KR20140092156A - Photoluminescence Nano Capsule and Method of Manufacturing the Same - Google Patents
Photoluminescence Nano Capsule and Method of Manufacturing the Same Download PDFInfo
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- KR20140092156A KR20140092156A KR1020130004572A KR20130004572A KR20140092156A KR 20140092156 A KR20140092156 A KR 20140092156A KR 1020130004572 A KR1020130004572 A KR 1020130004572A KR 20130004572 A KR20130004572 A KR 20130004572A KR 20140092156 A KR20140092156 A KR 20140092156A
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- emulsion
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- capsules
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
Abstract
The present invention relates to a luminescent capsule having a size of 1 to 1000 nm and having a core material as an inner core and an encapsulated material coated with a polymer on the outer circumferential surface of the core material, to provide. According to the present invention, it is possible to manufacture a nanocapsule reduced in size by controlling an emulsifier, increase the luminous efficiency with an increased luminous surface area due to an increased number of capsules, and impart water dispersibility through a hydrophilic group outside the capsule.
Description
The present invention relates to a luminescent nanocapsule and a method of preparing the same. More particularly, the present invention relates to a method for producing a luminescent nanocapsule, ) europium as a core, and encapsulating the polymer by polymerization reaction of the monomer on the outer surface thereof, and a method for producing the same.
Generally, luminescent materials are aggregated in a solid state with a high price, and the efficiency is low due to limited area for emitting light. [1, 10-Phenanthroline] tris (1-thenoyl-3,3,3-trifluoroacetonato) europium, which exhibits red luminescence among these luminescent materials, is difficult to process and mold There was a problem.
Meanwhile, the method of encapsulating solid particles has been used mainly for the purpose of long-time exhibiting the effect of the drug by microencapsulating the drug, or for shielding the bitter taste. For example, the cellulose compound is dissolved in an organic solvent such as cyclohexane And the solution is cooled to precipitate the cellulose compound on the surface of the solid powder.
As an example of such a microencapsulation method, Korean Patent Laid-Open Publication No. 1997-042853 discloses a process for producing a water-soluble polymer by dissolving a photochromic dye in an organic solvent in which a cellulosic compound is dissolved, Preparing a W / O emulsion by first emulsifying the oil phase and water phase, adding a W / O emulsion while stirring an aqueous solution of an excess amount of the water soluble polymer, and emulsifying and emulsifying the organic solvent, And then curing the microcapsules to prepare microcapsules.
In addition, Korean Patent Laid-Open Publication No. 1995-009349 discloses an ink composition which is heated and dissolved in an oil of 16 to 20% by weight together with a spiro compound which is a photochromic agent in an amount of 0.1 to 1% by weight, 0.01 to 1% And a solution B in which 10 to 14% by weight of gelatin was heated in and dissolved in 58.8 to 71.8% by weight of water and maintained at a temperature of 70 to 75 캜 was prepared, Using the mechanical stirrer, the solution A was added dropwise to the solution B at a rate of 3 to 7 ml / sec while stirring the solution B at 3,000 to 8,000 rpm to form an emulsion. Then, the resulting
However, the conventional technique described above can only produce a capsule of micrometer unit using a dye as a core.
Accordingly, the present invention proposes a method of encapsulating a luminescent material into spherical particles having a maximum luminescent area and decreasing a capsule size, thereby securing a maximum luminescent area with a small luminescent material content, thereby increasing the luminescent efficiency. In addition, it is proposed that water dispersion can be performed due to the outer hydrophilic group of the prepared light emitting nanocapsules, which facilitates processing and molding.
SUMMARY OF THE INVENTION The present invention has been made in order to solve the above problems, and an object of the present invention is to provide an europium complex having a red luminescence upon UV irradiation as a core at its inner center, And to provide a spherical encapsulated light-emitting nanocapsule and a method for producing the same.
In particular, it is an object of the present invention to provide a light emitting nanocapsule and a method for manufacturing the same, which can reduce the size of capsules and increase the number of particles by controlling the content of emulsifiers and increase the luminous efficiency through the increased total luminous surface area.
Further, it is an object of the present invention to provide a light emitting nanocapsule capable of imparting water dispersibility through a hydrophilic group on the outer surface of a capsule, and a method for producing the same.
These and other objects and advantages of the present invention will become more apparent from the following description of a preferred embodiment thereof.
The object of the present invention is achieved by a light emitting nanocapsule characterized in that it comprises a core layer composed of an europium material which emits red light when irradiated with ultraviolet rays, and a coating layer coated with a polymer outside the core layer.
Here, the europium material is characterized by being a (1, 10-Phenanthroline) tris (1-thenoyl-3,3,3-trifluoroacetonato) europium.
Preferably, the polymer is polystyrene, polymethyl methacrylate, polyurethane, polyester, polyamide, polyethylene, polyvinyl alcohol, melamine resin, urea resin, gelatin, cellulose, epoxy or a mixture thereof .
