KR101453821B1 - Manufacturing method of ultraviolet curable coating composition comprising tungsten doped vanadium dioxide with phase transfer characteristics - Google Patents

Abstract

The present invention relates to a method for manufacturing an ultraviolet curable coating composition which includes 10-50 wt% of a material having characteristics of being cured by ultraviolet irradiation; 0.5-5 wt% of a compound forming a radical by absorbing ultraviolet rays; 1-20 w% of tungsten doped vanadium dioxide with phase transfer characteristics at about 30 °C; 0.1-5 wt% of a dispersion agent; 0.1-5 wt% of a leveling agent; and 15.0-88.3 wt% of a solvent. According to the present invention, reversible switching of blocking an infrared ray at high temperature in summer and transmitting an ultraviolet ray at low temperature in winter is possible by the phase transfer characteristics according to the outside temperature.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a tungsten-doped vanadium dioxide (VANO)

The present invention relates to a method of preparing an energy-saving coating liquid composition capable of controlling transmission and blocking of infrared rays by phase transition characteristics at a low temperature. More specifically, the present invention relates to a method for producing a tungsten doping The present invention relates to a method for producing an ultraviolet ray curable coating liquid composition having properties of controlling infrared transmittance using vanadium dioxide.

Recently, the price of chemical energy sources such as petroleum has skyrocketed and there is great interest in controlling energy consumption. In fact, more than 60% of household energy consumption is used for heating and cooling, and the energy consumed by windows is about 24%.

Recently, new buildings such as apartment buildings, office buildings, and residential complexes use a lot of buildings as glass windows to secure the beauty of the buildings and the view, but as the proportion of glass windows increases, heating and cooling costs increase and energy loss increases .

Of the light coming from the sun, infrared has a significant amount of thermal energy, about 53% of solar energy. Accordingly, energy-saving functional coating agents and materials capable of controlling the infrared transmittance with excellent transparency are urgently required.

As a first method for controlling the infrared transmittance with excellent transparency, a method of blocking sunlight by using an optical special glass, that is, LOW-E glass, is used for the window glass. Royi glass is a glass coated with sputtering processing and chemical vapor deposition (CVD) coating on a special metal film (usually silver and copper) having a high infrared reflectance inside a general glass, It is a glass that enhances performance. The special metal film is an energy-saving glass that transmits the visible light to increase the light-emitting property of the room, and reflects the infrared light to minimize the movement of indoor and outdoor heat, thereby reducing the temperature change in the room. In particular, the Roy multilayer glass is coated with a special metal film having excellent heat insulation effect on the plate glass, resulting in a high-thermal-insulating multilayer glass. In addition to the heat insulation performance, it has an excellent noise shielding effect and is capable of expressing various colors.

However, since the infrared ray blocking effect is insufficient and the long-wave radiant heat of the room is prevented from flowing out due to the long-wave reflection effect of the heat ray, the room temperature is rather increased, The energy consumption is increased. In addition, since expensive equipment is used for the coating method using the sputtering coating method and the chemical vapor deposition method in the coating method, the cost increases and the process proceeds under a precise atmosphere. Roy glass can be applied at the early stage of construction, but it is very limited in its use because it can not be used for buildings already completed or for existing buildings.

The second method is a method in which a wet coating material prepared by depositing a phthalocyanine-based infrared absorbing dye on a film or by directly solubilizing the same in an organic solvent is applied to a film to form an infrared ray shielding film. However, such a dye having an infrared ray absorbing property has a disadvantage in that transparency is lowered because a desired infrared ray shielding performance is realized by applying a large amount of dye, and there is a problem of discoloration and discoloration when exposed to direct sunlight.

The third method is a wet chemical coating method using a conductive oxide such as ATO (antimony tin oxide), ITO (indium tin oxide) or the like, or a wet coating material obtained by precisely dispersing it in a coating agent. This method, which occupies most of the infrared ray shielding film, has a good infrared blocking property but has a problem of poor transparency. In particular, in the case of ITO (indium tin oxide), the conversion of the indium, which is a raw material thereof, It is urgent.

A problem to be solved by the present invention is to provide an ultraviolet curable coating composition composition capable of reversible switching that blocks infrared rays at a room temperature of about 30 ° C. or more in summer and infrared rays at low temperatures in winter due to phase transition characteristics according to external temperature .

