemist and Colorist, Vol. 1, p. 415, 1969 and Vol. 2, p. 337, 1970.

Moist cure finishing, also called damp crosslinking, is a type of treatment that is popular in Europe for producing fabrics with high wet and dry wrinkle resistance. Cotton or cotton blend fabric is impregnated with a solution of crosslinking agent and strongly acidic catalyst, dried to a specific moisture level in the range of about 6-12 percent, sealed in a package to prevent change of moisture content, held at room temperature for about 12-24 hours, then neutralized and washed. Additional details of this type of finishing are available in US. Pat. No. 3,409,462.

One-step dry-cure finishing is a treatment method in which fabric is impregnated with a treatment solution and dried and cured in a one-step operation. These treatments are similar to mild cure finishing (no predry step) except that treatment temperatures ranging up to 180C are used. With treatment above C, the fabric is essentially completely dry and the fibers are totally collapsed during the crosslinking reaction. In Germany, treatments of this kind in which drying and curing are carried out in one operation are called shock curing. Some information on shock curing is given in Textilveredlung, Vol. 5, p. 334, 1970.

A description of solvent vapor cure finishing is available in the Proceedings of AATCC Symposium Textile Solvent Technology-Update '73, published by the American Association of Textile Chemists and Colorists, p. 79. In this new method of finishing, a solution containing a cellulose crosslinking agent and a catalyst is applied and the impregnated fabric is cured in the vapors from a boiling organic solvent.

Superheated steam cure finishing is a method whereby suitably impregnated fabric is cured in an atmosphere of superheated steam rather than in heated air as in conventional processing.

SUMMARY OF THE INVENTION The value of wrinkle resistance in textile products is well recognized by those engaged in the textile, garment, retail, and chemical industries as well as by the consumer. It has been estimated that more than 3 billion yards of woven smooth-drying cotton and cottonblend fabric presently are produced per year in the United States alone. The property of smooth-drying is, of course, a result of the wrinkle resistance of the fabric. To achieve the level of wrinkle resistance needed for smooth-drying, cellulose containing textiles must be chemically treated, usually with formaldehyde or a formaldehyde-amide adduct. The present invention provides catalyst systems for such treatments.

The catalyst systems of the present invention exhibit a number of advantages over catalysts that have been used heretofore. Among these advantages are production of products with improved properties, economies of processing, and the ability to achieve certain treatments under processing conditions previously found impossible, These and other advantages are obvious to those skilled in the art.

Aluminum chlorhydroxide catalyst systems are versatile. They are effective in a diverse range of finishing treatments. In fact, Al (OH) Cl is unique in that no other known material is available which can function as it does in various catalytic situations. That is, it can serve alone as a catalyst; it can be used with strong mineral and sulfonic acids to moderate their catalytic activity; and it can be used with weaker inorganic acids, organic acids, and certain salts to provide increased catalytic activity through synergistic interaction.

In pad-dry-cure finishing, Al (OH) Cl functions well as a catalyst. It can be used with a variety of finishing agents, including urea, cyclic urea, uron and carbamate types. Al (Ol-l) C1 compares favorably with the widely used magnesium chloride, zinc nitrate, and zinc chloride as a catalyst in treatments at l40l60C. Mixtures of Al (OH) Cl and these salts are more active as catalysts than either component alone and, thus, permit lower curing temperatures or shorter curing times. For example, chlorine resistant finishes were produced at 120C whereas curing temperatures 140160C were required when the treatment was catalyzed by the salts or Al (OH) Cl alone. The savings afforded in processing costs and energy required (particularly in view of current shortages) by use of lower temperatures and shorter times are advantageous features of these catalyst systems.

Effective catalysis in pad-dry-cure finishing at temperatures considerably lower than those of conventional treatments has been obtained with a broad range of compositions consisting of Al OH) Cl and various organic acids.

Al (OH Cl also is an effective catalyst for post-cure finishing. In treatments with dimethylol dihydroxyethyleneurea, the most commonly employed agent for post-cure processing, little or no reaction takes place in the sensitization treatment of the fabric nor in prolonged storage of the sensitized fabric. Creasing, either with a home-type electric hand iron gives an effective post-cure or with a commercial-type steam press followed by an oven cure produces sharp creases and a smooth pressed appearance in the fabric durable to laundering. Because Al (Ol-l) Cl has sufficient catalytic activity for post-curing, is relatively inactive in sensitization, and does not have adverse (hydrolytic) effect in unwashed, finished fabrics, it is particularly valuable for this important type of fabric processing.

In mild cure finishing, Al .(OH) Cl alone does not provide sufficient catalysis. When it is used with hydrochloric, nitric, or hydroxymethanesulfonic acid as the catalyst, it functions as a buffer. The pH of the pad bath is raised and the catalytic activity of the strong acid is attenuated. This moderation is manifested in slightly lower wrinkle recovery angles but considerably higher strengths in the finished fabrics. Importantly, the need for neutralization and afterwashing of the finished fabric is precluded. It is well known that without afterwashing, the strength of fabric finished by the mild cure treatment process is further decreased from the hydrolytic action of residual acid. However, if A1 (0H),,Cl is included in the treatment, such continued degradation is overcome and strength remains unchanged without an afterwash.

