WO2014157737A1 - Procédé pour la production d'un film polarisant - Google Patents

Procédé pour la production d'un film polarisant Download PDF

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Publication number
WO2014157737A1
WO2014157737A1 PCT/JP2014/059699 JP2014059699W WO2014157737A1 WO 2014157737 A1 WO2014157737 A1 WO 2014157737A1 JP 2014059699 W JP2014059699 W JP 2014059699W WO 2014157737 A1 WO2014157737 A1 WO 2014157737A1
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Prior art keywords
film
swelling
treatment tank
treatment
expansion coefficient
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PCT/JP2014/059699
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English (en)
Japanese (ja)
Inventor
圭二 網谷
Original Assignee
住友化学株式会社
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Application filed by 住友化学株式会社 filed Critical 住友化学株式会社
Priority to CN201480017962.6A priority Critical patent/CN105103013B/zh
Priority to KR1020157023482A priority patent/KR102130185B1/ko
Publication of WO2014157737A1 publication Critical patent/WO2014157737A1/fr

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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
    • G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
    • G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/30—Polarising elements
    • G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state

Definitions

  • the present invention relates to a method for producing a polarizing film for use in a liquid crystal display device.
  • a polarizing film obtained by adsorbing and orienting a dichroic dye on a polyvinyl alcohol-based resin film has been used. That is, an iodine polarizing film using iodine as a dichroic dye, a dye polarizing film using a dichroic dye as a dichroic dye, and the like are known. These polarizing films are usually used as polarizing plates by attaching a protective film such as triacetyl cellulose via an adhesive made of an aqueous solution of a polyvinyl alcohol-based resin on at least one side, preferably both sides thereof. Used in liquid crystal display devices such as monitors and mobile phones.
  • the polarizing film is produced by subjecting the polyvinyl alcohol resin film to swelling treatment, dyeing treatment, stretching treatment, boric acid treatment (crosslinking treatment) and washing treatment, and finally drying.
  • This stretching process is usually performed by using a pair of nip rolls and changing the rotational peripheral speed of the nip rolls.
  • optical performance such as polarization performance tends to deteriorate.
  • the thickness of the film becomes non-uniform, and the uniformity of optical performance such as transmittance in the film surface also tends to deteriorate.
  • An image display device to which such a polarizing film is applied has a problem that unevenness occurs in display and the image quality deteriorates. Therefore, development of a method for producing a polarizing film having the requirements for the polarizing film as described above and excellent in productivity has been performed.
  • Patent Document 1 a plurality of swelling treatment tanks are provided, and the bath temperature of the swelling treatment tank located on the front side of them is set higher than the bath temperature of the swelling treatment tank located behind.
  • a method for producing a polarizing film is disclosed, which can produce a high-quality polarizing film in which color unevenness is suppressed by setting it high in a short time. According to this method, since the expansion amount of the resin film reaches saturation in a short time, the film is difficult to swell in the subsequent dyeing treatment, and color unevenness of the polarizing film due to this is suppressed.
  • An object of the present invention is excellent in productivity, and is excellent in appearance by suppressing unevenness of film thickness and generation of wrinkles in each treatment applied to a raw film made of polyvinyl alcohol resin, particularly in a swelling treatment. It is providing the manufacturing method of a polarizing film.
  • a method for producing a polarizing film by subjecting a raw film made of a polyvinyl alcohol resin to swelling treatment, dyeing treatment, boric acid treatment, and washing treatment in this order,
  • the thickness is 10 to 60 ⁇ m
  • the swelling treatment described above is passed through a plurality of swelling treatment tanks including at least a first swelling treatment tank and a second swelling treatment tank arranged in order from the side on which the raw film enters.
  • the expansion coefficient in the width direction of the film in the first swelling treatment tank is 90% or less of the saturation expansion coefficient when immersed in a treatment liquid having the same temperature and composition, and in the first swelling treatment tank
  • the absolute value of the difference when the expansion coefficient in the width direction of the film and the expansion coefficient in the width direction of the film in the second swelling treatment tank are respectively expressed as percentages is within 2 points.
  • the treatment temperature of the first swelling treatment tank is 35 to 45 ° C.
  • the treatment temperature of the second swelling treatment tank is 25 to 35 ° C. lower than the treatment temperature of the first swelling treatment tank. It is preferable.
  • the processing temperature of the first swelling treatment tank and the time for passing through the treatment tank are adjusted so that the expansion coefficient in the width direction of the film in the first swelling treatment tank is 15 to 25%. Is preferred.
  • a method for producing a polarizing film by subjecting an original film made of polyvinyl alcohol resin to a swelling process, a dyeing process, a boric acid process, and a washing process in this order.
  • the film has a thickness of 10 to 60 ⁇ m, and the above swelling treatment is applied by passing through one swelling treatment tank, and the expansion coefficient in the width direction of the film in the swelling treatment tank has the same temperature and composition. 90% or less of the saturated expansion coefficient when immersed in the film, and the absolute difference between the expansion coefficient in the width direction of the film in the swelling treatment tank and the expansion coefficient in the width direction of the film in the dyeing treatment tank, expressed as a percentage, respectively.
  • the method for producing a polarizing film wherein the treatment temperature of the swelling treatment tank and the dyeing treatment tank and the time for passing through the treatment tank are adjusted so that the value is within 2 points. It is provided.
