CN112711087A - Method and apparatus for producing polarizing film - Google Patents
Method and apparatus for producing polarizing film Download PDFInfo
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- CN112711087A CN112711087A CN202011151981.1A CN202011151981A CN112711087A CN 112711087 A CN112711087 A CN 112711087A CN 202011151981 A CN202011151981 A CN 202011151981A CN 112711087 A CN112711087 A CN 112711087A
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- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
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- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- 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
- 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
- G02B5/3041—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 comprising multiple thin layers, e.g. multilayer stacks
- G02B5/305—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 comprising multiple thin layers, e.g. multilayer stacks including organic materials, e.g. polymeric layers
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Polarising Elements (AREA)
Abstract
The invention provides a method and an apparatus for manufacturing a polarizing film, which can manufacture a polarizing film while keeping a processing solution for processing a precursor of the polarizing film in a sufficiently clean state. A method for manufacturing a polarizing film, comprising: a precursor treatment step of treating a precursor of the polarizing film with the 1 st solution; and an electrolytic treatment step of bringing the 1 st solution after the treatment of the polarizing film precursor into contact with an electrode group to perform a deposition treatment, thereby forming a 2 nd solution, wherein the polarizing film production method further comprises at least one of a first pH adjustment step of adjusting the pH of the 1 st solution after the treatment of the polarizing film precursor and a second pH adjustment step of adjusting the pH of the 2 nd solution.
Description
Technical Field
The present invention relates to a method for producing a polarizing film, and further relates to an apparatus for producing a polarizing film.
Background
Patent document 1 proposes a method for producing a polarizing film, in which a polarizing film is produced by subjecting a treatment solution after treating a precursor of the polarizing film to electrolytic treatment while keeping the treatment solution clean.
Documents of the prior art
Patent document
Patent document 1: japanese patent laid-open publication No. 2019-053294
Disclosure of Invention
Problems to be solved by the invention
In the process of processing the precursor of the polarizing film, the precursor of the polarizing film becomes relatively easily broken after the stretching treatment is performed, and pieces (japanese: broken pieces) that come off when the precursor passes through the dyeing bath are sometimes scattered into the processing solution. Since such fragments may cause defects in the film surface of the obtained polarizing film, it is very important to remove the fragments in the treatment solution and maintain the treatment solution in a clean state. In the production method described in patent document 1, metal ions and the like eluted from the electrode used in the electrolytic treatment may remain in the treatment solution, and thus the treatment solution may not be sufficiently kept clean.
In addition, in the step of treating the polarizing film precursor with the iodine-containing solution, the iodine-containing solution may increase the triiodide ion concentration by air oxidation. When the triiodide ion concentration is increased, the amount of the iodine-polyvinyl alcohol complex formed when the triiodide ion is adsorbed to the polyvinyl alcohol resin film is increased, and as a result, the transmittance of the polarizing film may be decreased. Further, potassium sulfite may be added to reduce the triiodide ion concentration, but if sulfate is present in the polarizing film, it is undesirable from the viewpoint of durability.
The purpose of the present invention is to provide a method and an apparatus for producing a polarizing film, which can produce a polarizing film while maintaining a sufficiently clean state of a treatment solution for treating a precursor of the polarizing film.
Another object of the present invention is to provide a method for producing a polarizing film, which can reduce the concentration of triiodide ions in an iodine-containing solution used in a process for treating a precursor of the polarizing film.
Means for solving the problems
[1] A method for manufacturing a polarizing film, comprising:
a precursor treatment step of treating a precursor of the polarizing film with the 1 st solution; and
an electrolytic treatment step of forming a 2 nd solution by bringing the 1 st solution after the treatment of the polarizing film precursor into contact with an electrode group to perform a deposition treatment,
the method for producing a polarizing film further comprises at least one of a first pH adjustment step of adjusting the pH of the 1 st solution after the polarizing film precursor is treated, and a second pH adjustment step of adjusting the pH of the 2 nd solution.
[2]According to [1]The method for producing a polarizing film, wherein the 1 st solution contains iodine (I) for dyeing a precursor of the polarizing film2) And (3) solution.
[3] The method for producing a polarizing film according to [1] or [2], further comprising an aeration-precipitation step of separating the 2 nd solution into a 3 rd solution and a precipitate by subjecting the 2 nd solution to aeration-precipitation treatment.
[4] The method for producing a polarizing film according to any one of [1] to [3], further comprising a filtration step of subjecting the 3 rd solution to a filtration treatment.
[5] The method for producing a polarizing film according to [3] or [4], further comprising a step of adjusting an iodine concentration of at least one of the 2 nd solution and the 3 rd solution.
[6] The method for producing a polarizing film according to any one of [3] to [5], further comprising a step of analyzing a metal concentration in at least one of the 2 nd solution and the 3 rd solution.
[7] A polarizing film manufacturing apparatus includes:
a1 st solution processing tank for receiving the 1 st solution for processing the precursor of the polarizing film, and an electrode group for forming a 2 nd solution by contacting the 1 st solution after processing the precursor of the polarizing film,
the polarizing film manufacturing apparatus further comprises at least one of a mechanism for adding a pH adjusting agent to the 1 st solution after the polarizing film precursor is treated, and a mechanism for adding a pH adjusting agent to the 2 nd solution.
[8] The polarizing film production apparatus according to [7], further comprising an aeration-sedimentation tank for storing the 2 nd solution and separating the solution into a 3 rd solution and sediment.
[9]According to [8]The polarizing film production apparatus further comprises a container for the No. 3 solution, and iodine (I) is added2) The iodine concentration adjusting tank of the mechanism (2).
[10] The polarizing film production apparatus according to any one of [7] to [9], which is provided with a metal concentration analyzer.
[11] A method for producing a polarizing film, which comprises adsorbing iodine to a polyvinyl alcohol resin film to produce a polarizing film,
the method for producing the polarizing film comprises a step of bringing an electrode assembly into contact with an iodine-containing solution,
the anode of the electrode assembly contains iron.
