CN104730611A - Optical laminate producing method - Google Patents
Optical laminate producing method Download PDFInfo
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- CN104730611A CN104730611A CN201410822343.6A CN201410822343A CN104730611A CN 104730611 A CN104730611 A CN 104730611A CN 201410822343 A CN201410822343 A CN 201410822343A CN 104730611 A CN104730611 A CN 104730611A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
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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
- 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
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- Optics & Photonics (AREA)
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- Crystallography & Structural Chemistry (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polarising Elements (AREA)
- Laminated Bodies (AREA)
Abstract
The invention relates to an optical laminate producing method and provides a method for producing a polarizing film with superior appearance. The method for producing an optical laminate in the embodiment of the invention comprises the following processes: producing a polarizing film on a resin base material by stretching and staining a laminate having the resin base material and a polyvinyl alcohol-based resin layer formed on one side of the resin base material; a cleaning step of immersing the laminate in a washing solution containing iodide for washing; and removing the washing solution in order that the adhesion amount of the washing solution in the resin base material side surface of the laminate is 0.005g / m2 or less, a step of drying the laminate.
Description
Technical field
The present invention relates to the manufacture method of the optical laminate with light polarizing film.
Background technology
For the liquid crystal indicator of representatively image display device, be configured with light polarizing film because of its image forming mode in the both sides of liquid crystal cells.As the manufacture method of light polarizing film, such as propose following methods: stretched by the duplexer with resin base material and polyvinyl alcohol (PVA) (PVA) resin, then implement dyeing process, resin base material obtains the method (such as Japanese Unexamined Patent Publication 2000-338329 publication) of light polarizing film.Utilize such method, the light polarizing film of thinner thickness can be obtained, therefore, it is possible to be conducive to the slimming of image display device in recent years and receive publicity.
But the light polarizing film using above-mentioned resin base material to make produces the apparent problems such as concavo-convex bad point sometimes.
Summary of the invention
the problem that invention will solve
The present invention makes to solve the problem, its main purpose is, provide the manufacture method of the improved light polarizing film of apparent problem such as concavo-convex bad point.
for the scheme of dealing with problems
About above-mentioned concavo-convex bad point, the present inventor etc. are studied, and its mechanism of result is as following supposition.That is, above-mentioned light polarizing film manufactures as follows: carried out stretching and dyeing by the duplexer with resin base material and PVA resin, then cleans with the cleaning fluid comprising iodide typically, finally carries out drying, thus manufactures.Herein, when carrying out drying under the state that duplexer left on surfaces has the cleaning fluid comprising iodide, compared with PVA resin (light polarizing film) side surface, on the resin base material side surface that hydrophobicity degree is high, iodide are separated out with larger particle diameter.Then, when the conveying of the duplexer conveying roller of such state or wound into rolls are reclaimed, due to the thinner thickness of light polarizing film, so infer that the shape of this precipitate is easily transferred to light polarizing film thus produces concavo-convex bad point.
The present inventor etc. are studied based on above-mentioned supposition, found that: by after utilizing the cleaning fluid comprising iodide to clean, the adhesion amount of the cleaning fluid on the resin base material side surface of above-mentioned duplexer is adjusted to the scope of regulation, then drying is carried out, thus can the apparent problems such as concavo-convex bad point be improved, this completes the present invention.
The manufacture method being laminated with the optical laminate of light polarizing film on resin base material of the present invention comprises following operation: undertaken stretching and dyeing by having the duplexer of resin base material with the one-sided polyvinyl alcohol resin layer being formed at this resin base material, thus make the operation of light polarizing film on this resin base material; The cleaning fluid that above-mentioned duplexer be impregnated in comprise iodide carries out the operation of cleaning; And, remove cleaning fluid, make the adhesion amount of the cleaning fluid on the resin base material side surface of above-mentioned duplexer be 0.005g/m
2below, then by the operation of above-mentioned duplexer drying.
In 1 embodiment, the water contact angle of the resin base material side surface of above-mentioned duplexer is 60 ° ~ 80 °.
In 1 embodiment, the thickness of above-mentioned light polarizing film is 0.5 μm ~ 15 μm.
In 1 embodiment, the iodide concentration in above-mentioned cleaning fluid is 0.5 % by weight ~ 10 % by weight.
In 1 embodiment, above-mentioned stretching comprises in water and stretching.
In 1 embodiment, the removal of the cleaning fluid on the resin base material side surface of above-mentioned duplexer is undertaken by wiping or blow gas.
According to another technical scheme of the present invention, provide optical laminate.Optical laminate of the present invention is obtained by above-mentioned manufacture method.
the effect of invention
According to the present invention, after the duplexer cleaning fluid comprising iodide being laminated with light polarizing film on resin base material is cleaned, the adhesion amount of the cleaning fluid on the resin base material side surface of this duplexer is adjusted to the scope of regulation, then drying is carried out, thus the precipitation of iodide can be suppressed, as its result, the apparent problems such as concavo-convex bad point can be improved.
Accompanying drawing explanation
Fig. 1 is the partial section of the duplexer of the preferred embodiment of the present invention.
Fig. 2 is the schematic diagram that the example being removed the drying process of the cleaning fluid of the resin base material side surface of duplexer by wiping is described.
Fig. 3 is the schematic diagram that the example being removed the drying process of the cleaning fluid of the resin base material side surface of duplexer by wiping is described.
