JP3480920B2 - Method for producing polyvinyl alcohol film - Google Patents

Description

Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention is useful as a material for manufacturing a polarizing film, and is a polyvinyl alcohol which can be stretched at a high magnification so that a polarizing film having excellent polarizing performance can be obtained. The present invention relates to a method for producing a film. 2. Description of the Related Art A polarizing plate having a function of transmitting and blocking light is a fundamental component of a liquid crystal display (LCD) together with a liquid crystal having a function of switching light. The range of application of this LCD is wide ranging from small devices such as calculators and wristwatches in the early days to laptop PCs, word processors, liquid crystal color projectors, in-car navigation systems, and liquid crystal televisions in recent years. Therefore, there is a demand for a polarizing plate having better polarization performance than conventional products. [0003] The polarizing plate is generally a polyvinyl alcohol film (hereinafter abbreviated as "PVA film", and the polyvinyl alcohol as a raw material thereof is referred to as a polyvinyl alcohol polymer, which is abbreviated as "PVA". Is sometimes uniaxially stretched and dyed, and cellulose triacetate (TA
C) A configuration in which a protective film such as a film is bonded. [0004] In order to improve the polarizing performance of a polarizing plate, processing conditions such as a formulation of a chemical solution and a stretching method in a processing step of a polarizing film, such as a degree of polymerization and a degree of saponification of PVA, are important. However, the stretchability of the PVA film used as the material of the polarizing film is most important. When the stretchability of the PVA film is low, it is difficult to improve the polarization performance. Accordingly, an object of the present invention is to provide a method for producing a polyvinyl alcohol film which is useful as a material for producing a polarizing film and which can be stretched at a high magnification so that a polarizing film having excellent polarization performance can be obtained. [0006] To achieve the above object, according to an aspect of the present onset Ming, using drum casting machine, the average degree of polymerization of 2
More than 000 polyvinyl alcohol and polyvinyl alcohol
0.01 to 1 part by weight per 100 parts by weight of alcohol
For polarizing film producing Po <br/> polyvinyl alcohol film for a polarization film from the film raw material containing surfactant
A method for producing a polyvinyl alcohol film, the uppermost
The polyvinyl alcohol for polarizing film is placed on the drum
A film of rucol film is formed at a temperature of 50C to 150C.
And when the volatile content reaches 10 to 50% by weight
In is peeled from the drum, the speed ratio between the winding device and the drum for winding a polyvinyl alcohol film for a polarizing film (peripheral speed of the winding speed / drum), 0.8
1.3 . An embodiment of the present invention will be described below with reference to the drawings. FIG. 1 shows an example of the production of a PVA film, in which a film-forming raw material (which may contain an organic solvent or the like) containing PVA in a solution or molten state is uniformly discharged onto a heated drum. 1 shows a drum type film forming machine that forms a film. This film forming machine uses a T-shaped slit die 1
Is discharged onto the surface of the first drum 3 for dry film formation which is positioned at the most upstream side and rotates, and is brought into contact with its circumferential surface to dry one surface of the PVA film 4. . Subsequently, the other surface of the PVA film 4 is dried by passing over the circumferential surface of the second drum 5, and further dried by passing through a plurality of drums 6 on the downstream side. The PVA film 4 is wound around a winding device 8. This drum film forming machine is provided with a drying device, a humidity control device, and the like. The speed of each drive is adjusted using a motor, a transmission, or the like. Drying temperature is 50
℃ and ~150 ℃. When the PVA film 4 is manufactured by the above-described drum film forming machine, the speed ratio between the winding device 8 and the first drum 3 (winding speed / peripheral speed of the first drum) is:
0.8 to 1.3, and 0.9 to 1.
