WO2010041513A1 - 光学フィルム、光学フィルムの製造方法、偏光板および液晶表示装置 - Google Patents
光学フィルム、光学フィルムの製造方法、偏光板および液晶表示装置 Download PDFInfo
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- WO2010041513A1 WO2010041513A1 PCT/JP2009/064122 JP2009064122W WO2010041513A1 WO 2010041513 A1 WO2010041513 A1 WO 2010041513A1 JP 2009064122 W JP2009064122 W JP 2009064122W WO 2010041513 A1 WO2010041513 A1 WO 2010041513A1
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- Prior art keywords
- optical film
- film
- resin
- cellulose ester
- acrylic
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- 229910001870 ammonium persulfate Inorganic materials 0.000 description 6
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Images
Classifications
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- B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
- B29K2995/0018—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular optical properties, e.g. fluorescent or phosphorescent
- B29K2995/0034—Polarising
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
Definitions
- the present invention relates to an optical film, an optical film manufacturing method, a polarizing plate, and a liquid crystal display device, and more particularly to an optical film, a polarizing plate, and a liquid crystal display device that are less likely to leak light and have good reworkability.
- a liquid crystal display device is composed of a liquid crystal cell in which a transparent electrode, a liquid crystal layer, a color filter, etc. are sandwiched between glass plates, and two polarizing plates provided on both sides thereof.
- a polarizer also referred to as a polarizer or a polarizing film
- two optical films polarizing plate protective films.
- a cellulose triacetate film is usually used as this polarizing plate protective film.
- liquid crystal display devices Due to recent technological advances, the enlargement of liquid crystal display devices has accelerated, and the applications of liquid crystal display devices have diversified. For example, it can be used as a large display installed on a street or in a store, or used as an advertising display in a public place using a display device called digital signage.
- an acrylic resin is combined with an impact-resistant acrylic rubber-methyl methacrylate copolymer or butyl-modified acetyl cellulose in a quantitative ratio of 60 to 90/40 to 10 (patented)
- the acrylic resin film is prone to breakage and brittleness (brittleness), and it can stabilize optical films for large liquid crystal display devices, especially during film production and breakage during rework processes. It was difficult to manufacture.
- acrylic resin films represented by polymethyl methacrylate (hereinafter abbreviated as PMMA) generally have a problem that their heat resistance is poor and their shape changes when used at high temperatures or for long-term use.
- This problem was an important issue not only as a physical property of a single film but also in a polarizing plate and a display device using such a film. That is, in the liquid crystal display device, the polarizing plate curls as the film is deformed, which causes a problem that the entire panel is warped.
- Patent Document 2 A technique of mixing an acrylic resin with a cellulose ester film to control a plasticizer and optical properties has also been proposed (Patent Document 2).
- Patent Document 2 A technique of mixing an acrylic resin with a cellulose ester film to control a plasticizer and optical properties has also been proposed (Patent Document 2).
- the molecular weight of the acrylic resin disclosed here is small, sufficient moisture resistance cannot be obtained, and light leakage due to problems such as deterioration of the polarizing plate and change in the optical value of the optical film in a high humidity environment. It was not possible to improve.
- Patent Document 3 proposes a film produced by mixing an acrylic resin and a cellulose ester resin and manufactured by a melt casting method. Even with this method, brittleness could not be improved sufficiently.
- Patent Document 3 also describes an example in which a plasticizer is added. However, heat resistance that is originally necessary is deteriorated, and both brittleness and heat resistance cannot be achieved.
- the present invention aims to provide an optical film having improved hygroscopicity, heat resistance and even brittleness.
- an optical film which hardly causes light leakage and has good reworkability, and its production. It is an object to provide a method, a polarizing plate, and a liquid crystal display device.
- the acrylic resin (A) and the cellulose ester resin (B) are in a mass ratio of 95: 5 to 30:70, and the weight average molecular weight Mw of the acrylic resin (A) is 110,000 to 1000000, and the cellulose ester resin (B).
- the acyl ester total substitution degree (T) is 2.0 or more and 3.0 or less, the substitution degree of the acyl group having 3 or more and 7 or less carbon atoms is 1.2 or more and 3.0 or less, and the cellulose ester resin
- the weight average molecular weight Mw of (B) is from 75,000 to 300,000, the tension softening point is from 105 to 145 ° C., the folding resistance is from 50 to 100 times, and it is produced by a melt casting film forming method.
- Optical film is from 75,000 to 300,000, the tension softening point is from 105 to 145 ° C.
- the optical film according to 1 is manufactured by stretching in at least one of a transport direction and a width direction, and a stretching temperature thereof is Tg to Tg + 50 ° C. of the optical film before stretching.
- a method for producing an optical film is provided.
- a polarizing plate comprising the optical film described in 1 above.
- a liquid crystal display device comprising the polarizing plate described in 3 above.
- an optical film having improved hygroscopicity, heat resistance and brittleness at the same time, thereby providing an optical film which is less likely to leak light and has good reworkability, a method for producing the same, a polarizing plate and a liquid crystal display can do.
- the acrylic resin (A) and the cellulose ester resin (B) are in a mass ratio of 95: 5 to 30:70, and the weight average molecular weight Mw of the acrylic resin (A) is 110,000 to 1000000.
- the acyl group total substitution degree (T) of the cellulose ester resin (B) is 2.0 or more and 3.0 or less, and the substitution degree of the acyl group having 3 or more and 7 or less carbon atoms is 1.2 or more and 3.0 or less.
- the weight-average molecular weight Mw of the cellulose ester resin (B) is 75,000 to 300,000 as a constituent requirement, and its properties are a tension softening point of 105 to 145 ° C. and a folding resistance of 50 to 100 times.
- the manufacturing method is a melt casting film forming method.
- the acrylic resin used in the present invention includes a methacrylic resin.
- the resin is not particularly limited, but a resin comprising 50 to 99% by mass of methyl methacrylate units and 1 to 50% by mass of other monomer units copolymerizable therewith is preferable.
- Examples of other copolymerizable monomers include alkyl methacrylates having 2 to 18 alkyl carbon atoms, alkyl acrylates having 1 to 18 carbon atoms, alkyl acrylates such as acrylic acid and methacrylic acid.
- Unsaturated group-containing divalent carboxylic acids such as saturated acid, maleic acid, fumaric acid and itaconic acid, aromatic vinyl compounds such as styrene and ⁇ -methylstyrene, ⁇ , ⁇ -unsaturated nitriles such as acrylonitrile and methacrylonitrile, Examples thereof include maleic anhydride, maleimide, N-substituted maleimide, glutaric anhydride and the like, and these can be used alone or in combination of two or more monomers.
- methyl acrylate, ethyl acrylate, n-propyl acrylate, n-butyl acrylate, s-butyl acrylate, 2-ethylhexyl acrylate, and the like are preferable from the viewpoint of thermal decomposition resistance and fluidity of the copolymer.
- n-Butyl acrylate is particularly preferably used.
- the acrylic resin (A) used in the optical film of the present invention has a weight average molecular weight (Mw) particularly from the viewpoint of improving brittleness as an optical film and improving transparency when it is compatible with the cellulose ester resin (B). Is 120,000 or more and 1000000 or less.
- the weight average molecular weight (Mw) of the acrylic resin (A) is most preferably in the range of 130,000 to 300,000.
- the weight average molecular weight of the acrylic resin of the present invention can be measured by gel permeation chromatography (hereinafter abbreviated as GPC).
- GPC gel permeation chromatography
- the production method of the acrylic resin (A) in the present invention is not particularly limited, and any known method such as suspension polymerization, emulsion polymerization, bulk polymerization, or solution polymerization may be used.
- a polymerization initiator a normal peroxide type and an azo type can be used, and a redox type can also be used.
- the polymerization temperature may be 30 to 100 ° C. for suspension or emulsion polymerization, and 80 to 160 ° C. for bulk or solution polymerization.
- polymerization can be carried out using alkyl mercaptan or the like as a chain transfer agent.
- acrylic resins can be used as the acrylic resin according to the present invention.
- Delpet 60N, 80N (Asahi Kasei Chemicals Co., Ltd.), Dialal BR52, BR80, BR83, BR85, BR88 (Mitsubishi Rayon Co., Ltd.), KT75 (Electrochemical Industry Co., Ltd.) and the like can be mentioned.
- Two or more acrylic resins can be used in combination.
- the cellulose ester resin (B) of the present invention has a total acyl group substitution degree (T) of 2.0 to 3.3 from the viewpoint of transparency particularly when it is improved in brittleness and is compatible with the acrylic resin (A).
- the substitution degree of the acyl group having 0 and 3 to 7 carbon atoms is preferably 1.2 to 3.0, and the substitution degree of the acyl group having 3 to 7 carbon atoms is preferably 2.0 to 3.0.
- the cellulose ester resin of the present invention is a cellulose ester resin substituted with an acyl group having 3 to 7 carbon atoms.
- propionyl, butyryl and the like are preferably used, but a propionyl group is particularly preferably used. .
