The United States of America As Represented by the Secretary of

Robert M Reinhardt

Russell M Kullman

Donald J Daigle

Eugene J Blanchard

Bethlehem K Andrews

Anionically dyeable smooth-dry crosslinked cellulose is produced by modifying cellulose-containing material with the combination of a hydroxyalkylamine or a hydroxyalkyl quaternary ammonium salt, one or more glycols, and a crosslinking agent. The reaction is typically catalyzed with salts such as zinc nitrate or magnesium chloride used either alone or in conjunction with citric acid. Types of usable anionic dyes include acid, direct, and reactive dyes. The cellulose-containing material may be in the form of fibers, threads, linters, roving, fabrics, yarns, slivers and paper.

Anionically dyeable smooth-dry crosslinked cellulosic material created

Anionically dyeable smooth-dry crosslinked cellulose is produced by modifying cellulose-containing material with the combination of a hydroxyalkylamine or a hydroxyalkyl quaternary ammonium salt, a methylolamide crosslinking agent and one or more reactively inert glycol ether swelling agents. The reaction is typically catalyzed with salts such as zinc nitrate or magnesium chloride used either alone or in conjunction with citric acid. Types of usable anionic dyes include acid, direct, and reactive dyes. The cellulose-containing material may be in the form of fibers, threads, linters, roving, fabrics, yarns, slivers and paper.

Anionically dyeable smooth-dry crosslinked cellulosic materials are produced by treatment of methylolamide crosslinked cellulosic materials with an alkali swelling agent such as sodium hydroxide prior to dyeing. Attainable color strength is dependent upon both the concentration and the contact time of the alkali swelling agent with the cellulosic material. Types of usable anionic dyes include acid, direct, and reactive dyes. The cellulose-containing material may be in the form of fibers, threads, linters, roving, fabrics, yarns, slivers and paper.

Post-crosslinking treatment of cellulosic materials for enhanced

Methods for lowering the free formaldehyde release in carbamate durable press treatment solution and finished fabric are disclosed. Concentrated carbamate finishing agent solution of lowered free formaldehyde content comprises oxidizing a carbamate finishing agent solution containing free formaldehyde with a sufficient amount of magnesium monoperoxyphthalate oxidant to decrease the free formaldehyde content of the solution. Sufficient amount of catalyst is added to this solution to produce press properties in cellulose containing fabric to make a treatment bath. Cellulose containing fabric is immersed in this bath for sufficient time and temperature to produce lowered free formaldehyde release carbamate durable press finished fabric. High free formaldehyde carbamate-finished durable press cellulose containing fabric can be treated with a solution of magnesium monoperoxyphthalate oxidant of sufficient concentration for sufficient time and temperature to oxidize the free formaldehyde and thereby produce a lowered free formaldehyde release carbamate durable press finished fabric.

Oxidation process to decrease free formaldehyde in durable press

Hydroxymethylated organic carbamates are reacted with water soluble alcohols to produce etherified hydroxymethylated carbamates which are used with an acid catalyst to treat cellulosic textiles for sufficient time and temperature to produce a durable press low formaldehyde release cellulosic textile. Carbamates from the group consisting of alkyl or alkoxyalkyl carbamates of less than six carbons can be used. Water soluble aliphatic monohydric and polyhydric alcohols of one to six carbons are also satisfactory. The hydroxymethylated carbamate is reacted with the alcohol at about 10.degree. C.-100.degree. C. for about 0.5 to 16 hours at a pH from about 1 to 6. Concentrations of acid catalyst range from 0.5 to 3.0% of the solution. Curing temperatures range from about 120.degree. C. to 160.degree. C. for about 0.5 to 10 minutes.

Agents to produce durable press low formaldehyde release cellulosic

Hydroxymethylated organic carbamates are reacted with water soluble alcohols to produce etherified hydroxymethylated carbamates which are used with an acid catalyst to treat cellulosic textiles for sufficient time and temperature to produce a durable press low formaldehyde release cellulosic textile. Carbamates from the group consisting of alkyl or alkoxyalkyl carbamates of less than six carbons can be used. Water soluble aliphatic monohydric and polyhydric alcohols of one to six carbons are also satisfactory. The hydroxymethylated carbamate is reacted with the alcohol at about 10.degree. C. to 100.degree. C. about 0.5 to 16 hours at a pH from about 1 to 6. Concentrations of acid catalyst range from 0.5 to 3.0% of the solution. Curing temperatures range from about 120.degree. C. to 160.degree. C. for about 0.5 to 10 minutes.

Process to produce durable press low formaldehyde release cellulosic

Zwitterions are employed as catalysts in a chemical finishing process to treat cellulosic textiles with crosslinking agents and produce easy-care properties in the finished materials. The process comprises treatment of the textile material, such as cotton fabric, by impregnating it with a solution containing a cellulose-crosslinking agent and, as catalyst a zwitterion, alone or in combination with a magnesium salt, drying and curing the fabric. Said finished fabrics are characterized by an unusual combination of useful, desirable properties--smooth-drying appearance, wrinkle resistance, serviceable strength, and inoffensive formaldehyde release.

