WO2018025583A1 - フィルムの処理方法、及び偏光フィルムの製造方法 - Google Patents

フィルムの処理方法、及び偏光フィルムの製造方法 Download PDF

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Publication number
WO2018025583A1
WO2018025583A1 PCT/JP2017/024939 JP2017024939W WO2018025583A1 WO 2018025583 A1 WO2018025583 A1 WO 2018025583A1 JP 2017024939 W JP2017024939 W JP 2017024939W WO 2018025583 A1 WO2018025583 A1 WO 2018025583A1
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Prior art keywords
bath
film
solution
iodine
liquid
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PCT/JP2017/024939
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English (en)
French (fr)
Japanese (ja)
Inventor
直紀 川上
龍一 井上
裕己 藤井
西川　雅之
隼 三島
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日東電工株式会社
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Priority to CN201780002396.5A priority Critical patent/CN107922654B/zh
Priority to KR1020177031185A priority patent/KR102203012B1/ko
Publication of WO2018025583A1 publication Critical patent/WO2018025583A1/ja

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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
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • 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
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/12—Chemical modification
    • 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
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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 a film processing method for producing a polarizing film or the like.
  • a polarizing film has been used as a constituent material for liquid crystal display devices and polarized sunglasses.
  • a polarizing film for example, an iodine-based polarizing film is known.
  • the iodine-based polarizing film is obtained by performing a film treatment in which iodine is adsorbed on the film and crosslinked with a boron compound.
  • the iodine-based polarizing film is dyed by immersing the film in a dyeing bath having a solution containing iodine, immersing the dyed film in a cross-linking bath containing a boron compound, and stretching the cross-linked film. It is obtained by performing a series of film treatments in which the film is immersed in a bath and stretched, and the stretched film is immersed in an adjustment bath containing an iodine compound such as potassium iodide to adjust the hue.
  • an iodine compound such as potassium iodide
  • the solution in the front treatment bath is mixed with the solution in the rear treatment bath as the film moves, and the concentration of the solution in the rear treatment bath changes.
  • the film after being immersed in the dyeing bath is introduced into the crosslinking bath in a state in which a solution containing iodine (dyeing bath solution) is attached, and the film after being immersed in the crosslinking bath is a solution containing a boron compound. It is introduced into the adjustment bath in a state where the (crosslinking bath solution) is adhered.
  • the solution of the crosslinking bath is a solution containing a boron compound and iodine and having a relatively low concentration of the boron compound
  • the adjustment bath is composed of the iodine compound and the boron compound.
  • a solution having a relatively low iodine compound concentration when the solution in the front treatment bath is mixed into the rear treatment bath, the concentration of the solution in the rear treatment bath changes from the initial set value.
  • the boron compound is replenished to maintain the concentration of the active ingredient in the solution in the crosslinking bath within an allowable range
  • the iodine compound is replenished and adjusted. The concentration of the active ingredient in the solution in the bath is maintained within an acceptable range.
  • Virgin material is generally used as the iodine compound to be replenished.
  • surplus liquid suplus liquid including an overflow liquid and the like
  • waste of the surplus liquid can be reduced and the material cost can be reduced.
  • potassium iodide is more expensive than a boron compound or the like, reuse thereof can greatly contribute to reduction of material costs.
  • Patent Document 1 surplus liquids from a dyeing bath, a crosslinking bath and a washing bath are stored together in a storage tank, and the surplus liquid in the storage tank is transferred to an electrodialyzer, and potassium iodide is used in the electrodialyzer. It is disclosed to separate potassium concentrate and reuse potassium iodide.
  • the electrodialysis apparatus cannot sequentially separate the excess liquid generated in a chain in association with the film processing, and is performed independently of the film processing (so-called batch processing method). For this reason, separation and reuse of the surplus liquid cannot be performed in series in accordance with the film processing.
  • the use of the electrodialysis apparatus requires a relatively large installation place, and the maintenance and management of the electrodialysis membrane is complicated, and the running cost such as the power cost becomes high.
  • An object of the present invention is to provide a film processing method and a polarizing film manufacturing method capable of separating active ingredients from a surplus liquid in series in accordance with film processing.
  • the processing method of the 1st film of this invention has the process (X) which immerses a film in the bath which has a solution containing a boron compound and an iodine compound, takes out a part of said solution from the said bath, Using a reverse osmosis membrane, a solution containing a boron compound and a solution containing an iodine compound are separated.
  • the step (X) has a solution containing an iodine compound as an active ingredient, the film taken out by dipping in a bath having a solution containing a boron compound as an active ingredient. It is a step of immersing in a bath.
  • a preferred first treatment method of the present invention is a dyeing step in which the film is immersed in a dyeing bath, a crosslinking step in which the dyed film is immersed in a crosslinking bath, an adjustment step in which the crosslinked film is immersed in an adjustment bath,
  • the adjustment step is the step (X), and the adjustment bath is replenished with a solution containing an iodine compound separated through the reverse osmosis membrane.
  • the film includes a polyvinyl alcohol film
  • the boron compound includes boric acid
  • the iodine compound includes potassium iodide.
  • the second film processing method of the present invention includes a step (Y) of immersing the film in a bath having a solution containing a boron compound and iodine, taking out a part of the solution from the bath, and inverting the solution. Using an osmotic membrane, a solution containing a boron compound and a solution containing iodine are separated.
  • the step (Y) is a bath having a solution containing a boron compound as an active ingredient, the film taken out by dipping in a bath having a solution containing iodine as an active ingredient. It is the process of immersing in.
