Method of producing coated heart-shaped particles

FIELD: colloid chemistry.

SUBSTANCE: method comprises dispersing water emulsion of hydrophobic polymer in a liquid immiscible with water containing emulsifier, producing the emulsion with enriched phase that comprises water dispersed phase containing the hydrophobic polymer, and inducing inter-phase reaction of polycondensation at least of one of the reagents of the inter-phase polycondensation to produce polymeric film around the hydrophobic polymer.

EFFECT: enhanced efficiency.

40 cl, 5 ex

 

The present invention relates to powder compositions that include particles comprising a hydrophobic polymeric core within the shell, which is a membrane, and to methods for producing these particles. The invention relates also to a stable homogeneous dispersions of polymer particles, and to methods for their preparation. Moreover, the invention relates to methods of regulating the release of active substances from such particles.

Preparation of particles having a configuration of the core in the shell, you know. One method includes the coacervation of the polymer around the core. Methods of obtaining koatservatnyh coating of the polymer solution around the jet core, which is acceptable to manufacturer of microcapsules suitable for introduction into a concentrated liquid detergent described, for example, in EP-A 356239 and WO 92/20771. The preparation of these methods of the product in which the enzyme satisfactorily contained in the particles inside concentrate, but easily released from these particles, when the concentrate is diluted in water for washing, involves problems of a technological nature.

In WO 97/24179 described powder composition comprising particles having a hydrophobic core within a shell, which is a membrane, and includes a combination products is KTA (a) condensation IFC, the resulting interaction between the first reagent IFC, with at least two first condensation groups and the second reagent IFC, with at least two second condensation groups, and (b) amphiphilic polymer stabilizer, which usually focuses on the interface between oil and water and which contains a repeating hydrophobic group and a repeating reactive hydrophilic groups that are associated with the second condensation groups.

In the US 4708816 described the method of preparation of microcapsules, which are stable in the sense that these microcapsules have a density that is adjusted in such a way that it was almost the same as the density of an aqueous solution of chemical bleach, in which they are dispersed. These microcapsules include inside the core and a polymeric outer shell, which is used to vary the density, so that the particles are compatible with the liquid medium in which they are dispersed. Thus, to implement this method, it is imperative that accurate synthesis of the walls of the shell so that the density of microcapsules corresponded to the density of this liquid medium. In practice, the preparation of appropriate microcapsules with achieving accurate density by about the westline method microencapsulation, the density of the microcapsules is determined only by the number of regulating the density of the polymer in the outer shell, can be fraught with problems of a technological nature. Thus, the carrier phase is inevitably more dense than constituting the wall material.

In the US 3676363 describes the preparation of heavier microcapsules introduction in forming the capsule material finely dispersed weighted connections. The number of input weight compounds usually depends on the target weight of the capsules, which depends on the specific gravity of the liquid. This reference specifically refers, apparently, to increase the density of particles for applications in high-density fluids, such as brine.

In the US 5723059 described improvement dispersion microencapsulating material phase transformations in poly-alpha-olefin coolant for electronic equipment by modifying the density of this fluid to match the density of the dispersed particles. This would be applicable only for systems in which you can change the density of the continuous phase is oil-based.

It is also known preparation of microparticles, which have a predetermined density, in order to obtain a homogeneous dispersion in the hydrocarbon liquid.

However, there is a need in the particles, which is capable of easily and according to form in the liquid homogeneous dispersion. There is also a need to develop an improved method for the preparation of such dispersions in which the particles or microcapsules are evenly distributed and which avoids surface separation of particles, "bundle" system, and avoids the deposition of particles. There is, in particular, the need to achieve this in the dispersions in nonaqueous liquids, mainly in hydrocarbons.

Moreover, there is also a need for improvement of particles containing active substances, and the development of improved methods of release of these active substances.

In accordance with the first object of the present invention features a powder composition comprising particles each of which consists of a core within the shell, where the core comprises a hydrophobic polymer, characterized in that the membrane is a semipermeable membrane.

For the effectiveness of the particles of the present invention is important that the core include at least some amount of the hydrophobic polymer. In one embodiment, the core includes an aqueous liquid containing particles of hydrophobic polymer dispersed in this aqueous liquid. In another embodiment, the core of which incorporates both a matrix of particles of a hydrophobic polymer. All of these versions of the invention the core is considered as a hydrophobic polymer core.

The particle can include a core that is a unified whole matrix of polymeric core material. In another embodiment, the core material includes cavities or pores are distributed throughout the matrix polymer. In addition, the core may also include other components, for example, distributed throughout a hydrophobic polymer core.

It is necessary that the hydrophobic polymer core comprised of any suitable material that is able to absorb, absorb or dissolve hydrophobic or not miscible with water liquid.

In one embodiment, the core also includes a hydrophobic liquid. It is necessary that the hydrophobic liquid has been absorbed or absorbed hydrophobic polymeric core material.

This preferred embodiment of the invention relates to a particle comprising a core, which contains the absorbed or soaked hydrophobic liquid, and semi-permeable membrane shell inside of which the core contains (I) an aqueous liquid containing a dispersed hydrophobic polymer particles, (II) agglomerates of hydrophobic polymer particles and the and (III) a hydrophobic polymeric matrix. In any case, it is necessary that the hydrophobic liquid has been absorbed or imbibed a hydrophobic polymer. This preferred variant implementation of the invention can be achieved by dispersion of the particles in the above-mentioned hydrophobic liquid for a time sufficient to allow the hydrophobic liquid to pass through a semipermeable membrane and inside the hydrophobic polymer core.

In one preferred embodiment, the particles contain active substance. The active substance may be any active component, either slowly out as part of the mechanism of controlled release, or it may perform some function by holding the inside of the particles. This active ingredient, which is kept inside of the particles, could serve as a pigment, dye or color-forming component, and the particle can be used to form a color. Typically, the active substance may be any substance selected from the group including aromatic oils, lubricating oils, essential oils, wax inhibitors, corrosion inhibitors, dyes, acceptors oxygen, antioxidants and vitamins.