Fig. 4 is the schematic diagram that the example being removed the drying process of the cleaning fluid of the resin base material side surface of duplexer by blow gas is described.
description of reference numerals
10 duplexers
11 resin base materials
12 polyvinyl alcohol resin layers (light polarizing film)
20 give damping roller
30 except liquid roller
40 scraper plates
50 blowning installations
60 dry components
Embodiment
Below, the preferred embodiment of the present invention is described, but the present invention is not limited to these embodiments.
The manufacture method of optical laminate of the present invention comprises following operation: undertaken stretching and dyeing by having the duplexer of resin base material with the one-sided polyvinyl alcohol resin layer being formed at this resin base material, thus make the operation of light polarizing film on this resin base material; The cleaning fluid that above-mentioned duplexer be impregnated in comprise iodide carries out the operation of cleaning; And, remove cleaning fluid, make the adhesion amount of the cleaning fluid on the resin base material side surface of above-mentioned duplexer be 0.005g/m
2below, then by the operation of above-mentioned duplexer drying.Below, each operation is described.
A. the production process of light polarizing film
A-1. duplexer
Fig. 1 is the partial section of the duplexer of the preferred embodiment of the present invention.Duplexer 10 has resin base material 11 and polyvinyl alcohol resin layer 12.Duplexer 10 makes by forming polyvinyl alcohol resin layer 12 on the resin base material 11 of strip.As the formation method of polyvinyl alcohol resin layer 12, method suitable arbitrarily can be adopted.Preferably, on resin base material 11, coating comprises the coating fluid of polyvinyl alcohol resin (hereinafter referred to as " PVA system resin "), carries out drying, thus forms PVA resin 12.
As the formation material of above-mentioned resin base material, thermoplastic resin suitable arbitrarily can be adopted.As thermoplastic resin, such as, can enumerate: ethylene series resin, polyamide series resin, polycarbonate-based resin, their copolymer resins etc. such as cyclic olefine resin, polypropylene such as ester system resin, norbornene resin such as PET series resin.Wherein, norbornene resin, amorphous PET series resin is preferably.
In 1 embodiment, preferably use amorphous (non-crystallization) PET series resin.Wherein, non-crystalline (being difficult to crystallization) PET series resin is particularly preferably used.As the concrete example of non-crystalline PET series resin, can enumerate: comprise further m-phthalic acid as dicarboxylic acid multipolymer, comprise the multipolymer of cyclohexanedimethanol as glycol further.
When adopting stretching mode in water in aftermentioned stretching, above-mentioned resin base material absorbs water, and water plays the effect of plastifier, can carry out plasticized.Its result, can make drawing stress reduce significantly, can stretch with high magnification, and compared with when stretching in the air, stretchability can be more excellent.Its result, can make the light polarizing film with excellent optical characteristics.In 1 embodiment, the water-intake rate of resin base material is preferably more than 0.2%, more preferably more than 0.3%.On the other hand, the water-intake rate of resin base material is preferably less than 3.0%, more preferably less than 1.0%.By using such resin base material, when can prevent from manufacturing, dimensional stability obviously reduces and the unfavorable conditions such as the deteriorated appearance of gained light polarizing film.In addition, when can stretch in anti-sealing, base material fracture or PVA resin are peeled off from resin base material.It should be noted that, the water-intake rate of resin base material such as by importing modified group to adjust in formation material.Water-intake rate is the value obtained according to JIS K 7209.
The glass transition temperature (Tg) of resin base material is preferably less than 170 DEG C.By using such resin base material, the crystallization of PVA resin can be suppressed, and the stretchability of duplexer can be guaranteed fully.And then, utilize the plasticized of the resin base material of water if consider and carry out well stretching in water, being then more preferably less than 120 DEG C.In 1 embodiment, the glass transition temperature of resin base material is preferably more than 60 DEG C.By using such resin base material, the coating fluid comprising above-mentioned PVA system resin is carried out coating and dry time, resin base material can be prevented to be out of shape unfavorable conditions such as (generations of such as concavo-convex, lax, fold etc.), duplexer can be made well.In addition, at suitable temperature (such as about 60 DEG C), the stretching of PVA resin can be carried out well.In other embodiments, the coating fluid comprising PVA system resin is carried out coating and dry time, as long as resin base material is indeformable, then also can be the glass transition temperature lower than 60 DEG C.It should be noted that, the glass transition temperature of resin base material such as can by be used in formed in material import modified group, crystallised material carry out heating thus adjusting.Glass transition temperature (Tg) is the value obtained according to JIS K 7121.
Thickness before the stretching of resin base material is preferably 20 μm ~ 300 μm, is more preferably 50 μm ~ 200 μm.When being less than 20 μm, the formation of PVA resin is had to become the worry of difficulty.During more than 300 μm, such as, in stretching in water, having resin base material to absorb water needs the long period, and stretching needs the worry of excessive load.
