KR101321691B1 - Infrared reflectance paint containing black, blue or green infrared reflectance pigment and manufacturing method thereof - Google Patents

Abstract

PURPOSE: A manufacturing method of an infrared ray shielding paint is provided to offer the infrared ray shielding paint having increased reflectance of the infrared ray and visible light by using platy black, blue, or green infrared shielding pigment in which a metallic oxide is covered with optimized thickness ratio. CONSTITUTION: A manufacturing method of an infrared ray shielding paint comprises: a step of making a slurry by dispersing the shielding pigment power of black, blue, or green infrared throughout the dispersion and stirring the dispersion at 10-30°C (S10); a step of making an infrared shielding pigment ink by dispersing a metallic oxide throughout the slurry (S20); a step of making an infrared reflecting material by covering the infrared shielding pigment with the metallic oxide by adding metallic salt and acid to the infrared shielding pigment ink to have a pH of 2-3 (S30); and a step of mixing the infrared reflecting material, a binder, an antifoaming agent, and a dispersing agent (S40). [Reference numerals] (AA) Start; (BB) End; (S10) Stirring step; (S20) Dispersing step; (S30) Covering step; (S40) Mixing step

Description

INFRARED REFLECTANCE PAINT CONTAINING BLACK, BLUE OR GREEN INFRARED REFLECTANCE PIGMENT AND MANUFACTURING METHOD THEREOF}

The present invention relates to a paint, and more particularly, to an infrared shielding paint including a plate-like black, blue or green pigment coated with a single layer or multiple layers of a metal oxide and a method of manufacturing the same. In particular, a coating material having a high reflectance in the infrared region, high visible light in the 280 to 2500 nm region, and an infrared shielding property, and having a stable infrared shielding layer with little change in chromaticity even when exposed to external light for a long time, a method of manufacturing the same, and a double layer manufactured thereby It relates to a coating film.

As the urbanization progresses, the surface temperature of concrete or steel in the middle of summer due to solar heat is increased due to the decrease of the green area and water surface, which increases the cooling load inside the building and heats up the heat island. Effect). In order to cope with this, the demand for energy-efficient materials is soaring in Korea.

As an infrared shielding material which has high infrared reflectance and high infrared shielding property in an infrared region, the material which coats the resin composition which blocks infrared rays and reflects and shields the light of an infrared region is known.

In addition, it is known to use various thermoplastic resins, such as polyester resin, acrylic resin, polyurethane resin, polyolefin resin, and polycarbonate resin, for the resin material used for forming a coating film.

However, the coating method using the organic pigment as described above has a problem that not only lowers the light resistance and heat resistance of the pearlescent pigment, but also increases the manufacturing cost.

In addition, in recent years, due to the difficulty of power supply and demand, as the demand of the infrared shield is soaring, a pigment having an infrared blocking function as well as aesthetics is required.

Japanese Laid-Open Patent Publication JP 2006-335949 Korean Registered Patent Publication No. 10-1123151

Accordingly, an object of the present invention is to solve such a conventional problem, and by using it as a plate-shaped black, blue or green infrared car pigment coated with metal oxide at an optimized thickness ratio, the reflectance of visible light and infrared light is increased. To provide an infrared shielding paint.

In addition, by using an inorganic pigment, to provide an infrared shielding paint with increased weather resistance, heat resistance and chemical resistance.

In addition, by using an infrared shielding pigment of black, blue or green, it is to provide an infrared shielding coating excellent in aesthetic sense.

The object comprises a binder, an infrared reflecting material, an antifoaming agent and a dispersing agent according to the present invention, wherein the infrared reflecting material is a plate-like black, blue or green infrared shielding pigment coated with a single layer or multiple layers of metal oxides. Is achieved by an infrared shielding paint comprising a black, blue or green infrared shielding pigment.

In addition, the infrared shielding paint may be 20 to 50 parts by weight of the infrared reflecting material, 20 to 25 parts by weight of the antifoaming agent, and 10 to 15 parts by weight of the dispersant based on 100 parts by weight of the binder.

In addition, the binder may be any one selected from the group consisting of an acrylic resin, an acrylic-silicone copolymer, a silicone resin, a water-soluble polyurethane resin, an acrylic-urethane copolymer, and an acrylic-silicon-urethane copolymer.

In addition, the infrared shielding pigment may be at least one of synthetic mica, natural mica, glass flake, iron oxide, titanium oxide, alumina, magnesium oxide, aluminum, calcium oxide, zinc oxide mica or mica titanium.

In addition, the infrared shielding pigment may have a width of 5 to 50 µm and a thickness of 0.2 to 5 µm.

In addition, the metal oxide may be at least one of titanium dioxide, cobalt, iron oxide, cobalt, iron-cyanide salt (Fe ₄ (Fe (CN) ₆ ) ₃ ), cobalt alumina (CoAl ₂ O ₄ ) or chromium oxide. have.

In addition, the infrared reflecting material may be a ratio of the length of the infrared reflecting pigment longitudinal direction and the thickness of the metal oxide 100: 0.01 to 100: 12.