  • the treatment temperature of the swelling treatment tank is 35 to 45 ° C.
  • the treatment temperature of the dyeing treatment tank is preferably lower than the treatment temperature in the swelling treatment and 25 to 35 ° C.
  • a polarizing film having an excellent appearance can be obtained efficiently.
  • a polarizing film is produced by subjecting an original film made of a polyvinyl alcohol resin to swelling treatment, dyeing treatment, boric acid treatment and washing treatment in this order. And the polarizing film obtained by performing a drying process after a washing process becomes a thing by which wrinkles etc. were suppressed, and is used suitably for a polarizing plate.
  • the present invention will be described in detail.
  • the polarizing film has a dichroic dye adsorbed and oriented on a polyvinyl alcohol resin film.
  • the polyvinyl alcohol resin used as a raw material is usually obtained by saponifying a polyvinyl acetate resin.
  • the degree of saponification is usually 85 mol% or more, preferably 90 mol% or more, more preferably 99 mol% or more.
  • the polyvinyl acetate-based resin include polyvinyl acetate, which is a homopolymer of vinyl acetate, and copolymers of vinyl acetate and other monomers copolymerizable therewith.
  • Examples of other monomers copolymerizable with vinyl acetate include unsaturated carboxylic acids, olefins, unsaturated sulfonic acids, vinyl ethers and the like.
  • the degree of polymerization of the polyvinyl alcohol-based resin is usually about 1000 to 10000, preferably about 1500 to 5000.
  • polyvinyl alcohol resins may be modified, and for example, polyvinyl formal, polyvinyl acetal, polyvinyl butyral and the like modified with aldehydes may be used.
  • a material for producing the polarizing film an unstretched film (raw film) of a polyvinyl alcohol-based resin film having a thickness of about 10 to 60 ⁇ m, preferably about 12 to 55 ⁇ m is used.
  • a film having a width of 1500 to 6000 mm is practical.
  • the thickness of the polarizing film obtained by subjecting this raw film to the swelling treatment, the dyeing treatment, the boric acid treatment (crosslinking treatment) and the washing treatment in this order and finally drying is about 5 to 25 ⁇ m, for example.
  • the polarizing film is produced by subjecting the raw film made of polyvinyl alcohol resin to the swelling treatment, the dyeing treatment, the boric acid treatment and the washing treatment in this order, as described above, during the boric acid treatment and as necessary.
  • Uniaxial stretching of the film is performed before boric acid treatment.
  • Uniaxial stretching may be wet stretching or dry stretching, and is wet stretching when performed during the boric acid treatment and during the swelling treatment or dyeing treatment before the boric acid treatment, and when performed before the swelling treatment, Become.
  • This uniaxial stretching may be performed in one step or in two or more steps, but is preferably performed in a plurality of steps.
  • stretching method is employable for the uniaxial stretching of this invention. Examples of the stretching method include inter-roll stretching that stretches with a difference in peripheral speed between two nip rolls that transport the film, hot roll stretching as described in Japanese Patent No. 2731813, tenter stretching, and the like.
  • a known widening device such as an expander roll (widening roll), a spiral roll, a crown roll, or a bend bar is used. It is preferable to transport the film while removing wrinkles of the film.
  • a swelling treatment tank having a high expansion coefficient of a film such as a first swelling treatment tank when performing a swelling treatment described later in a plurality of treatment tanks and a swelling treatment tank when performing a swelling treatment in one treatment tank. It is effective to use this widening device.
  • the water flow in the swelling treatment tank is controlled by an underwater shower, or an EPC device (Edge position control device) that detects the edge of the film and prevents meandering, etc. It is also useful to use in combination.
  • the film swells and expands in the film transport direction. If the film is not actively stretched, the speed of transport rolls such as nip rolls and guide rolls is eliminated to eliminate film slack in the transport direction. It is preferable to take measures to adjust the value. Further, when the raw film is subjected to swelling treatment, dyeing treatment and boric acid treatment in this order, uniaxial stretching may be performed in the swelling treatment, and the stretching ratio in that case is about 1.2 to 3 times. Preferably, it is 1.3 to 2.5 times.
  • the swelling treatment is performed using a plurality of swelling treatment tanks.
  • the swelling treatment is performed by passing through a plurality of swelling treatment tanks including at least a first swelling treatment tank and a second swelling treatment tank arranged in this order from the side where the raw film enters.
  • the treatment temperature in the first swelling treatment tank and the second swelling treatment tank and the time during which the film passes are appropriately adjusted so that the expansion coefficient in the width direction of the film in each treatment tank is within a predetermined range.
  • the expansion coefficient in the width direction of the film is the percentage of expansion in the width direction of the polyvinyl alcohol-based resin film produced by the swelling treatment. Specifically, first, a long raw film made of a polyvinyl alcohol-based resin is cut into pieces having a size of 50 mm in the length direction and 50 mm in the width direction, and the same processing conditions as the swelling treatment tank are applied to the film pieces. Apply swelling treatment. The amount of change in the width direction of the film piece before and after the swelling treatment (the length in the width direction after the swelling treatment ⁇ the length in the width direction before the swelling treatment) is divided by the length in the width direction at the time of cutting (50 mm). The expansion rate is expressed as a percentage.
  • the expansion coefficient in the width direction of the film in the first swelling treatment tank referred to in the present invention means that when the swelling treatment is performed on the above-described film fragments under the same treatment conditions as those in the first swelling treatment tank. Refers to the expansion rate.
