Classifications

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  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M159/00—Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
  • C10M159/12—Reaction products
  • C10M159/20—Reaction mixtures having an excess of neutralising base, e.g. so-called overbasic or highly basic products
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  • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
  • C10M2203/06—Well-defined aromatic compounds
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  • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
  • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
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  • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
  • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
  • C10M2203/102—Aliphatic fractions
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
  • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
  • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
  • C10M2207/122—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic
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  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
  • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
  • C10M2207/123—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
  • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
  • C10M2207/129—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • C10M2207/16—Naphthenic acids
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/10—Carboxylix acids; Neutral salts thereof
  • C10M2207/22—Acids obtained from polymerised unsaturated acids
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/281—Esters of (cyclo)aliphatic monocarboxylic acids
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/282—Esters of (cyclo)aliphatic oolycarboxylic acids
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/283—Esters of polyhydroxy compounds
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/286—Esters of polymerised unsaturated acids
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  • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
  • C10M2207/28—Esters
  • C10M2207/34—Esters having a hydrocarbon substituent of thirty or more carbon atoms, e.g. substituted succinic acid derivatives
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  • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
  • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
  • C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions
  • C10M2215/24—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant Compositions having hydrocarbon substituents containing thirty or more carbon atoms, e.g. nitrogen derivatives of substituted succinic acid
  • C10M2215/26—Amines
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  • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
  • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C10M2217/046—Polyamines, i.e. macromoleculars obtained by condensation of more than eleven amine monomers
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  • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
  • C10M2217/06—Macromolecular compounds obtained by functionalisation op polymers with a nitrogen containing compound
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  • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
  • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
  • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
  • C10M2219/046—Overbased sulfonic acid salts
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  • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
  • C10M2223/12—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions obtained by phosphorisation of organic compounds, e.g. with PxSy, PxSyHal or PxOy
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  • C10M2225/00—Organic macromolecular compounds containing phosphorus as ingredients in lubricant compositions
  • C10M2225/04—Organic macromolecular compounds containing phosphorus as ingredients in lubricant compositions obtained by phosphorisation of macromolecualr compounds not containing phosphorus in the monomers
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  • C10N2010/00—Metal present as such or in compounds
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  • C10N2070/00—Specific manufacturing methods for lubricant compositions
  • C10N2070/02—Concentrating of additives

Definitions

• an oil-soluble detergent'or dispersant ii. a basicalkaline earth compound, iii, a hydroxy containing organic compound, and iv. as promoter, an amine salt of an acid; b. treating the reaction mixture with an acidic gas;
• lubricants containing the overbased additives as detergents and dispersants.
• This invention relates to lubricant additives, and in particular to the prepartion of overbased lubricant additives, which are detergents and dispersants, and to compositions containing the additives so prepared.
• detergent and/or dispersant additives are commonly incorporated in lubricants to counteract such deposits. It has been found that basic detergents and dispersants, i.e., detergents and dispersants having a high content of an alkali or alkaline earth metal salt of a weak acid such as carbonate, are particularly useful. The basicity of such additives counteracts corrosive acidic compounds, e.g., combustion products, which are formed during the operation of engines.
• the basic additives are commonly prepared by a process consisting essentially of suspending a basic metal compound, e.g., calcium hydroxide or oxide, in an inert solvent (usually lubricating oil) containing a detergent or dispersant, such as a carboxylic or sulphonic acid or metal salt thereof, and passing an acidic gas, usually carbon dioxide, through the suspension.
• a basic metal compound e.g., calcium hydroxide or oxide
• an inert solvent usually lubricating oil
• a detergent or dispersant such as a carboxylic or sulphonic acid or metal salt thereof
• the product should be a clear liquid which is stable, i.e., the basic metal compound should not separate from the liquid phase, and in which the metal of the metal compound is present in an excess of the stoichiometric amount required to react with the acid groups of the detergent of dispersant.
• the overbasing process should have good repeatability. That is to say there should be a high degree of consistency in the quality of products obtained when the process is carried out repeatedly under identical conditions, as happens when commercial production is undertaken.