- the acrylic ester When the total substitution degree of the acyl group of the cellulose ester resin (B) is less than 2.0, that is, when the residual degree of the hydroxyl groups at the 2, 3, and 6 positions of the cellulose ester molecule is more than 1.0, the acrylic ester When the resin (A) and the acrylic resin (B) are not sufficiently compatible and used as an optical film, haze becomes a problem.
- the substitution degree of the acyl group having 3 to 7 carbon atoms is less than 1.2, still sufficient compatibility cannot be obtained, Brittleness will decrease.
- the substitution degree of the acyl group having 2 carbon atoms, that is, the acetyl group is high, and the substitution degree of the acyl group having 3 to 7 carbon atoms is 1.
- the compatibility is lowered and the haze is increased.
- the total substitution degree (T) is 2.0 to 3.0, and the substitution degree of the acyl group having 3 to 7 carbon atoms is 1.2 to 3. If it is 0.0, there is no problem, but the total degree of substitution of acyl groups other than those having 3 to 7 carbon atoms, that is, acetyl groups or acyl groups having 8 or more carbon atoms, is preferably 1.3 or less.
- the total substitution degree (T) of the acyl group of the cellulose ester resin (B) is more preferably in the range of 2.5 to 3.0.
- the acyl group may be an aliphatic acyl group or an aromatic acyl group. In the case of an aliphatic acyl group, it may be linear or branched and may further have a substituent.
- the number of carbon atoms of the acyl group in the present invention includes an acyl group substituent.
- the number of substituents X substituted on the aromatic ring is preferably 0 to 5. Also in this case, it is necessary to pay attention so that the degree of substitution of the acyl group having 3 to 7 carbon atoms including the substituent is 1.2 to 3.0. For example, since the benzoyl group has 7 carbon atoms, when it has a substituent containing carbon, the benzoyl group has 8 or more carbon atoms and is not included in the acyl group having 3 to 7 carbon atoms. Become.
- substituents substituted on the aromatic ring when the number of substituents substituted on the aromatic ring is 2 or more, they may be the same or different from each other, but they may be linked together to form a condensed polycyclic compound (for example, naphthalene, indene, indane, phenanthrene, quinoline). , Isoquinoline, chromene, chroman, phthalazine, acridine, indole, indoline, etc.).
- a condensed polycyclic compound for example, naphthalene, indene, indane, phenanthrene, quinoline.
- Isoquinoline chromene, chroman, phthalazine, acridine, indole, indoline, etc.
- a structure having at least one kind of an aliphatic acyl group having 3 to 7 carbon atoms is used as a structure used in the cellulose resin of the present invention.
- the substitution degree of the cellulose ester resin (B) according to the present invention is such that the total substitution degree (T) of acyl groups is 2.0 to 3.0, and the substitution degree of acyl groups having 3 to 7 carbon atoms is 1.2 to 3.0. 3.0.
- the total substitution degree of acyl groups other than an acyl group having 3 to 7 carbon atoms, that is, an acetyl group and an acyl group having 8 or more carbon atoms is 1.3 or less.
- the cellulose ester resin (B) according to the present invention is preferably at least one selected from cellulose acetate propionate, cellulose acetate butyrate, cellulose acetate benzoate, cellulose propionate, and cellulose butyrate, Those having an acyl group having 3 or 4 carbon atoms as a substituent are preferred.
- particularly preferable cellulose ester resins are cellulose acetate propionate and cellulose propionate.
- the portion not substituted with an acyl group usually exists as a hydroxyl group. These can be synthesized by known methods.
- substitution degree of the acetyl group and the substitution degree of other acyl groups were determined by the method prescribed in ASTM-D817-96.
- the weight average molecular weight (Mw) of the cellulose ester resin according to the present invention is 75,000 or more, particularly from the viewpoint of improving compatibility with the acrylic resin (A) and brittleness, and is preferably in the range of 75,000 to 300,000. It is more preferable that it is in the range of ⁇ 24,000, particularly preferably in the range of 160000 to 20,000.
- Mw weight average molecular weight
- the important average molecular weight (Mw) of the cellulose ester resin is less than 75,000, the effect of improving heat resistance and brittleness is not sufficient, and the effect of the present invention cannot be obtained.
- two or more kinds of cellulose resins can be mixed and used.
- the acrylic resin (A) and the cellulose ester resin (B) are contained in a mass ratio of 95: 5 to 30:70 and in a compatible state, preferably 95: 5 to 50. : 50, and more preferably 90:10 to 60:40.
- the mass ratio of the acrylic resin (A) and the cellulose ester resin (B) is more than 95: 5
- the effect of the cellulose ester resin (B) cannot be sufficiently obtained, and the mass ratio is
- the amount of acrylic resin is less than 30:70, the moisture resistance becomes insufficient.
- the acrylic resin (A) and the cellulose ester resin (B) are preferably contained in a compatible state.
- Whether the acrylic resin (A) and the cellulose ester resin (B) are in a compatible state can be determined by, for example, the glass transition temperature Tg.
- the two resins have different glass transition temperatures
- there are two or more glass transition temperatures for each resin because there is a glass transition temperature for each resin.
- the glass transition temperature specific to each resin disappears and becomes one glass transition temperature, which is the glass transition temperature of the compatible resin.
- the glass transition temperature referred to here is an intermediate value determined according to JIS K7121 (1987) using a differential scanning calorimeter (DSC-7 model manufactured by Perkin Elmer) at a heating rate of 20 ° C./min.
- the point glass transition temperature (Tmg) is an intermediate value determined according to JIS K7121 (1987) using a differential scanning calorimeter (DSC-7 model manufactured by Perkin Elmer) at a heating rate of 20 ° C./min.
- the point glass transition temperature (Tmg) The point glass transition temperature (Tmg).
- the acrylic resin (A) and the cellulose ester resin (B) are each preferably an amorphous resin, and either one may be a crystalline polymer or a partially crystalline polymer. In the present invention, the acrylic resin (A) and the cellulose ester resin (B) are preferably compatible with each other to become an amorphous resin.
- the weight average molecular weight (Mw) of the acrylic resin (A), the weight average molecular weight (Mw) of the cellulose ester resin (B), and the degree of substitution are different in solubility in the solvent of both resins. It is obtained by measuring each after use.
- fractionated resins can be identified by general structural analysis of polymers.
- the optical film of the present invention contains a resin other than the acrylic resin (A) and the cellulose ester resin (B), it can be separated by the same method.
- the weight average molecular weights (Mw) of the compatible resins are different, the high molecular weight substances are eluted earlier by gel permeation chromatography (GPC), and the lower molecular weight substances are eluted after a longer time. Therefore, it can be easily fractionated and the molecular weight can be measured.
- GPC gel permeation chromatography
- the molecular weight of the compatible resin is measured by GPC, and at the same time, the resin solution eluted every time is separated, the solvent is distilled off, and the dried resin is different by quantitatively analyzing the structure.
- the resin composition for each molecular weight fraction it is possible to identify each compatible resin.
- the molecular weight distribution of each of the resins separated in advance based on the difference in solubility in a solvent by GPC, it is possible to detect each of the compatible resins.
- containing acrylic resin (A) and cellulose ester resin (B) in a compatible state means mixing each resin (polymer) and resulting in a compatible state. This means that a state in which a precursor of acrylic resin such as monomer, dimer or oligomer is mixed with cellulose ester resin (B) and then polymerized by polymerization is not included. .
- the process of obtaining a mixed resin by mixing a precursor of an acrylic resin such as a monomer, dimer or oligomer with the cellulose ester resin (B) and then polymerizing it is complicated by the polymerization reaction.
- the resin is difficult to control the reaction, and it is difficult to adjust the molecular weight.
- graft polymerization, cross-linking reaction or cyclization reaction often occurs.
- the resin is soluble in a solvent or cannot be melted by heating. Since it is difficult to elute the resin and measure the weight average molecular weight (Mw), it is difficult to control the physical properties and it cannot be used as a resin for stably producing an optical film.
- Mw weight average molecular weight
- the optical film of the present invention may contain a resin and additives other than the acrylic resin (A) and the cellulose ester resin (B) as long as the function as the optical film is not impaired.
- the added resin may be mixed without being compatible even if it is in a compatible state.
- the total mass of the acrylic resin (A) and the cellulose ester resin (B) in the optical film of the present invention is preferably 55% by mass or more of the optical film, more preferably 60% by mass or more, and particularly preferably 70% by mass or more.
- the optical film of the present invention may contain acrylic particles.
- the acrylic particles (C) according to the present invention are present in the state of particles (also referred to as incompatible state) in the optical film containing the acrylic resin (A) and the cellulose ester resin (B) in a compatible state. Represents an acrylic component.
- the acrylic particles (C) are obtained, for example, by collecting a predetermined amount of the produced optical film, dissolving it in a solvent, stirring, and sufficiently dissolving / dispersing it, so that the pore diameter is less than the average particle diameter of the acrylic particles (C). It is preferable that the weight of the insoluble matter filtered and collected using the PTFE membrane filter is 90% by mass or more of the acrylic particles (C) added to the optical film.
- the acrylic particles (C) used in the present invention are not particularly limited, but are preferably acrylic particles (C) having a layer structure of two or more layers, particularly the following multilayer structure acrylic granular composite. It is preferable.
