KR20130028457A - Nano-particles typed inorganic ceramic coating composition having high dispersion stability and method for preparing the same - Google Patents

Nano-particles typed inorganic ceramic coating composition having high dispersion stability and method for preparing the same Download PDF

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KR20130028457A
KR20130028457A KR1020110092035A KR20110092035A KR20130028457A KR 20130028457 A KR20130028457 A KR 20130028457A KR 1020110092035 A KR1020110092035 A KR 1020110092035A KR 20110092035 A KR20110092035 A KR 20110092035A KR 20130028457 A KR20130028457 A KR 20130028457A
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weight
coating composition
parts
water
ceramic coating
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구영곤
김종길
백생규
이현표
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(주)바론에스엘
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14Colloidal silica, e.g. dispersions, gels, sols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16Antifouling paints; Underwater paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/20Diluents or solvents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/005Additives being defined by their particle size in general

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Abstract

The present invention relates to a method for dispersing an inorganic ceramic coating composition in the size of nanoparticles and to a method for producing dispersion stability by adding a water-soluble styrene or acrylic copolymer polymer resin together with nanoparticles of an inorganic ceramic coating composition. By commercializing, the coating composition has excellent storage stability, long-term storage and transportation is possible, and by coating on the surface of the material to be coated using the nanoparticle coating composition to commercialize it, it forms a high-strength smooth surface layer as well as The present invention relates to a ceramic coating composition having excellent appearance, surface gloss, adhesion, weather resistance, durability, stain resistance, chemical resistance, and the like.

Description

Nano-Particles Typed Inorganic Ceramic Coating Composition Having High Dispersion Stability And Method For Preparing The Same}

The present invention relates to an inorganic ceramic coating composition in the form of nanoparticles having excellent dispersion stability and a method for preparing the same. More specifically, the present invention comprises a styrene, acrylic or maleic acid water-soluble copolymer, an inorganic polymer binder, an alkoxysilane compound, a water-soluble organic solvent or a low molecular weight alcohol, a filler, a pigment, and water as a dispersant. It relates to an inorganic ceramic coating composition in the form of nanoparticles having a particle size and a method for preparing the same.

In general, inorganic paints and inorganic ceramic coating compositions have excellent properties such as heat resistance, weather resistance, fouling resistance, chemical resistance, and durability that cannot be compared with organic paints or organic coating compositions, but the specific gravity of inorganic paints and ceramic coating compositions Precipitation is likely to occur due to the high degree of 1 to 5 and poor dispersibility and dispersion stability. Due to the difficulty of grinding and processing, there is a limit to fine granulation, and the high-purity micro powder is too expensive to be suitable for commercial use of the general coating composition.

In addition, the conventional inorganic paints and inorganic coating compositions are significantly less dispersed stability of the product is transported in the container for a long time, or when stored in the warehouse for a long time, sediment occurs easily hardened from the bottom to lose product value and users productivity This has led to serious problems in economics.

Therefore, in the present invention, as a result of repeated studies to solve the problems of the conventional ceramic coating compositions, to find out that the storage stability can be greatly improved by pulverizing the composition of the specific components under specific conditions to complete the present invention Reached.

Accordingly, it is an object of the present invention to provide an inorganic ceramic coating composition in the form of nanoparticles and a method for producing the same which greatly improve storage stability.

1 is a schematic explanatory diagram of a particle impact high pressure dispersion machine used in the present invention.
2 is a schematic explanatory diagram of a horizontal bead disperser used in the present invention.
3 is a schematic explanatory diagram of a vertical bead disperser used in the present invention.

Summary of the Invention The first aspect according to the present invention is to provide an inorganic ceramic coating composition containing the following components and compositions and having a particle size of 0.1 nm to 1 μm, based on a total of 100 parts by weight of the composition:

(1) 1 to 25 parts by weight of a styrene-based, acrylic-based or maleic acid-based water-soluble copolymer as a water-soluble organic dispersant,

(2) 20 to 80 parts by weight of the inorganic polymer binder,

(3) 1 to 50 parts by weight of an alkoxysilane compound,

(4) 1 to 10 parts by weight of a water-soluble organic solvent,

(5) 5 to 50 parts by weight of a filler or pigment, and

(6) water (replenish up to 100 parts by weight).