• magnesium oxide or hydroxide as a source of magnesium have been uneconomic, e.g., by virtue of being multi-stage processes, and/or have produced additives lacking, to an unacceptable degree, one of more of the properties of clarity, basicity, consistency of quality and performance in engine tests.
• the products have been unsuitable therefore for economic or technical reasons.
• overbased magnesium-containing detergents have not been produced on a commercial scale from magnesium oxide or hydroxide and the only commercially used method employs magnesium metal, despite the unfavourable economics of using such expensive starting materials.
• the present invention provides a process for preparing an overbased lubricant additive, which process comprises:
• the inert solvent employed in the process ofthe pres ent invention may be a lubricating oil of the synthetic ester type well known in the art.
• An example of such esters is dioctyl sebacate. Further examples of these esters are described in U.l(. Pat. No. 1,205,177 the relevant portions of which are incorporated herein by reference.
• Such esters are also available commercially, for example, the range of pentaerythritol esters marketed under the trade name Hercolube.
• a hydrocarbon solvent such as a petroleum oil of the type used in lubricating compositions.
• the hydrocarbon oil vehicle may consist of a synthetic hydrocarbon oil, for example, an alkylated benzene fraction, or a mixture of such an oil with.
• the inert solvent may be a non-polar diluent, particularly a hydrocarbon diluent, as referred to hereinafter.
• a non-polar diluent particularly a hydrocarbon diluent, as referred to hereinafter.
• Such diluents of comparatively low viscosity may be useful when the detergent or dispersant is a pure sulphonic acid or salt thereof which is solid or a highly viscous liquid.
• the proportions of the inert solvent which is employed can vary widely depending on the proportions of the other components of the reaction mixture. Indeed the proportion of each component can vary according to the varying proportions of each of the other components. In view of this interdependency of the proportions it is convenient to take the amount of the inert solvent as a reference point and relate the proportions of other components thereto.
• Oil-soluble detergents or dispersants which are susceptible to overbasing are well known in the art and the material used in the present process may be selected from those conventionally used in overbasing pro Fallss, such as phosphosulphurised hydrocarbons, e.g., polyisobutylene treated with phosphorus pentasulphide, or metal salts of carboxylic acids, particularly alkanoic acids, e.g., acetic or fatty acids, or naphthenic acids.
• Suitable oil-soluble detergents or dispersants include those disclosed in the aforementioned U.S. Pat. Nos. 3,492,230 and 3,629,109. It is particularly preferred to use a sulphonic acid or metal salt thereof, especially a metal salt wherein the metal is an alkaline earth metal. In a preferred embodiment the metal is the same as the metal present in the basic alkaline earth compound.
• the sulphonic acid may be a petroleum sulphonic acid (also termed mahogany sulphonic acids) prepared by sulphonating petroleum feedstocks or it may be an alkyl, aryl or alkaryl sulphonic acid. Examples of such sulphonic acids include.
• petroleum sulphonic acids of molecular weight 350 to 750 dilauryl aryl sulphonic acid, lauryl-cetyl aryl sulphonic acid, paraffin waxsubstituted benzene sulphonic acid, didodecyl benzene sulphonic acid, polyolefin alkylated benzene sulphonic acids, such as polyisobutylene alkylated benzene sulphonic acids in which the polyisobutylene substituents have molecular weights of at least 200, preferably from 300 to 2,500, polypropylene alkylated benzene sulphonic acids in which the polypropylene substituents have molecular weights of at least 200, preferably from 290 to 1,500, naphthalene sulphonic acids and alkylsubstituted naphthalene sulphonic acids.
• Particularly preferred sulphonic acids are mono-alkyl substituted benzene sulphonic acids having molecular weights of from 450 to 550, for example, the commercially available product Monsanto M 5336 (straight chain monoalkyl substituted benzene sulphonic acid of molecular weight 470 to 480).
• the amount of detergent or dispersant employed may be varied over a wide range. We prefer to use from percent, more preferablyat least percent, up to 120 or even 150 percent by weight based onthe weight of the inert solvent. A particularly preferred proportion is from 60 to 120 percent by weight.
