Method of obtaining detergents for lubricants

FIELD: chemistry.

SUBSTANCE: invention relates to improved method of salicylates of alkaline earth metals for application as detergents for lubricating materials. Method of obtaining alkylated salicytates of alkaline earth metals includes following stages: A) alkylating salicylic acid with linear α-olefin, containing, at last, 14 carbon atoms, in presence of water-free methane sulfonic acid with formation of oil-soluble alkylated salicylic acid; B) neutralisation of oil-soluble alkylated salicylic acid; C) excessive alkalisation of oil-soluble alkylated salicylic acid by carboxylating lime by means of CO2 in presence of oxygen-containing organic solvent and surface-active substance; D) filtration of stage (C) product; and E) removal of solvent by distillation. Alternatively, alkylsalicylic acid can be subjected to interaction with preliminary processed with alkali highly-alkaline sulfonate of earth alkaline metal, for instance, with calcium sulfonate, in order to obtain salicylate salts of earth alkaline metals with different per cent content of dispersed salts of alkaline earth metals carbonates. In claimed method it is not necessary to filter end product which is preferable doe industry.

EFFECT: obtaining salicylates of alkaline earth metals for application as detergents for lubricating materials.

8 cl, 4 ex

 

The level of technology

1. The technical field to which the invention relates

This invention relates to a method for producing a high alkaline detergents on the basis of alkaline earth metals for use in lubricants.

2. Description of the prior art

Know the use of salts of alkaline earth metals, organic carboxylic acids as additives to compositions of lubricating oils. Mentioned salts possess dispersing ability, which helps to ensure the purity of the internal parts of the engine and prevents the deposition of carbon products on the pistons and on the grooves of the piston, preventing, thus, sticking of the piston and rings.

Known also getting alkaline or strongly alkaline) salts of such acids and alkaline earth metals. Excessive alkalization provides a supply of alkali, which when used in lubricating compositions react with acidic compounds to neutralize acidic compounds formed during operation of the engine in which the use of this composition. The result is that any contamination that may occur dispersed due to the dispersing effect of salt and acid, which would enhance the education of contaminants are neutralized.

High-alkaline salicylates obtained by redundantly what about alkalizing the corresponding alkyl salicylic acids. The alkyl group typically represents an alkyl group with a long chain containing more than 14 carbon atoms, which gives the acid solubility in oil. Alkylated salicylic acid is usually obtained by alkylation of phenol with the formation of alkylphenol and subsequent carboxylation of alkylphenol by the reaction of the Kolbe-Schmitt, which gives alkilirovanny salicylic acid. In addition to adverse economic factors associated with the use of high temperatures and/or pressures, the way to get alkyl salicylic acids by the reaction of the Kolbe-Schmitt is complicated by the fact that not all APS with long chain easily carboxydismutase at alkylation mostly linear connections. Specifically, conventional alkylation of phenol linear alkylating agent to give a mixture (about 50:50)ortho-alkylphenol andpair-alkylphenol. Receivedpair-alkylphenol with long chain easily carboxylases by the reaction of the Kolbe-Schmitt, whereas the obtainedortho-alkylphenol with long chain less reactive, and only about 70 percent of the total number of alkylphenol derived from essentially linear alkylating agent, usually turns into alkilirovanny salicylic acid during this reaction.

One way to get around this problem, is that is, to alkilirovanii alkylsalicylate (e.g., methyl salicylate) and then to hydrolyze received alkilirovanny alkylsalicylate in order to get alkilirovanny salicylic acid. Methods of alkylation alkylsalicylate described in U.S. patent No. 5434293.

In applications DD-A-269619 and DD-A-293108 described direct alkylation of salicylic acid-olefin using a catalyst acidic ion-exchange resin or polyphosphoric acid, respectively. In both applications indicate that the use of sulfuric acid as a catalyst (in the methods of the prior art, does not include alkylation acid-olefin) is undesirable, because it has many disadvantages, such as problems of corrosion and adverse reactions.

In German patent No. 689600 described the use perchloro acid as a catalyst.

In U.S. patent No. 1998750 described condensation of salicylic acid with any non-aromatic monohydroxy alcohol containing from 5 to 7 carbon atoms, or compounds capable of providing amyl-, hexyl-, cyclohexyl - or heptyl group, in the presence of sulfuric acid.

