Aqueous dispersions of polymer-encapsulated particles, associated coating compositions and coated bases

FIELD: chemistry.

SUBSTANCE: invention relates to a powder coating composition obtained from aqueous dispersion containing polymer-encapsulated particles, said particles including particles encapsulated in a brittle polymer which can easily break up under ambient conditions. The invention also discloses a method of preparing an aqueous dispersion of particles encapsulated in a brittle polymer, a base which is at least partially coated with a coating deposited from said composition, a multilayer composite coating, a method of preparing a powder coating composition, a method of preparing an aqueous dispersion of particles encapsulated in a brittle polymer and a powder coating composition formed from said dispersion prepared using said method, as well as a reflecting surface which is at least partially coated with a layer which gives the colour of an uncovered coating deposited from disclosed powder coating compositions.

EFFECT: obtaining aqueous dispersion of particles encapsulated in a brittle polymer in which repeated agglomeration of particles is minimised and which enables to obtain a powder coating composition which contains multiple polymer-encapsulated particles having maximum turbidity so that the coating has absorption or reflection in the visible spectrum which is close to that of the given coating.

22 cl, 14 ex, 1 tbl

 

Cross-reference to related applications

This application is a partial continuation of patent application U.S. 10/876,031, entitled “Aqueous Dispersions of Microparticles Having a Nanoparticulate Phase and Coating Compositions Containing The Same”, which claims the benefit of provisional application U.S. 60/482,167, filed on June 24, 2003, which are both incorporated herein by reference. This application is also a partial continuation of patent application U.S. 10/809,764, which was filed on March 25, 2004 and entitled “Process For Manufacturing Powder Coating Compositions Introducing Hard to Incorporate Additives and/or Providing Dynamic Color Control”; patent application U.S. 10/809,595, which was filed on March 25, 2004 and entitled “Focused Heat Extrusion Process For Manufacturing Powder Coating Compositions”; patent application U.S. 10/809,639, which was filed on March 25, 2004 and entitled “Apparatus For Manufacturing Thermosetting Powder Coating Compositions With Dynamic Control Including Low Pressure Injection Systems, each of which is incorporated herein by reference.

The technical field to which the invention relates.

The present invention particularly relates to aqueous dispersions decapsulating in the polymer particles, such as nanoparticles, methods of generating such aqueous dispersions of polymerized polymers applicable in this method, the compositions for powder coatings formed from such aqueous dispersions, and the basics at least partially covered so the th composition.

The level of technology

Compositions for coatings, such as compositions for powder coatings often include particles of colorant and/or filler to impart color and/or functional properties of the resulting coating. The pigment particles tend to have a strong affinity to each other and, if they are not in a divided state, tend to stick together to form agglomerates. Therefore, these agglomerates are often dispersed in the crushed resinous binder substance and, optionally, a dispersing means by rolling or rubbing using the technique of high shearing forces to break up the agglomerates. If desired nanoscale pigment particles, further grinding to obtain particles of the desired size.

Typically, the pigments and fillers are composed of hard crystalline particles with a diameter ranging from about 0.02 to 2 microns (i.e., from 20 to 2000 nm). Agglomeration is a serious problem especially for nanoscale particles of pigments and filler materials (such as soot), because these nanoparticles have a relatively large surface area. Thus, an acceptable dispersion of such nanoparticles often requires an excessive amount of resinous binder and/or dispersing the funds to ensure that de is glomeruli and prevent subsequent re-agglomeration of the nanoparticles.

However, the presence of such high concentrations of resinous binders and dispersing funds in the final composition of the coating can be harmful for final coating. For example, it is known that high concentrations of dispersing funds contribute to the sensitivity of the final coating to water. In addition, some resinous binder, for example, acrylic binders, can adversely affect the performance properties of coatings, such as resistance to splitting and flexibility.

Often desirable composition for powder coating to cover the different types of foundations. Such compositions for coatings can significantly reduce or even eliminate the use of organic solvents that are commonly used in compositions for liquid coatings. If the composition for powder coating is cured by heating, little, if any at all, volatile material is emitted into the environment. This is a significant advantage over compositions for liquid coatings, in which the organic solvent is emitted into the surrounding atmosphere, if the composition for coating is cured by heating.

It would also be desirable to provide an aqueous dispersion decapsulating in the resin particles, which minimized re agglomera the Oia particles, and that may be suitable for use in obtaining compositions for powder coating.

Brief description of the invention

In certain aspects the present invention relates to aqueous dispersions comprising zakopalova in the polymer particles, in which zakopalova in the polymer particles include particles, zakopalova in a brittle polymer. The present invention also relates to compositions for powder coatings comprising such zakopalova in the polymer particles, the basics at least partially coated with such compositions for powder coating, and the basics at least partially covered with a complex multi-layered coating in which at least one coating layer is applied from a composition for powder coating.

In other aspects the present invention relates to methods of producing aqueous dispersions decapsulating in the polymer particles. The methods include (1) receiving in an aqueous medium a mixture of (a) particles, (b) polymerizing the ethylene-unsaturated monomer and (C) dispersible in water polymerizable dispersant funds and (2) the polymerization of the ethylene-unsaturated monomer and polymerizable dispersant funds from education decapsulating in the polymer particles, comprising a dispersible polymer in water.

In other aspects of the present the invention relates to methods for decapsulating in the polymer particles. The methods include (1) receiving in an aqueous medium a mixture of (a) particles, (b) polymerizing the ethylene-unsaturated monomer and (C) dispersible in water polymerizable dispersant funds; (2) the polymerization of the ethylene-unsaturated monomer and polymerizable dispersant education aqueous dispersion comprising zakopalova in the polymer particles containing the dispersible in water brittle polymer; (3) removing water from the aqueous dispersion for the formation of solid material including zakopalova in the polymer particles, and (4) grinding the solid material.

In other aspects the present invention relates to methods of producing compositions for powder coatings comprising (1) introducing into an extruder (a) aqueous dispersion decapsulating in the polymer particles and (b) dry materials; (2) mixing (a) and (b) in the extruder; (3) removing volatiles from the mixture to form an extrudate; (3) cooling the extrudate, and (4) grinding the extrudate to particles of the desired size.

In still other aspects the present invention relates to methods to increase the color composition for powder coating. These methods include the inclusion in the composition for powder coating many decapsulating in polymer nanoparticles having a maximum turbidity of 10%.

In still other aspects of us who Aasee the invention relates to a method of matching a color of the specified protective and decorative coatings, deposited from the composition for liquid coatings. These methods include: (a) the definition of the visible colors specified coating by measuring the absorption or reflection of the specified coating and (b) the composition for powder coating, including a certain number decapsulating in polymer nanoparticles having a maximum turbidity of 10%, where the coating of the composition for powder coating, corresponds to visible color of the specified coating.

The present invention also relates to dispersible in water, the polymerizable polyester polyurethane containing a terminal ethylene-unsaturated groups. Polyurethanes derived from reactants comprising (a) a polyisocyanate, (b) a polyester polyol, (b) polyamine, (g) material containing ethylene unsaturated group and an active hydrogen group, and (d) a material containing an acid functional group or anhydride and an active hydrogen group.

Detailed description of the invention

For the purposes of the following detailed description should be understood that the invention can encompass various alternatives and sequential stages, unless explicitly stated otherwise. In addition, with the exception of any examples of implementation, or if stated otherwise, all numbers expressing, for example, the number of ingredients used in the description and f is rule of the invention, should be understood as being modified in all instances by the term “about”. Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following description and the attached claims are approximations that can be modified depending on the desired properties to be obtained in accordance with the present invention. At least, not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should be at least considered in light of the number of published significant digits and ordinary rounding techniques.

Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the invention are approximations, the numerical values set forth in the specific examples are listed as accurately as possible. However, any numerical value essentially contains certain errors necessarily resulting from the standard deviation found in their respective test measurements.

In addition, it should be understood that any numerical range shown herein is intended to include all of the included potentialof. For example, the interval from 1 to 10” is intended to include all potentialof between (and including) the defined minimum value of 1 and the specified maximum value 10, ie has a minimum value equal to or greater than 1 and the maximum value is equal to or less than 10.

In this application the use of the singular includes the plural, and the plural covers the singular, unless specifically stated otherwise. In addition, in this application the use of “or” means “and/or”, unless specifically stated otherwise, even though “and/or” can obviously be used in some examples.

As mentioned earlier, certain implementations of the present invention relates to aqueous dispersions decapsulating in the polymer particles. The term “dispersion”as used herein refers to a two-phase system where one phase consists of finely ground particles distributed throughout a second phase, which is a homogeneous phase. The dispersion of the present invention represents an emulsion of the type oil-in-water, in which the aqueous medium is homogeneous phase dispersion, in which zakopalova in the polymer particles suspended in the organic phase.

The term “water”, “water phase”, “water”, etc. used herein, refers to the environment, or which consists solely of water or comprises predominantly water in combination with other material, so the AK, for example, an inert organic solvent. In some embodiments of the amount of organic solvent present in the aqueous dispersions of the present invention, is less than 20 mass percent or less than 10 weight percent, or, in some cases, less than 5 weight percent, or, in yet other cases, less than 2 weight percent, with weight percents based on the total weight of the dispersion. Non-limiting examples of suitable organic solvents are monobutyl ether of propylene glycol, monohexadecyl ether of ethylene glycol, monobutyl ether of ethylene glycol, n-butanol, gasoline, alcohol, and white spirit.

The term “zakopalova in the polymer particles”as used herein, refers to particles that are at least partially enclosure (i.e. enclosed within the polymer to a degree sufficient for the physical separation of the particles from each other in aqueous dispersion, thereby preventing significant agglomeration of the particles. It will be understood, of course, that the dispersion of the present invention may also include particles that are not zakapsulirovannye in the polymer particles.

In some embodiments of the particles, zakopalova in the polymer in the aqueous dispersions of the present invention include nanoparticles. Term is n “nanoparticles” used herein, refers to particles that have an average particle size less than 1 micron. In some embodiments of the nanoparticles used in the present invention have an average particle size of 300 nanometers or less, namely 200 nanometers or less, or, in some cases, 100 nanometers or less. Thus, in some embodiments of the aqueous dispersions of the present invention include nanoparticles, which enclosure (polymer and, therefore, substantially non-agglomerated.

For the purposes of the present invention, the average particle size can be measured according to known methods of laser scattering. For example, the average particle size can be determined using laser diffraction device for determining particle size Horiba Model LA 900, which uses a helium-neon laser with a wavelength of 633 nm for the measurement of particle size and comes from the fact that the particles have a spherical shape, i.e., “particle size” refers to the smallest sphere that completely surrounds the particle. The average particle size may also be determined by visual investigation of electron micrograph images of transmission electron microscopy (“THE”) a representative sample of particles, measuring the diameter of the particles in the image, and calculating from the front of the main particle size of the measured particles on the basis of the zoom. The specialist will understand how to get THE image and to determine the primary particle size based on the magnification. The primary particle size of the particles refers to the smallest diameter of the sphere, completely surrounding the particle. The term “primary particle size”used herein refers to the size of the individual particles.

The shape (or morphology) of the particles may vary. For example, can usually be used a spherical morphology (such as solid beads, microbuses or hollow spheres), as well as particles, which are cubic, lamellar or acicular (elongated or fibrous). In addition, the particles can have an internal structure that is hollow, porous or free from voids, or a combination of any of the preceding, for example a hollow center with a porous or solid walls. For more information about the characteristics of suitable particles, see N. Katz and others (EDS.), Handbook of Fillers and Plastics (1987) at pages 9-10.

Depending on the desired properties and characteristics of the dispersion and/or compositions for the coating of the present invention (e.g., hardness, resistance to scratching, stability or color) can be used a mixture of one or more particles having different average particle sizes.

Particles, such as nanoc Stacy, present in the aqueous dispersions of the present invention, can be formed from polymeric and/or polimernyh inorganic materials, polymeric and/or polimernyh organic materials, composite materials, and mixtures of any of the preceding. “Formed from”as used herein, refers to open, for example “comprising”, the language of the claims. For this reason, the composition or substance, “formed from” list of these components are composition that includes at least the data specified components, and may also include other unspecified components during formation of the composition. In addition, it is understood that the term “polymer”as used herein includes oligomers and includes without limitation and homopolymers and copolymers.

The term “inorganic polymer material”as used herein, means a polymeric material having the repeating elements of the main circuit, based on the element or elements other than carbon. In addition, the term “polymeric organic materials”as used herein means a synthetic polymeric materials, synthetic polymeric materials and natural polymeric materials, all of the cat is, which contain the main chain of the repeating elements are carbon-based.

The term “organic material” used herein means a carbon-containing compounds in which the carbon is usually associated with the carbon and hydrogen and often also with other elements, and eliminates double compounds, such as carbon oxides, the carbides, carbon disulfide, etc.; such ternary compounds as the cyanides of metals, CARBONYLS metals, phosgene, carbondisulfide etc.; and carbon-containing ionic compounds, such as metal carbonates, such as calcium carbonate and sodium carbonate.

The term “inorganic material”as used herein means any material that is not organic material.

The term “composite material”as used herein, means a combination of two or more different materials. Particles formed from composite materials usually have a hardness at its surface, which is different from the hardness of the inner parts of the particles beneath the surface. More specifically, the surface of the particle can be modified by any method well known in the prior art, including, but not limited to, chemical or physical changes its surface properties using techniques known in the art.

For example, the particle may be the way the van from the core material, covered with, coated or encapsulated with one or more secondary material for the formation of composite particles, which has a softer surface. In some embodiments of the particles formed from composite materials can be formed from a primary material that is coated, plated or encapsulated by another form of the base material. For more information about the particles that are applicable in the present invention, see G. Wypych, Handbook of Fillers, 2nd Ed. (1999), pages 15-202.