- the multilayer structure acrylic granular composite is formed by laminating an innermost hard layer polymer, a cross-linked soft layer polymer exhibiting rubber elasticity, and an outermost hard layer polymer from the center to the outer periphery.
- the multi-layer structure acrylic granular composite is a multi-layer structure acrylic granular composite composed of an innermost hard layer, a crosslinked soft layer, and an outermost hard layer from the center to the outer periphery.
- This three-layer core-shell multilayer acrylic granular composite is preferably used.
- Preferred embodiments of the multilayer structure acrylic granular composite used in the acrylic resin composition according to the present invention include the following.
- Outermost obtained by polymerizing The layered polymer has a three-layer structure, and the obtained three-layered polymer is the innermost hard layer polymer (a) 5 to 40% by mass, the soft layer polymer (b) 30 to 60% by mass.
- an outermost hard layer polymer (c) having an insoluble part when fractionated with acetone, and having a methyl ethyl ketone swelling degree of 1.5 to 4.0. Complex.
- the innermost hard layer polymer (a) constituting the multilayer structure acrylic granular composite is 80 to 98.9% by mass of methyl methacrylate and 1 to 20 mass of alkyl acrylate having 1 to 8 carbon atoms in the alkyl group. % And a mixture of monomers consisting of 0.01 to 0.3% by weight of a polyfunctional grafting agent is preferred.
- examples of the alkyl acrylate having 1 to 8 carbon atoms in the alkyl group include methyl acrylate, ethyl acrylate, n-propyl acrylate, n-butyl acrylate, s-butyl acrylate, 2-ethylhexyl acrylate, and the like. And n-butyl acrylate are preferably used.
- the proportion of the alkyl acrylate unit in the innermost hard layer polymer (a) is 1 to 20% by mass.
- the thermal decomposability of the polymer is increased, while the unit is 20% by mass. If it exceeds 50%, the glass transition temperature of the innermost hard layer polymer (c) is lowered, and the impact resistance imparting effect of the three-layer structure acrylic granular composite is lowered.
- polyfunctional grafting agent examples include polyfunctional monomers having different polymerizable functional groups, such as allyl esters of acrylic acid, methacrylic acid, maleic acid, and fumaric acid, and allyl methacrylate is preferably used.
- the polyfunctional grafting agent is used to chemically bond the innermost hard layer polymer and the soft layer polymer, and the ratio used during the innermost hard layer polymerization is 0.01 to 0.3% by mass. .
- the crosslinked soft layer polymer (b) constituting the acrylic granular composite is an alkyl acrylate having from 9 to 8 carbon atoms having an alkyl group of 1 to 8 in the presence of the innermost hard layer polymer (a). What is obtained by polymerizing a mixture of monomers comprising, by mass, 0.01 to 5% by mass of a polyfunctional crosslinking agent and 0.5 to 5% by mass of a polyfunctional grafting agent is preferred.
- n-butyl acrylate or 2-ethylhexyl acrylate is preferably used as the alkyl acrylate having 4 to 8 carbon atoms in the alkyl group.
- Examples of other monofunctional monomers that can be copolymerized include styrene and substituted styrene derivatives.
- styrene and substituted styrene derivatives Regarding the ratio of alkyl acrylate having 4 to 8 carbon atoms in the alkyl group and styrene, the more the former, the lower the glass transition temperature of the polymer (b), that is, the softer it is.
- the refractive index of the soft layer polymer (b) at room temperature is set to the innermost hard layer polymer (a), the outermost hard layer polymer (c), and the hard heat. It is more advantageous to make it closer to the plastic acrylic resin, and the ratio between them is selected in consideration of these.
- polyfunctional grafting agent those mentioned in the section of the innermost layer hard polymer (a) can be used.
- the polyfunctional grafting agent used here is used to chemically bond the soft layer polymer (b) and the outermost hard layer polymer (c), and the proportion used during the innermost hard layer polymerization is impact resistance. From the viewpoint of the effect of imparting properties, 0.5 to 5% by mass is preferable.
- polyfunctional crosslinking agent generally known crosslinking agents such as divinyl compounds, diallyl compounds, diacrylic compounds, dimethacrylic compounds and the like can be used, but polyethylene glycol diacrylate (molecular weight 200 to 600) is preferably used.
- the polyfunctional cross-linking agent used here is used to generate a cross-linked structure during the polymerization of the soft layer (b) and to exhibit the effect of imparting impact resistance.
- the polyfunctional crosslinking agent is not an essential component because the crosslinked structure of the soft layer (b) is generated to some extent. Is preferably 0.01 to 5% by weight from the viewpoint of imparting impact resistance.
- the outermost hard layer polymer (c) constituting the multi-layer structure acrylic granular composite has a methyl methacrylate of 80 to 99 mass in the presence of the innermost hard layer polymer (a) and the soft layer polymer (b). % And a mixture of monomers consisting of 1 to 20% by mass of an alkyl acrylate having 1 to 8 carbon atoms in the alkyl group is preferred.
- the acrylic alkylate those described above are used, but methyl acrylate and ethyl acrylate are preferably used.
- the proportion of the alkyl acrylate unit in the outermost hard layer (c) is preferably 1 to 20% by mass.
- an alkyl mercaptan or the like can be used as a chain transfer agent to adjust the molecular weight for the purpose of improving the compatibility with the acrylic resin (A).
- the outermost hard layer with a gradient such that the molecular weight gradually decreases from the inside toward the outside in order to improve the balance between elongation and impact resistance.
- the outermost hard layer is divided into two or more monomer mixtures for forming the outermost hard layer, and the amount of chain transfer agent to be added each time is increased sequentially. It is possible to decrease the molecular weight of the polymer forming the layer from the inside to the outside of the multilayer structure acrylic granular composite.
- the molecular weight formed at this time can also be examined by polymerizing a mixture of monomers used each time under the same conditions, and measuring the molecular weight of the resulting polymer.
- the particle diameter of the acrylic particles (C) preferably used in the present invention is not particularly limited, but is preferably 10 nm or more and 1000 nm or less, and more preferably 20 nm or more and 500 nm or less. In particular, the thickness is most preferably from 50 nm to 400 nm.
- the mass ratio of the core and the shell is not particularly limited, but when the entire multilayer structure polymer is 100 parts by mass,
- the core layer is preferably 50 parts by mass or more and 90 parts by mass or less, and more preferably 60 parts by mass or more and 80 parts by mass or less.
- the core layer here is an innermost hard layer.
- Examples of such commercially available multilayered acrylic granular composites include, for example, “Metablene” manufactured by Mitsubishi Rayon Co., “Kane Ace” manufactured by Kaneka Chemical Co., Ltd., “Paraloid” manufactured by Kureha Chemical Co., Ltd., Rohm and Haas “Acryloid” manufactured by KK, “Staffyroid” manufactured by Ganz Kasei Kogyo Co., Ltd., “Parapet SA” manufactured by Kuraray Co., Ltd., and the like can be used alone or in combination of two or more.
- acrylic particles (C1) which are graft copolymers preferably used as the acrylic particles (C) preferably used in the present invention include unsaturated carboxylic acid esters in the presence of a rubbery polymer. Copolymerization of a mixture of monomers, unsaturated carboxylic acid monomers, aromatic vinyl monomers, and other vinyl monomers copolymerizable with these if necessary Examples thereof include a graft copolymer.
- the rubbery polymer used for the acrylic particles (C1) that are the graft copolymer is not particularly limited, but diene rubber, acrylic rubber, ethylene rubber, and the like can be used. Specific examples include polybutadiene, styrene-butadiene copolymer, block copolymer of styrene-butadiene, acrylonitrile-butadiene copolymer, butyl acrylate-butadiene copolymer, polyisoprene, butadiene-methyl methacrylate copolymer, Butyl acrylate-methyl methacrylate copolymer, butadiene-ethyl acrylate copolymer, ethylene-propylene copolymer, ethylene-propylene-diene copolymer, ethylene-isoprene copolymer, and ethylene-methyl acrylate copolymer A polymer etc. are mentioned. These rubbery polymers can be used alone or in a mixture of two or more
- the refractive index of the mixture of an acrylic resin (A) and a cellulose-ester resin (B) and the refractive index of an acrylic particle (C) must be near. From the viewpoint of obtaining a film with high transparency.
- the refractive index difference between the acrylic particles (C) and the acrylic resin (A) is preferably 0.05 or less, more preferably 0.02 or less, and particularly preferably 0.01 or less.
- a method of adjusting the monomer unit composition ratio of the acrylic resin (A) and / or a rubbery polymer or monomer used for the acrylic particles (C) The refractive index difference can be reduced by a method of adjusting the composition ratio, and an optical film excellent in transparency can be obtained.
- the refractive index difference referred to here is a solution in which the optical film of the present invention is sufficiently dissolved in a solvent in which the acrylic resin (A) is soluble to obtain a cloudy solution, which is subjected to an operation such as centrifugation. After separating the solvent-soluble part and the insoluble part and purifying the soluble part (acrylic resin (A)) and insoluble part (acrylic particles (C)), the measured refractive index (23 ° C., measuring wavelength: 550 nm). ) Difference.