In addition, the stirring step of dispersing the black, blue or green infrared shielding pigment powder in the dispersion and stirring at 10 to 30 ℃ temperature to prepare a suspension, the dispersion step of dispersing the metal oxide in the suspension to produce the infrared shielding pigment ink, A coating step and an infrared reflecting material and a binder to prepare an infrared reflecting material by coating the metal oxide on the infrared shielding pigment in a single layer or a multilayer by adding an acid while adjusting the metal salt and pH 2 to 3 to the infrared shielding pigment ink. It is achieved by an infrared shielding paint manufacturing method including a black, blue or green infrared shielding pigment, characterized in that it comprises a mixing step of mixing a defoaming agent and a dispersant.

In addition, the infrared shielding paint may be 20 to 50 parts by weight of the infrared reflecting material, 20 to 25 parts by weight of the antifoaming agent, and 10 to 15 parts by weight of the dispersant based on 100 parts by weight of the binder.

In addition, the binder may be any one selected from the group consisting of an acrylic resin, an acrylic-silicone copolymer, a silicone resin, a water-soluble polyurethane resin, an acrylic-urethane copolymer, and an acrylic-silicon-urethane copolymer.

In addition, the infrared shielding pigment may be at least one of synthetic mica, natural mica, glass flake, iron oxide, titanium oxide, alumina, magnesium oxide, aluminum, calcium oxide, zinc oxide mica and mica titanium.

In addition, the infrared shielding pigment may have a width of 5 to 50 µm and a thickness of 0.2 to 5 µm.

In addition, the metal oxide may be at least one of titanium dioxide, cobalt, iron oxide, cobalt, iron-cyanide salt (Fe ₄ (Fe (CN) ₆ ) ₃ ), cobalt alumina (CoAl ₂ O ₄ ) or chromium oxide. have.

In addition, the infrared reflecting material may be a ratio of the length of the infrared reflecting pigment longitudinal direction and the thickness of the metal oxide 100: 0.01 to 100: 12.

In addition, a binder, an infrared reflecting material, an antifoaming agent and a dispersing agent, wherein the infrared reflecting material is black, blue or green, characterized in that the plate-like black, blue or green infrared shielding pigment coated with a single layer or multiple layers. It is achieved by an infrared shielding coating film containing an infrared shielding pigment.

At this time, further comprising an insulating pigment, the insulating pigment may be any one selected from the group consisting of aluminosilicate, hollow glass beads, hollow silica, hollow polymer, inorganic silicate, borosilicate and chromite.

A top coat layer comprising a binder, an infrared reflecting material, an antifoaming agent and a dispersing agent, and an undercoat layer comprising the binder, the antifoaming agent, the dispersing agent, and the heat insulating pigment, wherein the infrared reflecting material is coated with a single layer or multiple layers of metal oxides. It is a plate-like black, blue or green infrared shielding pigment, and the insulating pigment may be any one selected from the group consisting of aluminosilicate, hollow glass beads, hollow silica, hollow polymer, inorganic silicate, borosilicate and chromite. .

In addition, the infrared reflecting material of the infrared shielding coating film may be a ratio of the length of the infrared reflecting pigment longitudinal direction and the metal oxide thickness of 100: 0.01 to 100: 12.

According to the present invention, by using an infrared shielding paint including a black, blue or green infrared shielding pigment coated with a ratio of the infrared reflecting pigment longitudinal length and the metal oxide thickness of 100: 0.01 to 100: 12, in the visible and infrared regions The reflectance is increased and the infrared shielding function is increased.

In addition, one of synthetic mica, natural mica, glass flake, iron oxide, titanium oxide, alumina, magnesium oxide, aluminum, calcium oxide, zinc oxide mica and mica titanium, which are inorganic heat resistant pigments, are relatively heat resistant instead of organic pigments. By using, it is possible to manufacture an infrared shielding coating excellent in weather resistance, light resistance, heat resistance and chemical resistance.

In addition, by using infrared reflecting pigments of black, blue or green, not only has excellent aesthetics, but also when used in buildings or exteriors of vehicles, it effectively shields infrared rays from the sun and thus has a shielding function that suppresses an increase in indoor temperature. Cooling energy can be saved.

1 is a flow chart related to an infrared shielding paint manufacturing method including a black, blue or green infrared shielding pigment of the present invention,
2 is a graph showing the surface temperatures of Examples 1 to 3 and Comparative Examples 1 and 2,
3 is a graph showing the surface temperatures of Examples 7 to 10 and Comparative Examples 3 to 4.
4 is a graph showing surface temperatures of Examples 11 to 14 and Comparative Examples 5 to 6. FIG.

Hereinafter, with reference to the accompanying drawings, a preferred embodiment of the present invention with respect to an infrared shielding paint including a black, blue or green infrared shielding pigment according to the present invention and a manufacturing method thereof. The present invention may be better understood by the following examples, which are intended to illustrate the present invention and are not intended to limit the scope of protection defined by the appended claims.

The present invention relates to an infrared shielding paint, and includes a binder, an infrared reflecting material, an antifoaming agent, and a dispersing agent.

