Patent GB-666299-A (GB)
Title: Manufacture of resin solutions suitable for making lacquers, and prepared from resinous ethylene oxide derivative of phenols
IPC: C08L61/10
Filed: 1949-07-05
Abstract: Ethylene oxide type resins suitable as constituents of lacquers are obtained by reacting 1 mol. of a resinous polyhydricphenol derivative containing at least two ethylene oxide groups with 1/8 -\ba6/5 of one equivalent of a polybasic carboxylic acid, of which the carboxyl groups are separated by at least 2 C atoms, and 0.06-0.6 mols. dicyandiamide, the reaction being carried out by heating the mixture in an organic solvent containing no free carboxyl groups and boiling above 100 DEG  C.  There may also be added an aldehyde condensation product of melamine, urea, dicyandiamide or phenol which contains etherified methylol groups, together with a further quantity of dicyandiamide.  The polycarboxylic acids may be used in the form of their anhydrides.  The preferred ethylene oxide-polyhydric phenol resins-are those obtained by reacting epi- or di-halogen hydrins with polyhydric polynuclear phenols specifically that obtained by reacting 4 : 41-dioxydiphenyl-dimethyl-methane with 1.65 mols. of epichlorhydrin in an aqueous solution of NaOH at 50-100 DEG  C. This resin is referred to in the Specification as "dimethylmethane" resin. Polybasic carboxylic acids specified are adipic, succinic, sebacic, maleic, citric, phthalic or their anhydrides.  Aldehyde condensation products containing etherified groups are alkyl ethers of methylol melamines, ureas, dicyandiamide or phenols, which may be formed in situ from their components in the course of the reaction.  Solvents specified are alcohols, ketones, chlorinated hydrocarbons, phenols, esters, ethers and glycols, particularly mixtures thereof.  In examples: (1) 300 parts dimethyl methane resins are dissolved in 133 parts cyclohexanone and the clear solution is mixed with 73 parts adipic acid and 42 parts dicyandiamide, the temperature being maintained at 120-130 DEG  C.  The resulting viscous resin is dissolved in a mixture of benzyl alcohol and o-dichlorobenzene. On dilution with usual solvents a lacquer is obtained which can be applied in several layers to copper wire, each of which layers may be individually hardened; (3) coating compositions of similar properties to those in Example 1 are obtained, employing an epoxide resin which is obtained by reacting 846 parts phenol and 540 parts formaldehyde at raised temperatures in presence of sulphuric acid as catalyst and reacting the condensate with 1656 parts epichlorhydrin; (4) a viscous resin obtained as in (1) is further reacted with dicyandiamide and a solution of hexamethylol-melamine butyl ether in butanol and benzyl alcohol; (6) the dimethylmethane resin and dicyandiamide are reacted with phthalic acid and the product further reacted with dicyandiamide and hexamethylol melamine; (8) a resin obtained by reaction of 2 mols. epichlorhydrin with 1 mol. o,o1-diphenol in alkaline solutions is reacted with sebacic acid and dicyandiamide and the product further reacted with dicyandiamide and dimethylol urea butyl ether in butanol, benzyl alcohol and glycol monoethyl ether; (9) the resin employed is that obtained by reacting resorcinol and epichlorhydrin. Samples have been furnished under Sect. 2 (5) of lacquer solutions obtained (1) by reacting dimethylmethane resin dissolved in cyclohexanol with adipic acid and dicyandiamide, dissolving the product in benzyl alcohol o-dichlorbenzene and monochlorbenzene, adding dicyandiamide, benzyl alcohol, hexamethylolmelamine and lactic acid, and heating the mixture at 110 DEG  C. until the hexamethylolmelamine is etherified; (2) by reacting the dimethylmethane resin-adipic acid-dicyandiamide condensate with an ether of a formaldehyde - cresol - phenol condensate obtained from 48 parts cresol, 21 parts phenol, 70 parts 30 per cent formaldehyde, 4 parts conc ammonia and 120 parts ethylene glycol monoethyl ether containing 1 part oxalic acid. Specification 636,696 is referred to.