Powdery covers with reduced luster with using free radicals

FIELD: powder covers.

SUBSTANCE: invention relates to a powder cover composition and to a method for its preparing that forms cover with reduced luster after hardening. Composition comprises one or some cross-linked basic polymers: cross-linked polyester, cross-linked polyurethane, cross-linked acrylated polyether and their combinations, about from 5 to 60 wt.-%; cross-linked acrylic polymer with solidification point about from 40°C to 100°C, and about 0.1 to 10 wt.-% of one or some free-radical initiating agents. Additional reducing luster and improved smoothness can be obtained by addition spheroidal particles to the powder cover composition. Proposed compositions can be used for making covers on metallic backings, such as vehicle bodies and on nonmetallic backings, such as backings made of pressed wood materials with impregnation used for making table tops of different species.

EFFECT: improved and valuable properties of covers.

21 cl, 4 tbl

 

The technical field to which the invention relates.

The present invention is directed to compositions for powder coatings and, more specifically, is directed to a class of powder coating compositions which, when cured, result in coatings with low luster, preferably having a smooth finish.

Prior art

Powder coatings are widely used to create decorative and/or protective coatings on substrates. They are becoming increasingly popular, because they are applied in the solid state or in suspension. Unlike conventional liquid compositions for coatings, for the composition of powder coatings do not use solvents or use them in small quantities. In addition, application of solid state makes possible the collection, treatment and reuse of powder.

UV-curable powders used in powder coating compositions. Typically, UV-curable powders are prepared from a solid cross stitched main resins with low Tg, such as cross stitched polyester resins; cross stitched copolymerizing resin with cross stitching groups, such as simple vinyl ethers; photoinitiators; agents for imparting fluidity and leveling agents; and, if necessary, pigments and fill the oil.

During the operations of coating, UV-curable powders are applied to the substrate in the usual way, using technologies such as electrostatic spraying. The substrate coated is then heated as long as it is necessary for the removal of volatile substances from the substrate and merge powders in a smooth molten film. Immediately after the merger, the molten film is exposed to UV light, which instantly utverjdaet and strengthens the film in the form of persistent, smooth, attractive surface.

In some applications, it is necessary or desirable to powder coating had a surface which preferably is smooth in appearance, but has a low sheen or gloss. Such applications are those cases where low gloss is aesthetically desirable, or that the glare from the surface of the coating can interfere with safe or contemplated use of the product with the coating, such as work desks, dining tables, counters or other horizontal surfaces, optical devices, motorized vehicles, aircraft and ships.

One of the drawbacks of UV-curable powders is that of these powders is very difficult to produce a coating with a low sheen (the EU is ü matte), because the coatings produced from them, tend to Shine. Reduce Shine, as a rule, can be obtained from traditional powder coatings by introducing a matting agent such as fillers or waxes that are associated with the surface during curing and cause the Mat by destroying the surface. However, due to the high speed of curing UV-curable powders, conventional fillers or waxes can't flocculate on the surface at a rate sufficient to obtain a low Shine, and they remain trapped in the coating. A large number of fillers or waxes that can be used to overcome this problem, have a tendency to bind powders and the formation of the pellet during normal storage and/or give coatings with surface relief orange peel, limiting a decrease in the gloss, which can be obtained.

One approach to solving the above problems associated with coatings with low gloss of the compositions for UV-curable powder coatings presented in U.S. patent No. 6017593. In U.S. patent No. 6017593, reduced gloss is obtained by use of a mixture of crystalline and amorphous resins and by adding a cooling stage after stage of melting, but dostudio photoinitiator curing, during which the crystalline resin precrystallizer. However, the method described in U.S. patent No. 6017593, limited in practical applications, only those substrates that have a homogeneous profile of heating and cooling. Thus, the method of U.S. patent No. 6017593 leads to differential crystallization, change the Shine and speckled appearance when it is used in conjunction with substrates having different spatial profiles of heating and cooling, such as non-metallic substrates or substrates with varying thickness, sharp edges and corners.

For this reason, it would be desirable to provide a method for obtaining coatings with an exterior, low sheen, compositions for UV-curable powder coatings on substrates having different spatial profiles of heating and cooling, such as non-metallic substrate.

U.S. patent No. 6017640 describes a dual thermosetting and ultraviolet-curable light powder coating containing a mixture of (a) unsaturated resin selected from unsaturated polyesters, unsaturated polyacrylates, unsaturated polymethacrylates and mixtures thereof; b) an optional jointly polymerizing agent for cross-linking resin; (c) photoinitiator; (d) a thermal initiator; and (e) substances, making the th material is opaque, selected from pigments, fillers, and mixtures thereof. Powder coating of U.S. patent No. 6017640 allow you to obtain a surface with exceptional smoothness and desired gloss, and the gloss of these surfaces is reduced by adding either fillers or substances to control Shine. As noted above, however, the high speed curing UV-curable powders does not allow conventional fillers or waxes to stick on the surface fast enough to get low gloss, invoking instead the capture inside the cover.

For this reason, it is desirable to find a way to get the powder coating with reduced gloss of the compositions of UV-curable powder coatings, which does not include any fillers or substances to control Shine.

The invention

The present invention is directed to a composition for powder coating, which, when cured, results in coatings with low Shine, this composition contains:

the base polymer selected from the group consisting of cross stitched complicated polyester, cross stitched polyurethane, cross stitched acelerando polyether, and combinations thereof;

from about 5 percent to about 60 percent of cross stitched acrylic polymer; and

the ome from 0.1 to 10 percent of one or more free radical initiators, all percentages are given as weight percent relative to the total mass of these cross stitched main and acrylic polymer in solid form.

The present invention is also directed to a method for obtaining coatings having reduced gloss, and this method comprises the stages:

applying on a substrate a layer of a powder coating composition with reduced gloss containing a base polymer selected from the group consisting of cross stitched complicated polyester, cross stitched polyurethane, cross stitched acelerando polyether, and combinations thereof; from about 5 percent to about 60 percent of cross stitched acrylic polymer; and from about 0.1 to 10 percent of one or more free radical initiators, all percentages are given as weight percent relative to the total mass of these cross stitched main and acrylic polymer in solid form;

heating of the specified layer to form a film; and

curing the specified film before formation of the specified coating having reduced gloss.

