KR102095585B1 - a film with excellent transmittance - Google Patents

Abstract

The present invention relates to a transmittance-enhancing film and a method for manufacturing the same, and more specifically, to prepare a high-refractive-coating layer on at least one side of the film and to manufacture a low-refractive-coating layer on the high-refractive-coating layer. It relates to a method and a transmittance improving film produced therefrom.
The present invention can provide a method of manufacturing a transmittance-enhancing film that can lower the reflectance of the film and increase the transmittance, and have excellent adhesion, durability, water resistance, and thermal stability.
In addition, the present invention is excellent in adhesive strength, durability, water resistance, heat stability, transmittance, etc. by forming a high-refractive coating layer and a low-refractive coating layer on the film, thereby improving the transmittance improving film that can be stably used for a long time in solar cells, polarizers, liquid crystal displays, lenses, etc. Can provide.

Description

A film with excellent transmittance

The present invention relates to a transmittance-enhancing film and a method for manufacturing the same, and more specifically, to prepare a high-refractive-coating layer on at least one side of the film and to manufacture a low-refractive-coating layer on the high-refractive-coating layer. It relates to a method and a transmittance improving film produced therefrom.

Optical films started later than general polymer films used in packaging materials, household goods, automobiles, etc., but the demand continues to increase as the development of LCD-related technologies and research on high functionalization of films progress.

The optical film includes a viewing angle enlargement film, an antireflection film, a compensation film, and a brightness increase film, and the most commonly used film for the optical film is a polyester film.

The polyester film has stable physical properties over a wide temperature range from low temperature to high temperature, has excellent chemical resistance compared to other polymer resins, and has good mechanical strength, surface properties, and uniformity in thickness. Since it has excellent applicability, it is widely applied to condensers, photographic films, labels, pressure-sensitive tapes, laminates, transfer tapes, polarizers, and ceramic sheets.

In order for the polyester film to be used as an optical film, it has to have excellent light transmittance and low reflectance, and various studies such as the use of an anti-reflection film to maximize these properties have been conducted (Korean Patent Publication No. 10-2013- 0015935, Korean Open Patent No. 10-2013-0021182, Korean Registered Patent No. 10-1205477).

However, the technique disclosed in the above document has a high refractive index and a high reflectance of the antireflection film, a low transmittance, and poor curing properties, and thus cannot be stably used as an optical film for a long time.

Korean Patent Publication No. 10-2013-0015935 Korean Patent Publication No. 10-2013-0021182 Korean Registered Patent No. 10-1205477

The present invention is to solve the problems of the prior art, it is possible to lower the reflectance of the film and increase the transmittance, and has an object to provide a method of manufacturing a transmittance improving film excellent in adhesion, durability, water resistance and thermal stability .

In addition, the present invention is excellent in adhesive strength, durability, water resistance, heat stability, transmittance, etc. by forming a high-refractive coating layer and a low-refractive coating layer on the film, thereby improving the transmittance improving film that can be stably used for a long time in solar cells, polarizers, liquid crystal displays, lenses, etc. It aims to provide.

In order to achieve the above object, the present invention comprises the steps of (a) washing the film; (b) preparing a first mixture by mixing titanium dioxide nanoparticles having a diameter of 10 to 200 nm, a silane compound, an acid compound, a catalyst, an epoxy compound, and a solvent; (c) preparing a second mixture by mixing silica nanoparticles having a diameter of 10 to 200 nm, a silane compound, an acid compound, a catalyst, an epoxy compound, and a solvent; (d) coating the first mixture on at least one side of the film and curing to prepare a high refractive index coating layer; And (e) coating the second mixture on the high-refractive-coating layer and curing to prepare a low-refractive-coating layer.

In one embodiment of the present invention, the step (b) is a step of preparing a first stir by mixing titanium dioxide nanoparticles having a diameter of 10 to 200 nm, 3-glycidoxypropyl trimethoxysilane, and an acid compound. ; Preparing a second stirring material by mixing propylene glycol methyl ether and methanol with the first stirring material; Preparing a third stirring material by mixing a catalyst with the second stirring material; Preparing a fourth stirring material by mixing butyl glycidyl ether with the third stirring material; And mixing the fourth stirring material with methanol to prepare a fifth stirring material.

