CN101852879B - Process for producing a polarizing film - Google Patents
Process for producing a polarizing film Download PDFInfo
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- CN101852879B CN101852879B CN201010141470.1A CN201010141470A CN101852879B CN 101852879 B CN101852879 B CN 101852879B CN 201010141470 A CN201010141470 A CN 201010141470A CN 101852879 B CN101852879 B CN 101852879B
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
- G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/133528—Polarisers
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Abstract
The invention provides a process for producing a polarizing film, performing swelling treatment, dyeing treatment, boric acid treatment washing treatment for polyvinyl alcohol films and performing single axle stretching before treatment and/or in treatment, wherein when the boron compound content in the film before washing is Y and the boron compound content in the film after washing is X, the residual rate of the boron compound content before and after washing treatment at one time is 0.7-0.98; or when the film width before washing treatment is A and the film width after washing treatment is B, A/B before and after washing treatment at one time is 0.97-1.03. The invention provides the process for producing the polarizing film having a good appearance without color deviation, foreign matter defects nor dints.
Description
Technical field
The present invention relates to the manufacture method of the good light polarizing film of a kind of outward appearance.
Background technology
All the time, adopt make dichromatism pigment be adsorbed onto on polyvinyl alcohol mesentery and there is orientation and the film that obtains as light polarizing film.That is to say, having as everyone knows iodine polarizing film, the dyestuff using dichroic dye as dichromatism pigment using iodine as dichromatism pigment is light polarizing film etc.Conventionally, these light polarizing film, at its at least one side, the diaphragms such as tackifier laminating triacetyl cellulose that preferably consist of the aqueous solution by polyvinyl alcohol resin etc. on two sides, are made Polarizer.
Manufacture method as light polarizing film, there is as everyone knows following method: use roll, guide roller, with described dichromatism pigment, polyvinyl alcohol mesentery is dyeed and by its extension, for iodine is anchored on film, polyvinyl alcohol mesentery is carried out to boric acid processing subsequently, the clean processing such as wash, then dry.
But, in above-mentioned manufacture method, below existing, reduce the problem of outward appearance in described clean processing: on film, occur wrinkling or because of boric acid, process the boronic acid compounds that causes and on film surface, separate out and occur in foreign matter defect, light polarizing film at gained, misalignment, foreign matter defect to occur, beat trace etc.
For example, in JP-3979688-B2, record, as the manufacture method of the good light polarizing film of optical property, dimensional stability, the boron atom content in film is setting.According to the record of the document, utilize washing to process and can adjust the boron atom content in light polarizing film.
But, in JP-3979688-B2, do not have to record the concrete content of cleaning the boron compound in the film of processing front and back, even if present situation is to use the method for recording in JP-3979688-B2, also may not fully suppress generation wrinkling, foreign matter defect.
In addition, in P2003-240947-A, JPH08-327823-A, record, as the manufacture method of the high polarizer of degree of polarization, the film of boric acid processing front and back is wide is setting.And, in JPH08-327823-A, record, as the manufacture method of the good light polarizing film of permanance, in the processing that utilizes boron compound, carry out uniaxial tension, this film before and after stretching is wide is setting.
But, at P2003-240947-A, wide all without any concrete record for the film of cleaning before and after processing in JPH08-327823-A, even if present situation is to use P2003-240947-A, the method of recording in JPH08-327823-A, also may not necessarily fully suppress generation wrinkling, foreign matter defect, and the manufacture method of the better light polarizing film of outward appearance is developed in expectation.
Summary of the invention
Problem of the present invention is for providing the manufacture method of the light polarizing film with good appearance.
In order to address the above problem, inventor of the present invention has carried out research with keen determination, and result has found the solution of following formation, and has completed the present invention.
(1) a kind of manufacture method of light polarizing film, polyvinyl alcohol mesentery is carried out successively swelling processing, dyeing processing, boric acid processing and cleans and process, before these are processed and/or in processing, carry out uniaxial tension, wherein, by the boron compound content in the film before clean processing be made as Y, when the boron compound content in the film of cleaning after processing is made as to X, the residual rate (X/Y) that makes once to clean the boron compound content in the film before and after processing is 0.7～0.98.
(2) according to the method (1) described, wherein, at least carry out 2 above-mentioned clean processing.
(3) according to the method (2) described, wherein, by the boron compound content in the film before initial clean processing be made as Yp, when the boron compound content in the film after last clean processing is made as to Xp, making the residual rate (Xp/Yp) of the boron compound content in the full film of cleaning before and after processing is 0.7～0.98.
(4) a kind of manufacture method of light polarizing film, polyvinyl alcohol mesentery is carried out successively swelling processing, dyeing processing, boric acid processing and cleans and process, before these are processed and/or in processing, carry out uniaxial tension, wherein, by the wide A of being made as of film before clean processing, when cleaning that film after processing is wide is made as B, making the A/B once cleaning before and after processing is 0.97～1.03.
(5), according to the method (4) described, wherein, at least carry out cleaning for 2 times and process.
(6) method according to (5), wherein, by the wide Ap of being made as of film before initial clean processing, by after processing film wide while being made as Bp, making the full Ap/Bp cleaning before and after processing is 0.97～1.03.
(7) according to the method (4) or (5) described, wherein, by the boron compound content in the film before clean processing be made as Y, when the boron compound content in the film of cleaning after processing is made as to X, the residual rate (X/Y) that makes once to clean the boron compound content in the film before and after processing is 0.7～0.98.
