Novel additives to transmission oils

FIELD: chemistry.

SUBSTANCE: invention relates to microcapsules, containing borates of alkali metals, method of their obtaining, as well as to lubricating oils, used as transmission lubricating materials, containing said microcapsules as anti-scuffing and/or anti-wear additives. Microcapsules include core, containing one or more of borates of alkali metals, possibly hydrated, dispersed in one or more basic lubricating oils of mineral, synthetic or natural origin, and polymer envelope. Microcapsules are obtained by method of on-surface polymerisation.

EFFECT: invention makes it possible to obtain microcapsules, containing borates of alkali metals, which make it possible to avoid phenomenon of crystallisation of borates of alkali metals in presence of water, and therefore, makes it possible to use lubricating composition, containing thereof, use, for instance, in gearbox, which does not have sealing system.

24 cl, 1 tbl, 3 ex

 

The technical field

The object of the present invention relates to new Borisovna, EP additives, useful, for example, for gear lubricants. These additives provide a transmission with a very effective protection from the phenomenon of pitting corrosion, and increased resistance to water.

Prior art

Transfer vehicles often operate under heavy load, so lubricants for transmissions contain EP additives (PP), which protect the friction surfaces, chemically forming a protective layer adsorbed on the surface.

In particular, lubricants for gearboxes play a role of increasing the resistance of the gear teeth against pitting corrosion, which is a typical cause of fatigue damage occurs due to repetitive strain under high load.

Pitting occurs after a long period of aging and precedes the visible destruction.

The mechanisms are poorly known, but the phenomenon begins with the appearance of cracks at a certain depth below the surface, these cracks propagate, and, when the formation of normal cracks on the surface, there is a sudden crushing of the material. The prevention of this phenomenon involves the reduction of con the akt stress using the appropriate geometry of the parts and the reduction of friction by preventing adhesion.

The lubricant is involved in this process prevent due to its viscosity and physicochemical reactivity of its additives. Specifications for transmission oils are extremely demanding with respect to resistance to pitting corrosion.

EP additives used in gear oils may be compounds containing sulfur, phosphorus, sulfur and phosphorus, nitrogen and sulfur, chlorine, boron, such as sulfurized olefins, phosphates, dithiophosphate, dithiocarbamate, hydrated borates of alkali metals.

The most common anti-wear additives which are commonly used are compounds containing sulfur, phosphorus or sulfur, and phosphorus. However, the hydrated borates of alkali metals are also used in the compositions transmission oils as EP additives, because they have a great ability to withstand load, and good heat resistance.

Acceptable temperature range for borates is much wider than for the sulfur-phosphorus compounds (from 0°C to 150°C), and currently no single technology with the use of sulfur -, phosphorus-or sulfur-phosphorus additive is not possible to achieve a level of performance that is achieved with the help of borates from the point of view of protection against pitting corrosion. As a result, the ATA, when the transmission oil containing borates as additives, are used in transmissions, gear teeth is not necessary to undergo expensive surface treatment to enhance their inherent resistance to pitting corrosion.

Borates act as a non-sacrificial film on the friction surfaces being deposited by electrodeposition. In addition, due to the reaction of borate with succinimido from the environment or with nitrogen, which is part of the material of the teeth can be formed (in extreme conditions of pressure and temperature) tribochemical film of boron nitride. As the electrodeposition and tribochemical film protects the surface during extreme contact pressures.

In addition to these excellent properties, as PP borates also have good resistance to oxidation, odorless, not toxic and does not react with elastomeric seals (which avoids the problems of leaks) and is not aggressive towards metals.

Borates are used as extreme pressure additives in lubricants usually are in the form of a crystalline solid nanospheres with a diameter mainly in the range from 1 to 300 nm, dispersed in an oil matrix by using surface-active substances.

Despite the excellent characteristics in terms of e is Strekalova pressure and its many benefits, the use of borates, however, is not desirable when there is a risk of contamination of the lubricant with water. As inorganic borates partially soluble in water, the amount of water contained in the molecule may increase, which will lead to a change in the structure of borate. In the presence of a large amount of water in the environment borates modified as a result of this structure can crystallize and form lamellar crystals larger than 100 microns.

If the phenomenon of crystallization, the proportion of spherical borates decreases, the proportion and size of crystals increases and the quality of borates from the point of view of antiwear and extreme pressure properties is reduced. In this case, the borates may even clog the system synchronization transmissions. It is therefore necessary to protect the borates from the water to fully guarantee their mechanical properties and to prevent jamming of the transmission.

One solution, for example, may consist in adapting the transmission accordingly by creating sealing systems, but this entails additional difficulties for manufacturers.

Problem sensitivity borrowing oils to the water are well known in the art and have never been fully resolved, despite an improvement.

The main work on the costumes is notowania focused on environmental borates medium (dispersant, detergents, friction modifiers, and so on) in order to restrict the flow of water in the core of supplements or changes to their degradation kinetics.

Application EP 0976813, for example, discloses compositions additives PP gear oils containing from 30 to 70 wt.% hydrated borates of alkali metals, from 10 to 30% of organic polysulfides, from 1 to 20% alkylacrylate ether of a polyhydric alcohol, from 0.5 to 20% coronaves sulfonated salicylates detergent or verhoeve sulfonated salicylate-phenolate mixture and possibly up to 20% of ester of fatty acid and polyhydric alcohol.