The second aspect of the present invention is excellent dispersion stability by spraying the initial particles of the inorganic ceramic coating composition according to the present invention at a pressure of 1,000 psi ~ 40,000 psi, preferably 5,000 psi ~ 25,000 psi in a particle impact high pressure dispersion machine It is to provide a method for producing an inorganic ceramic coating composition in the form of nanoparticles.

According to a third aspect of the present invention, nanoparticles having excellent dispersion stability by spraying initial particles of the inorganic ceramic coating composition according to the present invention for 30 minutes to 3 hours at a rotational speed of 100 rpm to 5,000 rpm in a horizontal or vertical bead dispersion machine. It is to provide a method for producing an inorganic ceramic coating composition in the form of particles.

The inorganic ceramic coating composition according to the present invention may be dispersed using a particle impact high pressure disperser, a horizontal bead disperser or a vertical bead disperser.

In the case of using a particle impact high pressure dispersion machine, the initial particles of the inorganic ceramic coating composition according to the present invention are sprayed at a discharge pressure of 1,000 psi to 40,000 psi, preferably 5,000 psi to 25,000 psi, thereby causing the particles to collide with each other. An acid stable composition is obtained. If the discharge pressure is less than 1,000 psi, the dispersing capacity is lowered. If the discharge pressure is higher than 40,000 psi, the dispersing capacity is good, but the life of the dispersing equipment is rapidly decreased.

In the case of using zirconia beads or yttria beads in a horizontal bead disperser, the initial particles of the inorganic ceramic coating composition according to the present invention are sprayed at a rotational speed of 100 rpm to 5,000 rpm to act as a dispersant in the coating composition and between the beads and the beads. By rotational friction, a composition having a stable dispersibility is obtained. The diameter of the beads used in such a horizontal bead disperser is 0.1 mm to 5 mm, preferably 0.1 mm to 1.5 mm. If the diameter of the beads is less than 0.1mm it is difficult to classify with the product, if larger than 1.5mm the dispersion capacity is poor.

Initial particles of the inorganic ceramic coating composition according to the present invention may be dispersed using a vertical bead disperser. The vertical bead disperser is the same as the horizontal bead disperser but slightly superior in terms of dispersion efficiency.

Water-soluble organic dispersants that can be used in the present invention include styrene- (meth) acrylic acid copolymer, styrene- (meth) acrylic acid alkyl ester copolymer, styrene-maleic acid copolymer, maleic acid-maleic anhydride copolymer , Polyethylene glycol mono (meth) acrylate, methoxy polyethylene glycol (meth) acrylate, and the like, and these can be used alone or in combination of two or more thereof.

In the present invention, by using a water-soluble organic dispersant by adjusting the degree of crosslinking between organic and inorganic to ensure the dispersibility by physical energy, thereby improving the dispersion stability as possible.

According to the invention, the water-soluble organic dispersant is used in an amount of 1 to 25 parts by weight, preferably 3 to 15 parts by weight, based on 100 parts by weight of the total composition. If the amount of the water-soluble organic dispersant is less than 1 part by weight, the dispersibility is poor. If the amount of the water-soluble organic dispersant is used more than 25 parts by weight, the dispersibility is good. Restrictions may apply when used for applications of heated cookware.

Inorganic polymer binders that can be used in the present invention include colloidal silica (pH 9 ~ 10.5, solid content 20 ~ 30% by weight, particle size 10 ~ 20 ㎛), colloidal alumina (pH 8.5 ~ 10.5, solid content 20 ~ 50% by weight , Particle size 5-100 μm) or the like, and these may be used alone or in combination.

According to the present invention, the inorganic polymer binder is used in an amount of 20 to 80 parts by weight, preferably 30 to 70 parts by weight. If the amount of the inorganic polymer binder is less than 20 parts by weight, the viscosity of the composition cannot be adjusted. If the amount of the inorganic polymer binder is greater than 80 parts by weight, the composition ratio of the inorganic polymer binder is too high, so that the composition ratio of the filler is relatively low.

