Microcapsules with water or water solution (versions) and method of their production (versions)

FIELD: process engineering.

SUBSTANCE: invention maybe used for efficient fire extinguishing, fast cooling of overheated structures and production of lower-flammability compounds. Microcapsules have a micro-sphere-like core containing water or water solution in gel state, main shell around said core to provide for core stable shape and composition and rule out water evaporation therefrom the core, and, additionally, comprises outer shell with lyophilic properties. Versions of proposed methods comprises producing aforesaid core via interaction of appropriate initial water solutions to be placed in microsphere and containing appropriate components of the shell with components of solutions to be precipitated and used for producing and cross-linking of gel, and producing additional lyophilic shell via interaction of components of initial solutions with appropriate components in organic medium.

EFFECT: high efficiency in fire extinguishing or fast cooling of overheated structures.

21 cl, 1 tbl, 10 ex

 

The invention relates to microcapsules containing water or aqueous solutions, and methods of microencapsulation of water or aqueous solutions for various applications, more specifically, to obtain "dry" or "loose" water in the form of microcapsules containing water or aqueous solutions are used, in particular, for effective suppression of fire, overheating protection of industrial reactors, obtaining compounds with low Flammability, and may find application in other industries, such as food, pharmaceutical industries and in the production of mineral fertilizers.

Water, due to the unique physico-chemical properties and high prevalence in nature and, accordingly, cheapness, has always been the primary means of fire fighting.

Of all known liquids (under normal conditions) water has the highest heat of vaporization, which largely determines its effectiveness in the fight against fire. In addition, the water is completely non-toxic, including in the conditions of fire, and does not introduce toxic or corrosive components in the combustion products.

However, water as the extinguishing agent has a number of disadvantages.

Due to the rapid development of electrical engineering and electronics, objects which is now full of industry and everyday life, to apply water to fight the fire was dangerous because of its conductivity, what causes short circuits and damage expensive equipment.

The ability of water to quickly flow to penetrate into the gaps, cavities and absorb much of the material leads to damage of documents, books, valuables and equipment.

Due to rapid spill water cannot accumulate in the volume of the burning object, therefore, its consumption and the required feed rate is extremely high.

Therefore, in the second half of the XX century in the world was established industry for the production of new fire extinguishing agents in liquid and gaseous state on the basis of fluorinated and fluorine-bromodomain hydrocarbons.

Undoubtedly, these substances have a highly effective fire-extinguishing apparatus, based on the occurrence of heavy free radicals by thermal influence, which tear up the kinetic chain of the combustion process. These substances are also safe for electrical and electronic systems.

However, the cost of these products is high. Thus their degradation products were not only toxic to people directly, but also cause the destruction of the protective ozone layer of the Earth's atmosphere. This was the basis for an international ban (the Montreal Protocol) the production and application of some of these products used for fire extinguishing systems fire safety

So the problem is the ability to extinguish fires "dry" water, which does not cause destruction of documents and books, electronic devices, does not cause short circuits in electrical systems, it is essential.

In addition, the "dry" water can be used preventively in situations of overheating chemical and nuclear reactors and the threat of a thermal explosion. The reactor is overheating, you may be bombarded with a large number of "dry water", and you can create a high mound up to fill the entire volume of the working space.

Packaging with the "dry" water allow to solve the problems with the transportation of water in its scope. For example, the packaging with the "dry" water can be discharged from the aircraft, because there is no water hammer, resulting in the destruction of the tanks with liquid water, which is important in the delivery of water in emergency zones. Packaging with the "dry" water can be used in conditions of weightlessness.

There are various ways to obtain "dry" or "loose" water through the formation of polymeric microcapsules containing water.

For example, the American company 3M offered samples of an aqueous solution of fertilizers (nitrates, phosphates) in the form of microcapsules having a shell made of low-melting polyethylene (Ave the t company "3M", 1974). By the nature of the microcapsules can be assumed that for the production of microcapsules was used the way "tube in tube"applied in inverted form to obtain capsules with fat-soluble vitamins, sedatives, solution of nitroglycerin and similar substances. However, this method is only suitable for small-scale production. The obtained microcapsules company "3M" were fragile and quickly lost the form.

A known method of producing microcapsules in which as the core of a slurry of microcapsules using a crystalline salts (DE, 102005002169, AND). This microencapsulation perform fusible material having a melting temperature higher than the crystalline. The water content is not specified, however, in the known crystalline, it does not exceed 50% by weight, which is not effective for fire suppression. Furthermore, the presence of salts leads to the corrosive effect on objects.

There are also known methods of encapsulation of aqueous solutions of drugs, biologically active substances and cultures.

For example, a method of obtaining microencapsulated pharmaceutically active agent, comprising: dispersing an aqueous solution of the pharmaceutically active agent in the solution containing the organic solvent of the polymer and the polymer are dissolved in it, which is of primary emulsion water in oil"; mixing the primary emulsion with an aqueous external phase containing water and a surfactant, and, in terms of air flow over the mixture, dispersing the specified primary emulsion in the specified external water phase to obtain a product containing microencapsulated pharmaceutically active agent dispersed in a mixture of (US, 6204308, In). The polymer used polietilensorbit, and the specified microencapsulated pharmaceutically active agent contains a coating, a matrix or shell from polietilensorbit. However, the resulting product has a chaotic distribution of the active agent due to the uneven distribution of polietilensorbit in its volume and may be on the surface membrane of uneven thickness, which, on the one hand, leads to unpredictability release agent, on the other hand, does not provide a guaranteed content of microcapsules agent, the said shell or coating is resistant to water and do not prevent the evaporation of water contained in the microparticles. This method is characterized by instability and multi-stage process, in this connection, it is difficult to industrial implementation.

A method of obtaining chitosan/alginate microparticles, comprising: spray drying of water is about solution containing a biologically active agent, and sodium alginate, through the nozzle at a temperature of 140C, to obtain the microparticles; and their subsequent joining of calcium chloride in 3%solution of acetic acid under stirring and subsequent immersion crosslinked microparticles in a solution of chitosan or poly-1-lysine in 3%acetic acid solution, then the obtained microparticles are separated by centrifugation, washed with distilled water and dried at room temperature. The obtained microparticles have a spherical shape with a glossy surface. The stitching was applied to increase the number of individual generowania particles inside the shell (Burka May A. Atilla Hincal, Skid Senel. Obtaining chitosan/alginate microparticles for mucosal vaccination. 15th international Symposium on Microencapsulation, Parma, Italy, September 18-21, 2005, str-330; Burcu Sayim A., Atilla Hincal, Scyda Senel. Preparation chitosan-alginate microparticles for mucosal immunization. 15th International Symposium on Microencapsulation, Parma (Italy), September 18-21, 2005, p.329-330). However, the content of the aqueous solution obtained in the microparticles is about 15%, which is associated with significant evaporation of water when spraying the original aqueous solution at temperatures above 100C. in Addition, complex compounds "chitosan-alginate", formed by the remaining alginate after crosslinking by calcium ions free Carbo is strong groups are unstable to water and do not prevent the evaporation of water contained in the microparticles.

Known lysozyme-containing chitosan-coated microspheres obtained by the method of successive emulsification in environments with a mass ratio per unit volume: 4%content of alginate 0,1%content of chitosan, 15%content of calcium chloride, 20%content of lysozyme and 10%content activated by heating Vibrio anguillarum (Torsin, Mu Cecchetto, Dvoynoy, Marcucci, Difilippo-Greek, Casarsa, Kalloni and Gsave. Lysozyme-containing chitosan-coated microspheres for oral vaccination. 15th international Symposium on Microencapsulation, Parma, Italy, September 18-21, 2005, p.153-154; L.Zorzin, M.Cocchietto, D.Voinovich, A.Marcuzzi, J. Fillipovich-Grcic, C.Casarsa, C.Mulloni and G.Sava. Lysozime-containing chitosan-coated alginate microspheres for oral immunization. 15th International Symposium on Microencapsulation, Parma (Italy), September 18-21, 2005, p.153-154). However, complex compounds "chitosan-alginate", formed by the carboxyl groups remaining free in the alginate after crosslinking by calcium ions are unstable to the action of water, do not prevent the evaporation of water contained in the microparticles, while the storage.

In addition, due to the uneven distribution of free carboxyl groups in the surface layers of crosslinked microparticles shell thickness is C complexes of chitosan-alginate" is also not the same, and microparticles have a high polydispersity.

A known method of producing microcapsules (WO 2005/018794 or GB 2388581, And; or RU, 2006108860, AND having a solid hydrophobic membrane containing dispersed water in the form of drops or droplets, which are optionally encapsulated in a specified shell or with its help, and the active ingredient or ingredients are dissolved or embedded in encapsulated drop or drops, including the following steps:

a) obtaining the aqueous phase and one or more active ingredients dissolved or embedded in the aqueous phase;

b) obtaining a hydrophobic phase in molten form;

c) dissolving or implementation kapsulirujushchej material or mixture kapsulirujushchej materials specified in the aqueous phase or in a hydrophobic phase;

d) combining the above aqueous and hydrophobic phases and homogenization or mixing of the phases with obtaining emulsion water in oil";

e) encapsulating the aqueous phase in the emulsion, resulting in forming a dispersion comprising dispersed water droplets, and thus the active ingredient or active ingredients encapsulated in droplets of water;

f) processing the dispersion obtained in step (e), for the formation of microcapsules, in which the encapsulated water droplets, in addition, encapsulated in utverzhdennuyu hydrophobic membrane or using it.

the ri this microcapsule is produced by spraying a specified emulsion water in oil when cooled. While in the specified method of the aqueous phase is chosen from the group consisting of water or a mixture of water and any mixing with the water solvent, such as ethanol, ethylene glycol, glycerin. This hydrophobic phase is chosen from the group consisting of animal oils and fats, fully hydrogenated vegetable or animal oils, hydrogenated unsaturated monoglycerides of fatty acids and other materials.

This kapsulirujushchej material selected from the group consisting of hydrocolloids, such as sodium alginates, gum Arabic, glue, starch, modified starch, guar gum, agar glue, pectin and other adhesives, chitosan, xanthan gum, gelatin, hyaluronic acid, cellulose derivatives, acrylic copolymers, soy protein, shellac, Zein, any synthetic or natural water-soluble polymers, any vadomarius microparticles as silicon dioxide, titanium dioxide, synthetic or natural granular polymer beads or any vadomarius solid particles that are acceptable to agglomeration (sintering).