As indicated above, the particles that are applicable in the present invention, can include any inorganic materials known in the prior art. Suitable particles can be formed from ceramic materials, metallic materials, and mixtures of any of the preceding. Non-limiting examples of such ceramic materials can include metal oxides, mixed metal oxides, metal nitrides, metal carbides, sulfides of metals, silicates of metals, borides of metals, metal carbonates, and mixtures of any of the above. Specific non-limiting examples of the metal nitride is boron nitride; specific non-limiting example of a metal oxide is zinc oxide; non-limiting examples of suitable mixed metal oxides are aluminum silicates and silicates m is fester; non-limiting examples of suitable sulfides of metals are molybdenum disulfide, tantalum disulfide, tungsten disulfide, and zinc sulfide; non-limiting examples of silicates of metals are aluminum silicates and magnesium silicates such as vermiculite.

In some embodiments of the present invention, the particles include inorganic materials selected from aluminum, barium, bismuth, boron, cadmium, calcium, cerium, cobalt, copper, iron, lanthanum, magnesium, manganese, molybdenum, nitrogen, oxygen, phosphorus, selenium, silicon, silver, sulfur, tin, titanium, tungsten, vanadium, yttrium, zinc and zirconium, including their oxides, nitrides, phosphides, phosphates, selenides, sulfides, sulfates, and mixtures thereof. Suitable non-limiting examples of the above inorganic particles include aluminum oxide, silicon dioxide, titanium dioxide, cerium oxide, zirconium oxide, bismuth oxide, magnesium oxide, iron oxide, aluminum silicate, boron carbide, nitrogen-doped titanium dioxide and cadmium selenide.

The particles can include, for example, the core is essentially individual inorganic oxide such as silica in colloidal, dispersed or amorphous form, alumina or colloidal alumina, titanium dioxide, iron oxide, cesium oxide, yttrium oxide, colloidal yttria,Zirconia, for example, colloidal or amorphous Zirconia, and mixtures of any of the above; or an inorganic oxide of one type, on which is deposited an organic oxide of another type.

Polimernye inorganic materials, applicable in the formation of particles used in the present invention may include inorganic materials selected from graphite, metals, oxides, carbides, nitrides, borides, sulfides, silicates, carbonates, sulfates, and hydroxides. A non-limiting example of applicable inorganic oxide is zinc oxide. Non-limiting examples of suitable inorganic sulfides include molybdenum disulfide, tantalum disulfide, tungsten disulfide, and zinc sulfide. Non-limiting examples of applicable inorganic silicates include aluminum silicates and magnesium silicates such as vermiculite. Non-limiting examples of suitable metals include molybdenum, platinum, palladium, Nickel, aluminum, copper, gold, iron, silver, alloys and mixtures of any of the foregoing.

In some embodiments of the particles can be selected from finely dispersed silicon dioxide, amorphous silica, colloidal silica, alumina, colloidal alumina, titanium dioxide, iron oxide, cesium oxide, yttrium oxide, colloidal yttria, dioxide circus is tion, colloidal Zirconia and mixtures of any of the above. In some embodiments of the particles include colloidal silicon dioxide. As disclosed above, these materials can be processed or unprocessed surface. Other applicable particles include silica surface modified, those described in U.S. patent 5 853 809 from column 6, line 51 to column 8, line 43, incorporated herein by reference.

As another option, the particle can be formed from a primary material that is coated, plated or encapsulated one or more secondary material to form a composite material, which has a more solid surface. Alternatively, the particle may be formed from a primary material that is coated, plated or encapsulated different shape base material with the formation of a composite material, which has a more solid surface.

In one example, and without limiting the present invention, the inorganic particle formed from an inorganic material such as silicon carbide or aluminum nitride, may be provided with a coating of silicon dioxide, carbonate or nanoglide for education applicable composite particles. In another unlimited example silane school is that the agent with alkyl side chains can interact with the surface of inorganic particles, formed of inorganic oxide to obtain the applicable composite particles having a “softer” surface. Other examples include cladding, encapsulating or covering the particles formed from polimernyh or polymeric materials with different polimernymi or polymeric materials. Concrete unlimited example of such composite particles is DUALITE™, which is a synthetic polymer particle coated calcium carbonate, which is commercially available from Pierce and Stevens Corporation of Buffalo, NY.

In some embodiments of the particles used in the present invention, have a lamellar structure. Particles having a lamellar structure composed of sheets or plates of atoms in a hexagonal lattice, with a strong bonding within the sheet and weak van der Waals bonding between the sheets, providing a low shear strength between sheets. Unlimited example lamellar structure is a hexagonal crystal structure. Particles of inorganic solid substance having a lamellar fullerene (i.e., baseball) structure is also applicable in the present invention.

Non-limiting examples of suitable materials having a lamellar structure, include boron nitride, graphite, metal dichalcogenides, Slu is, talc, gypsum, kaolinite, calcite, cadmium iodide, silver sulfide, and mixtures thereof. Suitable dichalcogenides metals include molybdenum disulfide, diselenide molybdenum, tantalum disulfide, diselenide tantalum, tungsten disulfide, diselenide tungsten and mixtures thereof.

Particles can be formed from polimernyh organic materials. Unlimited examples polimernyh organic materials, applicable in the present invention include, but are not limited to such, stearates such as zinc stearate and aluminum stearate), diamond, soot and stearamide.

The particles used in the present invention, can be formed from inorganic polymeric materials. Non-limiting examples of applicable inorganic polymeric materials include polyphosphazene, polysilane, polysiloxane, polygermane, polymeric sulfur, polymeric selenium, silicon containing materials and mixtures of any of the above. Specific non-limiting example of a particle formed from an inorganic polymeric material suitable for use in the present invention, is Tospearl, which is a particle formed from cross-linked siloxanes, commercially available from Toshiba Silicones Company, Ltd., Japan.

Particles can be formed from a synthetic organic polymer materials. Non-limiting examples of sentence is different organic polymeric materials include, but not limited to, thermoset materials and thermoplastic materials. Non-limiting examples of suitable thermoplastic materials include thermoplastic polyesters such as polyethylene terephthalate, polybutylene terephthalate and polyethylenterephthalat; polycarbonates; polyolefins, such as polyethylene, polypropylene and polyisobutene; acrylic polymers, such as copolymers of styrene and a monomer of acrylic acid and polymers containing methacrylate, polyamides, thermoplastic polyurethanes, vinyl polymers, and mixtures of any of the foregoing.

Non-limiting examples of suitable thermoset materials include thermosetting polyesters, vinyl esters, epoxy materials, phenolic resins, aminos, thermoset polyurethanes and mixtures of any of the above. Specific non-limiting example of a synthetic polymer particles formed from an epoxy material, is the particle epoxy microgel.

Particles may also be hollow particles formed from materials selected from polymeric and polimernyh inorganic materials, polymeric and polimernyh organic materials, composite materials and mixtures of any of the above. Non-limiting examples of suitable materials from which may be formed hollow part is s, above.

In some embodiments of the particles used in the present invention include organic pigment, for example, azo compounds (monoazo, diazo, β-naphthol, azo-pigmented varnishes type of salt Naphthol AS, benzimidazolone,

vasocongestion, isoindoline, isoindoline) and polycyclic (phtalocyanine, chinaredorbit, Pereladova, perinova, diketopiperazine, thioindigo, antrahinonovye, indanthrene, accreditedonline, flavanonol, philanthropie, anthanthrene, dioxazine, triarylamine, chieftancy) pigments and mixtures of any of the above. In some embodiments of an organic material selected from perylenes, kinokritikov, phthalocyanines, isoindolines, dioxazines (i.e., tribendimidine), 1,4-declareroles, entrepremedia, anthanthrene, flavanonol, indanthrene, perinone, paratroop, thioindigo, 4,4'-diamino-1,1'-diantaranya, and their substituted derivatives and mixtures thereof.

Perylenebis pigments used in the practical implementation of the present invention can be unsubstituted or substituted. Substituted perylenes can be substituted, for example, imenik nitrogen atoms, and the substituents may include from 1 to 10 carbon atoms, the alkyl groups of from 1 to 10 carbon atoms, alkoxy groups and halogen (such as chlorine) Ilyich combination. Substituted perylenes can contain more than one of any Deputy. Preferred diimide and dianhydride perylene-3,4,9,10-tetracarbonyl acid. Untreated perylenes can be obtained by methods known in the art.

Can be used phthalocyanine pigments, especially metal phthalocyanines. Although copper phthalocyanines are more easily available, can also be used for other metal-containing phthalocyanine pigments, such as those based on zinc, cobalt, iron, Nickel and other such metals. Also suitable not containing metal phthalocyanines. Phthalocyanine pigments may be unsubstituted or partially substituted, for example, by one or more alkyl (containing 1 to 10 carbon atoms); alkoxy containing from 1 to 10 carbons), halogen, such as chlorine, or other substituents typical of phtalocyanine pigments. Phthalocyanines can be obtained in any of several ways known in the prior art. They are usually produced by reaction of phthalic anhydride, phthalonitrile or derivatives thereof, with a donor metal, a donor of nitrogen (such as urea or phthalonitrile) and an optional catalyst, preferably in an organic solvent.

Chinaredorbit pigments that are used in this document, include unsubstituted alsamixergui chinagreen (for example, with one or more alkyl, alkoxy, halogen, such as chlorine, or other substituents typical of chinagruzovik pigments) and are suitable for the practical implementation of the present invention. Chinaredorbit pigments can be obtained in any of several ways known in the prior art, but is preferably obtained by thermal closure rings in various predecessors 2,5-dianilinoethane acid in the presence of polyphosphoric acid.

Isoindoline pigments, which may not necessarily be symmetrically or asymmetrically substituted, also suitable for the practical implementation of the present invention can be obtained by methods known in the art. Suitable isoindoline pigment, pigment yellow 139, is symmetrical adduct iminoisoindolin and predecessors barbituric acid. Dioxazine pigments (i.e., tribendimidine) are also suitable organic pigments and can be obtained by methods known in the art.

Can also be used mixtures of any of the previously described herein inorganic particles and/or organic particles.

Particles that are applicable in the aqueous dispersions of the present invention may include giving the color of the particles. The term "giving color particle" refers to what asticou, which largely absorbs some wavelengths of visible light, that is, wavelengths ranging from 400 to 700 nm; a greater extent than it absorbs other wavelengths in the visible region.

If desirable, the above particles can be formed into nanoparticles. In some embodiments of the nanoparticles are formed in situ during the formation of a water dispersion decapsulating in the polymer particles, which are described in more detail later. In other implementations, however, the nanoparticles are formed before their inclusion in the aqueous dispersion. In these embodiments of the nanoparticles can be formed by any of various methods known in the art. For example, nanoparticles can be obtained by grinding and fractionation of dry dispersed material. For example, the volume pigments, such as any of the inorganic or organic pigments, discussed above, can be reduced with grinding media having a particle size of less than 0.5 millimeters (mm), or less than 0.3 mm, or less than 0.1 mm, the pigment Particles are usually crushed to the size of the nanoparticles in the mill high power in one or more solvents (or water, organic solvent, or a mixture of the two), optionally in the presence of polymeric binders. If necessary, can be included aspergilosis agent, for example, if in an organic solvent) SOLSPERSE® 32000 32500 or available from Lubrizol Corporation, or (if in water) SOLSPERSE® 27000, also available from the Lubrizol Corporation. Other suitable methods for nanoparticles include crystallization, deposition, gas-phase condensation and chemical abrasion (i.e., a partial dissolution).

In some embodiments of zakopalova in the polymer to give the color particles used in the present invention include, for example, a polymer selected from acrylic polymers, polyurethane polymers, polymeric esters, polymeric ethers, polymers, silicon-based, their copolymers and their mixtures. Such polymers can be obtained by any suitable method known to experts in the field that applies the present invention. Suitable polymer includes disclosed in patent application U.S. 10/876 031 [0061] to [0076]cited of which is incorporated herein by reference, and published patent application U.S. 2005/0287348 A1 [0042] to [0044], the cited portion of which is incorporated herein by reference.

However, as indicated, in other embodiments of the aqueous dispersions of the present invention include particles, zakopalova in a brittle polymer. The term "brittle polymer"used herein refers to poly is ERU, which is easily crushed when environmental conditions. Thus, after removing the liquid material from the dispersion, the resulting solid material is readily broken into small fragments or portions, such that would be suitable as the solid material feed in the extruder to obtain a coating composition of the powder material. On the other hand, film-forming polymer after removal of the liquid materials of the dispersion formed would napravicemo continuous film on at least a horizontal surface of the substrate. As used herein, the term "environment" refers to the environmental conditions, which often represent approximately a pressure of one atmosphere, 50% relative humidity and 25°C.

