ES2529391B1 - Composition of microparticles containing chromatic and / or aromatic compounds - Google Patents

Abstract

The present invention has as its object a composition of microparticles containing chromatic and / or aromatic compounds, a final chemical composition comprising said microparticles that allows to change the physicochemical properties of the surface or material in which it is added, a process for obtaining the composition of microparticles as well as the final chemical composition that comprises it and the use of said final chemical composition to coat materials that achieve a physicochemical effect different from the natural one.

Description

DESCRIPTION

Composition of microparticles containing chromatic and / or aromatic compounds.

OBJECT OF THE INVENTION 5

The present invention has as its object a composition of microparticles containing chromatic and / or aromatic compounds, a final chemical composition comprising said microparticles that allows to change the physicochemical properties of the surface or material in which it is added, a process for obtaining the composition of 10 microparticles as well as the final chemical composition that comprises it and the use of said final chemical composition to coat materials that achieve a physicochemical effect different from the natural one.

BACKGROUND OF THE INVENTION 15

The chromogenic materials are altered their optical behavior under the influence of external parameters such as, for example, pressure, light, electric fields and temperature. Thermochromia includes the property of a material to change its color reversibly or irreversibly depending on the temperature. This can occur when changing the intensity and / or the maximum wavelength. In the Seeboth et al. The interaction between structure and thermochromy is described in detail in the Chinese Journal of Polymer Science 2007 (2) 123.

Materials based on different material components with common thermochromic properties are known in the state of the art. Chromogenic materials are characterized in that they undergo a color change or change of transparency to color or vice versa thermally induced. EP1084860, US4,028,118 and US4,421,560 describe the change in color effect based on a donor-recipient dye system with at least two additional components. The color change occurs in a wide temperature range, such as from 50 ° C to 120 ° C or from -40 ° C to 80 ° C. The dye system as a whole can also incorporate a polymeric matrix, if desired, as microcapsules with a diameter of approximately 50 µm.

The production of polymeric thermochromic materials with the help of printing (lined) of a thermochromic ink is a practical solution for some requirements and desires of the packaging industry but does not achieve the objective. Thus, according to US 2,037,421 a system with dye is printed on crystals for use as sun protection or according to US 4,121,010 polymers are coated with a thermochromic paint, which changes color thanks to the presence of sulfates, sulphides , arsenic, bismuth, zinc and other metals and their oxides.

The production of organic thermochromic composites has continued to be optimized to date. Thus a base composite consisting of at least one dye, developer and flux is doped with more and more substances. As for the microencapsulation or the control of the interaction between the dye, developer and the flux, the composite is increasingly doping with surfactant structures. Caprylates, malonates, oxalates, succinates, palminates, stearates, behenates or n-dodecylphenols, dodecylgalates are used, as described in EP0677564. fifteen

All of the thermochromic effects described above, reversible or irreversible, are based on a color change as the temperature increases, from colored to non-colored or from a colored state to another colored state. The change between different colors is done by combining several composites or by subtracting effects with combination 20 with non-thermochromic dyes. Thermochromic composites that pass from a non-colored state to a colored state with increasing temperature, that is, systems with reverse thermochromia, are less known to date.

However, all the compositions described above have the disadvantage that the pigments are exposed to degradation and are hardly dispersible in a final composition.

In addition, in no case of the state of the art is an aromatic effect obtained by releasing perfumed substances into the medium alone or in combination of thermochromic or photochromic compounds.

Therefore, it is necessary to obtain a versatile microparticulate composition that incorporates in its interior substances capable of being released by a change in the

physicochemical conditions, such as heat, light or friction. The microparticles of the present invention are characterized in that they encapsulate chromic compounds (thermochromic or photochromic) and / or aromatic compounds that will be subsequently released by changing the initial characteristics of the material that incorporates them.

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DETAILED DESCRIPTION OF THE INVENTION

The present invention has as its object a composition of microparticles comprising chromatic and / or aromatic compounds, a final chemical composition comprising said microparticles that allows changing the physicochemical properties of the surface or material in which it is added, a process for obtaining the microparticle composition as well as the final chemical composition that comprises it and the use of said final chemical composition to coat materials that achieve a physicochemical effect different from the natural one.

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For the purpose of the present invention, "microparticles", or "microcapsules" are understood interchangeably, to those particles of micrometer size, generally in the form of spheres (microspheres), which form structures under certain conditions from mixtures of compounds and that allow to include substances inside to protect them from the environment or achieve a specific physicochemical effect. In the case of the invention, the microparticles encompass or encapsulate chromic compounds (thermochromic or photochromic) and / or aromatic compounds that will be subsequently released by changing the initial characteristics of the material that incorporates them.

For the purpose of the present invention, "microparticulate composition", or "microparticle composition" is understood interchangeably, to the base composition comprising the microparticles which is in turn suspended or dispersed in the final chemical composition.