[12] The method for producing a polarizing film according to [11], wherein the step of bringing the electrode assembly into contact with the iodine-containing solution is performed through a crosslinking step.
[13] A method for producing a polarizing film, which comprises adsorbing iodine to a polyvinyl alcohol resin film to produce a polarizing film,
the method for manufacturing the polarizing film includes:
a step of bringing an electrode group into contact with an iodine-containing solution; and
and measuring the concentration of triiodide ions in the iodine-containing solution after the electrode group is contacted.
Effects of the invention
According to the present invention, it is possible to provide a method and an apparatus for producing a polarizing film, which can produce a polarizing film while sufficiently maintaining a clean state of a treatment solution for treating a precursor of the polarizing film.
Drawings
Fig. 1 is a diagram schematically showing an example of a precursor processing section in a polarizing film manufacturing apparatus.
Fig. 2 is a schematic view showing an example of an electrolytic processing section in the polarizing film manufacturing apparatus.
Fig. 3 is a schematic view showing an example of a precipitation tank in the polarizing film manufacturing apparatus.
Fig. 4 is a diagram schematically showing an example of an overflow device of a precipitation tank in a polarizing film manufacturing apparatus.
Description of the reference numerals
12 pay-off roll, 14 swelling bath, 16 dyeing bath, 18 crosslinking bath, 20 washing bath, 21 drying furnace, 22 take-up roll, 30 overflow device, 31 drain plate, 32 tank part, 37, 137 circulation system, 101 1 st solution treatment bath, 103 st 1 path, 105 precipitation bath, 107 nd 2 path, 109 filtration device, 111 th 7 path, 116A st 1 groove part, 116B nd 2 groove part, 118 filtration membrane, 120 guide roll, 130, 133 path, 140 aeration precipitation bath, 141 rd 3 path, 142pH regulator layer, 143 th 4 path, 144 metal concentration analysis device, 145 th 5 path, 146 iodine concentration regulation bath, iodine solution bath, 148 th 6 path, precursor of 200 polarizing film, 200' electrode group, polarizing film 318 filtration member, E1 st 1 electrode element, E2 nd 2 electrode element, L1 th 1 solution, L2 nd 2 solution, L3 rd 3 solution, L4 pH regulator, L5 iodine solution, P1 fragment 1, and P2 fragment 2.
Detailed Description
Hereinafter, embodiments of the present invention will be described with reference to the drawings, but the present invention is not limited to the embodiments below. In all the following drawings, the scale of each component shown in the drawings is appropriately adjusted to facilitate understanding of the components, and the scale may not coincide with the scale of the actual component.
< method for producing polarizing film >
(first embodiment)
The method for manufacturing a polarizing film according to the first embodiment of the present invention includes: a precursor treatment step of treating a precursor of the polarizing film with the 1 st solution; and a method for producing a polarizing film (hereinafter, also referred to as a first production method) comprising an electrolytic treatment step of forming a 2 nd solution by bringing the 1 st solution after treating a precursor of the polarizing film into contact with an electrode group to carry out a deposition treatment.
The first manufacturing method further includes at least one of a first pH adjustment step of adjusting the pH of the 1 st solution after the polarizing film precursor is treated, and a second pH adjustment step of adjusting the pH of the 2 nd solution.
[ precursor treatment Process ]
The precursor treatment step is a step of treating a precursor of a polarizing film (hereinafter, also simply referred to as a precursor) with the 1 st solution. The precursor treatment process may include, for example: a dyeing step of immersing the precursor in a dyeing bath to dye the precursor; and a crosslinking step of immersing the precursor after the dyeing step in a crosslinking tank containing a treatment liquid containing a crosslinking agent to perform crosslinking treatment. The 1 st solution may be a chemical solution used in a dyeing bath for dyeing a precursor of a polarizing film, for example, an aqueous solution containing iodine or dissociated iodide ions, or a solution used in a crosslinking bath for crosslinking treatment, for example, a solution containing boric acid, potassium iodide, zinc iodide, or a combination thereof. The dyeing liquid may be a dyeing liquid using a dye, or a dyeing liquid containing an azo dye as a dichroic dye.
The precursor treatment step may further include other steps than those described above. The concrete examples are: a swelling step of immersing the precursor before the dyeing step in a swelling tank containing a treatment liquid containing water; a cleaning step of immersing the precursor after the crosslinking step in a cleaning tank; and a drying step after the cleaning step. The precursor may be uniaxially stretched in any 1 or more stages of the precursor treatment step, more specifically, in any 1 or more stages of the stretching step from the swelling step to the crosslinking step, and preferably in any 1 or more stages of the stretching step from the dyeing step.
(polarizing film precursor)
The material of the precursor of the polarizing film contains polyvinyl alcohol (PVA) or other suitable material. The polarizing film precursor may be, for example, a polyvinyl alcohol resin film. The polyvinyl alcohol resin film may be in a long form. Polyvinyl alcohol can be formed by saponifying polyvinyl acetate. According to several embodiments, the polyvinyl acetate may be a homopolymer of vinyl acetate or a copolymer of vinyl acetate and another monomer, which may be an unsaturated carboxylic acid, an olefin, an unsaturated sulfonic acid, a vinyl ether, or the like.
In some embodiments, the polyvinyl alcohol is modified, for example, polyvinyl formal, polyvinyl acetal, or polyvinyl butyral, which is modified with aldehydes. In several embodiments, the thickness of the precursor of the polarizing film is about 15 μm or more and 100 μm or less.
(swelling step)
The swelling step may be a step of performing a treatment in which the precursor is immersed in a swelling tank containing a treatment liquid containing water. The swelling step can remove foreign matters on the surface of the precursor, plasticizers in the precursor, and the like, and is useful for the subsequent dyeing treatment and crosslinking treatment.
(dyeing step)
The dyeing step may be a step of performing a treatment in which the precursor is immersed in a dyeing bath containing a treatment liquid containing a dyeing agent. As the coloring agent, a dichroic dye or other suitable water-soluble dichroic dye can be used. In order to further enhance the effect of the dyeing treatment, the treatment liquid used in the dyeing bath may contain other additives such as boric acid.
