KR20110077523A - Cellulose ester film and method for producing the same - Google Patents

Cellulose ester film and method for producing the same Download PDF

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Publication number
KR20110077523A
KR20110077523A KR1020090134133A KR20090134133A KR20110077523A KR 20110077523 A KR20110077523 A KR 20110077523A KR 1020090134133 A KR1020090134133 A KR 1020090134133A KR 20090134133 A KR20090134133 A KR 20090134133A KR 20110077523 A KR20110077523 A KR 20110077523A
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KR
South Korea
Prior art keywords
cellulose ester
layer
weight
ester film
film
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Application number
KR1020090134133A
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Korean (ko)
Inventor
김한성
Original Assignee
주식회사 효성
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Priority to KR1020090134133A priority Critical patent/KR20110077523A/en
Publication of KR20110077523A publication Critical patent/KR20110077523A/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B23/00—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose
    • B32B23/14—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose characterised by containing special compounding ingredients
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B23/00—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose
    • B32B23/20—Layered products comprising a layer of cellulosic plastic substances, i.e. substances obtained by chemical modification of cellulose, e.g. cellulose ethers, cellulose esters, viscose comprising esters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/15—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state
    • B32B37/153—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state at least one layer is extruded and immediately laminated while in semi-molten state
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/16—Drying; Softening; Cleaning
    • B32B38/164—Drying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/16—Drying; Softening; Cleaning
    • B32B38/164—Drying
    • B32B2038/168—Removing solvent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/514—Oriented

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  • Polarising Elements (AREA)
  • Laminated Bodies (AREA)

Abstract

Disclosed are a cellulose ester film useful as a polarizing plate protective film of a liquid crystal display device and a method of manufacturing the same. The cellulose ester film, the front layer; Inner layer; And a back layer, wherein the front layer, the inner layer, and the back layer include two or more plasticizers and two or more ultraviolet absorbers, and the total plasticizer content is 10 to 20% by weight based on the total cellulose ester film. The total amount of the ultraviolet absorber is 0.01 to 5% by weight based on the total cellulose ester film, and the amount of the plasticizer included in the front layer and the rear layer is 10 parts by weight based on 100 parts by weight of the plasticizer included in the inner layer. Hereinafter, with respect to 100 parts by weight of the ultraviolet absorber contained in the inner layer, the content of the ultraviolet absorber contained in the front layer and the rear layer is 10 parts by weight or less, respectively.

LCD, protective film, cellulose ester film

Description

Cellulose ester film and its manufacturing method {Cellulose ester film and method for producing the same}

The present invention relates to a cellulose ester film and a method of manufacturing the same, and more particularly, to a cellulose ester film useful as a polarizing plate protective film of a liquid crystal display device and a manufacturing method thereof.

Recently, as the demand for portable information carriers increases, researches for improving image quality of liquid crystal displays (LCDs) and reducing manufacturing costs have been actively conducted. A liquid crystal display (LCD) is one of the representative flat panel displays commercialized, and displays an image while light emitted from a back light passes through an anisotropic liquid crystal material and a polarizing plate. The liquid crystal display device has a twisted nematic mode (TN) in which a liquid crystal having positive dielectric anisotropy is horizontally aligned between substrates facing each other, and a liquid crystal having negative dielectric anisotropy is vertically aligned between substrates facing each other. VA mode (Vertical Alignment mode), and other in-plane switching (IPS) mode liquid crystal display device.