Alkoxysilane compounds that can be used in the present invention include methyltrimethoxysilane, ethyltrimethoxysilane, methyltriethoxysilane, ethyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, phenyltrimethoxysilane And diphenyldimethoxysilane, and these can be used alone or in combination of two or more thereof.

Although the chemical formula of an alkoxysilane compound is represented by R-Si (OR ') n, functional groups R and R' have a C1-C5 alkyl group, an acyl group, or a phenyl group, n is 2-3. According to the present invention, when the functional group of the silane compound is larger than 3, the silane compound having a small functional group may be deteriorated due to mutual failure of the large functional group during the aging process and tend to gel, which may adversely affect the stability of the product. It is advantageous to use.

According to the present invention, the alkoxysilane compound is used in an amount of 1 to 50 parts by weight, preferably 5 to 40 parts by weight, based on 100 parts by weight of the total composition. Since the alkoxysilane compound serves to modify the surface of the inorganic polymer binder and to control the degree of crosslinking of hydroxyl groups present at the ends of the composition, it is difficult to control the hardness and strength of the coating film outside the above range. In other words, when the amount of the alkoxysilane compound used is less than 1 part by weight, the hardness and gloss of the coating film may be degraded. If the amount of the alkoxysilane compound is higher than 50 parts by weight, cracking of the coating film may occur after curing.

Water-soluble organic solvents that can be used in the present invention include low molecular weight alcohols such as methanol, ethanol, isopropanol, butyl cellosolve, and the like, and these may be used alone or in combination of two or more thereof. They should be polar organic solvents, the use of a non-polar organic solvent is less compatible, may adversely affect the dispersion stability, and may cause gelation side effects.

According to the present invention, the water-soluble organic solvent is used in an amount of 1 to 10 parts by weight based on 100 parts by weight of the entire composition. If the amount of the water-soluble organic solvent is less than 1 part by weight, curing of the coating film may be delayed. If the amount of the water-soluble organic solvent is more than 10 parts by weight, pinholes (pinholes, needle marks, or bear marks) may be formed in the coating film.

Inorganic fillers that can be used in the present invention include known calcium carbonate (CaCO 3 ), calcium oxide (CaO), calcium hydrooxide (Ca (OH) 2 ), zirconium oxide (ZrO 2 ), silicon oxide (SiO 2 ), Zinc Oxide (ZnO), Aluminum Oxide (Al 2 O 3 ), Aluminum Hydrooxide (Al (OH) 3 ), Silicon Carbide (SiC), Talc (3MgO.4SiO 2 .H 2 O) and Cobalt Oxide (Co 3 O 4 ), chromium oxide (CrO 3 ), and the like, and one or two or more thereof may be mixed and used. If necessary, a mixture of colored inorganic pigments, inorganic antimicrobial agents, and metal powders may be used.

The colored inorganic pigments that can be used in the present invention include titanium oxide (TiO 2 / Rutile) as a white pigment, zinc oxide, silver white, bengala, vermilion, cadmium red, iron oxide (Fe 2 O 3 , Fe 3 O as a red pigment 4 ), yellow pigments such as chrome yellow, cadmium yellow, titanium yellow, blue pigments such as Prussian blue, cobalt blue, black pigments such as carbon black, iron black, etc., of which one or two or more thereof may be mixed and used. .

According to the present invention, the inorganic filler and the pigment are used in an amount of 5 to 50 parts by weight, and preferably in an amount of 15 to 40 parts by weight, based on 100 parts by weight of the total composition. At this time, the average particle diameter of the filler or inorganic pigment is 10 ~ 45 ㎛ used one or two or more kinds, if the filler input amount is 5 parts by weight or less, the composition ratio of the filler is not low to form a strong coating film, drying is slow It has low rise and low adhesion. On the contrary, when the amount of the filler or pigment is more than 50 parts by weight, the composition ratio of the filler may be too high, resulting in cracking of the coating film. In the present invention, "rise" means that the coating film easily comes up when the coating (spray method, etc.) is used. If the amount of the filler is out of the above range, it is difficult to form a coating film of a suitable thickness.

The water used in the present invention is replenished until it is 100 parts by weight based on the total weight of the composition.

Hereinafter, the present invention will be described in more detail with reference to Examples.