  • This expansion rate is the same as that of the first swelling treatment bath in the state where the film piece is not tensioned for the same time as the film passes through the first swelling treatment tank in the production apparatus. Yes, it is immersed in an aqueous solution set at the same temperature, and the amount of change in the width direction of the film piece generated at that time is divided by the length (50 mm) in the width direction at the time of cutting, and expressed as a percentage. .
  • the expansion coefficient in the width direction of the film in the second swelling treatment tank referred to in the present invention is the second of the film fragments subjected to the swelling treatment under the same treatment conditions as the first swelling treatment tank.
  • the amount of change from the length in the width direction of the film piece at the time of cutting after being immersed in an aqueous solution having the same composition as the second swelling treatment bath and set at the same temperature without tension (The length in the width direction after the second swelling treatment—the length in the width direction at the time of cutting) is divided by the length in the width direction at the time of cutting (50 mm) and expressed as a percentage.
  • the saturation expansion coefficient referred to in the present invention is an expansion coefficient obtained under the same conditions as the calculation of the expansion coefficient in the above-described swelling treatment tank except for the immersion time, and a film fragment measuring 50 mm in the long direction and 50 mm in the width direction is the original. It is cut from the anti-film and refers to the expansion rate when it is immersed in a treatment bath for 10 minutes.
  • the saturation expansion coefficient is the amount of change in the width direction of a film piece that occurs when the film piece is immersed in a treatment bath for 10 minutes in a state where no tension is applied (the length in the width direction after immersion-the length in the width direction before immersion). ) Is divided by the length (50 mm) in the width direction at the time of cutting, and expressed as a percentage.
  • the treatment bath used here has the same composition as the first swelling treatment bath and an aqueous solution set at the same temperature when the saturation expansion coefficient in the first swelling treatment bath is desired.
  • the expansion coefficient in the width direction of the film in the first swelling treatment tank is immersed in a treatment liquid having the same temperature and composition.
  • the time for passing through the treatment tank is adjusted so as to be 90% or less of the saturated expansion coefficient.
  • the expansion coefficient in the width direction of the film in the first swelling treatment tank is preferably 70% or more. If the expansion rate is less than 70%, it is difficult to uniformly swell the film surface in the swelling treatment, and color unevenness and wrinkles are likely to occur.
  • the expansion coefficient in the width direction of the film in the first swelling treatment tank is too small and the expansion coefficient in the width direction of the film in the second swelling treatment tank becomes large, in the second swelling treatment tank, Since the film swells rapidly, the expansion coefficient may be biased between the end and the center of the film. As a result, when the above widening device is used inside the treatment tank, wrinkles may occur due to this bias in expansion coefficient.
  • the expansion coefficient in the width direction of the film in the first swelling treatment tank is too large, the film cannot be sufficiently widened by the widening device used inside the treatment tank, and wrinkles may occur.
  • the absolute value of the difference when the expansion coefficient in the width direction of the film in the first swelling treatment tank and the expansion coefficient in the width direction of the film in the second swelling treatment tank are each expressed as a percentage is within 2 points.
  • the first swelling treatment is performed so that the absolute value of the difference when the expansion coefficient in the width direction of the film in the first swelling treatment tank and the second swelling treatment tank is each expressed as a percentage is within 2 points.
  • the treatment temperature of the tank and the second swelling treatment tank and the time to pass through the treatment tank By adjusting the treatment temperature of the tank and the second swelling treatment tank and the time to pass through the treatment tank, the shortage of treatment in the first swelling treatment tank is suppressed, and the undesired rapid in the second swelling treatment tank Swelling can be suppressed.
  • the treatment temperature of the first swelling treatment tank and the second swelling treatment tank and the time for passing through the treatment tank it is possible to suppress the film thickness from becoming non-uniform during swelling. The generation of wrinkles is suppressed, and a polarizing film having good optical properties and appearance can be produced.
  • the treatment temperature of the first swelling treatment tank is higher than the treatment temperature of the second swelling treatment tank from the viewpoint of shortening the time of the swelling treatment.
  • the temperature is 35 to 45 ° C.
  • the temperature of the second swelling treatment tank is preferably 25 to 35 ° C.
  • the time for the film to pass through the first swelling treatment tank is 10 to 60 seconds, preferably 15 to 50 seconds.
  • the time for the film to pass through the second swelling treatment tank is also 10 to 60 seconds, preferably 15 to 50 seconds.
  • the swelling treatment is performed in only one swelling treatment tank.
  • the raw film is taken out of the swelling treatment tank and then conveyed to the dyeing treatment tank.
  • the treatment temperature in the swelling treatment tank and the dyeing treatment tank and the time during which the film passes are appropriately adjusted so that the expansion coefficient in the width direction of the film in each treatment tank is within a predetermined range.
  • the expansion coefficient in the width direction of the film in the swelling treatment tank is 90% or less of the saturated expansion coefficient when immersed in a treatment liquid having the same temperature and composition
  • the swelling treatment tank and dyeing so that the absolute value of the difference when the expansion coefficient in the width direction of the film in the swelling treatment tank and the expansion coefficient in the width direction of the film in the dyeing treatment tank are respectively expressed as percentages are within 2 points.
  • the processing temperature of a processing tank and the time which passes a processing tank are adjusted.