For the purpose of the present invention, "chemical composition", "final chemical composition" or "composite" is understood interchangeably, to the composition composed of microparticles containing chromic and / or aromatic compounds or substances that is finally administered on a surface with the purpose of altering the physicochemical characteristics when these substances are released for reasons such as a change

of temperature, a change in brightness or a friction phenomenon. The microparticles of the present invention are characterized in that they encapsulate chromic compounds (thermochromic or photochromic) and / or aromatic compounds that will be subsequently released by changing the initial characteristics of the material that incorporates them. 5

For the purpose of the present invention, "chromic compounds", "chromic substances", "chromatic compounds" or "chromatic substances" are understood interchangeably, to those substances or components encapsulated in the microparticles of the invention that cause a change of color on the material in which they are present as a result of 10 changes in brightness or temperature changes. When the color change is caused by a change of light, they are called "photochromic compounds or substances" or "photochromic" interchangeably. When the color change is caused by a change in temperature, they are called "thermochromic compounds or substances" or "thermochromic" interchangeably. fifteen

For the purpose of the present invention, "aromatic compound," "aromatic compounds," "aromatics," "indiscriminately," means those substances or components encapsulated in the microparticles of the invention that cause a change in odor on the material in which 20 are present when they are released into the environment.

According to a first aspect, the present invention protects a composition of microparticles containing chromatic and / or aromatic compounds and characterized in that it in turn comprises:

a) a thermochromic or photochromic pigment chosen from the group consisting of pyridinium-phenolate betaines, sulfophthalein structures, Reichhardt dyes, triphenylmethane dyes, pyranines, indicator dyes, azo dyes, leuco dyes and mixtures thereof and / or a selected aromatic compound from group 30 formed by essential oils, essences, fragrances and perfumes,

b) a non-volatile hydrophobic solvent selected from the group consisting of fatty acids, amides and alcohols, and

c) a weak acid that functions as a developer.

Preferably, but not limited to, the leuco dye used in the present invention as a color former in the thermochromic systems of the present invention is selected from the group consisting of spirolactones, fluoranos, spiropyranos, felids and all their derivatives or mixtures. More preferably, it is selected from the group consisting of diphenylmethane derivatives, phenylindolylphthalide phthalate derivatives, indolylphthalide derivatives, diphenylmethane azaftalide derivatives, phenylindolylazaphthalide derivatives, 10 fluorane derivatives, styrynoquinoline derivatives, and lactone-rhodamine derivatives which may include: 3 , 3-bis (p-dimethylaminophenyl) -6-dimethylaminophthalide; 3- (4-diethylaminophenyl) -3- (1-ethyl-2-methylindole-3-yl) phthalamide; 3,3-bis (1-n-butyl-2-methylindole-3-yl) phthalamide; 3,3-bis (2-ethoxy-4-diethylaminophenyl) -4-sazaphtalide; 3- [2-ethoxy-4- (N-ethylanilino) phenyl] -3- (1-ethyl-2-methylindole-3-yl) -4-azaphthalamide; 3,6-dimethoxyfluoran; 3,6-di-n-butoxyfluoran; 2-methyl-6- (N-ethyl-Np-tolylamino) 15 fluoran; 3-chloro-6-cyclohexylaminofluoran; 2-methyl-6-cyclohexylaminofluoran; 2- (2-Chloroanilino) fluoran -6-di-n-butylamino; 2- (3-Trifluoromethylanilino) -6-diethylaminofluorane; 2- (N-Methylanilino) -6- (N-ethyl-Np-tolylamino) fluoran, 1,3-dimethyl-6-diethylaminofluorane; 2-chloro-3-methyl-6-diethylaminofluorane; 2-anilino-3-methyl-6-diethylaminofluorane; 2-anilino-3-methyl-6-di-n-butylamino fluoran; 2-xylidino-3-methyl-6-diethylaminofluorane; 1,2-benzo-6-20 diethylaminofluorane; 1,2-benzo-6- (N-ethyl-N-isobutylamino) fluoran, 1,2-benzo-6- (N-ethyl-N-isoamylamino) fluoran; 2- (3-methoxy-4-dodecoxystyryl) quinoline; spiro [5H- (1) benzopyran (2,3-d) pyrimidine-5,1 '(3'H) isobenzofuran] -3'-one; and 2- (di-n-butylamino) -8- (di-n-butylamino) -4-phenyl and trisubstituted pyridines.

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Preferably but not limitingly, the weak acid used as a color developer acts as a proton donor causing a color to occur when the dye molecule changes between its leuco form and its protonated color form. Preferably, the weak acid used in the present invention is selected from the group consisting of: bisphenol A; bisphenol F; tetrabromobisphenol A; 1'-methylene-2-naphthol; 1,1,1-tris (4-30 hydroxyphenyl) ethane; 1,1-bis (3-cyclohexyl-4-hydroxyphenyl) cyclohexane; 1,1-bis (4-hydroxy-3-methylphenyl) cyclohexane; 1,1-bis (4-hydroxyphenyl) cyclohexane; 1,3-bis [2- (4-hydroxyphenyl) -2-propyl] benzene; 1-naphthol; 2-naphthol; 2,2 bis (2-hydroxy-5-biphenylyl) propane; 2,2-bis (3-cyclohexyl-4-hydroxy) propane; 2,2-bis (3-sec-butyl-4-hydroxyphenyl) propane; 2,2-bis (4-hydroxy-3-