[Example]

(Production of composition)

Example  One

The component ratios of the compositions according to the invention were prepared as follows.

2.5 kg of styrene- (meth) acrylic acid copolymer as a water-soluble organic dispersant, 35 kg of colloidal silica as an inorganic polymer binder, 5 kg of methyltrimethoxysilane as an alkoxysilane compound and 10 kg of distilled water were added to a 200 liter mixing tank. While stirring, 8 kg of isopropanol as a water-soluble organic solvent, 2.5 kg of styrene maleic acid copolymer as a water-soluble organic dispersant, and 2 kg of butyl cellosolve as a water-soluble organic solvent were added and mixed uniformly, followed by titanium oxide (TiO 2 / Rutile) as a pigment. 15 kg and 20 kg of zirconium oxide (ZrO 2 ) were slowly added as a filler, followed by stirring for 30 minutes to obtain a homogeneous composition.

Example  2 to 10

The composition was prepared in the same manner as in Example 1 by varying the composition ratio as shown in Table 1 below.

ingredient Example One 2 3 4 5 6 7 8 9 10 Styrene (meth) acrylic acid copolymer 2.5 0.5 1.5 3.5 4.5 5.5 6.5 7.5 10 12.5 Styrene-maleic acid copolymer 2.5 0.5 1.5 3.5 4.5 5.5 6.5 7.5 10 12.5 Colloidal silica 35 36 35 34 33 32 31 30 30 30 Methyltrimethoxysilane 5.0 6.0 7.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 Isopropyl alcohol 8.0 - - 7.0 - - 6.0 - - 5.0 ethanol - 8.0 - - 7.0 - - 6.0 - - Methanol - - 8.0 - - 7.0 - - 6.0 - Butyl Cellosolve 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 Titanium oxide 15 - - - - 15 - - - - Zirconium oxide 20 20 20 20 20 20 20 18 15 12 Black pigment - 15 - - - - 15 - - - Blue pigment - - 15 - - - - 15 - - Red pigment - - - 15 - - - - 14 - Yellow pigment - - - - 15 - - - - 12 Distilled water 10 12 10 10 9.0 9.0 8.0 9.0 8.0 9.0

(Preparation of Nanoparticle Form Composition Using High Pressure Impact Disperser)

Example  11

The main composition of the coating composition was prepared by passing the composition obtained in Example 1 five times at a discharge pressure of 20,000 psi in a high pressure impact disperser. As a result of analyzing the degree of dispersion of the particles, as shown in Table 2 below, an average particle diameter was 313 nm, but a dispersion composition containing 4.7% of some undispersed additives in the range of 2.6 μm to 5.5 μm was obtained.

Figure pat00001

Example  12 to 20

In the present embodiments, the composition of the corresponding embodiment (for example, the composition of Example 3 in Example 13) is used, and the discharge pressure, the number of injections, and the average particle diameter of the high pressure impact disperser are different as shown in Table 3 below. A composition was prepared in the same manner as in Example 11 except for one. Particle size distribution graphs for Examples 12 to 20 are omitted for convenience.

(Evaluation of dispersion stability)

Very good (◎): The average particle diameter after dispersion is 350nm or less, the dispersion composition is kept in a container and left for 48 hours, after which the precipitate at the bottom is uniformly loosened and mixed even under minute shaking.

Good (○): The average particle diameter after dispersion is 600nm or less, the dispersion composition is stored in a container and left to stand for 48 hours.

Moderate (△): The average particle diameter after dispersion is 1000nm or less, the dispersion composition is stored in a container and left for 48 hours, after the precipitate at the bottom shakes 3 to 5 times, it is uniformly loosened and mixed.

Poor (X): The average particle diameter after dispersion is 1000nm or more, the dispersion composition is stored in a container and left for 48 hours, and even if the precipitate on the bottom is shaken 3 to 5 times, it is not mixed uniformly.

Very poor (XX): The average particle size after dispersing is 1500nm or more, the dispersion composition is stored in a container and left for 48 hours, after which the sediment on the bottom hardens like mud or sand and does not mix uniformly even when shaken vigorously.