3, preferably 0.9 to 1.2, and more preferably 0.9 to 1.1. When the speed ratio is smaller, the stretching ratio can be increased when the polarizing film is produced. However, when the speed ratio is smaller than 0.8, the PVA film 4 is moved from the first drum 3 to the winding device 8 at the time of dry film formation. Sagging wrinkles,
It is wound around each drum and cut. On the other hand, if the speed ratio exceeds 1.3, the desired draw ratio of 4 or more cannot be obtained when producing a polarizing film. When the PVA film 4 shifts from the first drum 3 to the second drum 5, the PVA film 4
Film 4 when peeling off the first drum 3
Has a volatile content of 10 to 50% by weight.
% Is more preferred. When the volatile content is less than 10% by weight, the PVA film may be whitened,
If the amount is more than the weight percentage, wrinkles may occur during film formation.
Processing a PVA film having wrinkles or whitening into a polarizing film is not preferable because it may cause staining spots. The PVA film has a thickness of 20 to 150.
μm is preferable, and 40 to 120 μm is more preferable. As the polyvinyl alcohol-based polymer (PVA) constituting the PVA film of the present invention, a vinyl ester-based polymer obtained by polymerization of a vinyl ester-based monomer is saponified to convert the vinyl ester unit into a vinyl alcohol unit. Can be used. Examples of the vinyl ester monomer include vinyl formate, vinyl acetate, vinyl propionate, vinyl valerate, vinyl laurate, vinyl stearate, vinyl benzoate, vinyl pivalate, vinyl versatate, and the like. Of these, vinyl acetate is preferably used. When copolymerizing a vinyl ester-based monomer, if necessary, a copolymerizable monomer may be used within a range that does not impair the purpose of the present invention (preferably 15 mol% or less, more preferably 5 mol% or less. ). Examples of such a monomer copolymerizable with the vinyl ester monomer include olefins having 3 to 30 carbon atoms such as ethylene, propylene, 1-butene and isobutene; acrylic acid and its salts; methyl acrylate , Ethyl acrylate, n-propyl acrylate, i-propyl acrylate, n-butyl acrylate, i-butyl acrylate, t-butyl acrylate, acrylic acid 2
Acrylates such as ethylhexyl, dodecyl acrylate and octadecyl acrylate; methacrylic acid and salts thereof; methyl methacrylate, ethyl methacrylate;
Methacrylates such as n-propyl methacrylate, i-propyl methacrylate, n-butyl methacrylate, i-butyl methacrylate, t-butyl methacrylate, 2-ethylhexyl methacrylate, dodecyl methacrylate, octadecyl methacrylate And acrylamide,
Acrylamide derivatives such as N-methylacrylamide, N-ethylacrylamide, N, N-dimethylacrylamide, diacetone acrylamide, acrylamidopropanesulfonic acid and its salts, acrylamidopropyldimethylamine and its salts, N-methylolacrylamide and its derivatives; methacryl Amide, N-
Methacrylamide derivatives such as methyl methacrylamide, N-ethyl methacrylamide, methacrylamidopropanesulfonic acid and salts thereof, methacrylamidopropyldimethylamine and salts thereof, N-methylol methacrylamide and derivatives thereof; N-vinylformamide, N-vinyl N-vinylamides such as acetamide and N-vinylpyrrolidone; methyl vinyl ether, ethyl vinyl ether, n-propyl vinyl ether, i-propyl vinyl ether, n-butyl vinyl ether, i
-Butyl vinyl ether, t-butyl vinyl ether,
Vinyl ethers such as dodecyl vinyl ether and stearyl vinyl ether; nitriles such as acrylonitrile and methacrylonitrile; vinyl chloride, vinylidene chloride;
Vinyl halides such as vinyl fluoride and vinylidene fluoride; allyl compounds such as allyl acetate and allyl chloride; maleic acid and its salts or esters; itaconic acid and its salts or esters; vinylsilyl compounds such as vinyltrimethoxysilane Isopropenyl acetate, N-
Examples include N-vinylamides such as vinylformamide, N-vinylacetamide, and N-vinylpyrrolidone. The average degree of polymerization of the PVA constituting the PVA film is determined in terms of film strength and polarization performance.