The present invention also is directed to a method for obtaining a powder coating composition with a low sheen, which includes stages:

mixing of the basic polymer selected from the gr is PPI, consisting of transversely stitched complicated polyester, cross stitched polyurethane, cross stitched acelerando polyether, and combinations thereof, together with from about 5 percent to about 60 percent of cross stitched acrylic polymer and from about 0.1 to 10 percent of one or more free radical initiators, to form a mixture, all percentages are given as weight percent relative to the total mass of these cross stitched main and acrylic polymer in solid form;

heating of this mixture before formation of the molten mixture;

extrusion from the melt specified molten mixture to obtain molten extrudate;

curing the specified molten extrudate to obtain a solid extrudate;separation of the specified solid extrudate fragments; and

grinding of these fragments.

A detailed description of the preferred embodiments

As here defined:

Coverage with low gloss" means coatings that have glitter within from 0.1 to 80, preferably in the range from 1 to 50, more preferably from 10 to 30, when it is measured at an angle of reflection of 60°using a Micro-Tri-Gloss Giossimeter, supplied by BYK Gardner, Pomano Beach, Florida.

"Smooth coating" means a coating having a VI is emuu smoothness and smoothness, sufficient for writing. The coating is considered smooth enough for writing, if the line is drawn manually, using a ballpoint pen on the writing paper of standard quality, placed directly on the surface with the coating is visually perceived as continuous (no breaks) and regular (without twists). The apparent smoothness of the coating is determined on a scale from 1 to 10, using the standards of smoothness PCI Powder Coating Institute, Alexandria, Virginia), where 1 is very uneven orange peel, and 10 represents the highest degree of smoothness.

"Cross link polymer" means a polymer having one or more double bonds in the carbon-carbon located in the main polymer chain, arranged in the form of side groups, branched from the main chain of the polymer located at the ends of the main chain of the polymer, or combinations thereof.

The term "spheroidal"as it is used here, refers generally spherical in shape. More specifically, this term refers to materials fillers, which contain less than 25% of the agglomerates of particles or islomania particles containing sharp or rough edges. Spheroidal particles must not be reactive or inert, so as not to negatively affect other properties of the composition.

"The substrate of pressovanne the x wood impregnation" (DSP) means, substrates derived from wood particles, fibers, chips or shavings, such as solid particleboard, fibreboard medium density fibreboard of oriented fibers, also known as wafer stove, wood stove, Bindery cardboard and fiberboard of wood particles. Such chipboard, as a rule, produced under the action of heat and pressure from particles, fibers, chips or shavings. Particleboard is produced by processing particles, chips, shavings or fibers with a binder, and then, placing these treated particles, shavings, chips or fibers in the form of a Mat, in dry or wet conditions. Then this Mat is compressed in the form of a dense substrate, usually in the form of a sheet by application of heat and pressure. Binder binds the particles, chips, shavings or fibers and increases the structural strength and integrity of the DSP and its resistance. Particleboard, if desired, may be formed in a desirable shape or provided with a textured surface, such as the structure of the wood layers. Some examples of chipboard, which include fiberboard medium density fiberboard of oriented fibers, particleboard from particles, a plate of crumbs and the base for the floors, adds the who.

"Fibreboard medium density" means the stove, made from lignocellulosic fibers bonded under heat and pressure, by carefully dispersed synthetic resin or similar binder. This plate is made with a relative density of from 0.50 to 0.88 to.

"Fibreboard of oriented fibers (OSB)" means the stove, made from crumb type of lignocellulosic fiber, purposefully aligned in a certain direction, which makes the resulting plate more durable, stiffer and having improved properties keeping the dimensions in the direction of alignment compared to a plate having a random orientation crumbs. OSB is also known as a flat plate pressing.

"Chipboard particle" means a plate manufactured from particles of wood, connected by the action of heat and pressure by carefully dispersed synthetic resin or similar binder. This plate includes a conventional particle Board from particles obtained by extrusion and formed in the shape of a plate.

"Wood-fiber plate of crumbs" means a plate made of wood are bonded aggregate under the action of heat and pressure by carefully dispersed synthetic see the crystals or similar binder.

"Ground floor" means smooth flat chipboard used as a panel for the floor, which can be glued elastic covering for the floor.

"The slab of pressed wood impregnation" means a laminated panel of wood, made of relatively thin layers of plywood, with a core of adjacent layers at right angles to each other, or a panel made of plywood, in combination with a core of lumber or particleboard.

The powder coating composition of the present invention provide for a user the ability to control the brilliance of the final coating, while minimizing or eliminating negative effects known from the literature attempts to control Shine; that is, the loss of fluidity of the coating and the formation of surface defects such as orange-peel.

Applicants unexpectedly found that the gloss of the coatings produced from the compositions of UV-curable powder coating can be controlled by the use of mixtures of one or more svobodnoradikal curable basic polymers and one or more svobodnoradikal curable acrylic polymers for coatings with low Shine, presumably through the mechanism of differential hardening. This effect can be complement the flax reinforced through the use of spheroidal particles.

The composition of the powder coating, which yields a coating with a low Shine, when cured, provides a base polymer selected from the group consisting of cross stitched complicated polyester, cross stitched polyurethane, cross stitched acelerando polyether, and combinations thereof; from about 5 percent to about 60 percent, preferably from about 10 mass percent to about 50 mass percent, more preferably from about 20 to about 40 percent of the mass transversely stitched acrylic polymer and from about 0.1 to about 10 percent, more preferably from about 0.1 percent to about 4 percent of one or several free radical initiators, all percentages are given as weight percent relative to the total mass of cross stitched main and acrylic polymer in solid form.

The base polymer may have a concentration of cross stitching groups within from about 0.3 percent to about 10 percent, preferably from about 0.5 percent to about 5 percent, more preferably from about 0.7 percent to about 3 percent relative to the weight of the cross stitched main polymer. Obtained using GPC srednevekovaja molecular mass, using the policy is irola as the standard of the basic polymer, may be in the range from 500 to 20000, preferably from 1500 to 10000.

Some of transversely stitched groups, which are suitable for use for cross stitching complicated polyester include acrylate, methacrylate, maleate, fumarate and their combination.

If desired, cross stitched polyesters can be blended with other usable cross stitched polymers.