Thus combining the aqueous phase with a hydrophobic phase can be made by mixing, homogenization - mixing with shear layers or linear mixing and encapsulation performed by coacervation or agglomeration, or melirovanie, or none.

If this is kapsulirovanie by coacervation can be used kapsulirujushchej material to increase its solubility by increasing the temperature, changes in pH, addition of hydrocolloids or any acceptable initiating the coacervation agent. And in this case kapsulirujushchej material selected from the group consisting of shellac, Zein, or synthetic or natural hydrophobic polymers, as fats, emulsifiers, waxes or mixtures thereof.

This encapsulation agglomeration can be accomplished with the use of solid particles as kapsulirujushchej material and microparticles, such as silicon dioxide, titanium dioxide, synthetic or natural granular polymer beads or other water-insoluble solid particles fused in a film surrounding aqueous phase.

This encapsulation can be carried out by melirovanie and melirovanie the aqueous phase in the emulsion can be made by lowering the temperature of the emulsion to a temperature of melirovanie kapsulirujushchej material, as kapsulirujushchej material select material from the group consisting of generouse hydrocolloids such as gelatin, starch, agar glue and other.

In addition, encapsulation of the aqueous phase can be achieved through blending using kapsulirujushchej material selected from the group consisting of proteins, gelatin, starches, chitosan, cellulose derivatives, synthetic or natural water-soluble polymer acceptable for the Sevki heating, knitting with the change of the acid-base state of the environment or chemical processing, and mixtures thereof.

Obtained using the above method, one microcapsule may contain from 1 to 100 water drops placed in the hydrophobic shell matrix, and the active ingredient or active ingredients dissolved in water droplets or included in them.

However, in the above-described method of producing microcapsules multi-stage multi-technology makes the method complicated when implemented in production. In addition, when spraying the emulsion water in oil" for the formation of a shell around the aqueous droplets of the aqueous phase, having a tendency to agglomerate, forming a thick skin, which occupies a significant place in the volume of the microcapsules. Thus obtained microcapsule contains water in an amount of not more than 50% by weight, and the shell contains wax, grease and other combustible substances, which, in aggregate, excludes the possibility of using the obtained microcapsules as a fire-extinguishing means.

In addition, the method of producing microcapsules by spray predetermine the high polydispersity of the obtained microcapsules that the use of such microcapsules in conditions of high temperatures leads to non-simultaneous release of water from them and, therefore, inefficient evaporation of water, which then prevents the use of such microcapsules to extinguish or cooling protected from overheating objects.

When developing the present invention was tasked with creating a slurry of microcapsules for maximum efficiency target to use any water in them, including extinguishing fires or for rapid cooling of objects, such as reactors when abnormal overheating, and thus should be achieved qualitative and quantitative indicators of microcapsules:

the content of water or aqueous solution in microcapsules should be the maximum possible, almost - not less than 90 mass%,

- the content of the combustible part, which is determined by the mass of the shell, in the microcapsule must be minimized and thus the microcapsules should be strong, dry and infusible,

the polydispersity of the finished microcapsules (range of sizes) should be minimized so that when the critical temperature of the release of water or aqueous solution, the effect of the release (evaporation) of water was simultaneous (co-op).

Was also tasked with creating formative core of the microcapsules, ensures retention of water or aqueous solution uniformly in the whole volume of the nucleus, while the spherical shape of the nucleus with a uniform pressure distribution of the water or aqueous solution from the inside to the surface of the sphere, also most ramlau for posting on it shell of uniform thickness.

In addition, the task was the development of a microcapsule containing core water or an aqueous solution and having a membrane that prevents water evaporation from the kernel.

Was also tasked to provide for increased wettability of the outer surface lyophilic liquid through the creation of additional shells on the surface of the microcapsules. This is important when applying a slurry of microcapsules as fillers, for example, polymer compounds having low Flammability.

It is known that increasing the wettability of the surface of the filler liquid polymer matrix (decrease in contact angle) leads to the possibility of increasing the degree of filling, which is important to improve the resistance of the materials to ignition and spread of flame when filling the microcapsules with water. In addition, after curing provides a higher strength of the compound, which is an important technical feature. Therefore, the achievement of freeze-drying the surface of the microcapsules with water is an essential task for their use as fillers in polymer compounds with low Flammability.

In the claimed invention was also given the task of developing methods for producing microcapsules containing water or an aqueous solution, allowing forms which illustrate the same size melirovanie drops of an aqueous solution (aqueous microspheres), coated their shell, preventing the evaporation of water during storage, and have a sustainable strength, good flowability and high water content.

The task was solved by the creation of microcapsules containing water or an aqueous solution in generowania condition, having a core in the form of microspheres containing water or an aqueous solution, melirovanie using crosslinked by calcium ions dissolved in the specified water or aqueous solution gel electrolytes having a carboxyl group.

Thus according to the invention, the microcapsule as mentioned gelling polyelectrolytes may contain sodium alginate, and/or pectin, and/or gum Arabic, and/or any other polysaccharides containing carboxyl groups.

The task was solved by the creation of microcapsules containing water or an aqueous solution in generowania condition, having a core in the form of microspheres containing water or an aqueous solution, melirovanie using crosslinked by calcium ions dissolved in the specified water or specified aqueous solution of a gelling polyelectrolytes having a carboxyl group, and having on the surface of the microspheres primary shell, preventing evaporation contained in the specified kernel of water.

Thus according to the invention, the microcapsule as specified Geleos asousi polyelectrolytes may contain sodium alginate, and/or pectin, and/or gum Arabic, and/or any other polysaccharides containing carboxyl groups.

Thus according to the invention it is reasonable that the main shell of the microcapsules has a thickness, the minimum required to prevent evaporation contained in the kernel of water.

In addition, according to the invention it is expedient that the main shell has been formed is placed on the outer surface of the specified core complex compounds of high molecular weight first acomponent who are bearers of the same charge, high molecular weight second acomponentname who are carriers of opposite charge.

Thus according to the invention it is desirable that the main shell was formed complex compounds of high molecular weight first acomponent having negative charges on the polymer molecule with high molecular weight second acomponentname having positive charges on the polymer molecule.

In addition, according to the invention it is desirable that the main shell was formed complex compounds of high molecular weight first acomponent having negative charges on the polymer molecule due to the presence of carboxyl groups with high molecular weight second acomponentname having positive charges on the polymer molecule for the odd presence of amine groups.

Thus according to the invention it is desirable that the main shell was formed complex compounds acatitla cellulose with chitosan.

In addition, according to the invention, it is possible that the main shell was formed complex compounds of polyacrylic acid and polyvinylpyrrolidone.

The task was solved by the creation of microcapsules containing water or an aqueous solution in generowania condition, with the core in the form of microspheres containing water or an aqueous solution, melirovanie using crosslinked by calcium ions dissolved in the specified water or specified aqueous solution of a gelling polyelectrolytes having a carboxyl group and having a primary shell on the surface of the microspheres, preventing evaporation contained in the specified core water, and additional outer shell having lyophilic properties. Thus according to the invention, the microcapsule as mentioned gelling polyelectrolytes may contain sodium alginate, and/or pectin, and/or gum Arabic, and/or any other polysaccharides containing carboxyl groups.

Thus according to the invention, it is wise to main shell of the microcapsules has a thickness, the minimum required to prevent evaporation contained in the kernel of water.

To the ome, according to the invention it is expedient that the main shell has been formed is placed on the outer surface of the specified core complex compounds of high molecular weight first acomponent who are bearers of the same charge, high molecular weight second acomponentname who are carriers of opposite charge.

Thus according to the invention it is desirable that the main shell was formed complex compounds of high molecular weight first acomponent having negative charges on the polymer molecule with high molecular weight second acomponentname having positive charges on the polymer molecule.

In addition, according to the invention, it is desirable that the main shell was formed complex compounds of high molecular weight first acomponent having negative charges on the polymer molecule due to the presence of carboxyl groups with high molecular weight second acomponentname having positive charges on the polymer molecule due to the presence of amine groups.

Thus according to the invention it is desirable that the main shell was formed complex compounds acatitla cellulose with chitosan.

In addition, according to the invention, it is possible that the main shell was formed complex soy is inanami polyacrylic acid and polyvinylpyrrolidone.

Thus, according to the invention, it is expedient to provide additional outer shell was formed by polycarbamide.

Thus, according to the invention, it is possible that additional outer shell was formed by polimochevinnykh.

Thus, according to the invention described microcapsules have a diameter in the range from 0.25 to 5.0 mm with a distribution of diameter not less than 90% and contain water or an aqueous solution in an amount of not less than 90% by weight of microcapsules.

Thus the microcapsules according to the invention may include aqueous solutions, including useful features such as therapeutically useful substances, suspensions cultures of microorganisms, and other components that are compatible or inert with respect to these polyelectrolytes and cocomponent.

The task was solved by the creation of a method of microencapsulation of water or aqueous solutions to produce microspheres containing water or an aqueous solution, melirovanie using crosslinked by calcium ions dissolved in the specified water or an aqueous solution of a gelling of the electrolyte, which includes the following steps:

a) obtaining a source of an aqueous solution containing dissolved in water, at least a gelling polyelectrolytes having a carboxyl group;

b) obtaining oshivelo aqueous solution, soteriades is dissolved in it, at least one source of divalent calcium ions;

c) the introduction of the original aqueous solution obtained in stage a), in osiewalsi aqueous solution obtained in stage b), drops under stirring oshivelo solution at 20-25C for a time sufficient to education in asarualim the dispersion solution containing the microspheres, in which the initial aqueous solution is in the form of a gel formed gel polyelectrolytes obtained in stage a), made of divalent calcium ions, obtained in stage b);

d) isolation of the microspheres obtained in step (C), of the variance oshivelo solution by filtration;

e) placing the resulting microspheres in a tightly closed container, drained dry.

Thus according to the invention it is expedient as mentioned gelling polyelectrolytes to use sodium alginate, and/or pectin, and/or gum Arabic, and/or other polysaccharides containing carboxyl groups, as a source of divalent calcium ions to use aqueous solutions of calcium dichloride, and/or calcium lactate and/or calcium glycerol, and/or any other water soluble calcium salts.