In this case, the binder is a raw material that influences the physical properties such as durability and weather resistance of the paint. In the case of the exterior infrared shielding paint, the weather resistance and durability should be excellent, and the solar coating reflects pollutants due to the pollutants. It should be excellent in stain resistance so as not to degrade.

Thus, the binder may be selected from the group consisting of acrylic resins, acrylic-silicone copolymers, silicone resins, water-soluble polyurethane resins, acrylic-urethane copolymers, and acrylic-silicone-urethane copolymers, preferably acrylic resins. .

In addition, the infrared reflecting material of the present invention uses a plate-shaped black, blue or green infrared shielding pigment in which the metal oxide is monolayered or multi-layered, or preferably coated with three layers. In order to improve the shielding performance, a low refractive index plate-shaped infrared shielding pigment is coated with a high refractive index metal oxide so that the amount of light is reflected by reflection and scattering due to the difference in refractive index among the infrared shielding pigments. For sake.

Thus, the infrared shielding pigment is at least one of synthetic mica, natural mica, glass flakes, iron oxide, titanium oxide, alumina, magnesium oxide, aluminum, calcium oxide, zinc oxide mica and mica titanium, preferably oxidized It may be titanium.

In addition, in order to increase the reflectance and scattering rate as the infrared shielding pigment, the width of the infrared shielding pigment particles may be 5 to 50 ㎛, preferably 9 to 25 ㎛, plate thickness of 0.2 to 5 ㎛ may be. .

In addition, the infrared reflecting material may be a ratio of the length of the infrared reflecting pigment longitudinal direction and the thickness of the metal oxide 100: 0.01 to 100: 12.

In the present invention, the metal oxide used as a coating material for coating the infrared shielding pigment may use an inorganic pigment having a refractive index of 1.5 or more in order to increase the solar reflectance to exhibit shielding performance.

Accordingly, the metal oxide may be at least one of titanium dioxide, cobalt, iron oxide, cobalt, iron-cyanide salt (Fe ₄ (Fe (CN) ₆ ) ₃ ), cobalt oxide alumina (CoAl ₂ O ₄ ), or chromium oxide. May be cobalt oxide alumina, green may be chromium oxide, or black may be iron oxide and cobalt. This improves the concealment rate of the paint and increases heat resistance by suppressing the reception of heat in the coating by reflecting light.

Antifoaming agent is possible to use the antifoaming agent generally used in the art, preferably mineral oil-based or silicone-based antifoaming agent can be used, to remove unnecessary or harmful bubbles in the paint.

Dispersants may also be used in general dispersants used in the manufacture of coatings, naphthalene sulfonate formalin condensates, melamine sulfonate formalin condensates, polycarboxylic compounds, polycarboxylic ethers, aromatic amino sulfonic acid polymers and metal salts of lignin sulfonic acids It may be one or more materials selected from the group consisting of.

In addition, freeze stabilizers, thickeners, pH regulators, sedimentation agents and the like used in conventional paints may be added to improve paint properties, and these additives may be 0.05 to 20% by weight relative to the total weight.

In this case, propylene glycol, ethylene glycol may be used as the freeze-stabilizer, and the thickener may be a hydroxyethyl cellulose, a urethane-based thickener may be partially used to complement smooth workability. The pH adjusting agent may be 2-amino-2-methyl-1-propenol, and preservatives may be isothiazophone.

In addition, an insulating pigment may be further added, and the insulating pigment may be any one selected from the group consisting of aluminosilicate, hollow glass beads, hollow silica, hollow polymer, inorganic silicate, borosilicate, chromite, and the like. For example, it may be hollow glass beads. In a preferred embodiment of the present invention, undercoat systems with good thermal insulation performance use hollow glass beads having a low thermal conductivity of 0.047-0.2 W / m · K in various inorganic fillers. Preferably 5 to 10% by weight of hollow glass beads having a particle size of 30-120㎛. In particular, the hollow glass beads have a low oil absorption compared to other pigments to maintain the storage stability of the paint, and improve the painting workability. It is also used as an insulator for very good heat since it is in the form of a closed cell.

In addition, the infrared shielding paint may be 20 to 50 parts by weight of the infrared reflecting material, 20 to 25 parts by weight of the antifoaming agent, and 10 to 15 parts by weight of the dispersant based on 100 parts by weight of the binder.

Hereinafter, a method for preparing an infrared shielding paint including a black, blue or green infrared shielding pigment according to the present invention will be described in detail.

1 is a flow chart showing a method for manufacturing an infrared shielding paint including a black, blue or green infrared shielding pigment according to the present invention.

Referring to Figure 1, an infrared shielding paint manufacturing method including a black, blue or green infrared shielding pigment according to the present invention, the stirring step (S10), dispersion step (S20), coating step (S30) and mixing step (S40) Include.

Stirring step (S10) is a step of preparing a suspension by dispersing the black, blue or green infrared shielding pigment powder in the dispersion in a mixed vessel at 200 to 400rpm at a temperature of 10 to 30 ℃.