In several embodiments, the stain may contain iodine (I)2) And potassium iodide. The treatment liquid used in the dyeing bath may be iodine (I) containing for dyeing a precursor of the polarizing film2) And (3) solution. The treatment liquid used in the dyeing bath may be an aqueous solution containing, for example, 0.003 to 0.3 parts by mass of iodine and 0.1 to 10 parts by mass of potassium iodide per 100 parts by mass of water. The temperature of the dyeing treatment may be, for example, 10 to 50 ℃, and the time of the dyeing treatment may be, for example, 10 to 600 seconds. The treatment liquid in the dyeing bath may contain, for example, precipitates based on polyvinyl alcohol or precipitates of a precursor of a polarizing film, and the precipitates may contain, for example, insoluble debris generated by the action of dissolved polyvinyl alcohol and boric acid.
(crosslinking step)
The crosslinking step may be a step of performing a treatment of immersing the precursor after the dyeing step in a crosslinking tank containing a treatment liquid containing a crosslinking agent. Boric acid may be used as the crosslinking agent. The treatment liquid used in the crosslinking bath may further contain an optical modifier. When the concentration of the optical adjusting agent is changed, the hue of the polarizing film can be adjusted. The optical modifier may use potassium iodide, zinc iodide, or a combination thereof.
The treatment liquid used in the crosslinking tank may be an aqueous solution containing 0.3 to 10 parts by mass of boric acid and 1 to 30 parts by mass of potassium iodide per 100 parts by mass of water, for example. The temperature of the crosslinking treatment may be, for example, 10 to 70 ℃, and the time of the crosslinking treatment may be, for example, 10 to 600 seconds.
A plurality of crosslinking steps may be provided.
After the crosslinking step, a step of immersing the precursor in a liquid containing an optical modifier without boric acid (hereinafter, may be referred to as a hue adjusting step) may be performed in order to adjust the hue of the polarizing film.
The treatment liquid in the crosslinking tank may contain, for example, precipitates based on polyvinyl alcohol or precipitates of a precursor of a polarizing film, and the precipitates may contain, for example, insoluble debris generated by the action of dissolved polyvinyl alcohol and boric acid.
(stretching Process)
The stretching step may be a step of performing a uniaxial stretching treatment while passing through a swelling bath, a dyeing bath, and/or a crosslinking bath. The uniaxial stretching treatment may be either dry stretching in which stretching is performed in air or wet stretching in which stretching is performed in a groove, or both. The uniaxial stretching treatment may be, for example, inter-roll stretching in which longitudinal uniaxial stretching is performed by providing a circumferential speed difference between 2 nip rolls, hot roll stretching, tenter stretching, or the like, and is preferably inter-roll stretching. The stretching ratio at which the precursor accumulates between the swelling step and the crosslinking step (the cumulative stretching ratio of the precursor when the stretching treatment is performed in two or more stages)) may be, for example, 3 times or more and 8 times or less.
(cleaning Process)
In the cleaning step, the precursor after the crosslinking step may be immersed in a treatment liquid (cleaning liquid) contained in a cleaning tank. The cleaning liquid may be water (for example, pure water) or an aqueous solution to which a water-soluble organic solvent such as alcohol is added. The temperature of the cleaning liquid may be, for example, about 5 ℃ to 40 ℃.
(drying Process)
In the drying step, the precursor after the washing step may be dried. The polarizing film can be obtained by conducting a drying process by introducing the precursor after the cleaning process into a drying process while continuously transporting the precursor.
[ electrolytic treatment Process ]
The electrolytic treatment step may be a step of subjecting the 1 st solution after the treatment of the precursor of the polarizing film to electrolytic treatment. The electrolytic treatment may be electrocoagulation, for example. As an example of the electrocoagulation method, there is a step of forming aggregates by flocculating metal hydroxide or metal ions eluted from an electrode with ground pieces by an electric current. The 1 st fragment is easily removed by the aeration-precipitation step and the filtration step described later by forming the 2 nd fragment having a larger size. The solution 1 may be subjected to pH adjustment in a first pH adjustment step described later.
The 1 st fragment may contain undesired fragments and water-soluble polymers resulting from the passage of the precursor of the polarizing film from the 1 st solution, such as chips, additives, and organic foreign substances in the processing bath, which are detached from, eluted from, or precipitated from the precursor of the polarizing film. When the precursor is a polyvinyl alcohol resin film, the 1 st fragment may contain a polyvinyl alcohol (PVA) flake or a small molecular oligomer. The particle size of the 1 st fragment distributed in the 1 st solution may be, for example, 10nm or more and 1000nm or less. The fragment 1 may be dissolved in water, may be a solid insoluble in water, or may be agglomerated and dispersed in a micelle form. The content of PVA in the solution may be detected by a method of calculating the total organic carbon content (TOC).
The electrolytic treatment may be performed in a precipitation tank containing the solution 1 provided with an electrode group. The electrode group may be provided with, for example, a1 st electrode element and a 2 nd electrode element, which may be a positive electrode and a negative electrode, respectively, and have opposite polarities. The material of the 1 st and 2 nd electrode elements may be, for example, a metal material such as iron (Fe), aluminum (a1), nickel (Ni), copper (Cu), or other suitable conductive material, or a non-metal material such as carbon. Since the metal compounds forming aggregates with the 1 st fragment are generated by the electrolytic reaction, it is preferable that at least one of the electrodes is composed of a material containing a metal.
In the precipitation tank, the 1 st electrode element and the 2 nd electrode element are immersed in the 1 st solution and contacted with the 1 st solution to apply a voltage, and a current is passed through the elements, so that a water-soluble metal compound is generated in the 1 st solution from the electrode components, and the generated metal compound is flocculated with the 1 st fragments to form 2 nd fragments, thereby forming a 2 nd solution containing the 2 nd fragments. The current value of the electrode group can be appropriately adjusted by the amount to be treated, and may be, for example, 0.2 to 100 amperes, preferably 1 to 80 amperes. When the current value is within the above range, the dissociated ion concentration in the 2 nd solution can be efficiently brought to an optimum value. The particle size of the fragment 2 may be, for example, 2 μm or more and 10 μm or less.