Application EP 1298191 discloses lubricating compositions comprising hydrated borates of alkali metals, dispersed in the base oil and the mixture of dispersant comprising a dispersant based polyalkylacrylate and salt polyisobutenylsuccinic and any metal.

The document US 2007/145326 describes compositions intended for heat production and including the coating layer and the core, including the matrix and agent generates heat, and heat-emitting agent is surrounded by a hydrophobic wax.

However, existing borates with dispersant and specific friction modifiers do not prevent the formation of lamellar crystals in the presence of water, which means that they still can't get IP is to olsavica gearboxes, not covered by the sealing system. There is therefore a need for new solutions to protect the borates from the water in the lubricating compositions.

The aim of the invention is to solve this problem by microencapsulation of borates in microparticles incorporating a protective shell.

Microencapsulation is a process by which the product is hollow microparticles, comprising a shell or membrane (usually polymer), surrounding a solid or liquid core containing the specified product. These particles, whose diameter is usually from 0.1 to 1000 μm are indicated by the term "microcapsules".

Depending on the encapsulated molecules have applications in agriculture (fertilizers, pesticides), healthcare (medicine), cosmetics, and textiles.

Application WO 2008/151941, for example, discloses a method of production of microcapsules having a core consisting of a liquid hydrocarbon and wax, surrounded by a polymeric membrane, made of acrylic resin or resin type of aminoplast. In this application also provides numerous possible applications for microcapsules.

In the publication M. Masuko et al. / Tribology International 41 (2008), 1097-1102 also described the production of microcapsules containing anti-wear additive used in lubricants, namely dialkyldithiophosphate zinc, to increase the sustainability of this is th additives to oxidation.

Patent US 5112541 also describes the microencapsulation of lubricants and soluble in oil additives.

However, all methods known from the previous level techniques to obtain these microcapsules, using the stage of formation of the emulsion of a hydrophobic oil phase, for example, lubricating oils, possibly containing additives, which is dispersed in the aqueous medium, and then polymerized at the interface oil/water.

Get containing borates microcapsules using these known methods is not desirable, because the very purpose, which is achieved by microencapsulation, here is the protection of borates from the water. The implementation of the methods known from prior art, as in our case would lead to a change in the structure of borate crystals when in contact with water, which would make them unsuitable for use as extreme pressure additives in lubricants, in particular gear oil.

Methods of surface polymerization according to the prior art are not generally suitable for the preparation of microcapsules, including:

a core containing a hydrophobic phase and additives, and

polymer shell,

if the characteristics of these additives deteriorate under the action of water.

There is therefore a need for methods that allow p in order to obtain microcapsules, which include a polymer membrane and a core containing a hydrophobic phase and additives, without the use of the aqueous phase, thus, to protect these additives from degradation under the action of water. This method is a further object of the invention.

Brief description of the invention

The object of the present invention relates to microcapsules, including:

- the core containing one or more than one alkali metal borate, possibly hydrated, dispersed in one or more than one mineral, synthetic or natural base oil, and

polymer shell.

Preferably borates of alkali metals contained in the core of the microcapsules, are compounds with the General formula:

MO1/2mBO3/2nH2O(1)

where M is alkali metal, preferably sodium or potassium, m is a number from 2.5 to 4.5 is n - number from 0.50 up to 2.40, and a Monomeric repeating unit of the formula (I) may be repeated several times.

Preferably the polymer, which is part of the shell, which are selected from polyesters, polyurethanes, polyamides, politician or their copolymers, polyacrylonitrile, vinyl resins or aminoplastic resins, preferably from politician.

According to one embodiments of the invention, these microcapsules have a diameter of from 0.1 to 50 μm, preferably from 0.1 to 1 micron.

Preferably, the borate contained in the core of the microcapsules are nanospheres having a diameter of 1 to 300 nm, preferably from 10 to 200 nm, preferably from 20 to 40 nm.

Preferably the core contains, in addition, soluble in oil dispersant selected from sulfonates, preferably polyisobutenylsuccinic, salicylates, sulfonated or desulfuromonas, naphthenates, reaction, sulfonated or not sulfonated, polyalkyleneglycol, preferably of polyisobutenylsuccinic, amines or Quaternary ammonium salts, individually or in a mixture.

The next subject of the present invention is a lubricating oil comprising microcapsules, such as described above.

Preferably, the lubricating oil contains an amount of boron measured in accordance with standard NFT 60-106 of 500 to 5000 M. D. (mi the million shares) in weight.

This lubricating oil can, in addition, contain:

- one or more than one anti-wear or EP additive, preferably selected from organic polysulfides, phosphates, phosphites, demercaptanization, benzotriazoles, and/or

- one or more than one friction modifier, preferably selected from monoamino polyols and fatty acids.

The next subject of the present invention is the use of lubricating oils, such as described above, as the transmission oil, preferably as a lubricant for gearboxes or axles.

The next subject of the present invention is a method of preparation of microcapsules using surface polymerization, in which the hydrophobic phase, denoted by S1, containing the first monomer, denoted by M1, and one or more than one additive is dispersed in the dispersion medium formed by the non-aqueous organic solvent, denoted by S2, is not miscible with the above hydrophobic phase, and containing either the initiator, enabling the chain polymerization of M1, or the monomer M2, leading to polycondensation with M1, resulting in the formation of polymers or copolymers constituting the shell of the microcapsules.

