Patent GB-498011-A (GB)
Title: Improvements in the manufacture and production of high quality siccatives
IPC: C09F9/00
Filed: 1937-06-29
Abstract: In the manufacture of driers from organic acids containing at least 7 carbon atoms, or water-soluble salts thereof, and salts, oxides or hydroxides of base metals capable of forming water-insoluble salts with the said acids, the driers also containing organic amine bases, the said amine bases are added to the driers at the end of the manufacture.  Specified amine bases are triethanolamine, trimethylene diamine, ethylene diamine, pyridine, quinoline, aniline, benzylaniline, dimethylaniline, diethylaniline, cyclohexylamine, diphenylamine and aminobenzyl alcohol, and an addition of 0,1-0,3 molecular proportion of the amine base to 2 molecular proportions of the organic acid employed, is generally sufficient.  A part of the amine base may be co-precipitated with the drier, and the remainder added, in free form, at the end of production.  According to examples: (1) naphthenic acid is neutralized with a solution or caustic soda, and a drier is precipitated by the addition of cobalt sulphate solution.  The precipitate is washed and dehydrated by fusion, and triethanolamine is added; (2) linoleic acid is saponified with caustic soda, and solutions of lead nitrate and of cobalt sulphate are then added.  After washing the precipitate, trimethylene diamine is added, and the whole dehydrated in vacuo; (3) colophony is dissolved in caustic soda solution, and benzylaniline added. The drier is then precipitated by the addition of a mixed solution of cobalt chloride and zinc sulphate.  After washing, further benzylaniline is added to the drier, which is then dehydrated; (4) naphthenic acid is dissolved in lacquer benzene, and the solution heated with calcined cobalt acetate.  Cyclohexylamine is added to the resulting cobalt naphthenate drier; (5) a carboxylic acid obtained by oxidizing paraffin wax is neutralized with caustic soda, and the solution precipitated with a mixed solution of cobalt sulphate, manganese sulphate and zinc sulphate.  The precipitate is washed, dehydrated by melting, and dimethylaniline is stirred in; (6) a mixture of wool grease fatty acid and naphthenic acid is heated with manganese acetate and cobaltous oxide.  After cooling, mineral spirit and benzylaniline are stirred in; (7) a mixture of iso-carboxylic acids prepared from primary alcohols of high molecular weight are neutralized with caustic potash.  Hydroxyethylamine and a solution of cobalt sulphate are then added.  The precipitate is washed, aminobenzyl alcohol is added, and the whole is dehydrated; (8) a mixture of semi-esters of phthalic acid, obtained by condensing phthalic anhydride with the mixture of alcohols formed during the synthesis of methanol, is neutralized with caustic soda.  This solution is weakly acidified with naphthenic acid and precipitated with a solution of copper sulphate.  After washing, diethylaniline and quinoline are added, and the mixture dehydrated; (9) a mixture of semiesters of phthalic acid, and iso-carboxylic acid obtained by oxidizing high molecular weight primary alcohols, and naphthenic acid, are heated with zinc oxide and hydrated cobaltous oxide. When the reaction is terminated, copal oil and diphenylamine are added; (10) naphthenic acid is neutralized with caustic potash, and aniline and a solution of aluminium sulphate are added.  The precipitate is washed, triethanolamine is added, and the mixture is dehydrated. Specification 370,550 is referred to.