The United States of America As Represented by the Secretary of

Bethlehem K Andrews

Clark M Welch

Robert M Reinhardt

Robert J Harper, Jr

Leon H Chance

Gary F Danna

Darrell J Donaldson

John G Frick, Jr

Wilson A Reeves

Norton A Cashen

Nancy M Morris

Catalysts for the rapid esterification and crosslinking of fibrous cellulose in textile form by polycarboxylic acids at elevated temperatures are disclosed. The catalysts are acidic or weakly basic salts selected from the alkali metal dihydrogen phosphates and alkali metal salts of phosphorous, hypophosphorous, and polyphosphoric acids. Suitable polycarboxylic acids include saturated, unsaturated and aromatic acids, as well as alpha-hydroxy acids. The textiles so treated exhibit high levels of wrinkle resistance and smooth drying properties durable to repeated laundering in alkaline detergents, and do not contain or release formaldehyde. Textiles treated by the polycarboxylic acids and alkali metal phosphite or hypophosphite catalysts, and having residues of these catalysts present, may be identified by infrared spectroscopy and electron spectroscopy for chemical analysis, because these textiles exhibit the presence in infrared spectra of the phosphorus-hydrogen bond and the ester groups of cellulose crosslinked with the polycarboxylic acids, and the presence of trivalent phosphorus in spectra from electron spectroscopy for chemical analysis.

Catalysts and processes for formaldehyde-free durable press finishing of

Catalysts for the rapid esterification and crosslinking of fibrous cellulose in textile form by polycarboxylic acids at elevated temperatures are disclosed. The catalysts are acidic or weakly basic salts selected from the alkali metal dihydrogen phosphates and alkali metal salts of phosphorous, hypophosphorous, and polyphosphoric acids. Suitable polycarboxylic acids include saturated, unsaturated and aromatic acids, as well as alpha-hydroxy acids. The textiles so treated exhibit high levels of wrinkle resistance and smooth drying properties durable to repeated laundering in alkaline detergents, and do not contain or release formaldehyde.

The acetals, 2,3-dihydroxy-1,1,4,4-tetramethoxybutane, 3,4-dihydroxy-2,5-dimethoxytetrahydrofuran, and glyceraldehyde dimethylacetal, when applied to cotton fabric by conventional pad-dry-cure procedures using special combined acid catalysts, were found to crosslink cellulose hydroxy groups at a very rapid rate (e.g., 20 seconds at 160.degree. C.), thereby imparting improved wrinkle recovery in the range of that required for durable press finishing. Cotton fabrics treated with these acetals have the advantage of no formaldehyde release.

Agents for non-formaldehyde durable press finishing and textile products

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

To the surface of knitted cotton fabrics is applied from 20 to 90% wet add-on of crosslinking agent in a novel geometric pattern by any of several techniques including kiss-roll padding, printing, or transferring the solution of crosslinking agent from impregnated material to the surface of the knitted fabric, followed by drying and curing the moist textile at elevated temperatures, and finally by washing the cured fabric to effect differential shrinkage of the fabric in the applied design, which novel shrinkage in the fabric is fixed through the life of the fabric and is stable through subsequent launderings.

Knitted cotton fabric durably patterned by differential shrinkage

Knitted cotton fabrics in tubular form are impregnated to 20 to 35% wet add-on of crosslinking agent by any of several techniques including sprinkling, spraying, printing, or slop padding the solution of crosslinking agent to the outer surfaces of the fabric tube, or transferring the solution of crosslinking agent from impregnated material to the outer surfaces of the fabric tube, followed by a mechanical agitation step wherein the impregnated tubes are mechanically agitated at elevated temperatures under closed conditions, thereby eliminating agent migration toward fabric surfaces during drying of the cotton containing knitted fabrics in chemical treatments for smooth-drying properties and dimensional stabilization.

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New Orleans, LA, United States of America

Bethlehem K Andrews