The present invention relates to a tantalum oxide film comprising 10 to 50% by weight of a material having properties of being cured by ultraviolet irradiation, 0.5 to 5% by weight of a compound capable of absorbing ultraviolet rays to form a radical, 1 to 20% 0.1 to 5% by weight of a dispersing agent, 0.1 to 5% by weight of a leveling agent and 15 to 88.3% by weight of a solvent, and the material having a property of being cured by ultraviolet irradiation is selected from dipentaerythritol hexaacrylate, pentaerythritol triacryl Acrylate, urethane acrylate, urethane acrylate, urethane acrylate, 1,6-hexanediol diacrylate, tripropylene glycol diacrylate, trimethylolpropane triacrylate, polyethylene glycol diacrylate, hydroxypropyl acrylate, At least one material selected from the group consisting of acrylate, methacrylate, methacrylate, acrylate, melamine acrylate, N-vinylpyrrolidone and silicone acrylate, The tungsten-doped vanadium dioxide is a material which is doped with vanadium dioxide and tungsten in a range of 0.01 to 20 wt%.

The compound capable of absorbing ultraviolet light to form a radical is selected from the group consisting of hydroxycyclohexyl phenyl methanone, 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenylpropan- ≪ / RTI > hydroxypropylmethylcellulose, hydroxypropylmethylcellulose, hydroxypropylmethylcellulose, < RTI ID = 0.0 >

The dispersant may be a silicone-based, acrylic-based or polyester phosphate-based compound.

The leveling agent may be a silicon-based or acrylic-based compound.

The tungsten-doped vanadium dioxide has an average particle size of 50~100nm, the vanadium dioxide can have the non-stoichiometric formula of _{V x O y (x = 1} , 1.5 <y <2 or 2 <y <2.5) .

The present invention also relates to a method for producing a light emitting device, comprising the steps of: (a) adding a substance having a property of being cured by ultraviolet irradiation to a container in which light is blocked, a compound capable of forming radicals by absorbing ultraviolet rays, Doped vanadium dioxide having a phase transition characteristic with a dispersing agent by adding and dispersing a solvent into the dispersion to form a tungsten-doped vanadium dioxide sol, and (c) placing the resultant obtained in the step (a) Doped vanadium dioxide sol, and stirring the mixture to obtain an ultraviolet curable coating liquid composition. The material having the property of being cured by ultraviolet ray irradiation is added to the ultraviolet curable coating liquid composition in an amount of 10 to 50 wt% The compound capable of absorbing ultraviolet rays to form radicals is added to the ultraviolet curable coating liquid composition at a ratio of 0.5 Wherein the tungsten-doped vanadium dioxide is contained in an amount of 1 to 20 wt% in the ultraviolet curable coating liquid composition, the dispersing agent is contained in the ultraviolet curable coating liquid composition in an amount of 0.1 to 5 wt%, and the leveling agent is contained in the ultraviolet- And the solvent is contained in the coating liquid composition in an amount of 0.1 to 5 wt%, the solvent is contained in the ultraviolet curable coating liquid composition in an amount of 15 to 88.3 wt%, and the material having the property of being cured by ultraviolet ray irradiation is dipentaerythritol hexaacrylate, But are not limited to, acrylic acid esters such as erythritol triacrylate, 1,6-hexanediol diacrylate, tripropylene glycol diacrylate, trimethylolpropane triacrylate, polyethylene glycol diacrylate, hydroxypropyl acrylate, urethane acrylate, , Epoxy acrylates, melamine acrylates, N-vinylpyrrolidone Silicon acrylate, and the tungsten-doped vanadium dioxide is a material in which vanadium dioxide and tungsten are doped in the range of 0.01 to 20 wt%. .

The compound capable of absorbing ultraviolet light to form a radical is selected from the group consisting of hydroxycyclohexyl phenyl methanone, 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenylpropan- &Lt; / RTI &gt; hydroxypropylmethylcellulose, hydroxypropylmethylcellulose, hydroxypropylmethylcellulose, &lt; RTI ID = 0.0 &gt;

The dispersant may be a silicone-based, acrylic-based or polyester phosphate-based compound.

The leveling agent may be a silicon-based or acrylic-based compound.

The tungsten-doped vanadium dioxide has an average particle size of 50~100nm, the vanadium dioxide can have the non-stoichiometric formula of _{V x O y (x = 1} , 1.5 <y <2 or 2 <y <2.5) .

