KR20150017796A - Method for preparation of liquid micro-capsule containing nano-particles - Google Patents

Abstract

The present invention relates to a method for preparing a liquid micro-capsule containing nanoparticles. Specifically, the method comprises the steps of: preparing a solution in which nanoparticles are dispersed and a polymer solution for forming a coated layer of a capsule; encapsulating two types of solutions; and curing the coated layer of the capsule.

Description

[0001] The present invention relates to a method for preparing a liquid microcapsule containing nanoparticles,

The present invention relates to a method of preparing liquid microcapsules containing nanoparticles, and more particularly, to a method of microencapsulating a solution in which nanoparticles are dispersed by various physical / chemical methods.

BACKGROUND ART [0002] Recently, the manufacture and application of a display, a printing apparatus using a medium in which nanoparticles are dispersed, and a film therefor have been actively promoted. In order to perform the above-described application, a micro-sized encapsulation process of a medium in which nanoparticles are dispersed is required.

BACKGROUND ART Microcapsules are generally used for sealing liquid or solid materials with fine capsule wall materials, and they are used for protecting or inducing release of internal substances, and they are widely used in various fields such as foods, cosmetics, medicines and fragrances have. In general, microcapsules can be prepared by a variety of methods such as emulsion polymerization, multiple emulsion polymerization, condensation polymerization, solvent extraction and evaporation, suspension polymerization, coacervation, extrusion, spraying and the like.

However, in order to produce liquid microcapsules of a medium in which nanoparticles are dispersed, it is extremely difficult to produce the liquid microcapsules. In addition, in the conventional preparation methods, excessive polar or non-polar solvents must be used in the manufacturing and cleaning processes. , The temperature and the concentration of the emulsifier vary greatly in the average particle size and the distribution thereof, which makes it difficult to manufacture an intended micro-sized capsule and to mass-produce it, and it is difficult to manufacture liquid microcapsules of several micro-sizes And therefore new technologies are needed to solve these problems.

Therefore, in the present invention, a method for producing a microcapsule capable of producing uniform and large-scale production including nanoparticles is described.

It is an object of the present invention to provide a method and apparatus for producing liquid-phase microcapsules of uniform size including a medium in which a plurality of nanoparticles are dispersed.

In order to achieve the above object, a liquid microcapsule according to the present invention includes a medium in which a plurality of nanoparticles are dispersed and a polymer in which a polymer to be used as a coating material is melted, wherein a plurality of nanoparticles are dispersed in a core And forming a microcapsule containing the medium and drying at a high temperature to cure the coating.

The liquid microcapsule according to the present invention includes a medium including a medium in which a plurality of nanoparticles are dispersed and a medium in which a plurality of nanoparticles are dispersedly dispersed in a core using a medium in which a polymer to be used as a coating material is melted And forming a microcapsule and cooling at a low temperature to cure the coating.

The liquid microcapsule according to the present invention includes a medium including a medium in which a plurality of nanoparticles are dispersed and a medium in which a plurality of nanoparticles are dispersedly dispersed in a core using a medium in which a polymer to be used as a coating material is melted And forming a microcapsule and irradiating ultraviolet rays to cure the coating.

The liquid microcapsule according to the present invention includes a medium including a medium in which a plurality of nanoparticles are dispersed and a medium in which a plurality of nanoparticles are dispersedly dispersed in a core using a medium in which a polymer to be used as a coating material is melted And forming a microcapsule and ionizing it to cure the coating.

The nanoparticles may be selected from the group consisting of Fe, Ni, Co, Ti, C, Zn, S, Au, (Ba), strontium (Sr), lead (Pb), aluminum (Al), tungsten (W), molybdenum (Mo), or the like.

The nanoparticles may be formed of a polymer material such as polystyrene (PS), polyethlylene (PE), polypropylene (PP), polyvinyl chloride (PVC), or polyethylene terephthalate (PET).

The nanoparticles may comprise a cluster form.