The task was solved by the creation of a method of microencapsulation of water or aqueous solutions to produce microcapsules with the poison is in the form of microspheres, containing generowania the condition of water or aqueous solution, and the primary shell, preventing evaporation contained in the kernel of water, comprising the following steps:

a) obtaining a source of an aqueous solution containing dissolved in water, at least a gelling polyelectrolytes having a carboxyl group, and a macromolecular first acomponent who are bearers of the same charge and acceptable for the formation of the primary shell;

b) obtaining oshivelo solution containing dissolved in water, at least one source of divalent calcium ions and macromolecular second acomponent carrying charge opposite to the above first acomponent obtained in stage a), and acceptable for the formation of the primary shell;

c) the introduction of the original aqueous solution obtained in stage a), in osiewalsi the solution obtained in stage b), drops under stirring oshivelo solution at 20-25C for a time sufficient to education in asarualim the dispersion solution containing the microspheres, in which the initial aqueous solution is in the form of a gel formed gel polyelectrolytes obtained in stage a), made of divalent calcium ions, obtained in stage b);

d) aging the dispersion, recip is authorized in step C), at 20-25C for a time sufficient for the formation of microcapsules having a core in the form of microspheres obtained in step (C)enclosed inside the main shell formed in a surface layer of microspheres complex compounds first acomponent primary shell, obtained in stage a), with the second acomponentname primary shell, obtained in stage b);

e) the selection of the microspheres obtained in step d), of oshivelo solution by filtration;

(f) washing the microcapsules obtained in stage e), and drying them in the air;

g) processing of microcapsules obtained in stage f), - caking agent;

h) placing the resulting microcapsules in a tightly closed container, drained dry.

Thus according to the invention it is expedient as mentioned gelling polyelectrolytes to use sodium alginate, and/or pectin, and/or gum Arabic, and/or other polysaccharides containing carboxyl groups.

Moreover, according to the invention is suitable as a source of divalent calcium ions to use aqueous solutions of calcium dichloride, and/or calcium lactate and/or calcium glycerol, and/or any other water soluble calcium salts.

Moreover, according to the invention is suitable as a first acomponent primary shell, which is what SITENAME same charge, to use high-molecular compounds having in the polymer molecule has a negative charge and as a second acomponent primary shell, which are carriers of the opposite charge, to use high-molecular compounds having in the polymer molecule has a positive charge.

Moreover, according to the invention is suitable as a first acomponent primary shell to use high-molecular compounds having negative charges on the polymer molecule due to the presence of carboxyl groups, and as a second acomponent primary shell to use high-molecular compounds having positive charges on the polymer molecule due to the presence of amine groups.

Thus according to the invention, preferably, as the first acomponent primary shell to apply acatitla cellulose, and as the second acomponent primary shell to apply chitosan.

In addition, according to the invention may be used as the first acomponent primary shell to use polyacrylic acid, and as a second acomponent primary shell to use polyvinylpyrrolidone.

The task was solved by the creation of a method of microencapsulation of water or aqueous solutions to produce microcapsules having a core in the form of microspheres which, containing water or the aqueous solution in generowania condition, the primary shell, preventing the evaporation is contained in the kernel of water, and additional shell having lyophilic properties, comprising the following steps:

a) obtaining a source of an aqueous solution containing dissolved in water, at least a gelling polyelectrolytes having a carboxyl group, and a macromolecular first acomponent acceptable to the formation of the primary shell, which is the same charge carriers;

b) obtaining oshivelo solution containing dissolved in water, at least one source of divalent calcium ions and macromolecular second acomponent acceptable to the formation of core-shell carrying charge opposite to the above first acomponent obtained in stage a);

c) the introduction of the original aqueous solution obtained in stage a), in osiewalsi the solution obtained in stage b), drops under stirring oshivelo solution at 20-25C for a time sufficient to education in asarualim the dispersion solution containing the microspheres, in which the initial aqueous solution is in the form of a gel formed gel polyelectrolytes obtained in stage a) and sewn dwuhvalentnami calcium, obtained in step b);

d) aging the dispersion obtained in stage C)at a temperature of 20-25C for a time sufficient for the formation of microcapsules having a core in the form of microspheres obtained in step (C)enclosed inside the main shell formed by the interaction in the surface layer of the microspheres of the first acomponent obtained in stage a), with the second acomponentname obtained in step b);

e) the selection of the dispersion treated in step d), the filtering of the microcapsules obtained in stage d) and containing on the outer surface of the primary shell trace amounts of water for use in the future as the first acomponent when forming the additional outer shell;

f) obtaining an organic medium containing a volatile organic liquid which is injected second acomponent acceptable to the formation of additional shell having lyophilic properties, and dispersed catalyst, soluble in water, but insoluble in organic liquids;

g) introduction of microcapsules obtained in stage e), in an organic environment, obtained in stage f), with stirring to obtain a dispersion of these particles in the specified organic environment;

h) exposure of the dispersion obtained in step (g)at a temperature of 20-25C during the time sufficient for the formation on the outer surface of the microcapsules contained in the dispersion obtained in step (g), and having a core in the form of microspheres containing water or an aqueous solution, surrounded by a main shell having on the surface trace amounts of water, the outer is more lyophilic shell when the interaction of these first acomponent additional membrane in the form of trace quantities of water obtained in stage e), with the second acomponentname additional membrane obtained in step f), in the presence of the specified catalyst;

k) the allocation of microcapsules obtained in step h), from the organic medium by filtration;

m) washing the microcapsules obtained in step k), the same volatile organic liquid used in step (f);

n) placing the microcapsules obtained in step m), in a tightly closed container, drained dry.

Thus according to the invention it is expedient as mentioned gelling polyelectrolytes in stage a) use sodium alginate, and/or pectin, and/or gum Arabic, and/or other polysaccharides containing carboxyl groups.

Moreover, according to the invention is suitable as a source of divalent calcium ions in step (b) to apply aqueous solutions of calcium dichloride, and/or calcium lactate and/or calcium glycerol, is/or any other water soluble calcium salts.

Moreover, according to the invention is suitable as a first acomponent primary shell, which is the same charge carriers, to use high-molecular compounds having in the polymer molecule has a negative charge and as a second acomponent primary shell, which are carriers of the opposite charge, to use high-molecular compounds having in the polymer molecule has a positive charge.

Moreover, according to the invention is suitable as a first acomponent primary shell to use high-molecular compounds having negative charges on the polymer molecule due to the presence of carboxyl groups, and as a second acomponent primary shell to use high-molecular compounds having positive charges on the polymer molecule due to the presence of amine groups.

In addition, according to the invention, preferably, as specified first acomponent primary shell to apply acatitla cellulose, and as mentioned second acomponent primary shell to apply chitosan.

In addition, according to the invention is possible as these first acomponent primary shell to use polyacrylic acid, and as mentioned second cocomponent the basis of the shell to apply polivinilpirrolidon.

Thus according to the invention, preferably, as specified organic medium in step (f) to use carbon tetrachloride or dimethylcarbonate.

Thus according to the invention it is advisable to obtain a microcapsule having an extra shell formed by polycarbamide. Thus according to the invention, preferably, as a second acomponent additional shells to use a polyisocyanate or a mixture of MDI with toluylenediisocyanate.

Moreover, according to the invention is suitable as a catalyst to use phosfolan, preferably, 1-oxo-1,3-dimethylphosphate.

The task was solved by the creation of a method of microencapsulation of water or aqueous solutions to produce microcapsules having a core in the form of microspheres containing water or the aqueous solution in generowania condition, the primary shell around the core and additional outer shell having lyophilic properties, comprising the following steps:

a) obtaining a source of an aqueous solution containing dissolved in water, at least a gelling polyelectrolytes having a carboxyl group, macromolecular first acomponent who are bearers of the same charge and acceptable for the formation of the primary shell, and the first acomponent, Raplamaa to provide an additional lyophilic shell;

b) obtaining oshivelo solution containing dissolved in water, at least one source of divalent calcium ions and macromolecular second acomponent acceptable to the formation of core-shell carrying charge opposite to the above first acomponent primary shell, obtained in stage a);

c) the introduction of the original aqueous solution obtained in stage a), in the specified osiewalsi the solution obtained in stage b), drops under stirring oshivelo solution at 20-25C for a time sufficient to education in asarualim the dispersion solution containing the microspheres, in which the initial aqueous solution is in the form of a gel formed gel polyelectrolytes obtained in stage a) and cross-linked divalent calcium ions, obtained in stage b);

d) aging the dispersion obtained in stage C)at a temperature of 20-25C for a time sufficient to obtain microcapsules having a core in the form of microspheres obtained in step (C)enclosed inside the main shell formed in a surface layer of microspheres in the interaction between the first acomponentname primary shell, obtained in stage a) and the second acomponentname primary shell, obtained in stage b);

e) isolation of the microcapsules, the floor is obtained in stage d), of the variance oshivelo solution by filtration;

f) obtaining an organic medium containing a volatile organic liquid which is injected second acomponent acceptable to the formation of additional shell having lyophilic properties;

g) introduction of microcapsules obtained in stage e), in an organic environment, obtained in stage f), with stirring to obtain a dispersion of microcapsules in an organic environment;

h) exposure of the dispersion obtained in step (g)at 20-25C for a time sufficient to obtain microcapsules having a core in the form of microspheres containing water or an aqueous solution in generowania state, surrounded by the main shell and more lyophilic sheath;

k) the allocation of microcapsules obtained in step h), from the organic medium by filtration;

m) washing the microcapsules obtained in step k), the same volatile organic liquid used in step (f);

n) placing the microcapsules obtained in step m), in a tightly closed container, drained dry.

Thus according to the invention it is expedient as mentioned gelling polyelectrolytes to use sodium alginate, and/or pectin, and/or gum Arabic, and/or other polysaccharides containing carboxyl groups.

Thus according to the invention teleshop the EIT as a source of divalent calcium ions to use aqueous solutions of calcium dichloride, and/or calcium lactate and/or calcium glycerol, and/or any other water soluble calcium salts.

Moreover, according to the invention is suitable as a first acomponent, the main shell, which is the same charge carriers, to use high-molecular compounds having in the polymer molecule has a negative charge and as a second acomponent primary shell, which are carriers of the opposite charge, to use high-molecular compounds having in the polymer molecule has a positive charge.

Moreover, according to the invention is suitable as a first acomponent primary shell to use high-molecular compounds having negative charges on the polymer molecule due to the presence of carboxyl groups, and as a second acomponent primary shell to use high-molecular compounds having positive charges on the polymer molecule due to the presence of amine groups.

Thus according to the invention, preferably, as the first acomponent primary shell to apply acatitla cellulose, and as the second acomponent primary shell to apply chitosan.