As the PVA system resin forming above-mentioned PVA resin, resin suitable arbitrarily can be adopted.Such as can enumerate polyvinyl alcohol (PVA), ethylene-vinyl alcohol copolymer.Polyvinyl alcohol (PVA) is by obtaining saponifying polyvinyl acetate.Ethylene-vinyl alcohol copolymer is by obtaining vinyl-vinyl acetate copolymer saponification.The saponification degree of PVA system resin is generally 85 % by mole ~ 100 % by mole, is preferably 95.0 % by mole ~ 99.95 % by mole, more preferably 99.0 % by mole ~ 99.93 % by mole.Saponification degree can be obtained according to JIS K 6726-1994.By using the PVA system resin of such saponification degree, the light polarizing film of excellent in te pins of durability can be obtained.When saponification degree is too high, there is the worry that gelation occurs.
The average degree of polymerization of PVA system resin suitably can be selected according to object.Average degree of polymerization is generally 1000 ~ 10000, is preferably 1200 ~ 5000, more preferably 1500 ~ 4500.It should be noted that, average degree of polymerization can be obtained according to JIS K 6726-1994.
Above-mentioned coating fluid is typically for making above-mentioned PVA system resin dissolves in the solution of solvent.As solvent, such as, can enumerate: the amines such as polyalcohols, ethylenediamine, diethylenetriamine such as water, dimethyl sulfoxide (DMSO), dimethyl formamide, dimethyl acetamide, 1-METHYLPYRROLIDONE, various glycols, trimethylolpropane.They can be used alone, or are used in combination of two or more.Wherein, water is preferably.The PVA system resin concentration of solution is preferably 3 weight portion ~ 20 weight portions relative to 100 parts by weight solvent.If be such resin concentration, then can form the uniform coated film closely sealed with resin base material.
Can compounding adjuvant in coating fluid.As adjuvant, such as, plastifier, surfactant etc. can be enumerated.As plastifier, such as, can enumerate the polyvalent alcohol such as ethylene glycol, glycerine.As surfactant, such as, non-ionic surfactant can be enumerated.These adjuvants can in order to improve the homogeneity of gained PVA resin further, dyeability, stretchability use.In addition, as adjuvant, such as, can enumerate easy bonding composition.By using easy bonding composition, the adaptation of resin base material and PVA resin can be improved.Its result, such as, can suppress PVA resin from unfavorable conditions such as base material strippings, can carry out well stretching in aftermentioned dyeing, water.
As above-mentioned easy bonding composition, such as, the modified PVAs such as acetoacetyl modified PVA can be used.As acetoacetyl modified PVA, the polymkeric substance at least with the repetitive shown in following general formula (I) preferably can be used.
In above-mentioned formula (I), n is preferably 1% ~ 10% relative to the ratio (modification degree) of l+m+n.
The saponification degree of acetoacetyl modified PVA is preferably more than 97 % by mole.In addition, the pH of 4 % by weight aqueous solution of acetoacetyl modified PVA is preferably 3.5 ~ 5.5.
Modified PVA preferably adds with more than 3 % by weight of the weight of PVA system resin entirety contained in above-mentioned coating fluid, and more preferably more than 5 % by weight.On the other hand, the addition of this modified PVA is preferably less than 30 % by weight.
As the coating process of coating fluid, method suitable arbitrarily can be adopted.Such as can enumerate: rolling method, spin-coating method, line rod rubbing method, dip coating, mould are coated with method, curtain painting method, spraying process, scraper for coating method (comma rubbing method etc.) etc.
Coating/the baking temperature of above-mentioned coating fluid is preferably more than 50 DEG C.
Thickness before PVA resin stretches is preferably 3 μm ~ 40 μm, is preferably 5 μm ~ 20 μm.
Before formation PVA resin, surface treatment (such as corona treatment etc.) can be implemented to resin base material, also can form easy adhesive linkage on resin base material.Wherein, easy adhesive linkage (coating process) is preferably formed.As the material forming easy adhesive linkage, such as, acrylic resin, polyvinyl alcohol resin etc. can be used, particularly preferably polyvinyl alcohol resin.As polyvinyl alcohol resin, such as, can enumerate polyvinyl alcohol resin and modifier thereof.As the modifier of polyvinyl alcohol resin, above-mentioned acetoacetyl modified PVA can be enumerated.It should be noted that, the thickness of easy adhesive linkage is preferably set to about 0.05 ~ 1 μm.By carrying out such process, the adaptation of resin base material and PVA resin can be improved.Its result, such as, can suppress PVA resin from unfavorable conditions such as base material strippings, can carry out well stretching in aftermentioned dyeing, water.
The water contact angle of the resin base material side surface of duplexer is generally 60 ° ~ 80 °, such as, be 65 ° ~ 75 °.Water contact angle utilizes sessile drop method to measure.
A-2. the stretching of duplexer
As the drawing process of duplexer, method suitable arbitrarily can be adopted.Specifically, can stretch for stiff end, also can stretch for free end (such as by duplexer between the roller that peripheral speed is different by carrying out the method for uniaxial tension).Be preferably free end to stretch.
The draw direction of duplexer can suitably set.In 1 embodiment, the length direction along the duplexer of strip stretches.In above-mentioned situation, adopt typically by duplexer between the roller that peripheral speed is different by carrying out the method stretched.In other embodiments, the Width along the duplexer of strip stretches.In above-mentioned situation, adopt typically and use tentering drawing machine to carry out the method stretched.
Being not particularly limited stretching mode, can be aerial stretching mode, also can be stretching mode in water.Be preferably stretching mode in water.Utilize stretching mode in water, can stretch at the temperature of the glass transition temperature (being about 80 DEG C typically) lower than above-mentioned resin base material, PVA resin, for PVA resin, its crystallization can be suppressed, and stretch with high magnification.Its result, can make the light polarizing film with excellent optical characteristics.
