KR101114425B1 - Nano particle complex having a uniform surface particle and method of manufacturing thereof - Google Patents

Abstract

The present invention relates to a nanocomposite particle body and a method for producing the aggregated surface particles are removed, and more particularly to a dry composite comprising a polymer particle as a parent particle and a nanoparticle as a subparticle, wherein the dry complex is added to a solution. Dispersing and dissolving and removing the nanoparticles agglomerated on the surface of the dry composite to prepare a nanocomposite, and further adding nanoparticles to the nanocomposite to produce a second dry composite, followed by the second The present invention relates to a nanocomposite particle having a high particle fraction dispersed by dispersing the dry complex in a solution to dissolve the nanoparticles agglomerated on the surface of the second dry complex.

Nanocomposite Particle, Core Cell

Description

Nanocomposite particle having a uniform surface particle and method of manufacturing thereof

The present invention relates to a nanoparticle composite from which surface particle agglomeration has been removed, and a method of manufacturing the same. After the dry composite is prepared, the dry composite is dispersed in a solution to dissolve and remove the nanoparticles agglomerated on the surface of the dry composite surface. The present invention relates to a technique for producing a nanoparticle composite from which particle agglomeration is removed.

Dry nanocomposite particles produced using the existing high-speed rotating device is made in such a way that the composite particles are produced by a simple collision. In this case, the nanoparticles are made in such a way that the subparticles are externally entrapped by the collision with the parent particles and then dug inward by the additional collision.

FIG. 1 is an enlarged view of a conventional core cell nanocomposite, and in order for the magnetic particles located on the surface of the mother particle to be deeply embedded in the mother particle, the composite may be formed only in a manner in which other magnetic particles strike the existing magnetic particles from the surface. . However, when the composite particles are produced in this manner, a phenomenon occurs in which the magnetic particle distribution is concentrated on the mother particle surface. In particular, as shown in FIG. 1, the outermost layer of particles is provided with a layer of magnetic particles to form a core-shell structure. In this case, when a nanocomposite particle having a uniform distribution of the parent particles and the magnetic particles is required, the overall physical properties are degraded by the magnetic particles aggregated on the surface.

For example, when the conductive nanoparticles are used as the magnetic particles and the insulating polymer is used as the parent particles, the nanocomposite particles produced must have insulation performance as a whole, but the conductive nanoparticles are coated on the surface to act as an overall conductor. Can be mentioned.

FIG. 2 is an enlarged view showing that it is difficult to complex additional nanoparticles due to nanoparticles having partition walls formed outside the existing parent particles, and a dry hybridization process using a high-speed rotating device in manufacturing nanocomposite particles. When used, the core-shell structure, once formed, forms a barrier on the outside of the parent particle, which inhibits the complexation of additional nanoparticles. For this reason, the amount of nanocomposites that can be complexed to the parent particles is limited, which causes problems in manufacturing high-concentration nanocomposites.

The present invention is to solve the problems of the prior art as described above, by dispersing the dry complex in a solution that dissolves the nanoparticles but not the polymer particles, the nanoparticle composite to remove the nanoparticles agglomerated on the surface of the composite and It provides a manufacturing method.

The present invention to achieve the above object,

In a dry composite comprising a polymer particle as a mother particle and a nanoparticle as a child particle, the present invention provides a nanocomposite body in which nanoparticles agglomerated on the surface of the dry compound are dissolved and removed. In the primary dry composite including nanoparticles as particles, the nanoparticles aggregated on the surface of the primary dry composite are dissolved and removed to prepare a nanocomposite particle, and the nanoparticles are further added to the nanocomposite particle. After supplying the secondary dry composite to prepare, the nanocomposite particle is characterized in that the high particle fraction removed by dissolving the nanoparticles agglomerated on the surface of the secondary dry composite again.

The parent particle is a polymer particle is characterized in that the spherical polyethylene resin or a spherical PMMA resin, the nanoparticles are magnetic particles are nanocomposite particles characterized in that the MgO or Ag.

In addition, the present invention comprises the steps of preparing a primary dry composite by complexing the nanoparticles of the magnetic particles to the mother particles using the high-speed rotation equipment; And dispersing the primary dry composite in a solution in which only the nanoparticles are dissolved, thereby removing nanoparticles agglomerated on the surface of the primary dry composite. In addition, using the high-speed rotation equipment to the primary dry composite from which the nanoparticles agglomerates removed from the surface using a high-speed rotating equipment to prepare a secondary dry composite by nanoparticles; And dispersing the secondary dry composite in a solution in which only the nanoparticles are dissolved, thereby removing nanoparticles agglomerated on the surface of the secondary dry composite. to provide.