In this case, the black, blue or green infrared shielding pigment powder may be at least one of titanium oxide, alumina, magnesium oxide, aluminum, calcium oxide, zinc oxide mica and mica titanium, preferably titanium oxide, and pulverized and powdered. The pigment powder may be used, or the pigment powder may be prepared under the above-described conditions through a conventional process, and then ground and powdered.

When the size of the particle size is less than 2 μm, the coating layer for color realization may not be exhibited due to the scattering of light due to the reduction of the angular ratio, and the same color having the same refractive index. Formation can be difficult. Therefore, it is preferable that the diameter of an infrared shielding pigment is 5-50 micrometers, and thickness is 0.2 micrometer-5 micrometers.

In this case, the dispersion may use primary purified water (DI water) if the inorganic pigment particles to be coated on the surface of the infrared shielding pigment powder are hydrophilic, and if the hydrophobic one is alcohol-based solution, for example, ethanol (C ₂ H ₅ OH) or methanol ( CH ₃ OH) can be used.

At this time, it may be dispersed in 10 to 30 ℃, preferably at 25 ℃, there is no need for a separate heating process or cooling process process step is reduced economic effect.

In addition, if the stirring speed is less than 200rpm or the stirring time is less than 5 minutes, the stirring may be insufficient, whereas if the stirring speed exceeds 400rpm or the stirring time exceeds 30 minutes, only the process time will be longer without further dispersion effect As it can be, it is preferable to stir at a stirring speed of 200 to 400rpm or preferably 300rpm.

Dispersion step (S20) is a step of preparing an infrared shielding pigment ink by dispersing the metal oxide in the infrared suspension formed by the suspension manufacturing step.

In this case, the metal oxide may be at least one of titanium dioxide, cobalt, iron oxide, cobalt, iron-cyanide salt (Fe ₄ (Fe (CN) ₆ ) ₃ ), aluminum cobalt oxide (CoAl ₂ O ₄ ), or chromium oxide. May be cobalt oxide alumina, green may be chromium oxide, or black may be iron oxide and cobalt.

The coating step (S30) is a step of adding a metal salt to the infrared shielding pigment ink and adjusting the pH to 2 to 3, wherein the metal oxide is coated on the infrared shielding pigment.

In addition, as the metal salt, a compound containing at least one of calcium (Ca), aluminum (Al), zinc (Zn), barium (Ba), and magnesium (Mg) may be used.

In addition, the pH is adjusted using a dilute solution of hydrochloric acid (HCl) or sodium hydroxide (NaOH, caustic soda), the titration is adjusted by adjusting the pH of the suspension of the metal salt dumped to a range of 1-9 using the diluent. The pH range of the suspension is maintained to facilitate efficient coating of metal oxides on the surface of the infrared shielding pigment powder.

In this case, when the pH value is less than 1, the metal oxide particles are difficult to coat on the infrared shielding pigment powder. When the pH value is above 9, the infrared shielding pigment coating layer is not uniform and has irregular size and shape due to excessive aggregation of the metal. The saturation and coating state of the final pigment may be lowered.

In addition, when the thickness of the metal oxide layer is thin, there is a problem that it is difficult to coat, and when the thickness is thick, it may not significantly affect the efficiency of total solar reflectance (TSR) due to light scattering. The infrared reflecting material formed by coating the metal oxide on the infrared shielding pigment may have a thickness of 0.01 to 6 when the thickness of the infrared reflecting pigment is 100 thickness.

In addition, the metal oxide layer coated by the infrared reflecting material manufacturing step is a single layer of a high refractive index material or a low refractive index material, preferably a high refractive index material, or a multilayer in which a high refractive index material, a low refractive index material, and a high refractive index material are laminated. Can be.

The infrared reflector prepared above was dehydrated with a suspension containing a metal oxide layer, washed with primary purified water or an alcoholic solution and dried for 4 to 8 hours at a temperature of about 80 to 150 ° C. The process of obtaining the powder may further be carried out.

In addition, by using a mesh suitable for the particle size of the dried powder as described above to remove foreign matters by screening to remove the aggregated particles to finally prepare an infrared reflecting material powder coated with a metal oxide.

At this time, if the drying temperature is less than 80 ℃ drying time is long, economic efficiency and productivity may be lowered, and if the drying temperature exceeds 150 ℃ may be a phenomenon that the coagulation between powder particles increases.

The infrared reflecting material has an infrared shielding function with at least 40% of solar radiation reflecting infrared rays among sunlight in a wavelength range of 280 to 2500 nm of sunlight, and an interference color of black, blue or green depending on the material of the metal oxide. It is a black, blue or green infrared reflecting material having a.

In this case, the white infrared reflecting material may include a metal oxide layer made of titanium oxide, and the red infrared reflecting material may include a metal oxide layer made of iron oxide.

The infrared reflecting material formed as described above is economical because the production cost is reduced by using metal oxide which is an inorganic pigment which is cheaper than using organic pigment.

The mixing step (S40) is a step of preparing an infrared shielding paint by mixing an infrared reflecting material prepared through the infrared reflecting material manufacturing step with a binder, an antifoaming agent, and a dispersant.