In U.S. patent No. 4810398 described the basic salt of the alkali earth metal and mixtures of organic carboxylic acids, obtained (a) by mixing one equivalent of a mixture of organic carboxylic acids and more than one EQ is Valens hydroxide and/or oxide of alkaline earth metal in a hydrocarbon solvent; (b) the introduction of carbon dioxide in the mixture in amounts of at least 0.5 equivalent of carbon dioxide equivalent excess alkaline earth metal; and (c) removing residual solids, if any, and the aqueous layer, if present; in accordance with what a mixture of organic carboxylic acid contains C8-30alkylsalicylate acid and one or more alkenylboronic acids in which the alkyl residue is branched and contains from 4 to 40 carbon atoms. This salt has dispersing properties and is claimed to be suitable for use in the compositions of lubricating oils and fuels.

In U.S. patent No. 4869837 describes how to obtain basic salts of the alkali earth metal with a mixture of organic carboxylic acids, which comprises (a) mixing one equivalent of a mixture of organic carboxylic acids and more than one equivalent of hydroxide and/or oxide of alkaline earth metal in a hydrocarbon solvent; (b) introducing carbon dioxide into the resulting mixture in an amount of at least 0.5 equivalent of carbon dioxide equivalent excess alkaline earth metal and (c) removing residual solids, if any, and the aqueous layer, if present, in accordance with what a mixture of organic carboxylic acid contains soluble in oil al is EliLilly acid and one or more uglevodorodnykh succinic acids or anhydrides, in which the average molecular weight hydrocarbon radical is from 120 to 5000.

In U.S. patent No. 4876020 described lubricant composition comprising a lubricating base oil, one or more alkali salts, alkaline earth metal aromatic carboxylic acid and a stabilizer selected from polyalkoxysiloxanes alcohol, molecular weight which ranges from 150 to 1500.

In U.S. patent No. 5049685 described substituted in the nucleus salicylic acid represented by the following General formula:

in which R1means methyl group, isopropyl group,tert-boutelou group,tert-amylou group,tert-hexoloy group,tert-aktiline group α,α-dialkylamino group or substituted in the nucleus α,α-dialkylamino group, and R2meanstert-boutelou group,tert-amylou group,tert-hexoloy group,tert-aktiline group α,α-dialkylamino group or substituted in the nucleus α,α-dialkylamino group and its salt. Substituted in the nucleus of salicylic acid and its salts, as claimed, have good solubility in water, organic solvents or organic polymeric compounds, and they are used as bactericides and germicides, stabilization of the Directors of polymer compounds or color developers for registration materials.

In U.S. patent No. 5415792 described strongly alkaline alkylsalicylate, which are considered to be useful additives for compositions of lubricating oils. Specifically, the composition of additives give ability and dispersibility of the composition of lubricating oils, as well as provide reserve alkalinity.

In U.S. patent No. 5434293 described by way of alkylation alkylsalicylate, which use acid alkylation catalyst and an approximately equimolar amount of alkylsalicylate and alkylating raw materials.

In U.S. patent No. 5451331 described method of production of concentrate additives to lubricating oils with a TBN greater than 300, which includes the interaction at a high temperature component (A) is a derivative of salicylic acid, component (B) is the Foundation of the alkaline earth metal to be added or a single portion or multiple portions by adding at intermediate points during the reaction, the component (C) at least one compound which is a (i) water, (ii) a polyhydric alcohol containing 2-4 carbon atoms, (iii) di(C3or C4)glycol, (iv) three(C2-C4)glycol, (iv) simple alkilany ether mono - or polyalkyleneglycol formula (I) R(OR1)xOR2(I), where R is C1-C6alkyl group, R1means alkylenes group, R2about the means hydrogen or C 1-C6alkyl group and x represents an integer from 1 to 6, (vi) C1-C20monohydroxy alcohol, (vii) C1-C20ketone, (viii) C1-C10ester of carboxylic acid or (ix) C1-C20a simple ether, component (D) lubricating oil, component (E) carbon dioxide added after adding the component (C) or after each addition of component (F) is specified carboxylic acid or its derivative, component (G) at least one connection, which is (i) an inorganic halide (ii) of alkanoate ammonium or formate or alkanoate mono-, di-, tri - or tetraalkylammonium, provided that when component (G) is a (ii), component (F) is not an acid chloride of the acid, and the ratio of the masses of all components is such as to obtain a concentrate with a TBN greater than 300.

In U.S. patent No. 5734078 describes a method for alkylsalicylate acid in which the alkyl substituent contains at least 6 carbon atoms, including interaction of salicylic acid with an olefin containing at least 6 carbon atoms, at an elevated temperature in the presence of sulfuric acid as a catalyst. Described as additives to lubricating oils containing metal salt such alkyl salicylic acids and the method of their manufacture.