In some embodiments of the present invention brittle polymer includes the reaction product of (i) a polymerizable polyester polyurethane, and (ii) an ethylene-unsaturated monomer. The term "polymerizable polyester polyurethane"as used herein refers to a polymer that includes a variety of ester units

and many of urethane units

has functional groups which are capable of polymerization with the formation of larger polim the RA, and where R1is alkyl, cycloalkyl or oxyalkylene functional group, R2is alkyl or cycloalkyl functional group, and R3is alkyl, cycloalkyl, aranceles or aromatic functional group. In some embodiments of polymerizable polyester polyurethane comprises a polyester polyurethane having terminal ethylene unsaturation. As used herein, the term “terminal ethylene unsaturation” means that at least some of the terminal ends of the polyester polyurethane containing functional group containing ethylene unsaturation. Such polyether polyurethanes may also include, but need not necessarily include, internal ethylene unsaturation. As a result, in some embodiments of the aqueous dispersions of the present invention include polymerizable polyester polyurethane having terminal ethylene unsaturation, which is obtained from reactants comprising (a) a polyisocyanate, (b) a polyester polyol and (C) a material comprising ethylene-unsaturated group and an active hydrogen group. In some embodiments of polymerizable polyester polyurethane, used in the aqueous dispersions of the present invention, the image is raised from the reagents, including additional (g) polyamine and/or (d) a material comprising an acid functional group or anhydride and a functional group capable of reacting with isocyanate or hydroxyl groups. The term “active hydrogen group”used herein refers to functional groups which are relatively reactive isocyanates, as determined by the test Zerewitnoff, which is described in the JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, Vol.49, str (1927).

The polyisocyanates suitable for use in obtaining a polymerizable polyester polyurethane, include aliphatic, cycloaliphatic, analiticheskie and/or aromatic isocyanates and mixtures thereof.

Examples of applicable aliphatic and cycloaliphatic polyisocyanates include 4,4-methylenebisacrylamide diisocyanate (hydrogenated MDI), hexamethylene diisocyanate (HDI), isophorone diisocyanate (EPDI), Methylenebis(cyclohexyl isocyanate), trimethyl hexamethylene diisocyanate (TMDI), meta-tetramethylsilane diisocyanate (TMXDI) and cyclohexyl diisocyanate (hydrogenated XDI). Other aliphatic polyisocyanates include isocyanurate IPDI and HDI.

Examples of suitable aromatic polyisocyanates include tollen diisocyanate (TDI) (i.e., 2,4-toolen diisocyanate, 2,6-toolen diisocyanate or a mixture thereof), difenilmetana-4,4-diisocyanate (MDI), n is ftolen-1,5-diisocyanate (NDI), 3,3-dimethyl-4,4-biphenylene diisocyanate (TODI), crude TDI (i.e., a mixture of TDI and its oligomer), polymethylenepolyphenylene the polyisocyanate, crude MDI (i.e., a mixture of MDI and its oligomer), xylylene diisocyanate (XDI) and the diisocyanate of phenylene.

Suitable polyisocyanate are derived, obtained from hexamethylenediisocyanate, 1-isocyanato-3,3,5-trimethyl-5-isocyanatomethyl (“IPDI”), including its isocyanurate and/or 4,4'-bis(isocyanatophenyl)methane.

In some embodiments of the amount of MDI used to obtain the polymerizable polyester polyurethane, varies in the range from 20 to 70 mass%, namely from 30 to 60 weight percent, or, in some cases, from 40 to 50 weight percent, with weight percents are based on the total weight of solids of the resin used to obtain the polymerizable polyester polyurethane.

Polyester polyols suitable for use in obtaining a polymerizable polyester polyurethane, can be obtained by any suitable means, for example using a saturated dicarboxylic acids or their anhydrides (or combination of acids and anhydrides and polyhydric alcohols, or hinged ring caprolactone, for example the Epsilon caprolactone. Such polyether polyols with the ranks molecular weights are commercially available. Aliphatic dicarboxylic acids suitable for the production of polyesters include those containing from 4 to 14, namely from 6 to 10 carbon atoms inclusive. Examples of such dicarboxylic acids include succinic acid, glutaric acid, adipic acid, timelineview acid, cork acid, azelaic acid and sabotinova acid. Can also be used the corresponding anhydrides. Usually use adipic and azelaic acid.

Polyhydric alcohols used in obtaining polyesters of polyols suitable for use in obtaining a polymerizable polyester polyurethane, used in some embodiments of the present invention include, without limitation, aliphatic alcohols containing at least 2 hydroxyl groups, for example, glycols with a linear chain containing from 2 to 15, in particular from 4 to 8 carbon atoms inclusive. In some embodiments of the glycols contain hydroxyl groups in the terminal positions. Non-limiting examples of such polyhydric alcohols include ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, 1,3-propandiol, 1,3-butanediol, 1,4-butanediol, 1,5-pentanediol, 2,2-dimethylpropanoyl, 1,5-hexanediol, 1,7-heptanediol, 1,8-octanediol, 1,10-decandiol and mixtures of such polyols.

In kotoryj embodiments of polyester polyol get the reaction of the dicarboxylic acid (or its anhydride) with a polyhydric alcohol in the presence of an esterification catalyst, such as ORGANOTIN catalyst. The amount used of the acid and alcohol will vary and depend on the desired molecular weight of the polyester. Polyesters with terminal hydroxyl groups obtained using an excess of the alcohol, thereby obtaining a linear chain containing a predominant amount of terminal hydroxyl groups. Examples of polyesters include poly(1,4-butylene adipate), poly (1,4-butylene succinate), poly(1,4-butylene glutarate), poly(1,4-butylene pimelate), poly(1,4-butylene, suberate), poly (1,4-butylene azlat), poly(1,4-butylene sebacina) and poly(Epsilon caprolactone). In some embodiments of polyester polyol to be used to obtain khrupkogo polymerizable polyester polyurethane, used in the aqueous dispersions of the present invention has a mass-average molecular weight of from 500 to 3000, in particular from 500 to 2500, or, in some cases, from 900 to about 1300.

In some embodiments of the amount of polyester polyol used to produce polymerizable polyester polyurethane, included in some of the embodiments of the present invention, varies from 10 to 60 mass percent, namely from 20 to 50 mass percent or, in some cases, 30 to 40 weight percent, with weight percents are based on the total weight of solids of the resin, used for polucheniya polymerizable polyester polyurethane.

As indicated, the polymerizable polyester polyurethane in some embodiments of the aqueous dispersions of the present invention are formed from a material comprising ethylene-unsaturated group and an active hydrogen group. Suitable ethylene-unsaturated groups include, for example, acrylates, methacrylates, allyl carbamates and allyl carbonates. Acrylate and methacrylate functional groups can be represented by the formula CH2=C(R1)-C(O)O-, where R1is hydrogen or stands. The allyl carbamates and carbonates may be represented by the formula CH2=CH-CH2-NH-C(O)O-, and CH2=CH-CH2-O-(O)O-, respectively.

In some embodiments of the material comprising the ethylene unsaturated group and an active hydrogen group that is used to obtain polymerizable polyester polyurethane, includes hydroxyalkyl (meth)acrylate. Suitable hydroxyalkyl(meth)acrylates include those containing from 1 to 18 carbon atoms in the alkyl radical, the alkyl radical is substituted or unsubstituted. Specific non-limiting examples of such materials include 2-hydroxyethyl (meth)acrylate, 2-hydroxypropyl (meth)acrylate, 2-hydroxybutyl (meth)acrylate, hexane-1,6-diol mono(meth)acrylate, 4-hydroxybutyl(meth)acrylate, as well as their mixtures. It is implied that the term "(meth)acrylate"used herein includes both acrylates and methacrylates.

In some embodiments of the amount of material comprising the ethylene-unsaturated group and an active hydrogen group, used to obtain a polymerizable polyester polyurethane, varies from 1 to 12 mass%, namely from 2 to 8 mass percent or, in some cases, from 4 to 6 weight percent, with weight percents are based on the total weight of solids of the resin used to obtain the polymerizable polyester polyurethane.

As mentioned previously, in some embodiments of polymerizable polyester polyurethane present in some embodiments of the aqueous dispersions of the present invention, is obtained from polyamine. Applicable polyamine include, but are not limited to such, primary or secondary diamines or polyamine, in which groups connected to the nitrogen atoms can be saturated or unsaturated; aliphatic; alicyclic; aromatic; aliphatic, substituted aromatic; aromatic, substituted aliphatic; and heterocyclic. Typical suitable aliphatic and alicyclic diamines include 1,2-Ethylenediamine, 12-propylene diamine, 1,8-octane diamine, isophorone diamine, propane-2,2-cyclohexyl amine, etc. Typical suitable aromatic diamines include phenylendiamine and toluene diamines such as o-phenylenediamine and p-toolen diamine. These and other suitable polyamine described in detail in U.S. patent 4 046 729 from column 6, line 61 to column 7, line 26, the cited portion of which is incorporated herein by reference.

In some embodiments of the amount polyamine used to obtain polymerizable polyester polyurethane, varies from 0.5 to 5 mass percent, namely from 1 to 4 mass percent or, in some cases, from 2 to 3 weight percent, with weight percents are based on the total weight of solids of the resin used to obtain the polymerizable polyester polyurethane.

As indicated previously, in some embodiments of polymerizable polyester polyurethane in certain embodiments of the aqueous dispersions of the present invention are obtained from a material comprising an acid functional group or anhydride and a functional group reactive towards isocyanate or hydroxyl groups of other components from which the material is formed of polyurethane. Apply acid-functional materials include compounds is within the structure:

X-Y-Z,

where X is HE, SH, NH2or other, a R includes alkyl, aryl, cycloalkyl, substituted alkyl, substituted aryl and substituted cycloalkyl groups and mixtures thereof; Y comprises an alkyl, aryl, cycloalkyl, substituted alkyl, substituted aryl and substituted cycloalkyl groups and mixtures thereof; a Z includes OSO3H, COOH, OPO3H2, SO2OH, POOH and PO3H2and mixtures thereof.

Examples of suitable acid functional materials include hydroxypivalic acid, 3-hydroxy-butane acid, D,L-tropovoe acid, D,L-hydroxy malonic acid, D,L-maleic acid, citric acid, thioglycolic acid, glycolic acid, amino acid, 12-hydroxy stearic acid, Dimethylol propionic acid, mercapto propionic acid, mercapto butyric acid, mercapto succinoyl acid and mixtures thereof.

Applicable anhydrides include aliphatic, cycloaliphatic, olefinic, cycloolefinic and aromatic anhydrides. Substituted aliphatic and aromatic anhydrides are also applicable, if the substituents do not adversely affect the reactivity of the anhydride or the properties of the resulting polyurethane. Examples of the substituents include chlorine, alkyl and alkoxy. Examples of anhydrides include succinic (succinoyl) anhydride, macilenta is hydrated (methylsuccinate) anhydride, dodecanesulfonyl anhydride, octadecadienyl anhydride, phthalic anhydride, tetrahydrophthalic anhydride, methyltetrahydrophthalic anhydride, hexahydrophthalic anhydride, alkyloxytriphenylene anhydrides, such as methylhexahydrophthalic anhydride, tetrachlorophthalic anhydride, endometrin tetrahydrophthalic anhydride, trimellitic anhydride, florentintsy anhydride, itacademy anhydride, citraconic anhydride, maleic anhydride and mixtures thereof.

In some embodiments of the acid functional material or anhydride to provide polymerizable polyester polyurethane with an ionisable anionic groups that can be ionized to solubilize the polymer in water. As a result, in some embodiments of the polymerized polyester polyurethane present in some embodiments of the aqueous dispersions of the present invention is dispersible in water. The term “dispersible in water”as used herein means that the material can be dissolved in water without excipients or application of surfactants. The term “ionizable”as used herein means a group capable of becoming the ion, that is capable of dissociating ions or become electric is Eski charged.

The acid may be neutralized by the base with the formation of the carboxylate salt group. Examples of anionic groups include-OSO3-, -COO-, -OPO3=, -SO2O-POO-; and PO3=.

In some embodiments of the amount of material comprising an acid functional group or anhydride and a functional group reactive in relation to the isocyanate or hydroxyl groups, used to obtain a polymerizable polyester polyurethane, varies from 5 to 20 mass percent, namely from 7 to 15 mass percent or, in some cases, from 8 to 12 mass percent mass percent based on the total weight of solids of the resin used to obtain the polymerizable polyester polyurethane.

As indicated, in some embodiments of the acid groups are neutralized by a base. Neutralization may vary from about 0.6 to about 1.1, namely from 0.4 to 0.9 or, in some cases, from 0.8 to 1.0 from total theoretical neutralization equivalent. Suitable neutralizing tools include inorganic and organic bases, such as sodium hydroxide, potassium hydroxide, ammonia, amines, alcohol amines having at least one primary, secondary or tertiary amino groups and, at least one hydroxyl group. Suitable amines include aliphatic aminoalcohols, such as monoethanolamine, diethanolamine, dimethylaminoethanol, diisopropanolamine etc.

Polymerizable polyester polyurethane, used in some embodiments of the aqueous dispersions of the present invention, can be formed by combining the above components in any suitable order. For example, the polymerizable polyester polyurethane can be obtained using the techniques of polymerization in solution, which is clear to experts in the field of technology to which the present invention relates.

As should be evident from the preceding description, the polymerizable polyester polyurethane present in some embodiments of the present invention may be nonionic, anionic or cationic. In some embodiments of polymerizable polyester polyurethane will have srednevekovoy molecular weight of less than 150 000 grams per mole, and it is from 10,000 to 100,000 grams per mole, or, in some cases, from 40 000 to 80 000 grams per mole. The molecular weight of the polyurethane and other polymeric materials used in the practical implementation of the invention is determined by gel permeation chromatography using a polystyrene standard.

How would the ü is evident from the preceding description, the present invention relates to dispersible in water polymerizable polyester polyurethane containing a terminal ethylene-unsaturated groups and formed from components comprising (a) a polyisocyanate, (b) a polyester polyol, (b) polyamine, (g) material containing ethylene unsaturated group and an active hydrogen group, and (d) a material containing an acid functional group or anhydride and an active hydrogen group. In some embodiments of the present invention relates to dispersible in water, the polymerizable polyester polyurethane containing a terminal ethylene-unsaturated groups, formed from components containing (a) the polyisocyanate is present in a quantity which varies from 20 to 70 mass%, (b) a polyester polyol in amounts varying from 10 to 60 mass%, (b) polyamine in amounts varying from 0.5 to 5 mass percent (g) material containing ethylene unsaturated group and an active hydrogen group that is present in a quantity varying from 1 to 12 mass%, and (d) a material containing an acid functional group or anhydride and an active hydrogen group, present in amounts varying from 5 to 20 mass percent.