• the basic akaline earth compounds useful in over- I basing processes are also well known, examples being oxides and hydroxides such as magnesium, barium and calcium oxides and hydroxides, the magnesium compounds, especially magnesium oxide, being preferred.
• the process of the present invention can also be'used for preparing overbased additives containing other metals.
• the amount of the basic alkaline earth compound to be employed may be readily calculated from the intended basicity of the additive product.
• the maximum basicity which can be achieved will depend, inter alia, on the degree of susceptibility of the detergent of dispersant.
• T.B.N total base number
• Additives having this level of basicity are regarded as highly basic and the process of the present invention is particularly suitable for preparing such highly basic additives.
• additives of lower basicity are also useful commercial products and may also be prepared by the process of the present invention.
• magnesium oxide is the most preferred basic alkaline earth compound for use in the present invention.
• Magnesium oxide is commercially available in two forms, sometimes referred to as light and heavy magnesium oxide.
• the former is a relatively active form, usually derived from extraction from sea water.
• Heavy magnesium oxide sometimes called dead burned, is produced by mining and roasting of the mineral material and is commonly considered a less active form of magnesium oxide.
• either form of magnesium oxide may be used.
• Light magnesium oxide such as the commercially available material Merck Maglite Y3234 supplied by Merck Chemical Division, N.J., is preferable from the viewpoint of providing a somewhat more easily controlled process and somewhat better product; whereas heavy magnesium oxide, which is less expensive,
• the hydroxy compound employed in the reaction mixture is believed to act as a co-promoter with the amine salt of an acid.
• suitable hydroxy compounds include alcohols, glycols and glycol monoeth'ers.
• the choice of hydroxy compound is not critical. However, for ease of removal of the hydroxy compound from the product of the process it is preferred that the hydroxy compound has as low a boiling point as possible. For this reason the hydroxy compound preferably contains from one to four carbon atoms and the preferred hydroxy compounds are therefore lower alcohols, particularly alkanols, glycols containing from one to four carbon atoms, e.g., ethylene glycol, propylene glycol, butylene glycol or diethylene glycol, and
• monoethers of glycols containing from one to four carbon atoms e.g., ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monoisopropyl ether, ethylene glycol mono-n-propyl ether, propylene glycol mono-ethyl ether, propylene glycol mono-methyl ether, diethylene glycol monomethyl ether or butylene glycol mono-methyl ether.
• the lower alkanols, particularly methanol, are especially preferred.
• the amount of hydroxy compound used is a reaction promoting amount preferably at least 5 percent, more preferably 25 percent to 50 percent by weight based on the weight of the inert solvent.
• water is also present in the reaction mixture, for example in an amount of from 5 to 50 percent, more preferably 15 to 30 percent by weight based on the weight of the inert solvent.
• water may be desirable to subsequently add a further quantity of water, for example from 10 to 25percent by weight based on the weight of the inert solvent, during the treatment of the reaction mixutre with acidic gas.
• the amine salt of an acid which is used as a promoter in the process of the present invention may be a salt of a mono-, dior poly-amine with an inorganic acid or an organic acid, eg a mono-, dior poly-carboxylic acid and the amine and/or the acid may be aliphatic or aromatic, Alternatively, a heterocyclic amine may be used.
• the promoter may be selected from salts of a large number of amines, although among these certain salts are preferred.
• salts of aliphatic amines with aliphatic carboxylic acids, particularly monocarboxylic acids, are especially useful.
• the salts are preferably neutral salts.
• the promoter is a salt of a carboxylic acid. If an aromatic carboxylic acid is sued, this preferably consists only of carbon and hydrogen atoms other than the two oxygen atoms in the, or each, carboxyl group. However salts of aliphatic carboxylic acids are preferred. Diand polycarboxylic aliphatic acids which may be used include those containing two to ten carbon atoms, examples being adipic, maleic, glutaric, succinic, and azelaic acids. Monocarboxylic acids, such as aklanoic acids, may also be used.