- the method of blending the acrylic particles (C) with the acrylic resin (A) is not particularly limited. After the acrylic resin (A) and other optional components are previously blended, usually at 200 to 350 ° C. A method of uniformly melt-kneading with a single-screw or twin-screw extruder while adding acrylic particles (C) is preferably used.
- a method in which a solution in which acrylic particles (C) are dispersed in advance is added to and mixed with a solution (dope solution) in which acrylic resin (A) and cellulose ester resin (B) are dissolved, acrylic particles (C) and A method such as in-line addition of a solution obtained by dissolving or mixing other optional additives can be used.
- acrylic particles can also be used as the acrylic particles according to the present invention.
- Examples thereof include Metablen W-341 (C2) (manufactured by Mitsubishi Rayon Co., Ltd.), Chemisnow MR-2G (C3), MS-300X (C4) (manufactured by Soken Chemical Co., Ltd.), and the like.
- the optical film of the present invention preferably contains 0.5 to 30% by mass of acrylic particles (C) with respect to the total mass of the resin constituting the film, and is in the range of 1.0 to 15% by mass. It is more preferable to contain.
- the optical film of the present invention includes a plasticizer for imparting processability to the film, an antioxidant for preventing deterioration of the film, an ultraviolet absorber for imparting an ultraviolet absorbing function, and fine particles (matting agent) for imparting slipperiness to the film. It is preferable to contain additives such as ⁇ Plasticizer>
- the plasticizer include phthalate ester, fatty acid ester, trimellitic ester, phosphate ester, polyester, and epoxy.
- polyester-based and phthalate-based plasticizers are preferably used.
- Polyester plasticizers are superior in non-migration and extraction resistance compared to phthalate ester plasticizers such as dioctyl phthalate, but are slightly inferior in plasticizing effect and compatibility.
- the polyester plasticizer is a reaction product of a monovalent or tetravalent carboxylic acid and a monovalent or hexavalent alcohol, and is mainly obtained by reacting a divalent carboxylic acid with a glycol.
- Representative divalent carboxylic acids include glutaric acid, itaconic acid, adipic acid, phthalic acid, azelaic acid, sebacic acid and the like.
- glycol examples include glycols such as ethylene, propylene, 1,3-butylene, 1,4-butylene, 1,6-hexamethylene, neopentylene, diethylene, triethylene, and dipropylene. These divalent carboxylic acids and glycols may be used alone or in combination.
- the ester plasticizer may be any of ester, oligoester, and polyester types, and the molecular weight is preferably in the range of 100 to 10,000, and preferably in the range of 600 to 3000, which has a large plasticizing effect.
- the viscosity of the plasticizer has a correlation with the molecular structure and molecular weight, but in the case of an adipic acid plasticizer, the range of 200 to 5000 MPa ⁇ s (25 ° C.) is preferable because of compatibility and plasticization efficiency. Furthermore, some polyester plasticizers may be used in combination.
- the plasticizer is preferably added in an amount of 0.5 to 30 parts by mass with respect to 100 parts by mass of the optical film of the present invention. If the added amount of the plasticizer exceeds 30 parts by mass, the surface becomes sticky, which is not preferable for practical use.
- Antioxidant> In this invention, what is generally known can be used as an antioxidant.
- lactone, sulfur, phenol, double bond, hindered amine and phosphorus compounds can be preferably used.
- the phenolic compound preferably has a 2,6-dialkylphenol structure.
- trade names of Ciba Japan Co., Ltd. “Irganox 1076”, “Irganox 1010”, and ADEKA “ADEKA STAB AO-50” And those commercially available.
- the phosphorus compounds are, for example, from Sumitomo Chemical Co., Ltd., “Sumizer GP”, from ADEKA Co., Ltd., “ADK STAB PEP-24G”, “ADK STAB PEP-36” and “ADK STAB 3010”, from Ciba Japan Co., Ltd. “IRGAFOS P-EPQ”, commercially available from Sakai Chemical Industry Co., Ltd. under the trade name “GSY-P101” is preferable.
- the above-mentioned hindered amine compounds are preferably those commercially available from Ciba Japan Co., Ltd. under the trade names of “Tinuvin 144” and “Tinvin 770” and from ADEKA Co., Ltd. “ADK STAB LA-52”.
- the above sulfur compounds are preferably those commercially available from Sumitomo Chemical Co., Ltd. under the trade names “Sumilizer TPL-R” and “Sumilizer TP-D”.
- the above-mentioned double bond compound is preferably commercially available from Sumitomo Chemical Co., Ltd. under the trade names of “Sumilizer GM” and “Sumilizer GS”.
- the amount of these antioxidants and the like to be added is appropriately determined in accordance with the process for recycling and use, but generally 0.05 to 20% by mass, preferably with respect to the resin as the main raw material of the film Is added in the range of 0.1 to 1% by mass.
- antioxidants can obtain a synergistic effect by using several different types of compounds in combination rather than using only one kind.
- the combined use of lactone, phosphorus, phenol and double bond compounds is preferred.
- a colorant means a dye or a pigment.
- the colorant means an effect of making the color tone of a liquid crystal screen blue, adjusting the yellow index, and reducing haze.
- Various dyes and pigments can be used as the colorant, but anthraquinone dyes, azo dyes, phthalocyanine pigments and the like are effective.
- ⁇ Ultraviolet absorber> Although the ultraviolet absorber used in the present invention is not particularly limited, for example, oxybenzophenone compounds, benzotriazole compounds, salicylic acid ester compounds, benzophenone compounds, cyanoacrylate compounds, triazine compounds, nickel complex compounds, inorganic powders Examples include the body. It is good also as a polymer type ultraviolet absorber.
- ⁇ Matting agent> In the present invention, it is preferable to add a matting agent in order to impart film slipperiness.
- any inorganic compound or organic compound may be used as long as it has heat resistance at the time of melting without impairing the transparency of the obtained film.
- talc mica, zeolite, diatomaceous earth, Calcined siliceous clay, kaolin, sericite, bentonite, smectite, clay, silica, quartz powder, glass beads, glass powder, glass flakes, milled fiber, wollastonite, boron nitride, boron carbide, titanium boride, magnesium carbonate, Heavy calcium carbonate, light calcium carbonate, calcium silicate, aluminum silicate, magnesium silicate, magnesium aluminosilicate, alumina, silica, zinc oxide, titanium dioxide, iron oxide, magnesium oxide, zirconium oxide, aluminum hydroxide, calcium hydroxide, water Magne oxide Um, calcium sulfate, barium sulfate, silicon carbide, aluminum carbide, titanium carbide, aluminum nitride
- High transparency and slipperiness can be achieved at the same time by using particles having different particle sizes and shapes (for example, needle shape and spherical shape).
- silicon dioxide is particularly preferably used since it has a refractive index close to that of cellulose ester and is excellent in transparency (haze).
- silicon dioxide examples include Aerosil 200V, Aerosil R972V, Aerosil R972, R974, R812, 200, 300, R202, OX50, TT600, NAX50 (manufactured by Nippon Aerosil Co., Ltd.), Sea Hoster KEP-10, Sea Hoster KEP- 30, Seahoster KEP-50 (above, manufactured by Nippon Shokubai Co., Ltd.), Silo Hovic 100 (manufactured by Fuji Silysia), Nip Seal E220A (manufactured by Nippon Silica Industry), Admafine SO (manufactured by Admatechs), etc. Goods etc. can be preferably used.
- the shape of the particles can be used without particular limitation, such as indefinite shape, needle shape, flat shape, spherical shape, etc. However, the use of spherical particles is preferable because the transparency of the resulting film can be improved.
- the particle size is preferably smaller than the wavelength of visible light, and more preferably 1 ⁇ 2 or less of the wavelength of visible light. . If the size of the particles is too small, the slipperiness may not be improved, so the range of 80 nm to 180 nm is particularly preferable.
- the particle size means the size of the aggregate when the particle is an aggregate of primary particles. Moreover, when a particle is not spherical, it means the diameter of a circle corresponding to the projected area.
- a hydrogen bonding solvent can be added for the purpose of reducing the melt viscosity.
- the hydrogen bonding solvent is J.I. N.
- the glass transition temperature of the cellulose resin used alone is higher than that.
- the melting temperature of the cellulose resin composition can be lowered by the addition of a hydrogen bonding solvent, or the melt viscosity of the cellulose resin composition containing a hydrogen bonding solvent can be lowered at the same melting temperature as the cellulose resin. .
- the brittleness index is determined based on the criterion of whether or not it is “an optical film that does not cause ductile fracture”.
- the ductile fracture is a fracture that occurs due to a stress that is greater than the strength of a certain material, and is defined as a fracture that involves significant elongation or drawing of the material before the final fracture.
- whether or not it is “an optical film that does not cause ductile fracture” is evaluated by the fact that no breakage such as breakage is observed even when a large stress is applied such that the film is folded in two. . (This evaluation is called folding resistance.) If it is an optical film that does not cause ductile fracture even when such a large stress is applied, it is used as a polarizing plate protective film for an enlarged liquid crystal display device. Even in such a case, it becomes possible to sufficiently reduce problems such as breakage at the time of manufacture. Further, even when the optical film is used after being peeled off once, the breakage does not occur. It can sufficiently cope with thinning.