The ultraviolet curable coating liquid composition using tungsten-doped vanadium dioxide having phase transition characteristics according to the present invention is a composition applied to a polymer film such as a PET (polyethylene terephthalate) film. Unlike coating directly on glass, Because it uses film, it is very easy to apply and it can be applied to a glass window of an existing building, so its application range can be greatly expanded.

According to the present invention, infrared rays are blocked at a high temperature of about 30 ° C or more in a summer room temperature due to the phase transition characteristic according to an external temperature, and reversible switching can be performed by transmitting infrared rays at a low temperature of 25 ° C or less in winter. When an infrared ray blocking film to which a UV curable coating composition containing tungsten-doped vanadium dioxide having a phase transition characteristic at a temperature of about 30 ° C. is applied is applied to a window, the amount of infrared rays entering the room through the window glass can be efficiently controlled to provide a pleasant indoor environment And can conserve energy consumption for heating and cooling.

In addition, according to the present invention, it is possible to solve the problem of transparency deterioration and durability which is a problem of the existing infrared ray shielding coating agent, and it is possible to switch to a substitute material due to the depletion of indium.

In addition, the ultraviolet curable coating composition of the present invention has excellent durability and can realize a product that does not change its IR blocking performance over time.

FIG. 1 is a graph showing transmittances according to wavelengths of a coating film obtained by coating a coating liquid composition prepared according to Comparative Examples 1, 2, and 1 and 2. FIG.
FIG. 2 is a graph showing the transmittance of a coating film obtained by coating the coating liquid composition prepared according to Example 1 with respect to a wavelength at a temperature of 25 ° C. and 35 ° C. FIG.
FIG. 3 is a graph showing transmittance according to wavelengths at 25 ° C. and 35 ° C. for a coating film obtained by coating a coating liquid composition prepared according to Example 2. FIG.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, it should be understood that the following embodiments are provided so that those skilled in the art will be able to fully understand the present invention, and that various modifications may be made without departing from the scope of the present invention. It is not.

The present invention provides an energy-saving functional coating liquid composition capable of reversible switching that blocks infrared rays at high temperatures in summer and infrared rays at low temperatures in winter due to phase transition characteristics according to external temperatures.

The ultraviolet curable coating liquid composition using tungsten-doped vanadium dioxide having phase transition characteristics according to the present invention is a composition applied to a polymer film such as a PET (polyethylene terephthalate) film. Unlike coating directly on glass, Because it uses film, it is very easy to apply and it can be applied to a glass window of an existing building, so its application range can be greatly expanded. When an infrared ray shielding film applied with a UV curable coating composition containing tungsten-doped vanadium dioxide having phase transition characteristics at a temperature of about 30 ° C is applied to a window, the amount of infrared rays entering the room through the window glass can be efficiently controlled to provide a pleasant indoor environment And can conserve energy consumption for heating and cooling.

The composition of the ultraviolet curable coating liquid using tungsten-doped vanadium dioxide having phase transition characteristics according to a preferred embodiment of the present invention is characterized by containing 10 to 50% by weight of a material having properties of being cured by ultraviolet irradiation, a compound capable of forming a radical by absorbing ultraviolet rays 0.5 to 5 wt%, 1 to 20 wt% of tungsten-doped vanadium dioxide having phase transition characteristics at about 30 DEG C, 0.1 to 5 wt% of a dispersing agent, 0.1 to 5 wt% of a leveling agent and 15 to 88.3 wt% .

A method of preparing a UV curable coating liquid composition using tungsten-doped vanadium dioxide having phase transition characteristics according to a preferred embodiment of the present invention comprises: (a) a step of curing a UV- (B) adding a solvent to the container and agitating the mixture, and adding tungsten-doped vanadium dioxide having a phase transition characteristic to the dispersant at a temperature of about 0 ° C, and dispersing the mixture to disperse the tungsten doping Forming a vanadium dioxide sol, and (c) placing the resultant obtained in the step (a) in a container in which light is shielded, adding a leveling agent and the tungsten-doped vanadium dioxide sol, and stirring to obtain an ultraviolet curable coating liquid composition , And the material having properties of being cured by ultraviolet ray irradiation is the ultraviolet ray hardening type The tungsten-doped vanadium dioxide is contained in an amount of 10 to 50% by weight in the composition of the liquid composition, and the compound capable of absorbing ultraviolet rays to form radicals is contained in the ultraviolet curable coating liquid composition in an amount of 0.5 to 5% Wherein the leveling agent is contained in the composition of the ultraviolet curable coating liquid in an amount of 0.1 to 5 wt% and the solvent is contained in the ultraviolet curable coating liquid composition in an amount of 0.1 to 5 wt% To be contained in the composition in an amount of 15 to 88.3% by weight.

