Patent GB-531751-A (GB)
Title: A process for improving the properties of cellulosic fibres or materials containing them
IPC: D06M15/423
Filed: 1939-05-01
Abstract: 531,751. Treating cellulose dyeing. SOC. OF CHEMICAL INDUSTRY IN BASLE. May 1, 1939, Nos. 12964 and 12965. Convention dates, May 5, 1938, and April 19, 1939. Sample furnished. [Classes 2 (ii) and 15 (ii)] Basic nitrogen is fixed on cellulose or compounds containing cellulose by treatment with a carboxylic acid methylolamide in which the carbonyl group is united by a carbon-to-carbon linkage to a residue free from basic nitrogen atoms and containing at least one halogen atom, followed by heating and further treatment with a basic nitrogen compound which reacts with the halogen-containing residue. Methylolamides of aliphatic, aromatic, mixed aliphaticaromatic, cycloaliphatic or heterocyclic carboxylic acids may be employed ; specified aremethylolchloracetamide ; #-chloropropionic, α-bromobutyric and α-bromolauric acid methylolamides ; chlorosuccinic acid dimethylolamide; p-chloromethylmethylolbenzamide, and methylolamides of naphthenic and resin acids containing halogen atoms capable of exchange. The material may be impregnated with aqueous or organic solvent solutions or dispersions of the methylolamides, advantageously in the presence of an acid catalyst, e.g. formic, acetic, oxalic, lactic or glycollic acid : urea nitrate, or potassium bisulphate. The methylolamide may be produced during the treatment by using a bath containing the carboxylamide and formaldehyde. After optional drying at a low temperature, the impregnated material is heated, e.g. to 110C. The basic nitrogen compound may comprise ammonia, or a primary, secondary or tertiary amine. e.g. methylamine ; mono-ethanolamine, diethanolamine, trimethylamine, triethanolamine, pyridine or dimethylaniline. The treated materials may be dyed with acid dyestuffs, e.g. acid wool dyestuffs, dyestuffs which contain metal in complex union, mordant dyestuffs, sulphuric acid ester salts of vat dyestuffs, or dyestuff esters or amides as described in Specifications 480,358, 482,184, and 505,504 ; acid dyestuff intermediates are also absorbed on the fibre. Acid dyestuffs may, in suitable cases, be diazotized on the fibre and developed with azo-compounds and suitable dyestuffs may be treated on the fibre with diazonium compounds. The impregnated material may also be caused to react with a basic nitrogen atom to form a dyestuff, for instance, by further treatment with aminoanthraquinones, e.g. 1:4-di-(p-aminophenyl)- aminoanthraquinone Specified cellulose materials are cotton, viscose and copper artificial silk, paper and mixtures of cellulose with other fibres, e.g. wool. The material may be cleansed by a de-sizing operation before treatment. In an example, cotton cloth is treated at 30-40C. with an aqueous solution of methylol-chlor acetamide, squeezed, dried at 50-60C. and heated to 110-115C., rinsed in boiling water, centrifuged and immersed in pyridine at 60-80C., again squeezed, rinsed in boiling water and dried. The treated fabric has pronounced capacity for dyeing with acid wool dyestuffs. Similar results are obtained with methylolamides of #-chloropropionic, α-bromo-lauric and α-bromonaphthoic acids, or with 4-w-chloromethyl-methylolbenzamide. A sample has been furnished under Sect. 2 (5) of cotton treated with methylolchloracetamide and dyed greenishblack by further treatment with 1:4-di-paminophenyl )-aminoanthraquinone. The Specification as open to inspection under Sect. 91 describes also the following matters : (1) treatment of the impregnated material with a sulphonic acid to impart a soft finish and (2) treatment of cellulosic materials with an hydrooxylated methylolamide to render the materials susceptible to dyeing with a diazonium compound. A further example of (1) is also given in which cotton is treated with a solution of N-oxymethylsalicylic acid amide and further treated with a diazo compound, e.g. diazotized aniline or diazotized 1-amino-2-methoxy-4- nitrobenzene. This subject-matter does not appear in the Specification as accepteo.