Patent GB-907558-A (GB)
Title: Improved process for the production of organometallic complexes
Inventor: BISHOP ROY REGINALD
IPC: C07F7/00
Filed: 1958-04-02
Abstract: Paints and varnishes having a drying oil basis comprise, as a drier, an organometallic complex prepared from a non-resinous reaction product, having no oxidative drying properties and prepared by heating a tri- or tetra-valent metal alkoxide with a b -keto carboxylic ester or a malonic ester in such proportions that the said product contains unreacted alkoxy groups, by condensing the nonresinous product by reaction with an amount of water not substantially in excess of one mole per 2 equivalents of unreacted alkoxy groups to eliminate alkanol (see Group IV(b)). The products may be derived from aluminium, titanium or iron (III) isopropoxides and/or butoxides and methyl, ethyl or butyl aceto acetate or diethyl malonate.ALSO:Paints and varnishes containing alkyd resins comprise, as a drier, in amount sufficient to provide 0,2-1,5% metal based on solids, an organo-metallic complex prepared from a non-resinous reaction product, having no oxidative drying properties and prepared by heating an alkoxide of a tri- or tetra-valent metal with a b -keto carboxylic ester or a malonic ester in such proportions that the said product contains unreacted alkoxy groups, by condensing the non-resinous product by reaction with an amount of water not substantially in excess of one mole for each two equivalents of unreacted alkoxy groups to eliminate alkanol (see Group IV(b)).  The complexes may be used in drying oil as modified alkyd resins may contain conventional driers such as manganese or cobalt naphthenate. Examples describe complexes obtained as above from (1) ethyl aceto acetate and aluminium isopropoxide or butyl titanate and (2) diethyl malonate and aluminium isopropoxide, which are incorporated to give 0,5% metal content in a 69% oil length pentaerythritol glycerol alkyd base containing manganese naphthenate (0,04% metal), yielding a quick drying paint.  Analogous complexes containing ferric iron are mentioned.ALSO:Organo metallic complexes are prepared from non-resinous reaction products, having no oxidative drying properties and prepared by heating an alkoxide of a metal which is tri- or tetra-valent with a b -keto carboxylic acid ester or a malonic acid ester in such proportions that the said product contains unreacted alkoxy groups, by condensing the nonresinous product by reaction with an amount of water not substantially in excess of one mole of water for each two equivalents of unreacted alkoxy groups, to eliminate alkanol.  It is believed that the condensation involves water reacting with an alkoxy group in each of two moles of non-resinous reaction product with elimination of alkanol and the joining of the two residues of reaction product by an oxygen linkage.  Preferably, all the alkoxy groups present are so reacted.  The water, which may be diluted with water-miscible inert organic solvent is preferably added gradually.  The non-resinous starting materials preferably contain 1 or 2 alkoxy groups and may be prepared from the propoxides, butoxides and mixed propoxides/butoxides of aluminium, titanium and ferric iron and methyl, ethyl or butyl aceto acetate or diethyl malonate.  The condensation products may be used in paints and varnishes (see Group III).  In Examples: (1) -(2) ethyl aceto acetate is reacted with aluminium isopropoxide at 90 DEG -100 DEG C. yielding products containing 1-1 2/3 alkoxy groups per mole and aqueous ethanol is added and the mixture distilled to remove the alcohols; (3) butyl titanate and ethyl aceto acetate and (4) diethyl malonate and aluminium isopropoxide are similarly reacted yielding products averaging one alkoxy group per mole, which products are condensed as above with aqueous ethanol.