Cross stitched polyesters, typically produced by the condensation of carboxylic acids or polycarboxylic acids (or their anhydrides) with hydroxy - or polyhydroxy-functional monomers. Usable acids include 1,2,4-benzotriazolyl acid, 1,2-benzylcarbamoyl acid (ortho-phthalic acid), 1,3-benzylcarbamoyl acid, 1,4-benzylcarbamoyl acid (terephthalic acid), cyclohexanecarbonyl acid; C2-C12linear aliphatic decollate, such as adipic acid and dodecadienol acid; adipic anhydride, succinic anhydride, dodecadienol anhydride, maleic acid, maleic anhydride, fumaric acid, taconova acid, C1-C20aromatic and aliphatic monocellate, such as acetic acid, benzoic acid; and ethylene-unsaturated acid is such as acrylic acid and methacrylic acid. Suitable for the use of hydroxy-functional monomers include polyols such as 2-hydroxymethyl-2-methyl-1,3-propandiol; 2,2-bis-(2-hydroxymethyl)-1,3-propandiol; C2-C12linear diols, for example, 1,2-ethanediol, 1,3-propandiol, 1,4-butanediol and 1,6-hexanediol; branched C2-C12diols, for example, 2-methyl-1,3-propandiol, 2,2-dimethyl-1,3-propandiol and 2-ethyl-2-butyl-1,3-propandiol; alicyclic diols, for example, 1,2-cyclohexanediol, 1,4-cyclohexanediol and 1,4-cyclohexanedimethanol.

Some of usable commercial cross stitched polyesters include those which are supplied:I. UCB Chemicals, Smyrna, Georgia, under the trade name Uvecoat® 1000, resin-based unsaturated polyesters with methacrylate end groups, Uvecoat® 1100, resins based on unsaturated polyesters with methacrylate end groups, Uvecoat® 2000, resins based on unsaturated polyesters with methacrylate end groups, Uvecoat® 2100, resins based on unsaturated polyesters with methacrylate end groups, Uvecoat® 2101, resins based on unsaturated polyesters, Uvecoat® 2200, resins based on unsaturated polyesters with methacrylate end groups, Uvecoat® 2300, resins based on unsaturated polyesters with metake innymi end groups, Uvecoat® 9000, crystalline resins based on unsaturated polyesters with methacrylate end groups, Uvecoat® 9010, crystalline resins based on unsaturated polyesters with methacrylate end groups and Uvecoat® D 8337, resins based on unsaturated polyesters, and Uvecoat® 3101, resins based on unsaturated polyesters.

II. DSM Coating Resins, Zwolle, The Netherlands, under the trade name Uracross® ZW 4892 P, unsaturated complex polyester, Uracross® ZW 4557 P, resin-based unsaturated polyesters, Uracross® ZW 4989 P, resin-based unsaturated polyesters with methacrylate end groups, Uracross® ZW 5125 P, resin-based unsaturated polyesters, Uracross® 5026 P, resin-based unsaturated polyesters with GMA functional groups, Uracross® ZW 4901 P, resin-based unsaturated polyesters with maleate end groups, and Uracross® P 3125, resins based on unsaturated polyesters with maleate finite groups.

III. Solutia lnc, St Louis, Missouri, under the trade name Viaktin® VAN 1743, resins based on unsaturated polyesters, Viaktin® 03490, resins based on unsaturated polyesters with methacrylate end groups, Viaktin® 03890, resins based on unsaturated polyesters with methacrylate end groups, Viatin® 03929, resins based on unsaturated polyesters with methacrylate end groups, Viaktin® 03732, resins based on unsaturated polyesters with methacrylate end groups, and Viaktin® 03729, the semi-crystalline resins based on unsaturated polyesters with methacrylate end groups.

IV. Cray Valley, Saint Celani, Spain, under the trade name Reafree® ND-1291, resins based on unsaturated polyesters, Reafree® ND-1530, resins based on unsaturated polyesters with acrylate groups and Reafree® ND-1446, resins based on unsaturated polyesters.

V. Panolam, Auburn, Maine, under the trade name Pioester® 1937, resins based on unsaturated polyesters, Pioester® 275, resins based on unsaturated polyesters and Pioester® 202 HV, resins based on unsaturated polyesters.

Suitable for use mixtures of cross stitched polyesters and other cross stitched polymers include Uvecoat® 3000, a mixture of resins based on unsaturated polyesters and epoxyacrylate resin, Uvecoat® 3001, a mixture of resins based on unsaturated polyesters and epoxyacrylate resin, Uvecoat® 3002, a mixture of resins based on unsaturated polyesters and epoxyacrylate resin and Uvecoat® 3003, a mixture of resins based on unsaturated polyesters and VC is xialilang resin, they all come UCB Chemicals, Smyrna, Georgia.

Some of transversely stitched groups, which are suitable for use, for cross stitched polyurethane include acrylate, methacrylate, maleate, fumarate, itaconate, alkenone and their combination.

If desired, cross stitched polyurethane can be mixed together with other usable cross stitched polymers.

Cross stitched polyurethane, typically prepared by condensation of polyisocyanates with polyols, which are described above, and with monomers bearing cross stitching group described above. Suitable polyisocyanates include aliphatic or cycloaliphatic di-, tri - or Tetra-isocyanates, which may or may not be the ethylene-unsaturated. Some specific examples of aliphatic polyisocyanates include 1,2-propylene diisocyanate, trimethylene diisocyanate, tetramethylene diisocyanate, 2,3-butylene diisocyanate, hexamethylene diisocyanate, octamethylene diisocyanate, 2,2,4-trimethyl hexamethylene diisocyanate, 2,4,4-trimethyl hexamethylene diisocyanate, dodecamethyl diisocyanate, the diisocyanate simple omega-DIPROPYLENE ether, 1,3-cyclopentane diisocyanate, 1,2-cyclohexane diisocyanate, 1,4-cyclohexane diisocyanate, isophorone diisocyanate, 4-methyl-1,3-di is socialecological, TRANS-vinylidene diisocyanate, dicyclohexylmethane-4,4'-diisocyanate, 3,3'-dimethyl-dicyclohexylmethane 4,4'-diisocyanate and meta-tetramethylsilane diisocyanate; polyisocyanates, which has structural units, such as isocyanurate hexamethylene diisocyanate and isocyanurate isophorone diisocyanate; the adduct of 2 molecules of a diisocyanate, such as hexamethylene diisocyanate; uretdione hexamethylen diisocyanate; uretdione isophorone diisocyanate or isophorone diisocyanate; the adduct of 3 molecules hexamethylene diisocyanate and 1 molecule of water (available under the trade name Desmodur® N, Bayer Corporation, Pittsburgh, Pennsylvania). Examples of usable aromatic polyisocyanates include toluene diisocyanate and difenilmetana diisocyanate.