In U.S. patent No. 5792735 described composition of lubricating oils, which is claimed to be suitable for use in low-speed or medium-speed diesel engines and contains fuel oil with a residual oil content, characterized in that the composition of the lubricant additionally contains a concentrate hidrocarbonetos pinata with a TBN greater than 300 and at least one product from hidrocarbonetos musk and hidrocarbonetos sulfonate. Gidrokarbonatnyj feat preferably is Fantom modified by incorporating carboxylic acid of the formula RCH(R1)CO2H, where R is C10-C24alkyl group, and R1means hydrogen or C1-C4alkyl group, for example, stearic acid.

In U.S. patent No. 6034039 described complex detergents, which are said to provide better control of deposition and corrosion protection, lubrication for the crankcase (engine).

In U.S. patent No. 6444625 describes a method for alkali sulfonate calcium. The method comprises the stages: the feed to the reactor sulfonic acid; add in the lime reactor (i.e. calcium hydroxide or calcium oxide) in the quality of the reagent to neutralize and over-alkalizing, adding a lower aliphatic alcohol C1-C4and hydrocarbon process is Italia, getting into the reactor mixture, which in a handy case has a temperature of about 27° (80°F); insufflation of carbon dioxide into the reactor at the initial temperature 43-54° (110-130°F), up until essentially all the lime will not be carbonsilicon, while maintaining this exothermic reaction temperature in the range from 27 to 57°With (from 80 to 135°F), a is preferably from 43 to 52°With (110 to 125°F); adding a certain amount of oil to the mixture with the formation containing product mixture; clarification containing product mixture by filtering off the solid components and distillation of volatile hydrocarbon solvents and water, obtaining thus a transparent, high-alkaline (high excess alkali), high viscosity sulfonate calcium.

Descriptions of the above-mentioned patents are included in this application as references in its entirety.

The invention

This invention relates to a method of producing alkaline earth metal salicylates for use as a detergent for lubricants and compositions obtained in this way. The method includes two stages:

Stage 1:

The alkylation of salicylic acid is performed using linear α-olefins (C14or higher), receiving alkylsalicylate acid with outputs that are acceptable to the industry is nasty. In these conditions, the alkylation is mainly obtained monosubstitutedpair-alkylsalicylate acids, which are soluble in oil.

Stage 2:

Soluble in oil acid is then neutralized andexcessively alkalinizedthe carboxylation of lime, using CO2in the presence of an activator, such as methanol, and surface-active substances, for example, alkylsalicylate acid. The reaction mixture afterexcessive alkalizing filtered and the solvents removed by distillation.

Alternatively, alkylsalicylate acid can be subjected to interaction with the pre-treated with excess alkali detergent selected from the group consisting of high alkali sulfonates, Benatov or carboxylates of alkali or alkaline earth metals, and get salicylate salts of alkaline or alkaline earth metals with different percentages dispersed carbonate salts of alkali or alkaline earth metals. In this way you do not need to filter the final product, and therefore, it is preferable for the industry. It is also preferable that the high-alkaline detergent is pretreated with an excess of the alkali sulfonatealkaline earth metal such as calcium sulfonate.

It is shown that the structure of the olefin has the value for the operational qualities of the final products as differential scanning calorimetry under pressure (PDSC), and in compatibility and malorastvorimaja detergents. The preferred chain length is16-C18for optimal PDSC, although higher than18the carbon content improves the compatibility and maslorastvorimye additives.

More specifically, this invention relates to a method of producing alkaline earth metal salicylates, which includes stages:

A) alkylation of salicylic acid α-olefin containing at least 14 carbon atoms, in the presence of a strong acid catalyst to form a soluble oil alkilirovanny salicylic acid;

C) neutralizing soluble in oil alkilirovanny salicylic acid;

C) excessive alkalizing soluble in oil alkilirovanny salicylic acid by carboxylation of lime,using CO2in the presence of an activator and a surfactant;

D) filtering the product of stage (C), and

E) removing the solvents by distillation.

Another object of the present invention concerns a method of producing alkaline earth metal salicylates, which includes stages:

A) alkylation of salicylic acid α-olefin containing at least 14 carbon atoms, in the presence of a catalyst is a strong acid to form a soluble oil alkilirovanny Salic the gross acid;

In the interaction between soluble in oil alkilirovanny salicylic acid pre-treated with excess alkali detergent selected from the group consisting of high alkali sulfonates, Benatov or carboxylates of alkali or alkaline earth metals such as calcium sulfonate, leading to the formation of salts of salicylates of alkaline or alkaline earth metals with different percentages dispersed carbonate salts of alkali or alkaline earth metal.

Another object of the present invention relates musk alkaline earth metal produced by the process comprising the stages:

A) alkylation of salicylic acid linear α-olefin containing at least 14 carbon atoms, in the presence of a strong acid catalyst to form a soluble oil alkilirovanny salicylic acid;

C) neutralizing soluble in oil alkilirovanny salicylic acid;

C) excessive alkalizing soluble in oil alkilirovanny salicylic acid by carboxylation of lime,using CO2in the presence of an activator and a surfactant;

D) filtering the product of stage (C), and

E) removing the solvents by distillation.

