KR101854856B1 - Method for preparing pearlescent pigment coating organic fluorescence for security and safety applications - Google Patents
Method for preparing pearlescent pigment coating organic fluorescence for security and safety applications Download PDFInfo
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- KR101854856B1 KR101854856B1 KR1020160067065A KR20160067065A KR101854856B1 KR 101854856 B1 KR101854856 B1 KR 101854856B1 KR 1020160067065 A KR1020160067065 A KR 1020160067065A KR 20160067065 A KR20160067065 A KR 20160067065A KR 101854856 B1 KR101854856 B1 KR 101854856B1
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/62—Metallic pigments or fillers
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C2210/00—Special effects or uses of interference pigments
- C09C2210/50—Fluorescent, luminescent or photoluminescent properties
Abstract
More particularly, the present invention relates to a method for producing a security pigment, which comprises the steps of (a) preparing an organic binder solution containing organic phosphor particles, (b) mixing a flake substrate and a solvent, And (c) coating the organic phosphor particles on the surface of the flake substrate by mixing the substrate suspension and the organic binder solution to form a security pigment having both aesthetic effect and security characteristics at the same time And a manufacturing method that can be provided.
Description
The present invention relates to a method for producing a security pigment and a security pigment produced thereby. More specifically, the present invention relates to a security pigment prepared by using the organic phosphor as a pigment, To a method for producing a security pigment.
Imitation and anti-counterfeiting have become increasingly important for all types of products as well as proprietary products of recent high value-added. In particular, medicines and machine replacement parts are part of a product family that is easy to imitate and counterfeit, and consumers are exposed to the environment where they can inadvertently be directly or indirectly damaged.
In order to prevent such imitation and counterfeiting, a variety of printing-based anti-counterfeiting technologies such as a hologram in which the color varies depending on the viewing angle and an intaglio printing on the printing surface are developed using a fine diffractive structure. In addition, Fluorescent inks that exhibit fluorescence at wavelengths, color change inks that change color as temperature changes, magnetic inks that have magnetic properties, and pearl inks that use pearl luster pigments with interfering color effects. These include securities, passports, It is applied to seals used for goods or articles such as packaging of original products and is used for discriminating whether or not a product has been falsified.
However, as counterfeiting techniques of counterfeiters continue to become more sophisticated, technologies with security features that are more difficult to counterfeit are required.
It is an object of the present invention to provide a method for producing a security pigment having both aesthetic effect of a pearlescent pigment and a security characteristic based on fluorescence.
According to an aspect of the present invention, there is provided a method of manufacturing a security pigment, comprising: (a) preparing an organic binder solution containing organic phosphor particles; (b) mixing a flake substrate and a solvent, stirring and dispersing the flake substrate and the solvent to prepare a substrate suspension; And (c) coating the organic phosphor particles on the surface of the flake substrate by mixing the substrate suspension and the organic binder solution.
According to another aspect of the present invention, there is provided a method of manufacturing a security pigment, comprising: (a) preparing a mixed organic solvent containing organic phosphor particles and mixing at least two organic solvents; (b) mixing the mixed organic solvent and the flake substrate and stirring and dispersing the mixed organic solvent to prepare a substrate suspension; And (c) heating and stirring the substrate suspension to coat the organic phosphor particles on the surface of the flake substrate.
The method for producing a security pigment according to the present invention is advantageous in that it can provide a security pigment having security characteristics due to optical characteristics in addition to a unique aesthetic effect of a pearl luster pigment by economical, easy and new process.
1 is a flowchart illustrating a method of manufacturing a security pigment according to an embodiment of the present invention.
2 is a flowchart illustrating a method of manufacturing a security pigment according to another embodiment of the present invention.
3 is an SEM photograph of a security pigment prepared from the manufacturing method according to an embodiment of the present invention.
4 is a SEM photograph of a security pigment prepared from a manufacturing method according to another embodiment of the present invention.