(8) according to the method (7) described, wherein, at least carry out 2 described clean processing, by the boron compound content in the film before initial clean processing be made as Yp, when the boron compound content in the film after last clean processing is made as to Xp, making the residual rate (Xp/Yp) of the boron compound content in the full film of cleaning before and after processing is 0.7～0.98.
(9), according to the method described in any one in (1)～(8), wherein, the clean temperature of cleaning in processing is below 30 ℃.
(10) manufacture method for Polarizer, the diaphragm of fitting at least one side of the light polarizing film obtaining in the method with described in any one in (1)～(9).
The present invention has following effect: owing to can being suppressed on film, wrinkling, foreign matter defect occurs in cleaning processing, so can access to have without misalignment, foreign defect, nothing, beat the good light polarizing film of the outward appearances such as trace.
Embodiment
The manufacture method > of < light polarizing film
Below, the manufacture method of the light polarizing film the present invention relates to embodiment is described.It is resin saponification and the resin that obtains that the polyvinyl alcohol resin of formation polyvinyl alcohol mesentery is in the present embodiment exemplified as polyvinyl acetate conventionally.As saponification degree, be about more than 85 % by mole, preferably more than approximately 90 % by mole, be more preferably approximately 99～100 % by mole.As polyvinyl acetate, be resin, except the polyvinyl acetate of the homopolymer as vinyl acetate, can list, can with other monomers of vinyl acetate copolymerization and the multipolymer of vinyl acetate, such as vinyl-vinyl acetate copolymer etc.Other monomers as can copolymerization, can be exemplified as unsaturated carboxylic acid class, olefines, ethene ethers, unsaturated sulfonic acid class etc.As the degree of polymerization of polyvinyl alcohol resin, be about 1000～10000, be preferably approximately 1500～5000 left and right.
These polyvinyl alcohol resins can be modified, such as using by the polyvinyl formal of aldehydes modification, polyvinyl acetal, polyvinyl butyral etc.Conventionally, the parent material of manufacturing as light polarizing film, used thickness is about the unstretching film of the polyvinyl alcohol resin film of 20～100 μ m, preferred approximately 30～80 μ m.Industrial, the wide 1500～4000mm that is about of film is practical.
This unstretching film carries out successively swelling processing, dyeing processing, boric acid processing, cleans and process, finally be dried processing, and, swelling is processed, dyeing is processed, boric acid is processed and clean the processing of processing before and/or process in carry out the polyethenol series light polarizing film that uniaxial tension obtains thickness be for example about 5～50 μ m left and right.
The light polarizing film of present embodiment is the polyethenol series monadic stretching membrane that dichromatism pigment is adsorbed and orientation occurs, and as its manufacture method, is roughly divided into 2 kinds of manufacture methods.Method one is that uniaxial tension polyvinyl alcohol mesentery in air or non-active gas, then, carries out solution-treated with the order of swelling processing, dyeing processing, boric acid processing and clean processing, is finally dried.Other method is, in aqueous solution, to the polyvinyl alcohol mesentery not stretching with swelling process, dyeing is processed, boric acid is processed and clean the order of processing and carry out solution-treated, boric acid process and/or before processing in carry out wet type uniaxial tension, be finally dried.
In any method, uniaxial tension can carry out in a processing, also can in two above processing, carry out, and still, preferably in a plurality of processing, carries out.Drawing process can adopt known method, for example, at 2 roll shop buildings of transport membrane, impose between the roller that difference stretches and stretch, and can enumerate the hot-rolling pulling method of recording in JP2731813-B2, stenter pulling method etc.And, although processing sequence for as mentioned above, is processed the not restrictions such as the quantity of bathing, treatment conditions substantially.
And, do not need superfluous words, for other objects, can freely insert the processing of not recording in above-mentioned processing.As the example of this processing, can enumerate after boric acid is processed the dip treating (zinc processing) that utilize the dip treating (iodide processing) of not borated iodide aqueous solution or utilization not to contain boric acid, to contain the aqueous solution such as zinc chloride etc.
In order to remove the foreign matter on film surface, except the plastifier in striping, give the easy dyeing in subsequent treatment, the objects such as plasticization of film, carry out swelling processing.In the scope of the rough sledding such as extreme dissolving, devitrification of base material film, determine treatment conditions can realize these objects and not occur.When making to have carried out in advance the film swelling of stretching in gas, in the aqueous solution of for example approximately 20～70 ℃, preferred approximately 30～60 ℃, carry out film immersion.As the dip time of film, it is approximately 30 seconds～300 seconds, preferably about approximately 60 seconds～240 seconds.When the original membrane that makes always not stretch (former anti-Off ィ Le system) swelling, in the aqueous solution of for example approximately 10～50 ℃, preferred approximately 20～40 ℃, carry out film immersion.The dip time of film approximately 30 seconds～300 seconds, preferably about approximately 60 seconds～240 seconds.
In swelling is processed, film is swelling on cross direction, on film, easily there is to occur the problems such as wrinkling, therefore, preferably use known amplitude-expanding devices such as widening roller (spreader roll (expander roll)), propellers, crowned roll, two guide roller, bend bar, a cloth clamp to remove the wrinkling and transport membrane of film.And, for making stable conveying of film in bath, in water, spray is controlled the current of swelling in bathing and is useful with EPC device (Edge Position Control device (marginal position control device): detect the end of film, and prevent the device crawling of film) etc.In this processing, because film on the direction of travel of film also swelling expands, in order to make film lax on throughput direction, preferably use is such as the methods such as speed of controlling the conveying roller for the treatment of trough front and back.And, as the swelling of using, process and bathe, outside (pure) water, also can use and in the scope of approximately 0.01～10 % by weight, add boric acid (recording in JPH10-153709-A), chloride (recording in JPH06-281816-A), mineral acid, inorganic salts, water-miscible organic solvent, alcohols etc.In swelling is processed, also can process and similarly carry out the stretching of film with aftermentioned dyeing.