- the folding resistance is 50 to 100 times, even when used as a polarizing plate protective film for a large-sized liquid crystal display device, it is possible to sufficiently reduce problems such as breakage during manufacturing. Furthermore, even when the optical film is used after being pasted once and then peeled off again, no breakage occurs, and the optical film can be sufficiently reduced in thickness.
- the folding resistance is less than 50 times, breakage is likely to occur during production and the reworkability is poor.
- it in order to exceed 100 times, it can be achieved by increasing the film thickness, but it cannot cope with the thinning of the liquid crystal display device. Therefore, in the case of a thin film, 50 to 100 times is appropriate.
- the tension softening point is used as an index of heat resistance.
- the tension softening point is 105 ° C. to 145 ° C., it can be judged that sufficient heat resistance is exhibited. In particular, it is more preferable to control at 110 ° C. to 130 ° C.
- the tension softening point is less than 105 ° C., the heat generated by the backlight light source cannot be withstood, and the film is likely to be deformed or light leakage is likely to occur.
- the tension softening point is suitably from 105 ° C to 145 ° C.
- the optical film is cut out at 120 mm (length) ⁇ 10 mm (width).
- the temperature can be raised at a rate of 30 ° C./min while pulling with a tension of 10 N, and the temperature at the time when the pressure reaches 9 N is measured three times, and the average value can be obtained.
- the optical film preferably has a glass transition temperature (Tg) of 110 ° C. or higher. More preferably, it is 120 ° C. or higher. Especially preferably, it is 150 degreeC or more.
- Tg glass transition temperature
- the glass transition temperature referred to here is an intermediate value determined according to JIS K7121 (1987) using a differential scanning calorimeter (DSC-7 model manufactured by Perkin Elmer) at a heating rate of 20 ° C./min. Point glass transition temperature (Tmg).
- Haze value is used as an index for judging the transparency of the optical film in the present invention.
- liquid crystal display devices used outdoors are required to have sufficient brightness and high contrast even in a bright place. Therefore, the haze value is required to be 1.0% or less, and 0.5% or less. More preferably.
- the optical film of the present invention containing the acrylic resin (A) and the cellulose ester resin (B), high transparency can be obtained, but when using acrylic particles for the purpose of improving another physical property.
- acrylic particles for the purpose of improving another physical property.
- the particle diameter and addition amount of acrylic particles (C) should be kept within the above range, and the surface roughness of the film contact portion during film formation should be reduced. Is also effective.
- the hygroscopicity of the optical film in the present invention is evaluated by dimensional change with respect to humidity change.
- the following method is used as an evaluation method of dimensional change with respect to humidity change.
- the dimensional change rate (%) is expressed by the following formula.
- Dimensional change rate (%) [(a1-a2) / a1] ⁇ 100 a1: Distance before heat treatment a2: Distance after heat treatment
- a1 Distance before heat treatment
- a2 Distance after heat treatment
- the optical film of the present invention preferably has a defect with a diameter of 5 ⁇ m or more in the film plane of 1 piece / 10 cm square or less. More preferably, it is 0.5 piece / 10 cm square or less, more preferably 0.1 piece / 10 cm square or less.
- the diameter of the defect indicates the diameter when the defect is circular, and when it is not circular, the range of the defect is determined by observing with a microscope according to the following method, and the maximum diameter (diameter of circumscribed circle) is determined.
- the range of the defect is the size of the shadow when the defect is observed with the transmitted light of the differential interference microscope when the defect is a bubble or a foreign object.
- the defect is a change in the surface shape, such as transfer of a roll flaw or an abrasion
- the size is confirmed by observing the defect with the reflected light of a differential interference microscope.
- the film When the number of defects is more than 1/10 cm square, for example, when a tension is applied to the film during processing in a later process, the film may be broken with the defect as a starting point and productivity may be reduced. Moreover, when the diameter of a defect becomes 5 micrometers or more, it can confirm visually by polarizing plate observation etc., and when used as an optical member, a bright spot may arise.
- the coating agent may not be formed uniformly, resulting in defects (coating defects).
- the defect is a void in the film (foaming defect) generated due to the rapid evaporation of the solvent in the drying process of the solution casting, a foreign matter in the film forming stock solution, or a foreign matter mixed in the film forming. This refers to the foreign matter (foreign matter defect) in the film.
- the optical film of the present invention preferably has a breaking elongation in at least one direction of 10% or more, more preferably 20% or more in the measurement based on JIS-K7127-1999.
- the upper limit of the elongation at break is not particularly limited, but is practically about 250%. In order to increase the elongation at break, it is effective to suppress defects in the film caused by foreign matter and foaming.
- the thickness of the optical film of the present invention is preferably 20 ⁇ m or more. More preferably, it is 30 ⁇ m or more.
- the optical film of the present invention preferably has a total light transmittance of 90% or more, more preferably 93% or more. Moreover, as a realistic upper limit, it is about 99%. In order to achieve excellent transparency expressed by such total light transmittance, it is necessary not to introduce additives and copolymerization components that absorb visible light, or to remove foreign substances in the polymer by high-precision filtration. It is effective to reduce the diffusion and absorption of light inside the film.
- the optical film of the present invention can be particularly preferably used as a polarizing plate protective film for a large-sized liquid crystal display device or a liquid crystal display device for outdoor use as long as the above physical properties are satisfied.
- Method for producing optical film by melt casting method comprises melting an acrylic resin (A) and a cellulose ester resin (B) in a mass ratio of 95: 5 to 30:70, extruding them from a die, and placing them on a cooling roll. It is the manufacturing method of the optical film to cast.
- composition constituting the optical film comprising the acrylic resin (A), cellulose ester resin (B), and other additives used for melt extrusion is usually preferably kneaded in advance and pelletized.
- Pelletization may be performed by a known method. For example, dry acrylic resin (A), dry cellulose ester resin (B) and other additives are fed to an extruder with a feeder and mixed using a single-screw or twin-screw extruder. It can be smelted, extruded from a die into a strand, cooled with water or air, and cut.
- dry acrylic resin (A) dry cellulose ester resin (B) and other additives are fed to an extruder with a feeder and mixed using a single-screw or twin-screw extruder. It can be smelted, extruded from a die into a strand, cooled with water or air, and cut.
- cellulose ester easily absorbs moisture, it is preferable to dry it at 70 to 140 ° C. for 3 hours or more with a dehumidifying hot air dryer or a vacuum dryer so that the moisture content is 200 ppm or less, and further 100 ppm or less.
- Additives may be fed into the extruder and fed into the extruder, or may be fed through individual feeders.
- a small amount of an additive such as an antioxidant is preferably mixed in advance in order to mix uniformly.
- Mixing of the antioxidants may be performed by mixing solids, or if necessary, the antioxidant is dissolved in a solvent, and the acrylic resin (A) and cellulose ester resin (B) are impregnated and mixed. Or may be mixed by spraying.
- a vacuum nauter mixer is preferable because it can dry and mix simultaneously. Moreover, when touching with air, such as an exit from a feeder part or die
- the extruder is preferably processed at as low a temperature as possible so as to be able to be pelletized so that the shear force is suppressed and the resin does not deteriorate (molecular weight reduction, coloring, gel formation, etc.).
- a twin screw extruder it is preferable to rotate in the same direction using a deep groove type screw. From the uniformity of kneading, the meshing type is preferable.
- Film formation is performed using the pellets obtained as described above. It is also possible to feed the raw material powder directly to the extruder with a feeder and form a film as it is without pelletization.
- the pellets produced are extruded using a single-screw or twin-screw extruder, the melting temperature Tm during extrusion is set to about 200 to 300 ° C., filtered through a leaf disk type filter or the like to remove foreign matter, and then the T-die The film is coextruded into a film, solidified on a cooling roll, and cast while pressing with an elastic touch roll.
- Tm is the temperature of the die exit portion of the extruder.
- defects are also referred to as die lines, but in order to reduce surface defects such as die lines, it is preferable to have a structure in which the resin retention portion is minimized in the piping from the extruder to the die. . It is preferable to use a die that has as few scratches as possible inside the lip.
- the inner surface that comes into contact with the molten resin is preferably subjected to surface treatment that makes it difficult for the molten resin to adhere to the surface by reducing the surface roughness or using a material with low surface energy.
- a hard chrome plated or ceramic sprayed material is polished so that the surface roughness is 0.2 S or less.
- the cooling roll of the present invention is not particularly limited, but is a roll having a structure in which a heat medium or a coolant that can be controlled in temperature flows through a highly rigid metal roll, and the size is not limited. It is sufficient that the film is large enough to cool the film, and the diameter of the cooling roll is usually about 100 mm to 1 m.
- the surface material of the cooling roll includes carbon steel, stainless steel, aluminum, titanium and the like. Further, in order to increase the surface hardness or improve the releasability from the resin, it is preferable to perform a surface treatment such as hard chrome plating, nickel plating, amorphous chrome plating, ceramic spraying, or the like.