Another object of the present invention relates musk deliciosamente the first metal, obtained by the process comprising the stages:

A) alkylation of salicylic acid linear α-olefin containing at least 14 carbon atoms, in the presence of a strong acid catalyst to form a soluble oil alkilirovanny salicylic acid;

In the interaction between soluble in oil alkilirovanny salicylic acid pre-treated with excess alkali detergent selected from the group consisting of high alkali sulfonates, Benatov or carboxylates of alkali or alkaline earth metals such as calcium sulfonate, which gives salicylate salts with different percentages dispersed carbonates of alkaline or alkaline earth metals.

Description of the preferred embodiments of the invention

As noted above, the first stage in the method according to this invention comprises the alkylation of salicylic acid linear α-olefins (C14or higher) to obtain alkylsalicylate acids with outputs that are acceptable for industrial production. In the conditions of alkylation are mainly monosubstitutedpair-alkylsalicylate acid, soluble in oil.

Alkylsalicylate acid derived from salicylic acid and linear α-olefins, using as catalyst a strong sour is, preferably anhydrous methansulfonate acid. Other strong acids that can be used include, for example, sulfuric, hydrochloric, nitric, triperoxonane, perchloro and the like. Reaction conditions are such that the suspension of salicylic acid in the olefin could react at a temperature of from 120 to 150°C. the Products are a mixture ofortho- andpair-monoalkylammonium salicylic acid with some dialkylamines and trialkylamines salicylic acids. The content of the alkylphenol is very low, and the color of the product is excellent compared with the color of the product obtained by synthesis of the Kolbe-Schmitt. Acid number of alkyl salicylates approximately 85-95% of their theoretical values. Values determined PDSC and test "panel coker", for the corresponding high-alkaline calcium salts of these salicylic acid is comparable with the data for the control of industrial salicylate detergents or surpass them.

Alkyl substituent or substituents, which contains alkylsalicylate acid used in this way, provide its solubility in oil. It is possible that alkylsalicylate acid may contain more than one, for example, two or three alkyl substituent, but preferably if it contains tol is to one such Deputy, and it ispair-position. Preferably, if the number of carbon atoms in the alkyl(s), the substituent(s) is at least 14 and preferably ranges from 14 to 30. When alkylsalicylate acid contains primarily only one alkyl substituent, most preferably, if the alkyl group contains from 14 to 26 carbon atoms. Alkyl(s) group(s) can be linear or branched, but the most preferred are linear.Suitable olefins include, but are not limited to, 1-tetradecene, 1-hexadecene, 1 octadecene, 1 achozen, 1 dokusen, 1 tetracosane, mixtures of the above olefins, and the like.

Industrially produced salicylic acid can be used without additional purification.

The conditions of the reaction depend on the nature of the olefin. Experts in the art should understand that various olefins can be and most likely will be desirable distinguished optimal reaction conditions.

The temperature at which conduct the interaction between salicylic acid and olefin is preferably 50°C or above and may, respectively, be in the range from about 50°C to about 200°C. the Optimum temperature in this interval depends on the length of the carbon chain of the olefin. Usually for C14 -olefin optimum temperature is from about 100 to about 150°C, for example about 120°C.

Duration of response is usually not essential. The reaction time is from about 2 to about 36 hours is usually satisfactory.

The reaction can be carried out in a solvent, if necessary, but usually the solvent is not used.

Alkylsalicylate acid may be extracted from the reaction mixture by methods known in the art. For (C14or above)alkylsalicylate acids typically use solvent extraction.

In the second stage of the method according to this invention are soluble in the oil, the acid is neutralized and excessively alkalinized by carboxylation of lime, using CO2in the presence of an activator, such as methanol, and surfactants, for example alkylsalicylate acid. The reaction mixture after excessive alkalizing filtered and the solvents removed by distillation.

Alternatively, alkylsalicylate acid can be subjected to interaction with the pre-treated with an excess of the alkali sulfonate of alkaline earth metal such as calcium sulfonate, obtaining salicylate salts of alkaline earth metals with different percentages dispersed carbonate salts of alkaline earth metals. In this way no F. is mitrofania the final product, and, therefore, it is preferable for the industry.

Detergents-alkaline earth metal salicylates obtained by the method according to this invention, in an appropriate case, include thedetergent is a calcium salicylate, detergent-magnesium salicylateor mixtures thereof.

The amount of added base should be sufficient to obtain high-alkaline salts, i.e. salts in which the ratio of the number of equivalents of the rest of the metal to the number of equivalents balance alkylsalicylate acid is usually greater than about 1.2, and may be 4.5 or higher.

