Patent GB-865970-A (GB)
Title: Organic molybdenum blue derivatives and mineral lubricating oils containing them
IPC: C07F11/00
Filed: 1957-07-02
Abstract: The invention comprises organic sulphurmolybdenum blue compounds obtainable by interaction of an olefinically unsaturated alcohol or an organic nitrogenous base, each having a hydrocarbon radical containing 8-20 carbon atoms, with sulphur and then with molybdenum. The compounds, which are lubricant additives (see Group III), are preferably prepared by reacting the alcohol or organic nitrogenous base with approximately equimolar amounts of sulphur at an elevated temperature and then reacting the product, preferably in molar excess with molybdenum blue.  There are also described as components of a lubricating oil composition organic molybdenum blue compounds prepared by reacting the above-defined alcohols or nitrogenous bases with molybdenum blue in isobutanol solution, distilling off the butanol on a water-bath followed by heating of the residue.  The sulphur-containing additives may be rendered resistant to thermal decomposition by addition of a fatty acid containing at least 12 carbon atoms, or a reaction product thereof with an organic nitrogenous base such as oleic acid or its reaction product with 1-hydroxy ethyl-2-heptadecenyl glyoxalidine. In Examples: (1) the above-mentioned glyoxalidine is heated with elementary sulphur at 130-150 DEG C., the sulphurised base is dissolved in an isobutanolic solution of molybdenum blue and the mixture heated to remove the alcohol leaving an organic sulphur molybdenum blue as residue; (2) various sulphur-free organic molybdenum blues are prepared by adding hexadecenol, oleylamine, dehydroabietylamine and 1-hydroxyethyl-2-heptadecenyl glyoxalidine to separate solutions of molybdenum blue in isobutanol, each mixture then being stripped of alcohol under reduced pressure and further heated.  Other specified unsaturated alcohols and nitrogenous bases are tetradecenol, octadecenol, octylamine, 1-hydroxyethyl-2-heptadecyl glyoxalidine, the reaction products of ethylene oxide with an amine such as actodecyclamine, and nitrogenous bases generally which are obtainable by condensing amino alcohols with higher fatty acids.ALSO:Mineral lubricating oil compositions comprise about 0.5 to 5% by weight of an organic sulphur-containing molybdenum blue compound obtainable by interaction of sulphur with an olefinically unsaturated alcohol or an organic nitrogenous base, each having a hydrocarbon radical containing 8-20 carbon atoms, and then with molybdenum blue.  In a modification, the composition comprises about 0.5-5% by weight of a sulphur-free reaction product of molybdenum blue with an alcohol or nitrogenous base as defined above, and in addition elementary sulphur or an oil-soluble organic sulphur compound which liberates sulphur at the temperature created by lubricating friction.  The compositions may also contain, as oil-solubilisers, alcohols containing 8-20 carbon atoms.  The first-mentioned compositions may contain fatty acids containing at least 12 carbon atoms, or reaction products thereof with organic nitrogenous bases, to render the molybdenum blue additives heat-resistant.  Examples describe mineral oil compositions containing (1) an organic sulphurcontaining molybdenum blue, obtained by sulphurising 1 - hydroxyethyl - 2 - heptadecenyl glyoxalidine and reacting the product with molybdenum blue, and oil-solubilising alcohols containing 14-18 carbon atoms and also optionally oleic acid or its reaction product with the above-named glyoxalidine; or (2) sulphur or dibenzyl disulphide and a sulphur-free organic molybdenum blue prepared from hexadecenol, dehydroabietylamine, oleylamine or the above-named glyoxalidine.  The additives have extreme-pressure properties.  The additives may also be derived from tetradecenol, octadecenol, octylamine, 1-hydroxyethyl-2-heptadecyl glyoxalidine, reaction products of ethylene oxide with octadecylamine and like amines, and nitrogenous bases generally which are obtainable by condensing amino-alcohols with higher fatty acids.  Molybdenum blue is prepared by reacting metallic molybdenum with a solution of MoO3 in aqueous sulphuric acid and extracting the resulting molybdenum blue with isobutanol.