The nanoparticles may be particles whose surfaces have been processed (or coated) by organic compounds, particles whose surfaces have been processed (coated) by complex compounds, or particles whose surfaces have been processed (coated) by coordination compounds.

The nanoparticles may be in the form of a core-shell.

The nanoparticles have a diameter of 10 nm to 500 nm.

The nanoparticles may be dispersed in the medium as particles having electric charges.

The nanoparticles may comprise one of paramagnetic, super paramagnetic materials.

The nanoparticles vary in spacing between the particles according to at least one change in intensity or direction of the electric field, and the wavelength of the light reflected from the particles varies with the change in the spacing.

The nanoparticles can be used in a display device in which the movement of the particles is varied or limited according to a change in at least one of intensity or direction of an electric field.

The nanoparticles vary in spacing between the particles according to at least one of the strength or the direction of the magnetic field, and the wavelength of the light reflected from the particles may vary with the change in the spacing.

The medium may be selected from the group consisting of water, methanol, ethanol, propanol, butanol, propylene carbonate, toluene, benzene, hexane, Chloroform, Isopar-G, Isopar-M, and the like.

The medium may be transparent or colored.

Wherein the encapsulating material is a transparent polymer,

Azido carbonate (aginate), gelatin (gelatin), ethyl cellulose (ethyl cellulose), polyamide (polyamide), melamine-formaldehyde (melamine formaldehyde, and the like), polyvinyl pyridine (poly (vinyl pyridine)), polystyrene (polystyrene), polyurethane (urethane), polyurethane (polyurethane), methyl methacrylate (methyl methacrylate).

The encapsulating material may be cured at a high temperature, a low temperature, an ultraviolet, or an ionic condition.

The microcapsules have a diameter ranging from 1 μm to 1,000 μm.

The microcapsule may be mixed with a medium in which nano-particles are dispersed and a medium in which a polymer to be encapsulated is melted, using one or more of ultrasonic, stirring, vibration, and high-voltage application methods.

The encapsulating material of the microcapsule may have soft or hard characteristics depending on the concentration or type of the transparent polymer.

According to the method for producing liquid microcapsules containing nanoparticles according to the present invention, it is possible to select a medium of a polymer material to be used for various coatings depending on the polarity and non-polarity of a medium in which nanoparticles are dispersed, That is, by selecting methods such as ultrasonic wave, agitation, vibration, and high voltage application, it is easy to manufacture microcapsules of a size to be manufactured, and consumption of unnecessary media is reduced by using only a minimum amount of medium essential for microcapsule production, So that the production efficiency is high.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a diagram illustrating a configuration of a medium in which nanoparticles of the present invention are dispersed. FIG.
Fig. 2 is a view showing an exemplary structure of a liquid microcapsule containing a medium in which nanoparticles of the present invention are dispersed. Fig.
FIGS. 3 to 8 are views illustrating a process for producing liquid microcapsules containing a nanoparticle-dispersed medium according to an embodiment of the present invention.

The main technical features of the liquid microcapsule including the medium in which nanoparticles are dispersed according to an embodiment of the present invention are as follows. More particularly, the present invention is characterized in that it comprises a step of preparing a solution in which nanoparticles are dispersed and a polymer solution for forming a capsule film, an encapsulating step of the two kinds of liquid substances, and a curing step of curing the capsule coating.

FIG. 1 and FIG. 2 illustrate a structure of a medium in which nanoparticles are dispersed according to an embodiment of the present invention and a structure of a liquid-phase microcapsule containing the same.

First, referring to FIG. 1, nanoparticles according to one embodiment of the present invention may have a diameter of several nanometers to several hundred nanometers, but the nanoparticles are not necessarily limited thereto. The nanoparticles may be dispersed in the medium as charged particles, wherein the nanoparticles may be composed of a core-shell structure. The nanoparticles may also include paramagnetic or super paramagnetic materials.

The medium according to the present invention may be used in the form of water, which has polar or non-polar characteristics, methanol, ethanol, propanol, butanol, propylene carbonate, carbonate, toluene, benzene, hexane, chloroform, Isopar-G, Isopar-M, and the like.