It is preferable that the polymer particle which is the said parent particle is a spherical polyethylene resin or a spherical PMMA resin, and it is preferable that the nanoparticle which is the said magnetic particle is MgO or Ag.

According to the present invention, additional nanoparticles can be expected to be complexed through the nanoparticle composite having a uniform surface concentration, and the problems caused by surface particle aggregation can be solved, so that the original characteristics of the nanoparticle composite can be exhibited. There is an effect that can produce a particle body having a higher nanoparticle fraction.

The present invention provides a nanocomposite particle in which a nanoparticle aggregated on the surface of the dry compound is dissolved and removed in a dry composite comprising a polymer particle as a mother particle and a nanoparticle as a child particle. In a primary dry composite comprising particles and nanoparticles as self particles, nanoparticles aggregated on the surface of the primary dry composite are dissolved and removed to prepare nanocomposite particles, and nanoparticles in the nanocomposite particles. After further adding to prepare a secondary dry composite, it provides a nano-composite particles, characterized in that the high particle fraction removed by dissolving the nanoparticles agglomerated again on the surface of the secondary dry composite.

The parent particle is a polymer particle is characterized in that the spherical polyethylene resin or a spherical PMMA resin, the nanoparticles are magnetic particles are nanocomposite particles characterized in that the MgO or Ag.

The terms or words used in this specification and claims are not to be construed as being limited to their ordinary or dictionary meanings, and the inventors may appropriately define the concept of terms in order to best describe their invention. It should be interpreted as meaning and concept corresponding to the technical idea of the present invention based on the principle that the present invention.

Therefore, the embodiments described in the specification and the drawings shown in the drawings are only the most preferred embodiment of the present invention, and do not represent all of the technical idea of the present invention, which can be replaced at the time of the present application It should be understood that there may be various equivalents and variations.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.

Figure 3 is a step showing a particle body from which the surface particle agglomeration is removed according to an embodiment of the present invention.

In the case of using a dry hybridization process using a high speed rotating device in the manufacture of the nanocomposite particles, the nanoparticles of the self particles are adsorbed through the high speed rotating device on the surface of the polymer particles, which are the first parent particles.

In order for the magnetic particles located on the surface of the mother particles to be embedded deeply inside the mother particles, the composites can be formed only by other magnetic particles hitting the existing particles on the surface. However, when the composite particles are manufactured in the above manner, a phenomenon in which the magnetic particle distribution is dense on the surface of the mother particle occurs, and in particular, the outermost layer of the particle contains only a layer of magnetic particles, thereby forming a kind of core-shell structure. The primary dry complex of is produced.

It is preferable to use spherical polyethylene resin or spherical PMMA resin as the material of the polymer particles which are the parent particles, and MgO or Ag is used as the material of the nanoparticles which are the magnetic particles. In addition, the parent particles have a particle size of 1 ~ 100㎛, the nanoparticles of the magnetic particles to have a size of 1 ~ 900nm.

The primary dry composite is dispersed in a solution to remove nanoparticles formed on the surface, the solution is composed of a solution that dissolves nanoparticles but does not dissolve the polymer particles of the parent particles, such as acid Or preference is given to using a basic solution. In the primary dry composite dispersed in the solution, the nanoparticles entering the polymer particles are protected by the polymer from the solution.

As such, there is an effect that the original characteristics of the nanocomposite particles can be found by removing the nanoparticles aggregated on the surface. For example, FIG. 4 shows hydrophobic polymer particles and hydrophilic nanoparticles, and the prepared nanocomposite should have hydrophobicity depending on the properties of the polymer particles, but if the surface is agglomerated with hydrophilic nanoparticles, the entire nanocomposite particle It becomes hydrophilic in itself. Therefore, removing the aggregated particles as described above can effectively work when the nanocomposite particles are dispersed in hydrophobic materials.

Figure 5 relates to an embodiment of the present invention, by adsorbing the nanoparticles further with a particle sieve remove the surface particle agglomeration described above to make a secondary dry composite, to dissolve it to produce a particle sieve having a high particle fraction It is a step diagram which shows doing.

The nanoparticles, which are the self particles, are adsorbed to the surface of the particle body from which the surface particles are collected as the parent particles through a high speed rotating device. Of course, secondary dry complexes are created, in which not only the nanoparticles that get stuck inside, but also nanoparticles that stick to the outer surface are present.

In a similar manner, the secondary dry composite is dispersed in a solution to remove nanoparticles formed on the surface. The solution is composed of a solution which dissolves nanoparticles but does not dissolve polymer particles which are parent particles. In the secondary dry composite dispersed in the solution, the nanoparticles entering the inside of the polymer particles are protected by the polymer from the solution. Therefore, it is possible to produce a high particle fractional particle containing nanoparticles therein more than the particle body from which the surface particle agglomerates of the existing parent particles are removed.