Preferably, the method of manufacturing microcapsules involves the following stages:

(1) dissolution of monomer M1 in the hydrophobic phase S1, including the surrounding one or more oils, waxes or lubricants mineral, synthetic or natural origin, as well as one or more of the additives

(2) the formation of a dispersion of the mixture obtained in stage (1), in a dispersion medium comprising a solvent S2 and possibly one or more of surfactants,

(3) adding to the said dispersion medium initiator, enabling the chain polymerization of M1 or monomer M2, leading to polycondensation with M1, resulting in the formation of polymers or copolymers constituting the shell of the microcapsules.

According to one of embodiments a solvent S2 - polar aprotic solvent having a dielectric constant higher than 25, preferably greater than 30.

Preferably the solvent S2 is chosen from dimethyl sulfoxide (DMSO), 1-methyl-2-pyrrolidone, acetonitrile, formamide, methylformamide, dimethylformamide, ndimethylacetamide, methylacetamide, dimethylacetamide.

According to one embodiments, the dispersion of the hydrophobic phase in the dispersion medium is carried out using one or more of surfactants, preferably in the solvent S2.

Preferably, these surfactants are nonionic surfactants with a hydrophilic-lipophilic balance of from 10 to 15. Preferably you who eraut among fatty alcohols, fatty amines, fatty acids, esters of fatty acids and one or polyhydric alcohols, and these connections are or are not ethoxylated, preferably ethoxylated oleic acid, ethoxylated with christianforum, hexanolactam of polyoxyethylenesorbitan.

According to one of embodiments of the hydrophobic phase S1 includes borates of alkali metals, possibly hydrated, dispersed in one or more than one lubricating oil mineral, synthetic or natural origin.

The monomers M1 and possibly M2 are preferably at least bifunctionality monomers, preferably di - or trifunctional.

According to one embodiments the initiator, enabling the chain polymerization of M1, dissolved in stage (3).

According to another embodiment, the monomer M2 is dissolved in stage (3). In this last embodiment, M1 is preferably dichlorsilane acid or diisocyanate, and M2 is diola or diamine.

The next subject of the present invention, a technique such as described above, the manufacture of microcapsules in accordance with the invention.

The next subject of the present invention is the use of microcapsules, such as described above, as antiwear and/or extreme pressure additives for lubricating whom is Azizi.

Detailed description

Microcapsules

The term "microcapsule" means hollow microcapsules comprising a shell or membrane (usually polymer), surrounding a solid or liquid core containing the active substance must be protected and released in a controlled way. These microparticles having a diameter typically less than 1000 μm, in particular from 0.1 to 1000 μm, collectively referred to as microcapsules.

Microcapsules in accordance with the invention have approximately spherical shape. When talking about the diameter or size of the microcapsules, I mean their greatest dimension. The diameter of the microcapsules in accordance with the invention is preferably from 0.1 to 50 μm, more preferably from 0.2 to 10 μm, or from 0.1 to 1.5 microns, or from 0.3 to 4, or from 0.4 to 3, or from 0.1 to 1 μm. Preferably, the microcapsules were homogeneous in size. It is also desirable that the preferred homogeneous size was of the order of several hundreds of nanometers, typically less than 4 microns, for example less than 3 μm, in particular less than 1 or 2 microns, in order to facilitate the introduction of their suspension in the lubricating oil, which must be included as additives.

Taking into account the size of the spherical particles borates, which must be entered in the capsule, which is of the order of at least several tens of nanome is s, it is difficult to obtain microcapsules of less than 0.1 μm, even less than 0.2 μm, effectively including borates.

The size of the microcapsules can be measured by observation using optical microscopy with a magnification of about 1000 or using other methods known to experts in this field.

The nucleus

The core of the microparticles in accordance with the present invention includes borates of alkali metals, possibly hydrated, usually in the form of solid nanospheres dispersed in one or more than one lubricating base oil.

Borates

Borat is salt electropolishing connection with boron-oxygen compound, possibly hydrated. You can mention the example salts of borate ionsBO33-and ions metaborateBO2-. Ion BoratBO33-can give different polymer ions, for example, ion triborateB3O53-, ion tetraborateB O72-, pentaborate and so on

In this application, the term "borate" shall mean the borates of alkali metals, possibly hydrated. Preferred are compounds which can be represented General formula:

MO1/2mBO3/2nH2O(1)

where M is alkali metal, preferably sodium or potassium, m is a number from 2.5 to 4.5 and n is a number from 0.5 to 2.4. This Monomeric repeating unit of the formula (I) may be repeated several times.

Borates of sodium or potassium are preferred for use in transmissions, as they are more resistant to water. In particular, the preferred borates of sodium or of potassium-related items metal/boron from about 1:2.5 to 1:4.5 or 1:2.75 to 1:3.25 to, preferably about 1:3 and, in particular, triborate the Aliya with the formula KB 3O5·nH2O.

To prepare the borates in the form of additives that can be easily used in lubricating compositions create a suspension of solid nanospheres amorphous borate, for example, having a diameter from about 1 to 300 nm, dispersed in oil based greases the dispersant, which can be suktinimida, sulfonates, etc.,

Typically, these spheres have a diameter of between approximately 10 and 200 nm, typically less than 100 nm, or less than 50 nm, preferably from 20 to 40 nm.