As indicated previously, in some embodiments of podnyavshisj of the present invention is brittle polymer, which comprises the reaction product of (i) a polymerizable polyester polyurethane, such as the one described earlier, and (ii) an ethylene-unsaturated monomer. Suitable ethylene-unsaturated monomers include any of the polymerizable ethylene-unsaturated monomers known in the technology, including vinyl monomers. Non-limiting examples of applicable ethylene-unsaturated monomers containing functional groups carboxylic acid include (meth)acrylic acid, beta-carboxyethyl acrylate, aryloxyphenoxy acid, crotonic acid, fumaric acid, monoalkyl esters of fumaric acid, maleic acid, monoalkyl esters of maleic acid, taconova acid, monoalkyl esters basis of itaconic acid and mixtures thereof. The term "(meth)acrylic" and made from it the terms used herein are meant to include both acrylic and methacrylic.

Non-limiting examples of other applicable ethylene-unsaturated monomers containing no functional groups of the carboxylic acid include alkalemia esters of (meth)acrylic acid, such as ethyl (meth)acrylate, methyl(meth)acrylate, butyl (meth)acrylate, 2-ethylhexyl (meth)acrylate, 2-hydroxyethyl (meth)acrylate, hydroxypropyl (meth)acrylate, hydroxy butyl (meth)acrylate, from bornyl (meth)acrylate, lauryl (meth)acrylate, ethylene glycol di(meth)acrylate; vinyl aromatic hydrocarbons such as styrene and vinyltoluene; (meth)acrylamide, such as N-butoxymethyl acrylamide; Acrylonitrile; dialkylamino esters of maleic and fumaric acids; vinyl and vinylidene halides; vinyl acetate; simple vinyl ethers; simple allyl ethers; allyl alcohols; derivatives thereof and mixtures thereof.

The ethylene-unsaturated monomers may also include ethylene-unsaturated monomers with a beta-hydroxy ester functional group, such that the resulting reaction of the monomer having an ethylene-unsaturated acid functional group, such as monobasic carboxylic acid such as acrylic acid, epoxysilane, which does not participate in the initiated free radical polymerization with the monomer of unsaturated acids. Examples of such epoxy compounds are glycidyloxy ethers and esters. Suitable glycidyloxy esters include glycidyloxy ethers of alcohols and phenols such as butyl glycidyloxy ether, octyl glycidyloxy ether, phenyl glycidyloxy ether, etc.

In some embodiments of polymerizable polyester polyurethane and ethylene-unsaturated monomer present in the aqueous dispersions of the present invention in a weight ratio of from 95:5 to 30:70, and it is from 90:10 to 40:60, or, in some cases, from 80:20 to 60:40.

Aqueous dispersions containing zakopalova in the polymer particles of the present invention, include whether they are brittle polymer or not, can be obtained by any number of ways. For example, in some embodiments of the aqueous dispersions of the present invention obtained by the method containing (A) receiving in an aqueous medium a mixture of (i) particles, (ii) one or more polymerizable ethylene-unsaturated monomer and/or (iii) mixtures of one or more polymerizable unsaturated monomers with one or more polymers and/or (iv) one or more polymers, and the subsequent impact on the mix of high shearing forces in the presence of the aquatic environment.

Such methods are described in detail in patent application U.S. 10/876,031 [0054] to [0090], incorporated herein by reference, and published patent application U.S. 2005/0287348 [0036] to [0050], the cited portion of which are incorporated herein by reference.

However, in other embodiments of the aqueous dispersions of the present invention produced by the method comprising (1) receiving in an aqueous medium a mixture of (i) particles (ii) polymerizing the ethylene-unsaturated monomer and (iii) dispersible in water polymerizable dispersant funds, and (2) the polymerization of the ethylene-unsaturated monomer and polymerizable disingenuous the th education decapsulating in the polymer particles, containing dispersible in water the polymer. In these embodiments of polymer dispersing agent may include any polymerizable material which is dispersible in water and which in the course of polymerization with ethylene-unsaturated monomer forms zakopalova in the polymer particles, comprising dispersible in water the polymer, in some cases dispersible in water brittle polymer. In some embodiments of polymerizable dispersion means includes the previously described dispersible in water polymerizable polyester polyurethane having terminal ethylene unsaturation.

In these embodiments of dispersible in water polymer dispersing agent capable of dispersing itself and other materials, including ethylene-unsaturated monomers in an aqueous environment without the need for surfactants and/or conditions of high shearing forces. In the above method of obtaining a water dispersion decapsulating in the polymer particles are particularly suitable in situations where the application of high shearing forces, described in patent application U.S. 10/876,031 [0081] to [0084] of the published patent application U.S. 2005/0287348 in [0046]that is undesirable or impossible. Therefore, in some embodiments, the realization of the purpose of the water dispersion of the present invention is produced by way which does not include the stage of exposure to conditions of high shearing forces on the mixture of the particles of the polymerizable ethylene-unsaturated monomer and dispersible in water polymerizable dispersant tools.

In addition, the above method of the present invention allows to obtain nanoparticles in situ rather than having to formation of nanoparticles before the preparation of water dispersion. In these ways, the particles having an average particle size of 1 micron or more, after mixing with the ethylene-unsaturated monomer and dispersible in water polymer dispersing agent in an aqueous medium, can be formed into nanoparticles (i.e., the nanoparticles are formed in situ). In some embodiments of the nanoparticles formed by the fact that in the aquatic environment affected by the conditions of grinding. For example, the particles can be reduced grinding media having a particle size of less than 0.5 mm, or less than 0.3 mm, or, in some cases, less than 0.1 millimeters. In these embodiments of the particles can be reduced to nanoscale particles in a grinder high power in the presence of an aqueous medium, polymerizing the ethylene-unsaturated monomer and dispersible in water polymerizable dispersant funds. If desirable, can be used more dispersing redtwo, such as SOLSPERSE 27000, available from Avecia, Inc.

As indicated, the above methods of obtaining aqueous dispersions of the present invention include the stage of free radical polymerization of the ethylene-unsaturated monomer and polymerizable dispersant funds from education decapsulating in the polymer particles containing dispersible in water the polymer. In some implementations, if applicable, at least part of the polymerization occurs during the formation of nanoparticles. Can also be used free-radical initiator. Can be used initiators soluble in both water and oil.

Non-limiting examples of suitable water-soluble initiators include peroxydisulfate ammonium, peroxydisulfate potassium and hydrogen peroxide. Non-limiting examples of oil-soluble initiators include tert-butyl hydroperoxide, dilapilated and 2,2'-azobis(isobutyronitrile). In many cases, the reaction is carried out at a temperature ranging from 20° to 80°C. the Polymerization can be performed, or periodic, or continuous process. The length of time required to implement the polymerization may be within, for example, from 10 minutes to 6 hours, provided that this time is sufficient for the formation of a polymer in situ from one or more ethylene-Nena is sennoga monomer.

Once the polymerization process is completed, the resulting product is a stable dispersion decapsulating in the polymer particles in the aqueous medium, which may contain a certain amount of organic solvent. A number or all of the organic solvent can be removed by distillation under reduced pressure at a temperature of, for example, less than 40°Stermin “stable dispersion” or “stably dispersed”as used herein means that zakopalova in the polymer particles do not settle, do not coagulate, not flocculent over time from the water environment.

In some embodiments of zakopalova in the polymer particles present in the aqueous dispersions of the present invention in amount of at least 10 weight percent, or in the range from 10 to 80 mass%, or from 25 to 50 weight percent, or in an amount of from 25 to 40 weight percent, with weight percents are based on the weight of the total amount of solids present in the dispersion.

In some embodiments of dispersed zakopalova in the polymer particles have a maximum turbidity of 10% or, in some cases, the maximum turbidity 5% or, in yet other cases, the maximum hmotnost the 1%, or, in other implementations, the maximum turbidity of 0.5%. "Turbidity"is used herein, is determined in accordance with ASTM D1003.

Values of turbidity for decapsulating in the polymer particles described in this document define the first receiving particles, such as nanoparticles, dispersed in a liquid (such as water, organic solvent and/or dispersing agent, which is described in this document), and then measuring the dispersion is diluted with a solvent, such as butyl acetate, using Byk-Gardner TCS (The Color Sphere), with the path length of the cell 500 microns. As % of turbidity of the liquid sample depends on the concentration, % of turbidity, which is used in this document describes how to pass from about 15% to about 20% at the wavelength of maximum absorption. Acceptable turbidity can be achieved for relatively large particles, if the difference in refractive index between the particles and the environment is small. On the contrary, for smaller particles large differences in refractive index between the particle and the environment can provide acceptable opacity.

In the above methods of the present invention during the reaction the ethylene-unsaturated monomer with polymerizable dispersant means the m formed zakopalova in the polymer particles, which, as previously indicated, the inventors believe leads to a phase barrier that physically prevents re-agglomeration of the particles, especially nanoparticles in aqueous dispersion. In the foregoing methods of the present invention lead to a water dispersion of particles, such as nanoparticles, in which the re-agglomeration of the nanoparticles is minimized or completely eliminated.

In some embodiments of the present invention relates to methods for decapsulating in the polymer particles. These methods, as previously described, include methods of obtaining water dispersion decapsulating in the polymer particles, in which zakopalova in the polymer particles include brittle polymer and also include (1) removing water from the aqueous dispersion for the formation of a solid material containing zakopalova in the polymer particles, and (2) grinding the solid material. In these embodiments of the water can be removed from the water dispersion of any suitable drying method, namely using a drum dryer, roller dryer, spray dryer or the like. In addition, the solid material can be fragmented using any suitable methods, namely using a hammer mill or similar. After grinding the resulting granules can be further processed,as it is sifted through a sieve before packing.

The present invention relates also to compositions for powder coatings formed from the aqueous dispersion decapsulating in the polymer particles. The term "composition for powder coating"as used herein, refers to compositions that can be used to produce coatings which are embodied rather dispersed solid form than in liquid form. In some embodiments of the compositions for powder coating of the present invention zakopalova in the polymer particles contain nanoparticles.

In addition to decapsulating in the polymer particles of the composition for powder coating of the present invention can contain a dispersion of film-forming resin. Suitable film-forming resins include, for example, epoxy resin, namely containing epoxypropyl acrylic polymer or polyglycidyl ether of a polyhydric alcohol and a suitable curing agent for epoxy resins, such as polyfunctional material containing groups, carboxylic acid or dicyanamide. Examples of curable dispersed resinous materials described in the replacement U.S. patent No.'RE 32261 and U.S. patent 4804581, which is included by reference in this document. Examples of other suitable dispersion of film-forming resins are resins having functional groups of carboxylic acids, such as the polyesters with functional groups carboxylic acid and acrylic polymers, and suitable hardeners for such materials, such as hardeners, triglycidyl isocyanurate and beta hydroxyalkylated, which are described, for example, in U.S. patent 4 801 680 and U.S. patent 4988767, which is included by reference in this document.

In some embodiments of the composition for powder coating of the present invention contain from 50 to 90 mass%, in particular from 60 to 80 weight percent of the dispersed film-forming resin, based on the total weight of the composition of the coating of the powder material. In some embodiments of the composition for powder coating of the present invention contain from 0.1 to 50 mass percent, namely from 1 to 20 mass percent, decapsulating in the polymer particles, based on the total weight of the composition of the coating of the powder material.

Composition for powder coating of the present invention can optionally include other materials, namely, other pigments, fillers, light stabilizers, modifiers fluidity, means to prevent cracking, and antioxidants. Suitable pigments include, for example, titanium dioxide, ultramarine blue, phthalocyanine blue, phthalocyanine green, carbon black, graphite fiber, black iron oxide, green oxide of chromium, yellow ferride and red quindo.

The composition can be added to the funds of predator the ban crack to allow any volatile material to evaporate from the film during firing. Benzoin is the usual preferred means of preventing cracking, and if used, is generally present in amounts of from 0.5 to 3.0 mass% relative to the total mass of the composition for powder coating.

In some embodiments of the composition for powder coating of the present invention include finely dispersed silicon dioxide or the like to reduce caking of the powder during storage. A sample of finely dispersed silicon dioxide sold Cabot Corporation under the trademark CAB-O-SIL. Colloidal silicon dioxide is present in amounts ranging from 0.1 to 1 mass% relative to the total weight of the powder coating composition.

The present invention relates also to a method of creating a composition for powder coating. In certain implementations, where zakopalova in the polymer particles contain brittle polymer, zakopalova in the polymer particles, and other components covering all unite in the dried, particulate form, are mixed together and then melt during mixing in the extruder. However, in other implementations, such as those cases in which use aqueous dispersion decapsulating in the polymer particles, which do not contain what it brittle polymer, composition for powder coating of the present invention is manufactured by the process comprising (1) introducing into an extruder components of the composition for powder coating, comprising: (a) aqueous dispersion decapsulating in the polymer particles and (b) dry materials; (2) mixing (a) and (b) in the extruder; (3) removing volatiles from the mixture to form an extrudate; (4) cooling the extrudate, and (5) grinding the extrudate to the desired particle size. The term "removal of volatile substances"as used herein means the removal of volatile materials, including water and organic solvents. In some embodiments of such compositions for powder coatings produced by the method and/or device described in published patent applications U.S. 2005/0212159 A1; 2005/0213423 A1; and/or 2005/0212171 A1, the relevant disclosure of which is incorporated herein by reference.