In such a liquid crystal display device, in order to protect the polarizing plate, a cellulose ester film such as Triacetyl Cellulose is attached to one surface of the polarizing plate. Since the cellulose ester protective film is directly attached to the polarizing plate displaying an image, the cellulose ester protective film should not only have excellent optical characteristics and low surface scratches, but also block ultraviolet rays incident from external light, thereby preventing polarizing plates and liquid crystals. Should be prevented from deterioration. To this end, an ultraviolet absorber is used in the cellulose ester protective film, and to give flexibility to the film, a plasticizer such as phosphate ester should be included in the film. UV absorbers and plasticizers, which are organic additives included in the film, are bleed out during the high temperature drying process in the film manufacturing process, contaminating the surface of the film, resulting in defects on the surface of the film, and also contaminating the manufacturing equipment. There is a problem of deterioration. In addition, when the polarizing plate is manufactured using the manufactured film, it is bleed out in the alkaline saponification step and the drying step of the polarizing plate manufacturing process, thereby contaminating the polarizing plate manufacturing equipment. In addition, there is a disadvantage that the adhesion between the film surface and the coating layer in the coating treatment such as anti-glare coating, hard coating on the film surface is reduced. In order to prevent the plasticization of the plasticizer, only the non-phosphoric ester plasticizer may be used, but the manufacturing cost increases due to the high price.

Accordingly, an object of the present invention is to suppress the bleed out of the plasticizer and the ultraviolet absorber, to improve the productivity at the time of film production and to improve the yield, and to improve the adhesion between the film and the coating layer during the coating treatment on the film surface. It is to provide a cellulose ester film and a method for producing the same.

In order to achieve the above object, the present invention, the front layer; Inner layer; And a back layer, wherein the front layer, the inner layer, and the back layer include two or more plasticizers and two or more ultraviolet absorbers, and the total plasticizer content is 10 to 30% by weight based on the total cellulose ester film. The total amount of the ultraviolet absorber is 0.01 to 5% by weight based on the total cellulose ester film, and the amount of the plasticizer included in the front layer and the rear layer is 10 parts by weight based on 100 parts by weight of the plasticizer included in the inner layer. Or less, with respect to 100 parts by weight of the ultraviolet absorber included in the inner layer, the content of the ultraviolet absorber contained in the front layer and the rear layer is to provide a cellulose ester film, respectively 10 parts by weight or less.

In addition, the present invention, the first casting stock solution, the second casting stock solution and the third casting stock solution containing a cellulose ester component, a solvent for dissolving the cellulose ester component, two or more ultraviolet absorbers and two or more plasticizers of the belt Co-extrusion to a surface to apply a sheet, and evaporating the solvent present in the casting stock solution to form a cellulose ester film comprising a front layer, an inner layer, and a back layer; Peeling the cellulose ester film from the belt; And stretching and drying the exfoliated cellulose ester film, to provide a method for producing the cellulose ester film.

In the cellulose ester film according to the present invention, the content of the plasticizer and the ultraviolet absorber included in the front layer and the rear layer is 10 parts by weight or less, respectively, based on 100 parts by weight of the plasticizer and the ultraviolet absorber included in the inner layer, and thus the plasticizer and the ultraviolet absorber. It is possible to effectively suppress the bleed out of the film productivity can be improved, the coating layer and the surface of the cellulose ester film (front layer and / or back layer) when coating the surface (front layer and / or back layer) of the cellulose ester film The adhesion between the shells can be improved.

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

1 is an overall schematic view of a film manufacturing apparatus that can be used for producing a cellulose ester film according to the present invention, and FIG. 2 is a die and a belt in the film manufacturing apparatus shown in FIG. It is an enlarged sectional view of the part. As shown in Figures 1 and 2, the cellulose ester film according to the present invention is prepared by a solution flexible method. In order to manufacture the cellulose ester film according to the present invention, first, the first, second and third casting stock solution (2, 4, 6), through the die (20), to the surface of the belt (30) Is co-extruded and applied in the form of a sheet, and the solvent present in the casting stocks 2, 4 and 6 is evaporated by the temperature of the belt 30 to form a cellulose ester film 10. The die 20 is for extruding the casting stock solution 2, 4, 6, for example, a conventional T-die may be used. The belt 30 is a support for forming the film 10 by drying while transporting the casting stock solution (2, 4, 6), a stainless steel conveyor belt (belt) may be used as the belt 30, The thickness of the cellulose ester film 10 may be adjusted by adjusting the movement or rotation speed of the belt 30.