5 is a photograph showing optical characteristics of a security pigment coated with an organic phosphor according to the present invention.
6 is a graph showing emission spectra of a security pigment coated with an organic phosphor according to the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS The advantages and features of the present invention, and the manner of achieving them, will be apparent from and elucidated with reference to the embodiments described hereinafter in conjunction with the accompanying drawings. It should be understood, however, that the invention is not limited to the disclosed embodiments, but is capable of many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, To fully disclose the scope of the invention to those skilled in the art, and the invention is only defined by the scope of the claims. Like reference numerals refer to like elements throughout the specification.
Hereinafter, a method for preparing a security pigment according to the present invention and a security pigment prepared by the method will be described in detail.
1 is a flowchart illustrating a method of manufacturing a security pigment according to an embodiment of the present invention.
Referring to FIG. 1, a method for preparing a security pigment according to the present invention includes the steps of: (a) preparing an organic binder solution including organic phosphor particles (S110); (b) mixing the flake substrate and the solvent, and stirring and dispersing the flake substrate and the solvent to prepare a substrate suspension (S120); And (c) coating the organic phosphor particles on the surface of the flake substrate by mixing the substrate suspension and the organic binder solution (S130).
First, the step (a) (S110) relates to a step of preparing an organic binder solution containing organic phosphor particles.
The organic binder solution used in step (a) may be selected from the group consisting of cellulose, cellulose acetate, polyamide, epoxy resin, polyester, melamine resin, polyurethane, resin vinyl resin, silicon resin, acrylic acid ester, methacrylic acid ester, An organic binder resin containing one or more kinds of polymers or copolymers of styrene, ethylene, propylene, acrylic resins and their derivatives can be used. However, the organic polymer resin used in the present invention is not particularly limited But is not limited to.
In the organic binder solution, the organic polymer resin is preferably included in an amount of 5 to 50 parts by weight based on 100 parts by weight of the organic binder solution. If the amount of the organic polymer resin is less than 5 parts by weight, the required resin adhesiveness may not be obtained. On the other hand, if the amount of the organic polymer resin exceeds 50 parts by weight, the content of the organic polymer resin is too high relative to the amount of the binder resin, And may cause a phenomenon.
The organic phosphor used in the present invention may be an organic phosphor known in the art without any particular limitation, but it is preferable to use an organic phosphor having strong luminescence characteristics for security and safety applications.
The organic phosphor used in the present invention specifically includes tetraphenylnaphthacene (Rubrene), tris (1-phenylisoquinoline) iridium (III) (Ir (piq) 3), bis (dibenzoylmethyl) phenanthroline europium (III) (Eu (dbm) 3 (bp) 2 (acac) (phen), tris [4,4'-di-tert-butyl- (2,2 ') - bipyridine] ruthenium (III) complex (Ru (dtb- bpy) 3 * 2 (PF6) DCM2, Eu (Tetraethyltriethoxysilane) 3 (Eu (TTA) 3, butyl-6- (1,1,7,7-tetramethyljulolidyl-9-enyl) -4H- (1,1,7,7-tetramethyljulolidyl-9-enyl) -4H-pyran: DCJTB), (1,10-phenanthroline) -tris- (4,4,4- - (2-thienyl) -butane-1,3-dionate) 1,10-Phenanthroline tris [4,4,4-trifluoro-1- (2-thienyl) butanedionato] europium (III): Eu (TTA) 3Phen) or the like can be used, and as the polymeric light emitting material Polymers such as phenylene, phenylene vinylene, thiophene, fluorene and spiro-fluorene polymers, and aromatic-containing polymers containing nitrogen Compounds, and the like, but are not particularly limited thereto.
It is preferable that the organic phosphor is included in an amount of 5 to 60 parts by weight based on 100 parts by weight of the organic binder solution. If the amount of the organic phosphor is less than 5 parts by weight, the organic polymer resin and the binder resin may be relatively large in amount relative to the organic phosphor, resulting in poor binding efficiency. If the amount of the organic phosphor is more than 60 parts by weight The amount of the organic polymer resin and the binder resin is relatively small, so that a required binding effect can not be obtained.