In these ways the present invention the dry materials may contain dispersed film-forming resin described previously, as well as any other additives to the composition. Dry materials can first be mixed in a mixer with a large shearing force, such as a planetary mixer. Then, in some embodiments of the dry material and the water dispersion of the present invention are mixed in the extruder at the temperature of the tour in the range from 80°to 150°C. Then the extrudate is cooled and milled to disperse the mixture.

Composition for powder coating of the invention can be applied to multiple frameworks, including a metal base, such as aluminum and steel framework. Compositions for powder coatings are often applied by spraying, and in the case of the metallic base by sputtering in an electrostatic field or by using the liquefied layer. Composition for powder coating of the present invention can be applied in one pass or multiple passes to obtain a film having a thickness after curing of from about 1 to 10 mils (25 to 250 microns), typically from about 2 to 4 mils (50-100 microns). In many cases, after applying the coating composition of the powder material coated base is heated to a temperature sufficient to cure the coating, often to a temperature ranging from 250°F to 500°F (121, 1million°C to 260,0°C) during the time from 1 to 60 minutes, for example from 300°F to 400°F (148,9°C to 204,4°C) for 15 to 30 minutes.

In the present invention refers also to the basics, such as a metal base at least partially covered with a coating deposited from a composition for powder coating of the present invention.

Composition for powder coating of the present invention can be used for education about inanaga coverage, for example, Monoporeia, transparent top cover or base coating in a two-layer system, or both; or as one or more layers of the multilayer system, including the composition of the transparent top coating layer of the dye and/or composition of the base coating and/or primer layer, including, for example, electrolytic layer deposited primer and/or filler.

The present invention relates also to the basics, at least partially covered with a complex multilayer coating in which at least one layer of a coating deposited from such compositions. For example, in some embodiments of the composition for powder coating of the present invention includes a layer of base coating in complex multilayer coating comprising a base and top coat. As a result, in these cases the implementation after applying and curing the composition for powder coating of the present invention on the base layer can be applied, at least one layer of the upper surface. The top coating may, for example, be applied from the composition for a powder coating composition for coating an organic solvent or composition for coating water-based, what is known in the prior art. Film-forming composition of the surface coating can be any compositie is, applicable for coatings, including, for example, film-forming composition, which comprises a resinous binder selected from acrylic polymers, polyesters, including Alcide, and polyurethanes. The composition of the top coating can be applied by any conventional methods of coating, such as coating by brush, spray, dipping or pouring, but most often they are applied by spraying. Can be used with conventional spraying techniques and equipment for air spraying, airless spraying, and electrostatic spraying or manual methods or automated methods.

In some embodiments of the present invention relates to a reflective surface at least partially covered by a layer which imparts color pokryvailo coating of the composition for powder coating, including a certain number decapsulating in polymer nanoparticles having a maximum turbidity of 10%. In some embodiments of the layer of transparent coating may be applied over at least part of a layer to give the color pokryvailo coverage.

The term “reflective surface”as used herein refers to a surface containing a reflective material having a total reflectance of at least 30%, such as at least 40%. “Total reflectance” refers herein to the ratio of reflected light from the object to the incident light, which affects the object in the visible spectrum when integrating over all angles. “Visible spectrum” refers herein to the portion of the electromagnetic spectrum that lies between the wavelengths of 400 and 700 nanometers. “Angle” refers herein to the angle between the ray observations and the normal to the surface at the point of incidence. The values of the reflection coefficient, described herein, can be determined, for example, when using a Minolta Spectrophotometer CM-3600d according to the instructions provided by the manufacturer.

In some embodiments of the reflective surface includes, among other things, a base material, such as, for example, polished aluminum, cold rolled steel, chromed metal or metal deposited in vacuum on the plastic. In other embodiments of the reflective surface can include pre-coated surface, which may, for example, include a layer of reflective coating made from the composition for coating, such as, for example, a layer of a base coating of metallic silver; the layer of base coating of painted metal; a layer of base coating containing mica; or white lyrics by the second base coating, among others.

Such layers reflective coatings can be applied from film-forming compositions, which may, for example, include any of the film-forming resins commonly used in the compositions of the protective coating. For example, film-forming composition reflective coatings may include resinous binder and one or more pigments to function as a pigment. Applicable resinous binders include, but are not limited to these, acrylic polymers, polyesters, including Alcide and polyurethanes. The resinous binder for the composition of the reflective coating may, for example, be embodied in a composition for a powder coating composition for coating solvent-based or compositions for coating water-based.

As noted, the composition of the reflective coatings may contain pigments as colorants. Suitable pigments for the composition reflective coatings include, for example, metal pigments, which include aluminum flake, copper or bronze flakes and mica coated with metal oxide; non-metallic color pigments such as titanium dioxide, iron oxide, chromium oxide, lead chromate and carbon black; and organic pigments, such as, for example, phtalocyanine blue and phtalocyanine green.

Composition reflected the actual operation of the coatings can be applied on the basis of any conventional method of coating such as, among other things, brush application, spraying, dipping or pouring. Can be used with conventional spraying techniques and equipment for air spraying, airless spraying, and electrostatic spraying or manual, or automatic way. During application of the base coating on the basis of the film thickness of the base coating formed on the basis of, often is in the range from 0.1 to 5 mils (2.5 to 127 micrometers) or from 0.1 to 2 mils (2.5 to 50.8 micrometers to).

After forming the base film reflective coatings reflective coatings may be cured or, alternatively, to undergo the stages of drying, in which the solvent is removed from the base film of the coating during heating or drying air before applying the following coating compositions. Suitable drying conditions will depend on the specific composition of the base coating and the ambient humidity if the composition is water origin, but will often be sufficient drying time from 1 to 15 minutes at a temperature of from 75°F to 200°F (21°C to 93°C).

The reflective surface of the present invention at least partially covered by a layer which imparts color pokryvailo coating of the composition for powder coating of the present invention. The term “layer pokryvailo coverage”, to the which is used in this document refers to a layer of the coating, which when applied to the surface is visible below the surface of the coating layer. In some embodiments of the present invention, the surface below the layer pokryvailo coating is visible, if newsrevue layer is applied at a dry film thickness of 0.5 to 5.0 mils (from 12.7 to 127 microns). One way of assessing the lack of shelter is the measurement of opacity. “Opacity”is used herein, refers to the extent to which the material hides the canvas.

“Interest opacity” refers herein to the relationship of the reflection coefficient of the dried film coating over a black base with 5% or less of the reflection coefficient, the reflection coefficient of the same film coating, equivalent applied and dried over Foundation with 85% reflectance. The percentage of opacity of the dried film of the coating will depend on the thickness of the dried film coating and concentration to give the color of the particles. In some embodiments of the present invention, the layer to give the color pokryvailo coverage is the percentage opacity of not more than 90 percent, and it is not more than 50 percent when the dry film thickness of one (1) mil (about 25 microns).

In some embodiments, the " the reflecting surfaces of the present invention, the layer of transparent coating is applied on top, at least part of a layer to give the color pokryvailo coverage. The layer of transparent coating may be applied from a composition that contains any usual film-forming resin and can be applied on top to give the color pokryvailo layer for added depth and/or protective properties of the surface beneath it. Resinous binders for transparent coatings can be embodied in the form of a composition for a powder coating composition for coating an organic solvent or composition for coating water-based. Optional ingredients suitable for inclusion in compositions of the transparent cover, include those known in the technology of formation of protective coatings, namely materials that previously described. Composition for transparent coatings can be applied on the basis of any of the usual methods of coating, such as brush application, spraying, dipping or pouring, among others.

In some embodiments of the coating made from the composition for powder coating of the present invention, are “brighter” color compared to the same composition for powder coating, which does not include a number decapsulating in polymer nanoparticles having a maximum turbidity of 10%, such as described above. In d is the query result the present invention relates to a method of increasing the brightness of the color coating, deposited from the composition for powder coating. These methods include the inclusion in the composition for powder coating a number decapsulating in polymer nanoparticles having a maximum turbidity of 10%. The term “brightness”as used herein refers to the value of Lin the system description color CIELAB, which is described in U.S. patent No. 5 792 559 in column 1, lines 34 to 64, the cited portion of which is incorporated herein by reference, where a lower value of Lcorresponds to a higher level of brightness of the color. For the purposes of the present invention can be carried out to measure the color at different angles using a spectrophotometer X-RITE, namely multiplepage spectrophotometer MA68I, commercially available from X-Rite Instruments, Inc.

The present invention relates also to a method of matching a color of the specified protective and decorative coating made from the composition for liquid coatings. The inventors have found that, in contrast to compositions for powder coatings of the prior art, the powder coating composition of the present invention is able to produce coatings that exhibit color properties similar to the coatings deposited from compositions for liquid coatings. In the composition for powder what about the coating of the present invention can be used to adjust color coatings caused from compositions for liquid coatings. These methods include: (a) the definition of the visible colors specified coatings by measurement of absorption or reflectance of a given coating; and (b) the composition for powder coating, including a certain number decapsulating in polymer nanoparticles having a maximum turbidity of 10%, where the coating of the composition for powder coating, corresponds to visible color of the specified coating. In these methods determine the absorption or reflection of a given coating using a spectrophotometer (described above) and receive a curve of absorption or reflection in the wavelength interval corresponding to the likely range. This curve applies to a visible spectrum absorption or reflection. Get a composition for powder coating, which contains a number of decapsulating in polymer nanoparticles having a maximum turbidity of 10%, such that the coating composition of the powder coating had an absorption or reflection in the visible spectrum, close to the corresponding parameters of the specified coating.

The invention is illustrated by the following examples, which should not be construed as limiting the invention to their details. All proportions and percentages in the examples and elsewhere in the description, are Mac is UNIX, if not stated otherwise.

EXAMPLES

EXAMPLE 1

Dispersion of polyurethane

This example describes how to obtain a polyurethane dispersion which was subsequently used for the formation of a dispersion of a polyurethane/nanopigments Examples 2-4. The polyurethane dispersion was obtained from the following mixture of ingredients in these ways:

IngredientsWeight (grams)
Download I
Poly (neopentylglycol adipate)1780,0
Dimethylolpropionic acid (DMPA)280,7
The triethylamine127,1
Bottled hydroxytrol2,5
Triphenylphosphite2,5
Boot II
Hydroxyethyl methacrylate (DUMB)of 116.7
Butyl methacrylate791,2
Download III
Methylene bis(4-cyclohexylidene)1175,1
Download IV
Butyl methacrylateof 57.5
Download V
Deionized water4734,8
The Ethylenediamine49,2
Dimethylethanolamine40,6
Download VI
Butyl methacrylate50
1Poly (neopentylglycol adipate)with srednekamennogo molecular weight of 1000.

The polyurethane dispersion was obtained in chetyrehkolkoy round bottom flask, equipped with an electronic temperature probe, mechanical stirrer, refrigerator and mantle. Download I stirred 5 minutes in the flask at a temperature of 90°C. was Added boot II and cooled the mixture to 60°C. over a 10 minute period was added loading III. Added boot IV and the resulting mixture was gradually heated to 90°C for 45 minutes and then kept at 90°C for 3 hours. Download V AC is stirred in a separate flask and heated to 80°C. To download V added 3000,0 g of the reaction product downloads I, II, III and IV within 30 minutes. Added loading VI and the resulting mixture was cooled to room temperature. The final product was a transparent emulsion with an acid value of 12.1, viscosity Brookfield 872 CP (spindle No. 3 at 30 rpm), pH 7.75, and the content of non-volatile part of 29.4%as measured at 110°C for one hour.

EXAMPLE 2

The dispersion of the polyurethane/nanopigments

This example describes how to obtain a dispersion of nanosized pigment blue phtalocyanines PB 15:3. The variance was received from the following mixture of ingredients in these ways:

IngredientsWeight (grams)
Download I
The polyurethane dispersion of Example 14772,7
Deionized water2304,5
Methyl ether of hydroquinone (MEHQ)1,36
Pigment PB 15:32700,0
Shellsol OMS (Shell Chemical Co.)86,4
Boot II
Deionized water71,5
tert-butyl hydroperoxide (70%aqueous solution)5,8
Download III
Deionized water337,2
Ferrous sulfate-ammonium0,13
Metabisulphite sodium8,18
2Commercially available from BASF Corp.

The ingredients were mixed using a 4.5-inch Cowles blade attached to the pneumatic motor. Then the pre-mixture was dispersively in the shredder Premier Mill PSM-11, containing 353 ml of 1.2-1.7 mm grinding environment Zirconox YTZ®, for 1.25 hours at 1000 ft/min (308 m/min) for stirring blades and the pump speed 960 rpm, and then repeated the operation in the crusher Advantis V15 Drais containing 500 ml of 0.3 mm means crushing Zirconox YTZ® in one litre of the crushing chamber. The mixture was ground at 1400 rpm with the setting of the pump 19 rpm for a total time of 15 hours. The process of grinding was controlled by visual observation of changes in the transparency of the samples of thin films, deposited on top of black and white Leneta paper. Added boot II and the resulting mixture was stirred for 5 minutes. Download III added two aliquot within 5 minutes, the final product was a blue (blue) liquid with viscosity Brookfield 356 CP (spindle No. 3 at 30 rpm), pH 7,29 and content of non-volatile part of 28.9%as measured at 110°C for one hour.