Dyeing based on dichromatism pigment is processed, so that dichromatism pigment is adsorbed onto on film and the objects such as orientation occur and carries out.Can in the scope of the rough sledding such as extreme dissolving, devitrification of base material film, determine treatment conditions can realize these objects and not occur.In the situation that using iodine as dichromatism pigment, at the temperature of approximately 10～45 ℃, preferred approximately 20～35 ℃, and by weight, iodine/potassium iodide/water=approximately 0.003～0.2/ approximately 0.1～10/100, carries out approximately 30 seconds～600 seconds, preferred approximately 60 seconds～300 seconds dip treating.Also can replace potassium iodide with other iodide such as zinc iodide etc.And potassium iodide also can and be used with other iodide.And, also can make compound such as boric acid beyond iodide, zinc chloride, cobalt chloride etc. coexist.When adding boric acid, in the angle containing iodine and following boric acid, process difference.With respect to water 100 weight portions, if containing the iodine of having an appointment more than 0.003 weight portion, can be considered as staining trough.
While using water-soluble dichroic dye as dichromatism pigment, at the temperature of for example approximately 20～80 ℃, preferred approximately 30～70 ℃, and by weight, dichroic dye/water=approximately 0.001～0.1/100, carries out approximately 30 seconds～600 seconds, preferred approximately 60 seconds～300 seconds dip treating.The aqueous solution of the dichroic dye using can contain accelerant etc., also can contain such as the inorganic salts such as sodium sulphate, surfactant etc.Dichroic dye can be used separately, also can use two or more dichroic dye simultaneously.
As mentioned above, also can carry out stretched film with staining trough.Stretching can be by making the roll of staining trough front and back keep the methods such as difference to carry out.And, identical with swelling processing, setup of entrances and exits be can and/or bathe in dye bath and roller (spreader roll), propellers, crowned roll, two guide roller, bend bar etc. widened.
Boric acid is processed the polyvinyl alcohol mesentery that utilizes dichromatism pigment to carry out dyeing by dipping in aqueous solution and is implemented, in this aqueous solution, with respect to 100 weight parts waters, containing the proportional boric acid that is about 1～10 weight portion.
In the situation that dichromatism pigment is iodine, preferably containing the proportional iodide that are about 1～30 weight portion.As these iodide, can be exemplified as potassium iodide, zinc iodide etc.And the compound as beyond iodide, also can make such as zinc chloride, cobalt chloride, zirconium chloride, sodium thiosulfate, potassium sulfite, sodium sulphate etc. coexist.
For water-fastization based on crosslinked, prevent the adjustment of color such as partially blue etc., implement this boric acid and process.When carrying out water-fastization based on crosslinked, as required, also can except boric acid or together with boric acid, use glyoxal, the crosslinking chemical such as glutaraldehyde.
In addition, sometimes by titles such as resistance to hydration process, crosslinking Treatment, immobilization processing, call for the boric acid of water-fastization and process.And, sometimes with complementary color process, the title such as dyeing processings is called the boric acid processing for adjustment of color again.
As required, suitably change the concentration of boric acid and iodide, the temperature of processing bath is implemented this boric acid processing.For the boric acid of water-fastization, process and process not special difference for the boric acid of adjustment of color, can implement according to following condition.
When swelling, dyeing, boric acid are processed original membrane, to turn to object based on crosslinking chemical water-fast, carry out boric acid while processing, with respect to 100 weight parts waters, use containing the boric acid of have an appointment 3～10 weight portion boric acid, approximately 1～20 weight portion iodide and process and bathe, conventionally, at the temperature of approximately 50～70 ℃, preferred approximately 55～65 ℃, carry out.Dip time is generally approximately 30～600 seconds, preferably approximately 60～420 seconds, be more preferably approximately 90～300 seconds.In addition, to the film stretching in advance dye, boric acid is when process, boric acid is processed approximately 50～85 ℃ conventionally, preferably approximately 55～80 ℃ of the temperature of bathing.
After the boric acid for water-fastization is processed, also can carry out processing for the boric acid of adjustment of color.For example, when dichroic dye is iodine, for this object, with respect to 100 weight parts waters, uses containing the boric acid of have an appointment 1～5 weight portion boric acid, approximately 3～30 weight portion iodide and process and bathe, conventionally, at the temperature of approximately 10～45 ℃, carry out.Dip time is generally about approximately 3～300 seconds, preferably approximately 10～240 seconds.Process and compare with the boric acid for water-fastization, for the boric acid of adjustment of color, process and conventionally under low boric acid concentration, periodide concentration, low temperature, carry out.
Also can repeatedly carry out these boric acid processing, conventionally, carry out 2～5 times more.Now, the aqueous solution of each boric acid treatment trough of use forms, temperature in above-mentioned scope, can identical, also can be different.Also can repeatedly carry out respectively the above-mentioned boric acid for water-fastization processes, for the boric acid of adjustment of color, processes.In boric acid is processed, also can process and carry out in the same manner film stretching with dyeing.Final accumulation draw ratio is approximately 4.5～7 times, preferably approximately 5～6.5 times.