In one embodiment of the present invention, the weight ratio of propylene glycol methyl ether and methanol contained in the second stirring material is characterized in that 20 to 50:80 to 50.

In one embodiment of the present invention, step (c) is a first composition by mixing silica nanoparticles having a diameter of 10 to 200 nm, 3-glycidoxypropyl trimethoxysilane, methyl trimethoxysilane, and an acid compound. Preparing a; Preparing a second composition by mixing a catalyst with the first composition; Preparing a third composition by mixing butyl glycidyl ether with the second composition; And mixing the third composition with propylene glycol methyl ether and ethanol to prepare a fourth composition.

In one embodiment of the present invention, the weight ratio of the 3-glycidoxypropyltrimethoxysilane and methyltrimethoxysilane is 40-60: 60-40.

In addition, the present invention provides a transmittance improving film produced by the above manufacturing method.

The present invention is to solve the problems of the prior art, it is possible to lower the reflectance of the film and increase the transmittance, it is possible to provide a method of manufacturing a transmittance-enhancing film excellent in adhesion, durability, water resistance and thermal stability.

In addition, the present invention is excellent in adhesive strength, durability, water resistance, heat stability, transmittance, etc. by forming a high-refractive coating layer and a low-refractive coating layer on the film, thereby improving the transmittance improving film that can be stably used for a long time in solar cells, polarizers, liquid crystal displays, lenses, etc. Can provide.

Hereinafter, the present invention will be described in detail based on examples. The terms, examples, and the like used in the present invention are merely exemplified in order to explain the present invention in more detail and help a person of ordinary skill in the art understand, and the scope of the present invention should not be interpreted as being limited thereto.

Technical terms and scientific terms used in the present invention, unless otherwise defined, refer to meanings commonly understood by those skilled in the art to which this invention belongs.

The present invention (a) washing the film; (b) preparing a first mixture by mixing titanium dioxide nanoparticles having a diameter of 10 to 200 nm, a silane compound, an acid compound, a catalyst, an epoxy compound, and a solvent; (c) preparing a second mixture by mixing silica nanoparticles having a diameter of 10 to 200 nm, a silane compound, an acid compound, a catalyst, an epoxy compound, and a solvent; (d) coating the first mixture on at least one side of the film and curing to prepare a high refractive index coating layer; And (e) coating the second mixture on the high-refractive-coating layer and curing to prepare a low-refractive-coating layer.

The step (a) is a step of removing dust, oil, organic compounds, and contaminants remaining on the film, and the film may be washed with demineralized water, alcohol, an acidic or basic cleaning solution.

The film may be a polyethylene terephthalate, polyethylene naphthalate, polyester, polyamide, polycarbonate, polymethyl methacrylate, polystyrene film, sheet, or substrate without limitation.

In step (b), the first mixture may be prepared by mixing titanium dioxide nanoparticles having a diameter of 10 to 200 nm, a silane compound, an acid compound, a catalyst, an epoxy compound, and a solvent.

The step (b) comprises the steps of preparing a first stirring product by mixing titanium dioxide nanoparticles having a diameter of 10 to 200 nm, 3-glycidoxypropyl trimethoxysilane, and an acid compound; Preparing a second stirring material by mixing propylene glycol methyl ether and methanol with the first stirring material; Preparing a third stirring material by mixing a catalyst with the second stirring material; Preparing a fourth stirring material by mixing butyl glycidyl ether with the third stirring material; And mixing the fourth stirring material with methanol to prepare a fifth stirring material.

In the present invention, the first stirring material may be prepared by mixing titanium dioxide nanoparticles having a diameter of 10 to 200 nm, a silane compound, and an acid compound.

Through this step, the alkoxy group of the silane compound is hydrolyzed to form a hydroxyl group. The hydroxyl group can be bonded to the surface of the nanoparticles of titanium dioxide, whereby a silane compound can bind to the surface of the nanoparticles.