  • the preferable second film processing method of the present invention is that the film processing is performed by a dyeing step in which the film is immersed in a dyeing bath, a crosslinking step in which the dyed film is immersed in a crosslinking bath, and an adjustment in which the crosslinked film is immersed in an adjustment bath.
  • the crosslinking step is the step (Y), and a solution containing the boron compound separated using the reverse osmosis membrane is replenished to the crosslinking bath.
  • the manufacturing method of a polarizing film contains the processing method of one of the said films.
  • the film processing method and the polarizing film manufacturing method of the present invention use a reverse osmosis membrane to separate a solution containing a boron compound and a solution containing an iodine compound, or a solution containing a boron compound and a solution containing iodine.
  • a reverse osmosis membrane By using the reverse osmosis membrane, the active ingredient is separated from the surplus liquid in a series with the film treatment, and this can be supplemented to an arbitrary bath in conjunction with the film treatment.
  • the schematic reference figure which shows the film processing apparatus of 1st Embodiment The schematic reference figure which shows the separation apparatus of the film processing apparatus.
  • the schematic reference figure which shows the film processing apparatus of 2nd Embodiment The schematic reference figure which shows the separation apparatus of the film processing apparatus.
  • the processing method of the film of this invention has the process of immersing the solution containing an active ingredient in arbitrary films.
  • the process includes adsorbing, adhering, containing, or binding the active ingredient in the solution to any film.
  • an active ingredient means an ingredient required for the intended purpose of using the solution.
  • the film processing method of the present invention can be used for any film modification treatment, surface treatment, and the like.
  • a polarizing film can be manufactured using the film processing method of the present invention.
  • the present invention will be specifically described with a focus on film processing used in the production of polarizing films.
  • the film treatment according to the first embodiment includes a step (X) of immersing the film in a bath having a solution containing a boron compound and an iodine compound, and a part of the solution is taken out from the bath, and the solution is subjected to a reverse osmosis membrane. And separating the solution into a solution containing a boron compound and a solution containing an iodine compound.
  • This step (X) is, for example, a step of immersing a film taken out by immersion in a bath having a solution containing a boron compound as an active ingredient in a bath having a solution containing an iodine compound as an active ingredient.
  • FIG. 1 is a reference diagram illustrating a film processing apparatus according to the first embodiment
  • FIG. 2 is a reference diagram illustrating a separation apparatus including a reverse osmosis membrane included in the processing apparatus.
  • the white arrow in the figure indicates the traveling direction (conveying direction) of the film, and the arrow indicates the flow direction of each liquid.
  • the film processing apparatus is also a polarizing film manufacturing apparatus.
  • the film processing apparatus A includes a transport unit 9 that transports a long strip-shaped film B in the longitudinal direction, a plurality of baths having a solution, and a separation device 6 that separates an active ingredient from the solution.
  • the plurality of baths include, for example, a swelling bath 1, a dyeing bath 2, a crosslinking bath 3, a stretching bath 4, and an adjusting bath 5 in order from the front side (upstream side in the traveling direction of the film B).
  • the separation device 6 has a reverse osmosis membrane that takes a solution from at least one of the plurality of baths and separates an active ingredient from the solution.
  • the film B to be processed has a long strip shape.
  • the long belt shape refers to a rectangular shape whose length in the longitudinal direction is sufficiently larger than the length in the short direction (the short direction is a direction perpendicular to the long direction).
  • the length in the longitudinal direction of the long belt-like film B is, for example, 10 m or more, and preferably 50 m or more.
  • the film B is not particularly limited, but a hydrophilic polymer film is preferable because it is excellent in dyeability with iodine (easily dyed with iodine).
  • the hydrophilic polymer film is not particularly limited, and a conventionally known film can be used.
  • hydrophilic polymer film for example, polyvinyl alcohol (PVA) film, partially formalized PVA film, polyethylene terephthalate (PET) film, ethylene / vinyl acetate copolymer film, and partial saponification thereof.
  • PVA polyvinyl alcohol
  • PET polyethylene terephthalate
  • ethylene / vinyl acetate copolymer film ethylene / vinyl acetate copolymer film
  • partial saponification thereof A film etc.
  • polyene oriented films such as PVA dehydrated products and polyvinyl chloride dehydrochlorinated products, stretched and oriented polyvinylene films, and the like can also be used.
  • a PVA polymer film is preferable because it is particularly excellent in dyeability with iodine.
  • Examples of the raw material polymer for the PVA polymer film include a polymer saponified after polymerizing vinyl acetate, and a small amount of a copolymerizable monomer such as unsaturated carboxylic acid or unsaturated sulfonic acid with respect to vinyl acetate. And the like.
  • the degree of polymerization of the PVA polymer is not particularly limited, but is preferably 500 to 10,000, more preferably 1000 to 6000, from the viewpoint of solubility in water.
  • the saponification degree of the PVA polymer is preferably 75 mol% or more, more preferably 98 mol% to 100 mol%.
  • the thickness of the film B is not particularly limited, but is, for example, 15 ⁇ m to 110 ⁇ m, preferably 38 ⁇ m to 110 ⁇ m, and more preferably 50 ⁇ m to 100 ⁇ m.
  • the swelling bath 1 is provided to swell the film B.
  • the swelling bath 1 has a tank 11 and a solution 12 put in the tank 11.
  • the solution of the swelling bath 1 is referred to as “swelling liquid”.
  • the swelling bath may be omitted. In the illustrated example, only one swelling bath 1 is provided, but two or more swelling baths 1 may be provided in parallel in the traveling direction of the film B (not shown).
  • the swelling liquid for example, water can be used.
  • water obtained by adding an appropriate amount of glycerin and / or potassium iodide to water may be used as the swelling liquid.