When the 1 st solution does not contain a boric acid component, the 1 st solution may be subjected to an electrolytic treatment reaction in the precipitation tank to form the 2 nd fragment by electrocoagulation of the 1 st fragment. Further, as a mechanism for forming the 2 nd fragment by aggregating the 1 st fragment in the precipitation tank, the following is presumed: during the deposition process by applying current to the electrode assembly, water molecules in the 1 st solution chemically react with the electrode assembly to form metal hydroxide as a coagulant from the 1 st electrode element or the 2 nd electrode element (containing a metal material), and the 1 st fragments flocculate with the metal hydroxide, so that the volume thereof increases to become 2 nd fragments.
[ first pH adjustment step ]
The first pH adjustment step may be a step of adjusting the pH of the 1 st solution after the polarizing film precursor is treated. The first pH adjustment step may be disposed between the precursor treatment step and the electrolytic treatment step, or may be included in the electrolytic treatment step. By performing the pH adjustment of the 1 st solution, the concentration of the dissolved metal in the water in which the 2 nd fragment is not formed can be kept low.
When the first pH adjustment step is disposed between the precursor treatment step and the electrolytic treatment step, for example, pH adjustment may be performed in a first pH adjustment tank for storing the 1 st solution after the treatment of the precursor of the polarizing film. When the first pH adjustment step is included in the electrolytic treatment step, the pH adjustment may be performed in the aforementioned precipitation tank, for example. The first production method may include both the first pH adjustment step and the second pH adjustment step described later, or may include the first pH adjustment step without including the second pH adjustment step described later.
The pH of the solution 1 before pH adjustment is, for example, usually less than 7, preferably 3 to 6.5, and more preferably 3.5 to 6.
Examples of the method for adjusting the pH include a method of adding a pH adjuster to the solution 1. The pH adjuster may be an alkaline solution. Examples of the alkaline solution include an aqueous solution of potassium hydroxide (KOH) and sodium hydroxide (NaOH). When a potassium hydroxide aqueous solution is used, the potassium hydroxide concentration may be, for example, 1 mass% or more and 30 mass% or less. In the first pH adjustment step, the pH value of the pH-adjusted first solution after the treatment of the polarizing film precursor 1 may be, for example, 5 or more and 9 or less, and preferably 6 or more and 8.5 or less.
[ second pH adjustment step ]
The second pH adjusting step may be a step of adjusting the pH of the electrolyzed solution 2. The second pH adjustment step may be disposed after the electrolytic treatment step. When the first production method has an aeration-precipitation step described later, the aeration-precipitation step may include the second pH adjustment step, or the aeration-precipitation step may include the second pH adjustment step. By adjusting the pH of the 2 nd solution, the concentration of the metal dissolved in the solution after being eluted from the electrode group into the 2 nd solution in the electrolytic treatment step can be reduced. The first production method may include a second pH adjustment step instead of the first pH adjustment step.
When the second pH adjustment step is disposed after the electrolytic treatment, the pH adjustment may be performed in, for example, a second pH adjustment tank containing the 2 nd solution. When the second pH adjustment step is included in the aeration-precipitation step, the pH adjustment may be performed, for example, in an aeration-precipitation tank described later.
When the second pH adjustment step is disposed after the aeration-precipitation step, the second pH adjustment step may be disposed, for example, between the aeration-precipitation step described later and the filtration step described later, or between the filtration step described later and the iodine concentration adjustment step described later.
When the first production method does not include the first pH adjustment step, the pH value of the solution 2 before pH adjustment is, for example, usually less than 7, preferably 3 or more and 6.5 or less, and more preferably 3.5 or more and 6 or less.
Examples of the method for adjusting the pH value include a method of adding a pH adjuster to the solution No. 2. The pH adjuster may be an alkaline solution. The alkaline solution and the concentration thereof are applied within the ranges exemplified and preferred in the description of the second pH adjustment step. In the second pH adjustment step, the pH value of the solution 2 after pH adjustment may be, for example, 5 or more and 9 or less, and preferably 6 or more and 8.5 or less, regardless of the presence or absence of the first pH adjustment step.
[ aeration precipitation step ]
The first production method may further include an aeration-precipitation step after the electrolytic treatment. The aeration-precipitation step may be a step of separating the 2 nd solution into the 3 rd solution and the precipitate by subjecting the 2 nd solution to aeration-precipitation treatment. The aeration-precipitation treatment may be performed in an aeration-precipitation tank containing the 2 nd solution. When the electrode group contains iron (Fe), Fe (OH) generated by the electrolytic treatment can be used by exposing the 2 nd solution to the atmosphere2By aeration to become Fe (OH)3Thereby becoming easily precipitated. The precipitate contained the 2 nd fragment described above.
After the precipitation is completed, the supernatant may be collected as a 3 rd solution. The 3 rd solution may contain the 2 nd fragment, but when the amount of the 2 nd fragment is large, it is preferable to reduce the amount as small as possible because it causes clogging of a filter in a filtering step to be described later.
[ filtration Process ]
The first production method may further include a filtration step after the aeration-precipitation step. The filtration step may be a step of subjecting the 3 rd solution to filtration treatment. By subjecting the 3 rd solution to a filtration treatment, the 2 nd fragment contained in the 3 rd solution can be removed. The filtration treatment may be performed by passing the 3 rd solution through a filtration membrane.
The filtration membrane has filtration pores, and the pore size thereof may be, for example, 1 μm to 10 μm, or 2 μm to 5 μm, as long as the size is a size capable of blocking the 2 nd fragment. In addition, the filtering holes of the filtering membrane are smaller than the 2 nd fragment, but the filtering holes can be selected to be larger than the 1 st fragment, and the filtering membrane with the larger filtering holes has lower cost and long effective service life, and can be periodically maintained after a longer working time. Alternatively, the filtering membrane may have filtering holes smaller than the size of the 1 st fragment so that the 1 st fragment and the 2 nd fragment can be removed.
