| Carboxylated detergent- disperant additive for lubricating oils -> Monitor Keywords |
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  Carboxylated detergent- disperant additive for lubricating oilsRelated Patent Categories: Solid Anti-friction Devices, Materials Therefor, Lubricant Or Separant Compositions For Moving Solid Surfaces, And Miscellaneous Mineral Oil Compositions, Lubricants Or Separants For Moving Solid Surfaces And Miscellaneous Mineral Oil Compositions (e.g., Water Containing, Etc.), Organic -c(=o)o- Compound, Overbased Or Carbonated CarboxylatesThe Patent Description & Claims data below is from USPTO Patent Application 20070105730. Brief Patent Description - Full Patent Description - Patent Application Claims
FIELD OF THE INVENTION [0001] The present invention relates to a novel unsulfurized, carboxylate-containing additive for lubricating oils, comprising a mixture of alkaline earth metal salts (hydrocarbyl phenate/hydrocarbyl salicylate) and a reduced amount of unreacted hydrocarbyl phenols, as well as additive packages, concentrates and finished oil compositions comprising the same. Specifically, it relates to additives comprising said mixture in which said hydrocarbyl salicylate is primarily single-aromatic-ring hydrocarbyl salicylate. This additive improves antioxidant properties, high temperature deposit control, BN retention, corrosion control and black sludge control in lubricating oils. This invention is also directed, in part, to methods of preparing and using said novel additive. BACKGROUND OF THE INVENTION [0002] The preparation of hydrocarbyl phenates and hydrocarbyl salicylates is well known in the art. [0003] U.S. Pat. No. 3,036,971 discloses preparing detergent dispersant additives based on sulfurized alkylphenates of high basicity alkaline earth metals. These additives are prepared by sulfurization of an alkylphenol, neutralization of the sulfurized alkylphenol with an alkaline earth metal base, then super-alkalization by carbonation of the alkaline earth metal base dispersed in the sulfurized alkylphenate. [0004] French patent 1,563,557 discloses detergent additives based on sulfurized calcium alkylsalicylates. These additives are prepared by carboxylation of a potassium alkylphenate, exchange with calcium chloride, then sulfurization of the calcium alkylsalicylate obtained with sulfur in the presence of lime, a [0005] French patent application 2,625,220 discloses superalkalized detergent-dispersant additives based on alkylphenates and alkylsalicylates. These additives are prepared by neutralization of an alkylphenol with an alkaline earth metal base in the presence of an acid and a solvent, distillation of the solvent, carboxylation, sulfurization and superalkalization by sulfur and an alkaline earth metal base in the presence of glycol and solvent, followed by carbonation and filtration. [0006] PCT Patent Application Publication No. WO 95/25155 discloses a process that is able to improve substantially the performance of these additives, particularly in the tests relating to foaming, compatibility and dispersion in a new oil, and in the tests of stability towards hydrolysis. This process comprises neutralization with alkaline earth metal base of a mixture of linear and branched alkylphenols in the presence of a carboxylic acid, carboxylation by the action of carbon dioxide of the alkylphenate, followed by sulfurization and super-alkalization, then carbonation, distillation, filtration, and degasing in air. [0007] European Patent Application Publication No. 0933417 discloses an unsulfurized, alkali metal-free detergent-dispersant additive, comprising a mixture of alkaline earth metal salts (alkylphenate/alkylsalicylate) and unreacted alkylphenol. This additive improves antioxidant propties, high temperature deposit control, and black sludge control. [0008] U.S. Pat. Nos. 6,162,770 and 6,262,001 teach an unsulfurized, alkali metal-free, detergent-dispersant composition having from 40% to 60% alkylphenol, from 10% to 40% alkaline earth alkylphenate, and from 20% to 40% alkaline earth single-aromatic-ring alkylsalicylate, and a process for preparing the same. This composition may have an alkaline earth double-aromatic-ring alkylsalicylate as long as the mole ratio of single-ring alkylsalicylate to double-aromatic-ring alkylsalicylate is at least 8:1. This composition may be produced by the three-step process involving neutralization of alkylphenols, carboxylation of the resulting alkylphenate, and filtration of the product of the carboxylation step. The detergent-dispersant produced by the method can be used in an engine lubricating composition to improve antioxidant properties, high temperature deposit control, and black sludge control. SUMMARY OF THE INVENTION [0009] The present invention provides a novel unsulfurized, carboxylate-containing additive for lubricating oils, comprising a mixture of alkaline earth metal salts (hydrocarbyl phenate/hydrocarbyl salicylate) and a reduced amount of unreacted hydrocarbyl phenols, as well as additive packages, concentrates and finished oil compositions comprising the same. Specifically, it relates to additives comprising said mixture in which said hydrocarbyl salicylate is primarily single-aromatic-ring hydrocarbyl salicylate. [0010] The present invention also provides a method for producing the above described additive, which comprises the neutralization of