• acids from which the promoters may be formed are alkanoic acids containing from one to twenty carbon atoms (including the carbon atom present in the carboxylic group).
• the most preferred acids are formic acid and alkanoic acids containing from seven to twelve carbon atoms, e.g,m decanoic.
• the amines from which the salts are formed include monoamines, such as oleylamine and laurylamine, diamines, such as ethylene diamine or propylene diamine, and polyamines, such as diethylene triamine. These are representative aliphatic hydrocarbyl amines. Suitable amines also include those disclosed in the aforementioned US. Pat. No. 3,492,230. Preferred amines contain not more than carbon atoms. Diamines and polyamines are the most preferred amine moiety, particularly those containing from two to eight carbon atoms. Ethylene diamine is the most preferred amine and it is especially preferred to use as the promotoer the diformate salt of ethylene diamine.
• the amount of the promoter used is a reaction promoting amount and may be, for example, from 0.1 to 30 or 40 percent by wieght, based on the weight of the inert solvent, within which range optimum proportions may be selected according to the amine salt used and the intended basicity.
• the preferred proportions of promoter are from 0.1 to percent more preferably 1.0 to 10 percent by weight based on the weight of the inert solvent. This may be varied according to the intended basicity of the product. For example, from 5 to 7 percent by weight of promoter may be used in the preparation of an additive having a T.B.N. of 300 and from 7 to 10 percent by weight in the preparation of an additive having a T.B.N. of 400.
• the preferred proportions are such as to give the same molar ratio of promoter to other components of the reaction mixture as in the case of the preferred proportions of ethylene diamine diformate.
• non-polar diluent other than any used as, or as part of, the inert solvent, particularly a hydrocarbon diluent such as xylene, benzene, toluene or pertroleum ether.
• This diluent assists in maintaining the reaction mixture at a low viscosity during the overbasing process and is preferably a volatile diluent which can be varied over a very wide range depending on the choice of other components in the reaction mixture and their effect on viscosity.
• from 80 to 150 percent, more preferably 100 to 130 percent by weight, based on the weight of the inert solvent, of toluene is used as diluent.
• the components of the reaction mixture may be merely mixed in a reaction vessel and the order in which the components are added is not critical. However, a convenient technique is to prepare an aqueous solution of the promoter and add it to the remaining components previously mixed in the reaction vessel.
• an acidic gas is passed therethrough.
• the acidic gases which may be used in overbasing processes are also well-known in the art, examples being sulphur dioxide and hydrogen sulphide. However, a particularly preferred acidic gas is carbon dioxide.
• the pressure at which the reaction mixture is treated with the acidic gas is also not critical. A pressure above, below or at atmospheric may be used. Treatment at atmospheric pressure is convenient as not requiring equipment to establish and maintain the pressure at which the reaction is carried out.
• an increase in pressure over atmospheric may assist utilization of the acid gas.
• a small increase over atmospheric e.g., up to 4 or 5 p.s.i.g., will suffice and normally only 1 or 2 p.s.i.g. is sufficient.
• the temperature at which the process is carried out is likewise not critical and treatment with the acidic gas may take place at any temperature from ambient (about 20C) up to the decomposition temperature of the reaction mixture.
• the reaction is exothermic and the temperature of the reaction mixture will tend to increase as the reaction proceeds. If desired, this can be counterbalanced, e.g., by cooling, to maintain a low reaction temperature.
• the important factor in the decomposition temperature of the reaction mixture is the temperature at which significant deterioration of the product formed in the reaction mixture occurs. We prefer therefore to keep the reaction temperature below 180C., more preferably below C.
• the reaction temperature will also be affected by water, and non-polar diluent, if used, and the choice of hydroxy compound.
• reaction temperature therefore desirably does not exceed the boiling point of the most volatile component of the reaction mixture (normally methanol) or any azeotrope formed by components of the reaction mixture (e.g., a methanol/water/toluene azeotrope). It is normally advantageous therefore to carry out the reaction at or below the reflux temperature of the reaction mixture.
• treatment at the reflux temperature has the advantage that a constant temperature is easily maintained.