isopropylphenyl) propane; 2,2-bis (4-hydroxy-3 methylphenyl) propane; 2,2-bis (4-hydroxyphenyl) propane; 2,3,4-trihydroxydiphenylmethane; 4,4 '- (1,3-dimethylbutylidene) diphenol; 4,4 '- (2-ethylidene) diphenol; 4,4 '- (2-hydroxybenzylidene) bis (2,3,6-trimethylphenol); 4,4'-biphenol; 4,4'-dihydroxydiphenyl ether; 4,4'-dihydroxydiphenylmethane; 4,4'-methylidenebis (2-methylphenol); 4- phenol (1,1,3,3-tetramethyl-butyl); 4-phenylphenol; 4-tert-butylphenol; 9,9-bis (4-hydroxyphenyl) fluorine; 4,4'-5 (ethane-1,1-diyl) diphenol; alpha, alpha'-bis (4-hydroxyphenyl) -1,4-diisopropylbenzene; alpha, alpha, alpha'-tris (4-hydroxyphenyl) -1-ethyl-4-isopropylbenzene; benzyl 4-hydroxybenzoate; bis (4-hydroxyphenyl) sulfide; bis sulfone (4-hydroxyphenyl); Propyl 4-hydroxybenzoate; Methyl 4-hydroxybenzoate; resorcinol; 4-tert-butyl-catechol; 4-tert-butyl-benzoic; 1, f-methylene-2-naphthol 1,1,1-tris (4-hydroxyphenyl) ethane; 1,1-bis (3-cyclohexyl-4-hydroxyphenyl) cyclohexane; 1,1-bis (4-hydroxy-3-10 methylphenyl) cyclohexane; 1,1-bis (4-hydroxyphenyl) cyclohexane; 1,3-bis [2- (4-hydroxyphenyl) -2-propyl] benzene; 1- naphthol 2,2'-biphenol; 2,2-bis (2-hydroxy-5-biphenylyl) propane; 2,2-bis (3-cyclohexyl-4-hydroxyphenyl) propane; 2,2-bis (3-sec-butyl-4-hydroxyphenyl) propane; 2,2-bis (4-hydroxy-3-isopropylphenyl) propane; 2,2-bis (4-hydroxy-3-methylphenyl) propane; 2,2-bis (4-hydroxyphenyl) propane; 2,3,4-trihydroxydiphenylmethane; 2- naphthol; 4,4 '- (1,3-dimethylbutylidene) diphenol; 4,4 '- (2-ethylhexylidene) diphenol 4,4' - (2-hydroxybenzylidene) bis (2,3,6-trimethylphenol); 4,4'-biphenol; 4,4'-dihydroxydiphenyl ether; 4,4'-dihydroxydiphenylmethane; 4,4'-ethylidenebisphenol; 4,4'-methylenebis (2-methylphenol); 4- phenol (1,1,3,3-tetramethyl-butyl); 4-phenylphenol; 4-tert-butylphenol; 9,9-bis (4-hydroxyphenyl) fluorine; alpha, alpha'-bis (4-hydroxyphenyl) -1,4-diisopropylbenzene; α, α, α-tris (4-hydroxyphenyl) -1-ethyl-4-isopropylbenzene; Benzyl 4-20 hydroxybenzoate; sulfidem bis (4-hydroxyphenyl); methyl bis (4-hydroxyphenyl) sulfone 4-hydroxybenzoate; resorcinol; tetrabromobisphenol A; 3,5-di-tert-butyl-salicylic acid; zinc 3,5-di-tertbutylsalicylate; 3-phenyl-salicylic acid; 5-tert-butyl salicylic acid; 5-n-octyl-salicylic acid and 2,2'-biphenol; 4,4'-di-tert-butyl-2,2'-biphenol; Alkyl-4,4'-di-n-2,2'-biphenol; and 4,4'-di-halo-2,2'-biphenol, wherein the halogen is chlorine, fluorine, bromine, or iodine. 25

Preferably, the thermochromic pigment or dye is pH sensitive and more preferably is from the spirolactone family.

Preferably, the thermochromic pigment or dye is a substance that is supplied in a solid state, specifically in powder form.

According to another important aspect, the invention also relates to a chemical composition comprising the microparticle composition described above for coating metal surfaces.

According to another important aspect, the chemical composition comprises the composition 5 of microparticles described above, a conventional non-chromatic pigment and a coating layer selected from the group consisting of dyes, paints or varnishes.

According to another aspect, the chemical composition allows changing the physicochemical properties of the surface or material in which it is added thanks to the release of the content of the microparticles and the behavior of the effect is reversible or irreversible.

According to another aspect, the present invention relates to a process for achieving a chemical composition with a chromatic or flavoring effect when applied on a metal surface, comprising the steps of:

a) Weigh a first component (1) and a second component (2) separately comprising said first component (1) a composition of microcapsules containing at least one thermochromic pigment, a photochromic pigment or an aromatic substance, in which the second component (2) is a binding agent 20

b) Pour the second component (2) into a container, add the first component (1), and mix by rotation until a homogeneous and lump free mixture is obtained, and

c) Grind the mixture until it is homogeneous and fluid. 25

According to an important aspect of the process described above, the first component (1) is in a proportion of 1 to 50% by weight with respect to the second component (2).

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According to an important aspect, the binding agent can be aqueous (water based), solvent (solvent based), and even without solvents, UV curing.

According to an important aspect of the procedure described above, the thermochromic pigment is of the leuco type.According to an important aspect of the procedure described above, the photochromic pigment is chosen from the group consisting of pyridinium-phenolate betaines, sulfophthalein structures, Reichhardt dyes, triphenylmethane dyes. , pyranines, indicator dyes, azo dyes, leuco dyes and their 5 mixtures. Preferably, the photochromic pigment is leuco and is selected from the group consisting of spirolactones, fluoranos, spiropyranos, felids and all its derivatives or mixtures.