Example 11 12 13 14 15 16 17 18 19 20 Discharge pressure
(psi)
20,000 18,000 15,000 10,000 9,000 7,000 5,000 3,000 2,000 1,000
Number of injections 5 5 5 5 5 5 5 5 5 5 Average particle diameter
(nm)
313 337 350 412 582 774 969 1737 3360 5000
More than
Dispersion stability X XX XX

Preparation of Composition in Nanoparticle Form Using Horizontal Bead Disperser

Example  21

The composition obtained in Example 1 was filled with yttria beads of 0.4 mm in diameter in a horizontal bead disperser and dispersed at 300 rpm for 30 minutes, and then the rotor speed was increased to 1,500 rpm for 3 hours. The subject matter of the coating composition was prepared. As a result of analyzing the degree of dispersion of the particles, as shown in Table 4 below, a dispersion composition having an average particle diameter of 235 nm and a maximum particle size of 615 nm was obtained.

Figure pat00002

Example  22 to 30

In the present examples, the composition of the corresponding example (e.g., composition of Example 3 in Example 23) is used, except that the size of the beads in the horizontal bead disperser is varied as shown in Table 5 below. The composition was prepared in the same manner as in Example 21. Particle size distribution graphs for Examples 22 to 30 are omitted for convenience.

Example 21 22 23 24 25 26 27 28 29 30 Yttria bead
Diameter (0.4mm)
0.4 0.1 0.2 0.3 0.5 - - - - -
Zirconia Bead Diameter (0.3mm) - - - - - 0.7 1.0 1.5 2.0 3.0 Initial rotation speed *
Main rotation speed **
(rpm)
300
1500
300
1500
300
1500
300
1500
300
1500
300
1500
300
1500
300
1500
300
1500
300
1500
Average particle diameter
(nm)
235 159 187 201 257 320 468 727 1590 3278
Dispersion stability X XX

Initial rotation is carried out for 30 minutes.

** This rotation is performed for 3 hours.

Preparation of Composition Using Vertical Bead Disperser

Example  31

The composition obtained in Example 1 was filled with yttria beads having a diameter of 0.3 mm in a vertical bead disperser and dispersed for 30 minutes at a rotational speed of 300 rpm for 30 minutes, followed by raising the rotational speed of the rotor at 1,500 rpm for 3 hours. The subject matter of the coating composition was prepared. As a result of analyzing the dispersion degree of the particles, as shown in Table 6 below, a dispersion composition having an average particle diameter of 199 nm and a maximum particle size of 531 nm was obtained.

Figure pat00003

Example  32 to 40

The present examples use the composition of the corresponding example (e.g., the composition of Example 3 in Example 33), use yttria beads or zirconia beads in a vertical bead disperser, The composition was prepared in the same manner as in Example 31, except for the following differences. Particle size distribution graphs for Examples 32 to 40 are omitted for convenience.

Example 31 32 33 34 35 36 37 38 39 40 Yttria bead diameter (0.4mm) 0.3 0.1 0.2 0.4 0.5 - - - - - Zirconia Beads (Diameter 0.3mm) - - - - - 0.7 1.0 1.5 2.0 3.0 Initial rotation speed *
Main rotation speed **
(rpm)
300
1500
300
1500
300
1500
300
1500
300
1500
300
1500
300
1500
300
1500
300
1500
300
1500
Average particle diameter
(nm)
199 151 172 224 238 333 450 696 1320 2987
Dispersion stability X XX

Initial rotation is carried out for 30 minutes.

** This rotation is performed for 3 hours.

(Preparation of Composition Using High Pressure Impact Disperser and Horizontal Bead Disperser)

Example  41

After passing through the composition obtained in Example 1 three times at a discharge pressure of 15,000 psi in a high-pressure impact disperser, 70% of yttria beads having a diameter of 0.2 mm were filled in a horizontal bead disperser and dispersed at a rotational speed of 1,500 rpm for 3 hours. To prepare the subject of the coating composition. As a result of analyzing the dispersion degree of the particles, as shown in Table 8 below, a dispersion composition having an average particle diameter of 157 nm and a maximum particle size of 615 nm was obtained.