To 2000 or more, and most preferably 3500 or more. On the other hand, the upper limit of the degree of polymerization of PVA is preferably 10,000 or less from the viewpoint of film forming properties. The degree of polymerization (P) of the PVA is JIS K
It is measured according to 6726. That is, after PVA is re-saponified and purified, the intrinsic viscosity [η] (unit: dL / g, L is liter) measured in water at 30 ° C. is determined by the following equation. P = ([η] × 10 ³ /8.29) ^{(1 / 0.62) The} degree of saponification of PVA constituting the PVA film is 90 mol% from the viewpoint of the durability of the polarizing film.
Or more, more preferably 95 mol% or more, and 98% or more.
Mole% or more is more preferable. On the other hand, from the viewpoint of the dyeability of the PVA film, 99.99 mol% or less is preferable. The degree of saponification indicates the ratio of units actually saponified to vinyl alcohol units among units that can be converted into vinyl alcohol units by saponification. In addition, the saponification degree of PVA was measured by the method described in JIS. When producing the PVA film, it is preferable to add a polyhydric alcohol as a plasticizer.
Examples of the polyhydric alcohol include ethylene glycol, glycerin, propylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, trimethylolpropane, and the like, and one or more of these can be used. Among them, ethylene glycol or glycerin is preferably used from the viewpoint of the effect of improving the stretchability. The amount of the polyhydric alcohol added is PVA
1 to 30 parts by weight, preferably 3 to 30 parts by weight, per 100 parts by weight
It is more preferably 25 parts by weight, particularly preferably 5 to 20 parts by weight. If the amount is less than 1 part by weight, the dyeing properties and the stretchability may decrease. If the amount is more than 30 parts by weight, the film may be too flexible and the handleability may decrease. [0019] In producing the PVA film, it adds a surfactant. The type of the surfactant is not particularly limited, but an anionic or nonionic surfactant is preferable. As the anionic surfactant,
For example, a carboxylic acid type such as potassium laurate, a sulfate type such as octyl sulfate, and a sulfonic acid type anionic surfactant such as dodecylbenzenesulfonate are preferable. As the nonionic surfactant,
For example, alkyl ether type such as polyoxyethylene oleyl ether, alkyl phenyl ether type such as polyoxyethylene octyl phenyl ether, alkyl ester type such as polyoxyethylene laurate, alkyl amine type such as polyoxyethylene lauryl amino ether, poly Nonionics such as alkyl amides such as oxyethylene lauric amide, polypropylene glycol ethers such as polyoxyethylene polyoxypropylene ether, alkanolamides such as oleic acid diethanolamide, and allyl phenyl ethers such as polyoxyalkylene allyl phenyl ether Nonionic surfactants are preferred. One or a combination of two or more of these surfactants can be used. The amount of the surfactant added is PVA1
0.01 to 1 part by weight with respect to 00 parts by weight.
02-0.5 part by weight is more preferable, and 0.05-0.5 part by weight.
3 parts by weight are particularly preferred. If the amount is less than 0.01 part by weight, the effect of improving the stretchability and the dyeing property is difficult to appear, and if it is more than 1 part by weight, it is eluted on the film surface to cause blocking, and the handleability may be reduced. The volatile matter content of the PVA-containing film-forming raw material used in producing the PVA film is 50 to 90.
% By weight, more preferably 55 to 80% by weight.