An ultraviolet curable coating liquid composition containing tungsten-doped vanadium dioxide having the phase transition characteristics may be coated on a workpiece surface and dried to form a coating layer through an ultraviolet (UV) curing process.

The composition of the ultraviolet curable coating liquid using tungsten-doped vanadium dioxide having phase transition characteristics according to a preferred embodiment of the present invention is prepared by doping tungsten to vanadium dioxide, which is a ceramic particle having phase transition characteristics, and controlling the transition temperature to about 30 캜, Can be effectively controlled, can continuously exhibit its properties, is excellent in durability, and has properties of being cured by ultraviolet irradiation. When a coating film is formed using the coating liquid composition, the amount of infrared rays entering the room can be efficiently controlled to maintain a pleasant indoor environment and to save energy consumption for cooling and heating.

Examples of the material having properties of being cured by ultraviolet irradiation include dipentaerythritol hexaacrylate, pentaerythritol triacrylate, 1,6-hexanediol diacrylate, tripropylene glycol diacrylate, trimethylol propane triacrylate , Polyethylene glycol diacrylate, hydroxypropyl acrylate, urethane acrylate, polyester acrylate, epoxy acrylate, melamine acrylate, N-vinyl pyrrolidone, silicone acrylate, and mixtures thereof.

It is preferable that the material having the property of being cured by ultraviolet ray irradiation is contained in the ultraviolet ray curable coating liquid composition in an amount of 10 to 50% by weight. Durability and adhesion can be lowered when the content of the material having the property of being cured by ultraviolet irradiation is less than 10% by weight, and when the content exceeds 50% by weight, the amount of tungsten-doped vanadium dioxide having phase transition characteristics is reduced The amount of infrared rays can not be efficiently controlled.

The coating film formed by applying the ultraviolet ray curable coating liquid composition having the phase transition property according to the preferred embodiment of the present invention has a pencil hardness of 2H or more so that surface contamination and damage can be prevented.

The tungsten-doped vanadium dioxide used as ceramic particles with phase transition characteristics is characterized by a metal-insulator transition (MIT) phenomenon at a temperature of about 30 ° C. When the ambient temperature is higher than the phase transition temperature (about 30 ° C) of tungsten-doped vanadium dioxide, it reflects infrared rays. On the contrary, when the ambient temperature is lower than the phase transition temperature of vanadium dioxide (about 30 ° C), it transmits infrared rays. The tungsten-doped vanadium dioxide is preferably a material in which vanadium dioxide is doped with tungsten in a range of 0.01 to 20 wt%, tungsten is in a range of 0.01 to 20 wt%, vanadium dioxide is in a range of 80 to 99.99 wt% It is preferable to be doped with vanadium dioxide.

The tungsten-doped vanadium dioxide used in the present invention can be synthesized by adding sodium tungstate (Na ₂ WO ₄ ) using vanadyl sulfate (VOSO ₄ ) as a precursor. The coating liquid composition can be designed to effectively transmit or block infrared rays according to the ambient temperature through the tungsten-doped vanadium dioxide. The vanadium dioxide is not only a vanadium dioxide V _x O _y (x: y = 1: 2) having a chemical stoichiometric ratio of vanadium and oxygen of 1: 2 but also a non-stoichiometric vanadium dioxide V _x O _y (x = y &lt; 2 or 2 &lt; y &lt; 2.5).

Vanadium dioxide (VO ₂ ) has a monoclinic structure below the transition temperature and a tetragonal rutile structure above the transition temperature. The transition mechanism that causes the phase transition centering on the transition temperature takes place near the transition temperature as the temperature decreases. The electrical and optical properties of the vanadium dioxide (VO ₂ ) depend on the microstructure and lattice strain of the coating layer The transition temperature, the hysteresis width, the resistivity difference, and the like. By doping tungsten to vanadium dioxide and controlling the transition temperature to about 30 ° C, a more effective infrared barrier coating composition can be obtained.

Thermochromism is a phenomenon that exhibits a reversible change in optical properties that occurs at a certain temperature when heat is applied or cooled.