Phosphoric acid which has heretofore been unsuitable for mild cure treatments produced good durable press finishes when used in conjunction with Al (OH) Cl. Synergistic catalyst systems effective in mild cure finishing also resulted from combinations of Al (OH),-,C1 and various organic acids. Among these were acetic, lactic, formic, chloroacetic, oxalic, and trichloroacetic acid.

Similar synergism is operative between Al (OH) =,Cl and phosphoric acid in moist cure finishing (damp crosslinking). Al (OH) Cl alone can serve as catalyst for moist cure finishing with urea-formaldehyde. The latter often cannot be used because of polymerization induced by the strong acids usually employed in moist cure finishing.

Catalysis by Al (OH),=,Cl is efficient in one-step drycure treatments, which are similar to mild cure finishing but at temperatures up to C. Lower treatment temperatures are effective when Al (OH) Cl is augmented by even as weak an acid as acetic acid. However, crosslinking agents; with reactivities as diverse as those of formaldehyde and dimethylol ethyleneurea produce high durable press ratings when catalyzed by Al (OH) Cl alone.

Greater catalytic activity from a synergistic interaction between Al (Ol-l),-,Cl and organic acids is operative also in solvent vapor cure finishing. In this finishing method, the synergism can be obtained in two distinct ways. In one, Al (OH) Cl and an organic acid are included in the pad bath. The drying and heating action of the vapors from the boiling solvent promote the finishing reaction with the catalyst components 7 present in the fabric from padding application. In the other embodiment, the finishing agent and A1 (OH C1 are applied to the fabric by padding which is then cured in the vapors from a boiling mixture of an organic solvent and organic acid. That is, the synergistic catalyst activation results from one catalyst component applied from padding application and the second component from the hot vapors of the boiling solvent-acid mixture.

A1 (OI-I) C1 catalyst systems are operative with curing in superheated steam similar to their action in heated air. An Al (OH) C1/1actic acid catalyst system produced higher levels of wrinkle resistance than a magnesium chloride citric acid mixture in fabric finished in superheated steam at 116C. With steam superheated to 138C, Al (OH) =,C1 alone is sufficiently active as catalyst to give fabric with wrinkle resistance essentially equivalent to that of fabric similarly teeated but in an oven. Strength of the finish produced from curing in steam was about greater than that of the oven-cured finish.

Fully cured durable press fabrics can be creased by techniques that are applicable in commercial plants and in the home when A1 (OH) C1 or Al (OI-I) C1 in conjunction with certain mineral acids, organic acids, or salts (as disclosed above) serves as the catalyst system for both the finishing and creasing operations. These catalyst systems permit sharp, high quality, durable creases to be introduced into fully cured durable press fabrics composed of all-cotton and blends of cotton or other cellulosic fibers with synthetic fibers. The resulting creases are sharper and more durable than those which can be introduced into fully cure fabrics that were produced from treatment with conventionally-used catalysts. The term fully cured fabrics is used here in the sense that such fabrics have been treated so that they have a level of durable press smoothness sufficiently high that the fabric can be utilized, albeit without creases, without the need for further processing of any kind.

Creasing of the fully cured fabric can be carried out in several ways. These include: creasing on a commercial steam press followed by oven treatment; creasing on a commercial steam press followed by treatment on a hot-head press; creasing with a household-type hand iron; and creasing with a household steam iron fo1- lowed by treatment with a hand iron. The first two techniques are applicable for processing in a commercial plant while the last two are suitable for use in the home.

The finished fabric, of course, must not be washed before creasing, as extraction of residual catalyst pre- 8 vents breaking and reforming of crosslinks in the cotton component and inhibits introduction of a durable crease. Similarly, overcuring in application of the durable press finish must be avoided, or subsequent creasing IS poorer.

In addition to the more common Al (OH),-,C1, other aluminum chlorhydroxide complexes can be utilized in catalyst systems of the type described above for finishing cellulose containing textile materials for wrinkle resistance. Aluminum chlorhydroxide complexes of the general formula have been used wherein the value of n was 2-5. The acidity of the complex increases as the value of n decreases. The more acidic complexes (n 5) afford utilization of even lower concentrations, and less stringent processing conditions, i.e. shorter times and lower temperatures, than those detailed above for Al (OI-I) =,Cl catalyst systems.

DESCRIPTION OF SPECIFIC EMBODIMENTS The following examples further describe the invention. They are given merely as illustrations and should not be considered as limiting the scope of the invention.

In the examples, percentages reported in compositions and formulations are given as percentages by weight. Temperatures are given in degrees Centigrade. Properties of the fabrics were determined by standard test methods, when available, otherwise, unofficial, but generally recognized methods were used. The following procedures were used: breaking strength by ASTM D'1682-64; wrinkle recovery angles, conditioned by AATCC 66-1968 and wet by the same procedure on specimens soaked and blotted; durable press (DP) ratings, tumble-dried (TD) by AATCC 124-1969, Ill-B and line-dried (LD) by AATCC 124-1969, 111- A; crease ratings by evaluation under overhead lighting while mounted on an AATCC rating board, scale 5 (best) to 1 (poorest); damage due to retained chlorine (chlorination-scorch test) by AATCC 92-1967.

Nitrogen analyses reported were determined by the Kjeldhal method; formaldehyde analyses, by the chromotropic acid colorimetric method.

EXAMPLE 1 The use of Al (OI-I C1 as catalyst in finishing cotton fabric by the conventional pad-dry-cure method with various formaldehyde-amide adducts is illustrated by the data of Table 1.