In this case, the infrared reflecting material is preferably 20 to 50 parts by weight based on 100 parts by weight of the binder. When the content of the infrared reflector is less than 20 parts by weight, the subsequent reaction formation may be insufficient, and when the amount of the infrared reflector exceeds 50 parts by weight, the amount of the infrared reflector relative to the reaction solution may be too high to reduce the reaction efficiency.

In addition, the antifoaming agent may be 20 to 25 parts by weight, and the dispersant may be 10 to 15 parts by weight.

In this case, the binder may be any one selected from the group consisting of acrylic resins, acrylic-silicone copolymers, silicone resins, water-soluble polyurethane resins, acrylic-urethane copolymers and acrylic-silicone-urethane copolymers, preferably acrylic resins. have.

In addition, a binder, an infrared reflecting material, an antifoaming agent and a dispersant, the infrared reflecting material is a black, blue or green infrared shielding pigment, characterized in that the plate-shaped black, blue or green infrared shielding pigment coated with a metal oxide. Including infrared shielding coating film is possible

In this case, the binder is 50 to 60% by weight, the infrared reflecting material is 10 to 15% by weight, the antifoaming agent 10 and 30% by weight, the dispersant may be 5 to 10% by weight, the anti-settling agent 2% by weight or less in the coating film It is possible to manufacture a single layer of the coating film by adding an additional.

In addition, a single layer composite coating film may be prepared by adding a heat insulating pigment to the single layer coating film.

In this case, the insulating pigment may be any one selected from the group consisting of aluminosilicate, hollow glass beads, hollow silica, hollow polymer, inorganic silicate, borosilicate and chromite, and may be 5 to 10% by weight.

In addition, an additive 10 to 20% by weight may be added to the single layer composite coating film.

To prepare an infrared shielding double layer coating film comprising a black, blue or green infrared shielding pigment comprising a top coat layer comprising a binder, an infrared reflecting material, an antifoaming agent and a dispersing agent, and an undercoat layer comprising the binder, the antifoaming agent, the dispersing agent, and a heat insulating pigment. Production of a coating film excellent in infrared reflectance and shielding is possible.

At this time, the thermal insulation pigment contained in the undercoat layer maximizes the shielding function by blocking the heat of external visible and infrared rays introduced into the interior, and the insulating pigment is aluminosilicate, hollow glass beads, hollow silica, hollow polymer It may be any one selected from the group consisting of inorganic silicate, borosilicate, chromite and the like, or preferably hollow glass beads.

In this case, the top coat layer serves to reflect infrared rays as a reflective layer, and the bottom coat layer serves as a heat insulating layer to prevent heat from entering.

In addition, the infrared shielding bilayer coating film prepared by the above may include an infrared reflecting material having a ratio of the length of the outer reflecting pigment longitudinal direction and the metal oxide thickness of 100: 0.01 to 100: 12.

Hereinafter, the present invention will be described in detail with reference to Examples, but the present invention is not limited thereto.

Manufacture of Blue Infrared Shielding Paint

[Example 1]

60 parts by weight of the acrylic resin, 20 parts by weight of the infrared shielding pigment, 12 parts by weight of the antifoaming agent, 6 parts by weight of the dispersant, and 2 parts by weight of the sedimentation inhibitor were mixed to prepare 100 parts by weight of the total composition. The infrared shielding pigments used were blue pigments coated with aluminum cobalt particles (Aldrich) on 9-45 (μm) plate pigments of C-781K (CQV). To provide. The method of manufacturing the infrared shielding pigment used herein is to disperse 500 g of primary purified water in 30 g of TiO ₂ coated plate pigment (CQV product) in a 1 L beaker and dilute caustic soda (NaOH) and hydrochloric acid (HCl). Was used to adjust the pH to 7. Subsequently, stirring was performed at 200 rpm using a stirrer at 70 ° C. Disperse 10 wt% of CoAl ₂ O ₄ (Aldrich) to 200 mL beaker and 120 mL of purified water in the stirring plate pigment solution at a rate of 2 mL / min using an electronic pump. Titration was carried out for 2 hours. After completion of the reaction, the mixture was stirred for 16 hours, washed with primary purified water, dried at 100 ° C. for 2 hours, calcined at 850 ° C. for 2 hours, and screened using a mesh to carry out TiO. _An infrared shielding pigment, which is a blue pigment coated with CoAl ₂ O _4, was synthesized on the bivalent coated plate pigment particles.

[Example 2]

60 parts by weight of acrylic resin, 5 parts by weight of heat insulating material (hollow glass beads), 15 parts by weight of infrared ray shielding pigment used in Example 1, 12 parts by weight of antifoaming agent, 6 parts by weight of dispersant, and antisettling agent 2 A shielding paint was prepared by mixing parts by weight. At this time, the composition provides a single layer (composite) paint in which the heat insulation layer and the reflection layer are combined.

[Example 3]

60 parts by weight of acrylic resin, 15 parts by weight of additive (TiO ₂ ), 5 parts by weight of insulating material (hollow glass beads), 12 parts by weight of antifoam, 6 parts by weight of dispersant, and 2 parts by weight of antisettling agent are mixed with 100 parts by weight of the total composition. To prepare a shielding paint used for the undercoat layer, the topcoat was prepared by the infrared shielding paint in the method of Example 1. At this time, the composition provides a two-layer paint consisting of a top coat layer composed of a heat insulating layer and a reflective layer.

