Patent GB-1067666-A (GB)
Title: Fine particle production
IPC: C09D7/65
Filed: 1963-10-24
Abstract: A finely divided resinous pigment is prepared by mixing an incompletely condensed substantially water-insoluble reaction product of an aldehyde and a polyamino compound forming a resin therewith, with a liquid vehicle that is substantially insoluble in said reaction product, then subjecting the mixture to violent agitation and heating so that the condensation is advanced to effect the formation of a uniform finely divided solid dispersed phase, then cooling the mixture while retaining the dispersed phase, the continuous phase being liquid throughout and a colouring agent being added at any stage of the process.  The agitation may be effected by mechanical stirring, homogenization, kinetic dispersion or by ultrasonic means.  The initial softening point (s.p.) of the resin may be, e.g., 50-60 DEG  C., and this should be raised by, e.g., 20-50 DEG  C. to, e.g., 70 DEG  C., preferably at least 100 DEG  C. The initial s.p. may be lowered by addition of at least 5 wt. per cent of a solvent for the resin which is not soluble in the vehicle (e.g. DMF).  Preferred resins are cocondensates of a polyamino compound with formaldehyde and an aromatic sulphonamide.  Suitable polyamino compounds for this purpose include urea, thiourea, guanidine, dicyandiamide and biuret. Normally preferred polyamino compounds are heterocyclic rings substituted by NH2 groups, e.g. polyamino-triazines, -triazoles, -diazines and -diazoles, including guanazole and 1-phenyl-, 4-amino-, 1-carbamyl-, 1-guanyl-, 1-acetyl- and 1-benzoyl-guanazoles, 2: 4-diamino-6-hydroxypyrimidine, melamine, and the guanamines; others are cyclic ureides, e.g. dimethyl hydantoin.  Suitable sulphonamides are benzene and o- and p-toluene-sulphonamides.  The sulphonamide cocondensate should preferably be prepared from x moles of sulphonamide, y moles of polyamino compound and from x to x+3y moles of formaldehyde; where x>3y the product will be thermoplastic, below this value the nature of the product depends on the other reaction conditions. The continuous phase is preferably a liquid vehicle capable of forming a clear solid film, and should contain at least 40 wt. per cent of solids, preferably benzenoid compounds, e.g. oil-modified alkyd resins, styrenated alkyd resins and cyclized rubber vehicles, together with petroleum solvents, drying oils, and/or other liquid solvents.  In examples aqueous dispersions are prepared of condensates from para-formaldehyde and melamine or benzoguanamine (in Examples 17-19 and 59 and 8-10A of Example 53) with and without toluensulphonamide, and these are agitated and heated in ink vehicles comprising styrenated or oil alkyd resins and/or linseed or tung oil and optionally a phenolic resin (Example 25) or vinyl resin and, usually, a hydrocarbon solvent. In Examples 51 and 58 the resin is derived from hydantoin and toluenesulphonamide or melamine, and in Examples 27-29 from melamine, toluenesulphonamide and ethylene urea, and in run 7A of Example 53 from melamine and urea.  Colorants are introduced before, during or after the dispersion; those used include Rhodamine B Extra, Rhodamine 6GDN, and Brilliant Yellow 6G, and in Examples 42-47 various other dyes, in Example 55 TiO2. Other additives used include U.V. absorbers (Examples 14 and 41) and dimethylformamide as plasticizer (Example 49).