TABLE l-continued Properties of Finished Fabrics Wr. Rec. Ang. Finishing Agent( 1 N, Brk. Str. (W+F), dcg. DP Rating (W). lb. Cond. Wet TD LD Methylated ureaformaldehyde 2.02 27.7 278 259 4.4 4.3 Untreated 48.4 182 166 1.0 1.5

(1 )Cotton printclnth impregnated with a solution containing 109: ofthe indicated finishing agent and 2'7: A1,(OH) Cl. dried for 7 min. at 60C. cured for 3 min. at 160C, and washed.

EXAMPLE 2 TABLE IV Fabric The of 9 concentrations of A12(OH )5.Cl as 15 Composition Treatment( 1) Fabric Properties catalyst in the finishing of cotton by the conventional Cure DP Rating Brk Strpad-drycure method with dimethylol methyl carba- C n P I t C m] t E glb e mate 15 illustrated by the data of Table II. o on 0 yes er a ys g 75 25 2.5 135 TABLE II 75 25 A1 (0H) C1 140 4.3 92 75 25 Zn NO- 160 4.5 85 Conc., A1 (OH) C1( 1 0.25 0.5 0.75 1.0 1.5 2.0 65 35 i 109 DP Rating (TD) 2.7 3.3 3.5 3.9 4.2 4.5 65 35 A|2(OH)5C| 140 4A 00 (I)Cotton printcloth impregnated with a solution containing 10% dimethylol i 2 methyl carbamatc and the indicated concentration ofA1,(OH),,C1. dried for 7 min. 50 50 A] CI 140 138 for 3 min. at 160C and washed. 2 5 50 so 211010.12 160 4.7 129 5 35 65 3.3 160 2 35 65 Al (OH) .,C1 .140 4.6 148 35 65 Zn(NO.-;)2 160 4.5 122 EXAMPLE 3 The use of other aluminum chlorhydroxide complexes as catalysts in finishing cotton fabric by the paddry-cure method with dimethylol dihydroxyethyleneurea is illustrated by the data of Table 111.

TABLE 111 Treatment( 1 (Cotton printcloth impregnated (about 90% wet pickup) with Solution containing 9% dimethylol dihydroxyethyleneurea and the indicated catalyst. dried for 7 min. at 60C. cured as indicated. and washed.

EXAMPLE 4 A comparison of AI (OH) CI and Zn(NO as catalysts in the finishing of cotton/polyester blend fabrics by the pad-dry-cure method with dimethylol dihydroxyethyleneurea is illustrated by the data of Table IV.

(1)Cotton polyester twills impregnated with. solution containing 9% dimethylol dihydroxyethyleneurea and 2% A1,(OH),.,C1 or 0.67: Zn(NO 6H O, dried for 7 min. at C. cured for 3 min. at the indicated temperature. and washed.

EXAMPLE 5 The use of A1 OH) Cl/1actic acid catalyst systems in finishing cotton fabric by the pad-drycure method with dimethyloi dihydroxyethyleneurea is illustrated by the data of Table 5. The synergistic interaction of the catalyst components and the unusually low (for pad-drycure finishing) Curing temperature should be especially noted.

TABLE V Catalyst concentration( 1 A1 (OH) C1 2.0 1.67 1.33 1.0 0.67 0.33 0.0 71 lactic acid 0.0 0.33 0.67 1.0 1.33 1.67 2.0 DP Rating (TD) 3.3 4.3 4.5 4.9 4.7 4.4 1.6

( 1 )Cotton printcloth impregnated with a solution containing 97: dimethylol dihydroxyethyleneurca and the indicated concentration of A1 OH ),,C1 and lactic acid, dried for 7 min. at 60C, cured for 3 min. at l 10C, and washed.

EXAMPLE 6 TABLE VI Treatment( 1) Properties of Finished Fabrics C l t S stem Curing Str. Retained 3 -2' H O ZnCl Al (OH) Cl Temp., N. Brk. Str. in Cl-Scorch DP Rating 70 deg. C (W), lb. Test, TD LD TABLE Vl-continued Treatment( 1 Properties of Finished Fabrics Catalyst System Curing Str. Retained Zn( NO '6H O ZnCl Al (OH),-,(fl Temp. N. Brki Str. in C1-Scorch DP Rating '71 '70 deg. C '71 (W), 1b. Test. "/1 TD LD 2 100 0.95 36.1 26 2.7 2.9 2 120 1.39 31.9 58 4.0 3.5 2 140 1.34 26.3 99 4.7 3.6 2 160 1.31 24.0 H 92 4.9 4.6 1 2 100 1.10 31.6 31 3.7 3.0 1 2 120 1.25 26.1 90 4.6 3.3 l 2 140 1.27 23.0 97 4.7 4.5 1 2 160 1.09 20.5 94 4.6 4.5 1 100 0.53 44.0 7 2.5 2.3 1 120 1.06 33.4 11 3.3, 2.9 l 140 1.30 28.6 34 4.3 3.3 1 160 1.37 27.4 90 4.4 4:3 (Untreated) 49.6 1.0 r 1.5

( 1 )Cotton printcloth impregnated with a solution containing 971 dimethylol dihydrnxycthylcncurea and, the

7 min. at 60C. cured for 3 min. at the temperature listed 100-160C). and washed.

