Patent GB-744939-A (GB)
Title: Improvements in and relating to sulphamic acid derivatives
Inventor: LANTZ ROBERT LAZARE
Filed: 1953-07-29
Abstract: The invention comprises N4-phenyl-1,4-diaminobenzene-N1-sulphonic acid or its salts of metals of the second group of the periodic classification the atomic weights of which are less than that of strontium or its salts of nitrogen bases of formula <FORM:0744939/IV(a)/1> where R, R1 and R11 each represent H, or an alkyl, hydroxyalkyl, alkoxyalkyl or aminoalkyl radicle or R and R1 together form part of a heterocyclic ring.  The free acid is made by treating a solution of the sodium salt with an acid and the above salts are made by treating the free acid with the desired nitrogen base or an appropriate metal oxide or hydroxide or a salt of such a metal or the desired nitrogen base with a weak or volatile acid.  The sodium salt may be made by sulphonating. N4-phenyl-1,4-diamino-benzene with sulphur trioxide and a tertiary-amine and by treatment of the product thus obtained with a solution of caustic soda or sodium carbonate.  Alternatively the sodium salt may be prepared as in Specification 694,929.  The salts are used in the oxidation colouring of fibres and may be prepared in solutions and pastes used in such processes, particularly when the salt is of ammonia or another volatile base (see Group IV (c)). Specified metals are calcium and magnesium and specified nitrogen bases are ammonia, mono-, di- and tri-methyl-, -ethyl-and -ethanol-amines, diethylamino-ethanol, 1,2-diaminoethane, 1-amino-2-methoxyethane and morpholine.  In examples: (1) the free acid is obtained from a solution of sodium N4-phenyl-1,4 - diaminobenzene - N1 - sulphonate by th addition of hydrochloric acid, and the free acid is converted into its calcium and magnesium salts by treatment in (2) with calcium carbonate, and (3) with calcined magnesia and in (4) into its ammonium, mono- and dimethylamine, ethylamine and mono-ethanolamine salts by treatment with the necessary base.ALSO:Salts of N4-phenyl-1, 4-diaminobenzene-N1-sulphonic acid with metals of the second group of the periodic system of atomic weight less than that of strontium and of nitrogen bases of formula <FORM:0744939/IV(c)/1> where R, R1 and R11 are H, or an alkyl, hydoxyalkyl, alkoxyalkyl or aminoalkyl radicle or R and R1 together with N form heterocyclic ring are used in pastes and solutions for oxidation colouring dyeing and printing processes.  The paste or solution may be prepared by the addition of the appropriate base or metal salt to a paste or solution containing the materials required for oxidation colouring and the free acid. The latter method of preparation is particularly advantageous when ammonia or a volatile base is used.  Other methods of preparation of the salts and the free acid are described in Group IV(b).  Compounds such as calcium, magnesium and ammonium chlorates are preferred oxidation catalysts.  Calcium and magnesuim salts are specified together with salts of ammonia, mono-, di-, and tri-methyl, -ethyl- and -ethanolamines, diethylaminoethanol, 1, 2-diaminoethane, 1-amino-2-methoxyethane and morpholine.  Black shades are produced on cotton, mercerised cotton and viscose rayon when the materials are impregnated with pastes or solutions containing the sulphamates, dried, steamed and boiled in a soap solution containing sodium carbonate.  Examples are provided which illustrate the use in the dyeing or printing of the specified fabrics of the following salts of the sulphamic acid: calcium, magnesium, ammonium, mono-methyl- and -ethyl-amine and dimethylamine, specified constituents of the impregnating baths being 20 per cent ammonia solution, ammonium chloride and vanadates, calcium chloride, sodium, calcium and magnesium chlorates and a starch-tragacanth thickener.  Specification 694,929 [Group IV(b)] is referred to.