  • the dyeing treatment is performed for the purpose of adsorbing the dichroic dye on the polyvinyl alcohol-based resin film.
  • the dichroic dye iodine, a water-soluble dichroic dye, or the like can be used.
  • the treatment conditions are determined within a range in which these objects can be achieved and within a range in which problems such as dissolution and devitrification of the polyvinyl alcohol resin film do not occur.
  • the treatment bath has, for example, a concentration of iodine / potassium iodide / water by weight ratio of about 0.003 to 0.2 / about 0.1 to 10 / 100 aqueous solution can be used.
  • a concentration of iodine / potassium iodide / water by weight ratio of about 0.003 to 0.2 / about 0.1 to 10 / 100 aqueous solution can be used.
  • potassium iodide other iodides such as zinc iodide may be used, or potassium iodide and other iodides may be used in combination.
  • compounds other than iodide for example, boric acid, zinc chloride, cobalt chloride and the like may coexist.
  • boric acid When boric acid is added to the treatment bath, it is distinguished from boric acid treatment described later in that it contains iodine.
  • Any dye containing about 0.003 parts by weight or more of iodine with respect to 100 parts by weight of water can be regarded as a dyeing treatment bath.
  • the temperature of the treatment bath when dipping the film is about 10 to 45 ° C, preferably 25 to 35 ° C.
  • the immersion time of the film is about 30 to 600 seconds, preferably 30 to 300 seconds.
  • an aqueous solution having a concentration of dichroic dye / water about 0.001 to 0.1 / 100 by weight can be used for the treatment bath.
  • This treatment bath may contain a dyeing assistant and the like, and examples thereof include inorganic salts such as sodium sulfate, surfactants and the like.
  • the dichroic dye may be used alone or in combination of two or more dichroic dyes.
  • the temperature of the treatment bath when dipping the film is about 20 to 80 ° C., preferably 25 to 70 ° C., and the dipping time of the film is about 30 to 600 seconds, preferably 30 to 300 seconds.
  • the stretching process is performed by a method of giving a difference in peripheral speed between the pair of nip rolls.
  • the cumulative draw ratio until the dyeing treatment is usually 1.6 to 4.5 times, preferably about 1.8 to 4 times.
  • the cumulative stretch ratio until the dyeing treatment is less than 1.6 times, the frequency of breakage of the film increases, and the yield tends to deteriorate.
  • the film in the dyeing process, as in the swelling process, it is preferable to convey the film while stretching the wrinkles of the film using a known widening device such as an expander roll, a spiral roll, a crown roll, or a bend bar.
  • a known widening device such as an expander roll, a spiral roll, a crown roll, or a bend bar.
  • the swelling treatment tank and the dyeing are performed so that the expansion rate in the width direction of the film in the swelling treatment tank and the dyeing treatment tank is within a predetermined range.
  • the treatment temperature in the treatment tank and the time for the film to pass through are appropriately adjusted.
  • the expansion coefficient in the width direction of the film can be obtained in the same manner as the expansion coefficient in the width direction of the film in the first swelling treatment tank described above, and a film fragment obtained by cutting the raw film in the same manner as described above. Can be calculated from the amount of change in the width direction of the film fragments generated at this time and the length in the width direction at the time of cutting.
  • the saturation expansion coefficient in the swelling treatment tank can also be obtained by the same method as the saturation expansion coefficient in the first swelling treatment tank.
  • the expansion coefficient in the width direction of the film in the dyeing tank is the coefficient of expansion when the film pieces subjected to the swelling process under the same processing conditions as the swelling tank are further processed under the same processing conditions as the dyeing tank. Yes, it can be obtained in the same manner as the expansion coefficient in the second swelling treatment tank.
  • the film piece subjected to the swelling treatment under the same processing conditions as the swelling treatment tank is the same as the dyeing treatment bath in the state where the film piece is not tensioned for the same time as the film passes through the dyeing treatment tank.
  • the amount of change from the length in the width direction of the film piece at the time of cutting after being immersed in an aqueous solution set to the composition and temperature (the length in the width direction after the dyeing process ⁇ the length in the width direction at the time of cutting) Dividing by the length in the width direction at the time of cutting, it is expressed as a percentage.
  • the expansion coefficient in the width direction of the film in the swelling treatment tank is 90% of the saturation expansion coefficient when immersed in the treatment liquid having the same temperature and composition.
  • the time for passing through the treatment tank is adjusted to be as follows. By setting the saturation expansion coefficient to 90% or less, even when the film feed rate is increased, it is not necessary to use a huge apparatus, and the swelling treatment can be performed efficiently.
  • the expansion coefficient in the width direction of the film in the swelling treatment tank is preferably 70% or more. If the expansion rate is less than 70%, it is difficult to uniformly swell the film surface in the swelling treatment, and color unevenness and wrinkles are likely to occur.
  • the expansion coefficient in the width direction of the film in the swelling treatment tank is too small, and the expansion coefficient in the width direction of the film in the dyeing treatment tank becomes large, the film will swell rapidly in the dyeing treatment tank, The expansion coefficient may be biased between the end and the center of the film. As a result, when the above widening device is used inside the treatment tank, wrinkles may occur due to this bias in expansion coefficient. On the other hand, when the expansion coefficient in the width direction of the film in the swelling treatment tank is too large, the widening device used inside the treatment tank cannot sufficiently widen the film, and wrinkles may occur.