EXAMPLE 7 indicated catalyst system. dried for 9 EXAMPLE 8 The use of various Al (Ol-l) Cl/organic acid catalyst systems in finishing cotton fabric by the pad-dry-cure method with dimethylol dihydroxyethyleneurea is illustrated in Table Vlll.

TABLE V111 Catalyst System,( 1 Properties of Finished Fabrics conc., mmo1./100 g Brk. Wr. Rec. Ang. DP

pad hath Str. (W-l-F). d eg. Rating A1 (OH) C1 Organic acid %N 1b. Cond. Wet TD LD 5 0.72 34.8 249 223 2.9 2.6 2.5 2.5 propionic 0.62 37.9 230 215 3.2 2.9 5 propionic 0.05 50.6 18 3 155 1.3 1.5 2.5 2.5 succinic 0.83 30.4 267 249 4.0 3.4 5 succinic 0.22 52.4 174 191 1.2 2.0 2.5 2.5 mallc 0.93 27.0 280 257 4.4 3.7 5 malic 0.45 46.0 213 191 1.7 a 2.4 2.5 2.5 citric 0.88 19.8 285 266 4.7 3.5 5 citric 0.60 36.2 217 216 2.3 2.5 3 3 acetic 0.76 30.4 3.2 2.6 3 3 glycolic 0.82 27.3 4.3 4.5 3 3 cyanoacctic 0.87 23.6 4.3 3.7 3 3 lactic 0.83 27.4 3.7 3.2 3 3 acrylic 0.73 29.9 3.5 3.5 3 0.57 37.1 2.0 2.0

( l )(utton printcloth impregnated with a solution containing 971 dimethylol dihydroxycthyleneurca and the indicated catalyst system. dried for 7 min. at 60C, cured for 3 min. at 120C. and Washed.

droxyethyleneurea is illustrated in Table Vll.

TABLE Vll Treatment( 1 Catalyst Systcm Al-,(OH =,Cl MgCl-yoH O "/1 DP Rating Curing Temperature deg. C.

EXAMPLE 9 A sample of cotton printcloth was impregnated with a solution containing 10 percent dimethylol ethyleneurea'and 2 percent A1 (Ol-l) C1, dried for 7 min. at 60C. and cured for 3 min. at 160C. The sample was divided into five portions. One portion was washed immediately after curing. The remaining portions were stored under ambient room conditions and a portion withdrawn periodically and washed until the final portion had been held for days prior to washing. The various portions were then subjected to the chlorination-scorch test (AATCC Test Method 92-1967) to determine the damage due to retained chlorine. Wrinkle resistance also was determined on the first and last portion. The results are shown in Table TABLE IX-continued TABLE XI Days held before Str. Retained Wr. Rec. Angle Properties of Finished Fabric washing in Cl-Scorch (W-l-F), deg. Catalyst System( 1 Wr. Rec. Ang.

Test, 72 Cond. Wet HCl Al (OH);,Cl N Brk. Str. (W-l-F), deg. 7c (W) 1b. Cond. Wet

Untreated 50.2 179 155 Cure: 7 min. at 60C 2 0.06 50.1 174 167 These data were compared with those given in FIG. 3

2, American Dyestuff Reporter, vo1. 49, p. 531, 1960 I Cure: 2 min at 00C. for similar treatments but wlth zinc nitrate, magnesium 2 0.43 50.4 179 175 0.37 1.25 23.1 271 287 chloride, and amine hydrochloride catalysts. Resis- 037 L5 L 2 262 272 tance to chlorine damage was rapidly lost by the fabrics 037 2 1,20 28,6 2 1 266 treated with zinc nitrate, magnesium chloride, and 3 H3 32-2 is; amine hydrochloride catalysis, i.e., more than 15 285 298 strength was lost in tests carried out on these samples 32 5:2 295 0. 304 after only 21 days storage inthe unwashed state. How- U l L29 276 308 ever, the greater stability of the dimethylol 0.19 2.5 1.07 29.1 272 265 ethyleneurea-finished cotton in the presence of residg-ZZ 23-2 533 5:2 ual Al (OI-I) .,C1 catalyst is evident from Table IX, 20 27 293 above; even after days storage, strength retained in 1.11 7 300 the chlorination/scorch test was more than percent. Furthermore, the wrinkle resistance of the latter was unaffected by the storage.

(1)Cotton printcloth impregnated with a solution containing 15% dimethylol methyl carbamate and the indicated catalyst system, cured under the Conditions shown (no predry), and washed.

(2)A portion of this fahric was stored without washing (after curing). Strength remained unchanged through 84 days of storage without an afterwash. This is in 25 contrast to the loss suffered upon storage in the unwashed state by fabrics treated similarly but without Al (OH),,Cl in the catalyst system, cf. FIG. 4 in Textile The use of A1 OH) C1 as catalyst in post cure Chemist & Colorist, v01. 1. p. 411. 1969. finishing of cotton-containing fabrics is illustrated in Table X. Essentially equivalent results were obtained in similar treatments of cotton printcloth. EXAMPLE 12 TABLE X Wr. Rec. Angle, Brk. Str. (W+F), deg. DP Rating Crease Treatment(1) %N of Untr. Cond. Wet TD LD Rating (TD) 50/50 cotton/polyester poplin sensitized Stored 0 days and washed 0.03 99 231 247 3.0 2.6 Stored days and washed 0.32 240 266 3.3 3.2 Sensitized, Steam pressed, and Cured Stored 0 days, pressed, cured, and washed 0.91 86 274 277 4.6 2.7 5 Stored 90 days, pressed, cured, and

washed 0.84 83 281 278 4.5 3.5 5

50/50 cotton/polyester twill sensitized Stored 0 days and washed 0.04 225 232 3.2 3.5 Stored 90 days and washed 0.44 85 231 248 3.3 3.4 sensitized, Steam Pressed, and Cured Stored 0 days, pressed, cured, and washed 0.82 68 263 260 4.9 3.7 5 Stored 90 days, pressed, cured, and washed 0.85 69 264 262 4.6 3.7 5