The organic binder solution may further contain a dispersant and an antifoaming agent as required.
The dispersant may be any dispersant known in the art and may be used in an amount of 1 to 5 parts by weight based on 100 parts by weight of the organic binder solution. When the dispersing agent is contained in an amount of less than 1 part by weight, the required dispersing effect may not be obtained. When the dispersing agent is contained in an amount exceeding 5 parts by weight, the concentration of the dispersing agent is too high.
The antifoaming agent may be any antifoaming agent known in the art and may be used in an amount of 1 to 5 parts by weight based on 100 parts by weight of the organic binder solution. If the dispersant is contained in an amount of less than 1 part by weight, the required antifoaming effect may not be obtained. If the antifoaming agent is contained in an amount exceeding 5 parts by weight, the concentration of the antifoaming agent may be too high.
In addition, the step (a) (S110) may include: (a1) injecting organic phosphor particles into the organic binder solution; And (a2) pulverizing the organic phosphor particles to prepare an organic binder solution containing nano-sized organic phosphor particles.
The organic phosphor particles may be pulverized by a known grinding method without any particular limitation, but the organic phosphor particles contained in the organic binder solution may be pulverized to an appropriate size by using a milling machine equipped with a milling ball Is preferable in terms of process efficiency.
It is preferable that the organic phosphor particles have a particle size of 10 to 900 nm that is wider than the particle size distribution of 10 to 900 nm. If the particle size of the organic phosphor particles is less than 10 nm, there is no improvement in optical characteristics upon UV irradiation, The adhesion to the flake substrate can be reduced.
Next, the step (b) (S120) is a step of mixing a flake substrate and a solvent and stirring and dispersing the flake substrate and the solvent to prepare a substrate suspension.
The flake substrate is preferably at least one of synthetic mica, natural mica, glass flake, flaky iron oxide, flaky alumina, aluminum flake, flaky silica, talc and bismuth, although it is preferably a plate- May be used.
The flake substrate may also include a flake substrate having one or more metal oxides coated thereon. The metal oxide may be coated on the flake substrate with a single layer or a plurality of layers of various components such as TiO 2 , SiO 2 and Fe 2 O 3 depending on the required pearl characteristics.
The solvent may be an organic solvent known in the art. Specific examples thereof include hydrocarbon solvents such as hexane, octane, decane, isodecane, cyclohexane, methylcyclohexane, toluene, xylene and ethylbenzene; Alcohol solvents such as methanol, ethanol, propanol, isopropanol, butanol, isobutanol, hexanol, benzyl alcohol and cyclohexanol; Propylene glycol monoethyl ether, propylene glycol monopropyl ether, diglyme, propylene glycol monomethyl ether, propylene glycol monomethyl ether, propylene glycol monomethyl ether, ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, methyl cellosolve, ethyl cellosolve, butyl cellosolve, Propylene glycol monomethyl ether acetate, dipropylene glycol butyl ether acetate, diethylene glycol monobutyl ether, diethylene glycol monobutyl ether, diethylene glycol monobutyl ether, diethylene glycol monobutyl ether, diethylene glycol monobutyl ether, Glycol solvents such as acetate; Ether solvents such as diethyl ether, dipropyl ether, methyl cyclopropyl ether, tetrahydrofuran, dioxane and anisole; Ketone solvents such as methyl ethyl ketone, diethyl ketone, methyl isobutyl ketone, cyclohexanone, isophorone and acetophenone; Ester solvents such as methyl acetate, ethyl acetate, butyl acetate, propyl acetate, methyl butyrate, ethyl butyrate, caprolactone, methyl lactate and ethyl lactate; Halogenated solvents such as chloroform and dichloroethane; Amide solvents such as dimethylformamide, dimethylacetamide, 2-pyrrolidone, N-methylpyrrolidone and caprolactam; Dimethyl sulfoxide, sulfolane, tetramethyl urea, ethylene carbonate, propylene carbonate, dimethyl carbonate and the like can be used. However, the kind of the organic solvent used in the present invention is not particularly limited.