If the volatile content is less than 50%, the viscosity becomes high, so that film formation may be difficult. On the other hand, when the volatile content is more than 90%, the viscosity becomes too low, and the uniformity of the thickness of the PVA film tends to be impaired. When manufacturing the PVA film,
In addition to the above-described T-shaped slit die, for example, a hopper plate, an I-die, a lip coater die, or the like is used, and a film forming material is supplied to the peripheral surface of the first drum located at the most upstream side, and is volatilized on this drum. Alternatively, the film may be evaporated to form a film, sent to a subsequent process, and further dried and conditioned to adjust the film to an appropriate film and wound around a winding device. In the present invention, in addition to the melt extrusion method, for example, P
A cast film forming method using a film forming raw material solution containing VA can also be adopted. In order to produce a polarizing film from the PVA film of the present invention, for example, the PVA film may be dyed, uniaxially stretched, fixed, dried, and, if necessary, heat-treated. The order of each step is not particularly limited, and two steps such as dyeing and uniaxial stretching may be performed simultaneously. Further, each step may be repeated a plurality of times. The dyeing is performed before the uniaxial stretching, simultaneously with the uniaxial stretching,
Although any method can be used after uniaxial stretching, PVA is preferably dyed in any step prior to uniaxial stretching or during the uniaxial stretching step because the degree of crystallinity tends to increase due to uniaxial stretching and the dyeability may decrease. . The dye used for dyeing is iodine-potassium iodide or Direct black 17, 19, 154;
brown 44, 106, 195, 210, 223; Direct red 2, 2
3, 28, 31, 37, 39, 79, 81, 240, 242, 247; Direc
t blue 1, 15, 22, 78, 90, 98, 151, 168, 202, 2
36, 249, 270; Direct violet 9, 12, 51, 98; Dir
ect green 1, 85; Direct yellow 8, 12, 44, 86, 8
7; Dichroic dyes such as Direct orange 26, 39, 106 and 107 can be used. Dyeing can be usually performed by immersing the PVA film in a solution containing the dye, but the processing conditions and processing method are not particularly limited. The uniaxial stretching performed in the length direction of the PVA film can be performed by a wet stretching method or a dry heat stretching method, and can be performed in warm water (which may be in a solution containing the dye or in a fixing bath described below) or after absorbing water. It may be performed in air using a PVA film. Stretching is preferably carried out as far as possible to a point shortly before the PVA film is cut, specifically, preferably 4 times or more, particularly preferably 5 times or more. When the stretching ratio is smaller than 4 times, it is difficult to obtain practically sufficient polarization performance and durability performance. The stretching temperature is not particularly limited, but is 30 to 90 ° C. when the PVA film is stretched in warm water (wet stretching), and 50 to 1 ° C. when the dry heat stretching is performed.
80 ° C. is preferred. The thickness of the stretched PVA film is preferably from 3 to 75 μm, more preferably from 10 to 50 μm. For the purpose of strengthening the adsorption of the dye to the PVA film, a fixing treatment is performed. Usually, boric acid and a boron compound are added to the treatment bath used for the fixing treatment. Further, an iodine compound may be added to the treatment bath as needed. The drying treatment (heat treatment) of the PVA film is 3
It is preferably performed at 0 to 150 ° C, more preferably at 50 to 150 ° C. The polarizing film obtained as described above is usually used as a polarizing plate by laminating an optically transparent protective film having mechanical strength on both sides or one side thereof. As the protective film, a cellulose acetate film, an acrylic film, a polyester film or the like is usually used. EXAMPLES Hereinafter, the present invention will be described specifically with reference to Examples, but the present invention is not limited thereto. The polarizing films described in the examples and comparative examples were manufactured by the following methods, and the dichroic ratio and the volatile content (moisture) were measured by the following methods. Preparation method of polarizing film: pre-swelling, dyeing, washing, uniaxial stretching, fixing, drying,
The films were processed in the order of heat treatment to produce a polarizing film. That is, the PVA film was immersed in water at 30 ° C. for 1 minute to pre-swell, and the weight ratio of iodine / potassium iodide was reduced to 1/10.