EXAMPLE 3

The dispersion of the polyurethane/nanopigments

This example describes how to obtain a dispersion of nanosized pigment chinagreen red PR 122. The variance was received from the following mixture of ingredients in these ways:

IngredientsWeight (grams)
Download I
The polyurethane dispersion Example 14772,7
Deionized water2304,5
Methyl ether of hydroquinone (MEHQ)1,36
Pigment PR 1223700,0
Shellsol OMS (Shell Chemical Co.)86,4
Boot II
Deionized water 71,5
tert-butyl hydroperoxide (70%aqueous solution)5,8
Download III
Deionized water337,2
Ferrous sulfate-ammonium0,13
Metabisulphite sodium8,18
3Commercially available from Sun Chemical

The ingredients were mixed using a 4.5-inch Cowles blade attached to the pneumatic motor. Then the pre-mixture was dispersively in the shredder Premier PSM-11, containing 353 ml of 1.2-1.7 mm grinding environment Zirconox YTZ® for 1.5 hours at 1000 ft/min (308 m/min) for stirring blades and the pump speed 960 rpm, and then repeated the operation in the crusher Advantis V15 Drais containing 500 ml of 0.3 mm means crushing Zirconox YTZ® in one litre of the crushing chamber. The mixture was ground at 1260 ft/min with the setting of the pump 19 rpm for a total time of 15 hours. The process of grinding was controlled by visual observation changes the transparency of the samples of thin films, deposited on top of the black and white Leneta paper. Added boot II and the resulting mixture was stirred for 5 minutes. what the recalls III added two aliquot within 5 minutes. The final product was a red liquid with a viscosity Brookfield 28.1 centipoise (spindle No. 3 at 30 rpm), pH factor to 7.61, and the content of non-volatile part of 28.2%as measured at 110°C for one hour.

EXAMPLE 4

The dispersion of the polyurethane/nanopigments

This example describes how to obtain a dispersion of nanoscale diazo pigment yellow PY 128. The variance was received from the following mixture of ingredients in these ways:

IngredientsWeight (grams)
Download I
The polyurethane dispersion of Example 14872,7
Deionized water2204,5
Methyl ether of hydroquinone (MEHQ)1,36
Pigment PY 1284700,0
Shellsol OMS (Shell Chemical Co.)86,4
Boot II
Deionized water71,5
tert-Butyl hydroperoxide (70%aqueous solution) 5,8
Download III
Deionized water337,2
Ferrous sulfate-ammonium0,13
Metabisulphite sodium8,18
4Commercially available from CIBA.

The ingredients were mixed using a 4.5-inch Cowles blade attached to the pneumatic motor. Then the pre-mixture was dispersively drum chipper Premier PSM-11, containing 353 ml of 1.2-1.7 mm grinding environment Zirconox YTZ® for the 4.7 hours at a speed of 1000 ft/min for stirring blades and 960 rpm for the pump, and then repeated the operation in the crusher Advantis V15 Drais containing 500 ml of 0.3 mm means crushing Zirconox YTZ® in one litre of the crushing chamber. The mixture was ground at 1400 ft/min (431,2 m/min) with the setting of the pump 19 rpm for a total time of 18 hours. The process of grinding was controlled by visual observation changes the transparency of the samples of thin films, deposited on top of the black and white Leneta paper. Added boot II and the resulting mixture was stirred for 5 minutes. Download III added two aliquot within 5 minutes. The final product was a yellow liquid with elm is awn on Brookfield 48.1 centipoise (spindle No. 3 at 30 rpm), pH 7,40 and content of non-volatile part of 29.4%as measured at 110°C for one hour.

EXAMPLE 5 Drum drying the dispersion nanopigments

This example describes the conversion of a liquid dispersion of a polyurethane/nanopigments Example 3 in the dried material, suitable for mechanical grinding into powder feedstock for subsequent use in the preparation of a composition for powder coating. The dispersion described above in Example 3 was dried in a double drum dryer Bufolvak 6”×8” with a clearance of 10 mils at the cylinder temperature of 240°F, rotating 2,9 rpm, the resulting material is formed openwork sheet which is easily broken in a large powder with a dry residue 96,0%as measured at 110°C for one hour.

EXAMPLE 6

Dispersion of polyurethane

This example describes how to obtain dispersions of polyurethane, which is subsequently used for the formation of the corresponding dispersions of polyurethane/nanopigments in Examples 7-9 and 13. The polyurethane dispersion was obtained from the following mixture of ingredients in these ways:

IngredientsWeight (grams)
Download I
Poly(butylenes)5 to 355.6
Dimethylolpropionic (DMPA)119,2
The triethylamine54,0
Bottled hydroxytrol2,2
Triphenylphosphite1,1
Boot II
Hydroxyethyl methacrylate (DUMB)27,8
Butylmethacrylate48,4
Butyl acrylatespreads for about 319.2
Download III
Methylenbis(4-cyclohexylidene)558,9
Download IV
Butylmethacrylate55,6
Download V
Deionized water2086,3
Diethanolamin20,2
The Ethylenediamine26,9
Dimethylethanolamine19,7
Download VI
Butylmethacrylate50,0
5Poly(butylenes)with srednekamennogo molecular weight of 1000.

The polyurethane dispersion was obtained in chetyrehkolkoy round bottom flask, equipped with an electronic temperature probe, mechanical stirrer, refrigerator and mantle. Download I stirred in the flask for 5 minutes at a temperature of 125°C. was Added boot II and cooled the mixture to 70°C. Load III was added over a 10 minute period. Added boot IV and the resulting mixture was gradually heated to 90°C for 90 min and then kept at 90°C for 1 hour. Download V were mixed in a separate flask and heated to 60°C. 1387,8 g of the reaction product downloads I, II, III and IV were added to the download V for 10 minutes. Added loading VI and cooled the mixture to room temperature. The final product was a transparent emulsion with an acid value of 12.5, viscosity Brookfield 3710 CP (spindle No. 5 at 60 rpm), a pH of 7.6 and a dry residue of 29.4%as measured at 110°C for one hour.

EXAMPLE 7

The dispersion of the polyurethane/nanopigments

This example describes recip is the dispersion of nanosized pigment blue phtalocyanines PB 15:3. The variance was received from the following mixture of ingredients in these ways:

IngredientsWeight (grams)
Download I
The polyurethane dispersion of Example 67271,0
Deionized water3293,1
Methyl ether of hydroquinone (MEHQ)2,0
Pigment PB 15:31079,5
Shellsol OMS (Shell Chemical Co.)131, 5mm
Boot II
Deionized water102,4
Tert-Butyl hydroperoxide (70%aqueous solution)12,3
Download III
Deionized water512,1
Ferrous sulfate-ammonium0,15
Metabisulphite sodium12,3

The ingredients were stirred for 2.5 hours using a Ross mixer Model No. HSM-100L-type rotor/stator and then re-processed in the crusher Advantis V15 Drais containing 500 ml of 0.3 mm means crushing Zirconox YTZ® in one litre of the crushing chamber. The mixture was ground at 1400 rpm (431,2 m/min) during the total time 19,0 hours. The process of grinding was controlled by visual observation changes the transparency of the samples of thin films, deposited on top of the black and white Leneta paper. Added boot II and the resulting mixture was stirred 5 minutes at 11°C. the Loading III added two aliquot within 5 minutes. The temperature of the mixture increased to 13°C. the Final product was a blue liquid with a viscosity Brookfield 26 centipoise (spindle No. 1 at 60 rpm), pH 7.2 and content of non-volatile part of 30.0%as measured at 110°C for one hour.

EXAMPLE 8

The dispersion of the polyurethane/nanopigments

This example describes how to obtain a dispersion of nanosized pigment chinagreen red PR 122. The variance was received from the following mixture of ingredients in these ways:

IngredientsWeight (grams)
Download I
The polyurethane dispersion of Example 6 7271,0
Deionized water3293,1
Methyl ether of hydroquinone (MEHQ)2,0
Pigment PR 1221079,5
Shellsol OMS (Shell Chemical Co.)131, 5mm
Boot II
Deionized water102,4
tert-Butyl hydroperoxide (70%aqueous solution)12,3
Download III
Deionized water512,1
Ferrous sulfate-ammonium0,15
Metabisulphite sodium12,3

The ingredients were stirred for 2.5 hours using a Ross mixer Model No. HSM-100L-type rotor/stator and then re-processed in the crusher Advantis V15 Drais containing 500 ml of 0.3 mm means crushing Zirconox YTZ® in one litre of the crushing chamber. The mixture was ground at 1400 rpm/min for a total time of 23 hours. The progress of the grinding control the visual observation changes the transparency of the samples of thin films, applied on top of the black and white Leneta paper. Added boot II, and the resulting mixture was stirred 5 minutes at 24°C. the Loading III added two aliquot within 5 minutes. The temperature of the mixture raised to 26°C. the Final product was a red liquid with a viscosity Brookfield 27 centipoise (spindle No. 1 at 60 rpm), pH 7.4 and content of non-volatile part of 29.3%as measured at 110°C for one hour.

EXAMPLE 9

The dispersion of the polyurethane/nanopigments

This example describes how to obtain a dispersion of nanoscale diazo pigment yellow PY 128. The variance was received from the following mixture of ingredients in these ways:

IngredientsWeight (grams)
Download I
The polyurethane dispersion of Example 67271,0
Deionized water3293,1
Methyl ether of hydroquinone (MEHQ)2,0
Pigment PY 1281079,5
Shellsol OMS (Shell Chemical Co.)131, 5mm
Boot II
Deionized water102,4
tert-Butyl hydroperoxide (70%aqueous solution)12,3
Download III
Deionized water512,1
Ferrous sulfate-ammonium0,15
Metabisulphite sodium12,3

The ingredients were stirred for 5.5 hours using a Ross mixer Model No. HSM-100L-type rotor/stator and then re-processed in the crusher Advantis V15 Drais containing 500 ml of 0.3 mm means crushing Zirconox YTZ® in one litre of the crushing chamber. The mixture was ground at 1400 rpm (431,2 m/min) within a total time of 23 hours. The process of grinding was controlled by visual observation changes the transparency of the samples of thin films, deposited on top of the black and white Leneta paper. Added boot II, and the resulting mixture was stirred 5 minutes at 24°C. the Loading III added two aliquot within 5 minutes. The final product was a yellow liquid with a viscosity Brookfield 53 centipoise (spindle No. 1 at 60 rpm), pH 7.3 and content of non-volatile part of 28.8%as measured at 110°C for one h is sa.

EXAMPLE 10

Getting intermediate composition for powder coating

This example describes the preparation of formulations of the core dry materials used to obtain the composition for powder coating of the subsequent Examples. The formulation of the core was obtained from the following ingredients in the indicated relations:

Components 1-9 pre-mixed in a Henschel mixer for 1 min at 1000 rpm the mixture is Then squeezed through a twin screw extruder Coperion W&P 30 mm with rotation in one direction when the rotation speed of the screw 340 rpm and average torque of 30-40%. The extruder was equipped with a system input at low pressure and five zones of independently controlled temperature, as described in published patent applications U.S. 2005/0213423; 2005/0212159 A1 and 2005/0212171 A1. Five zones of independently controlled temperature was maintained at the following temperatures: Zone 1: 60°C; Zone 2: 120°C; Zone 3: 130°C; Zone 4: 120°C; Zone 5: 100°C. the Extrudate was cooled and crushed in a mechanical system grinding to a particle size of from about 28 to 30 microns. Particles of excessive size've removed and added the component 10.

EXAMPLE 11

Obtaining coating compositions of the powder material

Received various compositions for powder coating of the intermediate comp is the exposure to the powder coating of Example 10 and the dispersion of the polyurethane/nanopigments Examples 2-4 and 7-9, as well as various mixtures of these dispersions (mass ratio ranging from 90:10 to 10:90). Each of the compositions for powder coating was obtained under the conditions described in Example 10, using a twin-screw extruder Coperion W&P 30 mm with rotation in one direction, air entering at low pressure, and the five zones with independent temperature control, as described in published patent applications U.S. 2005/0213423; 2005/0212159 A1 and 2005/0212171 A1. Intermediate composition for powder coating of Example 10 was fed to the extruder at a speed of 280 grams per minute, and the dispersion of pigments was fed to the extruder at a speed of 105 grams per minute through a system of injection at low pressure. Zone 4 was equipped with a hole for removing volatile vapors. The extrudate was cooled and milled in the system mechanical grinding to a particle size of from about 28 to 30 microns.

EXAMPLE 12

A method of matching a color

This Example proves superior ability of compositions for powder coating of the present invention to match the color of the colored coating composition of the liquid coating. In this example, the standard color was purple/red coating of the composition for liquid coatings. Color indices that measured multiplay spectrophotometer MA6I at different angles, presented in the Table. Powder coating And showed the best match of color that could be achieved by using the composition for powder coating, with only the standard pigments. Powder coating is In the best match of color that could be achieved by using the composition for powder coating, which includes a combination of dispersions of nanopigments Examples 2-4 and 7-9.

Powder coating And
AngleLandbh
159,2-14,68,53-15,66,53
256,27-7,94of 5.68-8,464,86
458,195,165,715,35of 5.53
75 there is a 10.0317,53of 6.73MT 18 : 344,05
11010,69227,2422,972,95

-4,86
Powder coating B
AngleLandbh
15-9,58-9,21-1,6-8,57-3,72
25-5,59-5,98-3,27-5,13-4,49
450,250,09-5,751,06-5,56
751,755,86-5,54to 6.43
1101,846,02-4,266,32-3,8

In this Example, a positive trend values, showing, thus, the best matching color standard with face angles (15 and 25). When measuring the flop angles (45, 75, 110) negative trend indicates darker and more desirable color shifts. In the case of the above sample values for all three angles were decreased relative to the initial powder to the object, approaching, thus to the standard.