Although vanadium dioxide (VO ₂ ) is a thermochromic device, it has a transition temperature of about 70 ° C. before metal doping. In the present invention, by lowering the transition temperature to about 30 ° C. by doping vanadium dioxide with tungsten, And can be applied to an ultraviolet curable coating liquid composition.

As described above, tungsten-doped vanadium dioxide having a tetragonal rutile structure at a temperature of about 30 ° C or higher and having a monoclinic structure at about 30 ° C or higher can be used as a raw material for the thermochromic device.

The tungsten-doped vanadium dioxide has a characteristic that the crystal structure of the particles is a monoclinic loose structure at a low temperature of less than about 30 ° C. and has a property of transmitting infrared rays. When the temperature is changed to a high temperature state of about 30 ° C. or more, It becomes a dense structure in a tetragonal state and has a characteristic of blocking infrared rays. Therefore, if a film coated with a UV curable coating composition containing tungsten-doped vanadium dioxide having a phase transition property at a temperature of about 30 ° C is applied to an indoor glass window, infrared rays are transmitted through external light In the case of the summer when the ambient temperature is high, the infrared rays are cut off from the external light to lower the indoor temperature, thereby lowering the cooling ratio, thereby effectively reducing the energy.

The tungsten-doped vanadium dioxide having a phase transition property is preferably contained in an amount of 1 to 20 wt% in the ultraviolet curable coating liquid composition. When the addition amount of tungsten-doped vanadium dioxide having phase transition characteristics is less than 1 wt%, it may be difficult to obtain an infrared blocking / penetration effect. If the addition amount of tungsten-doped vanadium dioxide having phase transition characteristics is more than 20 wt% And it is difficult to form a coating film having desired characteristics.

The tungsten-doped vanadium dioxide preferably has an average particle diameter of 50 to 100 nm. When the average particle diameter of the tungsten-doped vanadium dioxide is larger than 100 nm, the coating surface becomes irregular when coated on the film and the coating efficiency is lowered, which may result in difficulty in forming a desired coating film. Further, . If the average particle diameter of the tungsten-doped vanadium dioxide is less than 50 nm, the synthesis may be difficult and expensive and uneconomical.

The compound capable of absorbing ultraviolet rays to form radicals leads to a reaction of ultraviolet (UV) light to form a coating film after coating, and is preferably contained in the ultraviolet curable coating liquid composition in an amount of 0.5 to 5 wt%. Examples of compounds capable of absorbing ultraviolet light to form radicals include hydroxycyclohexyl phenyl methanone, 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenylpropan- Hydroxymethyl acetophenone, benzophenone, or a mixture thereof, and the like can be used.

The dispersant preferably disperses vanadium dioxide uniformly and is contained in the ultraviolet curable coating liquid composition in an amount of 0.1 to 5 wt%. As the additive for uniformly dispersing the tungsten-coated vanadium dioxide having the phase transition property, the dispersant may be a silicone-based compound such as polydimethylsiloxane, or an acrylic-based or polyester-phosphate-based compound such as an acrylic copolymeric polymer.

The leveling agent is distributed on the surface of the coating, and the surface smoothness is used to solve such a problem and improve the properties of the surface of the coating film. The leveling agent is preferably contained in the ultraviolet curable coating liquid composition in an amount of 0.1 to 5% by weight. The leveling agent may be a silicone compound such as polydimethylsiloxane, or an acrylic compound such as an acrylic copolymeric polymer.

The solvent is used for dissolving the above-mentioned material having properties of being cured by ultraviolet irradiation, the compound capable of absorbing ultraviolet rays to form radicals, the dispersing agent and the leveling agent, If the compound, the dispersant and the leveling agent capable of absorbing ultraviolet rays to form radicals are not mixed with each other, the transmittance, haze, hardness, adhesion and the like are deteriorated when the coating film is formed. The solvent is preferably contained in an amount of 15 to 88.3% by weight in the ultraviolet curable coating liquid composition.

Examples of the solvent include propylene glycol monopropyl ether, propylene glycol monomethyl ether, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol Ether-based solvents such as monoethyl ether, diethylene glycol monopropyl ether, diethylene glycol monobutyl ether and diethylene glycol-2-ethylhexyl ether; alcohols such as isopropyl alcohol, methanol, ethanol, n-propanol, An ester solvent such as methyl ethyl ketone, methyl isobutyl ketone, ketone solvent such as acetone, an aliphatic hydrocarbon solvent such as kerosene, n-hexane, cyclohexanone, and volatiles, Aromatic hydrocarbon solvents such as xylene, toluene and benzene, The mixtures and the like.