The diameter of the titanium dioxide nanoparticles is 10 ~ 200nm, preferably 10 ~ 60nm. When the diameter is less than 10 nm, the moisture barrier property is deteriorated, and when it exceeds 200 nm, a uniform coating layer cannot be formed, and durability and weather resistance are deteriorated.

The silane compound has an organic functional group capable of bonding with an organic compound and a hydrolyzable group capable of reacting with an inorganic material, and the silane compound binds to the surface of the titanium dioxide nanoparticles, such as water resistance, moisture barrier properties, durability, weather resistance, etc. Indicates.

The content of the silane compound is preferably 20 to 50 parts by weight with respect to 100 parts by weight of the nanoparticles, it is difficult to expect to improve the adhesion when the content is less than 20 parts by weight, and if it exceeds 50 parts by weight, interfacial adhesion is achieved by using excessive silane compound The properties, transmittance and durability are reduced.

As the silane compound, an alkyl group-containing silane, an amino group-containing silane, an epoxy group-containing silane, an acrylate group-containing silane, an isocyanate group-containing silane, a fluorine group-containing silane, a vinyl group-containing silane, and the like can be used without limitation.

Examples of the alkyl group-containing silane include methyl trimethoxysilane, dimethyldimethoxysilane, and octyl triethoxysilane.

Epoxy group-containing silanes include 2-glycidoxyethylmethyldimethoxysilane, 2-glycidoxyethylmethyldiethoxysilane, 3-glycidoxypropylmethyldimethoxysilane, 3-glycidoxypropylmethyldiethoxysilane, 2 -Glycidoxyethyltrimethoxysilane, 2-glycidoxyethyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 2- (3,4- Epoxycyclohexyl) ethylmethyldimethoxysilane, 2- (3,4-epoxycyclohexyl) ethylmethyldiethoxysilane, 3- (3,4-epoxycyclohexyl) propylmethyldimethoxysilane, 3- (3,4 -Epoxycyclohexyl) propylmethyldiethoxysilane, 2- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, 2- (3,4-epoxycyclohexyl) ethyltriethoxysilane, 3- (3, 4-epoxycyclohexyl) propyltrimethoxysilane, 3- (3,4-epoxycyclohexyl) propyltriethoxysilane, and the like.

Examples of the silane-containing silane include 3-methacryloxypropylmethyldimethoxysilane, 3-methacryloxypropyltrimethoxysilane, 3-methacryloxypropylmethyldiethoxysilane, and 3-methacryloxypropyltriethoxysilane. , 3-acryloxypropyl trimethoxysilane, methacryloxymethyl triethoxysilane, and methacryloxymethyl trimethoxysilane.

Examples of fluorine-containing silanes include heptadecafluoro-1,1,2,2-tetradecyltrimethoxysilane, trifluoropropyltrimethoxysilane, tridecafluorooctyltrimethoxysilane, and heptadecafluorodecyl Trimethoxysilane, heptadecafluorodecyl triisopropoxysilane, and the like.

In order to improve the water resistance, moisture barrier properties, durability, weather resistance, and transmittance of the film, it is preferable to use an epoxy group-containing silane such as 3-glycidoxypropyl trimethoxysilane.

In addition, 3-glycidoxypropyl trimethoxysilane and methyl trimethoxysilane may be used in a weight ratio of 40 to 60:60 to 40.

As the acid compound, hydrochloric acid, acetic acid, sulfuric acid, nitric acid, and the like can be used, and is preferably used in the form of an aqueous solution. For example, 15% acetic acid aqueous solution can be used.

The content of the acid compound is preferably 10 to 20 parts by weight based on 100 parts by weight of the nanoparticles, and if the content is less than 10 parts by weight, it is difficult to expect an improvement in adhesion, and when it exceeds 20 parts by weight, transmittance and durability decrease.

A second stirring material may be prepared by mixing propylene glycol methyl ether and methanol with the first stirring material.

The propylene glycol methyl ether and methanol serve to control the viscosity of the composition and stabilize the composition.