The stretching of duplexer can be carried out with one-phase, also can carry out with the multistage.When carrying out with the multistage, such as, can combine above-mentioned free end and stretch and stiff end stretching, also can combine stretching mode and aerial stretching mode in above-mentioned water.In addition, when carrying out with the multistage, the stretching ratio that the stretching ratio (maximum tension multiplying power) of aftermentioned duplexer is each stage long-pending.
The draft temperature of duplexer can be set as value suitable arbitrarily according to the formation material, stretching mode etc. of resin base material.When adopting aerial stretching mode, draft temperature is preferably more than the glass transition temperature (Tg) of resin base material, and more preferably the glass transition temperature (Tg) more than+10 DEG C of resin base material, is particularly preferably more than Tg+15 DEG C.On the other hand, the draft temperature of duplexer is preferably less than 170 DEG C.By stretching at such temperatures, the crystallization of PVA system resin can be suppressed to advance fast, the unfavorable condition (such as hindering the orientation utilizing the PVA resin carried out that stretches) caused by this crystallization can be suppressed.
When adopting stretching mode in water, the liquid temperature of stretch bath is preferably 40 DEG C ~ 85 DEG C, is more preferably 50 DEG C ~ 85 DEG C.If be such temperature, then can suppress the dissolving of PVA resin, and stretch with high magnification.Specifically, as described above, the glass transition temperature (Tg) of resin base material is formed with relation with PVA resin, is preferably more than 60 DEG C.In above-mentioned situation, when draft temperature is lower than 40 DEG C, even if consider the plasticized utilizing the resin base material of water, also there is the worry cannot carrying out well stretching.On the other hand, the temperature of stretch bath is higher, and the dissolubility of PVA resin is higher, has the worry that cannot obtain excellent optical characteristics.The dip time of duplexer in stretch bath is preferably 15 seconds ~ 5 minutes.
When adopting stretching mode in water, preferably make duplexer impregnated in boric acid aqueous solution and carry out stretch (stretching in boric acid water).By using boric acid aqueous solution as stretch bath, the rigidity of the tension force applied when can give resistance to Tensile to PVA resin and be not dissolved in the water tolerance of water.Specifically, boric acid can generate tetrahydroxy acid anion in aqueous, is cross-linked by hydrogen bond with PVA system resin.Its result, can give rigidity and water tolerance to PVA resin, stretch well, can make the light polarizing film with excellent optical characteristics.
Above-mentioned boric acid aqueous solution obtains preferably by making boric acid and/or borate be dissolved in the water as solvent.Boric acid concentration is preferably 1 weight portion ~ 10 weight portion relative to 100 weight parts waters.By boric acid concentration is set to more than 1 weight portion, effectively can suppresses the dissolving of PVA resin, the light polarizing film of higher characteristic can be made.It should be noted that, can also to use except boric acid or borate also by boron compounds such as boraxs, glyoxal, glutaraldehyde etc. is dissolved in solvent and the aqueous solution obtained.
By aftermentioned dyeing, when being adsorbed with dichroic substance (being iodine typically) in advance on PVA resin, preferably compounding iodide in above-mentioned stretch bath (boric acid aqueous solution).By compounding iodide, can restrain adsorption in the stripping of the iodine of PVA resin.As iodide, such as, can enumerate: potassium iodide, lithium iodide, sodium iodide, zinc iodide, silver iodide, lead iodide, cupric iodide, barium iodide, calcium iodide, stannic iodide, titanium iodide etc.Wherein, potassium iodide is preferably.The relative concentration of iodide is preferably 0.05 weight portion ~ 15 weight portion in 100 weight parts waters, is more preferably 0.5 weight portion ~ 8 weight portion.
The stretching ratio (maximum tension multiplying power) of duplexer is preferably more than 5.0 times relative to the raw footage of duplexer.High stretching ratio so such as can realize by adopting stretching mode (stretching in boric acid water) in water.It should be noted that, in this instructions, " maximum tension multiplying power " refers to that duplexer is about to the stretching ratio before rupturing, and in addition, refers to and confirms the stretching ratio of duplexer fracture, the value of lower than its value 0.2.
In a preferred embodiment, above-mentioned duplexer is stretched in the air under high temperature (such as more than 95 DEG C), then carry out stretching and aftermentioned dyeing in above-mentioned boric acid water.Aerial stretching like this can orientate preparation stretching for stretching in boric acid water or assisting tension as, therefore hereinafter referred to as " aerial assisting tension ".
By combining aerial assisting tension, sometimes can with more high magnification stretching duplexer.Its result, can make the light polarizing film with more excellent optical characteristics (such as degree of polarization).Such as, when using PET series resin as above-mentioned resin base material, and carrying out by means of only stretching in boric acid water compared with stretching, combining when stretching in aerial assisting tension and boric acid water, stretching while resin base material orientation can be suppressed.Along with the raising of its orientation, tensile stress becomes large to this resin base material, and stable stretching becomes difficulty or ruptures.Therefore, by stretching with suppressing resin base material orientation, can with more high magnification stretching duplexer.