It should be noted, however, that the medium according to the present invention is not limited to those listed above, and can be appropriately changed within the scope of achieving the object of the present invention.

[Various embodiments]

Hereinafter, various embodiments of the liquid microcapsule manufacturing method including the medium in which the nanoparticles according to the present invention are dispersed will be described in detail.

[Example 1]

Referring to FIG. 3, a process for producing a liquid microcapsule including a medium in which nanoparticles are dispersed is illustrated. First, a medium (a central substance) in which nanoparticles are dispersed is prepared by ultrasonic dispersion. The nanoparticles may be dispersed by various methods such as ultrasonic dispersion, mechanical stirring dispersion, electrostatic dispersion, dispersing agent dispersion, etc. However, the present invention is not limited thereto and may be appropriately modified within the scope of achieving the object of the present invention. .

Next, a medium (wall material) in which a polymer to be used as a coating material is melted is prepared. At this time, the content of the polymer may be controlled to adjust the thickness and the size of the film by several% to several tens%, and the melting is proceeded while heating to 40 ° C to 80 ° C in general. The temperature at this time may vary depending on the polymer.

The two media are jetted through a coaxial nozzle having a size of several micrometers to several tens of micrometers together with high-temperature air into a space having a drying device heated to a high temperature or a space having a cooling device cooled to a low temperature So that the microcapsules are cured by drying the coating material of the microcapsules.

The nozzle may basically form a liquid microcapsule using the two-fluid-nozzle, and one of jetting, high-pressure jetting, and electrospraying may be used as the jetting method. Further, the temperature of the drying apparatus or the temperature of the cooling apparatus may differ depending on the characteristics of the medium.

A method of quickly producing liquid microcapsules having a size of 1 to 1,000 mu m including the medium in which nanoparticles are dispersed can be rapidly produced through the above-described manufacturing process.

[Example 2]

Referring to FIG. 4, a process for producing a liquid microcapsule including a medium in which nanoparticles are dispersed is illustrated. First, a medium (a central substance) in which nanoparticles are dispersed is prepared by ultrasonic dispersion. The nanoparticles may be dispersed by various methods such as ultrasonic dispersion, mechanical stirring dispersion, electrostatic dispersion, dispersing agent dispersion, etc. However, the present invention is not limited thereto and may be appropriately modified within the scope of achieving the object of the present invention. .

Next, a medium (wall material) in which a polymer to be used as a coating material is melted is prepared. At this time, the content of the polymer may be controlled to adjust the thickness and the size of the film by several% to several tens%, and the melting is proceeded while heating to 40 ° C to 80 ° C in general. The temperature at this time may vary depending on the polymer.

The medium in which the nanoparticles are dispersed is jetted through a nozzle having a size of several μm to several tens of μm at the bottom of the cooling reaction tank in the same manner as the flow of the gas and at the same time the polymer used as a coating material is cooled The injection is performed through a nozzle having a size of several μm to several tens of μm on the upper part of the reaction tank. Two media dispersed in the top and bottom form microcapsules in the reaction tank and then the coating material is dried to cure the microcapsules.

A method of quickly producing liquid microcapsules having a size of 1 to 1,000 mu m including the medium in which nanoparticles are dispersed can be rapidly produced through the above-described manufacturing process.

[Example 3]

Referring to FIG. 5, a process for producing liquid microcapsules containing a medium in which nanoparticles are dispersed is illustrated. First, a medium (core material) in which nanoparticles are dispersed is prepared by ultrasonic dispersion. The nanoparticles may be dispersed by various methods such as ultrasonic dispersion, mechanical stirring dispersion, electrostatic dispersion, dispersing agent dispersion, etc. However, the present invention is not limited thereto and may be appropriately modified within the scope of achieving the object of the present invention. .

Next, a medium (wall material) in which a polymer to be used as a coating material is melted is prepared. At this time, the content of the polymer may be controlled to adjust the thickness and the size of the film by several% to several tens%, and the melting is proceeded while heating to 40 ° C to 80 ° C in general. The temperature at this time may vary depending on the polymer.