• the reaction mixture may be agitated to improve contact between gas and reaction mixture.
• the acidic gas is passed through the reaction mixture until the basic alkaline earth compound is substantially converted to alkaline earth salt, whereafter the reaction mixture is heated to remove volatile components, e.g., water, methanol and any non-polar diluent.
• volatile components e.g., water, methanol and any non-polar diluent.
• the volatile components are removed under reduced pressure, e.g., by vacuum stripping.
• Basic alkaline earth compound not consumed during the overbasing process may be removed by filtration of the product.
• a filter aid such as diatomaceous earth, may be used in the filtration, which may be carried out after stripping, although we prefer to filter before stripping off volatile components.
• water and volatile hydroxy compound particularly in the case of methanol, are substantially removed before filtration, and any non-polar diluent and remaining water and volatile hydroxy compound are stripped off after filtration.
• v. about 0.1 to 40 percent by weight, based on the weight of the inert solvent, of a salt of an aliphatic amine and an alkanoic acid, preferably the diformate salt of ehtylene diamine, and, optionally,
• magnesium oxide or hydroxide by converting the magnesium oxide or hydroxide to magnesium carbonate is meant complexing or dispersing the magnesium in the inert solvent to form a stable, liquid product, by means of the treatment with carbon dioxide.
• the exact chemical structure of the additives of the present invention is not completely understood.
• the present invention further includes an overbased 40 lubricant additive whenever preapred by the process of the present invention and a composition comprising a lubricating oil and an overbased lubricant additive prepared by the process of the present invention.
• Such compositions may be lubricantcompositions containing a major amount of lubricating oil and a minor amount, for example 0.1 to 10 percent, preferably 0.5 to 5 percent by weight based on the total weight of the compositions of one or more overbased additives prepared by the process of the present invention.
• lubricant compositions may also contain conventional additives such as antioxidants, corrosion inhibitors, an ti-wear additives, detergents, dispersants, extreme pressure additives, viscosity index improvers, pour point depressants and/or load carrying additives.
• conventional additives such as antioxidants, corrosion inhibitors, an ti-wear additives, detergents, dispersants, extreme pressure additives, viscosity index improvers, pour point depressants and/or load carrying additives.
• compositions may be concentrates containing a minor amount of lubricating oil and a major amount of one of more overbased additives prepared by the process of the present invention or additive packages containing a minor amount of lubricating oil and a major amount of an additive consisting of one or more-additives prepared in accordance with the present invention in combination with one or more conventional additives.
• Esso HT 233 sulphonic acid branched chain mono-substituted alkyl benzene sulphonic acid of molecular weight about 500; 70 percent active
• Mineral Oil A a branched chain mono-substituted alkyl benzene sulphonic acid of molecular weight about 500; 70 percent active
• the product of the carbonation was filtered with the aid of a filter, aid. Toluene, water and methanol were removed from the product by vacuum stripping to 150C.
• the final product contained 6.7 percent by weight Mg., 30 percent by weight soap (magnesium sulphonate) and had a T.B.N. of 300 mg, KOH/g.
• Magnesium oxide (as in Example 1) 312g. Toluene 84g. Methanol A promoter was prepared by reacting l6g. formic acid with 10g. ethylene diamine in ml. water and the promoter was transferred to the flask with the aid of a further 25ml. water. The mixture was then carbonated under reflux in the same manner as in Example 1., whereafter a further 50ml. water was added and carbonation continued for a further 2 hours.
• Example 2 The product was filtered and vacuum stripped as in Example 1, to yield a final product containing 8.7 percent by weight Mg., 20 percent by weight soap and having a T.B.N. of 400mg. KOH/g.
• the sulphonic acid, base oil, toluene, methanol and magnesium oxide were weighed into a 2-litre reaction flask fitted with a stirrer, reflux condenser, thermometer and a sub-surface injection tube for carbon dioxide.
• the ethylene diamine and formic acid were dissolved separately in 25g. and 50g. water, respectively.