In addition, by combining aerial assisting tension, the orientation of PVA system resin can be improved, thus, after stretching in boric acid water, also can improve the orientation of PVA system resin.Specifically, be presumed as follows: by the orientation utilizing aerial assisting tension to improve PVA system resin in advance, when stretching in boric acid water, PVA system resin becomes easily crosslinked with boric acid, stretch under the state that boric acid becomes tie point, thus after stretching in boric acid water, the orientation of PVA system resin is also high.Its result, can make the light polarizing film with excellent optical characteristics (such as degree of polarization).
Stretching ratio in aerial assisting tension is preferably less than 3.5 times.The draft temperature of aerial assisting tension is preferably more than the glass transition temperature of PVA system resin.Draft temperature is preferably 95 DEG C ~ 150 DEG C.It should be noted that, the maximum tension multiplying power combined when stretching in aerial assisting tension and above-mentioned boric acid water is preferably more than 5.0 times relative to the raw footage of duplexer, is more preferably more than 5.5 times, more preferably more than 6.0 times.
A-3. dye
The dyeing of above-mentioned duplexer is adsorbed in PVA resin to carry out typically by making dichroic substance (being preferably iodine).As this adsorption method, such as, can enumerate: make PVA resin (duplexer) impregnated in the method for the dyeing liquor comprising iodine; PVA resin applies the method for this dyeing liquor; This dyeing liquor is sprayed to the method etc. of PVA resin.Duplexer is preferably made to impregnated in the method for dyeing liquor.This is because, iodine can adsorb well.
Above-mentioned dyeing liquor is preferably iodine aqueous solution.The compounding amount of iodine is preferably 0.1 weight portion ~ 0.5 weight portion relative to 100 weight parts waters.In order to improve the solubleness of iodine in water, preferably compounding iodide in iodine aqueous solution.The concrete example of iodide is described above.The compounding amount of iodide is preferably 0.02 weight portion ~ 20 weight portion relative to 100 weight parts waters, is more preferably 0.1 weight portion ~ 10 weight portion.Liquid temperature during dyeing for dyeing liquor, in order to suppress the dissolving of PVA system resin, is preferably 20 DEG C ~ 50 DEG C.When making PVA resin impregnated in dyeing liquor, for dip time, in order to ensure the transmitance of PVA resin, be preferably 5 seconds ~ 5 minutes.In addition, dyeing condition (concentration, liquid temperature, dip time) can be set, make the degree of polarization of the light polarizing film finally obtained or singleton transmittance be the scope specified.In 1 embodiment, setting dip time, makes the degree of polarization of gained light polarizing film be more than 99.98%.In other embodiments, setting dip time, makes the singleton transmittance of gained light polarizing film be 40% ~ 44%.
Dyeing process can be carried out under opportunity suitable arbitrarily.When carrying out stretching in above-mentioned water, carry out before preferably stretching in water.
A-4. other process
Above-mentioned duplexer, except stretching, dyeing, suitably can also implement the process being used for its PVA resin being made light polarizing film.As the process for making light polarizing film, such as, can enumerate insoluble process, crosslinking Treatment etc.It should be noted that, the number of times, order etc. of these process are not particularly limited.
Above-mentioned insoluble process is carried out typically by being impregnated in boric acid aqueous solution by PVA resin.By implementing insoluble process, water tolerance can be given to PVA resin.The relative concentration of this boric acid aqueous solution is preferably 1 weight portion ~ 4 weight portion in 100 weight parts waters.The liquid temperature of insoluble bath (boric acid aqueous solution) is preferably 20 DEG C ~ 50 DEG C.Insoluble process is preferably carried out before stretching, above-mentioned dyeing process in above-mentioned water.
Above-mentioned crosslinking Treatment is carried out typically by being impregnated in boric acid aqueous solution by PVA resin.By implementing crosslinking Treatment, water tolerance can be given to PVA resin.The relative concentration of this boric acid aqueous solution is preferably 1 weight portion ~ 5 weight portion in 100 weight parts waters.In addition, when carrying out crosslinking Treatment after above-mentioned dyeing process, preferred further compounding iodide.By compounding iodide, can restrain adsorption in the stripping of the iodine of PVA resin.The compounding amount of iodide is preferably 1 weight portion ~ 5 weight portion relative to 100 weight parts waters.The concrete example of iodide is described above.The liquid temperature of crosslinked bath (boric acid aqueous solution) is preferably 20 DEG C ~ 60 DEG C.Crosslinking Treatment is carried out before preferably stretching in above-mentioned water.In a preferred embodiment, carry out successively stretching in dyeing process, crosslinking Treatment and water.
A-5. light polarizing film
Above-mentioned light polarizing film is essentially the PVA resin film that gas absorption quantity has dichroic substance.The thickness of light polarizing film is less than 25 μm typically, is preferably less than 15 μm, is more preferably less than 10 μm, more preferably less than 7 μm, is particularly preferably less than 5 μm.On the other hand, the thickness of light polarizing film is preferably more than 0.5 μm, is more preferably more than 1.5 μm.Absorption dichromatism is demonstrated under any wavelength of light polarizing film preferably in wavelength 380nm ~ 780nm.The singleton transmittance of light polarizing film is preferably more than 40.0%, be more preferably more than 41.0%, more preferably more than 42.0%, be particularly preferably more than 43.0%.The degree of polarization of light polarizing film is preferably more than 99.8%, is more preferably more than 99.9%, more preferably more than 99.95%.