Hydrophobic polymeric core material may be any polymeric material that exhibits hydrophobic the properties. It can be a natural polymer, but the preferred synthetic polymer. It is necessary that this polymer was a condensation polymer, for example a complex polyester or polyamide. This polymer may be a reaction product of polycondensation of formaldehyde, such as phenol resin. Other useful polymers include polyurethanes. Preferred hydrophobic polymer core is produced by polymerization of the ethylene-unsaturated monomer or mixture of monomers. Typically, the monomer or mixture of monomers is hydrophobic, but may include any hydrophilic monomer, provided that the resulting polymer is hydrophobic. The term "hydrophobic" means that the solubility of hydrophobic monomer in water at 25°With less than 5 g / 100 cm3deionized water. The term "hydrophilic monomer means that the solubility of the hydrophilic monomer in water at 25°C is at least 5 g / 100 cm3deionized water. Typically, the monomers include monomers which have no ionic or hydrophilic functional groups. Suitable monomers are, for example, Acrylonitrile, esters of ethylene-unsaturated carboxylic acid, styrene and vinyl esters of saturated carboxylic acids such as vinyl acetate. In the preferred VA is iante hydrophobic polymer core derived from a hydrophobic monomer or mixture of monomers, include4-C30alkalemia ethers of ethylene-unsaturated carboxylic acid, more preferably4-C30alkalemia esters of (meth)acrylic acid. Particularly suitable monomers include 2-ethyl hexyl acrylate, laurelcrest, stearylamine, n-butylmethacrylate and isobutyronitrile and mixtures of these monomers. The monomer mixture may also include polyethylene-unsaturated monomers, which serve for crosslinking polymeric core material. Alternatively, it may be appropriate to carry out the stitching with the use of other cross-linking agents, which include two or more functional groups which are capable of forming cross-links between two or more polymer chains. However, in the preferred embodiment, using cross-linking agents, which are ethylene-unsaturated monomers that are compatible with the mixture of the monomers and form during the polymerization cross connection. Acceptable cross-linking monomers include divinylbenzene, etilenglikolevye, pentaerythrityl etc. At 25°in deionized water, the hydrophobic polymer is not soluble and does not swell.

Polymeric core material may be received via any acceptable method of polymerization, the implementation of which bresults the particles of the hydrophobic polymer. Particles of hydrophobic polymer can effectively prepare aqueous emulsion polymerization, for example as described in EP-A 697423 and US 5070136. When performing a typical method of polymerization of the monomer or monomer mixture is introduced into the aqueous phase, which contains a reasonable amount of emulsifier. Typically, the emulsifier may be any of commercially available emulsifiers suitable for preparation of an aqueous emulsion. It is necessary that these emulsifiers have high ability to dissolve in the aqueous phase than Monomeric not miscible with water phase, and the ability to manifest, thus, a higher hydrophilic-lipophilic balance (products HLB). The mechanism of emulsion polymerization involves the transition of the monomer through the aqueous phase in the polymerization reaction with the formation of micelles, resulting in emulsification not decisive. Further, the polymerization can be carried out using, if it is acceptable, initiation systems, such as UV initiator or thermal initiator. A suitable method of initiating the polymerization reaction could serve as a temperature increase water emulsion of monomer to above 70 or 80°and then adding in the range from 50 to 1000 hours/million of ammonium persulfate in recalculation on weight of monomer.

Alternatively the hydrophobic Serdtsev the hydrated polymer can be obtained in the form of technically available product for example product Alcomer 274 (trademark of Ciba Specialty Chemicals), which is an acrylic emulsion polymer.

It is necessary that the hydrophobic polymer was in the form of a dispersion of polymer particles in a liquid medium, in which the average size of the polymer particles is less than 10 μm. The preferred average particle size equal to less than 2 microns. Typical average diameter of such particles exceeds 100 nm, it is usually in the range from 200 nm to 1 μm, for example in the range from 500 to 750 nm.

According to the invention it is possible to obtain particles of any reasonable size. However, typically, the average particle diameter is less than 30 microns, and often is in the range from 0.5 to 30 μm. The preferred particle size is less than 10 or 20 μm, for example, is in the range from 750 nm to 2 μm, most preferably equal to about 1 micron.

The composition of the present invention can be prepared by obtaining a shell around the hydrophobic polymeric core material, where the membrane is a semipermeable membrane. The preferred membrane is produced by conducting interfacial polycondensation reaction. This can be achieved by mixing the first reagent interfacial polycondensation in the dispersion of hydrophobic polymer particles in the first liquid medium, and then preparing a first dispersion liquid, vklyuchayuschimisya particles, the second liquid medium, is not miscible with the first liquid. The interfacial polycondensation reaction can be carried out by adding the second reagent to interfacial polycondensation, which interacts with the first reagent, resulting in proceeds interfacial polycondensation reaction. Shell, which is formed may consist essentially of one membrane that covers the core material, or alternatively it may be formed of multiple layers of product interfacial polycondensation and may be in the form of a relatively rigid polymer shell. For the execution of the invention is that the shell consisted of a semi-permeable membrane. In the preferred embodiment, this shell as a whole is a semi-permeable barrier, and it can be called a semi-permeable membrane.

Under a semi-permeable barrier or semi-permeable membrane mean that through such a barrier or membrane is possible passage of small molecules but prevents the penetration of large molecules. Thus, when performing the present invention are relatively small molecules, such as molecules of oils and other hydrophobic liquids can pass through a semi-permeable barrier in the core, but at the same time prevents leakage of the polymeric core material. Therefore, under the present is to him the invention provides particles, comprising a hydrophobic core surrounded by a semipermeable membrane, which has a high osmotic potential of relatively hydrophobic liquid solvent for the polymer core. In the preferred embodiment, this osmotic potential should be relatively high, even when soaked relatively large amounts of hydrophobic liquid. Thus, in the preferred embodiment, a semi-permeable membrane allows the passage of small molecules, such as hydrophobic liquid, preventing the loss of the core material, and functions as a physical barrier that limits the extent of swelling and expansion of the core. Therefore, in this situation, the particles can be considered as fully swollen.

In addition, the variant in which the hydrophobic polymeric core material may include more than one of the special polymer materials. One way of achieving this is, apparently, in the use process of encapsulating a mixture of different water emulsion of hydrophobic materials. In this case, the mixture of emulsion polymers can include one, two or more different polymers from other hydrophobic polymers, and hydrophobic core material includes, therefore, a mixture of different hydrophobin the x polymers. The choice of different hydrophobic components for inclusion in the core can be planned in such a way that you can absorb the mixture of different hydrophobic liquids. This may be important for hydrophobic liquids such as essential oils, petroleum distillates, diesel fuel and crude oil. This way you can pick up a cocktail of specific hydrophobic polymeric materials to ensure maximum absorption capacity for a particular mixture of hydrophobic liquids. The choice and proportions of specific core materials generally depend on the composition and characteristics of the hydrophobic liquid, which is necessary to absorb.

In accordance with the second object of the invention proposes a method of making particles that comprise a core comprising a hydrophobic polymer inside the membrane, where the membrane is a semipermeable membrane. This method essentially comprises the following stages:

a) dispersing an aqueous emulsion of a hydrophobic polymer is not miscible with water fluids containing emulsifier, obtaining emulsion with reversed phase comprising aqueous disperse phase that includes a hydrophobic polymer,

b) inducing interfacial polycondensation reaction of at least one reagent interfacial polycondensation to obtain the district hydrophobic polymer polymer membrane with formation of a dispersion of particles,

C) optional dehydration of the dispersion particles by removal of particles of all residual water.

Therefore, when the stage (in) dehydration is not carried out, formed in this way particles typically include a shell surrounding the core of an aqueous liquid in which the dispersed particles of the hydrophobic polymer. Typically, the aqueous emulsion polymer to form particles of average diameter less than 1 micron, for example from 50 to 750 nm, and typically from 100 to 600 nm, preferably from 200 to 500 nm, mainly from 300 to 400 nm. Usually, when the core contains a hydrophobic polymer particles, these particles are characterized by the same average diameter.