At this time, the content of propylene glycol methyl ether is preferably 10 to 30 parts by weight with respect to 100 parts by weight of nanoparticles, and the content of methanol is preferably 20 to 50 parts by weight with respect to 100 parts by weight of nanoparticles.

In addition, the weight ratio of propylene glycol methyl ether and methanol is preferably 20 to 50:80 to 50, and if the weight ratio is less than 20:80, workability decreases, and when the weight ratio exceeds 50:50, transmittance and durability decrease.

A third stirring material may be prepared by mixing a catalyst with the second stirring material.

Examples of the catalyst include organic metal salts such as Cu, Fe, Co, Mn, Al, Ti, Zr and Ni, such as octylic acid, stearic acid, naphthenic acid and acetylacetonate; Metal alkoxides such as Ti, Sn, Bi, Zr and Al; Phenol compounds such as octylphenol and nonylphenol; Alcohols such as 1-butanol and 2-ethylhexanol; 2-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 1-cyanoethyl-2-phenylimidazole, 1-cyanoethyl-2-ethyl-4- And imidazole derivatives such as methyl-imidazole, 2-phenyl-4,5-dihydroxymethylimidazole, and 2-phenyl-4-methyl-5-hydroxymethylimidazole. It is preferred to use, for example, aluminum acetylacetonate.

The content of the catalyst is preferably 1 to 5 parts by weight with respect to 100 parts by weight of the nanoparticles, when the content is less than 1 part by weight, it is difficult to expect an improvement in adhesion, and when it exceeds 5 parts by weight, the transmittance and durability are reduced.

When a composition is coated on a film by using a catalyst, a coating layer is easily formed at a lower temperature, and the heat resistance, thermal stability, and the like of the coating layer are excellent.

The fourth stirring material may be prepared by mixing the third stirring material with an epoxy compound.

The epoxy compound may be combined with a silane compound bonded to the surface of the titanium dioxide nanoparticles, or may be combined with hydroxyl groups formed on the surface of the titanium dioxide nanoparticles.

The content of the epoxy compound is preferably 1 to 10 parts by weight with respect to 100 parts by weight of the nanoparticles, when the content is less than 1 part by weight, it is difficult to expect an improvement in adhesion, and when it exceeds 10 parts by weight, transmittance and durability are lowered.

Types of epoxy compounds include butyl glycidyl ether (BGE), trimethylolpropane triglycidyl ether (TMPTGE), ethylene glycol diglycidyl ether, triglycidyl ether, N, N, N ', N'-tetra Glycidyl ethylenediamine, glycerin diglycidyl ether, and the like can be used without limitation, and butylglycidyl ether is preferably used.

In addition, butyl glycidyl ether (BGE) and trimethylolpropane triglycidyl ether (TMPTGE) can be used simultaneously as an epoxy compound, wherein the weight ratio of butylglycidyl ether and trimethylolpropane triglycidyl ether is 60 to 80: It is preferable that it is 40-20.

A fifth stirring material may be prepared by mixing a solvent with the fourth stirring material.

The solvent controls the viscosity of the composition, ethanol, propylene glycol methyl ether (PGME), methanol, propanol, isopropanol, butanol, etc. can be used without limitation, and methanol is preferably used.

The content of the solvent is preferably 500 to 1,000 parts by weight with respect to 100 parts by weight of the nanoparticles, and if the content is less than 500 parts by weight, the workability decreases, and when it exceeds 1,000 parts by weight, transmittance and durability decrease.

In the step (c), a second mixture may be prepared by mixing silica nanoparticles having a diameter of 10 to 200 nm, a silane compound, an acid compound, a catalyst, an epoxy compound, and a solvent.

The step (c) comprises the steps of preparing a first composition by mixing silica nanoparticles having a diameter of 10 to 200 nm, 3-glycidoxypropyltrimethoxysilane, methyltrimethoxysilane and an acid compound; Preparing a second composition by mixing a catalyst with the first composition; Preparing a third composition by mixing butyl glycidyl ether with the second composition; And mixing the third composition with propylene glycol methyl ether and ethanol to prepare a fourth composition.

