公开(公告)号：GB697461A

公开(公告)日：1953-09-23

申请号：GB1604150

申请日：1950-06-27

Applicant: STANDARD OIL DEV CO

Inventor： RAE NORMAN SIDNEY ,  DAVIES ROY TREVOR

Abstract: In the preparation of lubricating oil additives, by the reaction of a barium, calcium, strontium, magnesium or zinc, mono- or poly-alkyl phenate with elemental sulphur, the reaction product is freed from unreacted alkyl phenols and other volatile matter by steam distillation below the decomposition temperature of the product, preferably at 120-180 DEG C., e.g. at 135-160 DEG C. In preferred modifications a mono-alkyl phenol, preferably a p-alkyl phenol, is reacted with an alkaline earth metal oxide, hydroxide or hydrated oxide in an inert diluent, non-volatile in steam, such as a lubricating oil and in the presence of a minor proportion of a C8-C20 saturated aliphatic alcohol, such as cetyl or stearyl alcohol; sulphur is added in an amount exceeding 2 1/2 times the amount required in the finished product and when sulphurization is complete the mixture is steam distilled at 120-180 DEG C., preferably at 135-160 DEG C, until the residual alkyl phenol is substantially all removed or is below the solubility limit in the mixture at O DEG C., the reaction product being blown with carbon dioxide either before during or after steam distillation. A preferred product is a sulphurized barium alkyl phenol containing between 3 and 4 per cent of sulphur and between 7 and 10 per cent of barium. In an example, p-tert-octyl phenol is dissolved in a mineral lubricating oil together with a minor proportion of mixed cetyl/stearyl alcohol and the mixture is blown with nitrogen and mixed with barium oxide at 350-390 DEG F., followed by the addition of sulphur at 300-350 DEG F., carbon dioxide is then blown in and the mixture is steam distilled at 250-350 DEG F. to remove volatile matter. Specifications 586,841, 599,729 and 600,825 are referred to.ALSO:A lubricating composition comprises a lubricating oil, preferably a mineral lubricating oil, and a minor proportion of an additive obtained by reacting a barium, calcium, strontium, magnesium or zinc, mono- or polyalkyl phenate such as barium p-iso octyl phenate with sulphur and removing free alkyl phenols or other volatile matter by steam distillation, (see Group IV(b)). Preferably the composition comprises a mineral oil and up to 15 per cent, suitably between 0.5 and 6 per cent, e.g. 2-3 per cent of the additive. The sulphurization reaction is conveniently carried out using mineral oil as an inert solvent and in the presence of a C8-C20 aliphatic alcohol such as cetyl or stearyl alcohol, in which case the additive is obtained as a concentrate in solution in mineral oil. An example describes the preparation of a concentrate containing 40 per cent of the additive derived from barium p-tertiary octyl phenate and sulphur in mineral oil. Specifications 586,841, 599,729 and 600,825 are referred to.

公开(公告)号：GB727655A

公开(公告)日：1955-04-06

申请号：GB2060951

申请日：1951-08-31

Applicant: STANDARD OIL DEV CO

Inventor： DAVIES ROY TREVOR ,  HANSON THOMAS KENNETH ,  RAE NORMAN SIDNEY

IPC: C10M169/00

Abstract: A solution of a divalent metal alkyl phenate or thiophenate in an inert solvent is reacted with elemental sulphur to give a complex reaction product as a concentrate in the inert solvent, and a proportion of a metal, ammonium or organic base salt of a petroleum mahogany acid is added to the concentrate. The final concentrate is useful as a detergent additive for lubricating oils and, as a result of the presence of the mahogany sulphonate, shows no tendency to deposit crystals on standing; in the absence of the mahogany sulphonate there is a tendency for the deposition of crystals of alkyl phenol or thiophenol, which is probably partially regenerated during the sulphurization reaction. The inert solvent may be lubricating oil and may contain a C8-C20 saturated aliphatic alcohol such as cetyl or stearyl alcohol to reduce foaming during the sulphurization reaction and to act as solubilizer of the sulphurized product. The divalent metal alkyl phenate or thiophenate may be an alkaline earth metal salt which may be a basic salt; similarly, the mahogany sulphonate may be an alkaline earth metal salt which may be a basic salt. The magnesium salts of both the alkyl phenol or thiophenol and the mahogany acid are also mentioned. The sulphurized product may be blown with carbon dioxide before or after the addition of the mahogany sulphonate. In an example, barium p-tert. octyl phenate, in mineral lubricating oil solution containing a mixture of cetyl and stearyl alcohols, is sulphurized and calcium mahogany sulphonate is then added. Specifications 586,841, 599,729 and 600,825 are referred to.

公开(公告)号：GB709903A

公开(公告)日：1954-06-02

申请号：GB864250

申请日：1950-04-06

Applicant: STANDARD OIL DEV CO

Inventor： PRIZEMAN ALLAN ,  RAE NORMAN SIDNEY ,  BURGESS BRUCE HENRY

IPC: C10M129/76

Abstract: A lubricating composition comprises a hydrocarbon lubricating oil, less than 1 per cent. by weight of an oil-soluble aliphatic partial ester of a polyhydric alcohol, and 1-5 per cent. of a detergent which is an alkaline earth metal derivative of an alkyl phenol sulphide or of a sulphurised alkylated phenol. The partial esters may be prepared from alkylene glycols on polycylcols such as ethylene glycol and glycerol, from pentaerythritol and from hexitols or partially dehydrated hexitols such as sorbitan, and higher fatty acids such as palmitic, stearic, oleic and linoleic acids; pentaerythritol mono-oleate and sorbitan mono-oleate are referred to. The detergent may be the barium salt of p-isooctyl phenol sulphide or the product obtained by heating barium isooctylphenate with sulphur. Optional additives are calcium or barium mahogany sulphonates, aliphatic-aromatic condensation products such as chlorinated, wax-napthalene condensation products, polymers and copolymers of unsaturated esters, for example polyalkyl-methacrylates, sulphurized fatty oils, sulphurized terpenes, sulphurized olefins, esters such as isopropyl oleate and aryl phosphates such as tricresyl phosphate. The Provisional Specification refers to a composition of a hydrocarbon lubricating oil, less than 1 per cent. of a partial ester of a polyhydric alcohol and optionally a detergent additive.