The two media are extruded together with a mobile phase gas through a two-fluid nozzle having an inner diameter of several μm to several tens of μm by using a pump. At this time, the moving speed of the two media can be adjusted, and the size of the capsule can be adjusted through this. Through this process, liquid microcapsules are formed, and the liquid microcapsules containing the medium in which the nanoparticles to be obtained by drying are collected by being passed through a cooling device to be cured immediately or collected in a container containing the third distilled water, can do.

A method of quickly producing liquid microcapsules having a size of 1 to 1,000 mu m including the medium in which nanoparticles are dispersed can be rapidly produced through the above-described manufacturing process.

[Example 4]

Referring to FIG. 6, a process for producing liquid microcapsules including a medium in which nanoparticles are dispersed is illustrated. First, a medium (a central substance) in which nanoparticles are dispersed is prepared by ultrasonic dispersion. The nanoparticles may be dispersed by various methods such as ultrasonic dispersion, mechanical stirring dispersion, electrostatic dispersion, dispersing agent dispersion, etc. However, the present invention is not limited thereto and may be appropriately modified within the scope of achieving the object of the present invention. .

Next, a medium (wall material) in which a polymer to be used as a coating material is melted is prepared. At this time, the content of the polymer may be controlled to adjust the thickness and the size of the film by several% to several tens%, and the melting is proceeded while heating to 40 ° C to 80 ° C in general. The temperature at this time may vary depending on the polymer.

The two media are extruded together with a mobile phase gas through a two-fluid nozzle having an inner diameter of several μm to several tens of μm by using a pump. At this time, the moving speed of the two media can be adjusted, and the size of the capsule can be adjusted through this.

In addition, fine microcapsules can be formed by passing the extruded liquid microcapsules through a jet cutter rotating at high speed. The liquid microcapsules formed by the series of processes can be prepared by storing the medium in which the nanoparticles to be obtained are obtained by storing the liquid microcapsules formed in the bottom reaction vessel in which the medium containing the crosslinking agent is rotated.

A method of quickly producing liquid microcapsules having a size of 1 to 1,000 mu m including the medium in which nanoparticles are dispersed can be rapidly produced through the above-described manufacturing process.

[Example 5]

Referring to FIG. 7, a process for producing liquid microcapsules containing a medium in which nanoparticles are dispersed is illustrated. First, a medium (core material) in which nanoparticles are dispersed is prepared by ultrasonic dispersion. The nanoparticles may be dispersed by various methods such as ultrasonic dispersion, mechanical stirring dispersion, electrostatic dispersion, dispersing agent dispersion, etc. However, the present invention is not limited thereto and may be appropriately modified within the scope of achieving the object of the present invention. .

Next, a medium (wall material) on which an ultraviolet curing agent to be used as a coating material is melted is prepared. At this time, the content of the curing agent may be adjusted from several% to several tens% in order to control the thickness and the size of the film.

The two media are extruded together with a mobile phase gas through a two-fluid nozzle having an inner diameter of several μm to several tens of μm by using a pump. The liquid microcapsules formed by irradiating ultraviolet rays to the side portions of the extrusion passage are cured and the liquid microcapsules containing the medium in which nanoparticles to be obtained by drying are collected in a container containing the third distilled water can be produced.

A method of quickly producing liquid microcapsules having a size of 1 to 1,000 mu m including the medium in which nanoparticles are dispersed can be rapidly produced through the above-described manufacturing process.

[Example 5]

Referring to FIG. 8, a process for producing liquid microcapsules containing a medium in which nanoparticles are dispersed is illustrated. First, a medium (a central substance) in which nanoparticles are dispersed is prepared by ultrasonic dispersion. The nanoparticles may be dispersed by various methods such as ultrasonic dispersion, mechanical stirring dispersion, electrostatic dispersion, dispersing agent dispersion, etc. However, the present invention is not limited thereto and may be appropriately modified within the scope of achieving the object of the present invention. .