According to an important aspect of the process described above, the aromatic compound 10 is selected from the group consisting of essential oils, essences, fragrances and perfumes or any other element that manifests an olfactory sensation.

According to an important aspect of the process described above, the mixing time is between 5 and 25 min and at a mixing speed between 750 and 1500 rpm using any means of mechanical agitation and the milling is carried out with a mill operating at a pressure between 1 and 5 bars, The milling or grinding process of the present invention can be carried out with a three-cylinder mill, a ball mill, a pearl mill, a sand mill, or any other type of mill that prevents the destruction of the microparticles during the milling process; Since any milling system that has an element that provides the necessary speed and force (either by cylinders, discs, bars, balls, etc.) to achieve separation without breaking the microparticles, can be used herein invention.

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In accordance with a final aspect, the present invention protects a composition for coating metal parts with thermochromic, photochromic and / or flavoring effects, obtained from the procedure described above, for use in packaging of products for cosmetics, perfumery or decoration.

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The composition for coating parts of the present invention can be present in various types of coatings, be they paint, ink, varnish, and these in turn, in different bases, solvent base, water base, and solvent-free (technology of cured

UV). They may also differ in the application method, air gun, spray, screen printing, pad printing.

The thermochromic pigments of the present invention are composed of three phases: a thermochromic phase or thermochromic dye, a color developer and an organic solvent where the dye and the developer are joined. 5

The thermochromic phase is in the form of a microcapsule called pigments. The microcapsule is round and its measurement is between 3 and 7 microns in the inner part, where the thermochromic compounds are found and the outer part of the particle is a transparent skin between 0.2 and 0.5 microns thick which is insoluble 10 and it does not melt, so it can protect thermochromic compounds from the invasion of water and other chemicals.

The thermochromic dye is pH sensitive and the most commonly used belong to the family of spirolactones that exhibit thermochromism through molecular change. fifteen

The developer is a weak acid that produces an opening of the discolored lactone ring to give the colored form, donating a proton. The non-volatile hydrophobic solvent, the most frequent are fatty acids, amides and alcohols.

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Leuco pigments are microencapsulated in a layer of protective polymer. Each microcapsule contains the entire system necessary to reproduce color changes. These pigments are 10 times larger than conventional pigment particles, are completely inert and insoluble and show dispersion problems. 25

Thermochromic pigments do not change temperature promptly, but in a range between 4 to 6 ° C. The color-temperature curve of the processes of hot and cold temperatures are not coincidental and usually when defining the temperature of a thermochromic pigment the heating method is taken into account (change from solid state to liquid state of the varnish of the microcapsule)

The color change temperature is not the same if it is passed from a hot to a cold state or vice versa, which makes thermochromic pigments not very precise to the

When indicating a given temperature, For example, there are thermochromic pigments with a nominal temperature of 40 ° C however these change color between 37 ° C and 43 ° C in a cooling cycle and between 43 ° C and 46 ° C in a heating cycle.

The heating and cooling cycles do not have to end in the same place where they started which means that in each cycle the initial color changes a little, which makes each ink have a certain number of life cycles being better when less change color in each cycle.

Thermochromic pigments change color at a certain temperature range, and go from having color to be transparent. 10

To make visible color changes, we need to add more thermochromic pigments or add conventional pigments, that is, pigments that do not change color and remain invariable at temperature. Therefore we can have from a mixture of a chromic pigment plus a conventional pigment to the mixture of up to 4 chromic pigments with a conventional one and even more possible combinations.

The thermochromic pigments of the present invention can be present in various types of coatings, be they paint, ink, varnish, and these in turn, in different bases, solvent base, water base, and solvent-free (UV curing technology). They can also differ in the application method, air gun, spray, screen printing, pad printing.

The final product on which the composition of the invention is applied will be used to form aluminum pieces with thermochromic effect, it is intended for the cosmetic, perfume and decoration sector. The functionalities can be those derived from the change, or 25 color changes of the coating on the piece in question. They can be mere aesthetic function, excessive temperature warning, product temperature conservation notice, etc.

EXAMPLES OF EMBODIMENT 30

The following specific examples provided herein serve to illustrate the nature of the present invention. These examples are included for purposes only.

illustrative and should not be construed as limitations to the invention claimed herein.

Example 1: Obtaining a composition of blue microparticles

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The present example relates to obtaining a microparticle composition according to the present invention consisting of the following essential steps:

a) Preparation Solution A. 2% of sodium alginate and 0.7% of an aqueous solution of water-soluble cationic urea resin (Uramine® P-10 1500) is dispersed in 100 grams of water.

b) Preparation Solution B. A solution is prepared containing 2.3% of the blue Pergascript Azul® dye (BASF-CAS No. 1552-42-7), 10.25% of bisphenol A, 8.25% of ethyl palmitate and 79% glycerol trilaurate. fifteen

c) Solution B is poured into solution A with constant stirring (5,550 rev / min) for about two minutes, then slowly add a solution of 25 grams of a 25% solution of melamine-formaldehyde and 75% water. The resulting emulsion is slowly stirred (700 rev / min), and kept in a water bath for 8 hours. After cooling, the suspension of the microcapsules object of the present invention is obtained.