After processing, boric acid cleans processing.This is cleaned and processes, for example, by being immersed in detergent remover, spraying detergent remover as shower or also with dipping and spraying, implementing for the polyvinyl alcohol mesentery after the boric acid processing of water-fastization and/or adjustment of color having carried out.In cleaning processing, also can process and carry out equally the stretching of film with dyeing.
Herein, in the present embodiment, the residual rate of once cleaning the boron compound content in the film before and after processing is 0.7～0.98.Like this, by the boron compound content before and after clean processing is controlled as particular value, thereby in the generation of cleaning wrinkling, the foreign matter defect that can suppress film in processing.To this, if described Retention less than 0.7 easily occurs wrinkling on film in clean processing.Its reason is speculated as, if above-mentioned residual rate less than 0.7, to process uneven possibility high for boric acid, therefore in cleaning and processing, in the part of film, occurs wrinkling.And if described residual rate surpasses 0.98, the boron compound content in film is excessive, therefore in cleaning processing, easily there is foreign matter defect.
Can calculate as described below described residual rate.That is, first, calculate the boron compound content in the film of cleaning before and after processing.Particularly, each film of the scheduled volume before and after clean processing is flooded 60 minutes respectively in the hot water of 95 ℃, it is dissolved completely, each solution of acid-base titration afterwards, and calculate the boron compound content in each film by film weight and titer.Then, bring each value obtaining into following formula (I), calculate described residual rate.
Residual rate=X/Y (1)
X: clean the boron compound content in the film after processing
Y: clean the boron compound content in the film before processing
As the boron compound content in the film of cleaning before processing, be 2.5～5 % by weight, preferably 3～4.7 % by weight left and right, as the boron compound content in the film of cleaning after processing, are 2%～4.5 % by weight, preferably 2.5～4.3 % by weight left and right.Described % by weight is the value of the film weight of (untreated) before processing with respect to swelling.
By adjusting the clean temperature of once cleaning in processing, the composition of detergent remover, clean time etc., described residual rate can be controlled be 0.7～0.98.
And clean number of times is not defined as 1 time, can in the scope of 2～4 left and right, at random select.
At clean number of times for repeatedly time, by the boron compound content in the film before initial clean processing be made as Yp, when the boron compound content in the film after finally clean processing is made as to Xp, preferably complete clean process before and after the residual rate of boron compound content in film be 0.7～0.98.
As clean temperature, can be below 30 ℃, preferably 3～30 ℃.As detergent remover, outside dewatering, can adopt and contain for example boron aqueous acid.With respect to the water of 100 weight portions, preferably contain the ratio of boric acid approximately 0.01～0.5 weight portion.When employing contains boron aqueous acid as detergent remover, a small amount of iodide preferably coexist in solution.These detergent removers of example can be used a kind, also can mix two or more use.
When adopting water as detergent remover, the clean time was preferably about 1～20 second, when adopting borated aqueous solution, preferably about 5～50 seconds.
Generally, each condition, in above-mentioned scope, has by the boronic acid containing or reduce containing ratio, increase the time of cleaning etc. not such as raise cleaning temperature, in detergent remover, reduces the tendency of described Retention.For Retention is controlled in 0.7～0.98 scope, experimentally by clean temperature, detergent remover composition, clean time etc. and determine at certain point and (for example clean temperature: 15 ℃, detergent remover: water, the time of cleaning: 10 seconds etc.), clean processing, confirm Retention.Its result, if the residual rate obtaining is not within the scope of this, consider that above-mentioned clean temperature, detergent remover form, clean the affect trend of condition on residual rate such as time, adjust each suitable condition, again clean processing, then confirm residual rate, repeatable operation, until residual rate is in 0.7～0.98 scope, thereby can adjust and determine each condition.
Clean the dry processing after processing, can in drying oven, at the temperature of approximately 40～100 ℃, carry out approximately 60～600 seconds, obtain thus the light polarizing film of present embodiment.In addition, in the present embodiment, during each after stretch processing processed, can implement tension force and control, so that the tension force of each film is certain in fact.In dyeing is processed, be through with while stretching, preferably after boric acid process and clean processing in control tension force.
Next, other embodiment of the manufacture method of light polarizing film of the present invention is described.In the present embodiment, by the wide A of being made as of film (hereinafter referred to as the wide A of film) before clean processing, when cleaning that film after processing is wide is made as B (hereinafter referred to as the wide B of film), the A/B once cleaning before and after processing is 0.97～1.03.Like this, by being particular value by the wide control of film of once cleaning before and after processing, can in cleaning processing, suppressing film and occur wrinkling.To this, if described (A/B) is less than 0.97 or be greater than 1.03, the wide variation of film of cleaning before and after processing becomes large, therefore clean process in film easily occur wrinkling.
As the wide A of film, the B before and after clean processing, according to wide, the degree of uniaxial tension of original membrane, the light polarizing film of gained wide etc., can adopt the value needing.That is, A/B can adopt the value needing in 0.97～1.03 scope.
Identical with above-mentioned embodiment, can be according to cleaning the clean temperature in processing, the composition of detergent remover, clean time, described (A/B) controlled is 0.97～1.03.