In addition, according to the invention may be used as the first acomponent primary shell to use polyacrylic acid, which as a second acomponent primary shell to use polyvinylpyrrolidone.

Thus according to the invention, preferably, as an organic environment to use carbon tetrachloride or dimethylcarbonate.

Thus according to the invention it is advisable to obtain a microcapsule having an extra shell formed by polimochevinnykh, and thus for the formation of additional shells to use as the first acomponent hexamethylenediamine were or polyethylenepolyamine and/or other di - and polyamine, soluble in water, and as the second cocomponent to use a polyisocyanate or a mixture of MDI with toluylenediisocyanate.

Methods of microencapsulation of water or aqueous solutions according to the invention with obtaining microspheres and microcapsules according to the invention is as follows.

In various embodiments, methods of microencapsulation according to the invention shall obtain microcapsules having only the microsphere, which serves as their core and containing the target product is water or an aqueous solution in generowania condition, or with the formation around the specified kernel one primary shell, or obtain microcapsules having as the core of the specified microsphere, with the formation of a nucleus of primary and secondary shells, providing the stability of the shape and composition of the microcapsules in different environments.

In some variations the tah ways to obtain microcapsules provide the formation of the primary shell simultaneously with the formation of the microspheres, that provides technically sound process of microencapsulation.

In other embodiments, the methods for producing microcapsules use located on the surface of microcapsules residual amount of water to provide an additional external lyophilic membranes, improving the performance properties of the microcapsules.

Using various aqueous solutions.

In the first method of microencapsulation to obtain microcapsules containing only microspheres, use:

- the original aqueous solution containing one or more gelling polyelectrolytes having a carboxyl group, preferably, sodium alginate, and/or pectin, and/or gum Arabic, and/or other polysaccharides,

- osiewalsi aqueous solution containing dissolved therein at least one source of divalent calcium ions, preferably, aqueous solutions of calcium dichloride, and/or calcium lactate and/or calcium glycerol, and/or any other water soluble calcium salts.

In the first variant of the second method of microencapsulation according to the invention for the production of microcapsules containing microspheres and is equipped with a main shell, use:

- the original aqueous solution containing one or more gelling polyelectrolytes having carboxyl groups, preferably lgint sodium, and/or pectin, and/or gum Arabic, and/or other polysaccharides, and dissolved the first high molecular acomponent future core shell microcapsules having the same charge, preferably acatitla cellulose;

- osiewalsi aqueous solution containing dissolved therein at least one source of divalent calcium ions, preferably aqueous solutions of calcium dichloride, and/or calcium lactate and/or calcium glycerol, and/or any other water soluble calcium salts, and dissolved in the second high molecular acomponent future core shell microcapsules having a charge opposite to the specified first acomponent primary shell, preferably chitosan.

In the second variant of the second method of microencapsulation according to the invention for the production of microcapsules containing microspheres and is equipped with a main shell, use:

- the original aqueous solution containing one or more gelling polyelectrolytes having carboxyl groups, preferably sodium alginate, and/or pectin, and/or gum Arabic, and/or other polysaccharides, and dissolved the first high molecular acomponent future core shell microcapsules having the same charge, preferably polyacrylic acid;

- osiewalsi aqueous solution containing dissolved therein, at least one source of divalent calcium ions, preferably aqueous solutions of calcium dichloride, and/or calcium lactate and/or calcium glycerol, and/or any other water soluble calcium salts, and dissolved in the second high molecular acomponent future core shell microcapsules having a charge opposite to the specified first acomponent primary shell, preferably polyvinylpyrrolidone.

In the first variant of the third way microencapsulation according to the invention for the production of microcapsules containing microspheres and provided with a main casing and an additional shell, use:

- the original aqueous solution containing one or more gelling polyelectrolytes having carboxyl groups, preferably sodium alginate, and/or pectin, and/or gum Arabic, and/or other polysaccharides, and dissolved the first high molecular acomponent future core shell microcapsules having the same charge, preferably acatitla cellulose;

- osiewalsi aqueous solution containing dissolved therein at least one source of divalent calcium ions, preferably aqueous solutions of calcium dichloride, and/or calcium lactate and/or calcium glycerol, and/or any other water soluble calcium salts is, and dissolved in the second high molecular acomponent future core shell microcapsules having a charge opposite to the specified first acomponent primary shell, preferably chitosan.

In the second variant of the third way microencapsulation according to the invention for the production of microcapsules containing microspheres, provided with a main casing and an additional shell, use:

- the original aqueous solution containing one or more gelling polyelectrolytes having carboxyl groups, preferably sodium alginate, and/or pectin, and/or gum Arabic, and/or other polysaccharides, and dissolved the first high molecular acomponent future core shell microcapsules having the same charge, preferably polyacrylic acid, and the first acomponent future additional shell, preferably di - or polyamine,

- osiewalsi aqueous solution containing dissolved therein at least one source of divalent calcium ions, preferably aqueous solutions of calcium dichloride, and/or calcium lactate and/or calcium glycerol, and/or any other water soluble calcium salts, and dissolved in the second high molecular acomponent future core shell microcapsules having a charge opposite from asanam first acomponent primary shell, preferably polyvinylpyrrolidone.

All methods of microencapsulation according to the invention, the source solution serves drops in pre-prepared osiewalsi aqueous solution. This osiewalsi the solution is stirred at a temperature of about 20-25C.

When immersed drops the specified source water solutions in the specified osiewalsi solution in the volume drops quickly happen diffusion of calcium ions and ion processes stitching gelling polyelectrolytes containing carboxyl groups, divalent calcium ions, resulting in the formation of a solid gel, forming a microsphere containing water or an aqueous solution of the desired composition, which can serve as the core of the microcapsules containing water or an aqueous solution.

Thus obtained slurry of microspheres may be used as an independent extinguisher, because without primary shell they quickly lose water and stick together during storage, and also lose flowability, which is an important property for such practical applications,

According to the invention in the methods of microencapsulation of water or aqueous solutions to obtain a microcapsule having a primary shell, preventing the evaporation of water from the core, around the obtained slurry of microspheres placed in osajima the General solution, simultaneously with the formation of the microspheres is formed and the main shell of the microcapsules.

When this occurs slower process of diffusion of macromolecular first and second acomponent forming the primary shell and representing the polyelectrolytes bearing opposite charges towards each other. The duration of the process of formation of the primary shell is limited by the speed of diffusion of the first acomponent primary shell formed from the water-containing microspheres and second acomponent primary shell of oshivelo solution to a surface layer formed of the water-containing microspheres, in which there is an interaction (complexation) between the said first and second acomponentname with education around melirovanie slurry of microspheres core shell microcapsules, preventing the evaporation of water from the kernel.

The process of formation of core shell microcapsules lasts about 1-2 hours, then it stops spontaneously, as formed the main shell prevents further diffusion of these cocomponent. This way of forming the shell allows you to receive the basic minimum required shell thickness, providing impeding the evaporation of water from the aqueous core of the microcapsules.

According to the scientists microcapsules, having a core in the form of microspheres containing generovanou water or melirovanie aqueous solution, and surrounding the microsphere primary shell, separated by filtration, treated with caking agent and placed in a tightly closed container, drained from moisture for storage. Microcapsules ready to use, for example, for fire extinguishing or cooling overheated objects.

According to the methods of microencapsulation of water or aqueous solutions according to the invention obtained as described above, the microcapsule containing water or an aqueous solution, can be provided with an additional outer lyophilic shell, placed on the surface of the primary shell.

For forming the outer additional lyophilic shell use the immersion of microcapsules, already having a primary shell, in an organic medium containing a volatile organic liquid which is injected second acomponent acceptable to the formation of additional shell having lyophilic properties, preferably a polyisocyanate or mixture of toluylenediisocyanate.

In the first variant of the third way as the first cocomponent to provide an additional lyophilic shell use trace amounts of water remaining on the outer surface of the primary shell after separation microcapsules dispersion by filtration, and ensure the interaction of the first and second acomponent additional shell in the organic medium in the presence of a catalyst, preferably in the form of dispersed, but not soluble in organic liquids, for example phospholane. In this embodiment, an additional outer lyophilic shell of the obtained microcapsules is formed by polycarbamide.

In the second variant of the third method according to the invention as the first cocomponent to provide an additional lyophilic shell in the original solution, prepared as in the first variant of the second method, in addition enter hexamethylenediamine were or polyethylenepolyamine and/or other di - and polyamine, soluble in water, and the interaction between these first and second acomponent (MDI or mixtures thereof with toluylenediisocyanate) will be formed without participation phospholane) additional lyophilic shell formed by polimochevinnykh.

The mechanism of formation of additional shell is as follows.

In terms of the first variant of the third way microencapsulation catalyst phosfolan contact the surface of microcapsules, on which there are trace amounts of water dissolved in them and catalyzes the reaction of interaction of these trace quantities of water with di - and polyisocyanat the AMI, diffusing to the surface of the microcapsules from the specified organic environment, and the result of this interaction is the formation of polycarbonite shell on the surface of the primary shell of the microcapsules.

In terms of the second variant of the third method of microencapsulation in the presence of the aqueous composition microspheres and others, in addition to water, the first acomponent additional shell di - and polyamines, on the surface of the microcapsules is also the reaction of their interaction with the second acomponentname additional shell di - and polyisocyanates, with the formation of the polyurea shell. In this organic environment with the microcapsules are mixed at a temperature of about 20-25C.

As education additional shell it creates a barrier to diffusion of the first and second acomponent towards each other, and the process stops. Thus, the process of obtaining additional shell is carried out to obtain the thickness, the minimum necessary to achieve the freeze-drying the surface of the microcapsules.

Then the obtained microcapsules having primary and secondary shell, washed with a solution of the same organic medium, preferably carbon tetrachloride or dimethylcarbonate, separate microcapsules by filtration and placed the x in tightly closed containers for storage.

Methods of microencapsulation of water or aqueous solutions according to the present invention for the formation of the cores of the microcapsules in the form of one microspheres, in which water or an aqueous solution of the desired composition is placed in the linked gel-like state, as well as providing the formation surrounding the aqueous core and additional shells that have the minimum required thickness, allow to obtain monodisperse microcapsules composition in a range of sizes (diameters) of from 0.25 to 5.0 mm with a high water content that it is almost impossible to obtain using other known methods to obtain slurry of microcapsules, such as technology spray or double emulsification.

Using methods of microencapsulation of water or aqueous solutions according to the invention allows to obtain microcapsules of a given diameter that can be achieved by using for the formation of drops of the original solution nozzles or needles having the corresponding diameter of the holes.