Hereinafter, the present invention will be described in detail with reference to the following Examples, but the following examples are merely to illustrate the present invention, and the present invention is not limited thereto. Analysis of the products prepared in Examples and Comparative Examples of the present invention is as follows. In the same way.

Example  One.

10 g of spherical polyethylene resin particles having a size of 5 μm and 2 g of 50 nm MgO (Aldrich) were quantified and added to a hybridizer capable of high-speed rotation and treated at 10,000 rpm for 5 minutes. 10 g of the obtained MgO-PE complex is dispersed in 1000 mL of 0.1N hydrochloric acid aqueous solution and reacted for 15 minutes. 8 g of solid content was obtained by filtration, dispersed in a wide petridish, and heated in an oven at 80 ° C. for 12 hours to obtain MgO-PE composite particles without surface MgO aggregation. The MgO-PE composite particles thus prepared were heated to 600 ° C. with TGA and the remaining weight was measured. The MgO fraction contained in the particles can be measured, and the measurement result can confirm the MgO particle fraction of 4.6%.

Example  2.

5 g and 50 nm MgO (Aldrich) particles 1g prepared in Example 1 was quantified and added to a hybridizer capable of high-speed rotation and treated at 10,000 rpm for 5 minutes. 5 g of the obtained MgO-PE complex is dispersed in 1000 mL of 0.1N aqueous hydrochloric acid solution and reacted for 15 minutes. Filter 4g solids, disperse in a wide petridish and heat in an oven at 80 ℃ for 12 hours. The surface MgO agglomeration is removed and a high concentration of MgO-PE composite particles are obtained. As measured by TGA up to 600 ° C., the MgO fraction was determined to be 9.3%.

Example  3.

10g of spherical PMMA resin particles having a size of 10um and 1g of 80nm Ag nanoparticles are quantified and placed in a hybridizer capable of high-speed rotation and treated at 10,000 rpm for 5 minutes. 10 g of the obtained Ag-PMMA complex is dispersed in 100 mL of 1N nitric acid and reacted for 60 minutes. Filter 8g of solids, wash with distilled water, disperse in wide petridish and heat in 80 ℃ oven for 12 hours. An Ag-PMMA composite particle having no surface Ag aggregation is obtained. As a result of measuring the electrical conductivity of the prepared Ag-PMMA composite particles, the insulation resistance is confirmed to be 10 ⁶ Ohm or more.

Although the present invention has been described with reference to one embodiment shown in the accompanying drawings, this is merely exemplary, and it will be understood by those skilled in the art that various modifications and equivalent other embodiments are possible. Could be. Accordingly, the true scope of protection of the present invention should be determined only by the appended claims.

1 is an enlarged view of a conventional core cell nanocomposite.

FIG. 2 is an enlarged view showing that it is difficult to complex additional nanoparticles due to nanoparticles having partition walls formed outside the existing parent particles.

Figure 3 is a step showing a particle body from which the surface particle agglomeration is removed according to an embodiment of the present invention.

4 is an enlarged view showing polymer particles having hydrophobicity and nanoparticles having hydrophilicity.

5 is a step diagram showing an embodiment of the present invention, making a secondary dry composite, and dissolving it to produce a particle body having a high particle fraction.

Claims (11)

delete delete delete delete delete delete delete Preparing a primary dry composite by combining nanoparticles as subparticles with polymer particles as mother particles using a high speed rotating device; And Dispersing the primary dry composite in a solution for dissolving only the nanoparticles to remove the nanoparticles agglomerated on the surface of the primary dry composite, the nanoparticle composite is removed from the surface particles. Manufacturing a primary dry composite by combining nanoparticles as subparticles with polymer particles as mother particles using a high speed rotating device; Dispersing the primary dry composite in a solution in which only the nanoparticles are dissolved to remove nanoparticles agglomerated on the surface of the primary dry composite; Preparing a secondary dry composite by complexing the nanoparticles again using a high speed rotating device to the primary dry composite from which the nanoparticles agglomerated on the surface are removed; And Dispersing the secondary dry composite in a solution in which only the nanoparticles are dissolved, thereby removing nanoparticles agglomerated on the surface of the secondary dry composite. The method according to claim 8 or 9, The polymer particles as the mother particles are spherical polyethylene resin or spherical PMMA resin, characterized in that the nanocomposite particle production method. The method according to claim 8 or 9, The nanoparticles as the magnetic particles are nano-composite particle manufacturing method characterized in that the MgO or Ag.

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