[ iodine concentration adjustment step ]
The first production method may further include an iodine concentration adjustment step of adjusting the iodine concentration of at least one of the 2 nd solution and the 3 rd solution. Iodine (I) in the liquid medicine after the electrolytic treatment2) Is reduced to iodide ion (I)-). An iodine solution may be added to at least one of the 2 nd solution and the 3 rd solution so that the iodine concentration becomes a predetermined concentration. The iodine solution may be an aqueous iodine solution. The iodine concentration in the iodine aqueous solution may be, for example, 10 mass% or more and 90 mass% or less, and preferably 20 mass% or more and 80 mass% or less.
In the case of adjusting the iodine concentration of the 2 nd solution, the adjustment of the iodine concentration may be performed between the electrolytic treatment step and the aeration-precipitation step. In the case of adjusting the iodine concentration of the 3 rd solution, the adjustment of the iodine concentration may be performed after the aeration-precipitation step.
The iodine solution can be added, for example, in an iodine concentration adjusting tank containing the 2 nd solution or the 3 rd solution. The 2 nd and 3 rd solutions whose iodine concentration has been adjusted in the iodine concentration adjusting tank may be transferred to a storage tank or a staining tank.
[ procedure for analyzing concentration of Metal in solution ]
The first production method may further include a step of analyzing a metal concentration of at least one of the 2 nd solution and the 3 rd solution. The concentration of the metal dissolved from the electrode group of the electrolytic processing bath can be obtained by the metal concentration analysis. The metal concentration may be, for example, a metal ion concentration, a metal hydroxide concentration, or the like. The iron concentrations in the 2 nd and 3 rd solutions were measured by metal concentration analysis when the electrode set contained iron.
The metal concentration analysis can be performed by, for example, an XRF (fluorescent X-ray) analyzer attached to a pipe for transporting the 2 nd solution or the 3 rd solution. In addition, the metal concentration analysis of the sample taken from the 3 rd solution can be performed by using ICP-OES (inductively coupled plasma optical emission analysis).
The first manufacturing method may be a continuous manufacturing method. The continuous circulation system can control the content of the 1 st fragment in the 1 st solution within the allowable range of the manufacturing process management, maintain the 1 st solution at a specified cleanliness, avoid the quality problem of structural defects caused by the adhesion of undesirable PVA fragments on the surface of the precursor of the polarizing film, and the like, and improve the yield of products.
As a specific embodiment of the first production method, for example, a method for producing a polarizing film, which comprises the following steps in order: a precursor treatment step of treating a precursor of the polarizing film with the 1 st solution; a first pH adjustment step of adjusting the pH of the 1 st solution after the polarizing film precursor is treated; an electrolytic treatment step of bringing the pH-adjusted solution 1 into contact with an electrode group to perform a deposition treatment, thereby forming a solution 2; an aeration and precipitation process; a filtering process; and an iodine concentration adjusting step.
As another specific embodiment of the first manufacturing method, for example, a method for manufacturing a polarizing film may be mentioned, which comprises the following steps in order: a precursor treatment step of treating a precursor of the polarizing film with the 1 st solution; an electrolytic treatment step of bringing the pH-adjusted solution 1 into contact with an electrode group to perform a deposition treatment, thereby forming a solution 2; a second pH adjustment step of adjusting the pH of the 2 nd solution; an aeration and precipitation process; a filtering process; an iodine concentration adjustment step; and a step of analyzing the concentration of the metal in the solution.
As still another specific embodiment of the first manufacturing method, for example, a method for manufacturing a polarizing film may be mentioned, which includes the following steps in order: a precursor treatment step of treating a precursor of the polarizing film with the 1 st solution; an electrolytic treatment step of bringing the 1 st solution, the iodine concentration of which has been adjusted, into contact with an electrode group to perform a deposition treatment, thereby forming a 2 nd solution; an aeration and precipitation process; a filtering process; an iodine concentration adjustment step; and a second pH adjustment step of adjusting the pH of the 2 nd solution.
As still another specific embodiment of the first manufacturing method, for example, a method for manufacturing a polarizing film may be mentioned, which includes the following steps in order: a precursor treatment step of treating a precursor of the polarizing film with the 1 st solution; an electrolytic treatment step of bringing the 1 st solution, the iodine concentration of which has been adjusted, into contact with an electrode group to perform a deposition treatment, thereby forming a 2 nd solution; an aeration and precipitation process; a filtering process; a second pH adjustment step of adjusting the pH of the 2 nd solution; and an iodine concentration adjusting step.
As still another specific embodiment of the first manufacturing method, for example, a method for manufacturing a polarizing film includes the following steps in order: a precursor treatment step of treating a precursor of the polarizing film with the 1 st solution; a first pH adjustment step of adjusting the pH of the 1 st solution after the polarizing film precursor is treated; an electrolytic treatment step of bringing the pH-adjusted solution 1 into contact with an electrode group to perform a deposition treatment, thereby forming a solution 2; a second pH adjustment step of adjusting the pH of the 2 nd solution; an aeration and precipitation process; a filtering process; and an iodine concentration adjusting step.
(second embodiment)
The method for producing a polarizing film according to the second embodiment of the present invention is a method for producing a polarizing film in which iodine is adsorbed to a polyvinyl alcohol resin film, and the method for producing a polarizing film includes a step of bringing an electrode assembly into contact with an iodine-containing solution (hereinafter, also referred to as a second production method).