In the present invention, the first composition may be prepared by mixing silica nanoparticles having a diameter of 10 to 200 nm, a silane compound, and an acid compound.

Through this step, the alkoxy group of the silane compound is hydrolyzed to form a hydroxyl group. The hydroxyl group may be bonded to the surface of the silica nanoparticles so that a silane compound can bind to the surface of the nanoparticles.

The diameter of the silica nanoparticles is 10 to 200 nm, and preferably 10 to 60 nm. When the diameter is less than 10 nm, the moisture barrier property is deteriorated, and when it exceeds 200 nm, a uniform coating layer cannot be formed, and durability and weather resistance are deteriorated.

The silane compound has an organic functional group capable of bonding with an organic compound and a hydrolyzable group capable of reacting with an inorganic material, and the silane compound binds to the surface of the silica nanoparticles to exhibit properties such as water resistance, moisture barrier properties, durability, weatherability, etc. Shows.

The content of the silane compound is preferably 40 to 80 parts by weight with respect to 100 parts by weight of the nanoparticles, and it is difficult to expect to improve the adhesion when the content is less than 40 parts by weight, and if it exceeds 80 parts by weight, interfacial adhesion is achieved by using excessive silane compound The properties, transmittance and durability are reduced.

As the silane compound, an alkyl group-containing silane, an amino group-containing silane, an epoxy group-containing silane, an acrylate group-containing silane, an isocyanate group-containing silane, a fluorine group-containing silane, a vinyl group-containing silane, and the like can be used without limitation.

Examples of the alkyl group-containing silane include methyl trimethoxysilane, dimethyldimethoxysilane, and octyl triethoxysilane.

Epoxy group-containing silanes include 2-glycidoxyethylmethyldimethoxysilane, 2-glycidoxyethylmethyldiethoxysilane, 3-glycidoxypropylmethyldimethoxysilane, 3-glycidoxypropylmethyldiethoxysilane, 2 -Glycidoxyethyltrimethoxysilane, 2-glycidoxyethyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 2- (3,4- Epoxycyclohexyl) ethylmethyldimethoxysilane, 2- (3,4-epoxycyclohexyl) ethylmethyldiethoxysilane, 3- (3,4-epoxycyclohexyl) propylmethyldimethoxysilane, 3- (3,4 -Epoxycyclohexyl) propylmethyldiethoxysilane, 2- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, 2- (3,4-epoxycyclohexyl) ethyltriethoxysilane, 3- (3, 4-epoxycyclohexyl) propyltrimethoxysilane, 3- (3,4-epoxycyclohexyl) propyltriethoxysilane, and the like.

Examples of the silane-containing silane include 3-methacryloxypropylmethyldimethoxysilane, 3-methacryloxypropyltrimethoxysilane, 3-methacryloxypropylmethyldiethoxysilane, and 3-methacryloxypropyltriethoxysilane. , 3-acryloxypropyl trimethoxysilane, methacryloxymethyl triethoxysilane, and methacryloxymethyl trimethoxysilane.

Examples of fluorine-containing silanes include heptadecafluoro-1,1,2,2-tetradecyltrimethoxysilane, trifluoropropyltrimethoxysilane, tridecafluorooctyltrimethoxysilane, and heptadecafluorodecyl Trimethoxysilane, heptadecafluorodecyl triisopropoxysilane, and the like.

In order to improve the water resistance, moisture barrier properties, durability, weather resistance, transmittance, etc. of the film, it is preferable to use a mixed silane compound of an alkyl group-containing silane and an epoxy group-containing silane, and the weight ratio of the epoxy group-containing silane and the alkyl group-containing silane is 40-60: It is preferable that it is 60-40.

For example, 3-glycidoxypropyltrimethoxysilane and methyltrimethoxysilane may be used in a weight ratio of 40-60: 60-40.