Preferably, the capsule has a diameter of 1 to 1000 nm.
Advantageously, the capsule is capable of increasing the number of capsules by reducing the size of the capsules through the control of the emulsifier.
Also, the above object can be accomplished by a process for preparing a mixture, which comprises mixing a monomer and a light emitting material in an amount of 5 to 100% by weight based on the weight of the monomer at a temperature of 30 to 50 캜 to prepare a mixture, And emulsifying the emulsion by stirring the emulsion at a temperature of 30 to 50 ° C to produce an emulsion; and adding 0.1 to 1% by weight of an initiator to the emulsion prepared in the emulsion preparation step, And stirring the mixture at a temperature of 50 to 100 DEG C for 12 hours to effect encapsulation by polymerization reaction.
Here, the light emitting material is characterized by being a (1, 10-Phenanthroline) tris (1-thenoyl-3,3,3-trifluoroacetonato) europium.
Preferably, the emulsifier is a methacrylic acid.
Preferably, the initiator is potassium persulfate, aminopropanesulfonic acid, azobismethylpropionitrile, or a mixture thereof.
Preferably, the emulsion preparation step is characterized by reducing the size of the capsules through the control of the emulsifier to increase the number of capsules.
According to the present invention, it is possible to provide an europium complex which exhibits red luminescence upon UV irradiation as a core at the inner center, a capsule can be prepared by coating a polymer on the outer circumferential surface of the europium complex, The light emitting efficiency can be increased through the light emitting surface area within the increased unit area by increasing the number of the light emitting layer, and the water dispersibility can be achieved through the hydrophilic group, thereby facilitating processing and molding.
1 is a sectional view of a nanocapsule having a light emitting function according to the present invention.
Hereinafter, the present invention will be described in detail with reference to embodiments and drawings of the present invention. It will be apparent to those skilled in the art that these embodiments are provided by way of illustration only for the purpose of more particularly illustrating the present invention and that the scope of the present invention is not limited by these embodiments .
FIG. 1 is a cross-sectional view of a nanocapsule having a light emitting function according to the present invention. As shown in FIG. 1, the light emitting nanocapsule according to the present invention includes a
The europium material according to the present invention is a 1 -10-phenanthroline tris (1-thenoyl-3,3,3-trifluoroacetonato) europium as a core in the nanocapsule, Means a substance emitting red light, and is not particularly limited as long as it has such a property.
The polymer according to the present invention has a capsule shape by coating the outer circumferential surface of the europium complex provided in the core form. Preferably, the polymer is a polystyrene, a polymethyl methacrylate, a polyurethane, a polyester, a polyamide, Polyvinyl alcohol, melamine resin, urea resin, gelatin, cellulose, epoxy or a mixture thereof. At this time, since the polymer covers the outer circumferential surface of the europium complex according to the present invention to form the outer wall of the nanocapsule, it can be used as a polymer layer.
Further, the light-emitting nanocapsule according to the present invention means a capsule having a diameter (D in FIG. 1) of nanometer size, preferably 1 to 1000 nm, more preferably 50 to 600 nm, Europium complex, and a polymer, preferably a polymer layer, is provided on the outside thereof to form a capsule.
The light emitting nanocapsules according to the present invention are characterized in that the number of capsules can be increased by decreasing the size of the capsules through the control of the emulsifier. In the emulsion preparation process described below, By increasing the number of capsules, the luminous surface area in the unit area of the capsule is increased, thereby increasing the luminous efficiency.
The method for preparing a light emitting nanocapsule according to the present invention comprises the steps of preparing a mixture by mixing 5 to 100% by weight of a light emitting material with a monomer and a monomer at a temperature of 30 to 50 ° C, 0.1 to 20% by weight of an emulsifier, and stirring the mixture at a temperature of 30 to 50 DEG C to emulsify the mixture to form an emulsion; and adding to the emulsion prepared in the emulsion preparing step 0.1 to 1 wt. % Of an initiator, and stirring the mixture at a temperature of 50 to 100 DEG C for 4 to 12 hours to effect encapsulation.
The monomer according to the present invention is preferably a methyl methacrylate monomer.
The emulsifier used in the emulsion preparation step is to emulsify the monomer and the europium complex to form a droplet, preferably a stable droplet of a small size. Any emulsifier may be used as long as it is used for this purpose. It is preferable to use an emulsifier commonly used in the art, more preferably methacrylic acid.
In addition, the initiator according to the present invention is added to the emulsion through the separation step so as to allow the monomer to undergo a polymerization reaction. Any conventional initiator used for this purpose may be used, It is preferred to use potassium persulfate (KPS), aminopropanesulfonic acid (APS), azobis methylpropionitrile (AIBN), or a mixture thereof, preferably using potassium persulfate It is good.