Example 4

The whole composition was the same as in Example 1, and the infrared shielding pigment used was a pigment coated with ferric ferrocyanide on a substrate coated with a single layer of TiO ₂ on 9-45 (μm) plate pigment particles. The method of preparing the infrared shielding pigment used herein is to disperse 500 mL of purified water of 30 g of TiO ₂ coated plate pigment (CQV), which is a basic base, in a 1 L beaker, and then use a 0.5 mol / L HCl diluent to adjust the pH. Adjusted to 4. Subsequently, stirring was performed at 200 rpm using a stirrer at 70 ° C. Into the plate pigment solution being stirred, 3.6% by weight of K ₃ Fe (CN) ₆ · 3H ₂ O and 3.1% by weight of FeCl ₃ · 6H ₂ O were added to 100% by weight of the plated pigment coated with TiO ₂ and stirred. After completion of the reaction, the mixture was stirred for 16 hours, washed with primary purified water, dried at 100 ° C. for 24 hours, and screened using a mesh to give TiO ₂ coated pigment particles. A blue infrared shielding paint coated with Fe ₄ (Fe (CN) ₆ ) ₃ was synthesized.

[Example 5]

The same conditions as in Example 2, wherein the infrared shielding pigment used was prepared in the shielding paint using the pigment of Example 4. The composition provides a single layer (composite) paint in which the heat insulation layer and the reflection layer are combined.

[Example 6]

The whole composition of the undercoat layer was the same as the undercoat conditions of Example 3, and the top coat layer produced the infrared shielding paint by the method of Example 4. At this time, the composition provides a double layer paint composed of a top coat layer composed of a heat insulating layer and a reflective layer.

Comparative Example 1

60 parts by weight of the acrylic resin, 20 parts by weight of the infrared reflecting material, 12 parts by weight of the antifoaming agent, 6 parts by weight of the dispersant, and 2 parts by weight of the antisettling agent were mixed with respect to 100 parts by weight of the total composition to prepare an infrared shielding paint.

In this case, the blue pigment used was a Cobalt aluminum oxide (Aldrich) pigment, and the composition provides a single layer (composite) paint in which the heat insulation layer and the reflection layer are combined.

Comparative Example 2

The whole composition of the undercoat layer was the same as the undercoat conditions of Example 3, and the top coat layer prepared the coating material by the method of the comparative example 1. At this time, the composition provides a double layer paint consisting of a bottom coat layer consisting of a heat insulating layer and a blue paint top coat layer.

Manufacture of Green Infrared Shielding Paint

[Example 7]

For the total composition, the same as in Example 1, where the infrared shielding pigment used was used as the pigment was coated with a Cr ₂ O ₃ to 9-45 (㎛) flaky pigment of synthetic mica (CQV Co.). In the method of preparing the infrared shielding pigments used herein, 500 g of primary purified water was dispersed in 30 g of plate pigment (CQV), which is a basic base, in a 1L beaker, and then the pH was adjusted to 4 using a dilute solution of hydrochloric acid (HCl). Subsequently, stirring was performed at 200 rpm using a stirrer at 70 ° C. And a 1mol / CrCl ₂ .6H ₂ O NaOH 25 mL of 25mL with 2mol / L of L to the plate-shaped stirring the pigment solution used for the electronic pump (electronic pump) by titration at a rate of 0.2mL / min subjected to stirring for 2 hours It was. After completion of the reaction, the mixture was stirred for 16 hours, washed with primary purified water, dried at 100 ° C. for 2 hours, calcined at 850 ° C. for 2 hours, and screened using a mesh to give a plate pigment. An infrared shielding coating, which is a green pigment coated with Cr ₂ O _3, was synthesized.

[Example 8]

For the whole composition, the same as in Example 1, wherein the infrared shielding pigment used

A shielding pigment coated with Cr ₂ O ₃ on a substrate coated with a single layer of TiO ₂ on 9-45 (μm) plate pigment particles was used. The method for preparing the infrared shielding pigment used herein is to disperse 500 mL of purified water of 30 g of TiO ₂ coated plate pigment (CQV product), which is a basic base, in a 1 L beaker, and then use 0.5 mol / L hydrochloric acid (HCl) diluent. To adjust the pH to 4. Subsequently, stirring was performed at 200 rpm using a stirrer at 80 ° C. Dissolve 20 wt% Cr ₂ O ₃ relative to the amount of the plated pigment in a 60 mL primary purified water in a 100 mL beaker and titrate at 0.2 mL / min using an electronic pump while stirring for 2 hours. Stirring was carried out. After completion of the reaction, the mixture was stirred for 16 hours, washed with primary purified water, dried at 100 ° C for 2 hours, calcined at 850 ° C for 2 hours, and screened using a mesh to carry out TiO ₂ Infrared shielding paint, which is a green pigment coated with Cr ₂ O _3, was coated on the coated plate pigment particles.