The iodine-containing solution is oxidized by contact with air, with the result that triiodide ions are generated. The electrode set may be suitably selected for the iodine-containing solution, and the anode is preferably an electrode set comprising a metal selected from the group consisting of iron, aluminum, nickel, and copper. By contacting these electrode sets, the triiodide ion concentration can be reduced. It is further preferable to contain iron in order to form stable ions from the surface of the anode and to prevent the electrolytic reaction from being inhibited by chemical species generated by the electrolytic reaction. The other electrode (cathode) may be an electrode generally used for electrolytic reaction, and is preferably a carbon electrode or a metal-containing electrode from the viewpoint of stably performing electrolytic reaction, and more preferably a transition metal from the viewpoint of stably continuing electrolytic reaction. The metals contained in the anode and the cathode may be the same or different. In the present invention, the anode refers to an electrode having a high potential.
The second manufacturing method may include a precursor treatment process. The precursor treatment step in the first production method described above is applied. The step of contacting the electrode group with the iodine-containing solution is preferably performed by a crosslinking step.
(third embodiment)
A method for producing a polarizing film according to a third embodiment of the present invention is a method for producing a polarizing film by adsorbing iodine to a polyvinyl alcohol resin film, the method including: a step of bringing an electrode group into contact with an iodine-containing solution; and a step of measuring the concentration of triiodide ions in the iodine-containing solution after contacting the electrode group (hereinafter also referred to as a third production method).
The third manufacturing method may include a precursor treatment process. The precursor treatment step in the first production method described above is applied. The step of bringing the electrode group into contact with the iodine-containing solution is preferably performed in the crosslinking step.
The concentration of triiodide ions in the iodine-containing solution after contacting the electrode assembly is preferably within a specified range. For example, the triiodide ion concentration in the crosslinking bath is preferably 1mM or less, more preferably 0.1mM or less, and still more preferably 0.05mM or less.
In order to control the triiodide ion concentration, the triiodide ion concentration in the iodine-containing solution after the electrode group is contacted may be measured. The measurement of the triiodide ion concentration may be an on-line measurement in which the concentration is measured by being directly connected to the tank, which is installed in the production apparatus, or an off-line measurement in which the liquid in the tank is taken out and the concentration is measured. The measurement method is not particularly limited, but measurement by ultraviolet-visible absorption spectroscopy is preferable in view of stable quantification even if other impurities are present. Specifically, the method shown in examples can be exemplified.
< apparatus for producing polarizing film >
Another polarizing film manufacturing apparatus according to another aspect of the present invention includes: a1 st solution treatment tank for receiving a1 st solution for treating a precursor of a polarizing film; and an electrode group which forms a 2 nd solution by performing an electrolytic reaction with the 1 st solution after the processing of the polarizing film precursor, and further comprises at least one of a mechanism for adding a pH adjusting agent to the 1 st solution after the processing of the polarizing film precursor and a mechanism for adding a pH adjusting agent to the 2 nd solution.
The polarizing film manufacturing apparatus may include a precursor processing unit for processing a precursor of the polarizing film and an electrolytic processing unit. Fig. 1 shows an example of a precursor processing section for processing a precursor of a polarizing film. The precursor treatment section shown in fig. 1 includes a delivery roll 12, a swelling tank 14, a dyeing tank 16, a crosslinking tank 18, a cleaning tank 20, a drying furnace 21, and a take-up roll 22. The 1 st solution treatment tank may be a staining tank 16 or a crosslinking tank 18.
The precursor 200 of the polarizing film is unwound by the unwinding roller 12, and then guided and conveyed by the guide roller 120 to pass through the respective processing tanks and processing devices in order in the direction indicated by the arrow. The polarizing film 200' thus formed may be wound again on the winding roll 22.
The polarizing film precursor, the 1 st solution, the 2 nd solution, the pH adjuster, and the production conditions of the respective tanks and devices are exemplified by the above-described polarizing film production method.
The precursor 200 of the polarizing film is first guided to the swelling tank 14 by the guide roller 120, so that the precursor 200 of the polarizing film can be subjected to the swelling treatment. Next, the polarizing film precursor 200 is guided to the dyeing tank 16 by the guide roller 120, and the polarizing film precursor 200 is subjected to dyeing treatment. The precursor 200 of the polarizing film is then guided to the crosslinking tank 18 by the guide roller 120, thereby performing a crosslinking process on the precursor 200 of the polarizing film. The precursor 200 of the polarizing film may be subjected to a stretching process. The stretching process may be performed while passing through the swelling tank 14, the dyeing tank 16, and/or the crosslinking tank 18. For example, the uniaxial stretching treatment may be performed by making a circumferential speed difference between the guide roller 120 provided at the inlet of the swelling tank 14 and the guide roller 120 provided at the outlet of the swelling tank 14.
FIG. 2 shows a solution treatment tank 101 and an electrolytic treatment section 1. The bath solution in the 1 st solution treatment bath 101 was the 1 st solution L1. The guide roller 120 transports the precursor 200 of the polarizing film through the 1 st solution L1 in the 1 st solution processing tank 101. The 1 st solution treatment tank 101 may be a staining tank 106 and/or a crosslinking tank 108 shown in fig. 1. The 1 st solution treatment tank 101 may be in communication with the circulation system 37.
The circulation system 37 may include the 1 st passage 103, the electrolytic processing unit 150, and the 7 th passage 111.
The electrolytic treatment section 150 may include the precipitation tank 105, the 2 nd passage 107, the aeration-precipitation tank 140, the 3 rd passage 141, the pH adjuster tank 142, the 4 th passage 143, the filter device 109, the metal concentration analyzer 144, the 5 th passage 145, the iodine concentration adjusting tank 146, the iodine solution tank 147, and the 6 th passage 148. The 1 st passage 103, the 2 nd passage 107, the 3 rd passage 141, the 4 th passage 143, the 5 th passage 145, and the 6 th passage 148 are respectively communicated with each tank, each device, and the like and can circulate the solution by using a pump (not shown).
Fragment 1P 1 may be formed into larger size fragment 2P 2 by electrolytic treatment in the precipitation tank 105.
