Patent GB-757821-A (GB)
Title: Improvements in or relating to the treatment of polychloro copper phthalocyanine
IPC: C09B67/00
Filed: 1954-04-20
Abstract: The invention comprises a polychloro copper phthalocyanine in pigmentary form containing at least 46 per cent chlorine and consisting predominantly of parallelopiped shaped particles of 0.5 to 0.2 micron length, said length being 2 to 3 times the width and 5 to 10 times the thickness, and exhibiting a bright, yellow-green hue when tested in lithographic ink drawdowns, and also a polychloro copper phthalocyanine having the same chlorine content and particle dimensions and giving an X-ray diffraction pattern distinguished by the following features; (a) the pattern has its tallest peak at Bragg angle 26.7 degrees; (b) the pattern has peaks at Bragg angles 28.5 degrees and 6.1 degrees; (c) the height of the peak at 28.5 DEG  is from 1.8 to 40 per cent of said tallest peak; (d) the horizontal width of the peak at 6.1 degrees at its half-height is less than 0.5 degrees, all heights being measured from a base line drawn to exclude the background scattering of the X-ray beam recorded by the apparatus, and the X-ray diffraction pattern being recorded by the aid of copper Ka  radiation using 1 degrees divergence slits and a 0.003 inch receiving slit at a distance of 170 mm. from the specimen. The invention also includes the manufacture of such polychloro copper phthalocyanines by treating an anhydrous intimate mixture of the crude polychloro copper phthalocyanine and at least 30 per cent by weight of aluminium chloride or bromide, or ferric chloride or bromide, with water an inert, water-immiscible, organic liquid, the amount of water being sufficient to dissolve the solube metal salt and the amount of organic liquid being at least 30 per cent by weight based on the weight of pigment, and then separating the insoluble pigment from the solution, and recovering the pigment in paste or dry form.  The water and organic liquid may be added in either order or simultaneously.  Water may be removed from the aqueous paste obtained by heating above 100 DEG C. in an organic liquid, and organic liquid may be removed, e.g. by filtration and washing with a water - miscible solvent, e.g. alcohol, or by steam distillation, which may be in presence of alkali, an oxidizing agent such as sodium chromate or sodium nitrite, or of a fat, soap, long chain fatty acid or ester, or long chain aliphatic alcohol or ester thereof.  The organic liquid may be a benzenoid hydrocarbon, or halogen or nitro derivative thereof, e.g. o - dichlorbenzene, chlorbenzene, trichlorbenzene, parachlortoluene, or o - nitrotoluene.  The initial anhydrous mixture used may be the crude mass obtained by chlorinating copper phthalocyanine in an aluminium chloride - sodium chloride melt or by contacting the already polychlorinated copper phthalocyanine with aluminium chloride or bromide of ferric chloride or bromide under anhydrous conditions.  Examples are given using the organic liquids specified above, and polychloro bodies prepared by chlorination of copper phthalocyanine in an aluminium chloride - sodium chloride melt, or by the fluidized - bed chlorination process of U.S.A. Specification 2,586,598, or by the sulphur dichloride process of U.S.A.  Specification 2,377,685.