For example, as the silane coupling agent, an alkyl group-containing silane (methyltrimethoxysilane, dimethyldimethoxysilane and octyltriethoxysilane) and 3-glycidoxypropyltrimethoxysilane can be used, wherein 3-glycine Doxypropyltrimethoxysilane and silane containing alkyl groups are used in a weight ratio of 40 to 60:60 to 40, and the weight ratio of methyltrimethoxysilane, dimethyldimethoxysilane and octyltriethoxysilane is 100: 10 to 200: 10. It is preferably 200.

As the acid compound, hydrochloric acid, acetic acid, sulfuric acid, nitric acid, and the like can be used, and is preferably used in the form of an aqueous solution. For example, 15% acetic acid aqueous solution can be used.

The content of the acid compound is preferably 15 to 35 parts by weight with respect to 100 parts by weight of the nanoparticles, and if the content is less than 15 parts by weight, it is difficult to expect an improvement in adhesion, and when it exceeds 35 parts by weight, transmittance and durability are lowered.

A second composition may be prepared by mixing a catalyst with the first composition.

Examples of the catalyst include organic metal salts such as Cu, Fe, Co, Mn, Al, Ti, Zr and Ni, such as octylic acid, stearic acid, naphthenic acid and acetylacetonate; Metal alkoxides such as Ti, Sn, Bi, Zr and Al; Phenol compounds such as octylphenol and nonylphenol; Alcohols such as 1-butanol and 2-ethylhexanol; 2-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 1-cyanoethyl-2-phenylimidazole, 1-cyanoethyl-2-ethyl-4- And imidazole derivatives such as methyl-imidazole, 2-phenyl-4,5-dihydroxymethylimidazole, and 2-phenyl-4-methyl-5-hydroxymethylimidazole. It is preferred to use, for example, aluminum acetylacetonate.

The content of the catalyst is preferably 1 to 5 parts by weight with respect to 100 parts by weight of the nanoparticles, when the content is less than 1 part by weight, it is difficult to expect an improvement in adhesion, and when it exceeds 5 parts by weight, the transmittance and durability are reduced.

When a composition is coated on a film by using a catalyst, a coating layer is easily formed at a lower temperature, and the heat resistance, thermal stability, and the like of the coating layer are excellent.

An epoxy compound may be mixed with the second composition to prepare a third composition.

The epoxy compound may be combined with a silane compound bonded to the surface of the silica nanoparticles or a hydroxyl group formed on the surface of the silica nanoparticles.

The content of the epoxy compound is preferably 1 to 10 parts by weight with respect to 100 parts by weight of the nanoparticles, when the content is less than 1 part by weight, it is difficult to expect an improvement in adhesion, and when it exceeds 10 parts by weight, transmittance and durability are lowered.

Types of epoxy compounds include butyl glycidyl ether (BGE), trimethylolpropane triglycidyl ether (TMPTGE), ethylene glycol diglycidyl ether, triglycidyl ether, N, N, N ', N'-tetra Glycidyl ethylenediamine, glycerin diglycidyl ether, and the like can be used without limitation, and butylglycidyl ether is preferably used.

In addition, butyl glycidyl ether (BGE) and trimethylolpropane triglycidyl ether (TMPTGE) can be used simultaneously as an epoxy compound, wherein the weight ratio of butylglycidyl ether and trimethylolpropane triglycidyl ether is 60 to 80: It is preferable that it is 40-20.

A fourth composition may be prepared by mixing a solvent with the third composition.

The solvent controls the viscosity of the composition, ethanol, propylene glycol methyl ether (PGME), methanol, propanol, isopropanol, butanol and the like can be used without limitation.

The content of the solvent is preferably 500 to 1,500 parts by weight with respect to 100 parts by weight of the nanoparticles, and if the content is less than 500 parts by weight, processability decreases, and when it exceeds 1,500 parts by weight, transmittance and durability decrease.

In the present invention, it is preferable to use ethanol and propylene glycol methyl ether simultaneously as a solvent.

At this time, the content of ethanol is preferably 600 to 1,400 parts by weight with respect to 100 parts by weight of nanoparticles, and the content of propylene glycol methyl ether is preferably 20 to 100 parts by weight with respect to 100 parts by weight of nanoparticles.