Usable monomers bearing the above cross stitching group include simple vinyl esters, such as a simple 2-hydroxyethyl vinyl ether and simple 4-hydroxybutyl vinyl ether, and esters such as 2-hydroxyethyl acrylate, 2-hydroxyethyl methacrylate, 4-hydroxybutyl acrylate and 4-hydroxybutyl methacrylate.

Some of usable commercially available cross stitched polyurethanes include those that are supplied:I. Cray Valley, Saint Celani, Spain, under the trade name Reafree® ND-1605, acelerou the Naya aromatic polyurethane resin and Reafree® ND-1605/2, arilirovaniya aliphatic polyurethane resin.

II. DSM Coating Resins, Zwolle, The Netherlands under the trade name Uracross® P 3898, minilaparotomy complex polyester, Uracross® ZW 5150 P, epoxyacrylate resin with maleate finite groups and Uracross® ZvV 5151 P, epoxyacrylate resin with maleate finite groups.

III. Solutia Inc. St. Louts, Missouri under the trade name Viaktin® 03545, unsaturated urethaneacrylate resin.

IV. Bayer Corp, Pittsburgh, Pennsylvania under the trade name FAC® 314, urethaneacrylate resin and FAC® 320 B, urethaneacrylate resin.

V. Bomar Specialty Company, Winstead, Connecticut, under the trade name XJH1-148 A, urethane acrylate and STC3-130 A, urethaneacrylate resin.

VI. DuPont Company, Wuppartal, Germany, under the trade name Dekatol® SK 1866, urethaneacrylate resin and Dekatol® SK 2092, urethaneacrylate resin.

VII. Estron, Calvery City, Kentucky, under the trade name of U-810, epoxyacrylate resin.

VIII. Dow Chemical, Freeport, Texas, under the trade name XZ92478.00, epoxyacrylate.

Cross stitched calironia polyesters, typically produced by the interaction of the epoxy-functional polyethers with ethylene-unsaturated carboxylic acids. Some of usable epoxy-functional polyesters include polymers of bisphenol A and epichlorohydrin; and polymers of bisphenol F and epichlorohydrin. Some and is suitable for use ethylene-unsaturated carboxylic acid include acrylic acid, methacrylic acid, maleic acid, taconova acid and fumaric acid.

Cross stitched acrylic polymer suitable for use in the present invention may have a glass transition temperature that is within about 40°C to about 100°C, preferably from about 45°C to about 65°C; obtained using GPC srednevekovoy molecular weight, using polystyrene as a standard, in the range of about 1000 to about 30000, preferably from about 2000 to about 20000. Cross stitched acrylic polymer may have a concentration of cross stitching groups within from about 0.3 percent to about 10 percent, preferably, from 0.5 percent to about 3 percent by weight of cross stitched acrylic polymer. Some of the usable cross stitched groups include acrylate, methacrylate, maleate, fumarate, itaconate and their combination.

Cross stitched acrylic polymer can be prepared by reacting at elevated temperatures, in the range of 50°C to 220°C, epoxy-functional acrylic polymer with (meth)acrylic acid, fumaric acid, taconova acid and maleic acid; hydroxy-functional acrylic polymer of the (meth)acrylic acid, fumaric acid, taconova acid and maleic acid and their anhydrides; or anhydride-functional polymer with a hydroxy-functional ethylene-unsaturated monomers.

Suitable for use epoxy-functional acrylic polymers can be a conventional polymers having obtained using GPC srednevekovoy molecular weight in the range of 1,000 to 30,000. Commercially available epoxy-functional acrylic polymers, among others, are supplied Anderson Acrylic Company, Adrian, Michigan, under the trade name Almatex® PD 7610 and Almatex® PD 7690.

Suitable for use hydroxy-functional acrylic polymers are conventional polymers having obtained using GPC srednevekovoy molecular weight in the range of 1,000 to 30,000. Commercially available hydroxy-functional acrylic polymers, among others, come S.C. Johnson Company, Racine, Wisconsin, under the trade name Joncryl® 802 and Joncryl® 804.

Free radical initiators suitable for use in the present invention include one or more free radical photoinitiators, one or more free radical thermal initiators or combinations thereof. Free radical photoinitiator initiated photolytic, and Svobodnaya the e thermal initiators are initiated during exposure to elevated temperatures. Can also be used a combination of UV photoinitiation and thermal initiation (dual cure). When they are used in combination, the mass ratio of thermal initiator and photoinitiator is in the range from 10:90 to 90:10, preferably from 25:75 to 75:25.

Some of usable free radical photoinitiators include oxides, bis-allforyou, such as 2,4,6-trimethylbenzoyl diphenylphosphine oxide; α-hydroxy ketones. Some of the other usable free radical photoinitiators include:

I. Free radical photoinitiator α-splitting, including benzoin and its derivatives, such as simple benzoic esters, such as simple isobutylbenzene ether, and benzylacetone, such as benzyldimethyl ketal, 2-hydroxy-2-methyl-1-phenylpropane-1-he 4-(2-hydroxyethoxy)phenyl-2-hydroxy-2-propyl ketone.

II. Arylketones, such as 1-hydroxycyclohexyl phenyl ketone, 2-benzyl-2-dimethylamino-1-(4-morpholinomethyl)butane-1-he, 2,2-dimethoxy-2-phenylacetophenone, a mixture of benzophenone and 1-hydroxycyclohexyl ketone, perfluorinated diphenyl titanocene and 2-methyl-1-(4-(methylthiophenyl)-2-(4-morpholinyl))-1-propanone.

Can be used photoinitiator removal of hydrogen free radical type, in combination with those mentioned above, or with the mi itself, such as michler ketone (4,4'-bidirectionalization), ethylketone Michler (4,4'-mediationarbitration), benzophenone, thioxanthone, anthrachinon, d,l-comparison, ethyl d,l-comparison, catechumen, anthracene or derivatives thereof.

Some of usable commercially available photoinitiators come Ciba Speciality Chemicals, Basel, Switzerland, under the trade name Irgacure® 819, bis-acyl phosphinoxide photoinitiator and Irgacure® 2959, a-hydroxy ketone photoinitiator.