Example 2: Preparation thermochromic coating

The thermochromic pigment is a substance that is supplied in solid state (powder). The difficulty is found in the dispersion of the latter in the medium and / or coating (paint, varnish, ink).

The researchers of the present invention have managed to disperse these thermochromic pigments in solvent and UV screen printing inks, by means of a three-cylinder mill and obtain thermochromic screen printing inks. Basically it consists of grinding the thermochromic pigment next to the transparent ink, or with some background color, in order to disperse through the continuous passage of the mixture through the cylinders (rollers) making it

finer and more homogeneous, without granules. The same can be done with other types of coatings, varnishes, paints, etc.

One of the selected screen printing inks is a two-component anodized aluminum and aluminum ink based on solvent. The trade name is MARAPOL-PY® 5 of the Marabú company. The mixing proportions depend on the covering power and the maximum amount allowed by the coating so as not to lose its basic properties of Appearance, Adhesion, Coloring, Abrasion resistance, Chemical resistance and its own coating properties. But they range from 1-50% thermochromic pigment with respect to the coating (by weight). 10

Example 3: Conformational and surface preparation of aluminum

3.1. Drawing process

To shape the product that will be screen printed, a process called 15 drawing has been used. Drawing is the mechanical process by which a piece of metal is shaped. In this example, it has split from an aluminum plate. With the help of special presses, it is gradually being shaped until the final product is obtained. Through this process pieces of different shapes, marks and edges are achieved:

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• Shapes: cylindrical, rounded, square, oval, flat

• Brands: logos, letters, shapes, tall and bas-relief.

• Edges: not sharp or bent

In addition, applying complementary decorative techniques such as: 25

• Die cut

• Side engravings: letters and frets

• Threads

• Beads and grooves 30

• Graffiti and borders

• Pickaxes

• Mechanical polishing

• Sandblasting

3.2. Anodizing process

Before describing the anodizing process, it should be noted that depending on the nature of the thermochromic coating, this can be applied without the need for anodizing. An example can be a protective paint with thermochromic pigments since it would meet the objectives of anodizing.

That said, the anodizing process has two objectives: 10

• The first is the protection of aluminum against external aggressions such as natural oxidation, deterioration of the appearance by scratches and rubbing, among others, since the piece has no protection.

• The second is the aesthetic function. Since this procedure allows different surface finishes and different colors to be obtained through variations in the process itself.

The process is composed of different phases:

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1. Degreasing the piece: It consists in the elimination of the oil from the drawing process.

2. Chemical or electrolytic polishing: It consists in leveling the surface structure of aluminum to obtain a specular surface where the reflection of light is maximum and therefore a great brilliance can be obtained. The process can be obtained by a chemical reaction of inorganic acids at temperature, called chemical polishing, or by an electrochemical reaction also of inorganic acids, called electrochemical polishing.

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3. Satin or tinted: Unlike point 2, when you want to obtain a nuanced or satin finish on the piece, the surface is attacked with alkaline substances, or others, whose function is to give a rough finish on the surface where the light will be reflected

in a diffuse way, obtaining, through variables applied to the treatment bath, different degrees of shading.

4. Oxidation: It consists of the formation, by means of an electrolytic process using continuous current in a solution of sulfuric acid, a layer of aluminum oxide on the surface of the piece that meets two previously mentioned objectives:

 Protection: Due to the same hardness of this layer of aluminum oxide, the surface is protected against the possible effects of bumps and scrubbing and therefore remains unaltered against small manipulations.

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 Aesthetics: The porosity that this layer of aluminum oxide possesses makes it suitable for coloring, a desired aesthetic finish for many of the products of perfumery, cosmetics or high-end, and decoration.

5. Sealing: It consists in making the properties of the aluminum oxide layer 15 formed in the previous phase durable. Its effect is to close or seal the pores produced, both to keep the surface unalterable to contamination of the pores and to prevent the loss of the color deposited therein. The closure of these pores is obtained by chemical solutions or high temperature water to give rise to the formation of large hydrated molecules on the pores that facilitate their sealing. twenty

6. Rinse: Between the different phases, the corresponding rinses are made with deionized water that prevent contamination by dragging from one bath to the other.

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7. Drying: It is the last phase of the process where the drying of the pieces in ovens with air and temperature is achieved.

When reference is made to the term "final application" in the present invention, it refers to the application of the thermochromic coating described above, in the anodized or un-anodised aluminum piece.

Example 4: Final application of the composition to a metallic material

The final application will depend a lot on the nature of the coating and the desired final finish. For example, a thermochromic paint can be applied by brush, brush, roller, spray gun, etc.

Different tests have been carried out with different coatings, basically with paint 5 initially, and today we focus on thermochromic screen printing inks.

The application of thermochromic screen printing ink does not differ from the technology used in a conventional screen printing ink.

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Example 5: obtaining blue thermochromic ink

The preparation process consists of two distinct phases:

• Initial mixing of the thermochromic resin and pigment (microcapsules) by means of a helix agitator. fifteen

• Grinding of the resulting mixture.

Initially, the resin with the trade name MARAPOL-PY® 910 and the commercial thermochromic pigment called “Thermochromique BLUE REFLEX” are supplied by Geminnov laboratories that can range in proportions from 99% to 1% up to (99% of 20 MARAPOL PY910 - 1 resin % Pigment) up to 50% -50%, respectively. The resin is epoxy and therefore the corresponding catalyst or hardener must be added at the time of application. The proportions depend on the covering power of the pigments used and obviously on the desired coverage.

