Patent GB-460147-A (GB)
Title: Improvements in the manufacture and production of colour lakes
IPC: C09B69/02
Filed: 1935-07-16
Abstract: A phthalocyanine sulphonic acid or a watersoluble salt thereof is caused to react in aqueous solution with an organic base to form a salt-like product in substance or on a cellulosic or other substratum.  The base may be an amine of the aliphatic, araliphatic, aromatic, hydroaromatic or heterocyclic series or a basic dyestuff. The products from weakly sulphonated phthalocyanines are, in general, lakes, and those from strongly sulphonated phthalocyanines are, in general, soluble in organic solvents and suitable for colouring lacquers and artificial resins of the phenol-formaldehyde, urea-formaldehyde and polyvalent alcohol-polybasic acid types. Specified cellulosic materials are cotton, viscose artificial silk, paper, cardboard and wood pulp and other specified substrata are alumina and barium sulphate.  In examples, (1) an aqueous solution of cyclohexylamine, slightly acidified with acetic acid, is added to an aqueous solution of the sodium salt of the dyestuff obtained by sulphonating with 5 times its weight of 40 per cent oleum for 1 hour at 70 DEG  C. the product obtained by heating phthalonitrile with cuprous chloride in pyridine; the precipitate is a brilliant blue-green lake; (2) dicyclohexylamine is added to an aqueous solution, acidified with acetic acid, of the sodium salt of the dyestuff obtained by sulphonating with six times its weight of 60 per cent oleum for 20 hours at 25 DEG  C. and 3 hours at 60 DEG  C. the product obtained by heating phthalonitrile with cuprous chloride in pyridine; the precipitate is suitable for colouring varnish lacquers greenish blue fast to light; (3) a slightly acidified aqueous solution of the amine mixture obtained by the action of ammonia on the product of reduction of palm kernel oil fatty acids is added to an aqueous solution of the sodium salt in (2) to precipitate a blue-green pigment; (4) an aqueous solution of barium chloride and a slightly acidified solution of dodecylamine are added to an aqueous solution of the sodium salt in (2) to precipitate a lake; (5) an aqueous solution of Rhodulin blue 6G is added to an aqueous solution of the sodium salt of the dyestuff obtained by sulphonating with 5 times its weight of 30 per cent oleum for 1 hour at 80 DEG  C. the product obtained by heating phthalonitrile with cuprous chloride in pyridine; the precipitate may be incorporated with a substratum prepared by adding aluminium sulphate and sodium carbonate solutions to an aqueous suspension of heavy spar and the product used for printing wallpaper; (6) an aqueous solution of the dyestuff obtained by sulphonating with 10 times its weight of p  fuming sulphuric acid (30 per cent SO3) for 1 hour at 50 DEG  C. the product obtained by heating phthalonitrile with cobaltous chloride in pyridine is added to a substratum prepared by mixing solutions of aluminium sulphate, sodium carbonate and barium chloride, and the whole is stirred with an aqueous solution of Methylene blue BB to obtain a deep blue lake; (7) an aqueous solution of the nickel-containing dyestuff corresponding to the cobalt-containing dyestuff in (6) is added to a substratum prepared by mixing solutions of aluminium sulphate and sodium carbonate and the product is treated with an aqueous solution of Rhoduline blue 5B to obtain a blue lake suitable for incorporation in a linseed oil varnish; (8) an aqueous solution of Brilliant green is added to a substratum prepared as in (7) and a lake is obtained by adding thereto a solution of a metal-free sulphonated phthalocyanine; (9) aqueous solutions of a sulphonated copper phthalocyanine and of Auramine are added to a substratum prepared as in (8) and precipitation is completed by adding barium chloride solution; (10) an aqueous solution of the sodium salt of the dyestuff obtained by sulphonating copper phthalocyanine with 60 per cent oleum for 20 hours at 25 DEG  C. and 5 hours at 50 DEG  C. is mixed with an aqueous solution of Brilliamt green or Auramine G; the precipitates obtained are suitable for colouring nitrocellulose lacquers or artificial resins; (11) a dyeing fast to light is obtained upon cotton or viscose artificial silk by treating it for 1 hour in a boiling bath containing Glauber salt, sodium carbonate and a copper phthalocyanine sulphonic acid, rinsing and treating in a second bath containing Methylene blue BB; (12) dodecyldimethylamine is added to an aqueous solution of the sodium salt of the dyestuff obtained by sulphonating copper phthalocyanine with 40 per cent oleum for 20 hours at room temperature and 2 hours at 90 DEG  C.; the precipitate is suitable for colouring nitro-cellulose lacquers; (13) dicyclohexylamine is added to an aqueous solution of the sodium salt of the dyestuff obtained by sulphonating zinc phthalocyanine with 30 per cent oleum for 20 hours at room temperature and 4 hours at 50 DEG C.; the precipitate is suitable for colouring nitro-cellulose lacquers or artificial resins.