Some of usable thermal free radical initiators include organic peroxides, such as benzoyl peroxide; diazepamonline, such as 2-4 dichlorobenzophenone, diethanolamide, decanoyl peroxide, eurailpress, succinic acid peroxide, acetylmuramic, benzoyl peroxide and Diisobutylene; acetylcholinesterase, such as acetylcyclohexanone; dialkyldithiocarbamate, such as di(n-propyl)PEROXYDICARBONATE, di(sec-butyl)PEROXYDICARBONATE, di(2-ethylhexyl)PEROXYDICARBONATE, diisopropylperoxydicarbonate and dicyclohexylperoxydicarbonate; complex peroxy esters, such as α-semiproletariat, α-semiperennial, tert-aminoalkanoic, tert-anilinoquinazolines, tert-butylperoxybenzoate, t is et-Liliaceae, tert-butyl peroxypivalate, 2,5-dimethyl-2,5-di(2-ethylhexanoylperoxy)hexane, tert-AMYLPEROXY-2-ethyl of hexanoate, tert-butyl peroxy-2-ethylhexanoate and tert-butylperoxyisopropyl; azobis(alkynylaryl)peroxy compounds such as 2,2'-azobis-(2,4-dimethylvaleronitrile),azobisisobutyronitrile and 2,2'-azobis-(2-methylbutyronitrile); tert-butylperoxyisopropyl acid, 1,1'-azobis(1-cyclohexanecarbonitrile); peroxy ketals such as 1,1-di(tert-BUTYLPEROXY)-3,3,5-trimethylcyclohexane; complex peroxy esters such as o,o'-tert-butyl-o-isopropylaminocarbonyl, 2,5-dimethyl-2,5-di(benzoylperoxy)carbonate, o,o'-tert-butyl-o-(2-ethylhexyl)nonoperational, tert-butyl peroxyacetate, tert-butyl peroxybenzoate, di-tert-butylperoxide and di-tert-butylperoxide; dialkylamide, such as dicumylperoxide, 2,5-dimethyl-2,5-di(tert-BUTYLPEROXY)hexane, tert-butylcumylperoxide, di-tert-butylperoxide and 2,5-dimethyl,2,5-di(tert-BUTYLPEROXY)hexyne-3; hydroperoxides, such as 2,5-dihydroperoxy-2,5-dimethylhexane, cumen hydroperoxide, tert-butylhydroperoxide and tert-AMYLPEROXY; cloperastine, such as n-butyl-4,4-bis(tert-BUTYLPEROXY)valerate, 1,1-di(tert-BUTYLPEROXY)-3,3,5-trimethylcyclohexane, 1,1'-di-tert-amyl-praxitelean, 2,2-di(tert-BUTYLPEROXY)butane, ethyl 3,3-di(tert-BUTYLPEROXY)butyrate, and a mixture of tert-bout is peroctoate and 1,1-di(tert-BUTYLPEROXY)cyclohexane; and diazocompounds, such as 1,1'-azobis(cyclohexanecarbonitrile)peroxide.

Additional thermal and photoinitiators are described in U.S. patent No. 5922473; in U.S. patent No. 6005017 and in U.S. patent No. 6017640, they are all included here as a reference.

In addition to the above, the powder coating composition of the present invention can contain other additives commonly used in powder coating compositions. Examples of such additives include fillers, disintegrating agents, additives to impart fluidity, catalysts, photostabilization, hardeners and pigments. Can also be added compounds having antimicrobial activity. Such compounds are described in U.S. patent No. 6093407, which is included here as a reference.

The gloss coating of the composition for powder coatings according to the present invention can be further reduced by incorporating from about 5 percent to about 60 percent, preferably from about 10 percent to about 50 percent, and more preferably, from about 20 percent to about 40 percent, spheroidal particles, all percentages are given as percentage of the mass relative to the total weight of the composition of the coating, where these spheroidal particles have a median diameter of particles in the range from about 1 micrometers to about 50 micrometers, preferably, from 15 micrometers to 50 micrometers. When the average particle diameter decreases, the surface per unit mass increases. The increase in surface area leads to the appearance trends, the filler to dry the coating to decrease turnover and leads to the roughness of the coating. Spheroidal particles having an average diameter less than 10 micrometers, have less effect in further reducing Shine, while with average diameters greater than 10 μm, in particular greater than 15 micrometers, the presence of spheroidal particles leads to an additional reduction of gloss.

The upper limit of the diameter of the spheroidal particles depends on the assumed thickness of the final coating, the particles should have a diameter less than the thickness of the coating. Most powder coatings, in particular decorative powder coatings designed for application at a dry film thickness of approximately 50 microns. Thus, in most applications, spheroidal particles should have a maximum diameter of less than about 50 microns, preferably 40 microns.

Spheroidal particles suitable for use in the present invention include glass microspheres, ceramic microspheres, spheroidal minerals, polymeric micro is very, metal microspheres or a combination thereof.

Some of usable commercially available spheroidal particles are listed below:

Table 1
Spheroidal agents to control Shine
Glass beads (Potters Industries, Inc., Valley Forge, Pennsylvania)
QualityMaxteam. (µm)Median dia. (µm)Reducing Shine
Spheriglass™ 3000E90% ≤ 60 microns3 micronsHigh1
Spheriglass™ 3000E sieved with a 45 μm4523High
Spheriglass™ 10000E63Low (too small)
Ceramic microspheres (3M Corporation, Minneapolis, Minnesota)
G200 Zeeospheres™124Low (too small)
G400 Zeeospheres™245Low (too small)
G600 Zeospheres™ 406Low (too small)
W610 Zeeospheres™4010No (too small)
G800 Zeeospheres™20018High1
G850 Zeeospheres™20040High1
G850 Zeeospheres™ sieved with a 45 μm4520High
Cristobalite (C.E.D. Process Minerals, Inc., Akron, Ohio)
Goresil™C-4001009Low (too small)1
Goresil™ 10454510No (too small)
Goresil™ 835358Low (too small)
Goresil™ 525255Low (too small)
Goresil™ 215152the izkuyu (too small)

The powder coating composition with low gloss can be prepared by using the following steps:

The base polymer selected from the group consisting of cross stitched complicated polyester, cross stitched polyurethane, cross stitched acelerando polyether, and combinations thereof; from about 5 percent to about 60 percent of cross stitched acrylic polymer and from about 0.1 to 10 percent of one or more free radical initiators are mixed in a conventional mixer to form a mixture. All the above percentages are given as percent of the mass relative to the total mass of cross stitched main and acrylic polymer in solid form. The mixture is then heated, usually in a conventional extruder, before the formation of the molten mixture. The temperature of the melt, depending on the chemical composition typically is in the range from 80 to 150°C. the molten mixture is extruded from the melt in the form of molten extrudate. Generally, stage of extrusion from the melt takes place at a pressure sufficient to obtain molten extrudate, which is then cured to a solid state extrudate, usually by passage through a cooled rolls. Then cured extraditables using conventional means, for example, by passing through rollers with teeth or grooves, into fragments, which are then convenient to grind the crushed fragments with a size in the range of 5 to 200, preferably from 10 to 100 micrometers. If desired, the uniformity of the particle size can be improved by passing the crushed fragments through a sieve, for example through a 180 micron sieve to remove large fragments. If desired, the crushed fragments can be added to water or aqueous medium for forming a water suspension.