And immersed in a 4% by weight aqueous solution of boric acid at 30 ° C. for 4 minutes appropriately selected at an iodine concentration of 30 to 50 g / L so that the transmittance of the polarizing film is 43 to 44%,
It is immersed in water at 30 ° C. for 0.5 minutes for washing, and the stretch ratio of the PVA film is increased as much as possible in an aqueous solution of 4% by weight of boric acid at 50 ° C. (until slightly before the PVA film is cut). Uniaxial stretching was performed. Subsequently, a fixation treatment was performed by immersing in a 40 g / L aqueous solution of 40 g / L of potassium iodide and 40 g / L of boric acid for 5 minutes. Thereafter, the PVA film was taken out and dried with hot air at 40 ° C. under a constant length.
Heat treatment was performed at 00 ° C. for 3 minutes. Dichroic ratio: The dichroic ratio was used as an index for evaluating the polarizing performance of the obtained polarizing film. This dichroic ratio is based on the standards of the Electronic Machinery Manufacturers Association of Japan (EIAJ) LD-2.
The transmittance Ts obtained by measuring and calculating in a C light source and a 2 degree field of view using a spectrophotometer in accordance with 01-1983.
(%) And the degree of polarization P (%) were determined from the following equation. Dichroic ratio = log (TS / 100−TS / 100 × P /
100) / log (TS / 100 + TS / 100 × P /
100) Measurement of volatile content (moisture content): The volatile content (moisture content) of the PVA film was measured using a fiber type infrared moisture meter (IM-3SCV MODEL-1900 (L), manufactured by Fuji Work Co., Ltd.). . Example 1 PVA 10 having a degree of saponification of 99.9 mol% and a degree of polymerization of 2400
0 parts by weight, glycerin 10 parts by weight, lauric acid diethanolamide 0.1 part by weight, and a volatile matter content of water of 70
Wt% of a film-forming material was discharged onto a chrome-plated metal first drum at 95 ° C.
It was dried with hot air at 5 ° C. to obtain a PVA film having an average thickness of 75 μm. At this time, the speed ratio between the winding speed of the PVA film and the peripheral speed of the first drum was 0.9, and the volatile content (water content) of the PVA film when peeled from the first drum was 22% by weight. Met. When this PVA film was processed into a polarizing film, the stretching ratio was 5.8 times, and the obtained polarizing film had a thickness of 26 μm and a transmittance of 43.5.
%, The degree of polarization was 99.5%, the dichroic ratio was 43.3, and no staining spots were observed. Example 2 PVA 10 having a saponification degree of 99.9 mol% and a polymerization degree of 2400
0 parts by weight, 10 parts by weight of glycerin, 0.1 part by weight of lauric acid diethanolamide, and a volatile content of 74 consisting of water
% By weight of a film-forming material was discharged onto a chrome-plated metal first drum at 85 ° C.
It was dried with hot air at 0 ° C. to obtain a PVA film having an average thickness of 75 μm. At this time, the speed ratio between the winding speed of the PVA film and the peripheral speed of the first drum was 1.1, and the volatile content (water content) of the PVA film when peeled from the first drum was 41% by weight. Met. When this PVA film was processed into a polarizing film, the stretching ratio was 5.6 times, and the obtained polarizing film had a thickness of 27 μm and a transmittance of 43.3.
%, The degree of polarization was 99.5%, and the dichroic ratio was 41.9, and no staining spots were observed. Comparative Example A PVA 10 having a saponification degree of 99.9 mol% and a polymerization degree of 2400
0 parts by weight, glycerin 10 parts by weight, lauric acid diethanolamide 0.1 part by weight, and a volatile content of 76
% By weight of a film-forming material was discharged onto a chrome-plated metal first drum at 75 ° C.
It was dried with hot air at 0 ° C. to obtain a PVA film having an average thickness of 76 μm. At this time, the speed ratio between the winding speed of the PVA film and the peripheral speed of the first drum was 1.1, and the volatile content (water content) of the PVA film when peeled from the first drum was 55% by weight. Met. In this case, several wrinkles occurred on the PVA film during the film formation. When this PVA film was processed into a polarizing film, the stretching ratio was 5.4 times, and the obtained polarizing film had a thickness of 28 μm and a transmittance of 43.5.