In step (d), the first mixture may be coated and cured on at least one side of the film to prepare a high refractive index coating layer.

The step (d) may use a known coating method, and as a coating method, bar coating, meniscus coating, spray coating, roll coating, spin coating, immersion coating, and the like may be used without limitation.

In step (d), the first mixture may be coated on the film and then cured at 60 to 150 ° C. to form a high refractive coating layer.

At this time, the high refractive index means that it has a refractive index of 1.7 to 1.9.

In step (e), the high-refractive coating layer may be coated with the second mixture and cured to prepare a low-refractive coating layer.

In step (e), a known coating method may be used, and as the coating method, bar coating, meniscus coating, spray coating, roll coating, spin coating, and dipping coating may be used without limitation.

In step (e), the second mixture may be coated on the high-refractive coating layer, and then cured at 60 to 150 ° C to form a low-refractive coating layer.

At this time, the low refractive index means having a refractive index of 1.4 to 1.6.

In addition, the present invention relates to a transmittance improving film produced by the above manufacturing method.

The film of the present invention can lower the reflectance and increase the transmittance, and exhibit excellent properties of adhesion, durability, water resistance and thermal stability.

In addition, the present invention is excellent in adhesive strength, durability, water resistance, thermal stability, transmittance, etc. by sequentially forming a high-refractive coating layer and a low-refractive coating layer on a film, and thus can be stably used for a long time in solar cells, polarizers, liquid crystal displays, lenses, and the like.

Hereinafter, the present invention will be described in detail through examples and comparative examples. The following examples are only exemplified for the practice of the present invention, and the contents of the present invention are not limited by the following examples.

(Example 1)

The polyethylene terephthalate film was washed with a cleaning agent to remove dust, oil, organic compounds, and contaminants present in the film.

A first stirring product was prepared by mixing 100 parts by weight of titanium dioxide nanoparticles having a diameter of 50 nm, 30 parts by weight of 3-glycidoxypropyl trimethoxysilane, and 15 parts by weight of an aqueous 15% acetic acid solution.

20 parts by weight of propylene glycol methyl ether and 30 parts by weight of methanol were mixed with the first stirring material to prepare a second stirring material.

A third stir was prepared by mixing 3 parts by weight of aluminum acetylacetonate with the second stir.

A fourth stir was prepared by mixing 5 parts by weight of butyl glycidyl ether with the third stir.

A fifth stir was prepared by mixing 800 parts by weight of methanol with the fourth stir.

A first composition was prepared by mixing 100 parts by weight of silica nanoparticles having a diameter of 50 nm, 30 parts by weight of 3-glycidoxypropyl trimethoxysilane, 30 parts by weight of methyl trimethoxysilane and 20 parts by weight of an aqueous 15% acetic acid solution.

A second composition was prepared by mixing 3 parts by weight of aluminum acetylacetonate with the first composition.

A third composition was prepared by mixing 5 parts by weight of butyl glycidyl ether with the second composition.

A fourth composition was prepared by mixing 40 parts by weight of propylene glycol methyl ether and 1,000 parts by weight of ethanol in the third composition.

After applying the fifth stirring material to the polyethylene terephthalate film with a bar coating, it was cured at 100 ° C. to form a high refractive coating layer.

After applying the fourth composition to the high-refractive coating layer with a bar coating and curing at 100 ° C to form a low-refractive coating layer, a transmittance-enhancing film was prepared.

(Example 2)

A film was prepared in the same manner as in Example 1, except that 10 parts by weight of propylene glycol methyl ether and 50 parts by weight of methanol were mixed with the first stirring material to prepare a second stirring material.

(Example 3)

A film was prepared in the same manner as in Example 1, except that 30 parts by weight of propylene glycol methyl ether and 20 parts by weight of methanol were mixed with the first stirring material to prepare a second stirring material.

(Example 4)

A film was prepared in the same manner as in Example 1, except that the first composition was prepared using 20 parts by weight of 3-glycidoxypropyl trimethoxysilane and 40 parts by weight of methyl trimethoxysilane.