- the surface roughness of the cooling roll surface is preferably 0.1 ⁇ m or less in terms of Ra, and more preferably 0.05 ⁇ m or less.
- the smoother the roll surface the smoother the surface of the resulting film.
- the surface processed is further polished to have the above-described surface roughness.
- Examples of the elastic touch roll of the present invention include JP-A-03-124425, JP-A-08-224772, JP-A-07-1000096, JP-A-10-272676, WO97-028950, JP-A-11-235747, JP-A-11-235747.
- a thin-film metal sleeve-covered silicon rubber roll can be used.
- the film obtained as described above is further stretched 1.01 to 3.0 times in at least one direction after passing through the step of contacting the cooling roll.
- the brittleness of the present invention can be realized by stretching.
- the film is stretched 1.1 to 2.0 times in both the longitudinal (film transport direction) and lateral (width direction) directions.
- the stretching method a known roll stretching machine or tenter can be preferably used.
- the optical film also serves as a polarizing plate protective film, it is preferable to stack the polarizing film in a roll form by setting the stretching direction to the width direction.
- the slow axis of the optical film becomes the width direction by stretching in the width direction.
- the draw ratio is 1.1 to 3.0 times, preferably 1.2 to 1.5 times
- the drawing temperature is usually Tg to Tg + 50 ° C. of the resin constituting the film, preferably Tg to Tg + 50 ° C. In the temperature range.
- the stretching is preferably performed under a uniform temperature distribution controlled in the longitudinal direction or the width direction.
- the temperature is preferably within ⁇ 2 ° C, more preferably within ⁇ 1 ° C, and particularly preferably within ⁇ 0.5 ° C.
- the film may be contracted in the longitudinal direction or the lateral direction for the purpose of adjusting the retardation of the optical film produced by the above method and reducing the dimensional change rate.
- Uniformity in the slow axis direction is also important, and the angle is preferably ⁇ 5 to + 5 ° with respect to the film width direction, more preferably in the range of ⁇ 1 to + 1 °, particularly ⁇ 0.
- a range of 5 to + 0.5 ° is preferable, and a range of ⁇ 0.1 to + 0.1 ° is particularly preferable.
- the height from the top of the adjacent mountain to the bottom of the valley is 300 nm or more, and there is no streak continuous in the longitudinal direction with an inclination of 300 nm / mm or more.
- the shape of the streak was measured using a surface roughness meter. Specifically, using a Mitutoyo SV-3100S4, a stylus (diamond needle) having a tip shape of a cone of 60 ° and a tip curvature radius of 2 ⁇ m was used. The film is scanned in the width direction of the film at a measurement speed of 1.0 mm / sec while applying a load of 0.75 mN, and a cross-sectional curve is measured with a Z-axis (thickness direction) resolution of 0.001 ⁇ m.
- the streak height reads the vertical distance (H) from the top of the mountain to the bottom of the valley.
- the slope of the streak is obtained by reading the horizontal distance (L) from the top of the mountain to the bottom of the valley and dividing the vertical distance (H) by the horizontal distance (L).
- the cleaning device there are no particular restrictions on the cleaning device. For example, there are a method of niping a brush roll, a water absorbing roll, an adhesive roll, a wiping roll, an air blow method of blowing clean air, a laser incinerator, or a combination thereof. is there.
- the optical film of the present invention is preferably a long film.
- the optical film has a thickness of about 100 m to 5000 m, and is usually in the form of a roll.
- the film width is preferably 1.3 to 4 m, more preferably 1.4 to 2 m.
- the film thickness of the optical film of the present invention is not particularly limited, but when used for a polarizing plate protective film described later, it is preferably 20 to 200 ⁇ m, more preferably 25 to 100 ⁇ m, and 30 to 80 ⁇ m. It is particularly preferred.
- a polarizing plate When using the optical film of this invention as a protective film for polarizing plates, a polarizing plate can be produced by a general method. It is preferable that an adhesive layer is provided on the back side of the optical film of the present invention, and is bonded to at least one surface of a polarizer produced by immersion and stretching in an iodine solution.
- the optical film of the present invention may be used, or another polarizing plate protective film may be used.
- a commercially available cellulose ester film for example, Konica Minoltack KC8UX, KC4UX, KC5UX, KC8UY, KC4UY, KC12UR, KC8UCR-3, KC8UCR-4, KC8UCR-5, KC8UE, KC4FR-4, KC4FR-3, KC4FR-3, KC4FR-4 -1, KC8UY-HA, KC8UX-RHA, manufactured by Konica Minolta Opto Co., Ltd.) and the like are preferably used.
- a polarizer which is a main component of a polarizing plate, is an element that allows only light of a plane of polarization in a certain direction to pass.
- a typical polarizer currently known is a polyvinyl alcohol-based polarizing film, which is polyvinyl alcohol.
- iodine is dyed on a system film and one in which dichroic dye is dyed.
- the polarizer is formed by forming a polyvinyl alcohol aqueous solution into a film and dyeing the film by uniaxial stretching or dyeing or uniaxially stretching, and then performing a durability treatment with a boron compound.
- a pressure-sensitive adhesive having a storage elastic modulus at 25 ° C. in the range of 1.0 ⁇ 10 4 Pa to 1.0 ⁇ 10 9 Pa in at least a part of the pressure-sensitive adhesive layer is used. It is preferable to use a curable pressure-sensitive adhesive that forms a high molecular weight body or a crosslinked structure by various chemical reactions after the pressure-sensitive adhesive is applied and bonded.
- urethane adhesives examples include, for example, urethane adhesives, epoxy adhesives, aqueous polymer-isocyanate adhesives, curable adhesives such as thermosetting acrylic adhesives, moisture-curing urethane adhesives, polyether methacrylate types
- curable adhesives such as thermosetting acrylic adhesives, moisture-curing urethane adhesives, polyether methacrylate types
- anaerobic pressure-sensitive adhesives such as ester-based methacrylate type and oxidized polyether methacrylate, cyanoacrylate-based instantaneous pressure-sensitive adhesives, and acrylate-peroxide-based two-component instantaneous pressure-sensitive adhesives.
- the above-mentioned pressure-sensitive adhesive may be a one-component type or a type in which two or more components are mixed before use.
- the above-mentioned pressure-sensitive adhesive may be a solvent system using an organic solvent as a medium, or an aqueous system such as an emulsion type, a colloidal dispersion type, or an aqueous solution type that is a medium containing water as a main component. It may be a solvent type.
- concentration of the pressure-sensitive adhesive liquid may be appropriately determined depending on the film thickness after adhesion, the coating method, the coating conditions, and the like, and is usually 0.1 to 50% by mass.
- polarizing plate By incorporating the polarizing plate bonded with the optical film of the present invention into a liquid crystal display device, it is possible to produce various liquid crystal display devices with excellent visibility, but particularly outdoors such as large liquid crystal display devices and digital signage. It is preferably used for a liquid crystal display device for use.
- the polarizing plate according to the present invention is bonded to a liquid crystal cell via the adhesive layer or the like.
- the polarizing plate according to the present invention includes a reflective type, a transmissive type, a transflective type LCD or a TN type, an STN type, an OCB type, a HAN type, a VA type (PVA type, MVA type), an IPS type (including an FFS type), and the like. It is preferably used in various drive LCDs. In particular, in a large-screen display device having a screen of 30 or more, especially 30 to 54, there is no white spot at the periphery of the screen and the effect is maintained for a long time.
- Example 1 [Preparation of acrylic resin] The following acrylic resins A2-A7 and MS1,2 were prepared by known methods.
- the following commercially available acrylic resins were used.
- compositions were further dried while being mixed in a vacuum nauter mixer at 80 ° C. and 1 Torr for 3 hours.
- the dried composition was melt-mixed at 235 ° C. using a twin-screw extruder and pelletized.
- the above pellets are laminated with a T-die using each single-screw extruder, melted and extruded into a film at a melting temperature of 240 ° C. on a first cooling roll having a surface temperature of 90 ° C., and a total film thickness of 150 ⁇ m.
- a cast film of was obtained by extrusion.
- the film was pressed on the first cooling roll with an elastic touch roll having a 2 mm thick metal surface.
- this film was stretched 1.3 times in the conveying direction at 155 ° C. (Tg 125 ° C. of the composition) by a stretching machine using a difference in roll peripheral speed, and further, a preheating zone, a stretching zone, a holding zone, a cooling zone (each zone). Introduced in a tenter which is a stretching machine in the width direction having a neutral zone for ensuring heat insulation between the zones in between, after stretching 1.3 times at 155 ° C. in the width direction, 30 The film was cooled to 0 ° C., then released from the clip, and the clip holding part was cut off to obtain an optical film 1 having a width of 2500 mm and a film thickness of 80 ⁇ m.
- optical film 1 The production of the optical film 1 was the same except that the types of acrylic resin (A) and cellulose ester resin (B), molecular weight, composition ratio, presence / absence of plasticizer, stretching conditions, and film thickness were changed as shown in Table 1. Thus, optical films 2 to 30 of the present invention and comparative examples were obtained.