%, The degree of polarization was 99.3%, and the dichroic ratio was 40.6. In this case, staining spots were partially generated due to wrinkles of the PVA film. Comparative Example B PVA10 having a saponification degree of 99.9 mol% and a polymerization degree of 2400
0 parts by weight, 10 parts by weight of glycerin, 0.1 part by weight of lauric acid diethanolamide, and a volatile content of 74 consisting of water
% By weight of a film-forming material was discharged onto a chrome-plated metal first drum at 85 ° C.
It was dried with hot air at 0 ° C. to obtain a PVA film having an average thickness of 74 μm. At this time, the speed ratio between the winding speed of the PVA film and the peripheral speed of the first drum was 1.2, and the volatile content (water content) of the PVA film when peeled from the first drum was 8% by weight. Met. In this case, the PVA film was partially whitened during film formation. When this PVA film was processed into a polarizing film, the stretching ratio was 5.3 times, and the obtained polarizing film had a thickness of 28 μm and a transmittance of 43.7.
%, The degree of polarization was 99.2%, and the dichroic ratio was 40.8. In this case, staining spots occurred partially due to whitening of the PVA film. Example 5 PVA10 having a degree of saponification of 99.9 mol% and a degree of polymerization of 4000
0 parts by weight, glycerin 10 parts by weight, lauric acid diethanolamide 0.1 part by weight, and a volatile content of 80
Wt% of a film-forming material was discharged onto a chrome-plated metal first drum at 95 ° C.
It was dried with hot air of 00 ° C. to obtain a PVA film having an average thickness of 75 μm. At this time, the speed ratio between the winding speed of the PVA film and the peripheral speed of the first drum is 1.1.
The volatile content (water content) of the PVA film when peeled from the drum was 25% by weight. When this PVA film was processed into a polarizing film, the stretching ratio was 5.3 times, and the obtained polarizing film had a thickness of 28 μm and a transmittance of 43.8.
%, The degree of polarization was 99.4%, the dichroic ratio was 43.9, and no staining spots were observed. Comparative Example C PVA 10 having a saponification degree of 99.9 mol% and a polymerization degree of 1700
0 parts by weight, 10 parts by weight of glycerin, 0.1 part by weight of lauric acid diethanolamide, and a volatile content of 65 consisting of water.
% By weight of a film-forming material was discharged onto a first chrome-plated metal drum at 80 ° C.
It was dried with hot air at 5 ° C. to obtain a PVA film having an average thickness of 75 μm. At this time, the speed ratio between the winding speed of the PVA film and the peripheral speed of the first drum was 1.1, and the volatile content (water content) of the PVA film when peeled from the first drum was 40% by weight. Met. When this PVA film was processed into a polarizing film, the stretching ratio was 5.8 times, and the obtained polarizing film had a thickness of 25 μm and a transmittance of 43.0.
%, The degree of polarization was 99.4%, the dichroic ratio was 38.7, and no staining spots were observed. Comparative Example 1 PVA 10 having a saponification degree of 99.9 mol% and a polymerization degree of 2400
0 parts by weight, glycerin 10 parts by weight, lauric acid diethanolamide 0.1 part by weight, and a volatile matter content of water of 70
Wt% of a film-forming material was discharged onto a chrome-plated metal first drum at 95 ° C.
It was dried with hot air at 5 ° C. to obtain a PVA film having an average thickness of 75 μm. At this time, the speed ratio between the winding speed of the PVA film and the peripheral speed of the first drum was 0.7, and the volatile content (water content) of the PVA film when peeled from the first drum was 20% by weight. Met. In this case, wrinkles occurred on the entire surface of the PVA film during film formation. When this PVA film was processed into a polarizing film, the stretching ratio was 5.6 times, and the obtained polarizing film had a thickness of 26 μm and a transmittance of 43.6.