  • the swelling is performed so that the absolute value of the difference when the expansion coefficient in the width direction of the film in the swelling treatment tank and the expansion coefficient in the width direction of the film in the dyeing treatment tank are each expressed as percentages is within two points. It is important to adjust the processing temperature of each of the processing tank and the dyeing processing tank and the time for passing through the processing tank.
  • the present invention relates to a swelling treatment tank and a swelling treatment tank so that the difference when the expansion coefficient in the width direction of the film in the swelling treatment tank and the expansion coefficient in the width direction of the film in the dyeing treatment tank are each expressed in percentage
  • the treatment time of the dyeing treatment tank and the time for passing through the treatment tank By adjusting the treatment time of the dyeing treatment tank and the time for passing through the treatment tank, insufficient treatment in the swelling treatment tank can be suppressed, and undesired rapid swelling in the dyeing treatment tank can be suppressed.
  • the treatment temperature of the swelling treatment tank and the dyeing treatment tank and the time for passing through the treatment tank it is possible to prevent the film thickness from becoming non-uniform during swelling. Is suppressed, and a polarizing film with good optical properties and appearance can be produced.
  • the temperature is preferably as high as possible within a range in which the film does not dissolve, and the treatment temperature of the swelling treatment tank is preferably 35 to 45 ° C. Further, the temperature of the dyeing tank is preferably 25 to 35 ° C. Furthermore, it is preferable to adjust the treatment temperature of the swelling treatment tank and the time for passing through the treatment tank so that the expansion coefficient in the width direction of the film in the swelling treatment tank is 15 to 25%.
  • Boric acid treatment The boric acid treatment is performed for the purpose of water resistance by cross-linking and hue adjustment (preventing blue and reddish film colors).
  • an aqueous solution containing about 1 to 10 parts by weight of boric acid with respect to 100 parts by weight of water is used.
  • iodide is added to water in addition to boric acid. It is preferable to contain 1 to 30 parts by weight with respect to 100 parts by weight.
  • iodide include potassium iodide, sodium iodide, zinc iodide and the like.
  • boric acid treatment for water resistance may be referred to by names such as cross-linking treatment, water resistance treatment, and immobilization treatment, and boric acid treatment for hue adjustment may be complementary color treatment, toning treatment, etc. Sometimes called by name.
  • This boric acid treatment is performed by appropriately adjusting the concentration of boric acid and iodide and the temperature of the treatment bath according to the purpose.
  • the boric acid treatment for water resistance and the boric acid treatment for hue adjustment are not particularly distinguished, but are performed under the following conditions.
  • the temperature of the treatment bath is usually about 50 to 70 ° C., preferably 55 to 65 ° C.
  • the immersion time of the film is usually about 10 to 600 seconds, preferably 20 to 300 seconds, more preferably 20 to 200 seconds. is there.
  • the temperature of the boric acid treatment bath is usually about 50 to 85 ° C., preferably 55 to 80 ° C.
  • the boric acid treatment for adjusting the hue may be performed after the boric acid treatment for water resistance.
  • the temperature of the treatment bath is usually about 10 to 45 ° C.
  • the immersion time of the film is usually about 10 to 300 seconds, preferably 10 to 100 seconds.
  • boric acid treatments may be performed a plurality of times such as boric acid treatment for water resistance and boric acid treatment for hue adjustment.
  • the aqueous solution composition and temperature of each boric acid treatment tank to be used may be the same or different within the above range.
  • you may perform the boric-acid process for water resistance, and the boric-acid process for hue adjustment in a some process, respectively.
  • the cleaning treatment is performed for the purpose of removing excess chemicals such as boric acid and iodine attached to the polyvinyl alcohol-based resin film after the boric acid treatment.
  • a polarizing film treated with boric acid for water resistance and / or color tone adjustment is immersed in water, water is sprayed by a shower, or both are used in combination. Is done.
  • the temperature of water in the washing treatment is usually about 2 to 40 ° C., and the treatment time is preferably about 5 to 120 seconds.
  • the polarizing film can be produced by drying the polyvinyl alcohol resin film.
  • the drying treatment is performed in a drying furnace at a temperature of about 40 to 100 ° C. for a time of about 60 to 600 seconds.
  • the final integrated draw ratio of the polarizing film thus produced is usually about 4.5 to 7 times, preferably about 5 to 6.5 times.
  • processing other than the above can be added for other purposes.
  • treatments that can be added include immersion treatment in an aqueous iodide solution that does not contain boric acid (iodide treatment), immersion treatment in an aqueous solution that does not contain boric acid and contains zinc chloride, etc. Zinc treatment).
  • the polarizing plate which is a laminated body of a polarizing film and a protective film is formed by bonding a protective film on the at least single side
  • protective films include acetyl cellulose resin films such as triacetyl cellulose, cycloolefin resin films, cycloolefin copolymer resin films, polyester resin films such as polyethylene terephthalate, polyethylene naphthalate, and polybutylene terephthalate. , Polycarbonate resin films, acrylic resin films such as polymethylmethacrylate, acyclic olefin resin films such as polypropylene and polyethylene, and the like.
  • the bonding surface of the polarizing film and / or the protective film is subjected to corona treatment, plasma treatment, flame treatment, ultraviolet treatment, primer treatment, Surface treatments such as saponification treatment, solvent treatment by solvent application and drying can also be applied.