• the two resulting solutions were carefully mixed together with a further g. of water and the ethylene diamine diformate solution added to the neutral magnesium sulphonate mixture.
• Carbon dioxide gas was injected into the stirred reaction mixture via the injection tube at a rate of 1.22 1itres per minute. The passage of gas was continued for one hour, during which period the reaction temperature rose from 43C to 68C maximum.
• the product was clear, bright and mobile.
• the total base number (TBN) was 396mg. KOH/g, with a total magnesium content of 9.3 percent.
• the soap content was 25 percent.
• Mineral Oil B used in this example had viscosities of about 22 and 4 cSt. at 100F and 210F respectively and a Viscosity Index of 95.
• EXAMPLE 4 An additive having a TBN of 338mg. KOH/g. and containing 26.6 percent by weight soap and 7.86 percent by weight Mg was prepared by a procedure identical to and using the same quantities of the same materials as in Example 3, except in that 207g. dioctyl sebacate was used in place of Mineral Oil B. The product was a clear, bright liquid.
• EXAMPLE 5 An additive having a TBN of 183mg. KOH/g. and containing 30.7 percent by weight soap and 4.64 percent by weight Mg was prepared by the same procedure as, and using the same quantities of the same materials as, Example 3 except for the following:
• Magnesium hydroxide (146g) was used in place of the magnesium oxide.
• EXAMPLE 6 An additive having a TBN of 377mg. KOH/g. and containing 25.5 percent by weight soap and 8.66 percent by weight Mg was prepared using the same quantities of the same material as, and following the procedure of, Example 3 except in that carbonation was continued for minutes and the temperature of the reaction mixture was maintained at 40C i 1C. throughout the carbonation. The product was a clear, bright liquid.
• EXAMPLE 7 An additive having a TBN of 298mg. KOH/g. and containing 27.6 percent by weight soap and 7.02 percent by weight Mg was prepared by the procedure of Example 3 except as follows:
• the product was a clear, bright, mobile liquid having excellent filterability.
• EXAMPLE 8 A very highly basic additive (TBN 543mg.KOH/g.) containing 21.8 percent by weight soap and 11.35 percent by weight Mg. was prepared from the following materials:
• Example 3 The procedure was the same as that of Example 3 except that durig carbonation the temperature rose, due to the exotherm, to a maximum of 61C after 20 minutes and carbonation was continued for a total of 1% hours.
• Table 1 shows the results obtained using various de' tergents and dispersants in the process of Example 3. Except in respect of the detergent or dispersant the materials used, and the quantities thereof, were the same as in Example 3.
• Table 2 summarizes the preparation of additives of varying soap content by the process of Example 3.
• the quantities of the sulphonic acid and Mineral Oil B were varied to adjust the final soap content. All other components, and the quantities thereof, were the same as in Example 3.
• Table 3 shows preparations wherein the same procedure as in Example 3 was used and the materials and quantities were the same as in Example 3, except in that the 70g. methanol was replaced by 70g. of various other hydroxy compounds.
• Table 4 summarizes preparations using the neutral formate salts of various amines
• Table 5 summarizes preparations using ethylene such as using larger quantities of the less viscous components of the reaction mixture, filtering before removing volatile components to improve filterability (the volatile components are in general also the less viscous diamine salts of various acids. Except for the indicated 5 components) and/or selection ofreaction mixture comvariations all the preparations were carried out using ponents (for example, in the case of the inert solvent the same procedure, materials and quantities thereof as synthetic ester lubricating oils normally have lower visin Example 3. cosities than mineral oils).
• PRODUCT NO. (gm.) (mg.KOH/g.)
• Polyisobutylene substituted succinic acid prepared by 9 reaction of maleic anhydride with Hyvis 100 (commercially 1160 available polyisobutylene of average molecular weight about 2000) Succinimide prepared by formation of 1:! molar reaction product of dicyandiamide and tetraethylene pentamine l0 and reaction of this product with a polyisobutylerie sub- 1160 38 stituted succinic acid as in Example 9.
