CN101281267A - Method for preparing bias photon and method for preparing polarized light slice - Google Patents
Method for preparing bias photon and method for preparing polarized light slice Download PDFInfo
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- CN101281267A CN101281267A CNA2007100937391A CN200710093739A CN101281267A CN 101281267 A CN101281267 A CN 101281267A CN A2007100937391 A CNA2007100937391 A CN A2007100937391A CN 200710093739 A CN200710093739 A CN 200710093739A CN 101281267 A CN101281267 A CN 101281267A
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Abstract
The invention discloses a method for preparing polarizing photon and polarizing sheet. The method for preparing polarizing photon includes providing a polyvinyl alcohol PVA film; soaking the PVA film in a first solution in order to execute preprocess, wherein the first solution includes at least a carboxyl acid or derivative thereof with at least two carboxyl, and at least a catalyzer catalyzing the reaction between the carboxyl acid and the PVA film surface; soaking the PVA film after preprocess in the dyeing solution to execute a tray dyeing process; soaking the PVA film after the tray dyeing process in a second solution, and meanwhile extending the PVA film, wherein the second solution includes a boric acid; and drying the PVA film after the extension process to form polarizing photon.
Description
Technical field
The present invention relates to the method for making of a kind of polarisation and polaroid, particularly relate to the method for making of polarisation in a kind of polaroid that is used in LCD.
Background technology
In LCD, polaroid is one of indispensable composed component, its purposes is originally not have the light of deflection polarity, produce polarization, be transformed into polar biased light, therefore, LCD just can be utilized this polar biased light, add the torque characteristic of liquid crystal molecule itself, reach whether passing through of light of control and presenting of color signal.And in recent years, along with liquid crystal display cells is widely used in such as in the various electronic equipments such as word processor (word processor), computer screen, mobile phone or LCD TV even aspects such as large-scale outdoor display board, vehicle, aircraft, autical instrument and satellite, therefore, the demand of polaroid is also increasing.
The cross-section structure of polaroid 10 of the prior art as shown in Figure 1; it mainly comprises polyvinyl alcohol (PVA) (polyvinyl alcohol; be designated hereinafter simply as PVA) polarization matrix layer (being polarisation) 12 and be coated on its up and down Triafol T (triacetyl cellulose is designated hereinafter simply as TAC) protective seam 14 and 16 of two sides.And attaching pressure sensing adhesive layer 18, fractal film 20 and another diaphragm 22.Sometimes, in order to prevent reflex, special processing also can be given again in protective seam 16 surfaces, for example adds last layer anti-dizzy (anti-glare) layer or anti-reflecting layer (anti-reflection).At present, the polaroid on the market is a main flow with the iodine polarizing sheet still, and this is because the iodine polarizing sheet has high light peneration, high contrast, and has the polarized light property than the wide area wavelength, and its manufacturing is upward more or less freely, relatively also makes its price comparatively cheap.
The method of making the iodine polarizing sheet in traditional skill is will (to contain iodine (I in polyvinyl alcohol (PVA) (PVA) film swelling in water (swelling), the staining trough earlier
2) and potassium iodide (KI)) (contain boric acid (H in dyeing (dyeing), the extension slot
3BO
3) and potassium iodide) extend, alternatively (optional) use boronic acid containing and liquor kalii iodide to carry out fixation and washing is handled, through oven for drying, and form above-mentioned PVA polarization matrix layer 12, as polarisation with polarized light property.Then re-use hydrogel (hydrogel) upper and lower faces and the protective seam 14 and 16 of PVA polarization matrix layer 12 are fitted, after super-dry, form the Polarizer semi-manufacture of three-decker.Wherein, boric acid is played the part of the role of crosslinking chemical (crosslinkingagent), except carrying out cross-linking reaction on PVA film surface and increasing the toughness of film, the iodine and the potassium iodide that also can prevent to dye in staining trough in the PVA film ooze out in follow-up impregnation process, cause the phenomenon that polarisation fades and make the optical property (as degree of polarization, penetrance, b value or the like) of polarisation destroyed.