The stirring speed in step (b) (S120) is preferably maintained at 100 to 500 rpm. If the stirring speed is less than 100 rpm, the dispersing effect is reduced, and the organic phosphor particles may agglomerate together. If the stirring speed is 500 rpm or more, further dispersion efficiency may be reduced.
Next, the step (c) (S130) is a step of coating the organic phosphor particles on the surface of the flake substrate by mixing the substrate suspension and the organic binder solution.
Here, it is preferable that the pH of the mixed solution is adjusted to a range of 7.0 to 10.0 by using a pH adjusting agent in a mixed solution in which the substrate suspension and the organic binder solution are mixed. If the pH is less than 7.0, aggregation of the particles may occur and the reaction effect may be reduced. If the pH is more than 10.0, the adhesion of the organic phosphor particles may be decreased.
The pH adjusting agent used in the present invention is not particularly limited, but an acidic solution containing one or more selected from among hydrochloric acid, sulfuric acid, acetic acid, acetic acid and the like, which exhibits acidity, may be used.
After step (c), if necessary, (d) washing and dehydrating the flake substrate; (e) drying the washed flake substrate; And (f) separating the flake substrate formed to a size larger than a predetermined size among the dried flake substrates.
The drying step according to the step (e) is preferably carried out at 60 to 180 ° C. If the drying temperature is less than 60 ° C, the drying time may be long and the productivity may be deteriorated. If the drying temperature exceeds 180 ° C, the organic phosphor particles may be damaged and the optical characteristics after drying may decrease.
In the screening step according to the step (f), it is preferable to separate the flake substrate having a particle size exceeding 100 mu m. Further, the step (f) has the effect of removing the aggregated particles formed during the reaction. The screening method of the screening step may be performed using a mesh having a predetermined size, but is not particularly limited thereto.
Hereinafter, a method of manufacturing a security pigment according to another embodiment of the present invention will be described in detail.
2 is a flowchart illustrating a method of manufacturing a security pigment according to another embodiment of the present invention.
Referring to FIG. 2, the method for preparing a security pigment according to the present invention includes the steps of: (a) preparing a mixed organic solvent containing organic phosphor particles and mixing two or more organic solvents; (b) mixing the mixed organic solvent and the flake substrate and stirring and dispersing the mixed organic solvent to prepare a substrate suspension (S220); And (c) heating and stirring the substrate suspension to coat the organic phosphor particles on the surface of the flake substrate (S230).
The step (a) (S210) relates to a step of preparing a mixed organic solvent containing organic phosphor particles and mixing two or more organic solvents.
In the step (a) (S210), the organic solvent may be an organic solvent known in the art, and specifically, hexane, octane, decane, isodecane, cyclohexane, methylcyclohexane, toluene, xylene, Hydrocarbon solvents such as ethylbenzene; Alcohol solvents such as methanol, ethanol, propanol, isopropanol, butanol, isobutanol, hexanol, benzyl alcohol and cyclohexanol; Propylene glycol monoethyl ether, propylene glycol monopropyl ether, diglyme, propylene glycol monomethyl ether, propylene glycol monomethyl ether, propylene glycol monomethyl ether, ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, methyl cellosolve, ethyl cellosolve, butyl cellosolve, Propylene glycol monomethyl ether acetate, dipropylene glycol butyl ether acetate, diethylene glycol monobutyl ether, diethylene glycol monobutyl ether, diethylene glycol monobutyl ether, diethylene glycol monobutyl ether, diethylene glycol monobutyl ether, Glycol solvents such as acetate; Ether solvents such as diethyl ether, dipropyl ether, methyl cyclopropyl ether, tetrahydrofuran, dioxane and anisole; Ketone solvents such as methyl ethyl ketone, diethyl ketone, methyl isobutyl ketone, cyclohexanone, isophorone and acetophenone; Ester solvents such as methyl acetate, ethyl acetate, butyl acetate, propyl acetate, methyl butyrate, ethyl butyrate, caprolactone, methyl lactate and ethyl lactate; Halogenated solvents such as chloroform and dichloroethane; Amide solvents such as dimethylformamide, dimethylacetamide, 2-pyrrolidone, N-methylpyrrolidone and caprolactam; Dimethyl sulfoxide, sulfolane, tetramethyl urea, ethylene carbonate, propylene carbonate, and dimethyl carbonate may be used. However, the type of the organic solvent used in the present invention is not particularly limited, and it is needless to say that other types of organic solvents may be used as needed.