  • thermoplastic resin a thermoplastic resin
  • optical compensation film which orientated the liquid crystal compound in the stretched film of thermoplastic resin or a thermoplastic resin
  • Known stretched films of these thermoplastic resins and optical compensation films in which a liquid crystal compound is oriented in a thermoplastic resin can be used as appropriate.
  • the adhesive used for laminating the polarizing film and the protective film is not particularly limited as long as it can join the polarizing film and the protective film, but an adhesive satisfying sufficient adhesive force and transparency is selected. From these points, an ultraviolet curable adhesive is preferably used for bonding a polarizing film and a protective film.
  • an aqueous adhesive for example, an aqueous solution of a polyvinyl alcohol-based resin and an aqueous solution in which a crosslinking agent is mixed with this, a urethane-based resin.
  • An emulsion adhesive or the like can be used.
  • the ultraviolet curable adhesive may be a mixture of an acrylic compound and a photo radical polymerization initiator, a mixture of an epoxy compound and a photo cationic polymerization initiator, or the like.
  • a cationic polymerizable epoxy compound and a radical polymerizable acrylic compound may be used in combination, and a photo cationic polymerization initiator and a photo radical polymerization initiator may be used in combination as an initiator.
  • the adhesive is cured by irradiating ultraviolet rays after the films are laminated.
  • the ultraviolet light source is not particularly limited, but preferably has a light emission distribution at a wavelength of 400 nm or less.
  • the low pressure mercury lamp, medium pressure mercury lamp, high pressure mercury lamp, ultra high pressure mercury lamp, chemical lamp, black light lamp, microwave excitation Mercury lamps and metal halide lamps are preferably used.
  • the light irradiation intensity for curing the ultraviolet curable adhesive is appropriately determined depending on the composition of the adhesive and is not particularly limited.
  • the irradiation intensity in the wavelength region effective for activating the polymerization initiator is 0.1 to 6000 mW / It is preferable to be cm 2 .
  • the light irradiation time is also selected according to the adhesive to be cured and is not particularly limited.
  • the integrated light amount expressed as the product of the irradiation intensity and the irradiation time is 10 to 10,000 mJ / cm 2. It is preferable to set as follows.
  • the integrated light amount By appropriately selecting the integrated light amount from this range, a sufficient amount of active species derived from the polymerization initiator can be generated, the curing reaction can proceed reliably, and the irradiation time can be shortened, thus maintaining good productivity. it can.
  • a UV curable adhesive is cured by irradiation of UV light with a laminated film including a polarizing film and a protective film, the polarization degree, transmittance and hue of the polarizing film, transparency of the protective film, etc. It is preferable to perform the curing under conditions that do not reduce the various functions.
  • an aqueous adhesive for example, apply the adhesive uniformly on the surface of the film or pour it between two films, overlap the two films via the coating layer, and bond them with a roll or the like. Then, a drying method can be adopted. After drying, it may be further cured at room temperature or slightly higher temperature, for example, about 20 to 45 ° C.
  • the thickness of the above adhesive layer is appropriately selected from the range of about 0.001 to 5 ⁇ m depending on the type of adhesive and the combination of two films to be bonded.
  • the thickness is preferably 0.01 ⁇ m or more, and preferably 2 ⁇ m or less.
  • the expansion coefficient of the film was calculated from the amount of change in the width direction of the film before and after immersion in the swelling treatment tank or the dyeing treatment tank to be measured.
  • a long polyvinyl alcohol film (raw film) used in each of the examples and comparative examples described below was cut into a size of 50 mm in the long direction and 50 mm in the width direction to obtain a film fragment.
  • the film piece was immersed in the treatment liquid having the same composition as the treatment bath for measuring the expansion coefficient at the same temperature as the actual treatment and for the same time as the film passed through the treatment tank. . This immersion was performed in a state where no tension was applied to the film.
  • the film piece is taken out from the processing solution, and the changed length in the width direction of the film piece before and after the treatment with respect to the length in the width direction at the time of cutting (length after treatment ⁇ length at the time of cutting 50 mm) is obtained.
  • the length of the film piece after the treatment was measured using a commercially available digital caliper [manufactured by Mitutoyo Corporation, “Coolant Digimatic Caliper CD-15PSX”], and the size of the film piece immediately after removal from the water tank was measured.
  • Example 1 Prepare a long polyvinyl alcohol film [trade name “Kuraray Poval Film VF-PE # 6000” manufactured by Kuraray Co., Ltd., polymerization degree 2400, saponification degree 99.9 mol% or more] having a thickness of 60 ⁇ m, and swelling treatment As described above, the film was immersed in a first swelling treatment tank containing pure water at 37 ° C. for 40 seconds while maintaining a tension state so that the film does not loosen. Thereafter, the film was immersed in a second swelling treatment tank containing pure water at 30 ° C. for 20 seconds. At this time, in the 1st swelling processing tank, the film was conveyed using the expander roll.
  • a first swelling treatment tank containing pure water at 37 ° C. for 40 seconds while maintaining a tension state so that the film does not loosen. Thereafter, the film was immersed in a second swelling treatment tank containing pure water at 30 ° C. for 20 seconds. At this time, in the 1st swelling processing tank, the film was convey
  • uniaxial stretching is performed up to 2.2 times while being immersed in a dyeing bath containing a 30 ° C. aqueous solution containing iodine and potassium iodide as a dyeing treatment, and potassium iodide / boric acid / water is weight While being immersed in a boric acid treatment bath containing a 55 / ° C. aqueous solution having a ratio of 12 / 4.4 / 100, and being subjected to water resistance treatment, uniaxial stretching is performed until the cumulative draw ratio from the raw material reaches 5.5 times. It was. Then, after immersing in a bath containing 40 ° C.