When carry out stage (C) dewatering, liquid water can be removed partially or completely. By removal of the water particles of the hydrophobic polymer will have the ability to blend into almost solid hydrophobic matrix core. In another embodiment, the hydrophobic polymer particles may be partially discharged or stick to each other to form one or more agglomerates of hydrophobic polymer particles. The primary particle agglomerates are typically characterized by the same size as formed by aqueous emulsion polymerization. The choice of the hydrophobic polymer can be carried out depending on whether plasmatica or agglomerates. Thus, the hydrophobic polymer with a higher melting point is usually an inherent tendency to form agglomerates, whereas hydrophobic polymer with a lower melting point is usually an inherent tendency to virtually merge to form a single, solid matrix.

In another embodiment of the invention in accordance with the second object of the invention the active component is contained in is not miscible with water liquid. In this embodiment, the invention is not miscible with water, the liquid containing the active component, absorb or absorb hydrophobic polymer. Thus, the shell is formed around the hydrophobic polymer containing not miscible with water, the liquid and the active component. After the formation of the wall of the shell can be realized a stage of dehydration, in which the core will remove the water, leaving a core comprising a solid hydrophobic polymer matrix or agglomerated particles of hydrophobic polymer, where the core contains the active component.

In another embodiment, the active component can be dissolved in not miscible with water fluid, and in this case, the active component can also absorb hydrophobic polymer, allowing the incumbent whom onent distributed around the hydrophobic polymer. Instead, the active component may be dispersed, but not dissolved in not miscible with water liquid. In this case, the active component may be a water-soluble substance, which, consequently, is not absorbed hydrophobic polymer, but instead manifests, apparently, the tendency to sequester hydrophobic polymer core surrounded by the shell. Instead, these water-soluble active components can be dissolved in the aqueous phase of an aqueous emulsion of a hydrophobic polymer. Thus, when implementing a stage of dehydration of the active component tends to deposition and, therefore, this active component is captured by the cavities between the hydrophobic polymer particles. When the hydrophobic polymer core forms a continuous matrix, a water-soluble active component may be distributed throughout the matrix, for example in the form of solids, physically linked hydrophobic polymer.

In the preferred embodiment, this second object of the invention the shell forming interfacial polycondensation reaction is essentially oil-soluble first reagent interfacial polycondensation with at least two first condensation groups, with almost water-soluble second reagent interfacial polycondensation, budushego at least two second condensation groups, the latter includes the combination of the second reagent interfacial polycondensation with a water emulsion of a hydrophobic polymer before carrying out stage (a) of this method, followed by mixing the first reagent interfacial polycondensation to induce interfacial polycondensation reaction stage (b), and then conducting the reaction between the first and second reagents interfacial polycondensation to obtain a shell.

As is not miscible with water liquid, it is advisable to use oil acceptable for emulsion polymerization. Preferred is not miscible with water liquid is a hydrocarbon. This liquid usually can be, for example, that described in EP-A 150933. However, it may be necessary to use particularly clean is not miscible with water liquids. It may be necessary to use high-purity paraffin oil medical varieties. One particularly preferred paraffin oil, medical grade product is Kristol M 14 (RTM). Not miscible with water, the liquid can be chosen in such a way that it was easily absorbed hydrophobic polymer. However, for hydrophobic polymer can be an advantage ability to absorb or soak up not miscible with water liquid during the implementation stage of education is blocki.

As discussed in relation to the first object of the invention, as a hydrophobic polymeric core material can be used any polymer material that exhibits hydrophobic properties. It is necessary that the hydrophobic polymer core has the ability to absorb hydrophobic liquid. In General, the monomer or mixture of monomers is hydrophobic, but may include some amount of hydrophilic monomer, provided that the resulting polymer is hydrophobic. Typically, the monomers include those monomers which have no ionic or hydrophilic functional groups. Suitable monomers are, for example, Acrylonitrile, esters of ethylene-unsaturated carboxylic acid, styrene and vinyl esters of saturated carboxylic acids such as vinyl acetate. In a preferred embodiment, the hydrophobic polymer core derived from a hydrophobic monomer or mixture of monomers comprising From4-C30alkalemia ethers of ethylene-unsaturated carboxylic acid, more preferably4-C30alkalemia esters of (meth)acrylic acid. Particularly suitable monomers include 2-ethyl hexyl acrylate, laurelcrest, stearylamine, n-butylmethacrylate and isobutyronitrile and mixtures of these monomers. The monomers, the links of which are contained in the hydrophobic is alimera, and the ratio between them can be chosen in such a way that the polymer is more easily absorbed one hydrophobic liquid than another.

As an emulsifier in stage (a) of the method, you can use any acceptable emulsifier, mainly from those emulsifiers which are generally used in emulsion polymerization with reversed phase. The preferred emulsifier is a polymeric emulsion stabilizer, which has both hydrophilic and oleophilic residues, so it is associated with the interfacial layer, contributes to the stabilization of the dispersed phase and prevents agglomeration of the particles. Particularly preferred polymeric emulsifier is oil-soluble or swelling in oil amphiphilic polymer stabilizer.

There may be a need for the regulator, which in addition to the stabilization of the dispersed phase and to prevent agglomeration of the particles takes actual participation in the process of formation of the shell. Such chemically active stabilizer contains acceptable reactive groups that allow him to participate in the interfacial polycondensation reaction, but at the same time not hinder him to act as a stabilizer. Thus, the emulsifier can serve as a stabilizer, which contains povtoreaiusi the Xia hydrophobic group and a repeating reactive hydrophilic groups, which before being mixed with the first reagent interfacial polycondensation contact with the second condensation groups of the second reagent interfacial polycondensation.

The first reagent interfacial polycondensation should be added to the dispersion in any suitable way that allows the membrane to be formed without reducing stability. This can be achieved by mixing the first reagent interfacial polycondensation, which is carried out by mixing the dispersion and the first reagent interfacial polycondensation in the conditions in which the mass ratio between the variance and the first reagent interfacial polycondensation remains almost constant during the whole process of mixing. In this case, the operation of the education of the shell during the process as a whole was characterized by the constancy that is accompanied by a tendency to the formation of particles is more consistent in size and more stable system, which prevents the possibility of agglomerates. There is a great need for the particles according to the invention remained individual freely dispergirovannykh particles comprising a solid shell surrounding the core.

In other preferred methods according to the invention is formed of a dispersion of particles is not miscible with water, the liquid is treated by adding to the dispersion mixture is being a developing water organic liquid (which, for example, can serve as a surfactant) and distillation is not miscible with water liquid, so that mixing with the water organic liquid, a dispersion of particles. If necessary, the dispersion is not miscible with water liquid and/or miscible with water, the liquid can be subjected to distillation in such a way as to make it practically anhydrous.