  • the concentration is preferably 5% by weight or less
  • potassium iodide is added, the concentration is preferably 10% by weight or less.
  • the dyeing bath 2 is provided for dyeing the film B.
  • the dyeing bath 2 includes a tank 21 and a solution 22 placed in the tank.
  • the solution in the dyeing bath 2 is referred to as “dyeing solution”.
  • the dyeing solution is a solution for dyeing the film B, and a solution containing iodine as an active ingredient can be used.
  • a solution in which iodine is dissolved in a solvent can be used.
  • the solvent water is generally used, but an organic solvent compatible with water may be further added.
  • the concentration of iodine in the dyeing solution is not particularly limited, but is preferably 0.01% to 10% by weight, more preferably 0.02% to 7% by weight, and 0.025% by weight. More preferably, it is ⁇ 5% by weight. Furthermore, in order to further improve the dyeing efficiency, it is preferable to add an iodine compound to the dyeing solution.
  • the iodine compound is a compound containing elements other than iodine and iodine in the molecule.
  • Examples of the iodine compound include potassium iodide, lithium iodide, sodium iodide, zinc iodide, aluminum iodide, lead iodide, copper iodide, barium iodide, calcium iodide, tin iodide, and iodide.
  • Examples include titanium.
  • the concentration is preferably 0.01% by weight to 10% by weight, and more preferably 0.1% by weight to 5% by weight.
  • iodine When the staining solution contains iodine and an iodine compound, iodine may be the main component of the solution, or the iodine compound may be the main component of the solution.
  • a solution containing more iodine compound than iodine is used as the staining solution. That is, in this staining solution, iodine is an active component, but an iodine compound is the main component.
  • the main component means a component (excluding a solvent) that is contained most in the solution on a weight basis.
  • the crosslinking bath 3 is provided for crosslinking the film B on which the iodine is adsorbed.
  • the cross-linking bath 3 includes a tank 31 and a solution 32 placed in the tank 31.
  • the solution of the crosslinking bath 3 is referred to as “crosslinking solution”.
  • the crosslinking liquid is a solution for crosslinking the film B, and a solution containing a boron compound as an active ingredient can be used.
  • the crosslinking liquid a solution in which a boron compound is dissolved in a solvent can be used.
  • a solvent water is generally used, but an organic solvent compatible with water may be further added.
  • the boron compound include boric acid and borax. Among these, it is preferable to use boric acid.
  • the concentration of the boron compound in the crosslinking liquid is not particularly limited, but is preferably 1% by weight to 10% by weight, more preferably 2% by weight to 7% by weight, and 2% by weight to 6% by weight. Is more preferable.
  • an iodine compound is not particularly limited, and examples thereof include those exemplified in the staining solution. Of these, potassium iodide is preferred.
  • the concentration of the iodine compound is not particularly limited, but is preferably 0.05% by weight to 15% by weight, and more preferably 0.5% by weight to 8% by weight.
  • the ratio of the boron compound (preferably boric acid) and the iodine compound (preferably potassium iodide) is preferably in the range of 1: 0.1 to 1: 6 by weight.
  • the crosslinking liquid contains a boron compound and an iodine compound
  • the boron compound may be the main component of the solution
  • the iodine compound may be the main component of the solution.
  • the stretching bath 4 is provided to orient the film B that has adsorbed iodine and has been crosslinked.
  • the stretching bath 4 has a tank 41 and a solution 42 put in the tank 41.
  • the solution of the stretching bath 4 is referred to as “stretching solution”.
  • only one stretching bath 4 is provided, but two or more stretching baths 4 may be arranged in parallel in the traveling direction of the film B (not shown).
  • the stretching bath 4 can be omitted.
  • the stretching solution is not particularly limited, and for example, a solution containing a boron compound as an active ingredient can be used.
  • a solution in which a boron compound is dissolved in a solvent for example, a solution in which a boron compound is dissolved in a solvent, or a solution in which a boron compound and, if necessary, an iodine compound, various metal salts, a zinc compound, and the like are dissolved in a solvent can be used.
  • a solvent water is generally used, but an organic solvent compatible with water may be further added.
  • the boron compound include boric acid and borax, among which boric acid is preferably used.
  • the concentration of the boron compound in the drawing liquid is not particularly limited, but is preferably 1% by weight to 10% by weight, and more preferably 2% by weight to 7% by weight.
  • the stretching solution preferably contains an iodine compound.
  • the iodine compound is not particularly limited, and examples thereof include those exemplified in the staining solution. Of these, potassium iodide is preferred.
  • the concentration of the iodine compound in the stretching solution is not particularly limited, but is preferably 0.05% by weight to 15% by weight, and more preferably 0.5% by weight to 8% by weight.
  • the stretching solution contains a boron compound and an iodine compound
  • the boron compound may be the main component of the solution, or the iodine compound may be the main component of the solution.
  • a solution containing more iodine compound than boron compound is used as the stretching solution.
  • the adjustment bath 5 is provided to adjust the hue of the film B and to remove boron compounds and the like.
  • the adjustment bath 5 is a bath disposed on the rear side of the crosslinking bath having the crosslinking liquid (the crosslinking liquid is a solution containing a boron compound as an active ingredient).
  • the adjusting bath 5 is a bath disposed on the rear side of the stretching bath having the stretching solution (the stretching solution is a solution containing a boron compound as an active ingredient).
  • the film B taken out from the bath after being immersed in the crosslinking bath and / or the stretching bath is immersed.
  • the adjustment bath 5 includes a tank 51 and a solution 52 put in the tank 51.
  • the adjustment liquid is a solution for adjusting the hue of the film B, and a solution containing an iodine compound as an active ingredient can be used.