The UV-curable coating liquid composition using tungsten-doped vanadium dioxide having phase transition characteristics according to a preferred embodiment of the present invention is a wet type photo-curable coating liquid which is coated on a polymer film base such as PET (polyethylene terephthalate), dried and ultraviolet (UV) A coating film can be formed through a curing process. Unlike the infrared barrier glass window which is manufactured by depositing on an existing glass, the coating cost is reduced and the coating efficiency is increased. In addition, it can be mass-produced by coating on a film through a roll-to-roll process. As described above, the method of coating the film can be applied regardless of the size, shape, and shape of the window, and can be applied to any shape or form such as a curved window.

Hereinafter, embodiments according to the present invention will be specifically shown, and the present invention is not limited to the following embodiments.

&Lt; Example 1 >

100 g of linear structure urethane acrylate EB-1290 having 6 functional groups of UCB as a material having properties of being cured by ultraviolet irradiation in a 500 ml beaker covered with silver foil for blocking light and 20 g of pentaerythritol triacrylate (PETA) 40 g of ethyl acetate as a solvent and 32 g of toluene were charged and 8 g of hydroxy dimethyl acetophenone serving as a photoinitiator (a compound capable of absorbing ultraviolet light to form radicals) was added and stirred for about 60 minutes with a stirrer to obtain a first solution .

179 g of ethanol was added to a 500 ml beaker, and 1 g of silicon-based polydimethylsiloxane dispersant was added thereto while stirring. 20 g of tungsten-doped vanadium dioxide having a size of 50 nm was added thereto and dispersed with a disperser (Mill) for about 60 minutes to obtain tungsten- (sol). The dispersant used herein is Disperbyk-110, manufactured by BYK. The tungsten-doped vanadium dioxide was doped with tungsten in an amount of 10 wt%.

98 g of the first solution was recovered and placed in a 500 ml beaker wrapped in a tin foil. 2 g of BYK-306, a leveling agent of BYK, and 100 g of the tungsten-doped vanadium dioxide sol were added thereto and stirred with a stirrer for about 60 minutes to prepare an ultraviolet- Respectively.

&Lt; Example 2 >

In order to block light, a 500 ml beaker covered with a silver foil was cured by ultraviolet irradiation. 100 g of a linear urethane acrylate SU-520 having 10 functional groups of urea chemical and 100 g of dipentaerythritol hexaacrylate (DPHA ), 40 g of ethyl acetate and 32 g of toluene were added as a solvent, and 8 g of hydroxydimethyl acetophenone serving as a photoinitiator (a compound capable of absorbing ultraviolet rays to form radicals) was added thereto, followed by stirring for about 60 minutes with a stirrer, 1 solution.

179 g of ethanol was added to a 500 ml beaker, and 1 g of dispersant was added thereto while stirring. 20 g of tungsten-doped vanadium dioxide having a size of 100 nm was added thereto and dispersed with a disperser (Mill) for about 60 minutes to prepare tungsten-doped vanadium dioxide sol Respectively. The dispersant used herein is Disperbyk-110, manufactured by BYK. The tungsten-doped vanadium dioxide was doped with tungsten in an amount of 10 wt%.

98 g of the first solution was recovered and placed in a 500 ml beaker wrapped in a tin foil. 2 g of BYK-306, a leveling agent of BYK, and 100 g of the tungsten-doped vanadium dioxide sol were added thereto and stirred with a stirrer for about 60 minutes to prepare an ultraviolet- Respectively.

&Lt; Example 3 >

An appropriate amount of the ultraviolet curing type coating liquid composition prepared according to Example 1 and Example 2 was applied to a polyethylene terephthalate (PET) film base material having a thickness of 100 탆 and then uniformly coated using a bar coater (BAR-COATER # 10) , And then dried at a temperature of 60 DEG C for about 2 minutes to completely remove the solvent in the ultraviolet curable coating liquid composition. Next, Was irradiated to the PET film substrate to form a coating film whose infrared transmittance was controlled.

Comparative examples that can be compared with the embodiments of the present invention are presented to more easily grasp the characteristics of the first to third embodiments. It should be noted that Comparative Examples 1 to 3, which will be described later, are merely provided for comparison with the characteristics of the embodiments, and are not the prior art of the present invention.