The implementation of the methods according to the invention, in particular those that use the emulsifier, which is a polymer stabilizer, communicating in a certain way with the second reagent before the interaction of the first and second reagents, allows to obtain a satisfactory concentration more uniform particles and, in particular, allows you to cook almost stable dispersion of small encapsulated particles (with sizes of at least 90 wt.% less than 30 microns). Their implementation can have a positive impact on the receiving shell interfacial polycondensation. Thus, in particular, optimization of polymer stabilizer and quantity makes it possible to reduce the number of either or both of the reagents that you want to obtain membranes with defined properties. Moreover, particles prepared using the stabilizer, can be stably dispersing to another Jew the spine.

The methods according to the invention can include the subsequent stage of distillation of the core composition most or all of the water up until the particles will not consist of virtually anhydrous hydrophobic core encapsulated in a polymer shell, obtained by interfacial polycondensation. In a preferred embodiment, stage distillation carried out under reduced pressure. The distillation of this type are often referred to as azeotropic distillation, because with distilled water usually some amount of organic liquid, although for the formation of azeotrope the need for water and the organic liquid is absent.

In a preferred embodiment, the invention is used for the preparation of fine particles, typically with dimensions of at least 90 wt.% particles in the dry state less than 30 μm. The implementation of the invention not only allows for a relatively high concentration of such particles (e.g., from 25 to 50 wt.% in terms of the final product), but also allows them to prepare in the form almost of individual particles and almost stably dispersed in not miscible with water liquid.

Reference to the size of the particles in the dry state mean particle size, determined after distillation of the dispersion thus, to obtain essentially anhydrous core, for example harakteryzuyutsya total water content (based on the total weight of the particles below 20 wt.%, and usually below 10 wt.%. However, in the absence of any process to dry the dispersion of the size in the dry state can be calculated according to the results of measurement in wet conditions.

The implementation of the method according to the invention is acceptable to obtain particles of any suitable size. However, typically, the average particle diameter is less than 30 microns, and often is in the range from 0.5 to 30 μm. The preferred size of the particles is typically less than 10 or 20 μm, for example in the range from 750 nm to 2 μm, most preferably about 1 μm.

When it comes to the fact that the particles are almost individual and stable dispergirovannykh in not miscible with water fluid, we mean that the total number of particles (including agglomerated particles with sizes of greater than 30 μm is less than 10 wt.% and that in the preferred embodiment, no deposition of particles does not occur, but if it's in some degree occurs, then dropped into the sediment particles can easily re-dispersing careful mixing. In a preferred embodiment, the size of at least 80 wt.% (preferably at least 90 wt.%) particles in the dry state less than 15 or 20 microns, therefore the number of agglomerates larger than 15 or 20 microns, must also be low. In predpochtitelnye the size of at least 70 wt.% (and preferably 80 or 90 wt.%) particles is less than 10 μm. The particles may be so small that, for example, 50% of the particles less than 1 μm, but preferably at least 50 wt.%, and most preferably at least 70 wt.%, and their sizes are in the range from 1 to 5 microns.

According to another variant of okharakterizovanie size preferred average particle size (srednevekovoi basis) is less than 20 microns, and most preferably less than 10 μm, often in the range of from 1 to 5 microns.

At the beginning of the particles should be prepared dispersion in the environment type of water in the oil is not miscible with water liquid. In the preferred embodiment, this fluid does not contain halogenated hydrocarbons such as chloroform, and in the preferred embodiment is a hydrocarbon.

When making the initial stage of the process of preparing particles having a water core, including dispersed hydrophobic polymer particles, water composition, which is used to obtain core material is dispersed in not miscible with water non-aqueous liquid. This dispersion is injected essentially water-soluble reagent interfacial polycondensation with low or non-macrorestriction. In some cases, certain components (e.g., reagent MFP or the additive for regulating the pH), who designed the us for introduction into the shell or the core particles, can be added before, during or after encapsulation. If necessary, essentially water soluble reagent is mixed with the composition for aqueous core prior to its dispersion in not miscible with water liquid.

In a pre-prepared aqueous dispersion composition is not miscible with water, the liquid can be mixed with the reagent and optionally other relevant components (e.g., additive for regulating the pH, such as sodium hydroxide). In some cases, the reagent interfacial polycondensation can serve as the water in the aqueous core composition. In some cases, the formation of the shell can be made by holding two or more consecutive reactions.

In a preferred embodiment, a water-soluble reagent usually must have a solubility in the oil phase, sufficient to make it a small amount has dissolved in the oil phase or to at least have migrated to the interface between oil and water phases. This speeds up the formation of the target connection between the stabilizer and essentially water-soluble reagent.

In the preferred embodiment, as a water-soluble reagent interfacial polycondensation using Amin, oil-soluble reagent interfacial polycondensation is a KIS the GTC or the derivative acid, and the condensation polymer is a polyamide. More preferred water-soluble reagent interfacial polycondensation is Diethylenetriamine.

Preferred oil-soluble interfacial polycondensation is terephthaloylchloride. In another preferred system includes a polymeric emulsifier, which contains the carboxyl side groups, and a water-soluble second reagent interfacial polycondensation is an amine.

When using polymeric emulsifier, in the preferred embodiment, it usually is a statistical copolymer obtained by copolymerization in a mixture of ethylene-unsaturated hydrophilic and the ethylene-unsaturated hydrophobic monomers. As a polymeric emulsifier is particularly appropriate to use a statistical copolymer of at least one ionic ethylene-unsaturated monomer and at least one nonionic ethylene-unsaturated monomer. Suitable ionic monomer may be anionic monomer selected from acrylic acid, methacrylic acid and maleic acid (or anhydride). The nonionic monomer may be water-insoluble or relatively insoluble in water, preferably selected from sterols and fatty aliphatic esters etileno the unsaturated carboxylic acid.

Especially effective polymeric emulsifier is one that becomes covalently associated with the outer surface of the particles. Thus, for a polymer stabilizer is important that sufficient reactive groups. Such polymeric emulsifier typically may have reactive groups which are selected from epoxy and hydroxyl, and the covalent bond is a simple ester or reactive groups are amino groups, and covalent bond is an amide, or a reactive group represent the remains do not contain carboxylic acid groups or anhydrides, or golodnikov (or salts), and the covalent bond is an ester or amide.

Polymeric emulsifier may be a copolymer of a hydrophilic monomer unit, including parts of the anhydride of dicarboxylic acid, and a hydrophobic monomer unit. Polymeric emulsifier typically represents a speed obtained by the polymerization of the polymer of the hydrophobic monomer unit and a hydrophilic monomer unit, where hydrophobic monomer units include the remains do not contain carboxylic acid groups or links of residues of salts, acids, and reactive Monomeric units selected from glycidyloxy monomer unit and ang is gridnik of monomer units.

The third object of the present invention is a stable dispersion of particles uniformly distributed in the first hydrophobic liquid in which the particle includes a core within the shell and the core layer includes a hydrophobic polymer containing absorbed them a second hydrophobic liquid, characterized in that the membrane is a semipermeable membrane.