[Example 9]

The same conditions as in Example 2, wherein the infrared shielding pigments used were prepared in the shielding paints using the pigment of Example 8. The composition provides a single layer (composite) paint in which the heat insulation layer and the reflection layer are combined.

[Example 10]

The whole composition of the undercoat layer was the same as the undercoat condition of Example 3, and the top coat layer produced the infrared shielding paint by the method of Example 8. At this time, the composition provides a two-layer paint consisting of a top coat layer composed of a heat insulating layer and a reflective layer.

[Comparative Example 3]

For the whole composition, it was the same as Example 1, and the green coloring pigment used at this time used the Chromium oxide green (NIPPON DENKO company) pigment.

[Comparative Example 4]

The whole composition of the undercoat layer was the same as the undercoat conditions of Example 3, and the top coat layer produced the shielding paint by the method of the comparative example 3. At this time, the composition provides a double-layer paint consisting of a top coat layer composed of a heat insulating layer and a green paint layer.

Manufacture of Black Infrared Shielding Paint

[Example 11]

It is the same as that of Example 1 with respect to the whole composition. In this case, the infrared shielding pigment used was a black reflective pigment coated with 6 2-41 (㎛) plate pigment particles with a thickness of Fe ₂ O ₃ , Co (100 nm), to provide a single layer of paint. . In the method for preparing the infrared shielding pigment used herein, 50 g of synthetic mica having a size of 6-41 μm, which is a basic base in a 1 L beaker, was dispersed in 350 mL of first purified water, and then the pH was adjusted to 3 using a 0.5 mol / L HCl diluent. It was. Subsequently, stirring was performed at 450 rpm using a stirrer at 83 ° C. Titrate 20 wt% FeCl ₃ solution to 100 wt% of the stirring plate pigment solution. At this time, maintain the pH at 3 using caustic soda solution. After stirring for about 1 hour in this state, the pH was adjusted to 10 using a caustic soda solution, and then 23% by weight of CoSO ₄ · 7H ₂ O was titrated to 100% by weight of the plate pigment solution under stirring. At this time, the pH is maintained at 10 using a caustic soda solution. After stirring for about 1 hour in this state, washed with primary purified water, and then dried at 100 ℃ for 24 hours, and screened using a mesh (Feed) to the plate pigment particles Fe ₂ A black infrared shielding coating coated with O ₃ / Co was synthesized.

[Example 12]

It is the same as that of Example 1 with respect to the whole composition. At this time, the infrared shielding pigment used was a black infrared shielding pigment coated with Fe ₂ O ₃ , Co 40 (nm) thickness on the 5-25 (㎛) plate pigment particles, and provides a single layer of paint.

[Example 13]

The entire composition of the undercoat layer was the same as the undercoat conditions of Example 3, and the top coat layer was prepared by reflecting the IR reflector by the method of Example 11. At this time, the composition provides a double layer paint composed of a top coat layer composed of a heat insulating layer and a reflective layer.

[Example 14]

The same conditions as in Example 2, wherein the shielding paint was prepared using the pigment used in the infrared shielding pigment infrared shielding pigment 1 used. At this time, the composition provides a single layer (composite) paint in which the heat insulation layer and the reflection layer are combined.

[Comparative Example 5]

It is the same as that of Example 1 with respect to the whole composition. At this time, the color pigment used was C33-5198 (manufactured by Sun Chemical Co., Ltd.) and provides a single layer paint.

[Comparative Example 6]

The entire composition of the undercoat layer was the same as undercoat conditions of Example 3, and the overcoat was prepared by the method of Comparative Example 5. At this time, the composition provides a double layer paint composed of a top coat layer composed of a heat insulating layer and a reflective layer.

Hereinafter, the infrared radiation reflectance, brightness and saturation of the experimental example and the comparative example will be described.

Total solar reflectance (TSR) is obtained by measuring the baseline of the entire wavelength range of 200 ~ 2500nm using JASCO's V-570 and measuring the solar reflectance value including infrared rays from 200 ~ 2500nm. It was obtained by calculating through the following [Equation 1], the same applies in the examples and comparative examples of the present invention.

Here, R _λ is defined as the wavelength reflected on the object, I _λ is defined as the wavelength incident on the object. Color difference meter (L ^* , a ^* , b ^* ) of Examples 1 to 14 and Comparative Examples 1 to 6 were measured by the same product as the solar reflectivity measuring instrument, L ^* is the brightness index, a ^* is red (Red) , B ^* denotes the degree of yellow.

The solar reflectance and color difference values of the paints of Examples 1 to 6 and Comparative Examples 1 and 2 are shown in Table 1 below.

division hue
(L ^* , a ^* , b ^* ) Solar radiation
reflectivity
(%) Heat shield
Temperature
(℃) * L ^* a ^* b ^* Example 1 75.01 -3.64 -14.91 39.5 49 Example 2 57.98 -7.42 -33.24 43.9 47 Example 3 64.98 -12.93 -32.33 57.4 45 Example 4 60.51 -4.09 -41.91- 40.1 49 Example 5 51.25 -3.10 -39.20 28.0 47 Example 6 60.97 -12.78 -37.10 37.4 46 Comparative Example 1 28.51 9.35 -23.32 8.4 61 Comparative Example 2 32.54 12.92 -35.55 14.9 58

* The film thickness is 160 ~ 180mm.