&Lt; Comparative Example 1 &

10 g of diimmonium dye and 48 g of methyl isobutyl ketone were placed in a 500 ml beaker and stirred for about 20 minutes to completely dissolve the dye. 60 g of acrylic copolymer binder Neocryl B-838 from DSM, 80 g of butyl acetate and 2 g of BYK-306 from BYK as a leveling agent were added and stirred for about 60 minutes with a stirrer to prepare a heat-drying type infrared barrier coating composition.

&Lt; Comparative Example 2 &

60 g of Neocryl B-838, an acrylic copolymer binder manufactured by DSM, was added to a 500 ml beaker, and then 38 g of methyl isobutyl ketone as a solvent and 2 g of BYK-306 of BYK as a leveling agent were added and stirred with a stirrer. 100 g of an ITO (indium tin oxide) sol (sol) dispersed in isopropyl alcohol was added thereto and stirred for about 60 minutes with a stirrer to prepare a thermal drying infrared blocking coating composition. The ITO sol is a sol in which 30 wt% of ITO is dispersed in isopropyl alcohol.

&Lt; Comparative Example 3 &

The coating liquid composition prepared according to Comparative Example 1 and Comparative Example 2 was uniformly coated on a polyethylene terephthalate (PET) film substrate having a thickness of 100 μm using a bar coater (BAR-COATER # 10) And dried for 2 minutes to form an infrared shielding coating film.

The following experimental examples show experimental results comparing characteristics of the embodiments of the present invention and Comparative Examples 1 to 3 in order to more easily grasp the characteristics of Embodiments 1 to 3 according to the present invention .

Table 1 shows the results of measuring the haze, the transmittance, the infrared ray blocking factor and the heat conduction ratio of the coating film formed in Example 3. [ Here, the haze and the transmittance were measured using a haze meter (NDH 300A), and the infrared cutoff was measured using a UV-Visible sectrophotometer. The shielding coefficient and the heat conduction rate were measured by the KSL 2016 measurement method. The hardness of the coating film was measured by JIS K5401 measurement method (pencil hardness measurement method) and the adhesion was measured by KSM 5981 (Scotch Tape test method).

The characteristic data obtained by the above test are shown in Table 1 below, and a graph of transmittance according to the wavelength of the coating film is shown in FIG. In FIG. 1, 'a' refers to a coating film obtained using the coating solution composition prepared according to Comparative Example 1, 'b' refers to a coating film obtained using the coating solution composition prepared according to Comparative Example 2, 'c' 'D' represents a coating film obtained using the coating liquid composition prepared according to Example 1, and 'd' indicates a coating film obtained using the coating liquid composition prepared according to Example 2, respectively.

Evaluation items Example 1 Example 2 Comparative Example 1 Comparative Example 2 Haze (%) 4.8 4.9 5.5 5.9 Transmittance (%, @ 550 nm) 53.2 51.3 48.2 47.5 Infrared cutoff ratio (%, 900 to 2500 nm) 83.2 85.3 69.5 71.4 Shielding factor (-) 0.65 0.61 0.83 0.75 Thermal Permeability (W / m ² K) 5.75 5.80 6.01 6.09 Coating film hardness (H) 2H 2H F F Adhesion (100/100) 100/100 100/100 100/100 100/100

Referring to Table 1 and FIG. 1, the transmittance of the coating film obtained using the coating composition prepared according to Example 1 and Example 2 was higher than that of the coating composition obtained using the coating composition prepared according to Comparative Example 1 and Comparative Example 2 . It was confirmed that the coating film obtained using the coating composition prepared according to Example 1 and Example 2 had an infrared blocking rate of 80% or more, which was superior to the coating film obtained using the coating composition prepared according to Comparative Example 1 and Comparative Example 2 Able to know. It can also be seen that the hardness of the coating film obtained by using the coating solution composition prepared according to Example 1 and Example 2 is also better than that of the coating film obtained using the coating solution composition prepared according to Comparative Examples 1 and 1 and Comparative Example 2 .

Table 2 below shows durability data. The durability was measured by using an accelerated weathering tester (QUV Tester) under conditions of 100 mW / m &lt; 2 &gt; and 500 &lt; 0 &gt; C for 500 hours.

