Patent GB-1210748-A (GB)
Title: Finishing fibrous material consisting of or containing cellulose fibres
IPC: D06M15/423
Filed: 1968-10-17
Abstract: 1,210,748. Creaseproofing cellulosic materials. BADISCHE ANILIN-& SODA-FABRIK A.G. 17 Oct., 1968 [18 Oct., 1967], No. 49225/68. Heading DIP. Fibrous material which consists of or contains cellulose fibres e.g. cotton cloth, is creaseproofed by reacting it with a N-methylol amide of acrylic acid in a first stage in the presence of at least one stage or medium strength acid having a dissociation constant greater than or equal to 10<-4> as an acetalisation catalyst and in a second stage in the swollen condition in the presence of an alkaline catalyst, the first stage being carried out at a moisture content of the fibrous material of 4-16% by weight and at a temperature of not more than 50‹C without substantial loss of moisture. The N-methylol amide of acrylic acid used has the formula: in which R<x>, R<y> and R<z> are hydrogen atoms or alkyl radicals halving 1-4 carbon atoms. The N-methylolamide of acrylic acid may be used together with a crease resisting agent containing at least two N-methylol groups or ethers thereof e.g. a compound having the formula: in which R<1> and R<2> are hydrogen atoms or low molecular weight alkyl groups, R<3> and R<4> # are radicals of the formula R<5>-C-R<6>, which are connected together directly or via # R<7>-C-R<8>, -O- or N-R<9>, hydrogen atoms # or low molecular weight alkyl or alkoxymethyl groups, R<5>, R<7>, R<10> and R<11> are hydrogen atoms or low molecular weight alkyl groups, R<6> and R<8> are hydrogen atoms, hydroxyl groups or low molecular weight alkyl or alkoxy groups, R<9> is a hydrogen atom or a low molecular weight alkyl or hydroxyalkyl group, R<12> and R<13> are hydrogen atoms hydroxymethyl groups or low molecular weight alkyl or alkoxymethyl groups, A is a divalent aliphatic hydrocarbon radical having 2-8 carbon atoms and Z is zero or 1, or an unetherified or etherified N-methylol compound of melamine, ammeline, ammelide, guanidine, dicyanodiamide, dicyanodiamidine, thiourea or acetylenediurea. Suitable strong or medium strength acids are hydrochloric, sulphuric, phosphoric, oxalic, glycolic, maleic, monochloroacetic, trichloroacetic, tartaric or citric acid, which may be used in admixture with latently acid salts, e.g. ammonium chloride, sulphate, phosphate or nitrate, diethanolammonium hydrogen phosphate, ethanolammonium chloride, monoethanol ammonium hydrogen phosphate, 1 -hydroxy-2-methyl-propylammonium-2-chloride, magnesium, aluminium, zinc or zirconyl chloride or zinc nitrate or fluorborate. Suitalble alkaline catalysts are alkali metal hydroxides and carbonates and quaternary ammonium hydroxides. The fibrous material may be treated with the N-methylolamide of acrylic acid, acetalisation catalyst and if desired other creaseproofing agent successively or preferably together from an aqueous liquid or which may also contain wetting agents, optical brighteners, water repellents, softening agents or finishing agents by spraying, dipping or padding, squeezed to a pick-up of 50-100% by weight, dried to a moisture content of 4-16% by weight at a temperature of less than 130‹C and then either enclosed in a moisture impermeable sheet or stored in a chamber at the appropriate moisture content while reaction takes place at a temperature of not more than 50‹C for 2-36 hours. The fibrous material may then be washed or impregnated directly with an aqueous solution of the alkaline catalyst a further reaction effected with the material in a swollen condition at a temperature not exceeding 500‹C for 12-24 hours. The material may then be washed and dried.