It was found that the particles in accordance with the first object of the invention, which has absorbed the second hydrophobic liquid capable of forming a stable dispersion in the first hydrophobic liquid in which the particles are distributed uniformly. It was also established that when these particles include soaked hydrophobic liquid, in particular when these particles are in the form of swollen capsules, they are capable of forming a stable dispersion of particles of which not glomerida and not deposited over long periods of time. These particles may have any suitable size, but the preferred average particle diameter is less than 30 μm, often is in the range from 0.5 to 30 μm. The preferred particle size is less than 10 or 20 μm, for example, is in the range from 750 nm to 2 μm, most preferably about 1 μm.

In accordance with this third object of the invention CCA is i.i.d. stable dispersion can be formed, when the first and second liquids have approximately the same density. In a preferred embodiment, the first and second hydrophobic liquid are identical.

This object of the invention is particularly suitable for systems on a liquid basis, for the importance of a stable uniform distribution of particles. There is, for example, many applications in which particles or capsules use in liquid media as carriers of active substances. Thus, in a preferred embodiment, the invention features a stable dispersion of particles, which contain the active substance.

The active substance may be any active component, either slowly out as part of the mechanism of controlled release, or it may perform some function by holding the inside of the particles. This active ingredient, which is kept inside of the particles, could serve as a pigment, dye or color-forming component, and the particle can be used to form a color. As a rule to the active substances include, for example, aromatic oils, lubricating oils, essential oils, color-forming chemicals, aromatic chemicals, Poluchenie tools, herbicides, other pesticides, antimicrobials and catalysis of the Torah. This way you can capture the active substances to print and produce images for the manufacture containing no pigment transfer paper, such as inks, toners and dyes. Other active ingredients include industrial adhesives, sealants, fillers, paints, catalysts, pore-formers, solvents. Acceptable active ingredients include antioxidants and/or acceptors oxygen. Specific suitable antioxidant, in particular for use in lubricating oils, is a product Irganox L57 (RTM). Another active ingredient is used in the catalysts of the transfer of the dye or chemical accelerator bleaching, for example used in the detergent composition. This way you can encapsulate agrochemical means, such as herbicides, insecticides, anti-fouling, repellents, fertilizers. You can also effectively encapsulate for subsequent controlled release of active substances for food and feed, such as fragrances, flavors, preservatives, nutrients. The present invention can also be used for encapsulation and controlled release of pharmaceutical agents for permanent or long-term allocation of drugs or releasing VA is zindoga funds. The invention can be used in the composition of cosmetic and various healing tools and skin care, and also to apply in the preparation of household tools, such as Soaps, detergents and optical brighteners.

When the active component is a dye may be any dye, such as dye, pigment or colorful lacquer. Acceptable colorants normally include any organic or inorganic pigment or dye approved for use in cosmetics CTFA and the FDA, such as colorful lacquers, iron oxides, titanium dioxide, iron sulfides, and other conventional pigments used in cosmetic preparations. Examples of pigments include inorganic pigments such as carbon black, D&C Red 7, calcium lake, D&C Red 30, talc Lake, D&C Red 6, barium lake, Russet iron oxide, yellow iron oxide, brown iron oxide, talc, kaolin, mica, mica titanium, red iron oxide, magnesium silicate and titanium oxide, and organic pigments such as Red No. 202, Red No. 204, Red No. 205, Red No. 206, Red No. 219, Red No. 228, Red No. 404, Yellow No. 205, Yellow No. 401, Orange No. 401 and Blue No. 404. Examples of oil-soluble dyes include Red No. 505, Red No. 501, Red No. 225, Yellow No. 404, Yellow No. 405, Yellow No. 204, Orange No. 403, Blue No. 403, Green No. 202 and Purple No. 201. Examples of VAT dyes are Red No. 226, Blue No. 204 and Blue No. 201. Examples of lacquer dyes include the indicate various acid dyes, which turned into colorful lacquer aluminium, calcium or barium.

You can also use conventional dyes, which can be either oil soluble or water soluble. The preferred dye is an aqueous solution of water-soluble dye. Acceptable to perform the present invention dyes include FD&C Blue No. 11, FD&C Blue No. 12, FD&C Green No. 13, FD&C Red No. 13, FD&C Blue No. 140, FD&C Yellow No. 15, FD&C Yellow No. 16, D&C Blue No. 14, D&C Blue No. 19, D&C Green No. 15, D&C Green No. 16, D&C Green No. 18, D&C Orange No. 14, D&C Orange No. 15, D&C Orange No. 110, D&C Orange No. 111, D&C Orange No. 117, FD&C Red No. 14, D&C Red No. 16, D&C Red No. 17, D&C Red No. 18, D&C Red No. 19, D&C Red No. 117, D&C Red No. 119, D&C Red No. 121, D&C Red No. 122, D&C Red No. 127, D&C Red No. 128, D&C Red No. 130, D&C Red No. 131, D&C Red No. 134, D&C Red No. 139, FD&C Red No. 140, D&C Violet No. 12, D&C Yellow No. 17, Ext. D&C Yellow No. 17, D&C Yellow No. 18, D&C Yellow No. 111, D&C Brown No. 11, Ext. D&C Violet No. 12, D&C Blue No. 16 and D&C Yellow No. 110. Such dyes are well-known technically available materials, and their chemical structure is described, for example, 21 C.F.R. part 74 (revised from 1 April 1988) and CTFA Cosmetic Ingredient Handbook (1988), publishing company Cosmetics, Toiletry and Fragrancy Association, Inc. These publications included in the present description as a reference.

As discussed in relation to the first object of the invention, as a hydrophobic polymeric core material can be used Liu is Oh polymeric material, which exhibits hydrophobic properties. Suitable gidrofobnaya polymer core may have the ability to absorb hydrophobic liquid. In General, the monomer or mixture of monomers is hydrophobic, but may include some amount of hydrophilic monomer, provided that the resulting polymer is hydrophobic. Typically, the monomers include those monomers which have no ionic or hydrophilic functional groups. Suitable monomers are, for example, Acrylonitrile, esters of ethylene-unsaturated carboxylic acid, styrene and vinyl esters of saturated carboxylic acids such as vinyl acetate. In a preferred embodiment, the hydrophobic polymer core derived from a hydrophobic monomer or mixture of monomers comprising From4-C30alkalemia ethers of ethylene-unsaturated carboxylic acid, more preferably4-C30alkalemia esters of (meth)acrylic acid. Particularly suitable monomers include 2-ethyl hexyl acrylate, laurelcrest, stearylamine, n-butylmethacrylate and isobutyronitrile and mixtures of these monomers.

The composition according to the present invention can be prepared by forming a shell around the hydrophobic polymeric core material, where the membrane is a semipermeable membrane. In preference the sustained fashion version shell get interfacial polycondensation reaction. In the preferred embodiment, this is achieved in accordance with the second object of the invention.

In the preferred embodiment of this object of the invention particles have almost the same density as the first hydrophobic liquid.

