Patent GB-486527-A (GB)
Title: Improvements in the production of cellulose derivative yarns, foils and other materials
IPC: C08B15/06
Filed: 1936-12-03
Abstract: Cellulosic material, containing hydroxy groups or unsaturated radicles and free from halogen atoms, is made to react with ammonia or an organic nitrogen-containing compound in which the only reactive radicles are the nitrogen-containing radicles so as to introduce non-acidic nitrogen into the cellulosic material, and the reaction is carried out in the presence of a metal or metal compound which acts as a catalyst.  Natural cellulose materials such as cotton linters or chemical or mechanical wood pulps may be subjected to the process and they may be pretreated with organic or inorganic acids.  Regenerated cellulose materials, including those obtained by de-esterifying cellulose acetate or nitrate, and cellulose ester or ether materials containing hydroxy, carboxy, or unsaturated groups may be treated. Cellulose tri-esters may be treated provided the conditions are such that hydroxy groups are initially produced.  Natural cellulose materials may be in the form of cotton, linen, or hemp yarns, or paper.  Regenerated cellulose and cellulose derivatives may be in powder, grain, or flake form, or in the form of filaments, yarns, films, or foils, including effect threads obtained by partial esterification of cotton threads.  Yarns may be treated in bobbin or cake form or after association to form fabrics.  The nitrogen-compound may be gaseous or liquid ammonia, an alkylamine, alkylol-amine, ethylene diamine, acetamide, amino-acetic nitrile, ammonium or ethyl carbamate, urea, thiourea, piperidine, cyclohexylamine, aniline, or phenylene diamine.  The reaction may be carried out in presence of diluents such as alcohol, benzene, decahydronaphthalene, acetone, dioxane, or diamyl ether.  It may be conducted so that the cellulose derivative goes into solution or remains undissolved and retains its initial form.  Copper, iron, nickel, thorium oxide, tungstic oxide, alumina, zinc chloride, metal phosphates, manganese sulphate or chloride, platinic chloride, or copper sulphate, may be used as catalyst.  Metals forming nitrogenous complex salts may be introduced in uncombined form or as a nitrogenous complex.  The cellulosic materials may be impregnated with a solution of nickel carbonyl and then heated to decompose the nickel compound, or heated in liquid ethylene diamine under pressure to decompose the nickel compound and form the nitrogenous cellulose derivative in the same operation. Treatment with the nitrogenous compound is preferably carried out at raised temperature and pressure.  The products may be subjected to further treatments such as esterification or etherification. Free amino groups may be alkylated or acidylated.  Nitrile groups may be reduced, hydrated, or hydrolyzed to amino, amido, or carboxyl groups.  The products if not already in filament or film form may be made into such materials by dissolving and extruding or casting the solutions.  The products have good affinity for acid dyes.  The amino groups may be diazotized so that dyes may be formed by direct reaction with the products.  In an example, allyl cellulose is heated in a closed vessel with methylamine and copper sulphate.  In another example, regenerated cellulose filaments are impregnated with nickel carbonyl in a mixture of alcohol and benzene; they are heated in a closed vessel and the filaments thus impregnated with finely divided nickel are heated in a closed vessel with anhydrous ammonia.  Specifications 207,562, 249,173, 263,938, [all in Class 2 (ii)], and 345,989 are referred to.