(1)1-ahrics sensitized by impregnating with a solution containing 971 DMDHEU and 271 Al (OH) ,Cl, and drying at 60C. Storage was at ambient room conditions. Swatches were creased on a commercial-type steam press and cured in an oven at C; poplin for 3 min., twill for 4 min.

EXAMPLE 1 1 The use of Al (OH) Cl/HCl catalyst systems in mild cure finishing of cotton fabric with dimethylol methyl carbamate is illustrated in Table XI.

The use of Al (OH) Cl/ph0sph0ric acid catalyst systems in mild cure finishing of cotton fabric with dimethylol methyl carbamate is illustrated in Table XII.

TABLE XII Properties of Finished Fabric Catalyst System( 1) Wr. Rec. Ang. H PO, A1. ,(OH) C1 N Brk. Str. (W+F) deg. DP Rating 0 '72v (W) lb. Cond. Wet TD LD Untreated 48.8 196 153 2 0.43 50.4 179 1.3 1.8 1.5 0.94 39.5 215 193 3.2 2.2 1.5 l 1.13 23.9 273 255 3.7 2.7 1.5 2 1.11 28.3 277 242 4.0 3.0 1,5 4 1.08 31.2 266 236 4.3 3.3 0.5 2 0.92 39.5 259 236 3.7 2.9 l 2 1.01 31.7 262 250 4.0 3.4 2 2 1.12 26.8 284 281 4.7 3.9

TABLE X11-continued Properties of Finished Fabric (I)Cotton print cloth impregnated with solutions containing 15'71 dimcthylol mcthyl carhamatc and the indicated catalyst system, cured for 2 min. at 100 C. (no prcdry). and washed.

EXAMPLE 13 EXAMPLE 15 The use of Al (OH) Cl/organic acid catalyst systems The use of Al (OH) Cl and Al (O1-1) Cl/acetic acid in mild cure finishing of cotton is illustrated in Table catalyst systems in one-step dry-cure finishing of cotton X111. fabric with formaldehyde is illustrated by the data of TABLE X111 DMMC Acid* 15% DMMC Acid 2% Al (OH Cl* Wr. Rec. Ang. Wr. Rec. Ang Acid N, Brk. Str. W-l-F), deg. DP Rating N, Brk. Str. (W+F), deg. DP Rating .71 (W), lb. Cond. Wet TD LD (W), lb Cond Wet TD LD 1.271 Acetic Acid 0.02 48.8 172 171 1.2 2.0 0.68 37.5 237 220 3.0 2.4 1.8?! Lactic Acid 0.07 49.3 176 156 1.5 2.0 0.97 36.0 258 247 3.5 3.3 0.92?! Formic Acid 0.03 49.3 174 163 1.2 2.0 0.85 37.0 252 229 3.3 3.3 1.89% Chloroacetic Acid 0.15 49.3 165 165 1.2 2.0 1.13 30.6 275 267 3.9 3.9 2.5271 Oxalic Acid 0.99 31.6 236 219 2.7 2.7 1.10 30.6 272 277 4.0 3.5 3.2771 Trichloroacetic Acid 1.20 33.5 255 244 3.3 3.6 1.21 30.6 268 286 4.0 4.4 None 0.32 48.8 186 179 1.6 2.0

Cotton print cloth impregnated with the indicated solution (DMMC dimcthylol methyl carbamate), cured for 2 min. at 100C. (no predry), and washed. Breaking strength of the untreated fabric was 49.3 lb.; wrinkle recovery angles were 189 (cond.) and 133 (wet). The concentrations employed were equivalent to mmol. of acid per 100 g of solution.

Table XV. EXAMPLE l4 TABLE XV The use of A1 (OH) C1/phosphor1c acid and A1 H Cl 1' catal st s stems in moi t c r fin- HCHO' )5 1cm: acid y y e 1.2% Acetic Acid, 10% ncno, ishing (damp crosslmkmg) of cotton fabric with di- AMOHhC] 207, Amomscl methylol methyl carbamate is illustrated by the data of lreatment Table XIV. Temp. HCHO, DP Rating HCHO, DP Rating TABLE XIV Treatment* Properties of Finished Fabric Catalyst System Lactic H 1 0 AI (OH),,CI, Acid, pH of N, Brk. Str. DP Rating Yr bath 70 (W), 1h. TD LD 1.96 1.85 0.61 46.3 2.5 2.3 1.96 2 2.0 0.93 36.5 3.9 3.3 2 4.2 0.08 51.0 l .4 1.7 1.8 2.4 0.05 49.2 1.5 1.7 2 1.8 2 8 0.62 44.3 2.7 2.3 (Untreated) 49.6 1.0 1.6

"Cotton print cloth impregnated with a solution containing 15% dimethylol methyl carhamate and the indicated catalyst system, dried at 60C. to about 67: moisture. scaled in plastic bags and held for 24 hours at room temperature, and washed.