  • boric acid aqueous solution it is immersed in a cleaning treatment bath containing 12 ° C. pure water, and then dried at 70 ° C. for 3 minutes in a drying furnace to obtain a polarizing film. Produced. In the swelling treatment, no generation of wrinkles was observed, and no breakage of the film was observed.
  • the polyvinyl alcohol film “Kuraraypoval film VF-PE # 6000” used in Example 1 was cut into a size of 50 mm in the long direction ⁇ 50 mm in the width direction, and this was cut.
  • the expansion coefficient when immersed in a water tank (corresponding to the first swelling treatment tank) containing pure water at 37 ° C. for 10 minutes was defined as the saturation expansion coefficient, which was obtained.
  • the length of the film piece in the width direction was 62.70 mm. From the amount of change in length by immersion with respect to the length in the width direction before immersion, the saturation expansion coefficient in the first swelling treatment tank was 25.4%.
  • Example 2 As a raw film, a long polyvinyl alcohol film having a thickness of 50 ⁇ m (trade name “Kuraray Poval Film VF-PE # 5000” manufactured by Kuraray Co., Ltd., polymerization degree 2400, saponification degree 99.9 mol% or more) is used. A polarizing film was produced in the same manner as in Example 1 except that the swelling treatment in the first swelling treatment tank was changed to be immersed in pure water at 35 ° C. for 30 seconds. In the swelling treatment, no generation of wrinkles was observed, and no breakage of the film was observed.
  • (A) Saturation expansion coefficient in the first swelling treatment tank A film piece is cut from the polyvinyl alcohol film “Kuraray Poval Film VF-PE # 5000” used in Example 2, and the temperature of pure water in the water tank is set to 35 ° C.
  • the saturated expansion coefficient in the first swelling treatment tank was determined in the same manner as in Example 1 (A) except that the change was made. After immersion, the width of the film piece in the width direction was 62.10 mm. From the amount of change in length by immersion with respect to the length in the width direction before immersion, the saturation expansion coefficient in the first swelling treatment tank was 24.2%.
  • Example 3 A 60- ⁇ m-thick polyvinyl alcohol film (trade name “Kuraray Poval Film VF-PE # 6000” manufactured by Kuraray Co., Ltd., polymerization degree 2400, saponification degree 99.9 mol% or more) is used as a raw film.
  • the swelling treatment the film was immersed in a swelling treatment tank containing pure water at 37 ° C. for 40 seconds while keeping the tension state so that the film did not loosen. At this time, in the swelling processing tank, the film was conveyed using the expander roll. Next, uniaxial stretching is performed up to 2.2 times while immersing in a dyeing bath containing a 30 ° C.
  • aqueous solution containing iodine and potassium iodide as a dyeing treatment, and potassium iodide / boric acid / water is in a weight ratio.
  • a boric acid treatment bath containing an aqueous solution at 55 ° C., which is 12 / 4.4 / 100 water-proofing, uniaxial stretching is performed until the cumulative draw ratio from the original fabric becomes 5.5 times It was.
  • a washing bath containing 12 ° C. pure water and dried in a drying furnace at 70 ° C. for 3 minutes to produce a polarizing film. did.
  • the swelling treatment and dyeing treatment no wrinkles were observed and no film breakage was observed.
  • (A) Saturation expansion rate in the swelling treatment tank The swelling treatment tank was obtained in the same manner as in Example 1 (A) except that the film piece was cut from the polyvinyl alcohol film “Kuraray Poval Film VF-PE # 6000” used in Example 3. The saturation expansion coefficient at was determined. After immersion, the length of the film piece in the width direction was 62.70 mm. From the amount of change in length due to immersion with respect to the length in the width direction before immersion, the saturation expansion coefficient in the swelling treatment tank was 25.4%.
  • Example 1 A polarizing film was produced in the same manner as in Example 1 except that the immersion time of the film in the first swelling treatment tank was changed to 10 seconds. Wrinkles occurred in the first swelling treatment tank and the second swelling treatment tank, and the film was frequently cut during stretching. Moreover, when the external appearance of the obtained polarizing film was confirmed, wrinkles were seen.
  • Example 2 A polarizing film was produced in the same manner as in Example 2 except that the immersion time of the film in the first swelling treatment tank was changed to 10 seconds. Moreover, wrinkles occurred in the first swelling treatment tank and the second swelling treatment tank, and the film was frequently cut during stretching. When the appearance of the obtained polarizing film was confirmed, wrinkles were observed.
  • Example 3 A polarizing film was produced in the same manner as in Example 2 except that the immersion time of the film in the first swelling treatment tank was changed to 100 seconds. Wrinkles were not observed in the first swelling treatment tank and the second swelling treatment tank.
  • Example 4 A polarizing film was produced in the same manner as in Example 2 except that the treatment temperature in the first swelling treatment tank was changed to 50 ° C. Since wrinkles were generated in the first swelling treatment tank and the second swelling treatment tank, and the film was frequently cut during stretching, a polarizing film could not be produced.