%, The degree of polarization was 99.3%, and the dichroic ratio was 41.2, but due to wrinkles on the entire surface of the PVA film, staining spots were generated and the film was unsuitable as a polarizing film. Comparative Example 2 PVA10 having a saponification degree of 99.9 mol% and a polymerization degree of 2400
0 parts by weight, 10 parts by weight of glycerin, 0.1 part by weight of lauric acid diethanolamide and a volatile matter content of 73
% By weight of a film-forming material was discharged onto a chrome-plated metal first drum at 85 ° C.
It was dried with hot air at 0 ° C. to obtain a PVA film having an average thickness of 75 μm. At this time, the speed ratio between the winding speed of the PVA film and the peripheral speed of the first drum was 1.5, and the volatile content (water content) of the PVA film when peeled from the first drum was 42% by weight. Met. When this PVA film was processed into a polarizing film, the stretching ratio was 4.4 times, and the obtained polarizing film had a thickness of 29 μm and a transmittance of 43.3.
%, The degree of polarization was 98.3%, the dichroic ratio was 32.2, and no staining spots were observed. Comparative Example 3 PVA10 having a saponification degree of 99.9 mol% and a polymerization degree of 2400
0 parts by weight, 10 parts by weight of glycerin, 0.1 part by weight of lauric acid diethanolamide and a volatile matter content of 73
% By weight of a film-forming material was discharged onto a chrome-plated metal first drum at 75 ° C.
It was dried with hot air at 5 ° C. to obtain a PVA film having an average thickness of 75 μm. At this time, the speed ratio between the winding speed of the PVA film and the peripheral speed of the first drum was 1.5, and the volatile content (water content) of the PVA film when peeled from the first drum was 56% by weight. Met. In this case, several wrinkles occurred on the PVA film during the film formation. When this PVA film was processed into a polarizing film, the stretching ratio was 4.8 times, and the obtained polarizing film had a thickness of 28 μm and a transmittance of 43.0.
%, The degree of polarization was 98.9%, and the dichroic ratio was 34.3. However, due to wrinkles of the PVA film, spots were partially generated, which was not preferable as a polarizing film. Comparative Example 4 PVA 10 having a saponification degree of 99.9 mol% and a polymerization degree of 2400
0 parts by weight, 10 parts by weight of glycerin, 0.1 part by weight of lauric acid diethanolamide, and a volatile content of 75 consisting of water
% By weight of a film-forming material was discharged onto a chrome-plated metal first drum at 85 ° C.
It was dried with hot air at 20 ° C. to obtain a PVA film having an average thickness of 75 μm. At this time, the speed ratio between the winding speed of the PVA film and the peripheral speed of the first drum is 1.5.
The volatile content (water content) of the PVA film that had been peeled off from the drum was 9% by weight. In this case, during film formation, P
The VA film was partially whitened. When this PVA film was processed into a polarizing film, the stretching ratio was 3.8 times, and the obtained polarizing film had a thickness of 28 μm and a transmittance of 43.1.
%, The degree of polarization was 97.6%, and the dichroic ratio was 28.5. However, due to the whitening of the PVA film, partial staining was generated, which was not preferable as a polarizing film. Comparative Example 5 PVA10 having a saponification degree of 99.9 mol% and a polymerization degree of 4000
0 parts by weight, glycerin 10 parts by weight, lauric acid diethanolamide 0.1 part by weight, and a volatile content of 80
Wt% of a film-forming raw material is discharged to a chrome-plated metal first drum at 90 ° C.
It dried with the hot air of ° C, and obtained the PVA film of 75 micrometers in average thickness. At this time, the speed ratio between the winding speed of the PVA film and the peripheral speed of the first drum is 1.5, and the volatile content (water content) of the PVA film when peeled from the first drum is 52. % By weight. In this case, several wrinkles occurred on the PVA film during the film formation. When this PVA film was processed into a polarizing film, the stretching ratio was 4.3 times, and the obtained polarizing film had a thickness of 28 μm and a transmittance of 43.5.