Strongly alkaline alkaline earth metal salicylates can be obtained excessive alkalization neutral alkali earth metal salicylatewith the formation of carbonate of alkaline earth metal such as calcium carbonate and magnesium carbonate or borate of alkaline earth metal such as magnesium borate.

Base number of detergent musk metal is not specifically limited; however, the base number is usually from about 60 to about 350 mg KOH/g, preferably from about 150 to about 350 mg KOH/g

The base can add or at a time or add multiple intermediate points during the reaction.

In addition, high-alkaline reaction mixture contains, in the appropriate case, the activator, preferably CI is oradatabase organic solvent and, optionally, water. Suitable activators include C1-6-alcohols, polyhydric alcohols, such as glycol, propylene glycol, glycerin or 1,3-dihydroxypropane, ethers, such as simple C1-4monoether glycol or propylene glycol, simple diisopropyl ether, 1,3 - or 1,4-dioxane or 1,3-dioxolane. Preferably, when the activator is a C1-6-alcohol, in particular methanol.

The solvent for the reaction alkylsalicylate acid with a metal base can be

(1) a polyhydric alcohol containing 2-4 carbon atoms;

(2) di(C2-C4)glycol;

(3) three(C2-C4)glycol;

(4) simple alkilany ether mono - or polyalkyleneglycol formula

R1(OR2)xOR3,

in which R1means C1-C6alkyl group, R2means alkylenes group, R3means hydrogen or C1-C6alkyl group and x is an integer from 1 to 6;

(5) monohydroxy alcohol containing up to 20 carbon atoms;

(6) a ketone containing up to 20 carbon atoms;

(7) an ester of carboxylic acid containing up to 10 carbon atoms;

(8) volatile liquid hydrocarbon or

(9) a simple ether containing up to 20 carbon atoms.

The preferred solvent is an inert hydrocarbon, which may be either aliphatic or arene is political. Suitable examples include toluene, xylene, naphtha and aliphatic paraffins such as hexane and cycloaliphatic paraffins.

The combination of methanol, which acts as an activator of the reaction, and naphtha is especially preferred.

Taking into account the expected application of high alkaline products as additives to lubricating oils, preferably as an additional diluent base oil. The base oil may be an animal oil, vegetable or mineral oil. Preferably, when it is a lubricating oil obtained from petroleum, such as naphthenic base, paraffin base or mixed base oil. Alternatively, the lubricating oil may be a synthetic oil, such as synthetic ether complex or polymeric hydrocarbon lubricating oil.

Carbon dioxide used in the manufacture of alkali metal salts in the form of gas or solids, preferably in the form of gas, which can be bubbled through the reaction mixture. Carbon dioxide is usually added after addition of the base.

To obtain the alkali metal salt can be applied carboxylation catalyst. The specified catalyst may be either inorganic or organic compound, preferably near anicescu connection. Suitable inorganic compounds include the halides of hydrogen, halides of metals, halides of ammonium, alkanoate metals, alkanoate ammonium or formate or alkanoate di-, tri - or tetraalkylammonium. Examples of suitable catalysts include calcium chloride, ammonium chloride, calcium acetate, ammonium acetate, zinc acetate and the acetate of Tetramethylammonium. The catalyst is usually used in an amount of about 2 wt.%. A more complete description of the production of high-alkaline alkylsalicylate metals can be found in EP-A-0351052.

In an appropriate case, a higher temperature is used in the above reaction may be from about 100 to about 500°F (about 38° up to about 260°C).

Concentrate metal salt in the solvent can be removed by conventional means, such as distillation light ends. Finally, the concentrate can be filtered, if necessary.

In General, the method of obtaining high alkaline calcium salicylates includes the interaction of a solution of alkyl salicylic acids and, optionally, calcium sulfonate or sulfonic acid (for convenience, the subsequent discussion will concentrate on calcium compounds, but the usual experts in this field will readily understand that a similar method can be applied to compounds of magnesium, as well as mixtures of compounds of calcium and magnesium) in the asle with suspension oxide or calcium hydroxide and bubbling carbon dioxide through the reaction mixture, whereby the calcium salicylate is introduced excess of calcium carbonate and, if available, a calcium sulfonate, which provides the desired alkalinity of the product. In this way it was found that it is advantageous to add a low molecular weight alcohol, such as methanol, and water in order to accelerate the formation of a micellar dispersion of calcium carbonate.

When applied on an industrial scale calcium hydroxide as the sole agent of the reserve alkalinity in the reaction mixture, is used in large excess in order to achieve a high TBN (total base number) of the product.