Generally, by the clean temperature that raises, in detergent remover boronic acid containing or reduce containing ratio, increase the time of cleaning etc. not, and have the trend that reduces described (A/B).For described (A/B) being controlled in 0.7～0.98 scope, experimentally by clean temperature, detergent remover composition, clean time etc. and determine at certain point and (for example clean temperature: 15 ℃, detergent remover: water, the time of cleaning: 10 seconds etc.), clean processing, confirm the value of (A/B).Its result, if the value obtaining is not within the scope of this, consider that above-mentioned clean temperature, detergent remover form, clean the affect trend of condition on the value of (A/B) such as time, adjust each suitable condition, again clean processing, confirm the value of (A/B), repeatable operation, until value (A/B) is in 0.7～0.98 scope, thereby can adjust and determine each condition.
And clean number of times is not defined as 1 time, can in the scope of 2～4 left and right, at random select.
At clean number of times, for repeatedly time, by the wide Ap of being made as of film before initial clean processing, by the film after processing is wide while being made as Bp, preferably the full Ap/Bp cleaning before and after processing is 0.97～1.03.
And, identical with above-mentioned embodiment, boron compound content in the film of cleaning before processing is made as to Y, and when the boron compound content in the film after clean processing is made as X, the residual rate (X/Y) of preferably once cleaning the boron compound content in the film of processing front and back is 0.7～0.98.At clean number of times for repeatedly time, by the boron compound content in the film before initial clean processing be made as Yp, when the boron compound content in the film after finally clean processing is made as to Xp, preferably complete clean process before and after the residual rate of boron compound content in film be 0.7～0.98.Other formations are identical with above-mentioned embodiment, and therefore the description thereof will be omitted.
The manufacture method > of < Polarizer
At least one side in the above-mentioned light polarizing film making utilizes tackifier laminating diaphragm, and obtains Polarizer.As diaphragm; can give an example as; the film being formed by triacetyl cellulose, the such acetyl fibre prime system resin of diacetyl cellulose; the film being formed by polyethylene terephthalate, PEN, the such polyester based resin of polybutylene terephthalate; the film being formed by polycarbonate-based resin, the film being formed by cyclic olefine resin etc.As commercially available thermoplasticity cyclic olefine resin, can give an example as, " Upell " (trade mark) that " ZEONOR ", " ZEONEX " (being trade mark) that " ARTON " (trade mark) that topas (trade mark) the ,JSR company that Ticona (Ticona) company of Germany sells sells, JAPAN-Zeon company sell, Mitsui Chemicals, Inc. sell etc.Can adopt the film that makes such cyclic olefine resin film forming and obtain as diaphragm.In film forming, can adopt the known methods such as solvent casting method, extrusion by melting.The list marketing of cyclic olefine resin molding of making, " ェ ス シ mono-Na " sold such as ponding chemical industrial company etc. is suitable.
As the thickness of diaphragm, preferably thin, if but excessively thin, strength decreased, processability variation.And, if blocked up, produce the transparency and reduce, the problem such as curing time of needing after stacked is elongated.Therefore, the suitable thickness of diaphragm is that for example approximately 5～200 μ m left and right, are preferably approximately 10～150 μ m, are more preferably approximately 20～100 μ m.
In order to improve the tackiness between tackifier and light polarizing film and/or diaphragm, also can implement the surface treatments such as corona treatment, flame treatment, Cement Composite Treated by Plasma, ultraviolet ray irradiation, primary coat processing, saponification processing to light polarizing film and/or diaphragm.
Also can on diaphragm, implement alone or in combination the surface treatments such as non-glare treated, antireflection processing, hard painting processing, electrostatic prevention processing, antifouling processing.And diaphragm and/or diaphragm sealer can have the ultraviolet light absorbers such as benzophenone based compound, benzotriazole based compound, the plastifier such as phenyl phosphate based compound, phthalate compound.The diaphragm relating to can be fitted in the one side of light polarizing film, also can be fitted in two sides.
Can with hydrosolvent be tackifier, organic solvent be tackifier, hot melt be tackifier, solvent-free be that the tackifier such as tackifier come layered polarization film and diaphragm.As hydrosolvent, be tackifier, such as enumerating polyvinyl alcohol resin aqueous solution, water system two component polyurethane series emulsion adhesive etc.; As organic solvent, be tackifier, for example, can enumerate dual liquid type polyurethane series tackifier; As solvent-free be tackifier, such as enumerating one-pack-type polyurethane series tackifier etc.When acetylcellulose mesentery after the hydrophilicity-imparting treatment such as saponification processing is carried out in use as diaphragm to the bonding plane with light polarizing film, preferably use polyvinyl alcohol resin aqueous solution as tackifier.In the polyvinyl alcohol resin using as tackifier, except carrying out saponification, processes the alcotex obtaining the polyvinyl acetate of the homopolymer to as vinyl acetate, can exemplify into, the ethenol system interpolymer obtaining carrying out saponification processing with other monomers of vinyl acetate copolymerization and the multipolymer of vinyl acetate and partly to modified polyvinylalcohol based polymer after their hydroxyl modification etc.In this tackifier, can use polyaldehyde, soluble epoxide compound, melamine based compound etc. as adjuvant.
Method as laminating light polarizing film and diaphragm is not particularly limited, and can exemplify out, and at the surface uniform ground of light polarizing film or diaphragm coating binder, overlapping the opposing party's film on coated face, with laminatings such as rollers, carries out dry method etc.
After modulation, coating binder at the temperature of approximately 15～40 ℃, binding temperature is generally the scope of approximately 15～30 ℃ of left and right.After laminating, be dried processing, remove the water equal solvent containing in tackifier, baking temperature is now generally approximately 30～85 ℃, preferably the scope of approximately 40～80 ℃.Afterwards, also can approximately 15～85 ℃, preferably approximately 20～50 ℃, be more preferably under the environment temperature of approximately 35～45 ℃, conventionally carry out left and right slaking on the approximately 1st～90, make adhesive solidification.Long throughput rate variation of this curing time, so the curing time is about approximately 1～30 day, preferably approximately 1～7 day.