EXAMPLE 13

The dispersion of the polyurethane/nanopigments

This example describes how to obtain a dispersion of nanosized pigment perylenebis red PR-179. The variance was received from the following mixture of ingredients in these ways:

IngredientsWeight (grams)
The polyurethane dispersion of Example 66272,3
Deionized water4545,6
Pigment PR 179141818,2
Shellsol OMS (Shell ChemicalCo.) 218,2
14Commercially available from Sun Chemical

The ingredients were mixed and re-processed through the crusher Advantis V15 Drais containing 500 ml of 0.3 mm means crushing Zirconox YTZ® in one litre of the crushing chamber. The mixture was ground at the maximum value of 1350 rpm for a total time 42,75 hours. The final product was a red liquid that contains non-volatile part of 39.4 percent, as measured at 110°C for one hour.

EXAMPLE 14

In this Example, two compositions of powder coatings have been produced using the ingredients and the method described in Example 10. In Example 14a 3 mass parts of pigment PR 179, commercially available from Sun Chemical, were included in the composition of Example 10. In Example 14b 3 mass parts of a dispersion of a polyurethane/nanopigments were included in the composition of Example 10. The powder coating composition of Examples 14a and 14b was applied electrostatically to a 4"×12" panel with elecrodeposition coating. The panel was utverjdali at a suitable elevated temperature and cooled to ambient temperature. The performance of the paint was measured on multigluon spectrophotometer MA68I at different angles. The results are shown in the Table and are presented as the difference between the values of Example 14b compared to Primerose.

AngleLandbh
15-1,76-3,2-2,64-4,08-0,77
25-3-5,02-4,05-6,33-1,21
45-4,05-8,41-5,9-10,2-1,23
75to-4.5-10,17-6,52-12,06-0,65
110-4,59-10,85-6,68-12,74-0,18

In this Example, reducing the value of "L" testified to increase the brightness and the degree of color development.

Experts will understand that embodiments of, op the sled above, can be made without deviating from the General idea of the invention. Therefore understood that this invention is not limited to the specific disclosed variants of implementation, but it is intended to cover modifications that are within the essence and scope of the invention defined by the attached claims.

1. Composition for powder coatings derived from aqueous dispersions comprising zakopalova in the polymer particles, in which zakopalova in the polymer particles include particles, zakopalova in a brittle polymer, which is easily crushed when environmental conditions.

2. Composition for powder coating according to claim 1, in which the particles comprise nanoparticles.

3. Composition for powder coating according to claim 2, in which the nanoparticles comprise inorganic nanoparticles.

4. Composition for powder coating according to claim 3, in which the nanoparticles comprise inorganic nanoparticles selected from colloidal silica, fine silica, amorphous silica, alumina, colloidal alumina, titanium dioxide, iron oxide, cesium oxide, yttrium oxide, colloidal yttria, colloidal Zirconia, amorphous Zirconia, and mixtures thereof.

5. Composition for powder coating according to claim 3, in which the Oh of inorganic nanoparticles include a mixed metal oxide.

6. Composition for powder coating according to claim 2, in which the nanoparticles have a maximum turbidity of 10%.

7. Composition for powder coating according to claim 2, in which the nanoparticles comprise organic nanoparticles.

8. Composition for powder coating according to claim 7, in which the organic nanoparticles include organic pigments selected from perylenes, kinokritikov, phthalocyanines, isoindolines, dioxazines (namely, tribendimidine), 1,4-declareroles, entrepremedia, anthanthrene, flavanonol, indanthrene, perinone, paratroop, thioindigo, 4,4'-diamino-1,1'-diantaranya, azo compounds, their substituted derivatives and mixtures thereof.

9. A method of obtaining a water dispersion of particles, decapsulating in a brittle polymer that includes treatment of the water environment in terms of grinding, where the aqueous medium contains a mixture containing:
a) particles
b) an ethylene-unsaturated monomer and
C) dispersible in water ethylene-unsaturated polymer
this zakopalova in the polymer particles are formed by grinding at least part of the ethylene-unsaturated monomer with dispersible in water ethylene-unsaturated polymer under the conditions of grinding and brittle polymer is a polymer which is easily crushed when environmental conditions.

10. The method according to claim 9, in which dispersible in water and ethylene-n is a saturated polymer includes a polyester polyurethane, having terminal ethylene unsaturation.

11. The method according to claim 10, in which dispersible in water ethylene-unsaturated polymer having terminal ethylene unsaturation, derived from reactants containing: (a) a polyisocyanate; (b) a polyester polyol; and (C) a material containing ethylene unsaturated group and an active hydrogen group.

12. The method according to claim 11, in which dispersible in water ethylene-unsaturated polymer having terminal ethylene unsaturation, derived from reactants containing optional: (d) a polyamine; and (d) a material containing an acid functional group or anhydride and a functional group reactive towards isocyanate or hydroxyl groups.

13. The method according to claim 9, in which dispersible in water ethylene-unsaturated polymer has srednevekovoy molecular weight 40000-80000 grams per mole.

14. The basis of at least partially covered with a coating of the composition for powder coating according to claim 1.

15. Based on 14 in which the base includes a metal base.

16. Multilayer complex coating in which at least one layer of coating made from the composition for powder coating according to claim 1.

17. A method of obtaining a composition for powder coating, comprising: (1) introduction into the extruder components, comprising: (a) water dispers the Yu, containing zakopalova in the polymer particles, in which zakopalova in the polymer particles include particles, zakopalova in a brittle polymer, which is easily crushed when environmental conditions, and (b) dry materials; (2) mixing components (a) and (b) in the extruder; (3) removing volatile components from the mixture to form an extrudate; (4) cooling the extrudate, and (5) grinding the extrudate to the desired particle size.

18. A method of obtaining a water dispersion decapsulating in the polymer particles, comprising: (1) receiving in an aqueous medium a mixture of: (a) particles, (b) ethylene-unsaturated monomer and (C) dispersible in water polymerizable dispersant products containing dispersible in water ethylene-unsaturated polymer, and (2) the polymerization of the ethylene-unsaturated monomer and polymerizable dispersant education decapsulating in the polymer particles containing dispersible in water the polymer, where the method does not include the stage of exposure to the mixture of high shearing forces, and the polymer is brittle polymer, which is easily crushed under the conditions of the environment.

19. The method according to p, in which, after stage (1) particles are formed in the nanoparticles.

20. The method according to p, which is dispersible in water ethylene-unsaturated polymer has srednevekovoy molekularnu the mass 40000-80000 grams per mole.

21. Composition for powder coatings formed from the aqueous dispersion obtained by the method according to p.

22. The reflective surface at least partially covered by a layer which imparts color pokryvailo coating of the composition for powder coating according to claims 1 or 21, including many decapsulating in polymer nanoparticles having a maximum turbidity of 10%.



 

Same patents:

FIELD: chemistry.

SUBSTANCE: costing is obtained from a composition containing a film-forming resin and a plurality of particles dispersed in the resin. The average size of the particles ranges from 0.1 to 50 mcm. The particles have hardness which is sufficient to endow the coating with high resistance to dents and/or scratches compared to a coating in which such particles are not present. Also, the difference between the refraction index of the resin and the refraction coefficient of the particles ranges from 1 to 1.5. The invention also describes a method of preparing a powdered coating which includes particles dispersed in the resin and a coated substrate.

EFFECT: after hardening, the coatings have high resistance to dents and scratches, high resistance to breaking caused by mechanical impacts, as a result of mechanical or chemical wear.

19 cl, 9 ex, 2 tbl

FIELD: chemistry.

SUBSTANCE: disclosed is a dry paint composition in form of particles which contains at least two pigments, at least one ionic or nonionic dispersing agent and filler pigment. Each of the pigments is prepared in form of a separate aqueous pre-dispersion. At least two aqueous pre-dispersions are mixed together in the presence of the dispersing agent to form a tinting dispersion which, after drying, forms a dry paint composition in form of particles.

EFFECT: disclosed dry paint composition has colour tone which foreshows the colour of the tint coating composition and the applied coating.

5 cl, 6 tbl

FIELD: chemistry.

SUBSTANCE: composition contains components (A) and (B); component (A) contains 5-95 wt % base of powdered coating (A) from one or more polyester resins with saturated carboxyl functionality, acid number from 5 to 25 KOH/g, a hardener consisting of triglycidyltrimellitate (TML), diglycidylterephthalate (DGT) and glycidyl ethers based on aliphatic or cycloaliphatic epoxy resins and, optionally, a coating additive and, optionally, pigments and/or filling materials. The composition contains a component (B) containing 95-5 wt % powdered coating base from one or more polyester resins with saturated carboxyl functionality, acid number from more than 25 to 100 KOH/g, a hardener - triglycidyltrimellitate (TML), diglycidylterephthalate (DGT) and glycidyl ethers based on aliphatic or cycloaliphatic epoxy resins and, optionally, a coating additive pigments and/or filling materials. Described also is a method of preparing the powdered coating composition.

EFFECT: invention enables to obtain a coating with high flexibility, good stability and desired level of lustre.

14 cl, 2 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: method of producing modified inorganic oxygen-containing granular material involves the following steps: a) preparing a mixture of an aqueous suspension of inorganic oxygen-containing granular material and alkoxylated alcohol of formula where R1 is C1-C8-alkyl or phenyl, C4-C8-cycloalkyl or phenyl, R2 is a hydrogen atom or methyl, and n is an integer from 1 to 5; b) optional addition of a first resin and/or precursor of the first resin; c) adding a mixture of one or more cross-linking agents containing one or more elements selected from a group comprising Si, Al, Ti, Zr, B, Zn, Sn and V; d) optional addition of a second resin and/or precursor of the second resin to the obtained mixture. Water is optionally removed from the mixture at least partially before or during step b), c) or d) or after step d). Also, the precursor of the first resin can be converted to the first resin before, during or after step c) and/or the precursor of the second resin can be converted to the second resin after step d).

EFFECT: invention increases environmental safety and simplifies production of modified inorganic oxygen-containing granular material which is well compatible with resins.

11 cl, 4 tbl, 37 ex

FIELD: chemistry.

SUBSTANCE: invention relates to production of fine-grained polyarylene ether ketone used for application on metallic and ceramic articles and producing composite materials. Fine-grained polyarylene ether ketone is obtained by grinding porous polyarylene ether ketone whose BET surface is greater than 4 m2/g. The porous polyarylene ether ketone is obtained during spontaneous setting of polyarylene ether ketone solution in high boiling point organic solvent, for example diphenyl sulphone.

EFFECT: method lowers the cost of grinding and increases output of the powder.

7 cl, 3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to the paint industry, particularly to aqueous dispersions based on vinylidene fluoride for obtaining protective paints. The vinylidene fluoride-based aqueous dispersions contain polymer particles with average size of 0.260-0.3 micrometres, obtained via polymerisation of vinylidene fluoride-based emulsions, optionally in the presence of one or more fluorinated copolymers, in the presence of a bifunctional surfactant of formula: A - Rf - B (I), where: A = -O-CFX-COOM; B = -CFX-COOM; X = F, CF3; M=NH4 alkali metal, H; Rf denotes a straight or branched perfluorinated chain; or a (per)fluoropolyester chain.The average molecular weight (I) is in the range 650-800. Described also is use of vinylidene fluoride-based aqueous dispersions to produce water-based protective paints and protective paint for metal bases, obtained using vinylidene fluoride-based aqueous dispersions; use of aqueous dispersions of polymers based on vinylidene fluoride to obtain powder used in preparing protective paints for powder coatings.

EFFECT: coatings obtained using paints which contain vinylidene fluoride-based aqueous dispersions have good physical and mechanical properties.

17 cl, 5 tbl, 11 ex, 8 dwg

FIELD: chemistry.

SUBSTANCE: composition contains a homogeneous mixture consisting of at least one bromine-functionalised epoxy resin, at least one epoxy curing agent and at least one pigment, filler and/or coating additive. Content of bromine in the bromine-functionalised epoxy resin is equal to 5-60%. The composition also contains alkanol amine and at least one zinc borate compound. Alkanol amine is selected from a group consisting of diethanol amine and tris(hydroxymethyl)aminomethane. The method of preparing the composition involves mixing components, heating to melting point of the mixture, extrusion of the molten mixture, cooling, crushing and grinding to powder. The composition provides a coating with high glass transition temperature and acceptable flexibility when depositing the coating onto a metallic or plastic base, in particular metallic and plastic pipes.

EFFECT: coatings can have high adhesion in hot and humid conditions and optimum short-term and long-term protection from cathodic disbonding at high temperature and humidity.

14 cl, 3 tbl, 7 ex

FIELD: chemistry.

SUBSTANCE: powdered UV-curable composition contains 89.5-96.5 pts. wt oligoether(meth)acrylate, 1.0-2.7 pts. wt benzoyl-type photoinitiator, 1.0-1.5 pts. wt flow agent, 0.5-0.7 pts. wt degassing agent and a fluorine-containing modifying additive in form of a solid unsaturated compound with molecular weight of 850-2700 g/mol, obtained through synthesis from p-hydroxyethoxystyrene, diisocyanate in form of 1,6-hexamethylenediisocyanate or isophorone diisocyanate, and perfluorinated oligoester alcohol or oligoester diol with molecular weight of 500-2000 g/mol in amount of 1.0-5.6 pts. wt.

EFFECT: good physical and mechanical properties and obtaining coatings having high wear resistance, low dirt holding, good decorative and protective properties.