  • a solution in which an iodine compound is dissolved in a solvent can be used.
  • water is generally used, but an organic solvent compatible with water may be further added.
  • the iodine compound is not particularly limited, and examples thereof include those exemplified in the staining solution. Of these, potassium iodide is preferable.
  • the concentration of the iodine compound in the adjustment liquid is not particularly limited, but is preferably 0.5% by weight to 20% by weight, and more preferably 1% by weight to 15% by weight.
  • the adjustment bath 5 you may arrange
  • the cleaning section is provided to remove residual components such as iodine compounds and boron compounds remaining on the surface of the film B after passing through the adjustment bath 5. Water can be used as the cleaning liquid.
  • Concentrations of active ingredients of the swelling liquid, dyeing liquid, cross-linking liquid, stretching liquid, and adjusting liquid described in the columns of ⁇ swelling bath>, ⁇ dying bath>, ⁇ crosslinking bath>, ⁇ stretching bath>, and ⁇ regulating bath> Etc. are initial set values. As will be described later, when the processing apparatus is actually operated, the solution of the front bath is mixed into the solution of the rear bath and the active ingredient is impregnated into the film B. Note that it changes from time to time.
  • the separation device 6 is provided for separating and recovering the active ingredient from at least one solution selected from the respective baths.
  • the separation device 6 is provided in at least one of the baths.
  • the separation device 6 is provided in the adjustment bath 5.
  • the separation device 6 includes, for example, a transfer pump 612, a safety filter 632, a pressure pump 613, a reverse osmosis membrane 71, a mixer 671, a conductivity meter 652, and a return pipe 691.
  • the separation device 6 may have other members.
  • the adjustment bath 5 is provided with a water intake pump 611.
  • a part of the adjustment liquid 52 is taken out from the adjustment bath 5 by the intake pump 611.
  • a part of the solution taken out from the bath is referred to as “surplus liquid”, and in particular, a part of the adjustment liquid 52 taken out from the adjustment bath 5 is referred to as “surplus adjustment liquid”.
  • An auxiliary tank 621 is provided after the intake pump 611.
  • the auxiliary tank 621 is a tank that temporarily stores excess adjustment liquid.
  • a transfer pump 612 is provided after the auxiliary tank 621.
  • the auxiliary tank 621 is provided as necessary. When the auxiliary tank 621 is not provided, the transfer pump 612 takes out the excess adjustment liquid and sends it to the pressure pump 613.
  • a general-purpose filter 631 is provided to remove relatively large foreign matters that may be mixed in the excess adjustment liquid.
  • the safety filter 632 is provided to remove relatively small foreign matters in order to prevent the reverse osmosis membrane 71 from being clogged or damaged.
  • the safety filter 632 includes a filter element having an opening of about 1 ⁇ m.
  • the adsorption filter 633 containing activated carbon is provided for the purpose of removing organic substances.
  • the pressure pump 613 pressurizes the surplus adjustment liquid and sends it to the reverse osmosis membrane 71.
  • the pressure pump 613 is not particularly limited, and examples thereof include a centrifugal pump, a diffuser pump, a spiral mixed flow pump, a piston pump, a plunger pump, a diaphragm pump, a gear pump, a screw pump, a vane pump, a cascade pump, and a jet pump.
  • a reverse osmosis membrane 71 is provided after the pumping pump 613. Further, a flow meter 641 is provided between the pressure pump 613 and the reverse osmosis membrane 71.
  • a reverse osmosis membrane 71 that can separate the iodine compound and the boron compound contained in the excess adjustment liquid is used.
  • the reverse osmosis membrane 71 is not particularly limited as long as it can be separated as described above, and a conventionally known one can be used.
  • examples of the reverse osmosis membrane 71 include a spiral membrane element, a hollow fiber membrane element, a tubular membrane element, and a frame and plate membrane element.
  • the reverse osmosis membrane 71 one having one or a plurality of membrane elements can be used.
  • the plurality of membrane elements are usually connected in series.
  • the reverse osmosis membrane 71 may be single, and a plurality of reverse osmosis membranes 71 may be connected in series or in parallel.
  • the material which comprises a membrane element is not specifically limited, For example, various polymer materials, such as a cellulose acetate, polyvinyl alcohol, polyamide, polyester, can be used.
  • a commercially available product may be used as the reverse osmosis membrane 71. Examples of commercially available products that can be used in the present invention include the product name “LFC3LD” manufactured by Nitto Denko Corporation and the product name “ESPA4-7” manufactured by Nitto Denko Corporation.
  • the surplus adjustment liquid is separated into a permeate containing a boron compound and a concentrate containing an iodine compound.
  • a flow meter 642 and a conductivity meter 651 are provided on the permeate side of the reverse osmosis membrane 71 as necessary, and a storage tank 622 for containing the permeate is further provided as necessary.
  • the conductivity meter 651 measures the conductivity of the permeate.
  • a flow rate adjusting unit 661 for example, a valve
  • a flow meter 643 are provided as necessary.
  • the mixer 671 and the conductivity meter 652 are provided after that, and the storage tank 623 is provided as needed after that.
  • a diluting unit 662 for introducing a diluting solution into the concentrated solution is provided in front of the mixer 671.
  • a return pipe 691 having a transfer pump 614 is connected to the storage tank 623, and the tip of the return pipe 691 is opened to the adjustment bath 5.