As mentioned above, provided that the hydrophobic polymeric core material may include more than one specific polymer material. Thus, in this variant implementation of the invention offers a stable dispersion of particles comprising a core of at least two different selected core polymers, where the number themselves and the core material is chosen so that they were able to absorb the components of the hydrophobic liquid comprising two or more fractions. So, for example, particles comprising a number of different6-C10the alkyl(meth)acrylate polymers, usually easily absorb all of the components of liquid petroleum products. Thus, particles that absorb such liquid petroleum product that can easily form a stable dispersion in oil, in which the particles are evenly distributed.

The choice and proportions of specific core materials generally depend on the composition and characteristics of the hydrophobic liquid, you want to absorb, and from the hydrophobic liquid in which the which the particles must be atomized.

In accordance with the fourth object of the invention proposes a method of preparing a stable dispersion of particles that are evenly distributed throughout the first hydrophobic liquid,

includes the following stages:

(a) preparation of a powder composition comprising particles which have a core comprising a hydrophobic polymer inside the shell;

(b) the dispersion of these particles in the second hydrophobic liquid in which the hydrophobic Primera core soluble or able to swell and which is characterized by approximately the same density as the first hydrophobic liquid;

(C) providing sufficient time for the second hydrophobic liquid is absorbed into the hydrophobic polymer core;

(g) the transfer of particles comprising a second hydrophobic liquid treated in stage (b), the first hydrophobic liquid;

characterized in that the membrane is a semipermeable membrane. In a preferred embodiment, the first and second liquids is essentially the same substance.

In accordance with a fifth object of the invention features a method for controlling release of the active substance, comprising placing the substrate or the environment, which should be released active substance powder is obraznoi composition, including particles that have a core comprising a hydrophobic polymer inside the shell, and the core contains the active ingredient, characterized in that the membrane is a semipermeable membrane.

Suitable active substance can be selected from any of the above active substances.

In one embodiment, the active substance is dissolved or dispersed in a hydrophobic liquid and as the liquid and the active substance absorb core. Thus, in this case, the hydrophobic liquid should, apparently, be selected with the expectation that it was compatible with the active substance. Depending on the specific active substance and purpose of its use may be necessary to select a hydrophobic liquid with a specific volatility, which can speed up or slow down the release of the active substance. In another embodiment, the active substance is a hydrophobic liquid.

In one preferred embodiment of the present invention the hydrophobic polymer contained in the core may include more than one specific polymer material. Thus, in this embodiment, the present invention offers a stable dispersion of astiz, comprising a core material selected from at least two different wood polymers, where the number themselves and the core material is chosen so that they were able to absorb the components of the hydrophobic liquid comprising two or more fractions. So, for example, particles comprising a number of different3-C10the alkyl(meth)acrylate polymers, usually easily absorb all of the components of essential oils. Therefore, particles containing absorbed essential oil, can be placed in a special substrate and is adjustable to select. The choice and proportions of specific core materials generally depend on the composition and characteristics of the hydrophobic liquid, you want to absorb, and the applicable component.

Below are examples that illustrate the invention.

Example 1

The aqueous phase was prepared by diluting 5,9 am technically available latex poly-2-ethylhexyl acrylate (concentration of 42.6%) of 44.5 hours of deionized water. This aqueous mixture was added 1.0 hours of Diethylenetriamine (DETA).

Separately preparing an oil phase containing 5 o'clock 20%of amphiphilic stabilizer and 145 hours of non-volatile oil.

As amphiphilic stabilizer can use any stabilizers described in WO 97/24179, in particular the copolymer Mm 40000 sterilisability 90 is AC.% and methacrylic acid 10 wt.%. As a non-volatile oil used product Finalan 100S, which is dearomatization hydrocarbon solvent, representing a hydrocarbon, mainly in the range of C9-C16CAS N 64742-47-8 impregnated Fina PLC.

Further, when working wysokosciowe stirrer of Silverson the aqueous phase was slowly introduced into the oil phase and the mixture is homogenized to obtain an emulsion of water in oil with an average size of water droplets of 5 microns.

In this emulsion water in oil) was added 1.0 g of terephthaloylchloride (TFH)dissolved in 44 g of non-volatile oil, which results in interfacial polycondensation capsules with polyamide sheath. The resulting mixture of microcapsules was stirred for further 60 min with a mechanical stirrer until complete reaction with the formation of the capsule wall.

Then the microcapsules in the oil was transferred into a distillation flask and was added 40 g of volatile solvent. As the volatile solvent used Isopar G, which is isoparaffinic solvent fraction 158-175°manufactured by Exxon Mobil. The mixture was subjected to vacuum distillation to remove a mixture of water/volatile solvent. The initial temperature was 25°and in the process of refining its increased up to a maximum of 100°C. After removal of all volatile solvents, the final product was particularly the suspension of microcapsules in the non-volatile oil. These microcapsules contain the swollen polymer core, including oil soaked and the outer nylon shell.

Example 2

The experiment of example 1 was repeated, except that instead of poly-2-ethylhexylacrylate emulsion polymer used polyaryletherketones emulsion polymer.

Example 3

The experiment of example 1 was repeated, except that instead of poly-2-ethylhexylacrylate emulsion polymer used polistirolbetonny emulsion polymer.

Example 4

This example shows that when you add the microcapsules of examples 1 to 3 and for some period of time contain in vaseline oil (oil Kristol M 14), microcapsules remain dispergirovannykh and suspended in the mass of oil through the regulation of their density.

For each of the above examples 1 to 3 have separate trials. 10 g were in vitro oil Kristol M 14 was added 0.1 g of microcapsules and stirred to form a homogeneous mixture.

Upon completion of the storage period of 1 month at room temperature, the tubes containing microcapsules were examined to determine the sustainability of their content against the formation of sludge or stratification and, therefore, its ability to adjust the density.

During this period, the principal amount of the particles remained suspended in the liquid oil. In addition, each sample was examined under an optical microscope, which confirmed the presence of discrete swollen particles.

Example 5

This example illustrates the capture of powdery material with a core of hydrophobic particles. Product-749 is a complex connection aldimine manganese (manganese oxidation) and a catalyst used for oxidation of peroxide compounds, for example, used in detergent compositions.

5.0 g of the catalyst-749 was dispersible in water mixed with an emulsion polymer containing 45,5 g 35%product Alcomer 274 and 45.5 g of water. The addition of 1.0 M of sodium hydroxide solution the pH value of the resulting mixture was brought up to 10.0.

Further, when working wysokosciowe stirrer of Silversea above water mixture was injected into the oil mixture containing 10 g of amphiphilic stabilizer and 290 g of solvent Isopar G. the Resulting mixture is homogenized for 10 min to obtain a stable emulsion of water in oil, the average size of water droplets which were 5.0 microns.

The final emulsion polymer was transferred into a flask equipped with a mechanical paddle stirrer. It was added 1.3 g of Diethylenetriamine, first forming the wall of the shell monomer. After stirring the emulsion mixture for 10 minutes to relax the Lee of 1.3 g terephthaloylchloride, dissolved in 100 g of solvent Isopar G, forming a second wall of the shell monomer. Then the resulting mixture for microencapsulation was heated to 30°and was stirred for 2 h to complete the formation of the wall of the shell.