These dimensional characteristics can be measured, for example, using optical microscopy with a magnification of about 1000 or using other methods known to experts in this field.

Additive for gear oils containing sphere of triborate can be obtained, for example, by emulsification of an aqueous solution of K2B4O·4H2O and KB5O8·4H2O in mineral oil, stabilized by a dispersant based succinimide and calcium sulfonate.

Evaporation of water at 150°C gives borates in their solid form. The viscosity and polarity of the additive, thus obtained, is equivalent to the viscosity and polarity of the oil environment in which to prepare a dispersion.

Obtaining dispersions of borates that can form the core of the microcapsules in accordance with the invention, are described, for example, in C the turnout EP 1298191, paragraphs[0064]-[0066].

Typically, these dispersions contain from 5 to 10 wt.% or even 15 wt.% elemental boron, measured according to the standard NFT 60-106.

Dispersers

The core of the microcapsules in accordance with the present invention contains a borate dispersed in one or more mineral, synthetic or natural base oil. To atomized borates in the microcapsules of the present invention, it is possible to use any dispersant known to experts in the field of lubricating oils.

Examples of dispersing agents that can be used in the present invention, is described under the title "surface active agents" US patent 2987476 (column 3, line 35 to column 9, line 12). They are anionic compounds, such as, for example, soluble in oil, salts of organic acids containing at least 8 carbon atoms, sulfonates, reaction, salicylates, naphthenate, preferably salts of alkali and alkaline earth metals or salts of amines. They can also be cationic compounds, such as organic amines, imides or Quaternary ammonium salt. These compounds can be used singly or in a mixture.

Compounds containing nitrogen, in particular, type suktinimidov, show a synergistic effect with borates, as they contribute to the formation of a lubricating plait the key of boron nitride, which enhances the activity of borates in relation to the reduction of friction and extreme pressure. In the present invention, preference is given to the microcapsules, the core of which contains at least one dispersant operations type.

Application EP 1298191, for example, describes the dispersion of borates in the lubricating oil is prepared using a mixture of dispersant type polyalkyleneglycol, in particular, polyisobutenylsuccinic (PIB of succinimide) and metal salts polyisobutenylsuccinic.

Application EP 0976813 describes compositions based on borates in the lubricating oil comprising as a dispersant reaction products of polyhydric alcohols or of pentaerythritol with PIB-succinimido and alkylsalicylate and sulfonated alkylphenolate.

The compounds can also be used as a dispersant in the core of the microcapsules in accordance with the present invention.

Lubricating oil

The lubricating oil acting as a medium to obtain nanospheres borates, can be any lubricating base oil of a mineral, synthetic or natural origin. Commercially available dispersions are usually prepared in the mineral base oils of group 1, for example of the type 150 NS, but it is possible, for example, to use mineral foundations are a group II or III, synthetic bases type polyalphaolefin the new or esters, fundamentals of natural origin, for example containing methyl esters of fatty acids, and so on, or any other basis that is adapted for such use.

For the purposes of microencapsulation preference is given to dispersions in which the amount of base oil is minimal, in order to increase the efficiency thus obtained additives. Commercial dispersions contain base oil in the range of 35 wt.%. Preference is given to dispersions containing not more than 35 wt.% one or more base oils, preferably not more than 25 wt.%, more preferably not more than 20 wt.% and, further preferably not more than 15 wt.% base oil.

Polymer shell

The advantage of the microcapsules is the presence of a protective shell that isolates the active substances from the external environment, providing controlled release, in particular, by breaking the shell.

The shell of the microcapsules according to the invention is intended to protect the borates from the water, which can, eventually, get into gear oil during operation.

In the microcapsules in accordance with the invention, it is desirable to obtain not progressive diffusion of borates through the walls of the shell, and the release of borates on the border of the metal-metal. Therefore, it is not desirable that the borates would be released in the e, than at rupture of microcapsules under strong pressure, of the order of GPA, existing in the contact area.

Therefore, it is desirable that the shell of the microcapsules were Malopolskie formed polymer with a large number of cross-links. Therefore, to obtain microcapsules according to the present invention, it is preferable to use di - and trifunctional monomers, i.e. monomers containing multiple functional groups involved in the polymerization reaction.

It is also desirable that the polymer constituting the shell of the microcapsules in accordance with the invention, had a high heat resistance (i.e., not destroyed at high temperatures to which they will be subjected during operation, i.e., 150-160°C), and high mechanical strength, to be able to withstand high levels of mechanical stress to which they are exposed in transmissions.

The shell of the microparticles in accordance with the invention can be formed by polymer type, polyesters, polyamides, polyurethanes, polyureas, their copolymers, possibly with other monomers, polyacrylonitrile, vinyl resins or aminoplastic resins obtained by the condensation of urea and formaldehyde, etc.

Particularly preferred polyurea, known for its good water resistant properties. They are also about the present good mechanical resistance and good heat resistance.

The shell of the microcapsules according to the invention will be most effective if it will consist of a polymer material, characterized by insolubility in water or hydrophobicity. The specified connection is not able to interact with water and, in particular, to create hydrogen bonds with water. This, in particular, the above-mentioned polymers and most polymers produced from hydrocarbon derivatives. Some polymers of unsaturated carboxylic acids, in particular polymers of acrylic and methacrylic acid, should be avoided because of their ability to form gels with water. Preference is therefore given to the microcapsules, the shell of which contains at least one hydrophobic polymer.