  • the film treatment includes a step of conveying the film in the longitudinal direction, a swelling step of swelling the film, a dyeing step of dyeing the film, a crosslinking step of crosslinking the film, a stretching step of stretching the film, and a hue of the film. It has an adjustment process to adjust. You may have another process as needed. In at least one step selected from these steps, the active ingredient is separated from the solution, recovered, returned and used again. That is, the active ingredient in the solution is circulated and used. These steps are performed using the film processing apparatus A.
  • the long band-like film B is guided to the swelling bath 1 by the transport unit 9 and immersed in the swelling liquid 12.
  • the temperature of the swelling liquid is, for example, 20 ° C. to 45 ° C.
  • the immersion time in the swelling liquid is, for example, 20 seconds to 300 seconds.
  • the film B drawn out from the swelling bath 1 is introduced into the dyeing bath 2 and immersed in the dyeing solution 22.
  • the temperature of the staining liquid is, for example, 10 ° C.
  • the film B drawn out from the dyeing bath 2 is introduced into the crosslinking bath 3 and immersed in the crosslinking solution 32.
  • the temperature of the crosslinking liquid is, for example, 20 ° C. to 70 ° C.
  • the immersion time in the crosslinking liquid is, for example, 5 seconds to 400 seconds.
  • the film B drawn from the crosslinking bath 3 is introduced into the stretching bath 4 and subjected to stretching treatment.
  • the stretching ratio is, for example, 2 to 6.5 times as the total stretching ratio with respect to the original length of the film B.
  • Stretching can be performed in the dyeing step and the crosslinking step, and when stretching is performed in these steps, the stretching ratio in the stretching step is determined by taking into account the stretching ratio in these steps, and total stretching.
  • the magnification is set to be 2 to 6.5 times.
  • crosslinking process you may abbreviate
  • the stretched film B is introduced into the adjustment bath 5 and immersed in the adjustment liquid 52.
  • the temperature of the adjustment liquid is, for example, 15 ° C. to 40 ° C., and the immersion time in the adjustment liquid is 2 seconds to 20 seconds.
  • the film B drawn out from the adjustment bath 5 is washed as necessary and dried, and then wound into a roll.
  • a polarizing film is obtained through such treatment.
  • a polarizing plate is obtained by laminating a protective film on at least one surface of the obtained polarizing film.
  • the solution in the front bath front processing bath
  • the rear bath rear processing bath
  • the concentration of the solution in the rear treatment bath changes from the initial set value.
  • the crosslinking bath 3 since the dyeing solution containing iodine in the dyeing bath 2 is mixed in the crosslinking solution, the crosslinking solution is relatively lowered from the initially set concentration of the boron compound. Further, since the film B is impregnated with the boron compound in the crosslinking bath 3, the crosslinking solution is relatively lowered from the initial set concentration of the boron compound.
  • the adjustment liquid is obtained from the initially set concentration of the iodine compound. Relatively decreases. Furthermore, since the iodine compound impregnates the film B in the adjustment bath 5, the adjustment liquid is relatively lowered from the initially set concentration of the iodine compound. In order to correct such a change in the concentration of the solution in each bath, the solution in each bath is taken out as an excess liquid and a new solution containing an active ingredient is replenished.
  • the separation device 6 separates the active ingredient from the surplus liquid with the reverse osmosis membrane 71, collects it, and reuses it.
  • step (X) of immersing the film in a bath containing a solution containing a boron compound and an iodine compound a part of the solution is taken out from the bath, and the solution contains a boron compound using a reverse osmosis membrane. Separate into solution and solution containing iodine compound.
  • the swelling process, the dyeing process, the crosslinking process, the stretching process, and the adjusting process for example, the adjusting process is continuously performed after the crosslinking process or the stretching process.
  • the adjustment step is an adjustment in which a film taken out by dipping in a cross-linking solution containing a boron compound as an active ingredient or a film taken out by dipping in the cross-linking bath and the stretching bath in turn is taken as an active ingredient. It is a step of immersing in an adjustment bath having a liquid. This adjustment step corresponds to step (X) in the present specification.
  • ⁇ Separation process> As shown in FIG. 2, in the separation device 6 of the film processing apparatus A, a part of the adjustment liquid is taken out through the water intake pump 611 as an excess liquid (excess adjustment liquid).
  • the surplus liquid (surplus adjustment liquid) does not mean an excess liquid, but refers to a solution that is partially removed from the bath for separation treatment.
  • the surplus adjustment liquid is not limited to one that is directly extracted from the adjustment bath 5, and may contain a liquid that overflows from the adjustment bath 5.
  • the surplus adjustment liquid is taken out from the adjustment bath 5 at a flow rate that does not interfere with the film processing in the adjustment bath 5.
  • the surplus adjustment liquid is a solution mainly containing a boron compound (preferably boric acid) and an iodine compound (preferably potassium iodide) contained in the crosslinking liquid and / or the stretching liquid.
  • the surplus adjustment liquid contains an iodine compound as a main component.
  • the taken out excess adjustment liquid is temporarily stored in the auxiliary tank 621 as necessary.
  • the excess adjustment liquid is generally neutral (around pH 7). If the excess adjustment liquid is alkaline, it is preferable to mix the neutralization agent or the like to change the excess adjustment liquid to neutral or acidic.
  • boron compounds such as boric acid may be ionized, and the boron compound and iodine compound may not be well separated by the reverse osmosis membrane 71 described later.
  • the surplus adjustment liquid is sent through the transfer pump 612, and the surplus adjustment liquid is passed through the general-purpose filter 631, the safety filter 632, and the adsorption filter 633.
  • the surplus adjustment liquid that has passed through each filter is pressed into the reverse osmosis membrane 71 through the pressure pump 613.
  • the discharge pressure of the pressure pump 613 is appropriately set according to the performance of the reverse osmosis membrane 71 and the like, and is, for example, about 1 MPa to 10 MPa.