  • Example 5 A polarizing film was produced in the same manner as in Example 2 except that the treatment temperature in the first swelling treatment tank was changed to 20 ° C. Wrinkles occurred in the first swelling treatment tank and the second swelling treatment tank, and the film was frequently cut during stretching. When the appearance of the obtained polarizing film was confirmed, wrinkles were observed.
  • Example 1 that satisfies all the provisions of the present invention and Comparative Example 1 that uses the same raw film as Example 1 but does not satisfy the provisions of the present invention are compared.
  • Comparative Example 1 that uses the same raw film as Example 1 but does not satisfy the provisions of the present invention.
  • the film sufficiently swollen in the swelling treatment tank, wrinkles due to the difference in expansion coefficient in the second swelling treatment tank that occurs during production do not occur, and no wrinkles are confirmed in the obtained polarizing film.
  • Comparative Example 1 was not sufficiently swollen because the treatment time was short. As a result, wrinkles and film breakage occurred during production, and wrinkles were confirmed even in the obtained polarizing film. It was.
  • Example 2 when Example 2 using a raw film having a thinner film than Example 1 and Comparative Examples 2, 4 and 5 using the same raw film but not satisfying the provisions of the present application are compared, Example 2 is compared.
  • a polarizing film having a good appearance could be produced without causing wrinkles or film breakage during production, whereas in any of the comparative examples, wrinkles or film breakage occurred during production, and the polarized light obtained It was a result that wrinkles were also seen in the film, or breakage occurred frequently and a polarizing film could not be obtained.
  • Comparative Example 3 can produce a polarizing film with good appearance without producing film wrinkles or breakage during production, the treatment time in the first swelling treatment tank is long, and the production efficiency is higher than that in Example 2. It was low.
  • Example 3 which is another embodiment of the present invention, which is an example in which the swelling treatment is performed only in one swelling treatment tank, satisfies all the provisions of the present invention, and the film is sufficiently formed in the swelling treatment tank.
  • a polarizing film having an excellent appearance can be obtained efficiently.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Polarising Elements (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)

Abstract

Selon la présente invention, dans le procédé pour la production d'un film polarisant, dans les cas dans lesquels le gonflement est conduit avec une pluralité de réservoirs de gonflement, les températures de traitement dans un premier réservoir de gonflement et un second réservoir de gonflement suivant et les temps de traitement au cours desquels le film traverse les réservoirs de traitement sont commandés de telle sorte que le film dans le premier réservoir de gonflement a un degré de gonflement dans la direction de la largeur qui représente 90 % ou moins du degré de gonflement de saturation dans le liquide de traitement ayant la même température et la même composition, et de telle sorte que la différence entre le degré de gonflement du film dans le premier réservoir de gonflement et le degré de gonflement dans la direction de la largeur du film dans le second réservoir de gonflement se trouve dans 2 points en termes de valeur absolue. Dans les cas dans lesquels le gonflement est conduit avec un seul réservoir de gonflement, les températures de traitement dans le réservoir de gonflement et un réservoir de coloration suivant et les temps au cours desquels le film traverse les réservoirs de traitement sont commandés de telle sorte que le film dans le réservoir de gonflement a un degré de gonflement dans la direction de la largeur qui représente 90 % ou moins du degré de gonflement de saturation dans le liquide de traitement ayant la même température et la même composition, et de telle sorte que la différence entre le degré de gonflement du film dans le réservoir de gonflement et le degré de gonflement dans la direction de la largeur du film dans le réservoir de coloration se trouve dans 2 points en termes de valeur absolue.
PCT/JP2014/059699 2013-03-29 2014-03-26 Procédé pour la production d'un film polarisant WO2014157737A1 (fr)

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KR20170053037A (ko) * 2015-11-05 2017-05-15 스미또모 가가꾸 가부시키가이샤 편광자 및 그의 제조방법
JP6105795B1 (ja) * 2015-11-27 2017-03-29 住友化学株式会社 偏光子の製造方法
JP6105794B1 (ja) * 2015-11-27 2017-03-29 住友化学株式会社 偏光子の製造方法
WO2017094253A1 (fr) * 2015-11-30 2017-06-08 富士フイルム株式会社 Film à retard, son procédé de production, plaque polarisante pourvue d'un film à retard, et écran d'affichage à cristaux liquides
JP6776275B2 (ja) 2016-02-09 2020-10-28 株式会社クラレ 偏光フィルムの製造方法
CN107238881A (zh) * 2016-03-28 2017-10-10 住友化学株式会社 偏振膜的制造方法以及偏振膜的制造装置
JP2017182035A (ja) * 2016-03-28 2017-10-05 住友化学株式会社 偏光フィルムの製造方法および製造装置
JP7192198B2 (ja) * 2016-06-13 2022-12-20 三菱ケミカル株式会社 偏光膜用ポリビニルアルコール系フィルム、およびその製造方法、ならびに偏光膜、およびその製造方法
TWI740963B (zh) 2016-06-13 2021-10-01 日商三菱化學股份有限公司 聚乙烯醇系薄膜及其製造方法、以及使用該聚乙烯醇系薄膜之偏光膜
TWI762598B (zh) 2017-03-08 2022-05-01 日商可樂麗股份有限公司 偏光薄膜、偏光板、及其製造方法
KR102582196B1 (ko) 2017-03-08 2023-09-22 주식회사 쿠라레 편광 필름, 편광판, 및 그들의 제조 방법
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