Microcapsules according to the invention can be used as antiwear and extreme pressure additives in lubricating compositions, in particular gear oils, particularly oils for gearboxes and axles, preferably mechanical gearboxes and axles of heavy vehicles. In operation, the shell of the microcapsules protects borates from water that may be present in oily environments. Borates are released at the boundary of metal-metal, where the pressure is very high (HPa), and then play their usual role as EP additives, forming a square the GCC on the surface of the rubbing parts.

Gear lubricating oil

The next subject of invention relates to lubricating oils comprising the above microcapsules.

Microcapsules according to the invention can be included in the composition of the oil in different quantities depending on the method of use and quantities contained in them hydrated borates.

Lubricating compositions containing microcapsules according to the invention are used in particular as a lubricant for the transmission of light or heavy vehicles, more preferably for gearboxes, axles and, further, it is preferable for manual transmissions and axles of heavy vehicles.

As a rule, in the lubricating compositions for transmissions the weight percent of these microcapsules is selected so that the weight in terms of elemental boron in the transmission oil, measured according to NFT 60-106, was between 500 and 5000 M. D., preferably between 1000 and 3000 M. D., or between 1500 and 2800 M. D., preferably about 2500 M. D.

Other additives

Lubricating compositions in accordance with the invention can also contain any kind of additives, adapted for use in them, in particular, other antiwear and extreme pressure additives, friction modifiers, antioxidants, detergents, dispersants, corrosion inhibitors, etc.

Against the see wear and EP additives

These additives are often sulfur, phosphorous and sulphur-phosphorus compounds, for example, dithiocarbamate, thiadiazole, dimercaptotoluene, benzothiazole, organic polysulfides, in particular sulfonated olefins, in particular trisulfide, alkylphosphate or alkylphosphonate, phosphoric acid, phosphorous acid, mono-, di - and treatery of phosphorous acid and phosphoric acid and their salts, tiofosfornoy acid, thiophosphoric acid, esters of these acids and their salts and dithiophosphate etc.

All these compounds can be used singly or in a mixture in lubricating compositions according to the invention.

Friction modifiers

This is, for example, fatty alcohols, fatty acids, fatty amines, esters, in particular esters of fatty acids and polyhydric alcohols, such as monooleate pentaerythritol, phosphites or phosphates, already mentioned above as antiwear and extreme pressure additives.

Gear oils according to the invention can also contain enhancers viscosity index, for example, polymethacrylates, in particular low molecular weight, thickeners, for example, type polyisobutene, antioxidants, for example, amino or phenolic, etc.

Method of manufacturing microcapsules

Numerous methods for the manufacture of microcapsules containing polymer oblock and solid or liquid core by coating or spraying in a fluidized bed, surface polymerization in a dispersion medium, whether by radical polymerization or polycondensation. For radical polymerization is one of the phases contains dissolved monomer and another initiator, and polycondensation of one of the monomers dissolved in the dispersion medium, and the other in the dispersed phase.

Known methods of producing microcapsules by means of surface polymerization in a dispersion medium using oil-in-water emulsion. These methods cannot be applied here, because the addition of water in the environment will lead to the degradation of borates, the phenomenon that just want to avoid by imprisonment in a polymer shell. The receive mode of hydrated borates of alkali metals, dispersed in the lubricating oil, of an aqueous solution of borates includes a stage controlled evaporation of water. Repeated addition of water in a method of encapsulating these borates would lead to undesirable changes initially formed crystals.

The object of the present invention is a method of producing microcapsules by means of surface polymerization, in which the hydrophobic phase, denoted by S1, containing the first monomer, denoted by M1, and one or more additives, dispersed in the dispersion medium formed by the non-aqueous organic solvent, denoted by S2, is not smeshivaliss the specified hydrophobic phase containing initiator, allow to pass the chain polymerization of M1, or the monomer M2, leading to a polycondensation reaction with M1, with the formation of polymers or copolymers, which are a part of the shell of the microcapsules.

Methods of production of microcapsules according to the invention preferably include the following stages:

(1) dissolving an oil-soluble monomer M1, the precursor of the polymer constituting the shell of these microcapsules in a hydrophobic phase, S1, containing one or more oils, waxes or fats mineral, synthetic or natural origin, and possibly one or more additives, for example dispersed hydrated borates of alkali metals,

(2) formation of a dispersion (or emulsion) of the mixture obtained in stage (1), in the dispersion medium, comprising a non-aqueous solvent S2, is not miscible with the hydrophobic phase S1,

(3) adding to the said dispersion medium S2 or initiator that allows you to undergo chain polymerization M1 or monomer M2, leading to a polycondensation reaction with M1, with the formation of polymers or copolymers, which are a part of the shell of the microcapsules.

The obtained microcapsules can then be filtered and possibly subjected to one or more stages of washing.

Hydrophobic phase S1

Hydrophobic phase S1 can switch the th one or more oils, waxes, fats, mineral, synthetic or natural origin, alone or in a mixture.