Dispersing agent is an optional component of the method and product for high-alkaline detergent. One of the applicable dispersing agent is the reaction product hidrocarbonetos succinic acid or its anhydride with amines containing at least one nitrogen atom in a primary or secondary amino group, such as polyallylamine satisfy this requirement, as substituted polyamidoamine, and, in this case, ammonia. Bis-suktinimida also applicable as an optional dispersing agents. Bis-suktinimida get interaction hidrocarbonetos acid or its anhydride with an amine containing at least two primary and/or secondary nitrogen atom. Such bis-succinimide represent for example, polyisobutenyl-bis-suktinimida Ethylenediamine, Diethylenetriamine, or Triethylenetetramine, or Tetraethylenepentamine, or N-methyldiphenylamine etc. (e.g., Benoit, U.S. Patent No. 3438899). Various of the above-described dispersing agents can be used individually or in mixtures.

Strongly alkaline salicylate calcium present invention has an amorphous micellar structure. Strongly alkaline salicylate calcium or similar alkaline detergent is a stable dispersion of amorphous calcium carbonate.

Highly alkaline detergent is a calcium salicylate according to this invention can be added to the motor or lubricating oils in amounts of from 0.1 to 25 wt.% detergent or more.

This invention is applicable to a wide range of lubricating oils. The lubricating oil may be composed of one or more natural oils, one or more synthetic oils or mixtures thereof. Natural oils include animal oils and vegetable oils (e.g. castor oil, Lanovoi oil), liquid petroleum oils and hydrotreated treated with solvents or acids mineral lubricating oils of paraffinic, naphthenic and mixed paraffinic types. Oil with a viscosity of lubricants derived from coal or shale are also applicable as base oils.

Sin is eticheskie lubricating oils include hydrocarbon oils and halogen-substituted hydrocarbon oils, such as polymerized and copolymerizable olefins (for example, polybutylene, polypropylene, copolymers of propylene and isobutylene, chlorinated polybutylene, poly(1-hexene), poly(1-octene), poly(1-decene)); alkyl benzenes (e.g., dodecylbenzene, tetradecylbenzene, dinonylphenol, di(2-ethylhexyl)benzenes); polyfamily (e.g., biphenyls, terphenyls, alkylated polyphenols); alkylated diphenyl ethers and alkylated diphenylsulfide and their derivatives, analogues and homologues.

The polymers and copolymers of alkalisation and derivatives thereof where the terminal hydroxyl groups are modified by esterification with the formation of ester, esterification with the formation of simple ether and the like, constitute another class of known synthetic lubricating oils, which is illustrated by examples polyoxyalkylene polymers obtained by polymerization of ethylene oxide or propylene oxide, alkylamine and akrilovye ethers polyoxyalkylene polymers (for example, methyl simple air polyisopropylene having an average molecular weight of 1000, diphenyl simple ether of polyethylene glycol with a molecular weight of 500-1000, diethyl simple ether of polyethylene glycol with a molecular weight of 1000-1500); and esters of mono - and polycarboxylic acids, for example esters acetic acid is, mixed esters of C3-C8fatty acids and complex diesters With13exocyclic tetraethyleneglycol.

Another suitable class of synthetic lubricating oils comprises the esters of dicarboxylic acids (e.g. phthalic acid, succinic acid, alkylesters acids and alchemistry acid, maleic acid, azelaic acid, subernova acid, sabatinovka acid, fumaric acid, adipic acid, dimer of linoleic acid, malonic acid, allylmalonic acids, alkenylboronic acids) with a variety of alcohols (e.g., butyl alcohol, hexyl alcohol, dodecylamine alcohol, 2-ethylhexylamine alcohol, ethylene glycol, simple monoufia diethylene glycol, propylene glycol). Specific examples of these esters include dibutyltin, di(2-ethylhexyl)sebacate, di-n-sexyfemale, dioctylsebacate, diisooctylphthalate, diisodecylphthalate, dioctylphthalate,dodecylphenol, diacetylated, complex 2-ethylhexyloxy fluids dimer of linoleic acid, and the complex ester formed by the interaction of 1 mol sabatinovka acid with 2 mol of tetraethyleneglycol and 2 mol 2-ethylhexanoic acid.

Esters, used as synthetic oils also include esters, which are derived from C5-C12-monocarboxylic acids and polyols is polianovich ethers, such as neopentylglycol, trimethylolpropane, pentaerythritol, dipentaerythritol and tripentaerythritol.