The casting stock solution (2, 4, 6) is a cellulose ester component, a solvent for dissolving the cellulose ester component, two or more plasticizers for imparting flexibility to the cellulose ester film 10 and for blocking ultraviolet rays It contains two or more ultraviolet absorbers. The casting stock solution (2, 4, 6) is also referred to as dope, the content of the cellulose ester component in the casting stock solution (2, 4, 6) is usually 15 to 25% by weight, preferably 15 to It is 20 weight% and content of the said solvent is the remainder except the solid content containing the said cellulose ester component.

As the cellulose ester component, cellulose acetates such as triacetyl cellulose (TAC) and cellulose acetate propionate (CAP) may be used. The solvent may be methylene chloride (MC) or methyl acetate (Methyl Acetic acid). Organic solvents such as alcohols (eg, methanol) can be used.

As the plasticizer, conventional plasticizers used in protective films can be used, for example, triphenyl phosphate (TPP), biphenyl diphenylphosphate (BDP), tricresyl phosphate (tricresyl) phosphate ester plasticizers such as phosphate (TCP), phthalate ester plasticizers such as diethyl phthalate, dimethoxy ethyl phthalate, ethyl phthalyl ethyl glycolate (EPEG), Glycolic acid ester plasticizers, such as butyl phthalyl butyl glycolate (BPBG), polyhydric alcohol ester plasticizers, such as trimethylopropane tribenzoate (TMPTB), trimethyl propane triacetate, etc. 2 or more types can be used.

As the ultraviolet absorber, a conventional ultraviolet absorber used for a protective film may be used, for example, 2.2'-dihydroxy-4.4'-dimethoxybenzophenone (2.2'-dihydroxy-4.4'-dimethoxybenzophenone), Benzophenes, such as 2-hydroxy-4-methoxybenzophenone and 2-hydroxy-4-n-dodecyloxybenzophenone Non-system UV absorber, 2- (hydroxy-5-t-octylphenyl) benzotriazole, 2- (2'-hydroxy-5'-methylphenyl) Benzotriazole (2- (2'-hydroxy-5'-methylphenyl) benzotriazole), 2- (2'-hydroxy-3,5'-di-t-butylphenyl) -5-chlorobenzotriazole (2 Two or more kinds of benzotriazole compounds such as-(2'-hydroxy-3,5'-di-t-butyl phenyl) -5-choloro benzotriazole) can be used.

In the present invention, the casting stock solution 2, 4, 6, which is extruded from the die 20, includes the first casting stock solution 2, which forms the front layer 12 of the film 10, and the inside of the film 10. A second casting stock solution 4 forming a layer 14 and a third casting stock solution 6 forming a back layer 16 of the film 10. The cellulose ester component and / or the solvent constituting the first, second and third casting stock solutions 2, 4, 6 may be the same or different from each other, and the cellulose ester solution tubing 22, 24, 26 may Two or more kinds of UV absorbers and two or more plasticizers having different contents are mixed through side feeding, so that the two or more kinds included in the front layer 12, the inner layer 14, and the rear layer 16. The content of the plasticizer and the two or more ultraviolet absorbers can be adjusted. Here, the total thickness of the cellulose ester film 10 (the final thickness after stretching and drying, the same below) is usually 20 to 100㎛, the thickness of the front layer 12 and the back layer 16, respectively, the overall thickness of the film 5 to 20%, preferably 10 to 15% of the thickness of the inner layer 14 is 60 to 90%, preferably 70 to 80% of the total thickness of the film. In addition, the content of the total plasticizer contained in the cellulose ester film 10 is 10 to 30% by weight, preferably 15 to 25% by weight based on the total cellulose ester film 10, and the inner layer 14 The amount of the plasticizer included in the front layer 12 and the rear layer 16 is 10 parts by weight or less, preferably 5 to 8 parts by weight, respectively, based on 100 parts by weight of the plasticizer contained in the cellulose ester film ( The total amount of the ultraviolet absorber included in 10) is 0.01 to 5% by weight, preferably 0.1 to 3% by weight, based on the total cellulose ester film 10, and 100 of the ultraviolet absorbers included in the inner layer 14. The content of the ultraviolet absorber contained in the front layer 12 and the rear layer 16 is 10 parts by weight or less, preferably 3 to 8 parts by weight, and more preferably 3 to 5 parts by weight, based on parts by weight. to be. Here, if the thickness of the front layer 12, the inner layer 14 and the rear layer 16 is out of the range, there is a fear that the plasticizer and the ultraviolet absorber is bridging out, if the content of the total plasticizer is too small There exists a possibility that the flexibility of the film 10 may fall, and when there is too much, there exists a possibility that it may bleed out. In addition, if the content of the total ultraviolet absorbent is too small, there is a fear that the ultraviolet ray may not be blocked, if too much, there is a fear of bridging out, the plasticizer and the ultraviolet absorber included in the front layer 12 and the back layer 16 When the content of more than 10 parts by weight, the plasticizer and the ultraviolet additive may be bred out or the coating adhesion of the cellulose ester film 10 may be lowered.