Microcapsules containing water or an aqueous solution obtained by the method of microencapsulation of water or aqueous solutions according to the invention, may have a distribution of 90-100% for a given diameter and contain 90-96% of water in weight of the microcapsules.

Methods of microencapsulation of water or water what's solutions according to the invention are characterized by low energy consumption, almost no wastewater, environmental safety and short-time process to obtain slurry of microcapsules that, in General, determine their economic feasibility.

Below are examples of the method of microencapsulation of water or aqueous solutions according to the invention to produce different finished products:

- examples 1-4, which shows the main options for obtaining cores of microcapsules - aqueous microspheres (for comparison of their properties with microcapsules containing microspheres as the core of the microcapsules);

examples 5-10, which describes ways to obtain microcapsules with a core in the form of a slurry of microspheres placed in the membranes, including:

examples 5-7 obtain microcapsules having a primary shell,

examples 8-10 obtain microcapsules having primary and secondary shell.

Obtained in examples 1-4 slurry of microspheres and obtained in examples 5-10 microcapsules were subjected to the following tests:

Test:

Distribute the microspheres or microcapsules with a layer thickness of 5.0 mm in an open Petri dish and observe the weight loss at a temperature of 20-22C during the day. (This test is introduced solely for comparison purposes and is not used to assess the stability of the product).

Test:

100 g of the microspheres or microcapsules room is up in the glass tightly closed container and see in a month for the emergence of exudate and lipomastia.

Example 1. Obtaining a slurry of microspheres (without shells)

Get the original aqueous solution by adding 96,0 ml of distilled water 4.0 g of sodium alginate and conduct its dissolution under stirring for 4-5 hours at 20-25C.

Get osiewalsi a solution consisting of 150 ml of 2.5%aqueous solution of calcium dichloride.

The specified source solution is injected drops in osiewalsi solution.

Formed slurry of microspheres containing aqueous solution, melirovanie contained in molecules of sodium alginate, crosslinked divalent calcium ions contained in asarualim solution, soak in asarualim the solution with stirring for about 20 minutes Then the microspheres are separated by filtration, washed with water and placed in a tightly closed container.

The diameter of the resulting slurry of microspheres of 2.0 mm, a water content of 96% by mass.

Microspheres when tested on the test And lose 28% by weight, test observed In the exudation and adhesion of particles.

Example 2. Obtaining a slurry of microspheres (without shells)

Get the original aqueous solution by adding 92.0 ml distilled water, 8.0 g of sodium alginate and conduct its dissolution under stirring for 4-5 hours at 20-25C.

Get osiewalsi solution consisting of 50 ml of 2.5%aqueous solution of calcium dichloride.

The specified source solution is injected drops in osiewalsi solution.

Formed slurry of microspheres containing aqueous solution, melirovanie contained in molecules of sodium alginate, crosslinked divalent calcium ions contained in asarualim solution, soak in asarualim the solution with stirring for about 20 min, the obtained microspheres are separated by filtration, washed with water and placed in a tightly closed container.

The diameter of the resulting slurry of microspheres of 5.0 mm, a water content of 90% by mass.

Microspheres when tested on the test And lose 24% by weight, test observed In the exudation and adhesion of particles.

Example 3. Obtaining a slurry of microspheres (without shells)

Get the original aqueous solution by adding 96,0 ml of distilled water 4.0 g of pectin and conduct its dissolution under stirring for 4-5 hours at 20-25C.

Get osiewalsi a solution consisting of 150 ml of 2.5%aqueous solution of calcium dichloride.

The specified source solution is injected drops in osiewalsi solution.

Formed slurry of microspheres containing aqueous solution, melirovanie contained pectin molecules made of divalent calcium ions contained in asarualim solution, soak in asarualim races is teeming with stirring for about 20 minutes Then the microspheres are separated by filtration, washed with water and placed in a tightly closed container.

The diameter of the resulting slurry of microspheres of 2.0 mm, a water content of 96% by mass.

Microspheres when tested on the test And lose 28% by weight, test observed In the exudation and adhesion of particles.

Example 4. Obtaining a slurry of microspheres (without shells)

Get the original aqueous solution by adding 98% by weight of distilled water to 2.0 g of gum Arabic and held by dissolving under stirring for 4-5 hours at 20-25C.

Get osiewalsi a solution consisting of 150 ml of 4.0%aqueous solution of calcium dichloride.

The specified source solution is injected drops in osiewalsi solution.

Formed slurry of microspheres containing aqueous solution, melirovanie contained pectin molecules made of divalent calcium ions contained in asarualim solution, soak in asarualim the solution with stirring for about 20 minutes Then the microspheres are separated by filtration, washed with water and placed in a tightly closed container.

The diameter of the resulting slurry of microspheres of 0.25 mm, a water content of 94% by mass.

Microspheres when tested on the test And lose 28% by weight, test observed In the exudation and adhesion of particles.

Example 5. Receipt the microcapsules, containing aqueous solution having a primary shell on the surface of the water-containing microspheres

Get the original aqueous solution by adding 96,0 ml of distilled water, 3.0 g of sodium alginate and conduct its dissolution under stirring for 4-5 hours at 20-25C. Then the resulting solution dissolve 1.0 g of acatitla cellulose while stirring for 2-3 hours at 20-25C.

Get osiewalsi solution by dissolving in 150 ml of distilled water 2.25 g of chitosan under stirring for 2-3 hours at a temperature of 20-25C and then injected 3.75 g of calcium dichloride and dissolve it under stirring for 30-40 minutes.

The original solution is added in drops in osiewalsi solution, maintain the obtained microcapsules in the bath for 1.0 to 2.0 hours under stirring, separating the liquid phase on the filter, washed microcapsules with water, ensuring its full running off.

Then treated microcapsules by caking agent (Aerosil) and placed for storage in a tightly closed container.

Properties of microcapsules: the diameter of the microcapsules 1.5 mm, a water content of 91% by mass.

When testing microcapsules: the test And the water loss was not more than 4% by weight, when tested according to the test In the exudate is not allocated, the sticking of the particles does not occur. Flowability determined by the method equal to the slope, amounted to 32-34 degrees, which indicates good flowability of the product.

Weight loss during storage for six months in a tightly closed container does not occur.

These data demonstrate the stability of the obtained microcapsules subject to the conditions of storage in a closed container until the target application.

Example 6. Obtaining microcapsules containing water having a primary shell on the surface of the water-containing microspheres

Produce the same sequence of steps as in example 5 with the difference that instead of the sodium alginate used pectin.

Properties of the obtained microcapsules: the diameter of the microcapsules 4.0 mm, a water content of 96% by mass.

When testing microcapsules: the test And the water loss was not more than 4% by weight; when tested according to the test In the bleed and have exudate is not allocated, the sticking of the particles does not occur. Flowability determined by the method of the slope, amounted to 32-34 degrees, which indicates good flowability of the product.

Weight loss during storage for six months in a tightly closed container does not occur.

These data demonstrate the stability of the obtained microcapsules subject to the conditions of storage in a closed container until the target application.

Example 7. Obtaining microcapsules containing water having a primary shell on the surface of the water is containing microspheres

Produce the same sequence of steps as in example 5 with the difference that in osiewalsi solution instead of chitosan is administered 2.25 g of polyvinylpyrrolidone, and to obtain the original aqueous solution in 97,0 ml of distilled water is injected 3.0 g of sodium alginate and 1.0 g of polyacrylic acid.

Properties of the obtained microcapsules: the diameter of the microcapsules 0.25 mm, a water content of 90% by mass.

When testing microcapsules: the test And the water loss was not more than 4% by weight; when tested according to the test In the bleed and have exudate is not allocated, the sticking of the particles does not occur. Flowability determined by the method of the slope, amounted to 32-34 degrees, which indicates good flowability of the product.

Weight loss during storage for six months in a tightly closed container does not occur.

These data demonstrate the stability of the obtained microcapsules subject to the conditions of storage in a closed container until the target application.

Example 8. Obtain microcapsules having primary and secondary shell

To 30.0 g of microcapsules having a primary shell, containing acatitla cellulose and chitosan, obtained as in example 5, added to 50.0 ml of carbon tetrachloride (CCl4include a stirrer and type of 0.36 ml phospholane. The resulting mixture was stirred for 10-15 min, then gradually add 3.0 g of polii ocyanate, dissolved in 10 ml of CCl4. The stirring is continued for 3 hours at 20-25C. At the end of the process the liquid phase is separated on a filter, washed microcapsules 1 times CCl4, filtered and dried for about 30 min in a fume hood. After the microcapsules are placed in a tightly closed container.

When testing microcapsules: the test And the water loss was not more than 3.9% by weight, when tested according to the test In the exudate is not allocated, the sticking of the particles does not occur. Flowability determined by the method of the slope, amounted to 32-34 degrees, which indicates good flowability of the product.

Example 9. Obtain microcapsules having primary and secondary shell

The method is carried out as described in example 8, but in asarualim solution instead of 3 g of MDI using a mixture of MDI (2.1 g) with a diisocyanate (0.9 g), i.e. in the ratio of 70 mass% to 30 mass%.

When testing microcapsules: the test And the water loss was not more than 4% by weight, when tested according to the test In the exudate is not allocated, the sticking of the particles does not occur. Flowability determined by the method of the slope, amounted to 32-34 degrees, which indicates good flowability of the product.

Example 10. Obtain microcapsules having primary and secondary shell

Get the original aqueous solution by EXT is the case in 96,0 ml of distilled water, 3.0 g of sodium alginate and conduct its dissolution under stirring for 4-5 hours at a temperature of 20-25C, then the resulting solution dissolve 1.0 g of acatitla cellulose under stirring for two to three hours at a temperature of 20-25C. Next, enter the first acomponent additional shell, preferably 0.5 to 1.0 g of the diamine or polyethylenepolyamine, with stirring, for 25-30 minutes.

Get osiewalsi solution by dissolving in 150 ml of distilled water 2.25 g of chitosan under stirring for 2-3 hours at a temperature of 20-25C and then injected 3.75 g of calcium dichloride and dissolve it under stirring for 30-40 minutes.

The original solution is added in drops in osiewalsi solution, maintain the obtained microcapsules in the bath for 1.0 to 2.0 hours under stirring, separating the liquid phase on the filter, washed microcapsules with water, ensuring its full running off.