Silicone oils, such as polyalkyl, polyaryl, polyalkoxy and poliarizatsionnoy oils and silicateoil,comprise another useful class of synthetic lubricants; they include tetraethylsilane, tetraisopropyldisiloxane, Tetra-(2-ethylhexyl)silicate, Tetra-4-methyl-(2-ethylhexyl)silicate, Tetra-(p-tert-butylphenyl)silicate, hexa-(4-methyl-2-pentoxil)disiloxane, poly(methyl)siloxanes and poly(were)siloxanes. Other synthetic lubricating oils include liquid esters of phosphorus-containing acids (e.g., tricresylphosphate, trioctylphosphine, diethyl ether decylphosphonic acid), and polymeric tetrahydrofuran.

Unrefined, refined and regenerated oil can be used in the lubricants according to this invention. Unrefined oils are the oils obtained directly from natural or synthetic source without additional purification. For example, crude oils can be a shale oil obtained directly in the process of cracking petroleum oil obtained directly from distillation process, or ester oil obtained directly after the esterification and used without complement Inoi processing. Refined oils are similar to the unrefined, except that they are further treated, subjecting the cleaned in one or several steps to improve one or more properties. Specialists in this field there are many cleaning methods, such as distillation, solvent extraction, extraction with acids or bases, filtering and straining (percolation filtration). Regenerated oil is produced by methods similar to those used to obtain refined oils, but they apply to oils that have been worked out. Such recovered oil is also known as recovered or reprocessed oils and often are additionally processed to remove the used additives and degradation products of oil.

This invention specifically relates to the formulation of engine oils and additives to them. The term " engine oil" in this application is used to refer to lubricating oil, which can be used as motor oil, for example, includes oil for automotive or diesel engines. Composition of lubricating oils according to this invention is also applicable for the lubrication of marine diesel engines, including a 4-stroke trunk piston engines and 2-stroke crosshead engines.

The oil should have a viscosity in the range of values the viscosity of lubricants, typically, from about 45 SUS (on a universal scale Saybolt) at 100°F to 6000 SUS at 100°F (about 38°C). Lubricating oil also contains one or more high alkaline detergents on the basis of alkaline earth metals, at least one of which is a containing a metal neutral or strongly alkaline salicylate-based alkylsalicylate acid, as described in this application. Components of detergent together comprise an effective amount, which is typically the amount from 0.01 wt.% up to 25 wt.%, preferably 0.1 to 10 wt.%, more preferably from 0.1 to 5.0%. Unless otherwise stated, all percentages are expressed as wt.% by weight of the entire composition of lubricating oils.

The amount of concentrate additives that should be contained in the finished lubricating oil depends on the nature of the application. For lubricating oils used in marine conditions, it is generally sufficient to provide a TBN of from 9 to 100; for lubricating oil in automobile engines enough, when TBN is from 4 to 20.

In this application, the term "total base number" or "TBN" refers to the amount of base equivalent to milligrams of KOH in 1 gram of the additive. Thus, the higher the TBN values indicate more alkaline foods and, consequently, a larger supply of alkalinity. Total base number (TBN) is easily determined by test method D2896 p the ASTM or other equivalent methods.

The finished lubricating oil may also contain effective amounts of conventional additives to lubricating oils, one or more types, for example additives which improve the viscosity index, anti-wear agent, antioxidant, dispersing agent, a corrosion inhibitor, an agent lowering the freezing temperature and the like.

Benefits and significant features of this invention will be more clear from the examples below.

EXAMPLES

Example 1

The alkylation of salicylic acid

Salicylic acid (215,0 g) placed in a glass reactor with a volume of 3 l equipped with a stirrer, thermometer and a heating jacket. Add a mixture of C14-C18-olefins (367,7 g)followed by alkylation catalyst, such as methanesulfonate acid (45.1 g). The mixture is heated to 120°C and kept at this temperature for 24 hours Then injected white spirit (582,6 g) and transparent solution is allowed to settle to remove the spent catalyst. The extracted product is a yellowish alkylsalicylate acid, dilute yellowish white spirit, suitable for direct excess alkalizing or to interact with the pre-treated high-alkaline detergent.

Example 2

Receipt is salicylate calcium

In the reaction vessel, which contains 20 g of white spirit, 15 g of base oil and 20 g of methanol, add 35 grams of calcium sulfonate with a TBN 500. Once thoroughly mixed, slowly add 100 g alkylsalicylate acid, described in example 1, and increase the temperature to 420°F (about 216° (C) within the next 2 hours After the distillation of light fractions salicylate calcium is a light and transparent product with a viscosity of 45 CST, TBN 170 and the percentage calcium content of 6.1%.

The product of example 2 have the PDSC method (differential scanning calorimetry under pressure) and determine the induction time 109 minutes For the corresponding sulfonate calcium induction time OIT is less than 30 minutes

The same product have ability at high temperature, using the test panel coker", and find it gives 3.5 mg of sediment. The corresponding alkali sulfonate used as the source of the base (CaCO3in the above reaction, give 75 mg of sediment.