Referring again to FIG. 1, the casting stock solution 2, 4, 6 applied to the belt 30 moves with the belt 30 for a time and distance sufficient to be molded into the film 10, and then guides. It is peeled from the belt 30 by the peeling roller 32 which is a guide roller. The peeled film 10 is transferred to a stretching machine 40, stretched in a horizontal direction (TD) and / or mechanical direction (MD), and dried in a dryer 50. After the final cellulose ester film 10 is formed, it is wound in a winder 60 and shipped as a product.

The cellulose ester film 10 according to the present invention has a multilayer structure including a front layer 12, an inner layer 14, and a back layer 16, and the cellulose ester film 10 is subjected to a high temperature treatment (eg, For example, after heating at 150 ° C. for 20 minutes), the degree of plasticizer and UV absorber bleed out of the surface of the cellulose ester film 10 is analyzed by gas chromatography (GC). Less than 10%, preferably 1 to 8%, more preferably 1 to 5%, is to be bred out. Therefore, the cellulose ester film 10 according to the present invention can minimize the contamination of the film manufacturing equipment and the surface contamination of the cellulose ester film 10 by the plasticizer and the ultraviolet absorber during the film 10 manufacturing process. In addition, in order to improve scratch resistance, after coating the surface (front layer 12 and / or rear layer 16) of the film 10 with an ultraviolet curable acrylic hard coating agent or the like, the coating layer and the film ( 10) The result of confirming the adhesion (adhesive force) between the surfaces is 97/100 to 100/100. Here, the cross hatch method (ASTM D3359) draws gold with a knife to form 100 square grids on the surface of the coated film, attaches a sensitive tape on the 100 square grids, and then peels off the tape quickly to remain on the coated film surface. As a method of measuring the number of rectangular grids present, the relative adhesion between the coating layer and the film surface can be indicated.

The cellulose ester film 10 of the present invention is usually attached to one side or both sides of a polarizing plate made of polyvinyl alcohol (PVA), and serves to protect the polarizing plate, and the polarizing element with the cellulose ester film is a liquid crystal display device. It is attached to the top and / or bottom of the panel. In addition, if necessary, the polarizing plate and the cellulose ester protective film according to the present invention may be positioned at predetermined intervals (Cell Gap).

Hereinafter, the present invention will be described in more detail with reference to specific examples. The following examples are intended to illustrate the invention, and the invention is not limited by the following examples.

EXAMPLES Preparation and Evaluation of Cellulose Ester Film

15% by weight of the cellulose ester component (triacetylcellulose), 81.7% by weight of a mixed solvent of methylene chloride and butanol (weight ratio = 95: 5), 2.25% by weight of triphenylphosphate and 0.75% by weight of butylphthalylbutylglycolate, and As ultraviolet absorbers, 0.18% by weight of 2- (hydroxy-5-t-octylphenyl) benzotriazole and 2- (2'-hydroxy-3,5'-di-t-butylphenyl) -5-chlorobenzo Using 0.12% by weight of triazole, a casting stock solution for forming the front layer 12, the inner layer 14 and the back layer 16 of the cellulose ester film was prepared, but the plasticizer 100 contained in the inner layer 14 The front layer 12 and the plasticizer included in the front layer 12 and the rear layer 16 are each 10 parts by weight, and 100 parts by weight of the ultraviolet absorber included in the inner layer 14, relative to the parts by weight. 10 weight part of ultraviolet absorbers contained in the back layer 16 were made.