2 tbl, 16 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to a coating compositions. The coating composition contains a thermally crosslinking film-forming resin binder or resin binders, a polymer or copolymer levelling agent having molecular weight between 1000 and 100000 g/mol (Da). The polymer or copolymer levelling agent is obtained through polymerisation in the presence of an alkoxyamine initiator/regulating compound or monomer. The monomer is selected from a group of acrylate or methacrylate compounds. The said copolymer levelling agent is obtained from a composition which contains an ethylene-unsaturated monomer. The polymer levelling agent used is poly-tert-butyl acrylate or poly-tert-butyl methacrylate. The coating is obtained by depositing the composition onto a substrate and applying heat energy or electromagnetic radiation.

EFFECT: use of the said polymer or copolymer as a levelling agent in coating compositions enables to obtain smooth coating for surfaces.

3 cl, 21 ex, 10 tbl

FIELD: chemistry.

SUBSTANCE: invention refers to versions of solidificated powder coating composition and to method of cathodic protection of steel substrate. According to the first version, the composition contains as follows: (a) thermosetting resin, (b) zinc borate compounds in amount 0.5 to 4.75 wt % in relation to total solid weight, (c) curing agent for the specified structure, in amount effective for coating solidification, (d) filler, pigment and additive. Thermosetting resin is epoxy with functional groups of A/epichlorhydrin bicphenol. Curing agent is accelerated dicyandiamide or phenolic curing agent. According to the second version, the composition contains thermosetting epoxy, curing agent specified above, and zinc borate compound in amount 0.5 to 4.75 wt % in relation to total solid weight. Method of cathodic protection consists that steel substrate is machined and covered with the composition of the first version. It is followed with polarisation of steel substrate covered as cathode.

EFFECT: higher long-time cathodic disbandment resistance with high temperature and humidity application.

14 cl, 3 tbl, 6 ex, 1 dwg

FIELD: chemistry.

SUBSTANCE: disclosed is a colourless luminescent decorative paint containing a luminophor and binder. The luminophor is an organic luminophor with anomalously large Stokes shift which is greater than 100 nm, which is colourless in daylight and luminescent in the visible spectral region when illuminated with a source of UV radiation. The organic binder is a transparent organic substance which does not absorb long-wave ultraviolet radiation in the 365-420 nm range.

EFFECT: obtaining fast and stable luminescent paint which contains a colourless organic luminophor, which enables to create a latent image which appears upon illumination with UV radiation which is invisible in daylight as well as in the dark, in the absence of UV radiation, the paint ensures high strength of the polymer base of the decorative layer of the article obtained using said paint.

13 cl, 8 ex

FIELD: construction.

SUBSTANCE: anti-corrosion protective coating consists of the first element - a single-component moisture-hardened isocyanate primer, which contains at least 75 wt % of a nonvolatile residue and 6…8 wt % of isocyanate groups. The second element is a thick-layer external coating, to produce which a double-component polyurea-urethane mastic is used, containing an isocyanate prepolymer on the basis of diphenyl methane diisocyanate with mass portion of NCO-groups making 15…17% and dynamic viscosity at the temperature of (20±3)°C - 3…10 Pa·s, and the component it hardens with active atoms of hydrogen with hydroxyl number making 95…105 mgKOH/g, mass portion of total titrated nitrogen of 4.2…4.5%, containing a mixture of simple or complex polyester diol with molecular weight of 800…1000 c.u., sterically hindered diamine with amine number of 12…16.7%, oxypropylated ethylene diamine with hydroxyl number of 640…800 mgKOH/g and liposoluble organic pigments, at the ratio of isocyanate prepolymer to a component with active atoms of hydrogen, which ensures hardening of a thick-layer external coating until the required level of operational characteristics is produced.

EFFECT: coating ensures high level of adhesion, resistance to cathode lamination with preservation of the main physical-mechanical indices and ecological safety in process of insulation works.

3 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to compositions based on silane-functional polymers, which are suitable for adhesive binding, sealing and coating porous substrates. The composition contains at least one silane-functional polymer, at least one organosilane and at least one organotitanate. The silane-functional polymer is a silane-functional polyurethane polymer or can be obtained through hydrosilylation of polymers, having terminal double bonds. The organosilane contains at least one sulphur atom. The organotitanate has ligands bound to a titanium atom through an oxygen-titanium bond. The ligands are selected from a group consisting of an alkoxy group, a sulphate group, a carboxylate group, a dialkylphosphate group and an acetylacetonate group. Content of the organotitanate in the composition is between 0.1 and 10 wt %. Content of the organosilane in the composition is between 0.1 and 7 wt %. The composition also contains at least one filler, content of which is between 10 and 70 wt %. The composition is used for binding, sealing and coating substrates made from concrete, mortar, brick, tiles, plaster, natural stone such as granite or marble, glass, glass-ceramic, metal or metal alloy, wood, plastic and lacquer.

EFFECT: obtained article, which is bound, sealed or coated using the composition, is a building structure, more specifically a building or civil construction structure; the composition guarantees efficient adhesion to a substrate even after storage in the presence of water.

17 cl, 1 tbl

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of preparing an aqueous agent for applying coating, as well as an aqueous agent obtained using said method, and use thereof as binder in single-component (1K)-systems and a two-component (2K)-system, and for obtaining a coating on soaking substrates. The method involves the following: (I) polyurethane dispersion which is free from solvent and N-methylpyrrolidone is prepared, where the solvent free dispersion is a dispersion containing 0.9 wt % or less solvent, and the polyurethane dispersion (I) is simultaneously or separately mixed with (II) 1-7 wt % monohydroxyl-functional ethylene- or propyleneglycol ester, as well as (III) other lacquer additives. Wherein I.1) at the first step a NCO-prepolymer solution is obtained in a solvent with concentration of 66-98 wt %, where the solvent has boiling point lower than 100°C at nominal pressure, by reacting: (a) one or more polyisocyanates, (b) one or more polyols with average molecular weight Mn 500-6000, (c) one or more polyols with average molecular weight Mn 62-500, (d) one or more compounds containing a ion group or capable of forming an ion group and the NCO-prepolymer is free from a non-ionic hydrophilisising agent; I.2) at the second step the NCO-prepolymer I.1) is dispersed in water, where before, during or after dispersion, ion groups are at least partially neutralised; I.3) at the third step the chain is elongated by (e) one or more polyamines with average molecular weight Mn less than 500; and l.4) at the fourth step, the solvent is completely removed by distillation.

EFFECT: obtaining an aqueous agent for applying a coating, having improved film-forming properties, as well as obtaining coatings therefrom, having good chemical resistance and pendulum hardness higher than 75 seconds.

13 cl, 5 ex, 4 tbl

FIELD: chemistry.

SUBSTANCE: present invention relates to a polyurethane dispersing resin, primarily having a polyurethane chain which contains hydrophilic groups of the side chain based on polyalkylene oxide, where groups of the side chain are covalently bonded to the polyurethane backbone chain, and where content of polyalkylene oxide in the polyurethane dispersing resin is at least 45 wt % and not more than 80 wt %. Polyurethane also contains hydrophobic groups on the side chain, which are covalently bonded to the polyurethane backbone chain. The invention also describes a coating composition containing said polyurethane dispersing resin, methods of preparing said composition and use of the polyurethane dispersing resin to prepare a composition for mixing with a pigment.

EFFECT: providing a polyurethane dispersing resin which enables to prepare concentrates of pigments, which can be easily included in a coating composition, in which pigments are stably dispersed, as well as possibility of obtaining pigment compositions with a wide range of pigments and obtaining dyes having excellent properties and stability, especially hard-to-disperse and stabilised pigments.

24 cl, 16 ex, 4 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to a coating composition containing a) polyacrylate polyol obtained via polymerisation of unsaturated olefin monomers, where at least 40 wt % of the monomers include straight or branched alk(en)yl or alk(en)ylene groups, having at least 4 carbon atoms; b) polyether polyol obtained via esterification of component links having functional groups which form an ester, where at least 30 wt % of component links include straight or branched alk(en)yl or alk(en)ylene groups with at least 4 carbon atoms per functional group, which forms an ester, where he polyether polyol has hydroxyl number higher than 280 mg KOH/g and hydroxyl functionality of at least 2, and c) isocyanate-functionalised cross-linking agent. The invention also relates to a set of parts for preparing the coating composition and a method of applying the coating composition. The coating composition can be used as a top coating layer in multilayer paint coats, in finishing or reworking automobiles or large vehicles.

EFFECT: coating has high hardness, scratch resistance, lustre, longevity and wear resistance, chemical resistance and UV radiation resistance.

15 cl, 6 tbl

FIELD: chemistry.

SUBSTANCE: composition includes a polymer mixture which contains a) an aqueous dispersion of at least one polysiloxane and b) an aqueous dispersion of at least one polyurethane, in which content of the said at least one polysiloxane polymer varies from approximately 50 to 85 wt %, and content of the said at least one polyurethane varies from approximately 15 to 50 wt %, in terms of total weight of solid substances of the said at least one polysiloxane polymer and the said at least one polyurethane and c) polyolefin powder with ultrahigh molecular weight in amount of approximately 5-35 pts. wt per 100 total parts by weight of the said at least one or more polysiloxanes and the said one or more polyurethanes. The said polyurethane is obtained from at least one aliphatic or cycloaliphatic diisocyanate and at least one hydroxyl ending intermediate compound such as polycarbonate, polyester or polyether or combination thereof, and is heat-curable. The said aqueous dispersion contains approximately 7 wt % or less of an organic solvent in terms of total weight of the said dispersion composition, and the said polymer mixture contains from approximately less than 10 to 0 parts by weight of a substance for increasing adhesiveness per 100 total parts by weight of the said at least one polyurethane and the said at least one polysiloxane; and contains from approximately less than 10 to 0 parts by weight of a halogen-containing polymer per 100 total parts by weight of the said at least one polyurethane and the said at least one polysiloxane. The invention also describes versions of a polymer or rubber substrate and versions of a sealant for vehicles, at least partially coated with the dried composition described above.

EFFECT: low noise level when substrate coated with the said composition moves or is in contact with an article, as well as obtaining a surface with low coefficient of friction which does not increase with time.

17 cl, 14 ex, 10 tbl, 1 dwg

FIELD: chemistry.

SUBSTANCE: polyurethane material contains a first part of crystalline particles, having self-orientation and bonded so as to keep their orientation along a first crystallographic line at least in two directions, a second part of crystalline particles having self-orientation and bonded so as to keep their orientation along a second crystallographic line at least in two directions, wherein the first crystallographic line is different from the second crystallographic line and where the said crystalline particles constitute more than approximately 30% of the total volume of the polyurethane material, and where the polyurethane contains a product of reaction of components comprising: (a) approximately 1 equivalent of 4,4'-methylene-bis(cyclohexylisocyanate); (b) approximately 0.3 of a trimethylolpropane equivalent; and (c) approximately 0.7 of a butanediol or pentanediol equivalent, and where the polyurethane material undergoes thermal treatment at temperature ranging from approximately 35°C to approximately 150°C or holding.

EFFECT: production of polyurethane material, products of which are made through casting or reaction injection moulding and have good optical properties, high resistance to impact loads, high impact resistance, high K-ratio, good ballistic stability, good resistance to solvents and good weather resistance.

26 cl, 110 ex, 33 tbl, 26 dwg

FIELD: chemistry.

SUBSTANCE: disclosed is an aqueous polyurethane dispersion which does not contain N-methylpyrrolidone and solvents and contains a product of reaction of a mixture of 1-isocyanate-3,3,5-trimethyl-5-isocyanatemethylcyclohexane and 4,4'-diisocyanatedicyclohexylmethane, one or more polyols with average molecular weight of 500-3000, one or more compounds with at least one OH- or NH- functional group, which contain a carboxyl and/or carboxylate group, where at least 50 mol % acid incorporated in the overall resin consists of dimethylol propionic acid, one or more polyols and/or polyamines with average molecular weight less than 500 and, if necessary, one or more monoalcohols and/or monoamines, as well as preparation method thereof and use thereof as an agent for coatings having good resistance characteristics.

EFFECT: obtaining a polyurethane dispersion which does not contain N-methylpyrrolidone and solvents, and contains a hydrophilization agent in form of dimethylol propionic acid, which can be stored for over 8 weeks and is suitable for making transparent shining coatings with high resistance to dyes.

8 cl, 2 tbl, 8 ex

FIELD: chemistry.

SUBSTANCE: invention relates to aqueous coating compositions with low content of volatile organic compounds. The aqueous coating composition contains water, oxidative-curable resin, at least 1.5% of the weight of the composition of a non-structured alkali-soluble acrylate, having weight-average molecular weight Mw of 200000 g/mol or lower, and acid number of at least 15 mg KOH/g; and an emulsified second acrylate having Mw of at least 300000 g/mol. Content of the alkali-soluble acrylate in the composition is equal to at least 3 wt %. The weight ratio of the alkali-soluble acrylate to the second emulsified acrylate ranges from 1:0.5 to 1:5, and the weight ratio of the alkali-soluble acrylate to the oxidative-curable resin ranges from 1:0.5 to 1:10. The oxidative curable resin is an alkyd resin, alkyd-urethane resin. The second acrylate is cross-linkable, for example azomethine cross-linkable links.

EFFECT: aqueous coating composition has good physical and mechanical properties.

9 cl, 3 ex

FIELD: chemistry.

SUBSTANCE: described is a method of producing an olefin oligomer obtained via trimerisation of an olefin monomer with 2-6 carbon atoms using a trimerisation catalyst system. The catalyst system is prepared by mixing a chromium source, a nitrogen-containing ligand and alkyl aluminium. The alkyl aluminium is exposed to microwaves with frequency 0.3-20 GHz for 0.5-20 minutes.

EFFECT: high efficiency of trimerisation reaction at low pressure of olefin monomer.

8 cl, 3 ex

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