S1, for example, may include one or more mineral, synthetic or natural lubricant base oils, such as mineral base oil Group I type 150 NS or mineral base oil group II or III, a synthetic base oil type poly-alpha-olefins or esters, base oils of natural origin, for example, containing methyl esters of fatty acids, singly or in mixtures, etc., or any other base oil or a mixture of lubricating bases adapted for such use.

S1 may include mineral waxes, for example, including n-paraffins derived from petroleum sources, or synthetic waxes obtained by Fischer-Tropsch synthesis, or natural waxes, for example beeswax.

S1 may also contain fats, obtained by dispersion of a thickener, which may be, for example, soap-based metal salts of fatty acids, simple or complex, or inorganic thickening agent, one or more lubricating bases, such as, for example, described above.

This hydrophobic phase contains one or more additives, which may be soluble or dispergirovannykh in the hydrophobic phase by using a dispersant. For example, it can be additive for asiausa compositions or lubricants, for example, those used in the automotive industry, for example, for engines or transmissions, marine applications, industrial applications. For example, and in particular, it borates, such as described above.

The method according to the invention allows to protect these additives from the water.

Preferably hydrophobic phase S1 contains one or more mineral, synthetic or natural lubricating base oils and borates of alkali metals, possibly hydrated, dispersed in the lubricating oil (oils).

The solvent S2

The solvent S2, forming a dispersion medium in the method according to the invention, should not be mixed with the hydrophobic phase S1.

This can be achieved through the use in the method of surface polymerization according to the invention as a solvent S2 polar solvents, preferably having a dielectric constant higher than 25, more preferably above 30.

The polar nature minimizes the interaction with the hydrophobic phase, in particular, lubricating oils, preferably used as a medium for dispersion of borates with the formation of the cores of the microcapsules in accordance with the invention, most of which are non-polar.

Solvents having a dielectric constant higher than 25 and FAV is preferably above 30, form the most stable emulsions with hydrophobic oil phase.

These solvents are preferably aprotic. The result aprotic nature is that they do not lead to degradation of borates.

Examples of solvents S2, appropriate to the method of the present invention are dimethyl sulfoxide (DMSO), 1-methyl-2-pyrrolidone, acetonitrile, formamide (metaname), methylformamide, dimethyldecanamide (dimethylformamide), ndimethylacetamide, methylacetamide, dimethylacetamide. Preferably acetonitrile is used, as it can give a very stable emulsion with the oil.

The monomers M1 and M2

The methods according to the invention generally relate to methods in which the polymerization is carried out either by the mechanism of chain polymerization with an initiator, which can be a source of free radicals (e.g., peroxide) or a carbanion, or carbocation, or by polycondensation method.

The monomers M1 (and possibly M2 in the methods of polycondensation) are preferably di - or trifunctional monomers, i.e., each of them includes two or three reactive functional groups involved in the polymerization reaction, possibly different, preferably identical, in one molecule.

This ensures the formation of polymers with high molecular weight, adapted to the formation of micron the purs in accordance with the invention, and increases the degree of crosslinking, which reduces the porosity of the shell. Monofunctional monomers can reduce and even stop the growth of polymer chains before they reach a length suitable for the formation of capsules, while the monomers, including an excessive number of reactive functional groups, lead to a very rapid growth in molecular weight of the resulting polymer, which can precipitate before the formation of the capsules. Specialists in this field, therefore, will choose the number of functional groups of the polymer according to these principles.

In the present invention, the preferred methods of surface curing via polycondensation. They, in particular, allow to obtain microcapsules having a polymeric shell type polyurea.

In the method of surface polymerization through the polycondensation shell of the microcapsules in the General case is formed by polymerization of at least two monomers that are not miscible with each other (one of which, 2, is dissolved in the dispersion medium S2, and the other, M1, dissolved in a hydrophobic dispersed phase). These monomers are well known to specialists in this field and, for example, lead to the formation of polyamide membranes, polyester membranes, the polyurea membranes, polyurethane membranes, or their copolymers, in Sogno, with other monomers. Preferably, in the methods according to the invention using the monomers giving these polymers.

The polymer constituting the membrane of the capsule, can be obtained by using pairs of monomers (M1, M2), are listed in Table 1 below.

Table 1
The monomers that can be used for the production of microcapsules by surface polymerization
The monomer M2, soluble in the dispersion medium S2The monomer M1, soluble in the dispersed oil phaseThe resulting polymer
DiolDichlorohydrin acidPolyester
DiolDiisocyanatePolyurethane
DiamineDichlorohydrin acidPolyamide
DiamineDiisocyanatePolyurea

Water-soluble monomers M1, which are preferably used in the method of the invention, are selected, for example from treiso is anatov, diisocyanates, for example, etilendiamindisuktsinatov (MDI), 4,4'-dicyclohexylmethane (NMI), colordistance (TDI), poly(1,4-potentialcollision) (PMTDI) and polyfunctional aliphatic polyisocyanates, dichlorohydrin carboxylic acids, such as dichlorohydrin terephthalic, isophthalic or phthalic acid, trifunctionally of acylchlorides, such as trimetallic, trichloride 1,3,5-benzotriazoles acid, acid chloride trimellitic acid, trimethylolpropane, dichloride succinic, adipic, decandido, sabatinovka acids.