B. matting
In matting, make the duplexer being laminated with light polarizing film on resin base material obtained in the production process of above-mentioned light polarizing film impregnated in the cleaning fluid comprising iodide and clean.The concrete example of iodide is described above, is preferably potassium iodide.In 1 embodiment, cleaning fluid is potassium iodide aqueous solution.Iodide concentration in cleaning fluid is preferably 0.5 % by weight ~ 10 % by weight, is preferably 0.5 % by weight ~ 5 % by weight, is more preferably 1 % by weight ~ 4 % by weight.The temperature of cleaning fluid is generally 10 DEG C ~ 50 DEG C, is preferably 20 DEG C ~ 35 DEG C.Dip time is generally 1 second ~ 1 minute, is preferably 10 seconds ~ 1 minute.When cleaning insufficient, sometimes separate out boric acid from gained light polarizing film.
C. drying process
In drying process, remove cleaning fluid, make the adhesion amount of the cleaning fluid on the resin base material side surface of duplexer cleaned in above-mentioned matting be 0.005g/m
2below, 0.003g/m is preferably
2below, 0.002g/m is more preferably
2below, then that this duplexer is dry.Will with more than 0.005g/m on resin base material side surface
2amount be attached with cleaning fluid duplexer for drying process time, sometimes produce the concavo-convex bad point (such as diameter is the concavo-convex bad point of more than 150 μm) of visual size.
It should be noted that, after matting terminates, until being in general within 60 seconds for the time till drying process, in addition, the conveying of duplexer is owing at room temperature carrying out, therefore do not need the concentration change of cleaning fluid considering to be caused by natural drying etc., but the removal of above-mentioned cleaning fluid preferably duplexer by after cleaner bath immediately (within such as 30 seconds, preferably 15 seconds within) carry out.
The removal of above-mentioned cleaning fluid can utilize method suitable arbitrarily to carry out.The removal of cleaning fluid such as can be carried out by the cleaning fluid of the resin base material side surface of the above-mentioned duplexer of wiping or to this surperficial blow gas.
The wiping of cleaning fluid can utilize suction roll, carry out except Wiping members suitable arbitrarily such as liquid roller, scraper plates.Wiping member can be used alone, and also can use multiple by a kind of Wiping member, can also combine two or more Wiping members to use.Fig. 2 and Fig. 3 is respectively the schematic diagram that the example being removed the drying process of the cleaning fluid of the resin base material side surface of duplexer by wiping is described.
During use suction roll (with reference to Fig. 2), such as, the mode rotated with the conveying along with the above-mentioned duplexer 10 after dipping in cleaner bath 100, makes suction roll 20 contact with resin base material 11 side surface of duplexer 10.For suction roll, typically, surface is formed by porosints such as sponge, nonwoven fabrics, fabrics.As sponge, polyurethane sponge, cellular rubber, polyolefin sponge can be enumerated.Roller diameter is such as 80mm ~ 110mm.It should be noted that, 110 in figure is conveying roller.
Use except (with reference to Fig. 2 and Fig. 3) during liquid roller, such as, to clamp the mode of above-mentioned duplexer 10, make to remove liquid roller 30 for a pair and be oppositely disposed.Except liquid roller 30 while rotate along with the conveying of above-mentioned duplexer 10, from pros and cons extruding duplexer 10, carry out thus except liquid.Except liquid roller is rubber system typically.In addition, except liquid roller can have crown shape.By having crown shape, can carry out equably except liquid throughout the Width ground of duplexer.
When using scraper plate 40 (with reference to Fig. 3), typically, configuration scraper plate 40, makes the resin base material 11 side surface sliding contact of its front end and the above-mentioned duplexer 10 alongst carried.By being so configured, utilize scraper plate 40 from its resin base material 10 side surface wiping water along with the conveying of duplexer 10.As the formation material of scraper plate, rubber, resin, metal etc. can be enumerated.For the part of scraper plate and above-mentioned duplexer sliding contact, scratching from the view point of avoiding producing, can chamfer machining be curve shape.
Resin base material side surface blow gas to duplexer can use commercially available blowning installation to carry out.Fig. 4 is the schematic diagram that the example being removed the drying process of the cleaning fluid of the resin base material side surface of duplexer by blow gas is described.The mode that blowning installation 50 is preferably 25 ° ~ 65 ° with air relative to the spray angle of resin base material 11 side surface of duplexer 10 configures.The condition of blowing suitably can set according to the kind etc. of resin base material.The pressure of air is such as 20 ~ 25KPa.The wind speed of air is such as 20 ~ 60m/min.It should be noted that, as illustrated example, Wiping member (for suction roll 20 with except liquid roller 30 in illustrated example) and blowning installation 50 can be combinationally used.
The drying of removing the duplexer after cleaning fluid can be undertaken by drying means suitable arbitrarily such as natural drying, air-supply drying, heat drying, heated-air dryings.Be preferably the heat drying using the heaters 60 such as baking oven.Baking temperature is such as 30 DEG C ~ 100 DEG C, is preferably 40 DEG C ~ 100 DEG C.Drying time suitably can set according to baking temperature, such as, be 10 seconds ~ 10 minutes.