Preferably, the mixed organic solvent includes 50 to 80 parts by weight of acetone, 10 to 30 parts by weight of methanol, 2 to 10 parts by weight of toluene, and 2 to 5 parts by weight of MEK, have.
Needless to say, the organic solvent may contain various additives as needed.
In addition, the organic phosphor used in the present invention may be an organic phosphor known in the art without limitation, but it is preferable to use an organic phosphor having strong luminescence characteristics for security and safety applications.
The organic phosphor used in the present invention specifically includes tetraphenylnaphthacene (Rubrene), tris (1-phenylisoquinoline) iridium (III) (Ir (piq) 3), bis (dibenzoylmethyl) phenanthroline europium (III) (Eu (dbm) 3 (bp) 2 (acac) (phen), tris [4,4'-di-tert-butyl- (2,2 ') - bipyridine] ruthenium (III) complex (Ru (dtb- bpy) 3 * 2 (PF6) DCM2, Eu (Tetraethyltriethoxysilane) 3 (Eu (TTA) 3, butyl-6- (1,1,7,7-tetramethyljulolidyl-9-enyl) -4H- (1,1,7,7-tetramethyljulolidyl-9-enyl) -4H-pyran: DCJTB), (1,10-phenanthroline) -tris- (4,4,4- - (2-thienyl) -butane-1,3-dionate) 1,10-Phenanthroline tris [4,4,4-trifluoro-1- (2-thienyl) butanedionato] europium (III): Eu (TTA) 3Phen) or the like can be used, and as the polymeric light emitting material Polymers such as phenylene, phenylene vinylene, thiophene, fluorene and spiro-fluorene polymers, and aromatic-containing polymers containing nitrogen Compounds, and the like, but are not particularly limited thereto.
The organic phosphor may be included in an amount of 0.1 to 5 parts by weight based on 100 parts by weight of the mixed organic solvent. If the amount of the organic phosphor is less than 0.1 parts by weight, the required optical characteristics may be difficult to develop. On the other hand, if the amount of the organic phosphor is more than 5 parts by weight, the solubility of the organic phosphor is decreased, Problems may arise.
It is needless to say that the step of grinding the organic phosphor particles into nano-sized organic phosphor particles may also be performed in step (a) (S210).
The organic phosphor particles may be pulverized by a known milling method without any particular limitation, but milling equipment equipped with a milling ball may be used to pulverize the organic phosphor particles contained in the mixed organic solvent into an appropriate size Is preferable in terms of process efficiency.
It is preferable that the organic phosphor particles have a particle size of 10 to 900 nm. When the particle size of the organic phosphor particles is less than 10 nm, there is no improvement in the optical characteristics upon UV irradiation. When the particle size exceeds 900 nm, The property can be reduced.
Next, in step (b) (S220), the mixed organic solvent and the flake substrate are mixed and stirred and dispersed to prepare a substrate suspension.