Like this, the one or two sides laminating diaphragm by adhesive layer in light polarizing film, obtains Polarizer.
In the present invention, the function, brightness that diaphragm can have a phase retardation film improve the function of film, the function of the function of reflectance coating, semipermeable reflection film, the optical functions such as function of the function of diffusion barrier, optical compensation films.Now; except having these functions by improving the optical functional films such as film, reflectance coating, semipermeable reflection film, diffusion barrier, optical compensation films such as stacked phase retardation film on the surface of diaphragm, brightness, also can give diaphragm self such function.And the mode of diffusion barrier etc. that also can make diaphragm self improve the function of film to have brightness has a plurality of functions.
For example, by said protection film is implemented to the stretch processing that JP2841377-B2, JP3094113-B2 etc. record, the processing that JP3168850-B2 etc. record, the function that can give phase retardation film.And; in said protection film, utilize the method for recording in JP2002-169025-A, JP2003-29030-A, form fine holes; the centre wavelength reflecting by overlapping selection is in addition 2 layers of different above cholesteryl liquid crystal layers, thereby can give the function that brightness improves film.By utilizing evaporation, sputter etc. to form metallic film, the function that can give reflectance coating or semipermeable reflection film in said protection film.By coating in said protection film, contain fine-grained resin solution, the function that can give diffusion barrier.And, by being coated with the liquid-crystal compoundss such as disc-like liquid crystal compound and making its orientation, the function that can give optical compensation films in said protection film.And, also can use suitable tackifier, the brightness such as trade name: DBEF (3M company system) of directly fitting in light polarizing film improve film, trade name: the commercially available optical functional films such as phase retardation film of visual angle improvement film, trade name: the Sumikalite (trade mark) (Sumitomo Chemical Co. Ltd.) etc. such as WV film (photograph film company of Fuji system).
Below, by embodiment, the present invention is described in more details, but the present invention is not limited to these embodiment.In addition, the assay method of each physical property, evaluation method are as follows.
(residual rate of boron compound content)
First, calculate the boron compound content in the film of cleaning before and after processing for 1 time.That is, each film 0.2g cleaning before and after processing is flooded 60 minutes respectively in the hot water 100ml of 95 ℃, after it is dissolved completely, each solution is carried out to acid-base titration, and calculate the boron compound content in each film by weight and the titer of film.Then, each value obtaining is brought in above-mentioned formula (I), calculate the residual rate of the boron compound content in the film before and after cleaning.
(have or not wrinkling, foreign matter defect occur)
Film is carried out to visualization.
[embodiment 1]
In 30 ℃ of pure water, in the unflagging mode of film, keep tense situation to flood approximately 100 seconds the polyvinyl alcohol film of wide 450mm, thick 75 μ m (saponification degree is more than 99.9 % by mole for Kuraray vinylon VF-PS#7500, the degree of polymerization 2400), make the abundant swelling of film.
Then, at iodine/potassium iodide/water, in the aqueous solution for 0.02/1.5/100, flood, carry out uniaxial tension simultaneously.Then, in being 12/4.4/100 the aqueous solution of 55 ℃ by weight, potassium iodide/boric acid/water floods, when carrying out boric acid processing (resistance to hydration process), carry out uniaxial tension until be 5.5 times with respect to the accumulation stretching ratio of raw material, afterwards, in being 9/2.9/100 the aqueous solution of 40 ℃ by weight, potassium iodide/boric acid/water floods.
Then, in the pure water of 5 ℃, dipping cleaned for 8 seconds.This is dried 3 minutes after cleaning and processing at 70 ℃, obtains the light polarizing film that thickness is 28 μ m.Before clean processing at this moment, in film, boron compound content is 4.25 % by weight, cleans after processing, and the boron compound content in film is 4.17 % by weight.And the residual rate of the boron compound content in the film before and after this is clean is 0.98, does not find to occur on film wrinkling in clean processing.And, do not find foreign matter defect, the light polarizing film obtaining has without misalignment, foreign defect, nothing beats the good outward appearances such as trace.In addition, described % by weight is the value of the film weight of (untreated) before processing with respect to swelling.
[embodiment 2]
2 ablution grooves are set, the first stage, at potassium iodide/boric acid/water by weight be clean 8 seconds of dipping in the aqueous solution of 15 ℃ of 0.3/0.15/100; Subordinate phase, in the pure water of 15 ℃, dipping is cleaned 3 seconds, in addition, identical with described embodiment 1, obtains the light polarizing film that thickness is 28 μ m.
Now the boron compound content in the film before the clean processing of first stage is 4.25 % by weight, and this boron compound content of cleaning in the film after processing is 4.03 % by weight.And the boron compound content in the film before the clean processing of subordinate phase is 4.03 % by weight, this boron compound content of cleaning in the film after processing is 3.95 % by weight.And the described residual rate of first stage is 0.95, the described residual rate of subordinate phase is 0.98, cleans in processing at each, does not find to occur in film wrinkling.
And, also do not find to occur foreign matter defect, the light polarizing film of gained has without misalignment, foreign defect, nothing beats the good outward appearances such as trace.