Figure pat00004

Example  42 to 50

In the present examples, the composition of the corresponding example (for example, the composition of Example 3 in Example 43) is used, except that the rotational speed in the vertical bead disperser is varied as shown in Table 9 below. A composition was prepared in the same manner as in Example 41. Particle size distribution graphs for Examples 42 to 50 are omitted for convenience.

Example 41 42 43 44 45 46 47 48 49 50 Composition ratio example One 2 3 4 5 6 7 8 9 10 High Pressure Impact Disperser Pressure (psi)
Number of injections

15,000
3

15,000
3

15,000
3

15,000
3

15,000
3

15,000
3

15,000
3

15,000
3

15,000
3

15,000
3
Horizontal Bead
Disperser
Rotational Speed *
(rpm)

1,500

1,500

1,500

1,500

1,500

1,500

1,500

1,500

1,500

1,500
Average particle diameter
(nm)
157 161 159 148 147 579 310 265 141 139
Dispersion stability X

Rotation is carried out for 3 hours.

Comparative example  One

After the composition obtained in Example 1 was filled with glass beads having a diameter of 1.5 mm in a conventional dissolver and dispersed at 1,500 rpm for 3 hours, the main composition of the coating composition was prepared. As a result of analyzing the degree of dispersion of the particles, as shown in Table 10 below, a dispersion composition was obtained in a state beyond the measurement limit of the nanoparticle size analyzer.

Figure pat00005

Comparative example  2 to 6

In the comparative examples, a composition was prepared in the same manner as in Comparative Example 1 except for using the composition of the corresponding example (for example, the composition of Example 3 in Comparative Example 3). Particle size distribution graphs for Comparative Examples 2 to 6 are omitted for convenience.

Comparative example  7

The composition was prepared according to the method of Example 21, with the composition from which the dispersant was removed from the components of the composition of Example 1. The particle size distribution and dispersion stability of the composition are shown in Table 11 below.

Comparative example  8

The composition was prepared according to the method of Example 21, wherein the composition from which the polymeric binder was removed from the components of the composition of Example 1 was prepared. The particle size distribution and dispersion stability of the composition are shown in Table 11 below.

Comparative example  9

A composition prepared by removing the alkoxysilane compound from the components of the composition of Example 1 was prepared according to the method of Example 21. The particle size distribution and dispersion stability of the composition are shown in Table 11 below.

Comparative example  10

The composition which removed the organic solvent among the components of the composition of Example 1 was prepared according to the method of Example 21. The particle size distribution and dispersion stability of the composition are shown in Table 11 below.

Comparative Example One 2 3 4 5 6 7 8 9 10 Particle size distribution
(nm)
3500
More than
3500
More than
3500
More than
3500
More than
3500
More than
4500
More than
670 Come 590 542
Dispersion stability X X X X X XX XX

Claims (12)