After that, the mixture of microcapsules were subjected to vacuum distillation to remove the water.

The finished product was a suspension of microcapsules in oil. Microcapsules with nylon sheath included hydrophobic polymer core with contained in the solid catalyst C-749.

1. The dispersion of the powder particles, including particles that have a core inside the shell in which the core comprises a hydrophobic polymer, wherein the membrane is a semipermeable membrane.

2. The dispersion according to claim 1, in which the hydrophobic polymer contained in the core, which is able to absorb hydrophobic liquid.

3. The dispersion according to claim 1 or 2, in which the hydrophobic polymer in the core layer includes a hydrophobic liquid.

4. The dispersion according to claim 2 or 3, in which the hydrophobic liquid comprises an active substance.

5. Dispersion according to any one of claims 1 to 4, the active ingredient which is selected from the group including aromatic oils, lubricating oils, essential oils, wax inhibitors, corrosion inhibitors, colorants, famine, antioxidants and catalysts of migration of the dye.

6. Dispersion according to any one of claims 1 to 5, in which the core comprises a hydrophobic polymer derived from a hydrophobic monomer or mixture of monomers comprising From4-C30alkalemia ethers of ethylene-unsaturated carboxylic acid, preferably4-C30alkalemia esters of (meth)acrylic acid.

7. Dispersion according to any one of claims 1 to 6, in which the core includes at least two different polymeric substances.

8. Dispersion according to any one of claims 1 to 7, in which the shell is obtained interfacial polycondensation reaction.

9. Dispersion according to any one of claims 1 to 8, in which the average particle diameter is from 0.5 to 30 μm.

10. The method of preparation of a dispersion of powder particles according to claim 1, which includes a core comprising a hydrophobic polymer membrane, the implementation of the following stages:

a) dispersing an aqueous emulsion of a hydrophobic polymer is not miscible with water fluids containing emulsifier, obtaining emulsion with reversed phase comprising aqueous disperse phase that includes a hydrophobic polymer,

b) inducing interfacial polycondensation reaction of at least one reagent interfacial polycondensation to get around hydrophobic polymer polymer shell with the formation of the dispersion frequent the C,

C) optional dehydration of the dispersion particles by removal of particles of all residual water,

characterized in that the membrane is a semipermeable membrane.

11. The method according to claim 10, in which an aqueous emulsion or not miscible with water, the liquid is at the stage a) consists of the active component and in which it is not miscible with water, the liquid is absorbed hydrophobic polymer, where the resulting particles contain the active component, captured by the core.

12. The method according to claim 10 or 11, in which the shell forming interfacial polycondensation reaction is essentially oil-soluble first reagent interfacial polycondensation with at least two first condensation groups, with almost water-soluble second reagent interfacial polycondensation with at least two second condensation groups, and this method includes combining the second reagent interfacial polycondensation with a water emulsion of a hydrophobic polymer before carrying out stage (a) of this method, followed by mixing the first reagent interfacial polycondensation to induce interfacial polycondensation reaction stage (b), and then conducting the reaction between the first and second reagents interfacial polycondensation with obtaining shell.

13 the Method according to any of PP-12, in which the core comprises a hydrophobic polymer derived from a hydrophobic monomer or mixture of monomers comprising From4-C30alkalemia ethers of ethylene-unsaturated carboxylic acid, preferably4-C30alkalemia esters of (meth)acrylic acid.

14. The method according to any of PP-13, in which the core includes at least two different polymeric substances.

15. The method according to any of PP-14, in which the emulsifier is an oil-soluble or swelling in oil amphiphilic polymer stabilizer.

16. The method according to any of PP-15, in which the emulsifier is a polymeric and contains repeating hydrophobic group and a repeating reactive hydrophilic groups, which before being mixed with the first reagent interfacial polycondensation contact with the second condensation groups of the second reagent interfacial polycondensation.

17. The method according to any of p-16, in which the mixing of the first reactant interfacial polycondensation is conducted by mixing the dispersion and the first reagent interfacial polycondensation in the conditions in which the mass ratio between the variance and the first reagent interfacial polycondensation during the entire process of mixing remains almost constant.

18. The method according to any of PP-17, which is not miscible with water is the first liquid is a hydrocarbon liquid, containing no halogenated hydrocarbon.

19. The method according to any of PP-18, in which a water-soluble reagent interfacial polycondensation is an amine, an oil-soluble reagent interfacial polycondensation is an acid or acid derivative and a hydrophobic polymer is a condensation polymer, which is a polyamide.

20. The method according to any of PP-19, in which a water-soluble reagent interfacial polycondensation is Diethylenetriamine.

21. The method according to any of PP-20, in which oil-soluble reagent interfacial polycondensation is terephthaloylchloride.

22. The method according to any of PP-21, in which the average particle diameter is in the range of from 0.5 to 30 μm.

23. The method according to any of PP-22, in which the emulsifier is a polymeric and contains lateral carboxyl group, and the second reagent interfacial polycondensation is an amine.

24. The method according to any of PP-23, in which the emulsifier is a statistical copolymer obtained by copolymerization in a mixture of ethylene-unsaturated hydrophilic and the ethylene-unsaturated hydrophobic monomers.

25. The method according to any of PP-24, in which the emulsifier is a statistical copolymer of at least one ionic ethylene-what easymanage monomer and at least one nonionic water-insoluble ethylene-unsaturated monomer.

26. The method according A.25, in which ionic monomer selected from acrylic acid, methacrylic acid and maleic acid or anhydride, and a nonionic monomer selected from styrene and aliphatic fatty ethers of ethylene-unsaturated carboxylic acid.

27. The method according to any of p-26, in which the emulsifier becomes covalently associated with the outer surface of the particles.

28. The method according to item 27, in which the emulsifier contains reactive groups are epoxy or hydroxyl, and the covalent bond is a simple ester or reactive groups are amino groups, and covalent bond is an amide, or a reactive group represent the remains do not contain carboxylic acid groups or anhydrides, or golodnikov or salts and covalent bond is an ester or amide.

29. The method according to any of PP-28, in which the emulsifier is a copolymer of a hydrophilic monomer unit, including parts of the anhydride of dicarboxylic acid, and a hydrophobic monomer unit.

30. The method according to any of PP-29, in which the emulsifier is a speed obtained by the polymerization of the polymer of the hydrophobic monomer unit and a hydrophilic monomer unit, where hydrophobic monomer units include links to hostalkova containing carboxylic acid groups or salts of acids residues and reactive monomer units, selected from glycidyloxy monomer unit and anhydrous Monomeric units.

31. The method according to any of PP-30, in which the hydrophobic polymer core can absorb hydrophobic liquid.

32. A stable dispersion of powder particles according to claim 1, used in liquid media as carriers of active substances in which the particles are evenly distributed in the first hydrophobic liquid in which the particles include a core within the shell and the core layer includes a hydrophobic polymer containing absorbed them a second hydrophobic liquid, wherein the membrane is a semipermeable membrane.