In the step (b), the flake substrate may be contained in an amount of 10 to 50 parts by weight based on 100 parts by weight of the substrate suspension. When the flake substrate is contained in an amount of less than 10 parts by weight, the amount of the flake substrate is too small compared to the reaction liquid, so that the volatilization time of the mixed organic solvent is long and the reaction efficiency can be reduced. When the flake substrate is contained in an amount exceeding 50 parts by weight The amount of flake substrate relative to the reaction liquid is too large to cause agglomeration.
As described above, the flake substrate is not particularly limited as long as it is a plate-like substrate. However, the flake substrate is preferably a synthetic substrate such as synthetic mica, natural mica, glass flake, platelike iron oxide, flake alumina, aluminum flake, A substrate comprising one or more of bismuth may be used.
The flake substrate may also include a flake substrate having one or more metal oxides coated thereon. The metal oxide may be coated on the flake substrate with a single layer or a plurality of layers of various components such as TiO 2 , SiO 2 and Fe 2 O 3 depending on the required pearl characteristics.
Next, the step (c) (S230) is for heating and stirring the substrate suspension to coat the organic phosphor particles on the surface of the flake substrate.
In the step (c), the organic suspension is volatilized by heating and stirring the substrate suspension, whereby the surface of the flake substrate is coated with the organic phosphor particles.
The heating step is preferably performed at a temperature ranging from 40 to 70 ° C. When the heating temperature is lower than 40 ° C, the volatilization rate is slowed to reduce the reaction efficiency. When the heating temperature is higher than 70 ° C, the volatilization rate is too fast, so that the dispersion efficiency may decrease and coagulation may occur. Since the heating step is performed at a relatively low temperature, it is preferable to use an evaporator such as a vacuum distiller.
In the step (c), the agitation speed is preferably 100 to 300 rpm. If the stirring speed is less than 100 rpm, aggregation of the substrate may occur, and if the stirring speed is 300 rpm or more, the dispersion efficiency may be decreased.
After the step (c), (d) a screening step of separating the flake substrate formed in the flake substrate larger than a predetermined size may be further included.
In the screening step, it is preferred to separate the flake substrate with a particle size of greater than 100 mu m. Further, by passing through the screening step, aggregated particles formed during the reaction can be removed. The screening method of the screening step may be performed using a mesh having a predetermined size, but is not particularly limited thereto.
FIG. 5 is a photograph showing optical characteristics of a security pigment coated with an organic phosphor according to the present invention, and FIG. 6 is a graph showing an emission spectrum of a security pigment coated with an organic phosphor according to the present invention.
Referring to FIG. 5, it can be seen that the security pigment coated with the organic phosphor according to the present invention (the "coated" reagent on the right side of the figure) has a luminescence property upon UV light irradiation at 365 nm, (The " before coating " reagent on the right side of the drawing) has no luminescent property.
Also, referring to FIG. 6, the security pigment coated with the organic phosphor according to the present invention has an emission wavelength of 625 ± 30 nm when irradiated with 365 nm UV light, and thus has a unique aesthetic effect, It is possible to provide a security pigment having
The security pigments prepared by the production method according to the present invention described above can be used as authenticity determination objects. As mentioned above, by irradiating the object with ultraviolet rays, the authenticity of the object can be discriminated by recognizing the phosphor.
In addition, the security pigment manufactured by the manufacturing method according to the present invention can be used not only as a financial document such as a bank note, a check, a credit card, a stock, a passport, an ID card, a driver's license, a ticket, a stamp, a label, a packing material, Security pigments can be used in protected products such as clothing, shoes, household goods, consumer electronics, etc., which are applied directly to the product.
In particular, the security product to which the security pigment according to the present invention is applied may have any one of a paint, a coating, a powder coating, a printing ink, a coating composition, a plastic, an adhesive, a paper stock, The security pigment preferably has a content range of from 0.01 to 30% by weight based on the total weight of the security product.
