Patent GB-808558-A (GB)
Title: Process for the improvement of fibrous material comprising linear, high-melting polyesters
IPC: D06M15/61
Filed: 1955-05-31
Abstract: Textile material consisting of or containing a linear synthetic polyester, especially polyethylene terephthalate, is first treated with a solution of a high-molecular aromatic polyhydric compound of tanning character, especially with tannin itself, and then, preferably in the hot, with a 1:2-ethyleneimide or a 1:2-ethylene-urea which contains a hydrocarbon residue with at least 6 and preferably 12 or more carbon atoms, whereupon, after drying, the material is heated.  The hydrocarbon residue is preferably a residue of an aliphatic hydrocarbon, but may be a residue of a cycloaliphatic hydrocarbon such as cyclohexane or a substitution product thereof, or an aryl residue substituted by a high-molecular alkyl residue.  Examples of 1:2-ethylene ureas which may be used are N - (4 - methylcyclohexyl) - N1 - (1:2 - ethylene)-urea, N - octadecyl - N1 - (1:2 - ethylene) - urea, N - (4 - isohexylphenyl) - N1 - (1:2 - ethylene) - urea and N:N1 - hexamethylene - bis - o  - (1:2 - ethylene) - urea.  Examples of 1:2-ethyleneimides which may be used are N-dodecyl sulphonic acid-1:2-ethyleneimide and polyvalent ethylene-1:2-imide compounds, e.g. the addition product of ethylene-imine with N:N-dicrotyl-ethylene-diamine or with N-methyl - N - di - (g  - crotylamino) - propylamine.  Instead of tannin there may be used acetals of higher polyalcohols, e.g. reaction products of low-polymeric polyvinyl alcohols with aromatic hydroxyaldehydes, such as salicyl aldehyde, 3:4-dihydroxybenzaldehyde, and resorcyl aldehyde, or hydroxyaryl acetals of condensation products from glucamine and dicarboxylic acids, e.g. oxalic or adipic acid, or of soluble polyesters of mannitol with dicarboxylic acids, and analogous polyurethanes from mannitol and diisocyanates.  There may also be used esters of aromatic hydroxycarboxylic acids, such as p-hydroxybenzoic acid, and polyalcohols, e.g. polyglycide, or amides of such hydroxy-acids with polyamines such as polyethyleneimine.  The polyhydric compounds can be taken up from ammoniacal aqueous solutions, if required with the addition of reducing agents, such as dithionites, for preventing oxidation of the polyhydric compounds. When solutions of salts of polyphenols are used, it is advantageous to dry in air containing carbon dioxide or vapours of volatile organic acids, or to acidify with very dilute acetic acid.  The take-up of the polyhydric compounds by the polyester material may be increased by the presence of swelling-agents such as chlorobenzene, chlorotoluene, chloronaphthalene, tetrahydronaphthalene, methylphenylcarbinol, or o- or p-hydroxydiphenyl, or by previous treatment of the material with concentrated sulphuric acid or concentrated zinc chloride solution.  The material, after treatment with polyphenols, and prior to treatment with ethylene-imine derivatives is preferably treated with a fixing agent such as tartar emetic or an aluminium, zirconium or tin salt or a silicone.  The treatment of the material with the ethylene imide or ethylene urea solutions or dispersions may be carried out at 40-100 DEG  C. and the thermal after-treatment may be at 90-120 DEG  C.  During the imide or urea treatment the material may be treated with aminoplast precondensation products, e.g. methylol derivatives of urea compounds, such as acetylene-diurein, of melamine or of polyvalent urethanes, such as butanediol-1:4-bis-carbamic acid ester, or their ethers, especially methyl ethers.  Alternatively the imide or urea treatment may be accompanied by a treatment with a polymerizable silicone, especially of the type containing reactive Si-H groups, to impart water-repellency to the material. In an example, a dyed polyethylene terephthalate worsted knitting yarn is treated at 60 DEG C. with one per cent of tannin dissolved in water, the pH of the solution having been adjusted to 5 with oxalic acid, and two per cent of tartar emetic, based on the weight of the yarn, is then added. After rinsing with cold water the yarn is treated at 40 DEG  C. with a 0.15 per cent aqueous dispersion of N-octadecyl-N1-(1:2-ethylene)-urea, spin-dried at 60-70 DEG  C., and heated for 1 hour at 100 DEG  C.  The process improves the handle of the materials and renders them water-repellent and anti-static.