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The thermochromic pigment of the present example is blue in color and its change temperature is in the range of -15 ° C to 80 ° C. Mixing is done using a standard propeller stirrer. This phase has the objective of wetting and dispersing the pigment correctly, and of making a homogeneous paste. The duration is between 5-25 minutes at a speed of 750rpm-1500rpm. The amount that can be done orientatively, is a kilo of ink for a 10 cm shovel.

Once a homogeneous paste is obtained, without lumps, or incorporated air, it is milled in a three-cylinder mill in order to obtain a fluid ink with a fineness of between 3-10 microns (the measurement is made by grindometer).

The mill consists of three cylinders (rollers) in a horizontal position. Each cylinder rotates in a direction opposite to the adjacent cylinder with a small space between them, creating a large shear force that can finely disperse, mix, homogenize refine viscous materials as is the case with our mix. The force at which we have done this example ranges from 1 to 5 bars, and the space between cylinders, enough not to break the microcapsules. The ink is only passed once, at a production speed of 10 kg / h with 35 cm cylinders.

At this point we already have the thermochromic ink composed of a single blue thermochromic pigment. Now we only have the application using the screen printing technique. As we have mentioned before, the ink is epoxy, and needs a catalyst and / or hardener to obtain the desired printing properties. To perform application tests, a container has been taken and 100 g of the blue thermochromic ink and 10 g of Hardener H1 (concentration: 10% by weight with respect to the weight of the thermochromic ink) have been mixed. The H1 Hardener is a commercial reference of the manufacturer Marabu and is formaldehyde at a concentration of 10% by weight in water. 20 Subsequently we have homogenized the mixture with a simple spatula and slow solvent has been added to obtain the optimum viscosity, all without stopping to remove the resulting mixture. Both the Hardener and the solvent are from the Marabú supplier.

At this point, screenprints can now be made. The pieces have been made 25 with 150 weft, and oven dried 60-90 ° C for 5 to 10 minutes. Two finishes have been selected in the final piece, glossy and satin.

To verify its functionality, parts have been put in an oven, and we have observed its correct color change. In this specific case, the blue thermochromic color has disappeared, and has turned white-transparent, since we do not have a background color.

Example 5: Garnet Thermochromic Ink

As in the previous example, the preparation process consists of two distinct phases:

 Initial mixing of the thermochromic resin and pigment (Microcapsules) by means of a propeller stirrer. 5

 Grinding of the resulting mixture.

Initially, the commercial ink "MARAPOL Bright Red PY035" and the commercial thermochromic pigment called "Thermochromique BLUE REFLEX" are supplied by Ge-10 minnov in proportions that can range from 99% "MARAPOL Bright Red PY035" resin - 1% Pigment "Thermochromique BLUE REFLEX ”up to 50% -50%. The thermochromic pigment in question is blue and its approximate exchange temperature is between -15ºC to 80ºC. Mixing is done using a standard propeller stirrer. This phase has the objective of wetting and dispersing the pigment correctly, and making a homogeneous paste. The duration is between 5-25 minutes at a speed of 750rpm-1500 rpm. The quantity that can be done orientatively, is a kilo of ink for a 10 cm shovel.

Once we have a homogeneous paste, without lumps, or incorporated air, we will proceed to grind it in a three-cylinder mill in order to obtain a fluid ink with a fineness of between 3-10 microns (the measurement is made using a grindometer ). The mill consists of three cylinders (rollers) in a horizontal position. Each cylinder rotates in a direction opposite to the adjacent cylinder with a small space between them, creating a large shear force that can finely disperse, mix, homogenize refine viscous materials as is the case with our mix. The force at which we have performed the test ranges from 25 1 to 5 bars, and the space between cylinders, enough not to break the microcapsules. The ink is only passed once, at a production speed of 10 kg / h with 35 cm cylinders.

A fluid garnet color (Red + Blue) has been obtained, that is, we already have the garnet thermochromic ink 30 composed of two pigments, one blue thermochromic and the other conventional red. Now we only have the application using the screen printing technique. As we mentioned before, the ink is epoxy, and it needs a catalyst and / or hardener to obtain the desired printing properties.

To carry out application tests, we have taken a container and mixed 100 g of garnet thermochromic ink and 10 g of H1 Hardener (formaldehyde, concentration: 10% by weight in water), then we have homogenized the mixture with a simple spatula and slow solvent has been added to obtain the optimum viscosity, all while stirring the resulting mixture. Both the Hardener and the solvent are from the Marabú supplier.

At this point, we are ready to make screen-printed pieces. The pieces have been made with 150 weft, and oven dried 60-90 ° C for 5-10 minutes. We have selected two finishes in the final piece, glossy and satin. 10

To verify its functionality, we have put pieces in an oven, and we have observed its correct color change. In this specific case, the blue thermochromic color has disappeared, and has turned garnet to red, the color of the conventional pigment.

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Example 6: Violet Thermochromic Ink

We have produced this thermochromic ink from the Blue thermochromic ink. We have taken a container and mixed 100 g of the blue thermochromic ink, 10 g of Endu-receiver H1 (10% by weight), and 5 g of “transparent Vivo red ink”, then we have homogenized the mixture with a simple spatula and slow solvent has been added to obtain the optimum viscosity, all while stirring the resulting mixture. Both the Hardener and the solvent are from the Marabú supplier. The proportions may vary depending on the covering power and color to be obtained.