To 30.0 g of the microcapsules obtained in the described manner, added to 50.0 ml of carbon tetrachloride (CCl4include a mixer and gradually add 3.0 g of MDI dissolved in 10 ml of CCl4. The stirring is continued for 3 hours at 20-25C. At the end of the process the liquid phase is separated on a filter, washed microcapsules 1 times CCl4, filtered and dried for about 30 min in a fume hood.

When testing the obtained microcapsules: the test And the water loss was not more than 4 mass%, when Testino is assured by the test In the exudate is not allocated, sticking of the particles does not occur. Flowability determined by the method of the slope, amounted to 32-34 degrees, which indicates good flowability of the product.

Test results of the microcapsules obtained in examples 8-10, we can conclude that the obtained microcapsules having primary and secondary shell, showed no significant changes compared with the microcapsules obtained in examples 6-7, however, the nature of their surface has changed upwards of lyophilisate.

These properties were confirmed when determining the boundary of the limiting wetting angle of the obtained microcapsules. The results of measurements of the wetting angle of microcapsules shown in the table.

Microcapsules according to example No.The value of the wetting angle (in degrees)
liquid siloxaneepoxy
647.1668.90
(a microcapsule having a core in the form of microspheres, placed inside the main shell)
9At 42.27 55.25
(a microcapsule having a core in the form of microspheres, placed inside the main shell, and an additional outer shell)

Thus, the formation on the outer surface of the primary shell of the microcapsules according to the invention more lyophilic shell allows the use of microcapsules according to the invention as fillers that reduce the susceptibility of polymeric materials in fire, for example, as fillers, polymer compounds with low Flammability.

The above examples of implementation methods of microencapsulation according to the invention do not limit the possibilities of implementation of the present invention, is not beyond the scope of patent claims.

Methods of microencapsulation according to the invention is not limited to the described compositions options shells and allow you to adjust the properties of microcapsules containing water, such as lifelost membranes, for use in obtaining various compounds depending on the nature of the polymeric matrix.

Microcapsules according to the invention, containing water or aqueous solutions obtained by the methods according to the invention, under conditions of storage in a closed container is resistant to temperature influences, for a long time to achieve water conservation inside the microcapsules, their flowability and willingness to target to use as a fire extinguishing or cooling means.

Designed according to the invention methods of microencapsulation by lyophilization of the surface of the microcapsules by forming additional shells open the possibility of their use as fillers, polymer compounds with low Flammability.

Aqueous solutions and suspensions in microencapsulated form can be used in the creation of new bioactive drugs, drugs, living microbiological cultures, for example, programmable protect them from the external environment or to prolong their actions, in the food industry and other industries.

Specialists in the field of physical chemistry of polymers and microencapsulation should be clear that in the microcapsules according to the invention and methods for their preparation can be made various improvements, not beyond the scope of patent claims. For example, the composition of the primary and secondary membranes can be selected from acomponent acceptable for a contact, for example, with acid or alkali or other corrosive environments, or can be modified for the purpose programmable release of water or water-Rast is ora, contained in the microcapsules, in the given conditions at a given speed.

Microcapsules according to the invention, containing water or aqueous solutions, and the method of microencapsulation of water or aqueous solutions according to the invention can be implemented using known techniques and known substances. Microcapsules containing water or aqueous solutions, in addition to the application to resolve the main problems of fire fighting and emergency overheating chemical and nuclear reactors, electronic equipment, can find application in the technology of polymeric compounds filled with microencapsulated water to reduce their Flammability, and also used in food and pharmaceutical industries and in other industries.

1. The microcapsule containing water or an aqueous solution, melirovanie using crosslinked by calcium ions dissolved in said water or aqueous solution of a gelling polyelectrolytes having a carboxyl group, characterized in that the said water or aqueous solution contains one separate slurry of microspheres having a given diameter, the outer surfaces of which are in the interphase layer is formed of a solid spherical equal thickness was the main shell, which has hydrophilic properties and having a thickness and density of the shell, the minimum required to prevent evaporation of the water contained in the microsphere, with the main shell formed by a macromolecular complex compounds obtained by the counter diffusion in the interfacial layer of macromolecular first acomponent who carry a negative charge, and macromolecular second acomponent who carry a positive charge.

2. The microcapsule containing water or an aqueous solution, melirovanie using crosslinked by calcium ions dissolved in said water or aqueous solution of a gelling polyelectrolytes having a carboxyl group, characterized in that the said water or aqueous solution contains one separate slurry of microspheres having a given diameter, the outer surfaces of which are in the interphase layer is formed of a solid spherical equal thickness was the main shell, which has hydrophilic properties and having a thickness and density of the shell, the minimum required to prevent evaporation of the water contained in the microsphere, with the main shell formed by a macromolecular complex compounds obtained by the counter diffusion in the interfacial a layer of macromolecular first acomponent who carry a negative charge, and a second high molecular juice is mponents, being a carrier of positive charge, and the outer surface of the specified primary shell formed additional outer spherical shell of equal thickness was having lyophilic properties.

3. The microcapsule according to claim 1 or 2, characterized in that it contains the water or aqueous solution in an amount of not less than 90% by weight of microspheres having a given diameter, is selected in the range from 0.25 to 5.0 mm

4. The microcapsule according to claim 1 or 2, characterized in that it contains water or an aqueous solution, melirovanie using sodium alginate and/or pectin, and/or gum Arabic, and/or any other polysaccharides containing carboxyl groups, and crosslinked by calcium ions.

5. The microcapsule according to claim 1 or 2, wherein the primary shell formed by a macromolecular complex compounds obtained by the counter diffusion and interaction of acatitla cellulose with chitosan.

6. The microcapsule according to claim 1 or 2, wherein the primary shell formed by a macromolecular complex compounds obtained by the counter diffusion and interaction of polyacrylic acid and polyvinylpyrrolidone.

7. The microcapsule according to claim 2, characterized in that the additional outer shell formed by polycarbamide.

8. The microcapsule according to claim 2, characterized in that additionally the I outer shell formed by polimochevinnykh.

9. Method of microencapsulation of water or aqueous solutions to produce separate slurry of microspheres containing water or an aqueous solution, melirovanie using polyelectrolytes and cross-linked by calcium ions, comprising the following steps:
a) obtaining a source of an aqueous solution containing dissolved in water, at least a gelling polyelectrolytes: sodium alginate, and/or pectin, and/or gum Arabic, and/or any other polysaccharides containing carboxyl group;
b) obtaining oshivelo aqueous solution containing dissolved therein a source of divalent calcium ions, which is used as aqueous solutions of calcium dichloride, and/or calcium lactate and/or calcium glycerol, and/or any other water soluble calcium salts;
c) the introduction of the original aqueous solution obtained in stage a), in osiewalsi aqueous solution obtained in stage b), the drops having a given volume, providing microspheres having a given diameter, is selected in the range from 0.25 to 5.0 mm, with stirring oshivelo solution at 20-25C for a time sufficient to education in asarualim the dispersion solution containing the separated microspheres with monodispersity of not less than 90%, in which the initial aqueous solution is in the form of a gel, sformirovannogo the gelling polyelectrolytes, obtained in stage a), made of divalent calcium ions, obtained in stage b);
d) isolation of the microspheres obtained in step (C), of the variance oshivelo solution by filtration;
e) placing the resulting microspheres in the packaging, drained dry.

10. Method of microencapsulation of water or aqueous solutions to produce microcapsules containing water or an aqueous solution in a separate slurry of microspheres having a given diameter, the outer surfaces of which are in the interphase layer is formed of a solid spherical equal thickness was the main shell, which has hydrophilic properties and having a thickness and density of the shell, the minimum required to prevent evaporation of the water contained in the microsphere, comprising the following steps:
a) obtaining a source of an aqueous solution containing dissolved in water, at least a gelling polyelectrolytes: sodium alginate, and/or pectin, and/or gum Arabic, and/or any other polysaccharides containing carboxyl groups, and macromolecular first acomponent core shell microcapsules carrying a negative charge;
b) obtaining oshivelo solution containing dissolved in water, at least one source of divalent calcium ions and macromolecular second acomponent, Allaudin the carriers of positive charge;
c) the introduction of the original aqueous solution obtained in stage a), in osiewalsi the solution obtained in stage b), the drops having a given volume, providing microspheres having a given diameter, is selected in the range from 0.25 to 5.0 mm, with stirring oshivelo solution at 20-25C for a time sufficient to education in asarualim the dispersion solution containing the separated microspheres of a given diameter with monodispersity not less than not less than 90%, in which the initial aqueous solution is in the form of a gel formed gel polyelectrolytes obtained in stage a)made of divalent calcium ions, obtained in stage b);
d) aging the dispersion obtained in stage C)at a temperature of 20-25C for a time sufficient for the formation of microcapsules having a single microsphere obtained in stage C), provided on the surface of the main shell formed by macromolecules of complex compounds obtained by the counter diffusion in the interfacial layer of macromolecular first acomponent primary shell, obtained in stage a), and second acomponent primary shell, obtained in stage b);
e) isolation of the microcapsules obtained in stage d), oshivelo solution by filtration;
f) flushing water microcapsules obtained in atape), and drying them in the air;
g) processing of microcapsules obtained in stage f), - caking agent;
h) placing the resulting microcapsules in a tightly closed container, drained from moisture,
and at the same time as the source of divalent calcium ions using aqueous solutions of calcium dichloride, and/or calcium lactate and/or calcium glycerol, and/or any other water soluble calcium salts.

11. The method according to claim 10, characterized in that as the first acomponent primary shell use acatitla cellulose, and as the second acomponent primary shell using chitosan.

12. The method according to claim 10, characterized in that as the first acomponent primary shell using polyacrylic acid, and as a second cocomponent the basis of the shell using polyvinylpyrrolidone.

13. The method according to claim 10, characterized in that get microcapsules with monodispersity of not less than 90% in the range of diameters from 0.25 to 5.0 mm and containing water or an aqueous solution in an amount of not less than 90% by weight of microcapsules.