hydrocarbyl phenol using an alkaline earth base in the presence of a promoter to produce a hydrocarbyl phenate. Preferably, said promoter comprises at least one carboxylic acid containing from one to four carbon atoms, and said neutralization step is carried out in the absence of alkali base, in the absence of dialcohol, and in the absence of monoalcohol. The neutralization step is followed by carboxylation of the hydrocarbyl phenate produced in the neutralization step; and separation of the starting hydrocarbyl phenols from the product of the carboxylation step. [0011] The hydrocarbyl phenols may comprise a mixture of linear and/or branched hydrocarbyl constituents. For example, the hydrocarbyl phenols may be made up entirely of linear hydrocarbyl phenol, entirely of branched hydrocarbyl phenol, or a mixture of both. Preferably, the hydrocarbyl phenols contain up to 85% of linear hydrocarbyl phenol in mixture with at least 15% of branched hydrocarbyl phenol in which the branched hydrocarbyl radical contains at least nine carbon atoms. More preferably, the hydrocarbyl phenols are alkylphenols which contain from 35% to 85% of linear alkylphenol in mixture with from 15% to 65% of branched alkylphenol. The ratio of branched versus linear alkylphenol is given by weight. Preferably, the linear hydrocarbyl radical contains 12 to 40 carbon atoms, more preferably from 18 to 30 carbon atoms, and, if branched hydrocarbyl phenols are present, the branched hydrocarbyl radical contains at least 9 carbon atoms, preferably from 9 to 24 carbon atoms, more preferably 10 to 15 carbon atoms. [0012] Preferably, the alkaline earth base is selected from the group consisting of calcium oxide, calcium hydroxide, magnesium oxide, and mixtures thereof. [0013] Preferably, the carboxylic acid is a mixture of formic acid and acetic acid, more preferably a 50/50 by weight mixture of formic and acetic acid. [0014] Preferably, the neutralization step is carried out at a temperature of at least 200.degree. C., more preferably at least 215.degree. C. The pressure is reduced gradually below atmospheric in order to remove the water of reaction, in the absence of any solvent that may form an azeotrope with water. Preferably, the quantities of reagents used correspond to the following molar ratios: [0015] (1) alkaline earth base/alkylphenol of from 0.2:1 to 0.7:1, more preferably from 0.3:1 to 0.5:1; and [0016] (2) carboxylic acid/alkylphenol of from 0.01:1 to 0.5:1, more preferably from 0.03:1 to 0.15:1. [0017] In one embodiment, the neutralization step is carried out at a temperature of at least 240.degree. C. with a gradual reduction in pressure below atmospheric so as to reach a pressure of no more than 7,000 Pa (70 mbars) at 240.degree. C. [0018] The hydrocarbyl phenate obtained in the neutralization step is carboxylated in order to convert at least 20 mole % of the starting hydrocarbyl phenols to hydrocarbyl salicylate using carbon dioxide under carboxylation conditions. Preferably, at least 22 mole % of the starting hydrocarbyl phenols is converted, and this conversion occurs at a temperature between 180.degree. C. and 240.degree. C., under a pressure within the range of from above atmospheric pressure to 15.times.10.sup.5 Pa (15 bars) for a period of one to eight hours. [0019] More preferably, the starting hydrocarbyl phenols are alkylphenols and at least 25 mole % of the starting alkylphenols is converted to alkylsalicylate using carbon dioxide at a temperature equal to or greater than 200.degree. C., under a pressure of 4.times.10.sup.5 Pa (4 bars). [0020] The hydrocarbyl salicylate produced in the carboxylation step carboxylation step may comprise both single-aromatic-ring hydrocarbyl salicylate and double-aromatic-ring hydrocarbyl salicylate. Preferably, the mole ratio of single-aromatic-ring hydrocarbyl salicylate to double-aromatic-ring hydrocarbyl salicylate is at least 8:1. [0021] Preferably, the product of the carboxylation step is then filtered to remove any sediment formed in the carboxylation step. [0022] The product of the carboxylation step is then subjected to a separation procedure such as solvent extraction, distillatioin, membrane filtration, and the like wherein at least about 10% of the starting hydrocarbyl phenols are separated from the product of the carboxylation step. Preferably, at least about 30% to about 55% of the starting hydrocarbyl phenols are separated. More preferably, at least about 45% to about 50% of the starting hydrocarbyl phenols are separated from the product of the carboxylation step. [0023] Once the starting hydrocarbyl phenols are separated from the product of the carboxylation step, said hydrocarbyl phenols may advantageously be recycled to be used as starting materials in the process of the present invention or in any other process. Continue reading... Full patent description for Carboxylated detergent- disperant additive for lubricating oils Brief Patent Description - Full Patent Description - Patent Application Claims Click on the above for other options relating to this Carboxylated detergent- disperant additive for lubricating oils patent application. ###  How KEYWORD MONITOR works... a FREE service from FreshPatents1. Sign up (takes 30 seconds). 2. Fill in the keywords to be monitored. 3. Each week you receive an email with patent applications related to your keywords. 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