33. Variance p, in which the first and second liquids have approximately the same density.

34. Variance p or 33, in which the particles comprise the active substance.

35. Variance 34, in which the active substance is chosen from the group comprising aromatic oils, lubricating oils, essential oils, wax inhibitors, dyes, corrosion inhibitors, vitamins, active ingredients for print and obtain images for the manufacture containing no pigment transfer paper, industrial adhesives, sealants, fillers, paints, catalysts, pore-formers, solvents, agrochemical funds act is their substances for food and feed, the pharmaceutical agents, antioxidants, catalysts migration of the dye and cosmetics.

36. Dispersion according to any one of p-35, in which the second hydrophobic liquid comprises two or more components, and the core includes at least two different hydrophobic polymer.

37. Dispersion according to any one of p-36, in which the particles prepared according to the method according to any of PP-31.

38. Method of preparation of a stable dispersion of particles according to claim 1, which are evenly distributed throughout the first hydrophobic liquid, comprising the following stages:

(a) preparation of a powder composition comprising particles which have a core comprising a hydrophobic polymer inside the shell;

(b) the dispersion of these particles in the second hydrophobic liquid in which the hydrophobic polymer is soluble or able to swell and which is characterized by approximately the same density as the first hydrophobic liquid;

(C) providing sufficient time for the second hydrophobic liquid is absorbed into the hydrophobic polymer core;

(g) the transfer of particles comprising a second hydrophobic liquid, prepared in stage (b), the first hydrophobic liquid;

characterized in that the membrane is a semipermeable m is mbrane.

39. The method according to § 38, in which the first and second liquids is essentially the same substance.

40. Method for controlling release of the active substance, comprising placing the substrate or the environment, which should be released active substance, a dispersion of powder particles according to claim 1, comprising particles which have a core comprising a hydrophobic polymer inside the shell, and the material of this hydrophobic core contains the active ingredient, characterized in that the membrane is a semipermeable membrane.



 

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FIELD: colloid chemistry.

SUBSTANCE: method comprises dispersing water emulsion of hydrophobic polymer in a liquid immiscible with water containing emulsifier, producing the emulsion with enriched phase that comprises water dispersed phase containing the hydrophobic polymer, and inducing inter-phase reaction of polycondensation at least of one of the reagents of the inter-phase polycondensation to produce polymeric film around the hydrophobic polymer.

EFFECT: enhanced efficiency.

40 cl, 5 ex

FIELD: polymer materials.

SUBSTANCE: invention relates to cross-linkable polymeric binders, in particular to microcapsulated binders and produce containing such microcapsulated binder, and discloses composition of microcapsulated binder characterized by that binder forms in situ in capsules and comprises: essentially water-insoluble binder-forming material of core, which core includes at least first addition-type prepolymer, vitrification temperature of homopolymer Tg being less than about 0°C, inflammation temperature at least 75°C, and boiling temperature at least 175°C (at atmospheric pressure); solvent for binder-forming material of core, said solvent being essentially water-soluble and not reacting with prepolymer material; essentially water-insoluble free-radical-initiating substance in amount high enough for efficient catalysis, said substance being, in particular, azo-type initiating substance with half-life period at least 1 h at 25°C, which is soluble in prepolymer material to be polymerized and in solvent. Microcapsules are prepared by composing aqueous mixture comprising colloidal dispersion of microcapsule wall-forming material. In order to obtain core material particles less than about 250 μm in size, aqueous solution is subjected to vigorous stirring. Stirring at a first temperature leads to formation of microcapsule wall from microcapsule wall-forming material, while heating to a second temperature provides polymerization of prepolymer material of the core to form binder in microcapsule. Formation of the binder in microcapsule as well as microcapsuled binder composition and substrate are also described.

EFFECT: simplified binding of microcapsuled material.

56 cl, 2 tbl, 18 ex

FIELD: cattle breeding; methods of the fodder production.

SUBSTANCE: the invention is pertaining to microballs containing the derivative of pleuromutiline and the method of their production and also to production of the fodder granules containing the microballs and to the method of their production. The microballs have the average size from 1 micron up to 5000 microns and represent the polymeric matrix particles, where the polymeric compound is selected from the shellac, the polymeric compound on the basis of cellulose, the acrylic acid or the methacrylic acid, the maleic anhydride, polyvinyl pyrrolidone or polyvinyl alcohol, and which is highly dispersed in the solid or liquid form with the derivative of pleuromutiline of formula 1 or its physiologically tolerable acid-additive salts and quarternary ammonium salts: , where R1 means vinyl, between 1 and 2 carbonic atoms there is a single bond, and Ra and Rb mean each separately from each other hydrogenen or halogen, and Т represents -CH2-S-(CH2)K-N(R5)(R6), where "k" means the integer from 2 up to 5; R5 andR6 mean each separately from each other C1-C6-alkyl or Т represents -CH2-S-C(CH3)2-CH2-NH-C(O)-CH(NH2)-CH(CH3)2. The method of preparation of the microballs includes production the polymer solution selected from the shellac, the polymetric compound on the basis of cellulose, the acrylic acid or methacrylic acid, the maleic anhydride, polyvinyl pyrrolidone or polyvinyl alcohol, by dissolution of the shellac, the polymetric compound in the organic solvent, having the low affinity to the paraffinic oil or the organosilicic oil and with the dielectric constant from 10 up to 40, with addition of the water. Then the produced solution is introduced at intermixing with the derivative of the pleuromutiline and receive the first organic phase, which is not admixed with the paraffinic oil or the organosilicic oil. The first organic phase introduce at the intense intermixing into the second phase consisting of the paraffinic oil or the organosilicic oil, and prolong intermixing of the produced mixture until the microballs are formed at evaporation or the solvent removal. The microballs are separated, flushed and dried. The fodder granules for the livestock includes the effective number of the indicated above microballs, the milled dry fodder on the vegetable or animal base with or without the additives, such as proteins, vitamins and minerals. The method of preparation of the fodder granules includes the careful intermixing of the microballs with the organic, ground and homogenized components of the fodder. Then they add the water or the steam in the mixture in the amount from 5 up to 10 % of the total mass, press the mixture in the fodder rods at the heightened temperatures from 60 up to 80°С, and divide the rods into the fodder granules. The invention ensures stabilization of the pleuromutiline, which stays undamaged at the granules preparation and is kept safe for the rather long duration of storage.

EFFECT: the invention ensures stabilization of the pleuromutiline, which stays undamaged at the granules preparation and is kept safe for rather long duration of storage.

6 cl, 3 tbl, 3 ex

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EFFECT: improved writing quality and economic and environmental advantages.

33 cl, 1 dwg, 4 ex

FIELD: encapsulation of solid materials.

SUBSTANCE: method comprises forming a shell made of encapsulating material on the surface of the grain material when grain material and encapsulating material flow through the piping chamber. The material is transported and capsulated under the action of the spiral member rotating with a speed of 50-3000 rev/min. The length of the spiral member and piping chamber ranges from 5 to 100 of the lateral sizes of the chamber.

EFFECT: enhanced efficiency.

1 tbl, 3 ex

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