The monomers M2, soluble in the dispersion medium S2, which are preferably used in the method of the present invention, are selected, for example, from alkanediols, such as 1,4-butanediol, 1,5-pentanediol, poly(ethylene oxide)glycol (PEAG) of various molecular weights, alcantarillas, such as DIMETHYLPROPANE, di - or tripelenamine, such as ortho-, meta - or para-phenylenediamine, 1,6-hexamethylenediamine were (HMDA) or lysine, 1,2-Ethylenediamine, butylenediamine, Tris(2-amino-ethyl)amine, Triethylenetetramine.

Given the excellent properties of politician as waterproof barriers, preferred in the method of the invention is given to di - or triamines, separately or in a mixture as the monomer M2, and also di - or triisocyanate, separately or in mixtures, as mon the measure M1, in particular, above.

Surfactants

The method of the invention involves the step of emulsifying an oil phase containing borates, which are to be encapsulated, and the monomer M1 in the dispersion medium S2, and stabilize the emulsion. This stage of emulsification is preferably carried out with the use of surface-active substances are preferably present in the dispersion medium.

For this purpose can be any surfactant known to specialists in this field. The preferred surfactant with a hydrophilic-lipophilic balance (products HLB) of from 10 to 15, adapted to disperse an oil phase, such as lubricating oil (oil) contained in the core of the microcapsules according to the invention.

Preferably choose surface-active substances which do not react with the monomers M1 (and possibly M2) used in the method according to the present invention.

The preferred surfactant is a nonionic surfactant, derived from fats, such as fatty alcohols, fatty amines, fatty acids, esters of fatty acids and one or polyhydric alcohols, for example, sorbitan, ethoxylated or methoxylamine, preferably amoxillian the traveler butyric acid, the ethoxylated tridirectional, Exalead of polyoxyethylenesorbitan.

Examples

Example 1: obtaining microcapsules

Encapsulated additive is hydrated triborate potassium with formula KB3O5·H2O, in the form of nanospheres with an average diameter of 200 nm, dispersed in the mineral oil group I type 150 NS using a mixture of succinimide and calcium sulfonate as a dispersant. The content of elemental boron in the mixture of 6.66 wt.%.

10 grams of 4,4'-methyldiphenylamine (DHS, the monomer M1) was dissolved in 20 grams of a dispersion of hydrated borate described above, with the formation of the dispersible phase (solution 1).

160 grams of acetonitrile (S2) is mixed from 13.2 grams of surfactant (Exalead of polyoxyethylenesorbitan) forming a first part of the dispersion medium (solution 2).

4.6 grams of 1,6-diamine (HMDA, the monomer M2) was dissolved in 20 grams of acetonitrile, receiving the second part of the dispersion medium (solution 3).

Solution 2 is added to the reactor and subjected to vigorous stirring (500 to 800 rpm). Add a solution of 1, while continuing the stirring, receive emulsion solution 1 containing borate, in the dispersion medium formed by solution 2.

After stabilization of the emulsion is added slowly a solution of 3 when the stirring speed 200 rpm Is policon insatia DHS, GMDA at the interface of the dispersed phase/dispersion medium without deciding on any additional energy at normal temperatures, and it lasts for 4 hours.

Formed microcapsules consisting of a liquid core containing nanospheres dispersed borate, and the polyurea shell.

Then the capsule is filtered and subjected to subsequent washing with acetonitrile. They are then dried in a drying Cabinet. Thus obtained capsules have a uniform size of about 100 microns in diameter as observed under an optical microscope (magnification 1000*).

Elemental analysis of the thus obtained capsules, performed x-ray fluorescence method, shows the presence of potassium capsules that demonstrates the effective encapsulation of triborate potassium.

Example 2

Perform the same procedure as in Example 1, but:

- solution 1 get 3 grams of hydrated borate dispersion described in Example 1, in which is dissolved 1 gram of 4,4'-methyldiphenylamine (DHS),

- solution 2 get 40 grams of acetonitrile, mixed with 140 grams of surfactant (fatty acids with ethoxylated long carbon chain),

- solution 3 obtained from 20 g of acetonitrile, in which is dissolved 1 g of 1,6-diamine (HMDA).

Observations under the microscope showed that the formed capsules with a diameter of from 0.5 to 10 microns.

Example 3: Resistance to water

The stability of the microcapsules, preparation, is the R in examples 1 and 2, to water according to the following procedure was tested by modeling the mixture of oil/water operated gearbox.

Test samples were prepared by re-dispersion after washing, filtering and drying to about 10 wt.% these microcapsules in the base oil group I type 150 NS, using the p & b succinimide as a dispersant.

The control product was obtained by dispersion of nanospheres hydrated triborate sodium base oil 150 NS of the same composition as the dispersion used to obtain cores of the microcapsules obtained in examples 1 and 2.

Mixtures containing the test products and 1% vol. water, were obtained at 20°C. they were Then mixed on a magnetic stirrer and raised the temperature from 20 to 50°C for 10 minutes, maintaining the temperature of 50°C for the next 20 minutes. Then the mixture was kept at room temperature and measured the transparency in the beginning, after 1 and 10 days of storage.

Measurement of transparency did not show any differences between the dispersions of microcapsules and control dispersion.

However, observations under an optical microscope with magnification of 1000* showed the formation of lamellar crystals of large size about 100-200 μm in the control dispersion.