14. Method of microencapsulation of water or aqueous solutions to produce microcapsules containing melirovanie water or aqueous solution in a separate slurry of microspheres having a given diameter, the outer surfaces of which are in the interfacial layer formed t is Erda spherical equal thickness was the main shell, possessing hydrophilic properties and having a thickness and density of the shell, the minimum required to prevent evaporation of the water contained in the microsphere, and contains formed on the main shell of the additional outer shell having lyophilic properties and formed by polycarbamide that includes the following steps:
a) obtaining a source of an aqueous solution containing dissolved in water, at least a gelling polyelectrolytes: sodium alginate, and/or pectin, and/or gum Arabic, and/or any other polysaccharides containing carboxyl groups, and macromolecular first acomponent core shell microcapsules carrying a negative charge;
b) obtaining oshivelo solution containing dissolved in water, at least one source of divalent calcium ions and macromolecular second acomponent who carry a positive charge;
c) the introduction of the original aqueous solution obtained in stage a), in osiewalsi the solution obtained in stage b), the drops having a given volume, providing microspheres having a given diameter, is selected in the range from 0.25 to 5.0 mm, with stirring oshivelo solution at 20-25C for a time sufficient to education in asarualim restoredatabase, containing isolated microspheres of a given diameter with monodispersity not less than not less than 90%, in which the initial aqueous solution is in the form of a gel formed gel polyelectrolytes obtained in stage a), made of divalent calcium ions, obtained in stage b);
d) aging the dispersion obtained in stage C)at a temperature of 20-25C for a time sufficient for the formation of microcapsules having a core in the form of microspheres obtained in step (C), provided on the surface of the main shell formed by macromolecules of complex compounds obtained by the counter diffusion in the interfacial layer of macromolecular first acomponent primary shell, obtained in stage a), and second acomponent primary shell, obtained in stage b);
e) the selection of the dispersion treated in step d), the filtering of the microcapsules obtained in stage d) and containing on the outer surface of the primary shell trace amounts of water as the first acomponent for the formation of additional outer sheath;
f) obtaining a liquid organic medium, which is injected second cocomponent to generate additional outer shell having lyophilic properties, and a liquid catalyst, soluble in water, but insoluble in organic fluid is level positions;
g) introduction of microcapsules obtained in stage e), in an organic environment, obtained in stage f), with stirring to obtain a dispersion of these particles in the specified organic environment;
h) exposure of the dispersion obtained in step (g)at 20-25C for a time sufficient for formation on the outer surface of the microcapsules contained in the dispersion obtained in step g), an additional outer lyophilic shell when the interaction of these first acomponent additional membrane in the form of trace quantities of water obtained in stage e), with the second acomponentname additional membrane obtained in step f), in the presence of the specified catalyst;
i) isolation of the microcapsules obtained in step h), from the organic medium by filtration;
(k) washing the microcapsules obtained in stage i), such as volatile organic liquid used in step (f);
l) placing the microcapsules obtained in step k), in a tightly closed container, drained from moisture,
and this:
as a source of divalent calcium ions using aqueous solutions of calcium dichloride, and/or calcium lactate and/or calcium glycerol, and/or any other water soluble calcium salts,
as the liquid organic medium in step (f) using carbon tetrachloride or dimeticone is at,
as the catalyst used phosfolan, preferably 1-oxo-1,3-dimethylphosphine,
as the second acomponent additional outer shell using a polyisocyanate or a mixture of MDI with toluylenediisocyanate.

15. The method according to 14, characterized in that as the first acomponent primary shell use acatitla cellulose, and as the second acomponent primary shell using chitosan.

16. The method according to 14, characterized in that as the first acomponent primary shell using polyacrylic acid, and as a second cocomponent the basis of the shell using polyvinylpyrrolidone.

17. The method according to 14, characterized in that get microcapsules with monodispersity of not less than 90% in the range of diameters from 0.25 to 5.0 mm, containing water or an aqueous solution in an amount of not less than 90% by weight of microcapsules.

18. Method of microencapsulation of water or aqueous solutions to produce microcapsules containing melirovanie water or aqueous solution in a separate slurry of microspheres having a given diameter, the outer surfaces of which are in the interphase layer is formed of a solid spherical equal thickness was the main shell, which has hydrophilic properties and having a thickness and density of the shell, the minimum required toprevent water evaporation, contained in the microsphere, and contains formed on the main shell of the additional outer shell having lyophilic properties and formed by polimochevinnykh that includes the following steps:
a) obtaining a source of an aqueous solution containing dissolved in water, at least a gelling polyelectrolytes having a carboxyl group, macromolecular first acomponent primary shell having a negative charge, and the first cocomponent to provide an additional outer casing;
b) obtaining oshivelo solution containing dissolved in water, at least one source of divalent calcium ions and macromolecular second acomponent primary shell having positive charges;
c) the introduction of the original aqueous solution obtained in stage a), in osiewalsi the solution obtained in stage b), the drops having a given volume, providing microspheres having a given diameter, is selected in the range from 0.25 to 5.0 mm, with stirring oshivelo solution at 20-25C for a time sufficient to education in asarualim the dispersion solution containing the separated microspheres of a given diameter with monodispersity not less than not less than 90%, in which the initial aqueous solution is in the form of a gel, placer was generated is about gelling polyelectrolytes, obtained in stage a), made of divalent calcium ions, obtained in stage b);
d) aging the dispersion obtained in stage C)at a temperature of 20-25C for a time sufficient for the formation of microcapsules having a single microsphere obtained in stage C), provided on the surface of the main shell formed by macromolecules of complex compounds obtained by the counter diffusion in the interfacial layer of macromolecular first acomponent primary shell, obtained in stage a), and second acomponent primary shell, obtained in stage b);
e) the selection of the dispersion treated in step d) by filtration of the microcapsules obtained in stage d) and containing on the outer surface of the primary shell trace amounts of water;
f) obtaining a liquid organic medium, which is injected second acomponent for the formation of the additional outer shell having lyophilic properties;
g) introduction of microcapsules obtained in stage e), in an organic environment, obtained in stage f), with stirring to obtain a dispersion of these particles in the specified organic environment;
h) exposure of the dispersion obtained in step (g)at 20-25C for a time sufficient for formation on the outer surface of the microcapsules contained in the dispersion obtained is in step g), additional external lyophilic shell when the interaction of these first acomponent additional membrane obtained in stage a), with the second acomponentname additional membrane obtained in step (f);
i) isolation of the microcapsules obtained in step h), from the organic medium by filtration;
(k) washing the microcapsules obtained in stage i), the same liquid organic medium, as applied in step f);
l) placing the microcapsules obtained in step k), in a tightly closed container, drained from moisture,
and this:
as a source of divalent calcium ions using aqueous solutions of calcium dichloride, and/or calcium lactate and/or calcium glycerol, and/or any other water soluble calcium salts,
as the liquid organic medium in step (f) using carbon tetrachloride or dimethylcarbonate,
as the first acomponent additional outer shell using hexamethylenediamine were, or polyethylenepolyamine, and/or other di - and polyamine, soluble in water,
and as a second acomponent additional outer shell using a polyisocyanate or a mixture of MDI with toluylenediisocyanate.

19. The method according to p, characterized in that as the first acomponent primary shell use acatitla pulp and kachestvenyj of acomponent primary shell using chitosan.

20. The method according to p, characterized in that as the first acomponent primary shell using polyacrylic acid, and as a second acomponent primary shell using polyvinylpyrrolidone.

21. The method according to p, characterized in that get microcapsules with monodispersity of not less than 90% in the range of diameters from 0.25 to 5.0 mm, containing water or an aqueous solution in an amount of not less than 90% by weight of microcapsules.



 

Same patents:

FIELD: chemistry.

SUBSTANCE: invention relates to use of polymer material, and specificaly to use of particulate polymer material as an active agent carrier. The polymer material is a polymer obtained from copolymerisation of pyrrole with quadratic or croconic acid or its derivative.

EFFECT: use in accordance with the invention enables to use polymer material as a composition in form of particles as an absorbent or prolonged release agent.

16 cl, 8 dwg, 1 tbl, 10 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a solid re-dispersible emulsion which is a direct emulsion of fabric softener encapsulated in a polysaccharide shell which is stabilised by ions of polyvalent metals selected from Ca2+, Sr2+, Ba2+, Al3+, Cu2+, Zn2+, where the shell is initially insoluble in water but becomes soluble in water through ion donation. The polysaccharide is biodegradable and is selected from a group comprising alginates and carrageenans. Similar solid re-dispersible emulsions are primarily used in agents for washing or taking care of clothes. Powdered fabric softeners are easy to store, apportion and, if necessary, combine with powdered detergents during production.

EFFECT: invention enables production of fabric softeners previously produced as liquid compositions in solid powdered form.

14 cl, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to capsular additives for rubber, obtained in form of microcapsules with a polymer wall and a nucleus, which contains at least one additive for rubber. The capsule wall is formed by at least one component from a reactive resin and at least one component from a polyelectrolyte or ionomer component. The reactive resin is melamine formaldehyde resin and/or polyurea resin. The invention also relates to a method of preparing such microcapsules. The proposed microcapsules are used for vulcanising natural and synthetic rubber. The microcapsules are thermally and mechanically stable in conditions for preparing and processing rubber compositions in kneading machines, manglers or twin-screw extruders at temperatures ranging from 120C to 140C.

EFFECT: microcapsular additives are uniformly distributed in rubber mixture and prevent formation of a heterogeneous rubber/additive system.

30 cl, 12 ex

Microcapsules // 2359662

FIELD: medicine, pharmaceutics.

SUBSTANCE: microcapsules, in which water droplet or droplets including the dissolved active ingredient are incapsulated in the hardened hydrophobic cover-matrix, are described. Also the methods of obtaining of the specified microcapsules and their application are described.

EFFECT: development of microcapsules which possess the improved stability and provide the adjustable and-or prolonged release of an active ingredient.

40 cl, 8 dwg, 4 tbl, 8 ex

FIELD: medicine; pharmacology.

SUBSTANCE: carrying out of treatment of disease, in particular, diabetes, by implantation of the encapsulated devices containing a covering and cells, thus density of cells makes 100000 cells/ml, and the covering contains acrylate polyethylene alcohol (PEG) high density with molecular mass from 900 to 3000 Dalton, and also a sulfonated comonomer.

EFFECT: minimisation of the tissue response, augmentation of concentration of cells and augmentation of time of viability of cells in the specified devices.

83 cl, 33 dwg, 8 tbl, 20 ex

FIELD: chemistry.

SUBSTANCE: composition is used for making hollow micro-spheres, which are used as a component of boring solutions when finding and producing oil, as low density filler in various composite materials, used in machine building, aviation and ship building, space technology, and when making heat insulation materials. The composition contains the following, in the given mass ratios: resol phenol-formaldehyde resin with relative viscosity of 5000-9000 cP - 100, porofor (5), polyether based on ethylene oxide copolymer and propylene oxide with molecular mass of 4000-6000 (2-3).