D. optical laminate
The optical laminate of the present invention obtained through above-mentioned drying process possesses resin base material and is formed at its one-sided light polarizing film.Optical laminate of the present invention utilizes take-up mechanism to coil into web-like typically, for the operation etc. of the stacked optical functional film in the light polarizing film side (such as diaphragm) of taking care of or at duplexer.Optical laminate of the present invention is described above, owing to carrying out drying under the state of attachment decreasing the cleaning fluid on resin base material side surface, so the precipitation of iodide on resin base material side surface can be suppressed.Its result, even if when gained optical laminate is coiled into web-like, also can suppress the distortion of the light polarizing film caused by precipitate (as the result of this distortion, causing concavo-convex bad point).
The optical functional film duplexer (having the structure of [resin base material/light polarizing film/optical functional film]) being laminated with optical functional film directly can be used as Polarizer.Or; also resin base material can be peeled off from this optical functional film duplexer; stacked other optical functional films (such as diaphragm) in this release surface, are had the Polarizer of the structure of [optical functional film/light polarizing film/optical functional film].
Embodiment
Below, specifically describe the present invention by embodiment, but the present invention is not limited to these embodiments.It should be noted that, the assay method of each characteristic as described below.
1. thickness
Digital micrometer (manufacture of ANRITSU Co., Ltd., ProductName " KC-351C ") is used to measure.
2. glass transition temperature (Tg)
Measure according to JIS K 7121.
3. water contact angle
Use consonance interface science Co., Ltd. to manufacture automatic contact angle meter DM500 to measure, use FAMAS (contact angle determination Add-ons) to analyze.
4. the evaluation of concavo-convex bad point
The backlight side of 32 inches of TVs (model: THL32C3) that the 32 inches of TVs (model: LC32-SC1) manufacture SHARP and Panasonic manufacture and the light polarizing film depending on recognizing side are peeled off, replacing this light polarizing film, using bonding agent the optical laminate obtained in embodiment or comparative example to be pasted on backlight side and depending on recognizing side.In darkroom, light liquid crystal indicator be black display state, counting is the bright spot number of more than 150 μm depending on the major diameter recognized in region.
5. the mensuration of the amount of moisture of the resin base material side surface of duplexer
Make suction roll contact certain hour with the resin base material side surface of duplexer, absorb moisture, then gravimetry, measure the amount of moisture of per unit area according to the variable quantity of weight.
[embodiment 1]
As resin base material, use noncrystalline polyethylene terephthalate (A-PET) film (Mitsubishi chemical Co., Ltd's manufacture, trade name " NOVA CLEAR ", thickness: 100 μm) of strip and water-intake rate 0.60%, Tg80 DEG C, elastic modulus 2.5GPa.
Corona treatment (treatment conditions: 55Wmin/m are implemented to the one side of resin base material
2); at 60 DEG C; the aqueous solution comprising polyvinyl alcohol (PVA) (degree of polymerization 4200, saponification degree 99.2 % by mole) 90 weight portions and acetoacetyl modified PVA (degree of polymerization 1200, acetoacetyl modified degree 4.6%, saponification degree more than 99.0 % by mole, the Nippon Synthetic Chemical Industry Co., Ltd's manufacture, trade name " Gohsefimer Z200 ") 10 weight portions is coated this corona treatment face and drying; form the PVA resin of thickness 10 μm, make duplexer.The water contact angle of the resin base material side surface of gained duplexer is 60 °.
By gained duplexer in the baking oven of 120 DEG C, between the roller that peripheral speed is different, (length direction) free end uniaxial tension (aerial assisting tension) is to 1.8 times along the longitudinal.
Then, duplexer is made to impregnated in the insoluble bath (boric acid aqueous solution obtained for compounding 4 part by weight of boric acid of 100 weight parts waters) 30 seconds (insoluble process) of liquid temperature 30 DEG C.
Then, its dye bath that impregnated in liquid temperature 30 DEG C (for the iodine of compounding 0.2 weight portion of 100 weight parts waters, the potassium iodide of compounding 1.0 weight portions and the iodine aqueous solution that obtains) 60 seconds (dyeing process) is made.
Then, its crosslinked bath that impregnated in liquid temperature 30 DEG C (for the potassium iodide of compounding 3 weight portions of 100 weight parts waters, the boric acid of compounding 3 weight portions and the boric acid aqueous solution obtained) 30 seconds (crosslinking Treatment) is made.
Then, make duplexer while impregnated in the boric acid aqueous solution (for the boric acid of compounding 4 weight portions of 100 weight parts waters, the potassium iodide of compounding 5 weight portions and the aqueous solution obtained) of liquid temperature 70 DEG C, between the roller that peripheral speed is different, (length direction) carries out uniaxial tension (stretching in water) along the longitudinal.Herein, carry out stretching till duplexer is about to before fracture (maximum tension multiplying power is 6.0 times).
Then, duplexer is made to impregnated in cleaner bath (for the potassium iodide of compounding 4 weight portions of 100 weight parts waters and the aqueous solution obtained) (cleaning treatment) of liquid temperature 30 DEG C.
Then, as shown in Figure 2, the cleaning fluid of the resin base material side surface of duplexer is removed.Specifically, use a pair rubber except liquid roller, that carries out that self-cleaning bathe the duplexer transported removes liquid, then, configures 3 suction rolls (formed by polyurethane sponge material in the mode contacted with the resin base material side surface of duplexer
roller), make roller rotate along with the conveying of duplexer, thus wiping cleaning fluid.
