Patent GB-786103-A (GB)
Title: Improvements in or relating to low temperature methods for preparing high melting point greases
Filed: 1955-06-27
Abstract: A lubricating grease is prepared by forming a blend consisting essentially of a lubricating oil, an organic acid whose metal salts are thickening agents, sufficient of an oxide or hydroxide of a metal of Group I, II, III or IV of the Periodic Table for substantial neutralization of the organic acid, and alcohol or water as solvent for the oxide or hydroxide, heating the blend to a temperature below that sufficient for substantial saponification of the acid, and subjecting the blend to a shearing force sufficient to form a salt by saponification of the acid and to produce a stable dispersion of the salt in the oil.  Instead of the free organic acid, an ester thereof may be employed.  Suitable lubricating oils are mineral oil, oils derived from coal, alkylene polymers, alkylene oxide polymers and their esters and ethers, esters of dicarboxylic acids (particularly dibutyl or dihexyl adipates, di-2-ethylhexyl sebacate or di-n-hexyl fumarate polymer), alkyl benzenes, organic silicates, polysiloxanes and liquid esters of phosphorus acids.  Organic acids, whose metal salts are suitable thickening agents, include terephthalic acid, N-alkyl terephthalamic acids, N-alkyl isophthalamic acids, polyamic acids and fatty acids such as oleic, stearic and hydroxystearic acids.  Esters, which may be employed instead of the free organic acid, include alkyl esters of terephthalic acid or of N-alkyl terephthalamic acids.  Metals, whose oxide or hydroxide may be employed, include lithium sodium, potassium, calcium, barium, strontium, magnesium, zinc, cadmium, aluminium and lead.  The alcoholic solvent may be methanol, ethanol or glycerol.  The shearing may be effected with a Manton-Gaulin homogenizer, an Eppenbach colloid mill, a Cornell homogenizer or a high-speed gear pump.  In the examples, lubricating greases are prepared by (1) mixing mineral lubricating oil, methyl ester of N-alkyl terephthalamic acid (the alkyl being predominantly octadecyl, hexadecyl and octadecenyl also being present), barium oxide monohydrate or calcium hydroxide, and water, heating the mixture to about 200 DEG  F., cooling to 130 DEG F. and then shearing in a Manton-Gaulin homogenizer, or (2) mixing mineral lubricating oil, 12-hydroxy-stearic acid, lithium hydroxide monohydrate and water, heating the mixture to 180 DEG  F., cooling to 125 DEG  F. and then shearing in a Manton-Gaulin homogenizer.  The effect of temperature on the resultant grease is also described with respect to the preparation of a lubricating grease by mixing mineral lubricating oil, methyl ester of N-alkyl terephthalamic acid, sodium hydroxide and water, heating the mixture and then shearing in a Manton-Gaulin homogenizer.ALSO:Methyl esters of N-alkyl terephthalamic acids are used as starting materials for the preparation of thickening agents for lubricating oils (see Group III).  The methyl esters are prepared by first saponifying dimethyl terephthalate with potassium hydroxide to produce the potassium salt of monomethyl terephthalate.  This is hydrolysed with sulphuric acid to yield the monomethyl terephthalate, which is reacted with thionyl chloride to produce the corrsponding acid chloride.  The acid chloride is mixed with triethylamine and a commercial mixture of primary aliphatic amines (25 per cent hexadecylamine, 70 per cent octadecylamine and 5 per cent octadecenylamine) and the resulting product heated.  On addition of water, the methyl esters of N-alkyl terephthalamic acids are precipitated.