- Plasticizer 1 DOA (dioctyl adipate)
- the glass transition temperature was measured at a rate of temperature increase of 20 ° C./min using a differential scanning calorimeter (DSC-7 manufactured by Perkin Elmer). JIS K7121 (1987) The intermediate-point glass transition temperature (Tmg) (° C.) determined according to (Tension softening point) The following evaluation was performed using a Tensilon tester (ORIENTEC, RTC-1225A) in an atmosphere of 23 ° C. and 55% RH.
- DSC-7 differential scanning calorimeter
- the optical film was cut out at 120 mm (length) x 10 mm (width) and continuously heated at a heating rate of 30 ° C./min while pulling with a tension of 10 N, and the temperature (° C.) at the time when it reached 9 N was measured three times. And put out the average. (Folding resistance)
- the optical film is cut out at 120 mm (length) ⁇ 10 mm (width), conditioned for 4 hours in a room conditioned at a temperature of 23 ° C. and a relative humidity of 55% RH, and then cut by bending according to ISO877 6 / 2-1988. The number of round-trips was determined.
- a 120- ⁇ m-thick long roll polyvinyl alcohol film was immersed in 100 parts by mass of an aqueous solution containing 1 part by mass of iodine and 4 parts by mass of boric acid, and stretched in the transport direction 5 times at 50 ° C. to produce a polarizer.
- the optical film 1 produced in Example 1 was subjected to a corona treatment using an acrylic adhesive on one side of the polarizer, and then bonded.
- Konica Minolta Tack KC8UCR-5 manufactured by Konica Minolta Opto Co., Ltd.
- Konica Minolta Opto Co., Ltd. which is an alkali saponified retardation film
- polarizing plates P2 to P30 were produced using the optical films 2 to 30.
- Reworkability In an atmosphere of 23 ° C. and 55% RH, the produced polarizing plate is cut into a square with a size of 20 cm ⁇ 20 cm and bonded to a glass substrate using an acrylic adhesive. Next, the bonded polarizing plate is peeled off from the glass with a strength of 5N from the corner. This operation is performed with 100 polarizing plates for one type of sample, and the number of polarizing plates that are not peeled off completely is counted. Reworkability is ranked according to the following criteria.
- the rework property is ⁇ level or more, but it is preferably ⁇ level or more, ⁇ A level is particularly preferred.
- the optical film of the present invention is preferable in terms of reworkability, hardly leaks light, and is clearly improved over the comparison.
- Example 2 Preparation of acrylic particles (C1)> A reactor with a reflux condenser with an internal volume of 60 liters was charged with 38.2 liters of ion-exchanged water and 111.6 g of sodium dioctylsulfosuccinate, and the temperature was raised to 75 ° C. in a nitrogen atmosphere while stirring at 250 rpm. The effect of oxygen was virtually eliminated. 0.36 g of APS was added, and after stirring for 5 minutes, a monomer mixture consisting of 1657 g of MMA, 21.6 g of BA, and 1.68 g of ALMA was added all at once, and after the exothermic peak was detected, the mixture was held for another 20 minutes to polymerize the innermost hard layer. Completed.
- a small amount of the polymer latex thus obtained was collected, and the flat particle size was determined by the absorbance method, which was 0.10 ⁇ m.
- the remaining latex was put into a 3% by mass sodium sulfate warm aqueous solution, salted out and coagulated, and then dried after repeated dehydration and washing to obtain acrylic particles (C1) having a three-layer structure.
- the acrylic resin-containing film 2-3 was prepared in the same manner as 2-2 by adding the following ultraviolet absorber simultaneously with other resins.
- Tinuvin 109 (manufactured by Ciba Japan Co., Ltd.) 1.5 parts by mass Tinuvin 171 (manufactured by Ciba Japan Co., Ltd.) 0.7 parts by mass
- the solvent content of these optical films is 0.01% by mass. % Or less.
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Abstract
Description
本発明に用いられるアクリル樹脂には、メタクリル樹脂も含まれる。樹脂としては特に制限されるものではないが、メチルメタクリレート単位50~99質量%、およびこれと共重合可能な他の単量体単位1~50質量%からなるものが好ましい。
カラム: Shodex K806、K805、K803G(昭和電工(株)製を3本接続して使用した)
カラム温度:25℃
試料濃度: 0.1質量%
検出器: RI Model 504(GLサイエンス社製)
ポンプ: L6000(日立製作所(株)製)
流量: 1.0ml/min
校正曲線: 標準ポリスチレンSTK standard ポリスチレン(東ソー(株)製)Mw=2,800,000~500迄の13サンプルによる校正曲線を使用した。13サンプルは、ほぼ等間隔に用いることが好ましい。
本発明のセルロースエステル樹脂(B)は、特に脆性の改善やアクリル樹脂(A)と相溶させたときに透明性の観点から、アシル基の総置換度(T)が2.0~3.0、炭素数が3~7のアシル基の置換度が1.2~3.0であり、炭素数3~7のアシル基の置換度は、2.0~3.0であることが好ましい。即ち、本発明のセルロースエステル樹脂は炭素数が3~7のアシル基により置換されたセルロースエステル樹脂であり、具体的には、プロピオニル、ブチリル等が好ましく用いられるが、特にプロピオニル基が好ましく用いられる。
本発明の光学フィルムは、アクリル粒子を含有してもよい。
<その他の添加剤>
本発明の光学フィルムには、フィルムに加工性を付与する可塑剤、フィルムの劣化を防止する酸化防止剤、紫外線吸収機能を付与する紫外線吸収剤、フィルムに滑り性を付与する微粒子(マット剤)等の添加剤を含有させることが好ましい。
〈可塑剤〉
可塑剤としては、フタル酸エステル系、脂肪酸エステル系、トリメリット酸エステル系、リン酸エステル系、ポリエステル系、あるいはエポキシ系等が挙げられる。
〈酸化防止剤〉
本発明では、酸化防止剤としては、通常知られているものを使用することができる。
〈着色剤〉
本発明においては、着色剤を使用することが好ましい。着色剤と言うのは染料や顔料を意味するが、本発明では、液晶画面の色調を青色調にする効果またはイエローインデックスの調整、ヘイズの低減を有するものを指す。
〈紫外線吸収剤〉
本発明に用いられる紫外線吸収剤は特に限定されないが、例えばオキシベンゾフェノン系化合物、ベンゾトリアゾール系化合物、サリチル酸エステル系化合物、ベンゾフェノン系化合物、シアノアクリレート系化合物、トリアジン系化合物、ニッケル錯塩系化合物、無機粉体等が挙げられる。高分子型の紫外線吸収剤としてもよい。
〈マット剤〉
本発明では、フィルムの滑り性を付与するためにマット剤を添加することが好ましい。
〈粘度低下剤〉