  • the amount of excess adjustment liquid entering the reverse osmosis membrane 71 from the pressure pump 613 is measured by the flow meter 641. In the reverse osmosis membrane 71, the excess adjustment liquid is separated into a concentrated liquid and a permeated liquid.
  • the concentrate has a reduced concentration of boron compound and contains iodine compound as an active ingredient at a high concentration. Further, the permeate contains substantially no iodine compound and contains a boron compound at a high concentration as an active ingredient. For example, the permeate contains 60% to 90%, preferably 70% to 90% of the boron compound when the weight of the boron compound contained in the surplus adjustment liquid before entering the reverse osmosis membrane 71 is 100%. Including.
  • the permeated liquid that has permeated through the reverse osmosis membrane 71 passes through the flow meter 642 and the conductivity meter 651, is once put in the storage tank 622, and then discarded. In addition, the permeate may be discarded directly without entering the storage tank 622.
  • the conductivity meter 651 arranged on the permeate side shows a substantially constant value during implementation. When the value of the conductivity meter increases, the membrane element of the reverse osmosis membrane 71 may be damaged or the performance may be deteriorated. When the reverse osmosis membrane 71 is damaged, an iodine compound such as ionized potassium iodide is excessively mixed into the permeate.
  • the conductivity meter 651 disposed on the permeate side has a function of indicating the maintenance time of the reverse osmosis membrane 71.
  • the flow meter 642 measures the flow rate of the permeate.
  • the opening degree of the flow rate adjusting unit 661 is controlled through a control device (not shown) so that the value of the flow meter 642 maintains the set value.
  • the flow rate of the concentrate separated by the reverse osmosis membrane 71 is measured by a flow meter 643 disposed after the flow rate adjusting unit 661.
  • the discharge amount of the pressure pump 613 is controlled through a control device (not shown) so that the value of the flow meter maintains the set value.
  • the concentrated solution obtained from the reverse osmosis membrane 71 may be directly replenished to the adjustment bath 5, but it is usually preferable to adjust the concentration before replenishing it.
  • a diluent is introduced in the middle of returning the concentrate from the reverse osmosis membrane 71 to the adjustment bath 5 to adjust the concentration of the iodine compound that is the active ingredient of the concentrate.
  • the concentration of the iodine compound in the concentrated liquid obtained from the reverse osmosis membrane 71 is usually larger than the concentration of the iodine compound in the excess adjustment liquid. For this reason, by diluting with a diluting solution, the concentration of the concentrated solution is adjusted to the same concentration as the adjusting solution in the adjusting bath or a reference concentration for replenishment.
  • the diluting liquid it is preferable to use the same solvent as that of the adjusting liquid, and examples thereof include water or water to which an organic solvent compatible with water is added.
  • a concentrated solution diluted with the diluted solution (hereinafter, a concentrated solution whose concentration has been adjusted is referred to as a first replenisher solution) is mixed in a mixer 671 to make the concentration uniform.
  • the conductivity of the first replenisher mixed in the mixer 671 is measured by a conductivity meter 652.
  • This conductivity meter 652 is for monitoring whether or not the concentration of the iodine compound that is the active ingredient of the first replenisher is as set, and in accordance with the change in the value of the conductivity meter 652, the diluted solution Is introduced by the control device.
  • the conductivity meter value 652 when the conductivity meter value 652 is larger than the set value, control is performed to increase the amount of diluent introduced, and when the value is lower than the set value, control to reduce the amount of diluent introduced.
  • the first replenisher adjusted to the set concentration is placed in the storage tank 623 as necessary, drawn out by the transfer pump 614, and replenished to the adjustment bath 5 through the return pipe 691. Once the first replenisher is placed in the storage tank 623, a replenisher without concentration spots is obtained. However, the first replenisher adjusted to the set concentration may be directly replenished to the adjustment bath 5.
  • the present invention uses a reverse osmosis membrane to separate active components from excess liquid and reuse them in film processing.
  • the reverse osmosis membrane By using the reverse osmosis membrane, the separation and reuse of the surplus liquid can be performed in series according to the film processing. That is, according to the present invention, while the film is processed in each bath, the surplus liquid is removed from the bath, the active ingredient is separated, and the active ingredient is adjusted to a concentration suitable for each bath. And it can be refilled in the bath.
  • the installation location can be made relatively small, and further, running costs such as power costs can be kept low. In particular, since potassium iodide is relatively expensive, the running cost can be further reduced by reusing and circulating an iodine compound such as potassium iodide as in this embodiment.
  • the surplus liquid is taken out from the adjustment liquid as a solution containing a boron compound and an iodine compound.
  • the present invention is not limited to this.
  • the stretching liquid contains a boron compound and an iodine compound
  • the surplus liquid is removed.
  • the liquid may be separated into a permeate and a concentrated liquid with a reverse osmosis membrane and reused.
  • the first replenisher obtained in the separation device is replenished to the adjustment bath, but instead of or in combination with this, it is used for other baths. It is good (not shown).
  • the first replenisher containing the iodine compound separated from the surplus adjusting solution is used in these baths. Also good.
  • the permeate containing substantially a boron compound is discarded, but this may be used for other baths.
  • a solution containing a boron compound is used in a crosslinking bath, a stretching bath, or the like, but a permeate containing a boron compound separated from an excess adjustment solution may be used in these baths.
  • the permeate obtained from the reverse osmosis membrane may be used directly in the bath.
  • concentration of the boron compound, which is the active ingredient of the permeate is usually high, use it after adjusting the concentration. Is preferred.
  • the following second embodiment can be used as appropriate.