Zwitterion compounds as catalysts in easy-care finishing

An aluminum acetate salt solution containing sodium and chloride ions is prepared by reaction of aqueous aluminum chloride and sodium acetate. It is suitable for use as a catalyst in the treatment of cellulosic-containing textiles with formaldehyde or a formaldehyde-amide adduct crosslinking agent to produce durable press properties in the finished material. There is no discoloration in the thus-treated fabric which also exhibits greater strength than is normally present in fabric treated to the same level of wrinkle resistance with an aluminum salt catalyst.

Durable press finishing treatment for cellulose textiles employing an

An aluminum chlorhydroxide-phosphoric acid catalyst system has been devised that is practical for treatments of cellulose-containing textile materials with formaldehyde and formaldehyde-amide adducts under flash curing conditions to produce valuable, improved durable-press properties in the treated textiles.

Aluminum chlorhydroxide-phosphoric acid catalyst system for flash cure

Alkyl and aryl phosphonic acids and certain salts thereof have been found useful as catalysts for the chemical reactions involved in finishing cotton and other cellulosic textiles. These versatile catalysts can be employed in a variety of finishing treatments including dimensional stability, durable press, and flame resistance and are operative under a diverse range of processing conditions.

Catalyzing cellulosic textile finishing processes with phosphonic acid

A catalyst system composed of aluminum chlorhydroxide [Al.sub.2 (OH).sub.5 Cl] and hydrogen peroxide [H.sub.2 O.sub.2 ] is disclosed which through synergistic interaction of these components is highly efficient and effective in treatments of cellulose-containing textiles with formaldehyde-amide adduct crosslinking agents. Products with durable-press properties are produced through use of the new catalyst system in treatments employing flash curing conditions, i.e., short processing times at high temperatures, as well as in treatments employing curing temperatures down to 130.degree. C. with longer processing times. Unlike previously known synergistically activated catalyst systems based upon Al.sub.2 (OH).sub.5 Cl, the presently disclosed system utilizes the combination of Al.sub.2 (OH).sub.5 Cl with H.sub.2 O.sub.2, an oxidizing agent, rather than with an acid or a salt with latent acidic or Lewis acid properties.

Durable-press finishing of cellulose-containing textiles with aluminum

Salts of 1,3,5-triaza-7-phosphaadamantane can be utilized as catalysts for finishing cellulose-containing textile materials with methylol amide crosslinking agents to give products with improved wrinkle resistance and durable press properties. Inorganic, organic, and sulfonic acid salts, and mixed salt complexes of this new tricyclic phosphorus-containing compound provide effective catalysis in the chemical reactions needed for these finishing treatments. Salts of the corresponding phosphorus oxide, 1,3,5-triaza-7-phosphaadamantane-7-oxide, provided even stronger catalysis in similar treatments.

Durable press finishing with catalysis by triazaphosphaadamantane

Improvement in the strength of fabric finished for durable press properties with an N-methylol amide cross-linking agent and sulfuric acid catalyst is obtained by inclusion of magnesium sulfate in the finishing formulation.

Finishing of cellulose fabrics with N-methylol amide crosslinking

The invention provides a cellulose-dyeing dyestuff having the formula ##EQU1## wherein Z is the chromophoric radical of a cellulose-dyeing dyestuff containing a vinyl sulfone group (--CH.sub.2 CH.sub.2 SO.sub.2 --), e.g. Cl Reactive Violet 4 and Cl Reactive Black 5; B is --CH.sub.2 CH.sub.2 --, --CH.sub.2 CH.sub.2 CH.sub.2 --, or ##EQU2## A is --O-- or --S--; and X is --H, --CH.sub.2 OH, --CH.sub.2 OCH.sub.3, or ##EQU3## which dyestuff will dye a cellulosic material by heating in the presence of an acid catalyst. The cellulose-dyeing dyestuff of the invention is prepared by reacting a conventional cellulose-dyeing dyestuff having a chromophoric radical containing the aforesaid vinyl sulfone groups (e.g., Cl Reactive Black 5 and Cl Reactive Violet 4) with a hydroxy carbamate, and methylolating the resulting product. The utility of conventional cellulose-dyeing dyestuffs, which are normally reactive with cellulosic materials under alkaline conditions, is greatly extended by converting them to the methylolated derivatives of the invention, through prolonged shelf life and compatibility with selected acidic catalysts.

Methylolated reaction product of a hydroxy carbamate and

Improvement in strength and elimination of coloration are achieved in fabrics finished for durable press properties by treatment with an N-methylol amide crosslinking agent and aluminum sulfate catalyst when sodium dihydrogen phosphate is included in the finishing formulation. These effects are achieved when the weight ratio of sodium dihydrogen phosphate to aluminum sulfate is 2.05.

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New Orleans, LA, United States of America

Robert M Reinhardt