An inorganic ceramic coating composition having a particle size of 0.1 nm to 1 μm, based on a total of 100 parts by weight of the composition:
(1) 1 to 25 parts by weight of a styrene-based, acrylic-based or maleic acid-based water-soluble copolymer as a water-soluble organic dispersant,
(2) 20 to 80 parts by weight of the inorganic polymer binder,
(3) 1 to 50 parts by weight of an alkoxysilane compound,
(4) 1 to 10 parts by weight of a water-soluble organic solvent,
(5) 5 to 50 parts by weight of a filler or pigment, and
(6) water (replenish up to 100 parts by weight).
The water-soluble organic dispersant according to claim 1, wherein the water-soluble organic dispersant is a styrene- (meth) acrylic acid copolymer, a styrene- (meth) acrylic acid alkyl ester copolymer, a styrene-maleic acid copolymer, a maleic acid-maleic anhydride copolymer, polyethylene glycol mono (meth) acrylic acid A composition which is 1 type, or 2 or more types of mixtures chosen from the group which consists of a rate and a methoxy polyethyleneglycol (meth) acrylate. According to claim 1, wherein the inorganic polymer binder is colloidal silica (PH 9 ~ 10.5, solid content 20-30% by weight, particle size 10-20 ㎛), colloidal alumina (PH 8.5-10.5, solid content 20-50% by weight, Particle size 5-100 μm) or a mixture thereof. The alkoxysilane according to claim 1, wherein the alkoxysilane is methyltrimethoxysilane, ethyltrimethoxysilane, methyltriethoxysilane, ethyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, phenyltrimethoxysilane, di 1 or 2 or more types of mixtures selected from the group consisting of phenyldimethoxysilane. The composition according to claim 1, wherein the low molecular weight alcohol as the water-soluble solvent is one or a mixture of two or more selected from the group consisting of butyl cellosolve, methanol, ethanol and isopropanol. Based on a total of 100 parts by weight of the composition, the initial particles of the inorganic ceramic coating composition comprising the following components and compositions were 1 to 10 times at a pressure of 1,000 psi to 40,000 psi, preferably 5,000 psi to 25,000 psi, in a particle impact high pressure disperser. Process for preparing an inorganic ceramic coating composition in the form of nanoparticles having a particle size of 0.1 nm to 1 μm by spraying:
(1) 1 to 25 parts by weight of a styrene-based, acrylic-based or maleic acid-based water-soluble copolymer as a water-soluble organic dispersant,
(2) 20 to 80 parts by weight of the inorganic polymer binder,
(3) 1 to 50 parts by weight of an alkoxysilane compound,
(4) 1 to 10 parts by weight of a water-soluble organic solvent,
(5) 5 to 50 parts by weight of a filler or pigment, and
(6) water (replenish up to 100 parts by weight).
The water-soluble organic dispersant according to claim 6, wherein the water-soluble organic dispersant is a styrene- (meth) acrylic acid copolymer, a styrene- (meth) acrylic acid alkyl ester copolymer, a styrene-maleic acid copolymer, a maleic acid-maleic anhydride copolymer, a polyethylene glycol mono (meth) acrylic A method for producing an inorganic ceramic coating composition in the form of nanoparticles, which is one or a mixture of two or more selected from the group consisting of acrylates, methoxy polyethylene glycol (meth) acrylates. The method of claim 6, wherein the inorganic polymer binder is colloidal silica (PH 9 ~ 10.5, solid content 20-30% by weight, particle size 10-20㎛), colloidal alumina (PH 8.5-10.5, solid content 20-50% by weight, Particle size 5 ~ 100 ㎛) or a mixture thereof, a method for producing an inorganic ceramic coating composition in the form of nanoparticles. 7. The alkoxysilane according to claim 6, wherein the alkoxysilane is methyltrimethoxysilane, ethyltrimethoxysilane, methyltriethoxysilane, ethyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, phenyltrimethoxysilane, di A method for producing an inorganic ceramic coating composition in the form of nanoparticles, which is one or a mixture of two or more selected from the group consisting of phenyldimethoxysilane. The method for producing an inorganic ceramic coating composition according to claim 6, wherein the low molecular weight alcohol is one or two or more mixtures selected from the group consisting of butyl cellosolve, methanol, ethanol and isopropanol as a water-soluble solvent. . The inorganic ceramic coating composition according to any one of claims 6 to 9, wherein the initial particles of the inorganic ceramic coating composition are sprayed at a rotational speed of 100 rpm to 5,000 rpm in a horizontal or vertical bead disperser. Way. 10. The inorganic system according to any one of claims 6 to 9, wherein the initial particles of the inorganic ceramic coating composition are first dispersed in a high pressure dispersion machine and then secondly dispersed in a horizontal or vertical bead dispersion machine. A method of making a ceramic coating composition.
KR1020110092035A 2011-09-09 2011-09-09 Nano-particles typed inorganic ceramic coating composition having high dispersion stability and method for preparing the same KR20130028457A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20150039185A (en) * 2015-03-17 2015-04-09 (주)나노엘엔피 Ceramic composition and method for manufacturing the same, and heat radiating member using the same
CN105017843A (en) * 2015-07-27 2015-11-04 华南理工大学 Powdery silane coupling agent additive and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20150039185A (en) * 2015-03-17 2015-04-09 (주)나노엘엔피 Ceramic composition and method for manufacturing the same, and heat radiating member using the same
CN105017843A (en) * 2015-07-27 2015-11-04 华南理工大学 Powdery silane coupling agent additive and preparation method thereof

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