The electrode group E is provided in the precipitation tank 105. The electrode group E includes, for example, a1 st electrode element E1 and a 2 nd electrode element E2 having opposite polarities as a positive electrode and a negative electrode, respectively. The 1 st electrode element E1 and the 2 nd electrode element E2 may contain the materials exemplified in the description of the above-described method for manufacturing the polarizing film.
The precipitation tank 105 may be provided with a circulation system to improve the efficiency of the electrolytic treatment. In the circulation system 137 shown in fig. 3, the precipitation tank 105 may store the 1 st solution L1, and may include an electrode group E and at least one overflow device 30. The overflow device 30 may be provided with a drain plate 31 and a passage 130 (e.g., a drain pipe). The position of the drain plate 31 of the overflow device 30 can be adjusted to be lower than the liquid level of the solution, so that the solution can be introduced and discharged to the circulation system 137 outside the precipitation tank 105 via the passage 130. Here, by providing the filtration device 109 in the circulation system 137, the 2 nd fragment P2 in the 2 nd solution L2 was filtered, and the 2 nd solution L2 was returned to the precipitation tank 105 via the passage 133 for use.
As shown in fig. 4, the overflow device 30 may include a tank portion 32. The drain plate 31 may be movably disposed on at least one side of the case portion 32, whereby the position of the drain plate 31 can be adjusted according to the liquid level of the solution.
In another embodiment, overflow device 30 may be further provided with a filtering member 318. The filter member 318 is removably disposed within the case portion 32. The filter member 318 may be, for example, a filter net, a filter membrane, or the like. The filter member 318 further increases the efficiency of the filtering to remove debris by substantially filtering out the debris. The pore diameter of the filtration pores of the filtration membrane is, for example, 1 μm or more and 10 μm or less, or 2 μm or more and 5 μm or less.
The aerated precipitation tank 140 may expose the 2 nd solution L2 to the atmosphere. The precipitate precipitated in the aeration-precipitation tank 140 is sent to a solid-liquid separation device (not shown), and the 3 rd solution L3 as an upper layer liquid is sent to the filtration device 109 through the 3 rd passage 141. The filter unit 109 may have the 1 st tank section 116A, the 2 nd tank section 116B, and the filter membrane 118. Filter membrane 118 is positioned between tank section 1A and tank section 2 116B and allows filtration of solution 3L 3 from tank section 1A.
In the electrolytic treatment section shown in FIG. 2, the aeration-sedimentation tank 140 is provided with a pH adjuster tank 142 as a means for adding a pH adjuster L4 to the No. 2 solution. The pH of the 2 nd solution L2 in the aerated precipitation tank 140 can be adjusted by adding a pH adjusting agent L4 from the pH adjusting agent tank 142 to the aerated precipitation tank 140. As a means for adding the pH adjusting agent L4 to the solution 2, for example, a pH adjusting tank including a pH adjusting agent tank 142 may be provided between the precipitation tank 105 and the aeration and sedimentation tank 140 instead of providing the pH adjusting agent tank 142 in the aeration and sedimentation tank 140 as shown in fig. 2.
In another embodiment of the present invention, the precipitation tank 105 may be provided with a pH adjuster tank 142 as a mechanism for adding the pH adjuster L4 to the 1 st solution, or a pH adjuster tank provided with the pH adjuster tank 142 may be provided between the 1 st solution treatment tank 101 and the precipitation tank 105.
After the 3 rd solution L3 treated by the filtration device 109 passed through the metal concentration analysis device 144, iodine (I) was added by using an iodine concentration adjustment tank 1462) Whereby the iodine concentration is adjusted. Is contained in the iodine solutionThe iodine solution L5 in the tank 147 is applied within the ranges exemplified and preferred for the iodine solution L5 in the above-described method for producing a polarizing film. Next, the 3 rd solution L3 with the iodine concentration adjusted may be transferred to an iodine storage tank (not shown) through the 6 th path 148, or may be transferred to the 1 st solution treatment tank through the 7 th path 111. When the 3 rd solution L3 was sent to the 1 st solution treatment tank, the metal concentration analysis was also performed in the 1 st solution treatment tank. By measuring the metal concentration of the 1 st solution treatment tank containing the 3 rd solution L3, the management of the treatment solution for treating the precursor of the polarizing film is facilitated.
The polarizing film manufacturing apparatus of the present invention may be a continuous manufacturing apparatus. That is, the solution can be purified in the electrolytic processing section 150 while the polarizing film precursor 200 is processed, and therefore, the production efficiency tends to be excellent.
[ examples ] A method for producing a compound
The present invention will be described in further detail below with reference to examples. In the examples, "%" and "part" are% by mass and part by mass unless otherwise specified.
[ PVA removal Rate ]
The total organic carbon content of the 2 nd solution was determined, and the reduction rate thereof with respect to the total organic carbon content of the 1 st solution taken out from the iodine staining bath was determined. The total organic carbon content can be determined using a total organic carbon content (TOC) analyzer.
[ iron ion concentration ]
The iron ion concentration analysis was performed by ICP-OES (inductively coupled plasma optical emission analysis).
[ method for measuring Triiodide ion concentration ]
The triiodide ion concentration (M) was determined by measuring the maximum absorption peak of iodine with the absorption wavelength set to 350nm using an ultraviolet-visible spectrophotometer (UV-2450, Shimadzu).
< example 1>
The 1 st solution (I) after treating a precursor (polyvinyl alcohol resin film) of a polarizing film2: 0.03 part, KI: 1.5 parts) was taken out from the iodine staining bath. The pH of the taken-out solution 1 is 5-6. To the 1 st solution was added an aqueous KOH solution (KOH concentration: 20%) to adjust the pH to 9 (first pH adjustment)Step-saving). Subsequently, the 1 st solution was subjected to electrolytic flocculation reaction at 1.0 ampere for 12 minutes to obtain a 2 nd solution (electrolytic treatment step). The pH of the resulting solution 2 was measured, and found to be 7.5. The PVA removal rate was 26%, and the iron ion concentration in the aqueous solution was not more than the detection limit.