  • the film treatment of the second embodiment has a step (Y) of immersing the film in a bath having a solution containing a boron compound and iodine, taking out a part of the solution from the bath, and using the solution as a reverse osmosis membrane. And separating into a solution containing a boron compound and a solution containing iodine.
  • This step (Y) is, for example, a step of immersing a film taken out by immersion in a bath having a solution containing iodine as an active ingredient in a bath having a solution containing a boron compound as an active ingredient.
  • the second embodiment will be described. In the description, the configuration different from the first embodiment will be mainly described, and the description of the same configuration may be omitted.
  • FIG. 3 is a reference view showing a film processing apparatus of the second embodiment
  • FIG. 4 is a reference view showing a separation apparatus including a reverse osmosis membrane, which the processing apparatus comprises.
  • the film processing apparatus A of the second embodiment also separates the active ingredient from the solution, a transport unit 9 that transports the long strip-shaped film B in the longitudinal direction, a plurality of baths having the solution, and the solution.
  • the separation device 6 is provided for separating and recovering the active ingredient from at least one solution selected from the respective baths.
  • the separation device 6 is provided in the crosslinking bath 3.
  • the configuration of the separation device 6 up to the reverse osmosis membrane 71 is substantially the same as in the first embodiment. That is, a water intake pump 611, a storage tank 621, a transfer pump 612, filters 631, 632, 633, a pressure pump 613, and a flow meter 641 are provided between the crosslinking bath 3 and the reverse osmosis membrane 71.
  • the functions of these members are as described in the first embodiment, and some of these members may be omitted as necessary.
  • the reverse osmosis membrane 71 can use the same thing as 1st Embodiment.
  • a flow meter 642, a conductivity meter 651, and a storage tank 622 are provided on the permeate side of the reverse osmosis membrane 71, as in the first embodiment.
  • a return path for returning the permeate to the crosslinking bath 3 or the like is provided.
  • the storage tank 622 that stores the permeate is provided with a concentration meter 681 that measures the concentration of the boron compound.
  • the densitometer 681 for example, a densitometer that measures boric acid concentration can be used.
  • boric acid concentration meter for example, a boric acid concentration constant monitoring meter (model “SRM-1DB” manufactured by Ceres Co., Ltd.) can be used.
  • the storage tank 622 is provided with a transfer pump 615, followed by a concentration adjusting unit 663 and a mixer 672 for adjusting the concentration of the boron compound.
  • a storage tank 624 is provided after the mixer 672 as necessary.
  • a return pipe 692 including a transfer pump 616 is connected to the storage tank 624, and the tip of the return pipe 692 is opened to the bridging bath 3.
  • a flow rate adjustment unit 661 and a flow meter 643 are provided on the concentrated liquid side of the reverse osmosis membrane 71 as necessary, similarly to the first embodiment. Further, a storage tank 625 is provided thereafter as necessary. A return pipe 693 having a transfer pump 617 is connected to the storage tank 625, and the tip of the return pipe 693 is opened to the dyeing bath 2.
  • the film treatment is performed in the same manner as in the first embodiment, in which the film is conveyed in the longitudinal direction, the swelling process for swelling the film, the dyeing process for dyeing the film, the crosslinking process for crosslinking the film, and the film stretching.
  • the active ingredient is separated from the solution, recovered, returned and used again. That is, the active ingredient in the solution is circulated and used.
  • each process such as the swelling process is the same as in the first embodiment.
  • the solution in the step (Y) of immersing the film in a bath having a solution containing a boron compound and iodine, the solution is separated into a solution containing the boron compound and a solution containing iodine using a reverse osmosis membrane.
  • the swelling process the dyeing process, the crosslinking process, the stretching process, and the adjusting process, for example, the crosslinking process is continuously performed after the dyeing process.
  • the cross-linking step is a step of immersing the film taken out by dipping in a dyeing solution containing iodine as an active ingredient in a cross-linking bath having a cross-linking solution containing a boron compound as an active ingredient.
  • This crosslinking step corresponds to step (Y) in the present specification.
  • ⁇ Separation process> As shown in FIG. 4, in the separation device 6 of the film processing apparatus A, a part of the crosslinking liquid is taken out as an excess liquid (excess crosslinking liquid) through a water intake pump 611.
  • the surplus crosslinking liquid is not limited to one that is directly extracted from the crosslinking bath 3, and may contain a liquid that overflows from the crosslinking bath 3.
  • the surplus crosslinking liquid is taken out from the crosslinking bath 3 at a flow rate that does not hinder the film processing in the crosslinking bath 3.
  • the surplus crosslinking liquid is mainly composed of iodine and iodine compound (preferably potassium iodide) contained in the dyeing liquid, and boron compound (preferably boric acid) and iodine compound (preferably potassium iodide) contained in the crosslinking liquid. ). That is, the surplus crosslinking liquid is a solution containing iodine, a boron compound, and an iodine compound. Usually, the surplus crosslinking liquid contains a boron compound as a main component. However, depending on the composition of the cross-linking liquid, the surplus cross-linking liquid may contain an iodine compound as a main component. The removed excess crosslinking liquid is temporarily stored in the auxiliary tank 621 as necessary.
  • iodine and iodine compound preferably potassium iodide
  • boron compound preferably boric acid
  • iodine compound preferably potassium iodide
  • the surplus cross-linking liquid is generally neutral (about pH 7). If the surplus crosslinking liquid is alkaline, it is preferable to mix the neutralizing agent or the like to change the surplus crosslinking liquid to neutral or acidic.