The use of urea-formaldehyde (UF) in moist cure finishing is very difficult; in many cases, impossible. Precipitation of the pad bath due to polymerization of the 60 TD TD UF occurs immediately upon addition of the strong 22 2'6 Q03 15 acids usually used as catalysts. However, 2% A1 lg? -4 2.9 (OH) C1 as catalyst with UF in moist cure treatment 5: 3:2 22 (as detailed in the footnote to Table XIV) gave a fin- 2.27 4.5 2.02 4.4

' 1 65 lsh Cotton. Print cloth wlth rdnng of Print cloth impregnated with the indicated solutiomcurcd for 2 min. at IOU-180 and a breaking strength equal to Of the untreated (I. (no prcdry) and washed. Durable press rating of the untreated fabric was 1.0.

cotton. The pH of this bath was 4.1; there was no trouble with polymerization of the pad bath.

EXAMPLE 16 The use of Al (OI-I) C1 and Al (OH) =,Cl/acetic acid 18 the vapors from boiling perchloroethylene and from a 98:2 mixture (by weight) of perchloroethylene and acetic acid are exemplified in this table.

TABLE XVII Treatment Properties of Finished Fabric Br. Rec. Angle (W-l-F). deg.

Brk. Str. Pad Bath* Solvent Vapor** "/tN 7r o1 Untr. Cond. Wet

DMDHEU Perchl./acetic 0.27 98 190 209 DMDHEU/AI (OH) CI PerchL/acetic 0.73 Y 59 249 269 DMDHEU/Al (OI-I) =,Cl Perchloroethylene 0.60 79 234 220 DMDHEUIAMOHL CI Perchloroethylene*** 1.43 46 292 291 Untreated 100 206 162 Cotton print cloth impregnated (about 9071 wet pickup) with solutions containing 97: DMDHEU, 97 DMDHEU/2% A1 (OH),,Cl or 9% DMDHEU/1.1% Al- .(()H) Cl as indicated. DMDHEU dimethylol dihydroxyethyleneurea.

** Fabric dried for 7 min. at 60C. cured in the vapors of boiling solvent for 3 min., and washed. Vapors from perchloroethylene were 121C, and those from 98:2 mixture of perchloroethylene and acetic acid were 106C.

"*Cured for I min.

catalyst systems in one-step dry-cure finishing of cotton with dimethylol methyl carbamate is illustrated by the data of Table XVI.

I1 EXAMPLE 18 The use of A1 (OH) C1 catalyst systems in finishing treatments with curing carried out in superheated steam rather than in an atmosphere of heated air is i1- Iustrated by the data of Table XVIII.

TABLE XVIII Properties of Finished Fabric *Cotton print cloth impregnated (9071 wet pickup) with solutions containing 9'7: dimethylol dihydroxyethyleneurea and the indicated catalyst system. dried for 7 min. at C or not predried as indicated. cured in a chamber in an atmosphere of superheated steam for the time and temperature listed. and washed.

TABLE XVI Treatment* Properties of Finished Fabric Catalyst System Acetic Acid Al (OH),-,Cl Temp. N Brk. Str. DP Rating '/r "/1 Deg. C '71 (W), 1b. TD LD 1.2 2 0.04 47.9 1.6 2.2 1.2 2 0.85 32.1 3.3 2.6 1.2 2 1.15 29.1 4.4 3.3 1.2 2 1.20 25.0 4.5 3.7 1.2 2 1.15 23.3 4.7 4.3 1.2 2 1.14 22.2 4.6 4.7 1.2 100 0.02 49.6 1.0 1.8 1.2 160 0.11 47.7 1.4 1.9 2 80 0.04 53.2 1.5 1.7 2 100 0.36 47.6 2.3 2.0 2 120 0.72 37.8 2.9 2.6 2 140 0.98 34.4 3.7 2.9 2 160 1.08 30.1 4.0 3.7 2 180 1.10 26.0 4.2 3.7 (Untreated) 50.5 1.3 2.0

Cotton print cloth impregnated with a solution containing 157: dimethylol methyl carbamate and the indicated catalyst system. (no predry) cured for 2 min. at the indicated temperature. and washed.

EXAMPLE 17 The use of aluminum chlorbydroxides in the catalysis of finishing treatments with curing in the vapors from boiling solvents rather than in an atmosphere of heated air is illustrated by the data of Table XVII. Curing in EXAMPLE 19 A comparison showing the superiority of fully cured fabrics that have been finished with A1 (OH) C1 catalyst for subsequent creasing is given in Table XIX.

(a)Cotton/po1yester twills (of various fiber compositions) were fully cured by paddry-cure treatments with 971 dimethylol dihydroxyethyleneurea (DMDHEU) and 27: A1 (OH CI, and with 97: DMDHEU and (1.671 Zr\( NQM 'fiH O. They were not washed after curing. The fully cured fabrics were creased. as shown. than washed and tumble dried. DP ratings of the fully cured fabrics were 4.3-4.6. These values were essentially unchanged by the subsequent. creasing treatments.

(b)Creased by pressing on a commercial-type steam press at about 120C. for 15 TABLE XIX-continued Crease Rating Cotton/7: 35 50 65 75 Fully Cured Twill(a) Polyester. 71 65 50 35 25 sec. turned over, and pressed again. The creased fabric was then placed in a circulating air oven at 160C. for 3 min.