If desired, the mixture described above, may include the above-described spheroidal particles in the above-mentioned interest relations.

Smooth finish with low gloss, can be obtained in accordance with the following stages:

The layer described above, the powder coating composition with reduced gloss is applied to the substrate by conventional means, for example, by electrostatic spraying, thermal or flame spraying, or by dipping in a fluidized bed containing the powder coating composition. If desired, the powder coating composition may contain the above-described spheroidal particles in the above-described amounts. Coatings can be applied to metal or Nemeth is symbolic of the substrate. The thickness of the layer is chosen in order to obtain the range of coating thickness of 10 micrometers to 500 micrometers. You must understand that the thickness of the coating depends on its intended use. For example, when it is applied on a substrate made of pressed wood materials impregnated with, it can vary from 25 to 300 micrometers (1 to 12 mil), when it is applied on a metal substrate, it can be in the range of from 10 to 500 micrometers (0.5 to 20 mils).

After deposition of the layer of the powder coating composition on a substrate, the substrate is typically heated for melting the composition and to cause it to flow and form a film on the surface of the substrate. In certain applications, the substrate or the part of it that should be applied to the coating, can be pre-heated before applying the powder, and then, if desired, be heated again, after application of the powder. For these various stages of heating are commonly used gas or electric stoves, but there are other ways (e.g., microwave ovens). Typically, depending on the chemical composition of the composition for the coating layer is heated to a temperature in the range from about 80°C to about 200°C, preferably from about 80°C to about 150°C and valueproposition, about 80°C to about 120°C. typically, depending on the chemical composition of the coating layer to exhibit the above-described temperature, for about 0.5 to 10 minutes, preferably from about 1 to about 5 minutes. The higher the temperature, the shorter the time of exposure, and Vice versa.

After the formation of a film on a substrate, it is cured in the form of a coating with a low sheen, which can be smooth. The film may be cured with the help of several alternative means. For example, the film may be cured by the action of chemically active radiation, high temperatures, by acting on it consistently elevated temperatures, and then chemically active radiation by the step of chemically active radiation, and then elevated temperatures, preferably within about 5 to about 30 minutes; or by the simultaneous action of chemically active radiation and high temperatures.

Depending on the chemical composition of the coating, typical elevated temperatures are in the range from 90 to 220°C, preferably from 100 to 200°C, and more preferably from 100 to 170°C. thermal curing can be carried out using conventional means, which uses conduction,convection, radiation or any combination.

Depending on the chemical composition of the coating, a typical chemically active radiation includes UV radiation, electron beam radiation, or a combination thereof, at a dose of from about 0.25 to about 5.0 and preferably from about 0.5 to about 3 joules per square centimeter.

EXAMPLES

In the examples described below, lists the following components: polymer 1 (getting cross stitched acrylic polymer)

In a three-neck glass reactor equipped with a stirrer, thermocouple and a funnel, 700 mass parts (moschata) butyl acetate are heated to 20°C. the mixture is Then 1302 moschata glycidyl methacrylate, 348 moschata styrene and 747 moschata of methyl methacrylate added dropwise within a 6.5-hour period. At the same time also add a solution of 215 moschata of tertiary butylperoxide 250 miscast butyl acetate. After 6.5 hours to download add a further solution of 34 moschata of tertiary butylperoxide 34 miscast butyl acetate. Then 50 moschata butyl acetate is used for flushing of pipes for the supply of monomer and initiator. The load is maintained at 120°C for an additional 4-hour period. Then to boot add to 6.4 Mascali 4-methoxyphenol, and then adding 103 moschata Smoot the OIC acid and 210 moschata butyl acetate. The load is maintained at 120°C up until the acid number drops below 1 mg KOH/g solid resin products. After that, apply vacuum and the solvent is removed until until the solids content of products >99%. The obtained viscous acryloyl functional acrylic polymer was poured onto a flat tray and, after drying, is crushed. The polymer has a Tg equal 57-62°C (measured by DSC), melt viscosity at 150°C equal to 1800 SP, and the content of double bonds of 1.4% (calculated as C=C, is equal to 24D).

Uvecoat® 3002, resins based on unsaturated polyesters from UCB Chemicals, Smyrna, Georgia.

Uvecoat® 3001, a mixture of resins based on unsaturated polyesters and epoxyacrylate resin from UCB Chemicals, Smyrna, Georgia.

Uvecoat® 3101, resins based on unsaturated polyesters from UCB Chemicals, Smyrna, Georgia.

Uralac® 3125, resins based on unsaturated polyesters from DSM Coating Resins, Zwolle, The Netherlands,

Uracross® 3307, agent for cross-linking on the basis of simple deviceloop ether from DSM Coating Resins, Zwolle, The Netherlands.

Uvecoat® 2100, resins based on unsaturated polyesters from UCB Chemicals, Smyrna, Georgia.

Uvecoat® 9010, crystalline resins based on unsaturated polyesters with methacrylate end groups from UCB Chemicals, Smyrna, Georgia.

Irgacure® 819, photoinitiator from Ciba Specialty Chemicals, Basel, Switzerland.

Irgacure® 2959, photoinitiator from Ciba Specialty Chemicals, Basel, Switzerland.

R-706®, pigment based on titanium dioxide from E.I. DuPont de Nemours, Wilmington, Delaware.

Sphereiglasss® 3000E, the filler of glass beads from P.Q. Corporation, Valley Forge, Pennsylvania (sieved on a sieve of 325 mesh to remove particles greater than 45 microns)Modiflow® III, additive to improve fluidity from Solutia, St. Louis, Missouri.

Luperox® ACP35, thermal free-radical curing agent based on benzoyl peroxide from Specialty Chemicals Atofina, Philadelphia, Pennsylvania.