The test panel coker is a method to determine the tendency of the oils to form a solid decomposition products upon contact with surfaces at elevated temperatures. This test can be carried out using the apparatus Falex Panel Coking Test Apparatus, which is used to test Federal Test Standrd 791 B, Method 3462.

Example 3

Getting salicylate calcium

The reactor is placed one hundred and forty grams of alkylsalicylate, obtained as described in example 1, then add 50 g of base oil, 220 g of white spirit, nine grams of methanol, 7.5 g of a neutral calcium sulfonate and 23 g of slaked lime. The mixture is heated to 140°F (60° (C) and enter the CO2up until the lime will not turn into CaCO3. The reaction mixture is filtered and distilled, receiving liquid bright and clear detergent is a calcium salicylate.

PDSC testing showed that OIT is 140 minutes, while the test panel coker showed great ability at 8.5 mg of sediment.

Example 4

Getting salicylate calcium

Comparative example

Interaction alkylsalicylate acid with alkali-sulfonate requires adherence to certain conditions, otherwise produces undesirable crystalline calcium carbonate. Reaction conditions shown below, give the final salicylate, which contains CaCO3mainly in the form of Wouter.

Conditions identical to the conditions of example 2, except that the composition consisted of 20 g of water, in addition to 20 ml of methanol. Increased polarity destabilize the colloid-SAC and has resulted in the transformation of amorphous soluble in m the following CaCO 3in the crystal vaterite. The final product was a viscous, very muddy and not suitable for use.

Whereas numerous changes and modifications can be made without deviation from the principles underlying this invention, reference should be made to the accompanying claims for an understanding of the scope of protection afforded by this invention.

1. The method of obtaining alkyl salicylates of alkaline earth metals, including stage A) alkylation of salicylic acid linear α-olefin containing at least 14 carbon atoms, in the presence of anhydrous methanesulfonic acid with the formation of soluble oil alkilirovanny salicylic acid;

B) neutralizing soluble in oil alkilirovanny salicylic acid;

C) excessive alkalizing soluble in oil alkilirovanny salicylic acid via carboxylation of lime with CO2in the presence of oxygen-containing organic solvent and a surfactant;

D) filtering the product of stage (C), and

E) removing the solvents by distillation.

2. The method according to claim 1, in which stage alkylation is carried out at a temperature of from about 50 to about 200°C.

3. The method according to claim 1, in which linear α-ol the fin is chosen from the group consisting of 1-tetradecene, 1-hexadecene, 1 octadecene, 1 eicosene, 1 docosane, 1 tetracosane and mixtures thereof.

4. The method of obtaining alkyl salicylates of alkaline or alkaline earth metals, including stage A) alkylation of salicylic acid linear α-olefin containing at least 14 carbon atoms, in the presence of anhydrous methanesulfonic acid with the formation of soluble oil alkilirovanny salicylic acid;

B) interaction between soluble in oil alkilirovanny salicylic acid pre-treated with excess alkali detergent selected from the group consisting of high alkali sulfonates, Benatov or carboxylates of alkali or alkaline earth metals, with the formation of salts, salicylates of alkaline or alkaline earth metals with different percentages dispersed salts of carbonates of alkaline or alkaline earth metals.

5. The method according to claim 4, in which the phase alkylation is carried out at a temperature of from about 50 to about 200°C.

6. The method according to claim 4, in which linear α-olefin selected from the group consisting of 1-tetradecene, 1-hexadecene, 1 octadecene, 1 eicosene, 1 docosane, 1 tetracosane and mixtures thereof.

7. The method according to claim 4, in which stage the excess alkalizing carried out in the presence of oxygen-containing organic the definition of solvent.

8. The method according to claim 4, in which pre-treated with excess alkali detergent obtained by excessive alkalizing neutral alkaline earth metal carboxylates via carboxylation of lime with CO2in the presence of oxygen-containing organic solvent and a surfactant.



 

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< / BR>
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FIELD: chemistry.

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7 cl, 2 dwg, 3 ex, 1 tbl

FIELD: chemistry.

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10 cl, 4 ex

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3 cl, 1 tbl, 3 ex

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2 cl, 1 tbl, 1 ex

FIELD: chemistry.

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5 cl, 1 tbl, 14 ex

FIELD: chemistry.

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2 cl, 1 tbl, 8 ex

FIELD: chemistry.

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2 cl, 17 ex, 2 tbl

FIELD: organic compounds technology and industrial ecology.

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13 cl, 5 ex

FIELD: organic chemistry.

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EFFECT: accelerated process with reduced cost and increased effectiveness.

1 tbl, 9 ex

The invention relates to the production of acetic acid and/or methyl acetate

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