Afterwards, in the baking oven being maintained 60 DEG C, carry duplexer, heat 5 minutes, make the optical laminate with the light polarizing film of thickness 5 μm.Then, gained optical laminate take-up mechanism is coiled into web-like.It should be noted that, the amount of moisture (adhesion amount of cleaning fluid) on the resin base material side surface of the duplexer (just having passed through the 3rd to after damping roller) after just having removed cleaning fluid is 0.0016g/m
2.
[embodiment 2]
Replace suction roll to use blowning installation to remove the cleaning fluid of the resin base material side surface of duplexer, in addition, operate similarly to Example 1, make optical laminate, coil into web-like with take-up mechanism.The removal of cleaning fluid is specifically carried out as described below.Namely, what use a pair rubber removes liquid roller, carry out self-cleaning bathe the duplexer transported except liquid, then, 45 ° are about relative to the resin base material side surface of duplexer and the mode that the distance on injection orifice and this surface is about 2cm configures blowning installation (Hitachi Industrial Equipment Systems Co. with the spray angle of air, Ltd. manufacture, production code member " VB-060-E2 "), spray air.The pressure of air is 23kPa.In addition, the wind speed of air is 30m/min.It should be noted that, after just having removed cleaning fluid, the amount of moisture (adhesion amount of cleaning fluid) of the resin base material side surface of the duplexer of (after just spraying air) is 0.0045g/m
2.
[comparative example 1]
Use except liquid roller carries out, except liquid, not carrying out the removal of further cleaning fluid afterwards, and being delivered in baking oven by duplexer, in addition, operate similarly to Example 1, make optical laminate, coil into web-like with take-up mechanism.The amount of moisture (adhesion amount of cleaning fluid) being about to the resin base material side surface of the duplexer before being delivered to baking oven is 0.0064g/m
2.
The evaluation of the concavo-convex bad point in each embodiment and comparative example is shown in table 1.It should be noted that, panel is evaluated according to following benchmark depending on the quality of recognizing in region.
[metewand]
Good: in darkroom, to light liquid crystal indicator when being black display state, do not have major diameter to be the bright spot of more than 150 μm depending on recognizing in region.
Bad: in darkroom, to light liquid crystal indicator when being black display state, there is major diameter to be the bright spot of more than 150 μm depending on recognizing in region.
[table 1]
As shown in table 1, by dry duplexer under the state that the adhesion amount of the cleaning fluid on the resin base material side surface of duplexer is reduced to the scope of regulation, thus concavo-convex bad point can be reduced.
utilizability in industry
Optical laminate of the present invention suitablely can be used as the liquid crystal panel of LCD TV, liquid crystal display, mobile phone, digital camera, Digital Video, portable game, automated navigation system, duplicating machine, printer, facsimile recorder, clock and watch, electric stove etc., the antireflection film of organic el device.
Claims (7)
1. a manufacture method, it is the manufacture method of the optical laminate being laminated with light polarizing film on resin base material,
Described manufacture method comprises following operation:
Undertaken stretching and dyeing by having the duplexer of resin base material with the one-sided polyvinyl alcohol resin layer being formed at this resin base material, thus make the operation of light polarizing film on this resin base material;
The cleaning fluid that described duplexer be impregnated in comprise iodide carries out the operation of cleaning; And
Remove cleaning fluid, make the adhesion amount of the cleaning fluid on the resin base material side surface of described duplexer be 0.005g/m
2below, then by the operation of described duplexer drying.
2. manufacture method according to claim 1, wherein, the water contact angle of the resin base material side surface of described duplexer is 60 ° ~ 80 °.
3. manufacture method according to claim 1, wherein, the thickness of described light polarizing film is 0.5 μm ~ 15 μm.
4. manufacture method according to claim 1, wherein, the iodide concentration in described cleaning fluid is 0.5 % by weight ~ 10 % by weight.
5. manufacture method according to claim 1, wherein, described stretching comprises in water and stretching.
6. manufacture method according to claim 1, wherein, the removal of the cleaning fluid on the resin base material side surface of described duplexer is undertaken by wiping or blow gas.
7. an optical laminate, it is obtained by manufacture method according to claim 1.
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| Application Number | Priority Date | Filing Date | Title |
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| JP2013265171A JP5961158B2 (en) | 2013-12-24 | 2013-12-24 | Method for producing optical laminate |
| JP2013-265171 | 2013-12-24 |
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| JP (1) | JP5961158B2 (en) |
| KR (1) | KR101703504B1 (en) |
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| CN108539092A (en) * | 2017-03-03 | 2018-09-14 | 住友化学株式会社 | film manufacturing device and film manufacturing method |
| CN110125563A (en) * | 2019-04-30 | 2019-08-16 | 大族激光科技产业集团股份有限公司 | A method of except polarizing film iodine molecule layer |
| CN111231467A (en) * | 2018-05-08 | 2020-06-05 | 住友化学株式会社 | Laminate and method for producing same |
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Also Published As
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| CN104730611B (en) | 2017-05-31 |
| JP5961158B2 (en) | 2016-08-02 |
| KR20150075035A (en) | 2015-07-02 |
| TW201527809A (en) | 2015-07-16 |
| TWI570462B (en) | 2017-02-11 |
| JP2015121658A (en) | 2015-07-02 |
| KR101703504B1 (en) | 2017-02-07 |
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