Composition of powder coatings listed in tables 2, 3 and 4, prepared using a standard method. The components are combined and mixed in the bag, then ekstragiruyut from the melt. The extrudate utverjdayut between cooled rollers, then break and crushed to powder. The powders pass through a sieve of 80 mesh (180 micron)to remove large particles.

The coatings are produced by applying a powder compositions listed in tables 2 and 4 bar of mild steel, thickness to 0.032 inch, melting of the coating within 4 minutes, at 121°C-177°C (250-350°F), with the subsequent action within 15 seconds, ultraviolet radiation from the two lamps, lamp Fusion "V" and the lamp Fusion "H", for a total dose of approximately 2.5 j/cm2.

Coverage in table 3 are obtained by pre-heating the sample wood PL is you average density of 1 inch thick to the surface temperature of 65° C (150°F), powder-coating by electrostatic spraying, melting of the coating within 4 minutes, when 93-127°C (200-260°F), with the subsequent action within 15 seconds, ultraviolet radiation from the two lamps, lamp Fusion "V" and the lamp Fusion "H", for a total dose of approximately 2.5 j/cm2.

After cooling, the substrate with the coating are evaluated for gloss, smoothness and chemical resistance. Research on ASTM gloss at an angle of reflection of 60° represents ASTM D523-89. To determine the chemical resistance is used the following way:

Research on chemical resistance with IEC

(1) using a cotton swab soaked in methyl ethyl ketone (MEK), cut parts with a coat length of one inch is wiped with fifty double proteron. Double wiping consists of one passage surface coated up and one back, as if erasing the risks of a pencil. It uses about the same effort as when erasing with the eraser to the pencil.

(2) After all the double proteron, given the opportunity for evaporation of MEK and coverage is estimated as follows:

I. Wiping thoroughly, that is, the substrate is exposed.

II. Strong erasing, that is, removed a large percentage, more than 25% of the thickness of the coating, as determined by the visa is) but the substrate is not exposed. To cover with a color different from white, a large amount of pigment is observed on a cotton swab.

III. Moderate abrasion, i.e. removes moderate percentage of 10-25% of the thickness of the coating. To cover with a color different from white, a moderate amount of pigment is observed on a cotton swab.

IV. Easy erasing, that is, removed a small amount of coating, less than 10%. A small amount of pigment is observed on the swab. There is a loss of gloss.

V. the Absence of the effect, i.e. erasing does not occur. Loss of gloss is observed.

(3) Although the standard scores are 1, 2, 3, 4 or 5, mid-term evaluation (for example, 1.5, 2.5 and the like) can also be used when evaluating coatings.

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Table 2
The composition of the coatings (part of mass)
Component1Ctl 1Ctl 2Ctl 3Ctl 45678910111213/td> 14
Polymer 1100---------50302010505030503050
Uvecoat® 2100---100------5070809050---------------
Uvecoat® 3002------100------------------5070------
Uralac® 3125---------85---------------------355535
Uracross® 3307---------15---------------------151515
Spheridlass®

3000E(sifted through a sieve of 45 μm)
------------------------40--------- ---40
Properties of coatings
Shine (reflection under Polom 60°)8697979673314651476457614127
Smoothness364741632568537
Chemical resistance43,54353,52,52,544,5 42,5343
Notes
1. Ctl 1, Ctl 2, 3 Ctl and Ctl 4 are comparative examples.
2. All coatings also contain Modaflow®III, 1,3; Irgacure®819, 2.5 parts; Irgacure®2959, 0.5 parts; and R-706®40 parts.
3. Smoothness PCI: compared with standards from 1 (rough orange peel) to 10 (smooth).
4. Is determined by the impact on floor 50 double proteron using impregnated with methyl ethyl ketone cotton swab, estimates ranging from 1 (wiping completely) to 5 (no effect).
5. All of the above coatings have a smooth, suitable for writing.

Table 3
The composition of the coatings (part of mass)
Component1Ctl 51516
0,46X021-42---3030
Uvecoat® 300134,32424
Uvecoat® 310151,43 36
Uvecoat® 901014,3
Uvecoat® 901014,31010
Spheridlass®

3000E(sifted through a sieve of 45 μm)
40
Properties of the coating
Shine (reflection under Polom 60°)583626
Smoothness2899
Chemical resistance3444
Notes
1. Ctl 5 are comparative examples.
2. All coatings also contain Modaflow®6000, 1,3; Irgacure®819, 1.5 parts; Irgacure®2959, 1.0 part; and R-706®30 parts.
3. Smoothness PCI: compared with standards from 1 (rough orange peel) to 10 (smooth).
4. Is determined by the impact on floor 50 double proteron using impregnated with methyl ethyl ketone cotton swab, estimates ranging from 1 (wiping completely) to 5 (no effect).
5. All of the above coverage shall have a smooth, suitable for writing.

Discussion of results

The control (Comparative examples 1-4: These comparative examples which are outside the scope of the present invention demonstrate high gloss typical of commercial systems based on UV-curable resins. Coatings show orange peel, slight to moderate, and chemical resistance, from good to excellent.

The control (Comparative example 5: This example is outside the scope of the present invention, shows a smooth coating with the low gloss available at the present time, where low gloss is derived from combinations of resins, and where not included transversely stitched acrylic polymer.

Examples 5-8: These examples demonstrate the effect of different amounts of cross stitched acrylic polymer mixed with cross stitched a complex polyester (Uvecoat® 2100). The smallest Shine and optimum smoothness observed when the mixture contains 30 wt.% polymer 1. The gloss is reduced, as it is desirable, from 86 and 97 (Ctl.1 and Ctl.2) to 31 (PR), while smooth as is preferably maintained or increased from 6 and 4 (Ctl.1 and Ctl.2) to 6 (PR). There is minimal reduction in chemical resistance (between 3.5 and 4 (Ctl.1 and Ctl.2)) to 2.5 (PR).

Examples 10 and 11: These examples demonstrate that those who trends, observed in examples 5-8, is also observed for other combinations of acrylic polymer/complex polyester. Shine, as it preferably decreases from 86 and 97 (Ctl.1 and Ctl.3) to 64 and 57 (PR and Proverbs 11), and smoothness, as it preferably increases from 6 and 7 (Ctl.1 and Ctl.3) to 6 and 8 (PR and Proverbs 11). There is minimal reduction in chemical resistance of 3.5 and 3 (Ctl. 1 and Ctl. 3) to 2.5 (Proverbs 11).

