Patent GB-759374-A (GB)
Title: Manufacture of artificial filaments and films of improved mechanical properties
IPC: D01F1/10
Filed: 1953-10-07
Abstract: Artificial filaments or films of improved mechanical properties are obtained by uniformly mixing with the masses to be extruded, or with the raw materials or intermediate products employed in the production of such masses, a finely divided metalloid oxide or metal oxide, which has been produced in aerosol form by thermal decomposition of a volatile compound of a metal or metalloid in the vapour state by means of an oxidizing or hydrolysing agent and recovered in aerogel form as particles of less than 150 millimicrons in diameter, and then extruding the masses to form filaments or films.  The metalloid or metal oxide may be stannic oxide, silicon dioxide, titanium dioxide, or an oxide of aluminium, zinc or zirconium, and it may be produced by thermal decomposition of a volatile chloride, e.g. stannic tetrachloride or silicon tetrachloride, in the vapour state in the presence of gases containing oxygen.  The proportion of oxide incorporated may be from 0.05-10 per cent by weight of the filament or film-forming substance.  When the filaments or films are to be made from aqueous spinning solutions, the aerogel oxide may be stirred with water, dilute aqueous caustic soda or ammonia before being added to the material to be extruded.  In the viscose process, the aerogel oxide may be mixed with the alkali cellulose in the xanthating drums.  In the production of cellulose acetate filaments, the oxide may be added to the acetone or other solvent which is used. In the production of filaments and films from purely synthetic substances, the oxide may be added before or during polymerization or condensation.  It may be added to a molten polymer mass to be extruded.  Dyes, coloured pigments such as carbon black, or matting pigments, may be incorporated together with the aerogel oxide.  The tensile strength, resistance to rubbing and resistance to splitting of the filaments and films, are improved by the addition of the aerogel oxide.  In an example, there is incorporated in a viscose spinning solution 0.3 per cent by weight (calculated on the cellulose) of a silicic acid aerogel, of particle diameter of 40 millimicrons, obtained by decomposition of silicon tetrachloride vapour, and the solution is then extruded to form filaments.  A similar proportion of silica aerogel is incorporated in a cellulose-ammoniacal copper oxide solution which is then extruded to form filaments.  In another example, an aqueous suspension of a titanium dioxide aerogel, of mean particle size of 80 millimicrons and produced by thermal decomposition of titanium tetrachloride in an atmosphere containing steam, is intimately mixed with a condensation product of adipic acid with hexamethylene diamine.  The mixture is melt spun to form polyamide filaments.  In another example, titanium dioxide aerogel of particle size in the range of 5-150 millimicrons is mixed with dimethyl formamide to form a suspension which is then mixed with a solution of polyacrylonitrile in dimethylformamide.  The solution is extruded to form filaments which contain about 0.5 per cent of titanium oxide.