Patent GB-748261-A (GB)
Title: Improvements in and relating to the alcoholysis of ester waxes
IPC: C11C3/04
Filed: 1951-03-29
Abstract: The ester waxes sperm oil, wool wax, recovered wool grease or mixtures thereof are reacted with pentaerythritol in the presence of a free fatty acid or free monohydroxy fatty acid which contains more than 10 carbon atoms in the molecule and may be saturated or unsaturated or in the presence of free wool grease fatty acid or mixtures of two or more such acids, the molecular proportions of pentaerythritol and the ester wax plus fatty acid being in the ratio 1:3, at 400-600 DEG  F. under reflux conditions which allow any steam formed to escape, but which condense and return to the reaction mixture any reactants volatile at the reaction temperature, it being optional whether or not a catalyst is employed.  The free fatty acid may be added to the sperm oil or wool wax or may already be a natural constituent of a commercial grade thereof, e.g. recovered wool grease, the proportion of free fatty acid being not less than 2 per cent by weight of the sperm oil, wool wax or wool grease.  The free fatty acid may be lauric, palmitic, oleic, erucic, stearic, linoleic, or ricinoleic.  The wool grease acid which may be used may occur free or combined in wool grease or may be obtained therefrom by dry or steam distillation or by saponifying the wool grease with a caustic alkali followed by liberation of the free wool grease acids from the soaps thereby formed by acidification with a mineral acid.  A current of dry carbon dioxide or nitrogen may be passed through the mixture during the reaction, which is preferably carried out at sub-atmospheric pressures and may be completed in 8-12 hours. In an example three molecular equivalents of a commercial sperm oil containing about 2 per cent of free fatty acid are heated with one of pentaerythritol with continuous stirring at 400-600 DEG  F. for 8-12 hours under a water-cooled reflux condenser, a current of carbon dioxide being bubbled through the reaction mixture.  The product consists chiefly of a mixture of the sperm oil fatty acids triester of pentaerythritol and sperm oil monohydric alcohols, with minor proportions of tetraesters and mono- and di-esters and some of the initial reactants.  In other examples pentaerythritol is similarly reacted with sperm oil and oleic acid, wool wax alone and mixed with oleic acid, sperm oil mixed with wool grease acids, and wool grease mixed with added wool grease acids, respectively. The products may be used in the preparation of cutting and machinery lubricating oils, oils for lubricating and softening textile fibres and for the manufacture of cosmetic creams.ALSO:Sperm oil, wool wax, recovered wool grease or mixtures thereof are reacted with pentaerythritol in the presence of a free fatty acid or free monohydroxy fatty acid which contains more than 10 carbon atoms in the molecule and may be saturated or unsaturated, or in the presence of free wool grease fatty acid or mixtures of two or more such acids, the molecular proportions of pentaerythritol and the ester wax plus fatty acid being in the ratio 1:3, at 400-600 DEG F. under reflux conditions which allow any steam formed to escape, but which condense and return to the reaction mixture any reactants volatile at the reaction temperature, it being optional whether or not a catalyst is employed. The free fatty acid may be added to the sperm oil or wool wax or may already be a natural constituent of a commercial grade thereof, e.g. recovered wool grease, the proportion of free fatty acid being not less than 2 per cent by weight of the sperm oil, wool wax or wool grease.  The free fatty acid may be lauric, palmitic, oleic, erucic, stearic, linoleic or ricinoleic.  The wool grease acid which may be used may occur free or combined in wool grease or may be obtained therefrom by dry or steam distillation or by saponifying the wool grease with a caustic alkali followed by liberation of the free wool grease acids from the soaps thereby formed by acidification with a mineral acid.  A current of dry carbon dioxide may be passed through the mixture during the reaction, which is preferably carried out at sub-atmospheric pressures and may be completed in 8-12 hours.  In an example three molecular equivalents of a commercial sperm oil containing about 2 per cent of free fatty acid are heated with one of pentaerythritol with continuous stirring at 400 DEG -600 DEG F. for 8-12 hours under a water-cooled reflux condenser, a current of carbon dioxide being bubbled through the reaction mixture.  The product consists chiefly of a mixture of the sperm oil fatty acids triester of pentaerythritol and sperm oil monohydric alcohols, with minor proportions of tetraesters and mono- and di-esters and some of the initial reactants.  In other examples pentaerythritol is similarly reacted with sperm oil and oleic acid, wool wax alone and mixed with oleic acid, sperm oil mixed with wool grease acids, and wool grease mixed with added wool grease acids respectively.  The products may be used in the preparation of cutting and machinery lubricating oils, oils for lubricating and softening textile fibres and for the manufacture of cosmetic creams.