* Measurement temperature (error range ± 1 degree) after 20 minutes of specimens (painted on a 5.8 x 5.8 cm iron substrate) 25 cm away from a 250 watt infrared lamp.

The solar reflectance and color difference values of the paints of Examples 7 to 10 and Comparative Examples 3 to 4 are as shown in Table 2 below.

division hue
(L ^* , a ^* , b ^* ) Solar radiation
reflectivity
(%) Heat shield
Temperature
(℃) * L ^* a ^* b ^* Example 7 51.59 -18.41 12.21 28.1 50 Example 8 62.93 -12.72 30.97 33.1 48 Example 9 56.45 -7.51 24.29 28.6 46 Example 10 63.39 -6.77 29.91 37.8 43 Comparative Example 3 47.24 -20.32 17.02 28.1 52 Comparative Example 4 46.54 -18.92 15.89 32.8 48

* The film thickness is 160 ~ 180mm.

* Measurement temperature (error range ± 1 degree) after 20 minutes of specimens (painted on a 5.8 x 5.8 cm iron substrate) 25 cm away from a 250 watt infrared lamp.

The solar reflectance and color difference values of the paints of Examples 11 to 14 and Comparative Examples 5 to 6 are as shown in Table 3 below.

division hue
(L ^* , a ^* , b ^* ) Solar radiation
reflectivity
(%) Heat shield
Temperature
(℃) * L ^* a ^* b ^* Example 11 53.83 -1.4 -5.67 37.3 50 Example 12 48.72 0.95 2.69 30.7 58 Example 13 34.89 -1.54 -5.83 40.5 44 Example 14 33.10 -0.98 -5.15 38.1 48 Comparative Example 5 26.20 0.39 -0.71 4.9 61 Comparative Example 6 32.95 -0.86 -5.02 17.7 59

* The film thickness is 160 ~ 180mm.

* Measurement temperature (error range ± 1 degree) after 20 minutes of specimens (painted on a 5.8 x 5.8 cm iron substrate) 25 cm away from a 250 watt infrared lamp.

Although the preferred embodiments of the present invention have been described, the present invention is not limited thereto, and various modifications can be made within the scope of the claims, the detailed description of the invention, and the accompanying drawings, which are also within the scope of the present invention. It is natural to belong.

Claims (18)

delete delete delete delete delete delete delete A stirring step of dispersing the black, blue or green infrared shielding pigment powder in the dispersion and then stirring at a temperature of 10 to 30 ° C. to prepare a suspension;
A dispersion step of dispersing a metal oxide in the suspension to produce an infrared shielding pigment ink;
A coating step of preparing an infrared reflecting material by coating the metal oxide on the infrared shielding pigment by adding an acid to the infrared shielding pigment ink while adjusting the metal salt to pH 2 to 3; and
Infrared shielding paint manufacturing method comprising a black, blue or green infrared shielding pigment, characterized in that it comprises a mixing step of mixing the infrared reflecting material, binder, antifoaming agent and dispersant. The method of claim 8,
The infrared shielding paint is 20 to 50 parts by weight of the infrared reflecting material, 20 to 25 parts by weight of the antifoaming agent, and 10 to 15 parts by weight of the dispersant, based on 100 parts by weight of the binder. Infrared shielding paint manufacturing method including green infrared shielding pigment. The method of claim 8,
The binder is any one selected from the group consisting of an acrylic resin, an acrylic-silicone copolymer, a silicone resin, a water-soluble polyurethane resin, an acrylic-urethane copolymer, and an acrylic-silicone-urethane copolymer. Infrared shielding paint manufacturing method including infrared shielding pigment. The method of claim 8,
The infrared shielding pigment is mica, natural mica, glass flake, iron oxide, titanium oxide, alumina, magnesium oxide, aluminum, calcium oxide, zinc oxide mica or mica titanium, characterized in that at least one of Or an infrared shielding paint manufacturing method including a green infrared shielding pigment. The method of claim 8,
The infrared shielding pigment is a width of 5 to 50 ㎛, thickness is 0.2 to 5 ㎛ of plate-like pigment, characterized in that the infrared shielding paint production method comprising a black, blue or green infrared shielding pigment. The method of claim 8,
The metal oxide may be at least one of titanium dioxide, cobalt, iron oxide, cobalt, iron-cyanide salt (Fe ₄ (Fe (CN) ₆ ) ₃ ), cobalt alumina (CoAl ₂ O ₄ ), or chromium oxide. Infrared shielding paint production method comprising a black, blue or green infrared shielding pigment. The method of claim 8,
The infrared reflecting material is a method for producing an infrared shielding paint including a black, blue or green infrared shielding pigment, characterized in that the ratio of the length of the infrared shielding pigment in the longitudinal direction and the thickness of the metal oxide is 100: 0.01 to 100: 12.
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