[embodiment 3]
Except at potassium iodide/boric acid/water by weight be in the aqueous solution of 25 ℃ of 0.6/0.3/100 clean 48 seconds of dipping, identical with described embodiment 1, obtain the light polarizing film that thickness is 28 μ m.Boron compound content in film before clean processing is now 4.25 % by weight, and this boron compound content of cleaning in the film after processing is 3.40 % by weight.And described residual rate is 0.80, in cleaning processing, do not find to occur in film wrinkling.And, also do not find to occur foreign matter defect, the light polarizing film of gained has without misalignment, foreign defect, nothing beats the good outward appearances such as trace.
[comparative example 1]
In the pure water at 35 ℃, dipping is cleaned 48 seconds, identical with described embodiment 1, obtain the light polarizing film that thickness is 29 μ m.Boron compound content in film before clean processing is now 4.25 % by weight, and the boron compound content of cleaning in the film after processing is 2.76 % by weight.And described residual rate is 0.65, in cleaning processing, in film, occur wrinkling.
[comparative example 2]
In the pure water at 2 ℃, dipping is cleaned 1 second, identical with described embodiment 1, obtain the light polarizing film that thickness is 28 μ m.Boron compound content in film before clean processing is now 4.25 % by weight, and this boron compound content of cleaning in the film after processing is 4.22 % by weight.And described residual rate is 0.99, although in clean processing, do not find to occur in film wrinkling, in short-term, beginning is separated out boric acid to roller, and foreign matter defect has occurred on film.
The evaluation result of described embodiment 1～3 and comparative example 1,2 is shown in table 1.
[table 1]
1) zero: in cleaning processing, do not find generation wrinkling, foreign matter defect, the light polarizing film obtaining has without misalignment, foreign defect, nothing beats the good outward appearances such as trace.
*: in cleaning processing, find generation wrinkling, foreign matter defect.
[embodiment 4]
In 30 ℃ of pure water, in the unflagging mode of film, keep tense situation to flood approximately 100 seconds the polyvinyl alcohol film of wide 450mm, thick 75 μ m (saponification degree is more than 99.9 % by mole for Kuraray vinylon VF-PS#7500, the degree of polymerization 2400), make the abundant swelling of film.
Then, at iodine/potassium iodide/water, in the aqueous solution for 0.02/1.5/100, flood, carry out uniaxial tension simultaneously.Then, in being 12/4.4/100 the aqueous solution of 55 ℃ by weight, potassium iodide/boric acid/water floods, when carrying out boric acid processing (resistance to hydration process), carry out uniaxial tension until be 5.5 times with respect to the accumulation stretching ratio of raw material (former anti-), afterwards, in being 9/2.9/100 the aqueous solution of 40 ℃ by weight, potassium iodide/boric acid/water floods.
Then, in the pure water of 5 ℃, dipping cleaned for 8 seconds.This is dried 3 minutes after cleaning and processing at 70 ℃, obtains the light polarizing film that thickness is 28 μ m.Before clean processing at this moment, in film, boron compound content is 4.25 % by weight, cleans after processing, and the boron compound content in film is 4.17 % by weight, and the residual rate of the boron compound content in the film before and after this is clean is 0.98.And the wide A of film before cleaning is 270mm, the wide B of film after cleaning is 271mm (A/B=1.00), cleans not find to occur on film in processing wrinkling, and the light polarizing film obtaining has without misalignment, foreign defect, without beating the good outward appearances such as trace.
[embodiment 5]
Two ablution grooves are set, the first stage, at potassium iodide/boric acid/water by weight be clean 8 seconds of dipping in the aqueous solution of 15 ℃ of 0.3/0.15/100; Subordinate phase, in the pure water of 15 ℃, dipping is cleaned 8 seconds, in addition, similarly obtains with described embodiment 4 light polarizing film that thickness is 28 μ m.
Now the boron compound content in the film before the clean processing of first stage is 4.25 % by weight, and this boron compound content of cleaning in the film after processing is 4.03 % by weight.And the boron compound content in the film before the clean processing of subordinate phase is 4.03 % by weight, this boron compound content of cleaning in the film after processing is 3.95 % by weight.And the described residual rate of first stage is 0.95, the described residual rate of subordinate phase is 0.98.
And, the clean front wide A of film of first stage is 270mm, the wide B of film after cleaning is 273mm (A/B=0.99), the clean front wide A of film of subordinate phase is 273mm, the wide B of film after cleaning is 278mm (A/B=0.98), each does not find to occur wrinkling in cleaning and processing, the light polarizing film of gained has without misalignment, foreign defect, nothing beats the good outward appearances such as trace.
[embodiment 6]
Except at potassium iodide/boric acid/water by weight be in the aqueous solution of 25 ℃ of 0.6/0.3/100 clean 48 seconds of dipping, identical with described embodiment 4, obtain the light polarizing film that thickness is 28 μ m.Boron compound content in film before clean processing is now 4.25 % by weight, and this boron compound content of cleaning in the film after processing is 3.40 % by weight, and described residual rate is 0.80.And the wide A of film before cleaning is 270mm, the wide B of film after cleaning is 278mm (A/B=0.97), in cleaning and processing, does not find to occur in film wrinkling, and the light polarizing film of gained has without misalignment, foreign defect, without beating the good outward appearances such as trace.
[comparative example 3]
In the pure water at 35 ℃, dipping is cleaned 48 seconds, identical with described embodiment 4, obtain the light polarizing film that thickness is 29 μ m.Boron compound content in film before clean processing is now 4.25 % by weight, and the boron compound content of cleaning in the film after processing is 2.76 % by weight, and described residual rate is 0.65.And the wide A of film before cleaning is 270mm, the wide B of film after cleaning is 282mm (A/B=0.96), in cleaning processing, occurs wrinkling in film.