(Example 5)

A film was prepared in the same manner as in Example 1, except that the first composition was prepared using 40 parts by weight of 3-glycidoxypropyl trimethoxysilane and 20 parts by weight of methyl trimethoxysilane.

(Example 6)

A film was prepared in the same manner as in Example 1, except that a third composition was prepared by mixing 0.5 parts by weight of butyl glycidyl ether with the second composition.

(Example 7)

A film was prepared in the same manner as in Example 1, except that the third composition was prepared by mixing 15 parts by weight of butyl glycidyl ether with the second composition.

(Comparative Example 1)

A film was prepared in the same manner as in Example 1, except that butylglycidyl ether was not used when preparing the fourth stirring material.

(Comparative Example 2)

A film was prepared in the same manner as in Example 1, except that butylglycidyl ether was not used in preparing the third composition.

(reflectivity)

The adapter MPC 2200 was mounted on the spectrophotometer UV 2450 to measure the specular reflectance at an incident angle of 5 ° at an incident angle of 5 ° in the wavelength range of 380 to 780 nm, and the average reflectance of 450 to 650 nm was calculated.

(Transmittance)

The total light transmittance was measured using a transmittance meter (HM-150) according to ASTM D 1003.

The reflectance and transmittance of the films prepared from the examples and comparative examples were measured, and the results are shown in Table 1 below.

division Example Comparative example One 2 3 4 5 6 7 One 2 reflectivity(%) 4.4 5.7 5.8 5.1 5.2 5.0 5.1 6.3 6.6 Transmittance (%) 92.6 91.6 91.2 91.1 91.2 91.5 91.0 88.5 88.9

From the results of Table 1, it can be seen that Examples 1 to 7 had low reflectance and increased transmittance of the film. In particular, Example 1 has the best characteristics.

On the other hand, it can be seen that Comparative Examples 1 and 2 have inferior reflectance and transmittance compared to Examples 1 to 7.

Claims (6)

(a) washing the film;
(b) preparing a first mixture by mixing titanium dioxide nanoparticles having a diameter of 10 to 200 nm, a silane compound, an acid compound, a catalyst, an epoxy compound, and a solvent;
(c) preparing a second mixture by mixing silica nanoparticles having a diameter of 10 to 200 nm, a silane compound, an acid compound, a catalyst, an epoxy compound, and a solvent;
(d) coating the first mixture on at least one side of the film and curing to prepare a high refractive index coating layer; And
(e) coating the second mixture on the high-refractive-coating layer and curing, thereby producing a low-refractive-coating layer;
Step (b) is
Preparing a first stir product by mixing titanium dioxide nanoparticles having a diameter of 10 to 200 nm, 3-glycidoxypropyltrimethoxysilane, methyltrimethoxysilane, and an acid compound;
Preparing a second stirring material by mixing propylene glycol methyl ether and methanol with the first stirring material;
Preparing a third stirring material by mixing a catalyst with the second stirring material;
Preparing a fourth stirring material by mixing butyl glycidyl ether with the third stirring material; And
And mixing the fourth stirring material with methanol to prepare a fifth stirring material,
The weight ratio of the 3-glycidoxypropyl trimethoxysilane and methyl trimethoxysilane is 40 to 60:60 to 40,
The weight ratio of propylene glycol methyl ether and methanol contained in the second stirring material is 20 to 50:80 to 50,
Step (c) is
Preparing a first composition by mixing silica nanoparticles having a diameter of 10 to 200 nm, 3-glycidoxypropyltrimethoxysilane, methyltrimethoxysilane, and an acid compound;
Preparing a second composition by mixing a catalyst with the first composition;
Preparing a third composition by mixing butyl glycidyl ether with the second composition; And
Comprising the step of preparing a fourth composition by mixing propylene glycol methyl ether and ethanol to the third composition,
Method for producing a transmittance improving film, characterized in that the weight ratio of the 3-glycidoxypropyl trimethoxysilane and methyl trimethoxysilane is 40 to 60:60 to 40.
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