Examples 12 and 13: These examples demonstrate that the trend observed in examples 5-8 and 10-11, is also observed for combinations of cross stitched acrylic polymer with mixtures of cross stitched complicated polyester and cross stitched polyurethane. Shine, as it preferably decreases from 86 and 96 (Ctl.1 and Ctl.4) to 41 (PR. 13). There is minimal reduction in smoothness between 6 and 4 (Ctl.1 and Ctl.4) to 3 (PR). There is minimal reduction in chemical resistance between 3.5 and 5 (Ctl.1 and Ctl.4) to 4 (PR).

A couple of examples 5 and 9, a pair of examples 12 and 14 and a pair of examples 15 and 16: These pairs of examples demonstrate that a significant reduction in gloss and increase smoothness observed when adding spheroidal glass fillers. Adding 40 parts of spheroidal filler reduces Shine from 73 (PR) to 47 (PR), while improving the smoothness of from 1 to 5. Adding 40 parts of spheroidal filler reduces Shine from 61 (PR) to 27 (PR), thus improving the smoothness from 5 to 7. Adding 4 parts of spheroidal filler reduces Shine from 36 (PR) to 26 (PR), without affecting the smoothness.

Examples 15 and 16: These examples demonstrate that coatings with a low gloss can be obtained when the melting temperature of the powder 90-120°C, typically used for heat-sensitive substrates, such as fibreboard medium density. The presence of cross stitched acrylic polymer, compared with control 5, not only reduces glare, but also improves the smoothness.

1. The powder coating composition, which when cured provides a coating with low Shine, and this composition contains:

the base polymer selected from the group consisting of cross stitched complicated polyester, cross stitched polyurethane, cross stitched acelerando polyether, and combinations thereof;

from about 5 to about 60% of cross stitched acrylic polymer having a glass transition temperature of from about 40 to 100°C; and about 0.1 to 10% of one or more free radical initiators, all percentages are given as weight percent relative to the total mass of the specified cross stitched main and acrylic polymer in solid form.

2. The powder coating composition according to claim 1, additionally containing from about 5 to 50% of spheroidal particles, all percentages are given as mass% of the LLC with respect to the total mass of the composition for coating, and where these spheroidal particles have a median particle diameter from about 10 to about 50 microns.

3. The coating composition according to claim 2, where the spheroidal particles are selected from the group consisting of glass microspheres, ceramic microspheres, spheroidal minerals, polymeric microspheres, metal microspheres and combinations thereof.

4. The coating composition according to claim 1, where the specified cross stitched acrylic polymer has a glass transition temperature of from about 40 to about 100°C.

5. The coating composition according to claim 1, where the specified cross stitched acrylic polymer is defined using GPC srednevekovoy molecular weight of from about 1000 to about 30000.

6. The coating composition according to claim 1 to 4 or 5, where the specified cross stitched acrylic polymer has a concentration of cross stitching groups from about 0.3 to about 10% by weight of cross stitched acrylic polymer.

7. The coating composition according to claim 6, where these cross stitched groups are acrylate, methacrylate, maleate, fumarate, itaconate and their combination.

8. The coating composition according to claim 1, where the specified free radical initiator comprises a thermal initiator, photoinitiator or a combination thereof.

9. The method of obtaining coatings having reduced gloss, this method involves the following stages:

applying n the substrate layer of the powder coating composition with low Shine, containing the base polymer selected from the group consisting of cross stitched complicated polyester, cross stitched polyurethane, cross stitched acelerando polyether and a combination thereof; about 5 to about 60% of cross stitched acrylic polymer having a glass transition temperature of from about 40 to 100°C; and from about 0.1 to 10% of one or more free radical initiators, all percentages are given as weight percent relative to the total mass of the solid products of the specified cross stitched main and acrylic polymer

heating of the specified layer before formation of the film and

curing the specified film before formation of the specified coating having reduced gloss.

10. The method according to claim 9, where the specified coating composition additionally contains from about 5 to 50% of spheroidal particles, all percentages are given as percent of the mass relative to the total weight of the composition of the coating, and where these spheroidal particles have a median particle diameter from about 10 to about 50 microns.

11. The method according to claim 9 or 10, where at this stage of curing the layer is subjected to the action of chemically active radiation.

12. The method according to claim 9 or 10, where at this stage of curing the layer is subjected to the action of the increased tempo of the atmospheric temperature, in the range of 90 to 220°C.

13. The method according to claim 9 or 10, where at this stage of curing the layer is subjected to the action of chemically active radiation and elevated temperature, in the range of 90 to 220°C.

14. The method according to item 13, where at this stage of curing the layer additionally continue to be subjected to said elevated temperature for about 5 to about 30 min after the termination of that certain chemically active radiation.

15. The method according to claim 9 or 10, where at this stage of curing the layer is subjected to the action of chemically active radiation, followed by the action of elevated temperature, in the range of 90 to 220°or the effect of increased temperature in the range of 90 to 220°With the subsequent action of chemically active radiation.

16. The method according to claim 9 or 10, where the said coating is smooth.

17. The method according to claim 9 or 10, where this substrate is a vehicle body or a substrate made of pressed wood materials impregnated.

18. The production method of the powder coating composition with a low sheen, which includes stages:

mixing of the basic polymer selected from the group consisting of cross stitched complicated polyester, cross stitched item is of lauretana, cross stitched acelerando polyether, and combinations thereof, together with from about 5 to about 60% of cross stitched acrylic polymer having a glass transition temperature of from about 40 to 100°and from about 0.1 to 10% of one or more free radical initiators, with the mixture, all percentages are given as percent of the mass relative to the total mass of the solid products of the specified cross stitched main and acrylic polymer;

heating of this mixture before formation of the molten mixture;

extrusion from the melt specified molten mixture with the formation of the molten extrudate;

curing the specified molten extrudate with the formation of the solid extrudate;

separation of the specified solid extrudate fragments and

grinding of these fragments.

19. The method according to p, where the mixture further comprises from about 5 to 50% of spheroidal particles, all percentages are given as percent of the mass relative to the total mass of the composition for coating, and where these spheroidal particles have a median particle diameter from about 10 to about 50 microns.

20. The method according to p or 19, further comprising passing the crushed fragments through a 180 micron sieve to remove the deposits of large fragments.

21. The method according to p or 19, further comprising adding water to said fragments with the formation of the aqueous suspension.



 

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