Such crystals have not been observed in dispersions of microcapsules, whether at the beginning, after 1 or 10 days XP is in. The presence of a protective polymer shell microcapsules prevented the modification of the crystal structure of borates in the presence of water.

1. Microcapsules including:
- the core containing one or more of borates of alkali metals, possibly hydrated, dispersed in one or more than one mineral, synthetic or natural lubricating base oil, and
polymer shell.

2. Microcapsules under item 1, in which the borates of alkali metals are compounds of the General formula:

where M is alkali metal, preferably sodium or potassium, m is a number from 2.5 to 4.5, n is a number from 0.50 up to 2.40, and a Monomeric repeating unit of the formula (I) may be repeated several times.

3. Microcapsules under item 1, where the polymer is selected from polyesters, polyurethanes, polyamides, politician or their copolymers, polyacrylonitrile, vinyl or aminoplastic resins, preferably from politician.

4. Microcapsules under item 1, having a diameter from 0.1 to 50 μm, preferably from 0.1 to 1 micron.

5. Microcapsules under item 1, where the borates are nanospheres with a diameter of from 1 to 300 nm, preferably from 10 to 200 nm, preferably from 20 to 40 nm.

6. Microcapsules according to any one of paragraphs.1-5, where the core further comprises soluble in oil dispersing agents, preferably selected from sulfonates, suppose the equipment polyisobutenylsuccinic, salicylates, sulfonated or desulfuromonas, naphthenates, reaction, sulfonated or desulfuromonas, polyalkyleneglycol, preferably of polyisobutenylsuccinic, amines or Quaternary ammonium salts, singly or in a mixture.

7. Lubricating oil comprising microcapsules according to any one of paragraphs.1-6.

8. Lubricating oil under item 7, where the content of elemental boron, measured in accordance with standard NFT 60-106, is from 500 to 5000 memorial plaques in weight.

9. Lubricating oil under item 7, further including:
- one or more than one antiwear and extreme pressure additive, preferably selected from organic polysulfides, phosphates, phosphites, demercaptanization, benzotriazoles , and/or
- one or more than one friction modifier, preferably selected from monoamino polyhydric alcohols and fatty acids.

10. The use of lubricating oil according to any one of paragraphs.7-9 as lubrication of the transmission, preferably as a lubricant for gearboxes or axles.

11. The method of producing microcapsules using surface polymerization, in which the hydrophobic phase, denoted by S1, containing the first monomer, denoted by M1, and one or more additives dispersed in the dispersion medium formed of the non-aqueous organic solvent, denoted by S2, is not smachiwausa is the specified hydrophobic phase and containing either the initiator, allowing the flow of chain polymerization M1 or the monomer M2, leading to a polycondensation reaction with M1, with the formation of polymers or copolymers, which are components of the shell of the microcapsules, where the specified one or more additives contain one or more of borates of alkali metals.

12. The method of producing microcapsules according to p. 11, which includes stages:
(1) dissolution of monomer M1 in the hydrophobic phase S1, including one or more oils, waxes or greases, mineral, synthetic or natural origin and one or more additives, where the specified one or more additives contain one or more of borates of alkali metals,
(2) the formation of a dispersion of the mixture obtained in stage (1), in a dispersion medium comprising a solvent S2 and possibly one or more surfactants,
(3) adding to the said dispersion medium of the initiator, resulting in a chain polymerization of M1, or monomer M2, leading to a polycondensation reaction with M1, with the formation of polymers or copolymers that are components of the shell of the microcapsules.

13. The method according to p. 11, where the solvent S2 is a polar aprotic solvent having a dielectric constant higher than 25, preferably greater than 30.

14. The method according to p. 13, where the solvent S2 is chosen from dimethyl sulfoxide (DMSO), 1-methyl-2-pyrrolidon is a, acetonitrile, formamide, methylformamide, dimethylformamide, ndimethylacetamide, methylacetamide, dimethylacetamide.

15. The method according to p. 11, where the dispersion of the hydrophobic phase in the dispersion medium is performed by using one or more of surfactants, preferably contained in solvent S2.

16. The method according to p. 15, where the surfactants are nonionic surfactants with a hydrophilic-lipophilic balance in the range from 10 to 15.

17. The method according to any of paragraphs.15-16, where surfactants selected from fatty alcohols, fatty amines, fatty acids, esters of fatty acids and one or polyhydric alcohols, where these compounds ethoxycarbonyl or not ethoxycarbonyl; preferably ethoxylated butyric acid, ethoxylated of christianfree, hexalate of polyoxyethylenesorbitan.

18. The method according to p. 11, where the hydrophobic phase S1 includes borates of alkali metals, possibly hydrated, dispersed in one or more of the mineral, synthetic or natural lubricating oils.

19. The method according to p. 11, where the monomers M1 and possibly M2 are at least bifunctionality monomers, preferably di - or trifunctional.

20. The method according to p. 11, where the initiator, allowing the flow of chain polymerization M1, dissolved in stage 3).

21. The method according to p. 11, where the monomer M2 is dissolved in stage (3).

22. The method according to p. 19, where M1 represents dichlorohydrin or acid diisocyanate, and M2 represents a diol or diamine.

23. The method according to p. 11 for the production of microcapsules according to any of paragraphs.1-6.

24. The microcapsules according to any one of paragraphs.1-6 as antiwear and/or extreme pressure additives in lubricating compositions.



 

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