(c)Creased, as above on the steam press then the creased fabric was heat treated on a hot head press at 120C. for 30 turned over, and pressed again. (d)Creased by pressing with a home-type hand iron, surface temperature li (l('., for l min.

(e)Creased by pressing with a home-type steam iron, then pressed with a hometype hand iron, surface temperature 165C. for l min.

EXAMPLE 20 The creasing of fully cured all-cotton and cotton/polypropylene poplin fabrics that had been finished in Al (OH) Cl and Al (OH) Cl/lactic acid catalysis is illustrated in Table XX.

TABLE XX Finishing Treatment 9% DMDHEU chlorhydroxide complexes of the formula Al (OH),,Cl

,,, wherein n has a value of 2-5, as said catalyst.

2. A process for preparing cellulose-containing textiles with improved wrinkle resistance which process comprises:

a. padding a cellulose-containing fabric in an aqueous solution consisting essentially of water, about 0.1 to 5 weight percent of an aluminum chlorhydroxide complex of the formula Al (OH),,Cl wherein n has a value of 2-5 and about 9-15 weight percent ofa finishing agent selected from the group consisting of formaldehyde and formaldehyde-amide adducts,

b. drying the fabric from (a) at a temperature of about 60C. for a period of about 7 minutes, and

c. curing the fabric from (b) at a temperature of about 100-1 60C. for a period of about 3 minutes.

3. A process for preparing cellulose-containing textiles with improved wrinkle resistance which process comprises:

a. padding a cellulose-containing fabric in on aqueous solution containing about 0.1 to 5 weight percent of an aluminum chlorhydroxide complex of the formula Al (OH),,C, l ;.,,wherein n has a value of -5, about 9 to 15 weight percent of a finishing agent selected from the group consisting of formaldehyde and formaldehyde-amide adducts, and about 0.1 to 5 weight percent of an organic acid.

b. drying the fabric from (a) at a temperature of about 60C. for a period of about 7 minutes, and

c. curing the fabric from (b) at a temperature of about lOO-l 60C. for a period of about 3 minutes.

4. A process for preparing cellulose-containing textiles with improved wrinkle resistance which process comprises:

Lil

a. padding a cellulose-containing fabric in an aqueous solution containing about 2 weight percent of an aluminum chlorhydroxide complex of the formula Al (Ol-l),,Cl wherein n has a value of 2-5, about 9-15 weight percent of a finishing agent selected from the group consisting of formaldehyde and formaldehydeamide adducts and about 0.2 to 3 weight percent of a salt selected from the group consisting of zinc chloride, zinc nitrate and magnesium chloride,

b. drying the fabric from (a) at a temperature of about C for a period of about 7 minutes, and

c. curing the fabric from (b) at a temperature of about lOO-l 60C. for a period of about 3 minutes.

. 5. A process for preparing cellulose-containing textiles with improved wrinkle resistance which process comprises:

a. padding a cellulose-containing fabric in an aqueous solution containing about 0.1 to 5 weight percent of an aluminum chlorhydroxide complex of the formula A1 (OH),,Cl wherein n has a value of 2-5," about 9 to weight percent of a finishing agent selected from the group consisting of formaldehyde and formaldehyde-amide adducts, and about 0.1 to 5 weight percent of an acid selected from the group consisting of hydrochloric, nitric, hydroxymethanesulfonic, phosphoric acid, and

b. reducing the moisture content of the fabric from (a) to about 3-5 percent by curing said fabric by heating at a temperature of about 60l0OC. for a period of about 2 to 7 minutes, the higher temperature requiring the lesser time.

'6. A process for preparing cellulose-containing textiles with improved wrinkle resistance which process comprises:

padding a cellulose-containing fabric with an aqueous solution containing about 0.1 to about 5 weight percent of an aluminum chlorhydroxide complex of the formula Al (OH),,Cl wherein n has a value of 2-5, about 9 to 15 weight percent of a finishing agent selected from the group consisting of formaldehyde and formaldehyde-amide adducts, and about 0.1 to. 5 weight percent of an organic acid, and Y b. reducing the moisture content of the fabric from (a) to about 3-5 percent by heating at a temperature of about -60l0OC. for a period of about 2 to 7 minutes, the higher temperature requiring the lesser time.

7. A process for preparing cellulose-containing textiles with improved wrinkle resistance which process comprises: i

a. padding a cellulose-containing fabric with an aqueous solution containing about 15 weight percent of dimethylol methyl carbamate, about 2 weight percent of an aluminum chlorhydroxide complex of the formula Al (Ol-l),,Cl wherein n has a value of 2-5, and about O-2 weight percent of an acid selected from the group consisting of phosphoric and lactic acid, and

b. drying the fabric from (a) at a temperature of about 60C. to a moisture content of about 6 percent, and

c. curing the fabric from (b) at room temperature for about 24"hours, with the fabric sealed in a package q to prevent change of moisture content.

8. A process for preparing cellulose-containing textiles with improved wrinkle resistance which process comprises:

a. padding a cellulose-containing fabric with an aqueous solution consisting essentially of water, about 15 weight percent of urea-formaldehyde and about 2 weight percent of an aluminum chlorhydroxide complex of the formula Al (OH) -,Cl, and

b. drying the fabric from (a) at a temperature of about 60C. to a moisture content of about 6 percent, and

c. curing the fabric from (b) at room temperature for about 24 hours, with the fabric sealed in a package to prevent change of moisture content.