 25

"Vivid red ink" is made by a conventional pigment with very little covering power.

At this point, we are ready to make screen-printed pieces. The pieces have been made with 150 weft, and oven dried 60-90 ° C for 5-10 minutes. We have selected two finishes in the final piece, bright and satin.

To verify its functionality, we have put pieces in an oven, and we have observed its correct color change. In this specific case, the blue thermochromic color has disappeared, and has turned from Violet to pink, the color of the conventional pigment.

Example 7: Obtaining a green thermochromic ink

 5

We have produced this thermochromic ink from the Blue thermochromic ink, in the same way as in the previous example. We have taken a container and mixed 100 g of the blue thermochromic ink, 10 g of Hardener H1 (formaldehyde, concentration: 10% by weight in water) and 5 g of “yellow ink”, then we have homogenized the mixture with a simple spatula and slow solvent has been added to obtain the optimum viscosity, all while stirring the resulting mixture. Both the Hardener and the solvent are from the Marabú supplier.

At this point, we are ready to make screen-printed pieces. The pieces have been made with 150 weft, and oven dried 60-90 ° C for 5-10 minutes. We have selected a satin finish. To check its functionality, we have put pieces in an oven, and we have observed its color change. In this specific case, the blue thermochromic color has disappeared, and has turned the color of the conventional pigment from Green to yellow.

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Example 8: Obtaining a photochromic or white pigment

Photochromic pigments are those that change color when exposed to a UV source or sunlight. The change is reversibly, when it ceases to be irradiated, it loses the color progressively, until its total absence of color. Photo-25 chromic pigments are also pigments called "Leuco".

The preparation process consists of two distinct phases:

• Initial mixing of the resin and photochromic pigment (Microcapsules) using a propeller shaker.

• Grinding of the resulting mixture.

Initially, the “MARAPOL PY 910” resin and the photochromic pigment supplied by Geminnov commercially called “Photochromique MAGENTA” are mixed, which can be in proportions of 99% “MARAPOL PY910” resin - 1% “Photochromique MA-GENTA” pigment until 50% -50% respectively. The resin is epoxy and therefore, at the time of application, the corresponding catalyst or hardener 5 must be added for screen printing. The proportions depend on the covering power of the pigments used and obviously on the desired coverage. Mixing is done using a standard propeller stirrer. This phase aims to wet and disperse the pigment correctly, and make a homogeneous paste. The duration is between 5-25 minutes at a speed of 750 rpm-1500 rpm. The quantity that can be done orientatively, is a 10 kilo (1 kg) of ink for a 10 cm shovel.

Once we have a homogeneous paste, without lumps, or incorporated air, we will proceed to grind it in a three-cylinder mill in order to obtain a fluid ink with a fineness between 3-10 microns (the measurement is made using a grindometer) . fifteen

The mill consists of three cylinders (rollers) in a horizontal position. Each cylinder rotates in a direction opposite to the adjacent cylinder with a small space between them, creating a large shear force that can finely disperse, mix, homogenize refine viscous materials as is the case with our mixture. The force at which the test was performed ranges from 1 to 5 bars, and the space between cylinders must be sufficient not to break the microcapsules. The ink is only passed once, at a production speed of 10 kg / h with 35 cm cylinders.

Example 9: obtaining a microparticle composition with aromatic compounds

Specifically, the microparticles of this example are microcapsules that release aromas (odor) that basically consist of the encapsulation of essential oils for their subsequent release. The release occurs through the application of a mechanical friction (a friction or rubbing force), producing the release of the fragrance upon breaking-30 the microcapsule. That causes life to be very short, in addition to damaging the coating. The microcapsules we use in this invention do not break. Friction creates an increase in the pressure inside the microcapsule, causing vapors of the fragrance to be released through it. The steam released is replaced by oxygen. This supposes

hundreds of cycles These microcapsules are made of melamine, and have two layers, while the standards are made of gelatin.

The fragrances that have been tested in the present example are:

 5

• Lavender

• Freshly cut grass

• Strawberry

• orange

• Chocolate 10

• Vanilla

• Coffee

 The preparation process consists of two distinct phases:

 fifteen

• Initial mixing of the resin and microencapsulated fragrance by means of a propeller stirrer.

• Grinding of the resulting mixture

The commercial resin “MARAPOL PY 910” and the commercial co-20 fragrance supplied by Geminnov are initially mixed, which can go in proportions of 99% “MARA-POL PY910” resin - 1% Microencapsulated Fragrance ”up to 50% -50% . The resin is epoxy and therefore the corresponding catalyst or hardener must be added at the time of application. Mixing is done using a standard propeller stirrer. This phase has the objective of wetting and dispersing the microcapsules correctly, and making a homogeneous paste. The duration is between 5-25 minutes at a speed of 750 rpm-1500 rpm. The quantity that can be done orientatively, is a kilo (1 kg) of ink for a 10 cm shovel.