In addition, the method of the present invention can increase the number of capsules by reducing the size of the capsules through the control of the emulsifier. In the emulsion manufacturing process of the present invention, By increasing the number of capsules, the luminous surface area in the unit area of the capsule is increased, thereby increasing the luminous efficiency.
Accordingly, the present invention provides a light-emitting nanocapsule and a method of producing the same, wherein the europium complex exhibiting red light emission upon UV irradiation is provided as a core at the inner center, and the polymer is coated on the outer peripheral surface of the europium complex to be encapsulated, The size of the capsules can be reduced and the number of the capsules can be increased by controlling the emulsifier to increase the luminous efficiency through the light emitting surface area within the increased unit area and the manufactured capsules can be processed and molded by the hydrophilic group There is one advantage.
The luminous nanocapsules encapsulated by coating the polymer on the outer circumferential surface of the europium complex and the europium complex according to the present invention are provided at the inner center of the core and are widely used in various plastic coating agents, .
Hereinafter, the structure and effect of the present invention will be described in more detail with reference to examples and comparative examples. However, this embodiment is intended to explain the present invention more specifically, and the scope of the present invention is not limited to these embodiments.
[Example 1]
8 g of a methyl methacrylate monomer capable of being polymerized as an encapsulating material and 1 g of an europium (1, 10-Phenanthroline) tris (1-thenoyl-3,3,3-trifluoroacetonato) Lt; / RTI > to produce a mixture. Then, 0.1 to 1.5 g of methacrylic acid as an emulsifier was mixed with the mixture, and the mixture was stirred at 50 캜 to emulsify the mixture. Thereafter, 0.03 g of potassium persulfate, which is an initiator, was added to the emulsion, and the mixture was stirred at a temperature of 70 ° C for 6 hours to polymerize to produce a nanocapsule.
The size of the prepared nanocapsules and the intensity of photoluminescence (PL intensity) thereof are shown in Table 1 below.
(au)
[ Example 2]
Same as Example 1, except that the prepared mixture was dispersed in 200 g of distilled water. As a result, the size of the prepared capsules and the resulting photoluminescence intensity (PL intensity) are shown in Table 2 below.
(au)
[ Comparative Example One]
The photoluminescence intensity (PL intensity) of 1 g of pure europium complex [(1, 10-Phenanthroline) tris (1-thenoyl-3,3,3-trifluoroacetonato) europium] Respectively.
(au)
(1, 10-Phenanthroline) tris (1-thenoyl-3,3,3-trifluoroacetonato) europium, which shows red luminescence upon irradiation with ultraviolet light, was dispersed in 200 g of distilled water and photoluminescence intensity (PL intensity) are shown in Table 4 below.
(au)
It is to be understood that the present invention is not limited to the above embodiments and various changes and modifications may be made by those skilled in the art without departing from the spirit and scope of the invention.
1: core layer 2: coating layer (capsule membrane)
Claims (10)
And a coating layer coated on the outside of the core layer with a polymer.
Wherein the europium material is a (1, 10-Phenanthroline) tris (1-thenoyl-3,3,3-trifluoroacetonato) europium.
Wherein the polymer is selected from the group consisting of polystyrene, polymethyl methacrylate, polyurethane, polyester, polyamide, polyethylene, polyvinyl alcohol, melamine resin, urea resin, gelatin, cellulose, epoxy, .
Wherein the capsules have a diameter of 1 to 1000 nm.
Wherein the capsule is capable of increasing the number of capsules by reducing the size of the capsule through the control of the emulsifier.
An emulsion preparation step of mixing the mixture with 0.1 to 20% by weight of an emulsifier based on the weight of the monomer and stirring the mixture at a temperature of 30 to 50 캜 to emulsify the mixture to prepare an emulsion;
And encapsulating the emulsion by adding 0.1 to 1% by weight of an initiator to the emulsion prepared in the step of emulsion and stirring the mixture at a temperature of 50 to 100 ° C for 4 to 12 hours to effect polymerization reaction. , A method for producing a light emitting nanocapsule.
Wherein the light emitting material is a (1, 10-Phenanthroline) tris (1-thenoyl-3,3,3-trifluoroacetonato) europium.
Wherein the emulsifying agent is a methacrylic acid.
Wherein the initiator is selected from the group consisting of potassium persulfate, aminopropanesulfonic acid, azobismethylpropionitrile, and mixtures thereof.
Wherein the emulsion preparation step comprises increasing the number of capsules by reducing the size of the capsules through the control of the emulsifier.
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| KR1020130004572A KR20140092156A (en) | 2013-01-15 | 2013-01-15 | Photoluminescence Nano Capsule and Method of Manufacturing the Same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20170057918A (en) * | 2015-11-17 | 2017-05-26 | 단국대학교 산학협력단 | Method of fabricating Nanophosphor microcapsules |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20170057918A (en) * | 2015-11-17 | 2017-05-26 | 단국대학교 산학협력단 | Method of fabricating Nanophosphor microcapsules |
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