< example 2>
A 2 nd solution was obtained in the same manner as in example 1 except that in the first pH adjustment step in example 1, the pH was adjusted to 10 instead of 9. The pH of the resulting solution 2 was measured, and found to be 8.3. The PVA removal rate was 25%, and the iron ion concentration in the aqueous solution was not more than the detection limit.
< example 3>
A 2 nd solution was obtained in the same manner as in example 1, except that in the first pH adjustment step in example 1, the pH was adjusted to 11 instead of 9. The pH of the resulting solution 2 was measured, and found to be 8.5. The PVA removal rate was 22%, and the iron ion concentration in the aqueous solution was not more than the detection limit.
< comparative example 1>
A 2 nd solution was obtained in the same manner as in example 1, except that the electrolytic treatment step was performed without performing the first pH adjustment step in example 1. The pH of the resulting solution 2 was measured, and found to be 3.4. The PVA removal rate was 20%, and the iron ion concentration in the aqueous solution was 60 ppm.
The results of examples 1 to 3 and comparative example 1 are shown in Table 1.
[ TABLE 1]
< example 4>
Boric acid and potassium iodide were added to pure water at 65 ℃ so that the boric acid concentration was 3.4% and the potassium iodide concentration was 10%, thereby preparing a solution. The solution was clear immediately after preparation, and after 30 minutes the solution had a yellow color, and the triiodide ion concentration rose due to air oxidation. Immersing iron as an anode in the solution, and immersing iron as a cathode in the solutionThe resultant solution was immersed in the solution and applied with a current of 1A for 45 seconds to conduct electrolytic treatment. The triiodide ion concentration of the solution after the electrolytic treatment was measured, and as a result, it was reduced to 0.02X 10-4And M. There was no accumulation of sulfate.
< example 5>
The procedure of example 4 was repeated except that an aluminum plate was used as the anode.
< example 6>
The procedure of example 4 was repeated except that a copper plate was used as the anode.
< example 7>
The procedure of example 4 was repeated except that a nickel plate was used as the anode.
< comparative example 2>
The procedure of example 4 was repeated except that a 1% aqueous solution of potassium sulfite was added instead of the electrolytic treatment by immersing the electrode. The determination result of the triiodide ion concentration can be reduced to 0.03 multiplied by 10-4M, but there is a build up of sulphate.
The results of examples 4 to 7 and comparative example 2 are shown in Table 2.
[ TABLE 2]
Claims (13)
1. A method for manufacturing a polarizing film, comprising:
a precursor treatment step of treating a precursor of the polarizing film with the 1 st solution; and
an electrolytic treatment step of forming a 2 nd solution by bringing the 1 st solution after the treatment of the polarizing film precursor into contact with an electrode group to perform a deposition treatment,
the method for producing a polarizing film further comprises at least one of a first pH adjustment step of adjusting the pH of the 1 st solution after the polarizing film precursor is treated and a second pH adjustment step of adjusting the pH of the 2 nd solution.
2. The method of manufacturing the polarizing film according to claim 1, wherein the 1 st solution is iodine (I) containing for dyeing a precursor of the polarizing film2) And (3) solution.
3. The method for manufacturing a polarizing film according to claim 1 or 2, further comprising an aeration-precipitation step of separating the 2 nd solution into a 3 rd solution and a precipitate by subjecting the 2 nd solution to an aeration-precipitation treatment.
4. The method for producing a polarizing film according to any one of claims 1 to 3, further comprising a filtration step of subjecting the 3 rd solution to a filtration treatment.
5. The method for producing a polarizing film according to claim 3 or 4, further comprising a step of adjusting the iodine concentration of at least one of the 2 nd solution and the 3 rd solution.
6. The method for producing a polarizing film according to any one of claims 3 to 5, further comprising a step of analyzing a metal concentration in at least one of the 2 nd solution and the 3 rd solution.
7. A polarizing film manufacturing apparatus includes:
a1 st solution treatment tank for receiving the 1 st solution for treating the precursor of the polarizing film, and
contacting with the 1 st solution after processing the precursor of the polarizing film to form an electrode assembly of a 2 nd solution,
the polarizing film manufacturing apparatus further comprises at least one of a mechanism for adding a pH adjuster to the 1 st solution after the polarizing film precursor is treated, and a mechanism for adding a pH adjuster to the 2 nd solution.
8. The polarizing film production apparatus according to claim 7, further comprising an aeration and sedimentation tank for storing the 2 nd solution and separating the solution into a 3 rd solution and sediment.
9. The polarizing film production apparatus according to claim 8, further comprising a solution containing iodine (I) added in a state of accommodating the No. 3 solution2) The iodine concentration adjusting tank of the mechanism (2).
10. The polarizing film manufacturing apparatus according to any one of claims 7 to 9, which comprises a metal concentration analyzer.
11. A method for producing a polarizing film, which comprises adsorbing iodine to a polyvinyl alcohol resin film to produce a polarizing film,
the method for producing the polarizing film comprises a step of bringing an electrode assembly into contact with an iodine-containing solution,
the anode of the electrode assembly contains iron.
12. The method for producing a polarizing film according to claim 11, wherein the step of contacting an electrode group with the iodine-containing solution is performed in the crosslinking step.
13. A method for producing a polarizing film, which comprises adsorbing iodine to a polyvinyl alcohol resin film to produce a polarizing film,
the method for manufacturing the polarizing film includes:
a step of bringing an electrode group into contact with an iodine-containing solution; and
and measuring the concentration of triiodide ions in the iodine-containing solution after the electrode group is contacted.
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| JP2019194431A JP7360893B2 (en) | 2019-10-25 | 2019-10-25 | Polarizing film manufacturing method and manufacturing equipment |
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| JP2023038489A (en) * | 2021-09-07 | 2023-03-17 | 住友化学株式会社 | Polarizing film and manufacturing method for polarizer |
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| Publication number | Publication date |
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| JP2021067873A (en) | 2021-04-30 |
| JP7360893B2 (en) | 2023-10-13 |
| TW202120609A (en) | 2021-06-01 |
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