Next, a medium (wall material) in which a polymer to be used as a coating material is melted is prepared. At this time, the content of the polymer may be controlled to adjust the thickness and the size of the film by several% to several tens%, and the melting is proceeded while heating to 40 ° C to 80 ° C in general. The temperature at this time may vary depending on the polymer. Next, the film material is output in the form of a thin film and rotated in both directions from the center to the center. Two cylindrical rolls are located at the center of the reaction chamber, and a hole having a size of several micrometers to several hundreds of micrometers is processed in the cylinder.

The medium in which nanoparticles are dispersed is dropped through a nozzle having a size of several μm to several tens of μm by using a pump. At this time, the moving speed of the medium can be adjusted and the amount of the encapsulated medium can be adjusted.

The liquid microcapsules containing the medium in which the nanoparticles to be obtained are dispersed can be prepared through such a series of processes.

At this time, the size of the microcapsule can be controlled by the hole size of the cylinder, and the amount of the dropped medium, the falling speed, and the rotation speed of the roll are kept constant, so that the microcapsules of a certain size can be formed.

A method of quickly producing liquid microcapsules having a size of 1 to 1,000 mu m including the medium in which nanoparticles are dispersed can be rapidly produced through the above-described manufacturing process.

Claims (18)

A process for producing liquid microcapsules containing nanoparticles,
The nanoparticles may be selected from the group consisting of Fe, Ni, Co, Ti, C, Zn, S, Au, A material including elements such as Ba, Sr, Pb, Al, W, and Mo, or an oxide thereof. . Wherein the nanoparticles are made of a polymer material such as polystyrene (PS), polyethlylene (PE), polypropylene (PP), polyvinyl chloride (PVC), or polyethylene terephthalate (PET). Wherein the nanoparticles comprise a cluster. Wherein the nanoparticles are particles whose surfaces are processed (or coated) by an organic compound, particles whose surfaces have been processed (coated) by complex compounds, and particles whose surfaces have been processed (coated) by coordination compounds. Wherein the nanoparticles are in the form of a core-shell. Wherein the nanoparticles have a diameter of 10 nm to 500 nm. Wherein the nanoparticles are dispersed in a medium as charged particles. Wherein the nanoparticles comprise one of a paramagnetic, super paramagnetic material. Wherein the nanoparticles vary in spacing between the particles according to at least one of an intensity or direction of an electric field and the wavelength of light reflected from the particles varies with the change in the spacing. Wherein the nanoparticles are used in a display device in such a way that the movement of the particles is varied or limited according to a change in at least one of intensity or direction of the electric field. Wherein the nanoparticles vary in spacing between the particles in accordance with a change in at least one of an intensity or a direction of a magnetic field and a wavelength of light reflected from the particles changes with a change in the gap. The medium may be selected from the group consisting of water, methanol, ethanol, propanol, butanol, propylene carbonate, toluene, benzene, hexane, Characterized in that it comprises at least one material selected from the group consisting of chloroform, isopar-G, and isopar-M. Wherein the medium is transparent or colored. Wherein the encapsulating material is a transparent polymer, and the encapsulating material is selected from the group consisting of aginate, gelatin, ethyl cellulose, polyamide, melamine formaldehyde, polyvinylpyridine polyurethane, poly (vinyl pyridine), polystyrene, urethane, polyurethane, methyl methacrylate, and the like. Wherein the capsule coating material is cured by a high temperature condition, a low temperature condition, an ultraviolet ray condition, an ionic condition, or the like. Wherein the microcapsules have a diameter ranging from about 1 μm to about 1,000 μm. The microcapsule may be prepared by mixing one or more of a medium in which nanoparticles are dispersed and a medium in which a polymer to be used as a capsule coating material is melted by using one or more of the following methods: ultrasonic wave, stirring, vibration, . Wherein the encapsulating material of the microcapsule has properties of soft or hard depending on the concentration or type of the transparent polymer.

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