%, The degree of polarization was 99.2%, and the dichroic ratio was 39.5, but due to wrinkles of the PVA film, partial staining spots were generated, which was not preferable as a polarizing film. Comparative Example 6 PVA10 having a saponification degree of 99.9 mol% and a polymerization degree of 1700
0 parts by weight, 10 parts by weight of glycerin, 0.1 part by weight of lauric acid diethanolamide, and a volatile content of 65 consisting of water.
Wt% of a film-forming material was discharged onto a chrome-plated metal first drum at 65 ° C.
It was dried with hot air at 5 ° C. to obtain a PVA film having an average thickness of 75 μm. At this time, the speed ratio between the winding speed of the PVA film and the peripheral speed of the first drum was 1.5, and the volatile content (water content) of the PVA film when peeled from the first drum was 6% by weight. Met. In this case, during film formation, P
The VA film was partially whitened. When this PVA film was processed into a polarizing film, the stretching ratio was 3.6 times, and the obtained polarizing film had a thickness of 27 μm and a transmittance of 43.4.
%, The degree of polarization was 96.0%, and the dichroic ratio was 25.1. However, due to the whitening of the PVA film, partial staining spots were generated, which was not preferable as a polarizing film. Examples 1 , 2, 5 and Comparative Example A
To C, 1 to 6 are shown in Tables 1 to 3 below. Each of these tables shows the degree of polymerization of the PVA used for the PVA film. [Table 1] [Table 2] [Table 3] In Tables 1 to 3, D2 / D1 indicates the ratio between the winding speed and the peripheral speed of the first drum, and K indicates the first speed.
It shows the volatile content (moisture content) of the PVA film when peeled from the drum, and Rd shows the dichroic ratio. Further, in each column of Tables 1 to 3, ◎ indicates the most excellent one,
は indicates good, △ indicates bad, and × indicates bad and unusable. As is clear from the above tables, when the ratio of the winding speed to the peripheral speed of the first drum deviates from the range of 0.8 to 1.3, the stretchability of the PVA film becomes poor. Alternatively, dyeing unevenness occurs, and the quality of the polarizing film obtained from the PVA film deteriorates. From this fact, in order to obtain a polarizing film having good stretchability of the PVA film, less occurrence of stained spots, and excellent polarizing performance, the ratio of the winding speed to the peripheral speed of the first drum should be set to 0.1. It can be understood that it is necessary to be within the range of 8 to 1.3. As described above, according to the present invention, a PVA film which is useful as a material for producing a polarizing film and which can be stretched at a high magnification to obtain a polarizing film having excellent polarizing performance can be obtained. be able to.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic configuration diagram of a drum type film forming machine used in the production method of the present invention. [Description of References] 2 ... film forming raw material, 3 ... drum (first drum), 4 ... polyvinyl alcohol film (PVA film), 8 ... winding device.

────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. ⁷ Identification symbol FI C08L 29:04 C08L 29:04 (56) References JP-A-9-290427 (JP, A) JP-B-38-23037 (JP) , B1) (58) Field surveyed (Int. Cl. ⁷ , DB name) B29C 41/00-41/52

Claims (1)

(57) [Claims] [Claim 1] The average degree of polymerization is 2 using a drum film forming machine.
More than 000 polyvinyl alcohol and polyvinyl alcohol
0.01 to 1 part by weight per 100 parts by weight of alcohol
For polarizing film producing Po <br/> polyvinyl alcohol film for a polarization film from the film raw material containing surfactant
A method for producing a polyvinyl alcohol film, the uppermost
The polyvinyl alcohol for polarizing film is placed on the drum
A film of rucol film is formed at a temperature of 50C to 150C.
And when the volatile content reaches 10 to 50% by weight
In is peeled from the drum, the speed ratio between the winding device and the drum of the polyvinyl alcohol film for a polarizing film (peripheral speed of the winding speed / drum) is 0. 8 to 1.3 of
A method for producing a polyvinyl alcohol film for a polarizing film , comprising winding up under conditions .