In addition, the security document to which the security product is applied includes a banknote, a check, a bank credit card, a check card, a security certificate, an identification card, a certificate, an import notification, a stamp, an identification card, a train and airplane ticket, A test stamp and a packaging material, and the form of the security document is not particularly limited.
Hereinafter, the present invention will be described in more detail with reference to Examples of the present invention, but the scope of the present invention is not limited by the following Examples.
≪ Example 1 >
1. Preparation of Organic Binder Solution Containing Organic Phosphor Particles
36 g of an acrylic organic binder resin, 43 g of primary distilled water, 0.5 g of a dispersing agent and 0.5 g of a defoaming agent were charged in a 250-ml beaker, followed by stirring for 1 hour or longer using a magnetic bar. After mixing the binder solution with stirring, 20 g of Eu (TTA) 3Phen series organic fluorescent material was added, followed by stirring for 1 hour using a magnetic bar.
The organic binder solution prepared in the above procedure is put into a 250 ml PE bottle for ball milling together with 450 g of ZrO 2 Ball and milled for 35 to 72 hours using a milling machine.
2. Preparation of a security pigment comprising a flake substrate coated with organic phosphor particles
50 g of flaky alumina substrate and 450 g of methanol were charged into a 1 L beaker and stirred and dispersed at 20 to 25 캜 at 300 rpm to form a substrate suspension. Next, 12.5 g of the organic binder solution was titrated to the above substrate suspension using a pump. After the titration was completed, 5% hydrochloric acid solution was added to the mixed suspension of the substrate suspension and the organic binder solution to adjust the pH to 7.0. Thereafter, the reaction was terminated by stirring for 30 minutes, followed by washing with water and dehydration, followed by drying at 80 DEG C for 30 minutes. The dried flake substrate was screened using a mesh and flake substrates formed larger than a predetermined size were separated or aggregated particles formed during the reaction were removed.
Through the above process, a security pigment having an organic phosphor coated on the surface of the flake substrate was prepared.
Referring to FIG. 3, it can be seen that the security pigment according to Example 1 includes a flake substrate having a surface coated with organic phosphor particles.
≪ Example 2 >
1. Preparation of mixed organic solvent in which organic phosphor is dissolved
60 g of a mixed organic solvent having 80 parts by weight of acetone, 15 parts by weight of methanol, 3 parts by weight of toluene and 2 parts by weight of MEK was prepared in a beaker having a capacity of 100 mL and stirred at 20 to 25 캜 for 10 minutes.
0.5 g of Eu (TTA) 3Phen series organic fluorescent material was added to the mixed organic solvent, followed by stirring for 5 minutes using a magnetic bar to prepare a mixed organic solvent solution in which the organic fluorescent material was dissolved.
2. Preparation of a security pigment comprising a flake substrate coated with organic phosphor particles
10 g of flaky alumina substrate was added to a 100 ml beaker. Subsequently, the mixed organic solvent in which the organic phosphor prepared in the above process was dissolved was put in the beaker, followed by stirring at a stirring rate of 300 rpm at 60 DEG C, and the organic solvent was volatilized. After the organic solvent was volatilized, the dried flake substrate was screened using a mesh, and the flake substrate formed to have a predetermined size larger than 100 μm was separated or aggregated particles formed during the reaction were removed.
Through the above process, a security pigment having an organic phosphor coated on the surface of the flake substrate was prepared.
Referring to FIG. 4, it can be seen that the security pigment according to Example 2 includes a flake substrate having organic phosphor particles coated on its surface.
Claims (15)
(b) pulverizing the organic phosphor particles to prepare an organic binder solution containing organic phosphor particles having a particle size of 10 to 900 nm;
(c) mixing the flake substrate and the solvent, and stirring and dispersing the flake substrate and the solvent at a speed of 100 to 500 rpm to prepare a substrate suspension; And
(d) adjusting the pH of the mixed solution to a range of 7.0 to 10.0 by using a pH adjusting agent in a mixture of the substrate suspension and the organic binder solution, and coating the organic phosphor particles on the surface of the flake substrate; ≪ / RTI >
The organic binder solution
A dispersant, and a defoaming agent.