Once a homogeneous paste is obtained, without lumps, or incorporated air, the milling is carried out in a three-cylinder mill in order to obtain a fluid ink with a fineness of between 3-10 microns (the measurement is made by a grindometer) .The mill consists of three cylinders (rollers) in a horizontal position. Each cylinder rotates in one direction

opposite to the adjacent cylinder with a small space between them, creating a large shear force that can finely disperse, mix, homogenize refine viscous materials such as our mix. The force at which the example has been carried out ranges from 1 to 5 bars, and the space between cylinders must be sufficient not to break the microcapsules. The ink is only passed once, at a production speed of 10 kg / h 5 with 35 cm cylinders.

Example 10: obtaining a composition of microparticles with a mixture of different compounds: aromatic, photochromic and / or thermochromic.

 10

All microcapsules with their thermochromic, photochromic effects, perfumes and / or fragrances are fully compatible. Therefore their mixtures can result in special coatings.

For example, a mixture of blue thermochromic microcapsules, conventional yellow pigment, and microencapsulated banana fragrance can be had. In such a way that when rubbing the green-looking material, the blue thermochromic pigment disappears due to the temperature rise, and only the yellow color is observed, and in turn the banana fragrance is released.

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For the purpose of the present invention, different suppliers of micropar- ticles have been used whose processes for preparing and obtaining them are known in the state of the art. The manufacturers of thermochromic microcapsules include, but are not limited to, QCR Solutions Corporation (Port St. Lucie, Fla., US), Woo Jeong Ind. Inc. (Seoul, South Ko-rea), HW Sands Corp. (Jupiter, Fla., US), Devine Chemicals (Consett, England, UK), Chemi-25 cal Plus (Bangkok, Thailand), and PMC Chemicals Limited (Altrincham, England, UK).

Claims (18)

1. A composition of microparticles containing chromatic and / or aromatic compounds characterized in that it comprises:  5 a) .- a thermochromic or photochromic pigment chosen from the group consisting of pyridinium-phenolate betaines, sulfophthalein structures, Reichhardt dyes, triphenylmethane dyes, pyranines, indicator dyes, azo dyes, leuco dyes and mixtures thereof and / or a flavoring agent selected from the group consisting of essential oils, essences, fragrances and perfumes; 10 b) .- a non-volatile hydrophobic solvent selected from the group consisting of fatty acids, amides and alcohols, and c) .- a weak acid that functions as a developer. fifteen 2. A microparticle composition according to claim 1 characterized in that the thermochromic pigment is pH sensitive and is a substance that is supplied in powder form.  twenty 3. A microparticle composition according to claim 1 characterized in that the thermochromic pigment is selected from the group consisting of spirolactones, fluoranos, spiropyranos, felids and all its derivatives or mixtures. 4. A chemical composition comprising the microparticle composition of claims 1 to 3 for coating metal surfaces. 5. Chemical composition according to claim 4 characterized in that it comprises the microparticle composition of any one of claims 1 to 3, a conventional non-chromatic pigment and a coating layer selected from the group consisting of 30 dyes, paints or varnishes. 6. Chemical composition according to claim 4 characterized in that it allows to change the physicochemical properties of the surface or material in which it is added thanks to the release of the content of the microparticles. 7. Chemical composition according to any of the preceding claims characterized in that the effect behavior is reversible or irreversible 8. A process for achieving a chemical composition with a chromatic or flavoring effect when applied on a metal surface, characterized in that it comprises the steps of: a) Weigh a first component (1) and a second component (2) separately comprising said first component (1) a composition of microcapsules containing at least one thermochromic pigment, a photochromic pigment or an aromatic substance, in which the second Component (2) is an aqueous binder component. b) Pour the second component (2) into a container, add the first component (1), and mix by rotation until a homogeneous and lump free mixture is obtained, and  twenty c) Grind the mixture until it is homogeneous and fluid. 9. Method for the preparation of a coating according to claim 8, characterized in that the first component (1) is in a proportion of 1 to 50% by weight with respect to the second component (2). 25 10. Process for the preparation of a composition according to claim 8, characterized in that, because said thermochromic pigment is of the leuco type. 11. Method for the preparation of a composition according to claims 30 8 and 10, characterized in that the microcapsules contain at least one photochromic pigment, of the leuco type selected from the group consisting of spirolactones, fluoranos, spiropyranos, felids and all its derivatives or mixtures 12. Method for preparing a composition according to claim 8, characterized in that the microcapsules contain at least one flavoring compound selected from the group consisting of essential oils, essences, fragrances, perfumes or any flavoring agent.  5 13. Method for preparing a composition according to claim 8 characterized in that the mixing time is between 5 and 25 min and at a mixing speed between 750 and 1500 rpm using any means of mechanical agitation.  10 14. Method for the preparation of a composition according to claim 8 characterized in that the milling is carried out with a mill operating at a pressure between 1 and 5 bars. 15. Process for the preparation of a composition according to any one of claims 15 to 14, characterized in that the milled mixture obtained for coating parts of the present invention is in the form of paint, ink or varnish. 16. Process for the preparation of a composition according to any of claims 8 to 14 characterized in that the milled mixture obtained for coating parts of the present invention is solvent based, water based, or solvent free. 17. Composition for coating metal parts with thermochromic, photochromic and / or flavoring effects, obtained from the procedure described in claims 8 to 16, for use in packaging of products for cosmetics, perfumery or decoration. 18. Composition for coating metal parts with thermochromic, photochromic and / or flavoring effects, obtained from the procedure described in 30 claims 8 to 16, characterized in that it is applied on the parts with an air spray gun, with spray, with techniques screen printing or pad printing techniques.