  • the surplus cross-linking liquid is sent through the transfer pump 612, the surplus cross-linking liquid is passed through the general-purpose filter 631, the safety filter 632, and the adsorption filter 633, and is press-fitted into the reverse osmosis membrane 71 through the pressure feed pump 613.
  • the amount of surplus crosslinking liquid entering the reverse osmosis membrane 71 from the pressure pump 613 is measured by a flow meter 641.
  • the surplus crosslinking liquid is separated into a concentrated liquid and a permeated liquid.
  • the concentrate has a reduced concentration of boron compound and contains iodine and iodine compound in high concentration as active ingredients.
  • the permeate does not substantially contain iodine and an iodine compound, and contains a boron compound at a high concentration as an active ingredient.
  • the permeate contains 60% to 90%, preferably 70% to 90%, of the boron compound when the weight of the boron compound contained in the surplus crosslinking liquid before entering the reverse osmosis membrane 71 is 100%. Including.
  • the permeate may be replenished directly to the crosslinking bath 3, but it is usually preferable to adjust the concentration before replenishing it.
  • concentration of the boron compound that is the active component of the permeate is adjusted.
  • the permeated liquid that has permeated through the reverse osmosis membrane 71 passes through the flow meter 642 and the conductivity meter 651 and is once put into the storage tank 622.
  • the concentration of the boron compound in the permeate placed in the storage tank 622 is constantly measured with a densitometer 681.
  • the concentration adjusting unit 663 adjusts the concentration of the boron compound in the permeate while the permeate is being sent from the tank 622 through the transfer pump 615. For example, when the boron compound concentration measured by the densitometer 681 is smaller than the set concentration (the boron compound concentration of the crosslinking liquid in the crosslinking bath 3), the boron compound is introduced into the permeate by the concentration adjusting unit 663. And increase its concentration. When the boron compound concentration measured by the densitometer 681 is larger than the set concentration, the concentration adjusting unit 663 introduces a diluent such as water into the permeate and lowers the concentration.
  • a permeated liquid after concentration adjustment (hereinafter, the permeated liquid whose concentration has been adjusted is referred to as a second replenisher) is mixed in a mixer 672 and stored in a storage tank 624 as necessary. Thereafter, the second replenisher is drawn out by the transfer pump 616 and replenished to the crosslinking bath 3 through the return pipe 692.
  • the concentrated liquid obtained from the reverse osmosis membrane 71 mainly contains iodine and an iodine compound. After adjusting the concentration of iodine in this concentrated solution, it may be replenished to the dyeing bath 2, but in the illustrated example, the concentrated solution is directly replenished to the dyeing bath 2.
  • the flow rate of the concentrated liquid separated by the reverse osmosis membrane 71 is measured by the flow meter 643 as in the first embodiment, and the opening degree of the flow rate adjustment unit 661 and the pressure pump are controlled by the control device.
  • the discharge amount 613 is controlled.
  • the concentrated liquid is put in the storage tank 625 as necessary, drawn out by the transfer pump 617, and replenished to the dyeing bath 2 through the return pipe 693.
  • the iodine concentration of the staining solution may change from the set concentration.
  • a diluted solution such as water is added to the staining bath 2. Introduce and reduce its concentration.
  • iodine including potassium iodide for dissolving iodine, if necessary
  • concentration is determined. Increase.
  • a solution containing iodine and a boron compound can be separated into a solution containing iodine and a solution containing a boron compound, and these can be reused.
  • the surplus liquid is taken out from the cross-linking liquid as a solution containing iodine and a boron compound.
  • the present invention is not limited to this.
  • the stretching liquid contains iodine and a boron compound
  • a reverse osmosis membrane may be separated into a permeate and a concentrated solution and reused.
  • the second replenisher (concentration-adjusted permeate containing a boron compound) obtained in the separation device (separation step) is replenished to the crosslinking bath. It may be used in combination with other baths (not shown). For example, as described above, when a solution containing a boron compound is used in a stretching bath or the like, the second replenisher may be replenished to the bath.
  • the concentration of the permeate containing the boron compound is adjusted and replenished to the crosslinking bath 3 or the like.
  • the concentration may not be adjusted in advance and the permeate may be replenished to the cross-linking bath 3 or the like. Good.
  • the concentration of the boron compound in the crosslinking solution or the like may change from the set concentration. Therefore, it is preferable to adjust the concentration in the crosslinking bath 3 or the like.
  • the concentration of the boron compound in the crosslinking solution in the crosslinking bath 3 is constantly measured by a technique such as titration, and the measured concentration of the boron compound in the crosslinking solution is greater than the set concentration, a diluted solution such as water is added to the crosslinking bath.
  • a boron concentration of the dyeing solution measured is smaller than the set concentration, a boron compound is introduced into the crosslinking bath 3.
  • a film processing apparatus B film 1 swelling bath 2 dyeing bath 3 crosslinking bath 4 stretching bath 5 adjustment bath 6 separation device 71 reverse osmosis membrane

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PCT/JP2017/024939 2016-08-02 2017-07-07 フィルムの処理方法、及び偏光フィルムの製造方法 WO2018025583A1 (ja)

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JP7340325B2 (ja) * 2018-09-14 2023-09-07 住友化学株式会社 偏光フィルムの製造方法及び偏光フィルムの製造装置
JP7490500B2 (ja) 2019-09-12 2024-05-27 住友化学株式会社 ポリビニルアルコール除去装置及び偏光子の製造方法
JP2023175387A (ja) 2022-05-30 2023-12-12 住友化学株式会社 偏光フィルムの製造装置及び製造方法

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JP7117698B2 (ja) 2018-11-20 2022-08-15 伊勢化学工業株式会社 無機化合物含有水溶液の製造方法

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