The flake substrate
Characterized in that it comprises at least one of synthetic mica, natural mica, glass flake, flaky iron oxide, flake alumina, aluminum flake, flaky silica, talc and bismuth.
The flake substrate
Wherein the at least one metal oxide layer comprises a coated flake substrate.
After the step (c)
(d) washing and dehydrating the flake substrate;
(e) drying the washed flake substrate; And
(f) a screening step of separating a flake substrate formed larger than a predetermined size among the dried flake substrates.
(b) mixing the mixed organic solvent and the flake substrate and stirring and dispersing the mixed organic solvent to prepare a substrate suspension; And
(c) stirring the substrate suspension at a temperature in the range of 40 to 70 ° C. at a rate of 100 to 300 rpm to volatilize the two or more organic solvents, and coating the surface of the flake substrate with the organic phosphor particles; Wherein the method comprises the steps of:
The flake substrate
Characterized in that it comprises at least one of synthetic mica, natural mica, glass flake, flaky iron oxide, flake alumina, aluminum flake, flaky silica, talc and bismuth.
The flake substrate
Wherein the at least one metal oxide layer comprises a coated flake substrate.
After the step (c)
(d) a screening step of separating a flake substrate formed larger than a predetermined size among the flake substrates.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020160067065A KR101854856B1 (en) | 2016-05-31 | 2016-05-31 | Method for preparing pearlescent pigment coating organic fluorescence for security and safety applications |
| PCT/KR2017/005092 WO2017209415A1 (en) | 2016-05-31 | 2017-05-17 | Method for preparing a pearlescent security and safety pigment coated with organic fluorescent |
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| Application Number | Priority Date | Filing Date | Title |
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| KR1020160067065A KR101854856B1 (en) | 2016-05-31 | 2016-05-31 | Method for preparing pearlescent pigment coating organic fluorescence for security and safety applications |
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| KR101854856B1 true KR101854856B1 (en) | 2018-05-08 |
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| KR1020160067065A KR101854856B1 (en) | 2016-05-31 | 2016-05-31 | Method for preparing pearlescent pigment coating organic fluorescence for security and safety applications |
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| WO (1) | WO2017209415A1 (en) |
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| KR102146604B1 (en) * | 2018-05-29 | 2020-08-20 | 문승호 | Red luminous waterborne emulsion composition and method for preparing the same |
| CN109999710A (en) * | 2019-04-03 | 2019-07-12 | 重庆冠邦环保科技有限公司 | A kind of water-soluble environment protective material processing technique process |
| CN115294857A (en) * | 2022-08-04 | 2022-11-04 | 湖南福泰数码材料科技有限公司 | Fluorescent label and preparation method thereof |
| CN115537039B (en) * | 2022-09-23 | 2023-09-08 | 浙江凯色丽科技发展有限公司 | Preparation method of fluorescent pearlescent pigment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO1998042799A1 (en) * | 1997-03-21 | 1998-10-01 | Merck Patent Gmbh | Pigment flakes |
| JP4316127B2 (en) * | 2000-09-05 | 2009-08-19 | 化成オプトニクス株式会社 | Method for producing phosphor paste composition and vacuum ultraviolet light-excited light emitting device |
| KR20020025488A (en) * | 2000-09-29 | 2002-04-04 | 최 병호 | Phosphor paste |
| US6533858B1 (en) * | 2000-10-10 | 2003-03-18 | Engelhard Corporation | Effect pigments with improved colorant adhesion |
| KR20060111320A (en) * | 2005-04-23 | 2006-10-27 | 삼성에스디아이 주식회사 | A phosphor paste composition, a phosphor layer prepared therefrom, a plasma displaly panel comprising the same, and a method for preparing the plasma display panel |
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