Each casting stock solution for forming the front layer 12, the inner layer 14 and the back layer 16, using a die shown in FIG. 2, a sheet 90 mm thick and 600 mm wide on the surface of the metal belt. Casting was in the form of sheets. While rotating the metal belt, the solvent of the casting stock solution was evaporated, stretched and dried to have a total thickness of 80 µm and a thickness of the front layer 12, the inner layer 14 and the rear layer 16, respectively. The cellulose-ester film 10 which is micrometer, 64 micrometers, and 8 micrometers was formed into a film.

After heat-treating the prepared cellulose ester film 10 at 150 ° C. for 20 minutes, gas chromatography (GC) was used to measure the amount of plasticizer and ultraviolet absorber on the surface to evaluate the degree of breeding out. The content of the plasticizer bleed out to the surface (10) was 2% of the total plasticizer content, and the content of the ultraviolet absorber bleed out to the surface of the cellulose ester film 10 was 1% of the total ultraviolet absorbent content. In addition, after the UV-curable acrylic hard coating agent (manufactured by Daikin Corporation) was coated on the surface of the manufactured cellulose ester film 10, the adhesion (adhesive force) between the coating layer and the surface of the film 10 was confirmed by ASTM D3359 (Cross hatch method). The result was 98/100.

1 is an overall schematic view of a film production apparatus that can be used for the production of a cellulose ester film according to the present invention.

FIG. 2 is an enlarged cross-sectional view of a die and a belt portion in the film manufacturing apparatus shown in FIG. 1. FIG.

Claims (4)

Front layer; Inner layer; And a back layer, The front layer, the inner layer and the back layer includes two or more plasticizers and two or more ultraviolet absorbers, the total amount of the plasticizer is 10 to 30% by weight relative to the total cellulose ester film, the total amount of the ultraviolet absorber, 0.01 to 5% by weight based on the total cellulose ester film, and based on 100 parts by weight of the plasticizer included in the inner layer, the amount of the plasticizer included in the front layer and the rear layer is 10 parts by weight or less, respectively, To 100 parts by weight of the ultraviolet absorber included, the content of the ultraviolet absorber contained in the front layer and the back layer is 10 parts by weight or less, respectively. According to claim 1, wherein the total thickness of the cellulose ester film is 20 to 100㎛, the thickness of the front layer and the back layer is 5 to 20% of the total film thickness, respectively, the thickness of the inner layer of the film 60 to 90% of the cellulose ester film. The method according to claim 1, wherein the adhesion between the coating layer and the film measured using ASTM D3359 (Cross hatch method) when the front layer and / or back layer of the cellulose ester film is coated is 97/100 to 100/100. Cellulose ester film. The first casting stock solution, the second casting stock solution and the third casting stock solution containing a cellulose ester component, a solvent for dissolving the cellulose ester component, two or more ultraviolet absorbers and two or more plasticizers are coextruded to the surface of the belt to obtain a sheet ( sheet) and evaporating the solvent present in the casting stock solution to form a cellulose ester film consisting of a front layer, an inner layer and a back layer; Peeling the cellulose ester film from the belt; And Stretching and drying the peeled cellulose ester film, The content of the total plasticizer is 10 to 30% by weight based on the total cellulose ester film, the content of the total ultraviolet absorber is 0.01 to 5% by weight relative to the total cellulose ester film, and 100 parts by weight of the plasticizer included in the inner layer. The amount of the plasticizer contained in the front layer and the rear layer is 10 parts by weight or less, respectively, and the content of the ultraviolet absorber included in the front layer and the rear layer is 100 parts by weight of the ultraviolet absorber included in the inner layer. The manufacturing method of the cellulose ester film which is 10 weight part or less each.
KR1020090134133A 2009-12-30 2009-12-30 Cellulose ester film and method for producing the same KR20110077523A (en)

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