• ll Naphthenic Acid 97 181 Magnesium sulphonate prepared by double decomposition of a 50% solution in mineral oil (8.0. 0.9) of a sodium etroleum sulphonate with magnesium chloride.
• the sodium petroleum sulphonate had an average 12 molecular weight of 460 to 465 and the mineral oil 187 267 solution of the sulphonate consisted of parts of a mineral oil solution (50%) of a medium molecular weight sulphonate and 25. parts of a mineral oil solution (50%) of a high molecular weight sulphonate.
• Petroleum sulphonic acid being the acid from which 13 the sodium petroleum sulphonate of Example'l2 was derived).
• Patent No.3492230 Ethylene Diamine Di- 64 formate (20g. ethylene Example ll of U5. 3
• a reaction mixture of an oil soluble detergent or dispersant susceptible to overbasing selected from the group consisting of phosphosulphurized hydrocarbons, metal salts of carboxylic acids, sulphonic acids and metal salts of sulphonic acid, a basic magnesium compound in an amount sufficient to overbase said oil soluble detergent or dispersant, and a reaction promoting amount of a hydroxy-containing compound selected from the group consisting of alcohols and monoethers of glycols is formed in an inert solvent
• said reaction mixture is contacted with an acidic gas at a reaction temperature of from about 20C up to the decomposition temperature of the reaction mixture and the resultant product is heated
• the oil soluble detergent or dispersant is present in the amount of about 10 to 150 percent by weight based on the weight of the inert solvent
• the hydroxy containing organic compound is present in an amount of about 5 to 50 percent by weight, based on the weight of the inert solvent
• the salt of the amine and acid is present in the reaction mixture in an amount of about 0.1 to 40 percent by weight, based on the weight of the inert solvent, about 5 to 50 percent by weight, based on the weight of the inert solvent, of water is present in the reaction mixture and wherein the acidic gas is carbon dioxide.
• hydroxy containing organic compound is selected from the group consisting of monohydroxis alcohols, containing from one to four carbon atoms, glycols containing from one taining from one to four carbon atoms.
• reaction mixture is formed by admixing the inert'solvent, the oilsoluble detergent or dispersant, the basic magnesium compound and the hydroxy containing organic compound and thereafter adding thereto an aqueous solution of the amine salt of the acid.
• the inert solvent is selected from the group consisting of mineral oils, alkyla'ted benzene and mixtures thereof.
• non-plar diluent is selected from the group consisting of xylene, benzene, toluene and petroleum ether.
• the inert solvent is a hydrocarbon oil solvent
• the oil soluble detergent or dispersant is an oil soluble neutral magnesium salt of sulphonic acid in an amount of about 20 to 120 percent by weight, based on the weight of the hydrocarbon oil solvent
• the basic magnesium compound is magnesium oxide or magnesium hydroxide in an amount to provide an additive having a total base number of about 250 to 500 mg.
• the hydroxy-containing compound is methanol in an amount of about 25 to 50 percent by weight, based on the weight of the hydrocarbon oil solvent; the salt of an alkanoic acid and an aliphatic hydrocarbyl diamine is present in an amount of about 0.1 to 15 percent by weight, based on the weight of the hydrocarbon oil solvent; from about 5 to 50 percent by weight, based on the weight of the hydrocarbon oil solvent, of water is present in the reaction mixutre; and the reaction mixture is treated with carbon dioxide at a temperature of from about 20C up to the reflux temperature of the reaction mixture until the magnesium soluble additive according to claim 17.
• a lubricant comprising a major amount of lubricating oil containing from 0.1 to 10 percent by weight, based on the total weight of the lubricant, of an oilsoluble additive according to claim 18.
• a lubricant comprising a major amount of lubricating oil containing from 0.1 to 10 percent by weight, based on the total weight of the lubricant, of an oilsoluble additive according to claim 19.

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• Chemical & Material Sciences (AREA)
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• General Chemical & Material Sciences (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Organic Chemistry (AREA)
• Lubricants (AREA)
• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
• Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)

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• 1971
  • 1971-05-27 GB GB1760471A patent/GB1399092A/en not_active Expired
• 1972
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• 1974
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