Evaluation items Example 1 Example 2 Comparative Example 1 Comparative Example 2 Adhesion (100/100) 100/100 100/100 60/100 50/100

Referring to Table 2, in the case of a coating film obtained by using the coating liquid composition prepared according to Example 1 and Example 2, the product using ITO (indium tin oxide) is only 50/100, It can be seen that it is excellent.

In Table 3 below, the transmittance and the infrared blocking rate were measured by varying the temperature of the coating film obtained using the coating composition prepared in Example 1 and Example 2 at 25 ° C and 35 ° C, respectively, and data were displayed. FIG. 3 is a graph showing the transmittance of the coating layer obtained by using the coating composition prepared in Example 1, and FIG. 3 is a graph showing the transmittance of the coating layer obtained by using the coating composition prepared in Example 2.

Evaluation items 25 ℃ 35 ℃ Example 1 Example 2 Example 1 Example 2 Transmittance (%) (@ 550 nm) 53.2 51.3 53.2 51.3 Infrared blocking rate (%) (900 nm to 2500 nm) 21 20 83.2 85.3

Referring to Table 3, FIG. 2 and FIG. 3, the transmittance was the same at a low temperature (25 ° C.) and a high temperature (35 ° C.), but the transmittance of the coating layer obtained using the coating composition prepared according to Example 1 and Example 2 The infrared cutoff rate is about 20% at low temperature (25 ° C), but about 80% at high temperature (35 ° C). As a result, infrared blocking / transmission characteristics can be controlled according to the ambient temperature.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, This is possible.

Claims (10)

delete delete delete delete delete (a) adding a substance having a property of being cured by ultraviolet irradiation to a container in which light is blocked, a compound capable of forming a radical by absorbing ultraviolet rays, and a solvent, and stirring the mixture;
(b) adding and dispersing tungsten-doped vanadium dioxide having a phase transition property to a dispersing agent while stirring the solvent in a vessel to form a tungsten-doped vanadium dioxide sol; And
(c) placing the resultant obtained in the step (a) in a container in which light is blocked, adding a leveling agent and the tungsten-doped vanadium dioxide sol, and stirring to obtain an ultraviolet curable coating liquid composition,
The above-mentioned material having properties to be cured by ultraviolet irradiation is contained in the ultraviolet curable coating liquid composition in an amount of 10 to 50 wt%, and the compound capable of absorbing ultraviolet light to form radicals is added to the ultraviolet curable coating liquid composition in an amount of 0.5 to 5 wt% Wherein the tungsten-doped vanadium dioxide is contained in the ultraviolet curable coating liquid composition in an amount of 1 to 20 wt%, the dispersant is contained in the ultraviolet curable coating liquid composition in an amount of 0.1 to 5 wt%, and the leveling agent is contained in the ultraviolet curable coating liquid composition 0.1 to 5 wt%, and the solvent contains 15 to 88.3 wt% of the ultraviolet curable coating liquid composition,
The material having properties of being cured by ultraviolet irradiation is preferably selected from the group consisting of dipentaerythritol hexaacrylate, pentaerythritol triacrylate, 1,6-hexanediol diacrylate, tripropylene glycol diacrylate, trimethylolpropane triacrylate , At least one material selected from the group consisting of polyethylene glycol diacrylate, hydroxypropyl acrylate, urethane acrylate, polyester acrylate, epoxy acrylate, melamine acrylate, N-vinyl pyrrolidone and silicone acrylate,
Wherein the tungsten-doped vanadium dioxide is a material doped with vanadium dioxide and tungsten in a range of 0.01 to 20 wt%.
The compound according to claim 6, wherein the compound capable of absorbing ultraviolet light to form a radical is selected from the group consisting of hydroxycyclohexyl phenyl methanone, 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy- -1-one, hydroxydimethylacetophenone, and benzophenone. The method for producing a coating composition for ultraviolet curable liquid according to claim 1,
The method according to claim 6, wherein the dispersant is a silicone-based, acrylic-based or polyester phosphate-based compound.
The method according to claim 6, wherein the leveling agent is a silicone-based or acrylic-based compound.
7. The method of claim 6, wherein the tungsten-doped vanadium dioxide has an average particle size of 50-100 nm,
The vanadium dioxide is _{V x O y (x = 1} , 1.5 <y <2 or 2 <y <2.5) The method of the ultraviolet-curable coating composition characterized in that it has the non-stoichiometric formula of.

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