9. A process for preparing cellulose-containing textiles with improved wrinkle resistance which process comprises:

a. padding a cellulose-containing fabric with an aqueous solution containing about 9 to 15 weight percent of a finishing agent selected from the group consisting of formaldehyde and formaldehydeamidc adducts, about 0.1 to 5 weight percent of an aluminum chlorhydroxide complex of the formula Al (Ol-l),,Cl,, wherein n has a value of 2-5, and from to weight percent of an organic acid, and

b. curing the fabric from (a) by heating at a temperature of about 80 to 180C. for a period of about 2 minutes.

10. A process for preparing cellulose'containing textiles with improved wrinkle resistance which process comprises:

a. padding a cellulose-containing fabric with an aqueous solution consisting essentially of water, about 9 to weight percent of a finishing agent selected from the group consisting of formaldehyde and formaldehyde-amide adducts, and about 0.1 to 5 weight percent of an aluminum chlorhydroxide complex of the formula Al (OH),,Cl wherein n has a value of 2-5, and

b. drying the fabric from (a) at a temperature of about 60C. for a period of about 7 minutes, and

c. curing the fabric from (b) for from about 1 to 3 minutes in the vapors from a boiling solution selected from the group consisting of perchloroethylene and a mixture of 98 weight percent perchloroethylene and 2 weight percent acetic acid.

11. A process for preparing cellulosecontaining textiles with improved wrinkle resistance which process comprises:

a. padding a cellulose-containing fabric with an aqueous solution-containing about 9 weight percent of dimethylol dihydroxyethyleneurea, about 1 to 2 weight percent of an aluminum chlorhydroxide 5 complex of the formula Al (OH) Cl, and about 01 weight percent of lactic acid, and,

5 temperature of about 1 l6 l38C.

12. The process of claim 11 wherein the fabric from (a) is cured by treatment with superheated steam for about 6 minutes at a temperature of about 1 16l 38C.

13. A process for preparing durably creased, wrinkle resistant cellulose-containing textiles which process comprises:

a. padding a cellulose-containing fabric with an aqueous solution consisting essentially of water, about 9 weight percent of dimethylol dihydroxyethyleneurea and about 2 weight percent of an aluminum chlorhydroxide complex of the formula Al (OH),,Cl wherein n has a value of 2-5, and

b. drying the fabric from (a) at about C., and c. creasing the fabric from (b) by steam pressing, and d. curing the fabric from (c) by heating in an oven at about 160C. for a period of from 3 to 4 minutes.

14. A process for preparing durably creased, wrinkle resistant cellulose-containing textiles which process comprises:

a. padding a cellulose-containing fabric with an aqueous solution containing about 9 to 15 weight percent ofa finishing agent selected from the group consisting of formaldehyde and formaldehyde-amide adducts, about 0.1 to 5 weight percent of an aluminum chlorhydroxide complex of the formula Al (OH) Cl -n where n has a value of 25, and about 0 to 5 weight percent of an organic acid, and

b. drying the fabric from (a) at a temperature of about 60C. for a period of about 7 minutes and c. curing the fabric from (b) at a temperature of about to 180C. for a period of from about 2 to 3 minutes, and,

d. creasing the fully cured fabric from (c) by a method selected from the group consisting of i. creasing by pressing on a commercial-type steam press at about C. for 15 seconds, turning the creased fabric over and pressing again, followed by 45 heating in an oven at about C. for about 3 minutes.

ii. creasing on a steam press as in (i) then pressing on a hot head press at 120C for 30 seconds, turning the creased fabric over, and pressing again.

50 iii. creasing by pressing with a home-type hand iron with surface temperature at 180C. for about 1 minute.

iv. creasing by pressing with a home-type steam iron,

followed by pressing with :a home-type hand iron 5 with surface temperature at C. for about 1

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GB1107717A * Title not available
JPH07300600A * Title not available
JPH07327601A * Title not available
Non-Patent Citations
Reference
1 *Chemcon Database Reference - "Catalyst System for Creasing Fully Cured Durable Press Goods" U.S.D.A. ARS 72-98, 43-45, (1972).
Referenced by
Citing PatentFiling datePublication dateApplicantTitle
US4039282 *Jul 19, 1976Aug 2, 1977The United States Of America As Represented By The Secretary Of AgricultureDurable-press finishing of cellulose-containing textiles with aluminum chlorhydroxide-hydrogen peroxide catalyst system
US4088443 *Feb 6, 1976May 9, 1978The United States Of America As Represented By The Secretary Of AgricultureAluminum chlorhydroxide-phosphoric acid catalyst system for flash cure treatments to give improved durable-press properties in cellulose-containing textiles
US4176090 *Mar 10, 1978Nov 27, 1979W. R. Grace & Co.Pillared interlayered clay materials useful as catalysts and sorbents
US4248739 *Sep 4, 1979Feb 3, 1981W. R. Grace & Co.Stabilized pillared interlayered clays
US4469813 *Mar 18, 1983Sep 4, 1984Shell Oil CompanyProcess for the preparation of catalytically active cross-linked metal silicates
Classifications
U.S. Classification8/184, 502/231, 8/186, 8/187, 8/185
International ClassificationD06M15/423
Cooperative ClassificationD06M15/423
European ClassificationD06M15/423