本発明において、溶融粘度を低減する目的として、水素結合性溶媒を添加することができる。水素結合性溶媒とは、J.N.イスラエルアチビリ著、「分子間力と表面力」(近藤保、大島広行訳、マグロウヒル出版、1991年)に記載されるように、電気的に陰性な原子(酸素、窒素、フッ素、塩素)と電気的に陰性な原子と共有結合した水素原子間に生ずる、水素原子媒介「結合」を生ずることができるような有機溶媒、すなわち、結合モーメントが大きく、かつ水素を含む結合、例えば、O-H(酸素水素結合)、N-H(窒素水素結合)、F-H(フッ素水素結合)を含むことで近接した分子同士が配列できるような有機溶媒をいう。
a1:熱処理前の距離
a2:熱処理後の距離
液晶表示装置の偏光板用保護フィルムとして光学フィルムが用いられる場合は、吸湿による寸法変化により光学フィルムにムラや位相差値の変化が発生してしまい、コントラストの低下や色むらといった問題を発生させる。特に屋外で使用される液晶表示装置に用いられる偏光板保護フィルムであれば、上記の問題は顕著となる。しかし、上記の条件における寸法変化率(%)が0.5%未満であれば、十分な低吸湿性を示す光学フィルムであると評価できる。さらに、0.3%未満であることが好ましい。
<溶融流延製膜方法による光学フィルムの製造方法>
本発明の光学フィルムの製造方法は、アクリル樹脂(A)とセルロースエステル樹脂(B)を95:5から30:70の質量比で含有したものを溶融してダイから押出して、冷却ロール上に流延する光学フィルムの製造方法である。
溶融押出に用いるアクリル樹脂(A)、セルロースエステル樹脂(B)、その他の添加剤からなる光学フィルムを構成する組成物は、通常あらかじめ混錬してペレット化しておくことが好ましい。
まず、作製したペレットを1軸や2軸タイプの押出機を用いて、押し出す際の溶融温度Tmを200~300℃程度とし、リーフディスクタイプのフィルターなどでろ過し異物を除去した後、Tダイからフィルム状に共押出し、冷却ロール上で固化し、弾性タッチロールと押圧しながら流延する。
本発明では、上記のようにして得られたフィルムは冷却ロールに接する工程を通過後、さらに少なくとも1方向に1.01~3.0倍延伸することが好ましい。延伸により本発明の脆性を実現することができる。
<含有溶媒量>
本発明の光学フィルムは、溶融流延製膜方法によって作製することから、ロール状フィルムとして巻き取った時点で、含有している溶媒量が0.01質量%以下である。含有溶媒量は、下記の方法によって測定することができる。
機器:HP社 5890SERIES II
カラム:J&W社 DB-WAX(内径0.32mm、長さ30m)
検出:FID
GC昇温条件:40℃で5分間保持したあと、80℃/分で100℃まで昇温
ヘッドスペース加熱条件:120℃で20min
<清掃設備>
本発明の製造装置には、ベルトおよびロールを自動的に清掃する装置を付加させることが好ましい。清掃装置については特に限定はないが、例えば、ブラシ・ロール、吸水ロール、粘着ロール、ふき取りロール等をニップする方式、清浄エアーを吹き掛けるエアーブロー方式、レーザーによる焼却装置、あるいはこれらの組み合わせなどがある。
本発明の光学フィルムを偏光板用保護フィルムとして用いる場合、偏光板は一般的な方法で作製することが出来る。本発明の光学フィルムの裏面側に粘着層を設け、沃素溶液中に浸漬延伸して作製した偏光子の少なくとも一方の面に、貼り合わせることが好ましい。
本発明の光学フィルムを貼合した偏光板を液晶表示装置に組み込むことによって、種々の視認性に優れた液晶表示装置を作製することが出来るが、特に大型の液晶表示装置やデジタルサイネージ等の屋外用途の液晶表示装置に好ましく用いられる。本発明に係る偏光板は、前記粘着層等を介して液晶セルに貼合する。
〔アクリル樹脂の調製〕
以下のアクリル樹脂A2-A7、およびMS1、2を公知の方法によって調製した。
A3:モノマー質量比(MMA:MA=97:3)、Mw140000
A4:モノマー質量比(MMA:MA=97:3)、Mw200000
A5:モノマー質量比(MMA:MA=97:3)、Mw500000
A6:モノマー質量比(MMA:MA=97:3)、Mw550000
A7:モノマー質量比(MMA:MA=94:6)、Mw1000000
MMA:メチルメタクリレート
MA:メチルアクリレート
その他、以下の市販のアクリル樹脂を用いた。
A2を70質量部、セルロースエステルとしてセルロースアセテートプロピオネート(アセチル基の置換度0.19、プロピオニル基の置換度2.56、総アシル基置換度2.75、Mw=200000)30質量部、Tinuvin928(チバ・ジャパン(株)製)1.5質量部、ADK STAB PEP-36(旭電化工業(株)製)0.01質量部、Irganox1010(チバ・ジャパン(株)製)0.5質量部、SumilizerGS(住友化学(株)製)0.2質量部の割合で配合して、光学フィルム1を構成する組成物1を形成した。
《評価方法》
(ガラス転移温度)
延伸前の光学フィルムのTgは、作製した光学フィルムとほぼ同じなので、光学フィルムのTgを測定することにより、延伸前の光学フィルムのTgに代替した。
(張力軟化点)
23℃、55%RHの雰囲気下、テンシロン試験機(ORIENTEC社製、RTC-1225A)を用いて、以下のような評価を行った。
(耐折度)
光学フィルムを120mm(縦)×10mm(幅)で切り出し、温度23℃、相対湿度55%RHに調湿された部屋で4時間調湿した後、ISO877 6/2-1988に従い、折り曲げによって切断するまでの往復回数を求めた。
〈偏光板の作製〉
各光学フィルムを偏光板保護フィルムとした偏光板を、以下のようにして作製した。
(リワーク性)
23℃、55%RHの雰囲気下、作製した偏光板を20cm×20cmの大きさの正方形に断裁し、アクリル系接着剤を用いてガラス基板と貼り合わせる。次いで、貼り合わせた偏光板を角の部分から5Nの強さでガラスから剥がす。この作業を1種類のサンプルについて100枚の偏光板で行い、偏光板に裂け目が入って、完全に剥離されなかった偏光板の枚数を数える。リワーク性は以下の基準でランク付けする。
○△:6~10枚
△ :11~15枚
× :16枚以上
リワーク性は△レベル以上であれば実用上問題ないが、○△レベル以上であることが好ましく、○レベルであることが特に好ましい。
上記作製した各偏光板を使用して、光学フィルムの表示特性評価を行った。
黒表示時の光漏れを目視で下記基準により評価した。
×:強い光漏れが1~2箇所ある
〈アクリル粒子(C1)の調製〉
内容積60リットルの還流冷却器付反応器に、イオン交換水38.2リットル、ジオクチルスルホコハク酸ナトリウム111.6gを投入し、250rpmの回転数で攪拌しながら、窒素雰囲気下75℃に昇温し、酸素の影響が事実上無い状態にした。APS0.36gを投入し、5分間攪拌後にMMA1657g、BA21.6g、およびALMA1.68gからなる単量体混合物を一括添加し、発熱ピークの検出後さらに20分間保持して最内硬質層の重合を完結させた。
MA;メチルアクリレート
BA;n-ブチルアクリレート
ALMA;アリルメタクリレート
PEGDA;ポリエチレングリコールジアクリレート(分子量200)
n-OM;n-オクチルメルカプタン
APS;過硫酸アンモニウム
以下、アクリル樹脂(A)、セルロースエステル樹脂(B)、アクリル粒子(C)、組成比を表4の記載のように変えた以外は、実施例1に記載の光学フィルム2の製造方法と同様にして、光学フィルム2-1と2-2を、光学フィルム1の製造方法と同様にして、光学フィルム1-1~1-6を作製した。
チヌビン171(チバ・ジャパン(株)製) 0.7質量部
なお、これらの光学フィルムの含有溶媒量は、いずれも0.01質量%以下であった。
2 フィルター
3 スタチックミキサー
4 流延ダイ
5 回転支持体(第1冷却ロール)
6 挟圧回転体(タッチロール)
7 回転支持体(第2冷却ロール)
8 回転支持体(第3冷却ロール)
9、10、11、13、14 搬送ロール
12 延伸機
15 スリッター
16 巻き取り機
F 本発明の光学フィルム
Claims (4)
- アクリル樹脂(A)とセルロースエステル樹脂(B)を95:5から30:70の質量比で、前記アクリル樹脂(A)の重量平均分子量Mwが110000以上1000000以下であり、該セルロースエステル樹脂(B)のアシル基総置換度(T)が2.0以上3.0以下、炭素数が3以上、7以下のアシル基の置換度が1.2以上3.0以下であり、該セルロースエステル樹脂(B)の重量平均分子量Mwが75000以上300000以下であり、張力軟化点が105~145℃、耐折度が50~100回で、溶融流延製膜方法によって製造されたことを特徴とする光学フィルム。
- 請求項1に記載の光学フィルムが、搬送方向または幅手方向の少なくともいずれかの方向に延伸して製造されるものであり、その延伸温度が延伸前の光学フィルムのTg~Tg+50℃であることを特徴とする光学フィルムの製造方法。
- 請求項1に記載の光学フィルムを有することを特徴とする偏光板。
- 請求項3に記載の偏光板を有することを特徴とする液晶表示装置。
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JP2010532853A JP5397382B2 (ja) | 2008-10-06 | 2009-08-10 | 光学フィルム、光学フィルムの製造方法、偏光板および液晶表示装置 |
CN2009801388295A CN102171020B (zh) | 2008-10-06 | 2009-08-10 | 光学膜、光学膜的制造方法、偏振片以及液晶显示装置 |
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KR (1) | KR20110086797A (ja) |
CN (1) | CN102171020B (ja) |
TW (1) | TW201030080A (ja) |
WO (1) | WO2010041513A1 (ja) |
Cited By (3)
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JP2010275434A (ja) * | 2009-05-29 | 2010-12-09 | Nippon Shokubai Co Ltd | 光学フィルムの製造方法 |
JP2013029553A (ja) * | 2011-07-26 | 2013-02-07 | Fujifilm Corp | 光学フィルム及びその製造方法、積層光学フィルム、偏光板、並びに液晶表示装置 |
EP3923044A4 (en) * | 2019-02-28 | 2022-11-09 | Nitto Denko Corporation | OPTICAL LAYERED BODY |
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JP6075424B2 (ja) * | 2014-09-30 | 2017-02-08 | 住友化学株式会社 | 偏光板、液晶表示装置及び有機エレクトロルミネッセンス表示装置 |
KR102502463B1 (ko) * | 2015-06-19 | 2023-02-21 | 스미또모 가가꾸 가부시키가이샤 | 프로텍트 필름을 갖는 편광판의 제조 방법 |
CN109540895B (zh) * | 2018-12-27 | 2021-03-23 | 朱锦铃 | 一种燃气表膜质量检测装置 |
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Also Published As
Publication number | Publication date |
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KR20110086797A (ko) | 2011-08-01 |
TW201030080A (en) | 2010-08-16 |
CN102171020B (zh) | 2013-09-11 |
CN102171020A (zh) | 2011-08-31 |
JPWO2010041513A1 (ja) | 2012-03-08 |
JP5397382B2 (ja) | 2014-01-22 |
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