EFFECT: higher space factor of the boring solution micro-spheres, improved looseness of the micro-spheres, increased strength during hydrostatic compression.

1 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: group of invention covers the microcapsules consisting of at least one core which contains the rubber supplement, and the first polymeric coat of melamine-formaldehyde or phenol-formaldehyde resin; the second polymeric coat is applied upon the microcapsule and its content differs from that of the first one and consists of the low-molecular inorganic or organic compound as a sliding and wear layer to reduce the static friction.

EFFECT: method of preparation microcapsules and use in rubber vulcanisation.

20 cl, 14 ex, 2 tbl

FIELD: derivatives of chitosan.

SUBSTANCE: invention relates to preparing biologically active chitosan substances and their derivatives. Invention describes a modified chitosan substance showing pH-neutral reaction and plastic structure of chitosan particles as fractal chitosan particles of size of nanofractals from 1 nm, not less, and to 5000 nm, not above, or as cross-linked net-shaped polymer having multiple cavities of size from 1 nm, not less, to 50 nm, not above. Invention describes methods for their preparing. Invention provides high transdermal penetration of chitosan substance and enhanced capacity for administration of medicinal or biologically active substances into chitosan substance. Invention can be used in manufacturing cosmetic, curative-cosmetic, pharmacological preparations, biologically active food supplements and foodstuffs.

EFFECT: improved and valuable properties of chitosan substances.

14 cl, 4 tbl, 7 dwg, 9 ex

FIELD: food and pharmaceutical industries.

SUBSTANCE: object of invention is production of freely flowing alcohol-containing encapsulated products. Food fat and/or wax are melted in heated reactor at 55-65°C, after which required food additives or additive complexes are added, resulting mixture is stirred to achieve homogenous mass and alcoholic produce with alcohol content from 5 to 96.6% is added in amount 5 to 60 wt parts per 100 wt parts of the reactor charge. Emulsion obtained is supplied to atomization turbine wherein arising drops are solidified in air and collected in receiving device. Thus obtained powder is screened and tightly packaged. Granule size is controlled by turbine rotation speed and varied within a range of 0.1 to 1 mm.

EFFECT: enabled creation of fundamentally novel formulations and production technologies, improved quality, reduced expenses, and prolonged shelf time of produce.

3 cl, 6 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

Transportation line // 2415068

FIELD: transport.

SUBSTANCE: transportation line is intended for transportation of capsules between capsule filling station and capsule sealing station. Transportation line includes loading area (10), unloading area (20) and multiple transportation modules (30) on conveyor (40). Cavities (31) of each transportation module have the possibility of placing the groups of filled capsules consisting of two parts, when they are located in loading position in loading area, and output of groups, when they are located in unloading position in unloading area. Conveyor has the possibility of supporting transportation modules for their transportation from loading position to unloading position, and vice versa, at their being retained in one and the same position.

EFFECT: providing integrity and non-blockage of capsules to each other during their transportation.

14 cl, 4 dwg

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention relates to chemical-pharmaceutical industry and medicine. Method includes: formation of hollow capsules, their hardening and following packing, which differs in the act that as material for manufacturing of capsules applied are substances, able to dissolve in gastric juice with speed, depending on its acidity degree, and manufacturing of capsules is carried out in chamber with increased gas atmosphere pressure. Packing of capsules can also be carried out in chamber with increased pressure, it is necessary to do packing of capsule able to preserve said pressure and provide air-tightness during fixed term of capsule storage.

EFFECT: increased efficiency of method of manufacturing capsules for determination of gastric juice acidity.

3 cl, 1 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention relates to field of medicine and pharmaceutics, namely to medication for treatment or prevention of cardiovascular system and/or nervous system diseases. Medication contains ethylmethylhydroxypyridine succinate, pyridoxine hydrochloride, pharmaceutically acceptable salt of magnesium and auxiliary substances in quantities given in invention formula. Method of cardiovascular and/or nervous system diseases treatment includes peroral introduction of medication by invention in efficient quantity. Also described is method of obtaining claimed medication.

EFFECT: obtaining highly technological medication characterised by low cost and high therapeutic effect.

13 cl, 6 tbl, 3 ex

FIELD: medicine.

SUBSTANCE: invention relates to method and device for sealing of capsules with solid shell made of two parts inserted one into the other. Method includes the following: placement of capsule into fixed position of sealing in unit of capsules holder, application of sealing fluid medium evenly onto capsule space in specified position of sealing, turning capsule into fixed position of suction displaced by a certain angle relative to position of sealing and creation of lower pressure area around capsule in specified suction position to remove excessive sealing fluid from capsule.

EFFECT: invention provides for hardening of seam with minimum of mechanical actions.

37 cl, 5 dwg

FIELD: medicine.

SUBSTANCE: invention relates to spontaneously dispersed pharmaceutical compositions including substance P antagonist, 5-aryl-4(K)-arylcarbonylaminopent-2-enic acid, and carrier medium, including from 5 to approximately 85 wt % of lipophilic component, namely monoglycerides and diglycerides of C8-C10 fatty acids or purified with re-etherificated glycerol corn oil, and from 5 to approximately 90 wt % of surface active substance, namely l ether of polyethelene glycol and hydrogenised castor oil. Compositions by invention are stable and possess improved bioavailability.

EFFECT: invention also relates to methods of obtaining said compositions and methods of treating diseases which are cured with substance P antagonist, for instance respiratory diseases, intestinal disorders, enuresis and cough.

13 cl, 1 dwg, 3 ex

Container // 2386433

FIELD: medicine.

SUBSTANCE: invention refers to medicine, namely to pharmaceutical industry and concerns a container, and more specifically a capsule used for delivering dosages of pharmaceutical preparations, drugs, vitamins etc. In one version of implementation, the invention involves a container (200) which contains a cap (210) and a body (240) for sliding fit inside the cap (210), and wherein between the cap (210) and the body (240) there is a fluid gap (260) adjacent to an end of the cap (210). The first flute (220) of the cap (210) and the first flute (250) of the body (240) form a lock joint, while the second flute (222) of the cap (210) and the second flute (252) of the body (240) form a fluid block joint which essentially blocks sealant flow by the fluid gap (260).

EFFECT: development of the capsule preventing drug flow.

25 cl, 22 dwg

FIELD: medicine.

SUBSTANCE: present invention concerns medical products, particularly a pharmaceutical product for introduction of allergen that contains high-soluble solid dosage form introduced through tunica mucosa of mouth and containing matrix made by freeze drying from the solution containing 3-6.5 wt % pre-gelled starch and 3-5.5 wt % mannitol, or from the solution containing 2-10 wt % fish gelatine and 1-10 wt % mannitol; and allergen. Besides, invention concerns the method for making the specified product, a multidosage container, a set for allergy treatment, to the method of treating and applying the specified product.

EFFECT: preparation of allergen as a high-soluble uncompacted dosage form which is high-soluble, stable and low-fragile enough.

99 cl, 25 tbl, 1 ex

FIELD: medicine.

SUBSTANCE: invention concerns medications, particularly self-emulsifying system of butylphthalide drug delivery, including 1% to 65% of butylphthalide, 10% to 65% of emulsifying agent, and filler. Emulsifying agent is a mix of polyoxyetylene castor oil and polyethyleneglycol-8-glycerin caprilate/caprate, where polyoxyethylene castor oil to polyethyleneglycol-8-glycerin caprilate/caprate ratio is 1:0.5 to 1:1.5. Invention also concerns medication containing claimed delivery system, and method of system obtainment.

EFFECT: faster achievement of maximum butylphthalide concentration, increased maximum concentration, improved butylphthalide stability.

9 cl, 1 dwg, 3 tbl, 18 ex

FIELD: medicine.

SUBSTANCE: composition contains a pharmacological agent, water-soluble polymer and a fatty base. The pharmacological agent is chosen from a group, containing diclofenac, acetylsalicylic acid, paracetamol, ibuprofen, ketorolac, pentoxifeylline and ciprofloxacin. The water-soluble polymer is chosen from a group, containing hydroxypropylmethicellulose, polyvinylpyrrolidone, egg white, sodium caseinate, milk protein, guar gum, sodium alginate, pectin, chitosan acetate, polygalactomannan, dextran or their mixture. The fatty base relates to oils consumed by human beings, which melt at temperature between 30 and 36C and chosen from a group containing: cocoa bean oil, coconut oil, milk fat, pork fat, hydrofat or their mixture. The said pharmacological agent and water-soluble polymer are contained in the composition in form of a non-covalent complex.

EFFECT: obtaining a dosage form with intense prolonged effect.

3 cl, 3 dwg, 1 tbl, 1 ex

FIELD: medicine.

SUBSTANCE: invention concerns a dispersion of crystals or granules of active substance in lipophilic filler where crystals or granules are covered for taste masking. The invention also concerns chewing or quickly dissolved soft gelatinous capsules filled with the specified dispersion, and also a way of manufacture of such forms. Use of considerable quantities of active substance which should be accepted at unitary introduction, and maintenance of satisfactory release of active substance in vivo is possible.

EFFECT: new dosed out forms are stable throughout all period of storage.

15 cl, 17 tbl, 5 ex

FIELD: agriculture.

SUBSTANCE: water dispersion for protection of plants includes nanoparticle composition of reactant for plant protection, where nanoparticles have structure of nucleus-shell with average diametre of particles from 0.05 to 2.0 mcm; reactant for plant protection is radiologically amorphous, is in nucleus with one or more polymers, which are insoluble or partially soluble in water or water solutions, or mixtures of water with dissolvent, i.e. the second virial coefficient may not be below zero; - shell consists of stabilising wrapping matrix, containing interphase or surfactant polymer colloids, or low-molecular amphiphilic compounds or their mixtures. Nanoparticles are produced by making a reactant solution to protect plants in organic dissolvent, which is not mixed with water, by dissolving of nucleus polymer in organic dissolvent, which is not mixed with water and emulsification of mixture from (a) and (b) with water solution, containing components of wrapping matrix, by means of injection of according solutions in mixing chamber. After emulsification organic dissolvent is removed. Solid nanoparticle composition is produced by drying of water dispersion. Agrochemical composition contains solid carrier treated with specified water dispersion or solid nanoparticle composition. Seed material is etched with specified water dispersion or treated with solid composition. Undesirable fungi, plants or insects are treated with specified dispersion or composition.

EFFECT: invention allows increasing composition stability.

13 cl, 4 ex

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