[comparative example 4]
Except being immersed in potassium iodide/boric acid/water after stretching, be in 12/4.4/100 the aqueous solution of 55 ℃ by weight, beyond then in the pure water of 2 ℃, dipping is cleaned 1 second, identical with described embodiment 4, obtain the light polarizing film that thickness is 30 μ m.Boron compound content in film before clean processing is now 4.42 % by weight, and the boron compound content of cleaning in the film after processing is 4.37 % by weight, and described residual rate is 0.99.And the wide A of film before cleaning is 268mm, the wide B of film after cleaning is 258mm (A/B=1.04), in cleaning processing, foreign matter defect occurs in film.
The evaluation result of described embodiment 4～6 and comparative example 3,4 is shown in table 2.
[table 2]
Claims (11)
1. a manufacture method for light polarizing film, carries out successively swelling processing, dyeing processing, boric acid processing and cleans and process polyvinyl alcohol mesentery, before these are processed and/or in processing, carries out uniaxial tension, wherein,
By the boron compound content in the film before clean processing be made as Y, when the boron compound content in the film of cleaning after processing is made as to X, the residual rate X/Y that makes once to clean the boron compound content in the film before and after processing is 0.7～0.98.
2. method according to claim 1, wherein, at least carries out cleaning for 2 times and processes.
3. method according to claim 2, wherein, by the boron compound content in the film before initial clean processing be made as Yp, when the boron compound content in the film after last clean processing is made as to Xp, making the residual rate Xp/Yp of the boron compound content in the full film of cleaning before and after processing is 0.7～0.98.
4. method according to claim 1, wherein, by cleaning the wide A of being made as of film before processing, when cleaning that film after processing is wide is made as B, making the A/B once cleaning before and after processing is 0.97～1.03.
5. method according to claim 4, wherein, at least carries out cleaning for 2 times and processes.
6. method according to claim 5, wherein, by the wide Ap of being made as of film before initial clean processing, by the film after processing is wide while being made as Bp, making the full Ap/Bp cleaning before and after processing is 0.97～1.03.
7. according to the method described in claim 4 or 5, wherein, by the boron compound content in the film before clean processing be made as Y, when the boron compound content in the film of cleaning after processing is made as to X, the residual rate X/Y that makes once to clean the boron compound content in the film before and after processing is 0.7～0.98.
8. method according to claim 7, wherein, at least carry out 2 described clean processing, by the boron compound content in the film before initial clean processing be made as Yp, when the boron compound content in the film after last clean processing is made as to Xp, making the residual rate Xp/Yp of the boron compound content in the full film of cleaning before and after processing is 0.7～0.98.
9. according to the method described in any one in claim 1～6 and 8, wherein, the clean temperature of cleaning in processing is below 30 ℃.
10. method according to claim 7, wherein, the clean temperature of cleaning in processing is below 30 ℃.
The manufacture method of 11. 1 kinds of Polarizers, the diaphragm of fitting at least one side of the light polarizing film obtaining in the method with described in any one in claim 1～10.
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| KR101257648B1 (en) * | 2010-07-02 | 2013-04-29 | 닛폰고세이가가쿠고교 가부시키가이샤 | Polyvinyl alcohol film, method for producing polyvinyl alcohol film, polarizing film, and polarizing plate |
| JP6228359B2 (en) * | 2011-12-06 | 2017-11-08 | 住友化学株式会社 | Manufacturing method of polarizing film |
| US10114159B2 (en) | 2015-01-27 | 2018-10-30 | Lg Chem, Ltd. | Method for manufacturing polarizer and polarizer manufactured by the same |
| KR101746283B1 (en) * | 2015-01-27 | 2017-06-12 | 주식회사 엘지화학 | Method for manufacturing polarizer and polarizer manufactured by the same |
| JP6420747B2 (en) * | 2015-04-17 | 2018-11-07 | 日東電工株式会社 | Polarizer, polarizing plate, and method for producing polarizer |
| JP5956037B1 (en) * | 2015-08-11 | 2016-07-20 | 住友化学株式会社 | Polarizing film manufacturing method and manufacturing apparatus |
| JP6076449B1 (en) * | 2015-12-04 | 2017-02-08 | 住友化学株式会社 | Manufacturing method of polarizing film |
| JP6794106B2 (en) * | 2015-12-07 | 2020-12-02 | 住友化学株式会社 | Method of manufacturing polarizing film |
| JP2018091980A (en) * | 2016-12-02 | 2018-06-14 | 住友化学株式会社 | Polarizing film and manufacturing method of polarized laminate film |
| JP6594915B2 (en) * | 2017-01-06 | 2019-10-23 | 住友化学株式会社 | Manufacturing method of polarizing film |
| CN109782478B (en) * | 2019-03-21 | 2021-12-24 | 南京汉旗新材料股份有限公司 | TN/STN polarizing film hue control method |
| CN111025684B (en) * | 2019-12-31 | 2021-06-25 | 佛山纬达光电材料股份有限公司 | Manufacturing method of polarized PVA film for sunglasses and polarized PVA film |
| KR20230148329A (en) * | 2021-03-01 | 2023-10-24 | 닛토덴코 가부시키가이샤 | Polarizing film, polarizing film, image display panel, and image display device |
| CN114211792A (en) * | 2021-12-06 | 2022-03-22 | 恒美光电股份有限公司 | Polarizing film extension treatment device and process and polarizer |
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