Though boric acid has the crosslinking chemical function,, it also causes some shortcomings because of existing.Be that because the effect of boric acid makes the PVA film toughness increase, so can limit the extension ratio of PVA film at the process of extension mesoboric acid, therefore generally extension ratio can be between about 5.5 to about 6.0 times.The 2nd, because the toughness of PVA film improves at the crosslinked of its surface because of boric acid, therefore can cause the overtension that roller bears in the extension process.Be head it off, generally must make the softening tension force that reduces of PVA film by the high temperature extension.Elongating temperature (extension slot temperature) commonly used is generally between 50 to 55 ℃.But be to use high extension slot temperature to quicken the evaporation of tank liquor except meeting, outside liquor strength being changed strengthen, also can cause dye in the PVA film into easier the oozing out of iodine and forming fade.
Therefore, still need the method for making of a kind of better polarisation or polaroid,, make polarisation or polaroid with better quality to improve the disappearance of above-mentioned technology.
Summary of the invention
One object of the present invention is to provide a kind of manufacturing polarisation of improvement and the method for polaroid, polarisation or the polaroid that have good optical properties with manufacturing, and extension slot can have lower temperature, can improve the shortcoming of above-mentioned prior art.
The method of foundation manufacturing polarisation of the present invention comprises provides polyvinyl alcohol (PVA) (PVA) film; The PVA film is immersed in first solution, and to carry out pre-service, wherein first solution comprises at least a carboxylic acid or derivatives thereof with at least two carboxyls, and the catalyzer of at least a catalysis carboxylic acid and the surface reaction of PVA film; To be immersed in the staining solution through pretreated PVA film, carry out dip dyeing treatment; To be immersed in second solution through the PVA film of dip dyeing treatment, and extend the PVA film simultaneously, wherein second solution comprises boric acid; And will carry out drying through extending the PVA film of handling, form polarisation.
Method according to manufacturing polaroid of the present invention comprises: polyvinyl alcohol (PVA) (PVA) film is provided; The PVA film is immersed in first solution, and to carry out pre-service, wherein first solution comprises at least a carboxylic acid or derivatives thereof with at least two carboxyls, and the catalyzer of at least a catalysis carboxylic acid and the surface reaction of PVA film; To be immersed in the staining solution through pretreated PVA film, carry out dip dyeing treatment; To be immersed in second solution through the PVA film of dip dyeing treatment, and extend the PVA film simultaneously, wherein second solution comprises boric acid; To carry out drying through extending the PVA film of handling, form polarisation; And, form polaroid with sub and at least one protective seam applying of the polarisation of drying.
Alleged herein " polarisation ", or claim " light polarizing film ", be meant the rete that has the polarisation function in all layers of polaroid, for example iodine is polarizing film or dichromatism macromolecule polarizing film.
In the present invention, when carrying out the manufacturing of polarisation or polaroid, be that earlier to use the carboxylic acid or derivatives thereof with at least two carboxyls that PVA is carried out crosslinked, then just the crosslinked PVA film dye.Owing to before dyeing, carry out crosslinked to PVA, make the method for foundation manufacturing polarisation of the present invention and polaroid can have following advantage and effect: according to switching between manufacture process of the present invention and the traditional manufacture process easily, prepared polarisation is difficult for fading, can effectively reduce the extension slot temperature, have bigger elasticity for the adjustment of process parameters.
The invention provides a kind of method of making polarisation, include: polyvinyl alcohol (PVA) (PVA) film is provided; Described PVA film is immersed in first solution, and to carry out pre-service, wherein said first solution comprises at least a have carboxylic acid, or derivatives thereof and the described carboxylic acid of at least a catalysis of at least two carboxyls and the catalyzer of described PVA film surface reaction; To be immersed in the staining solution through described pretreated PVA film, carry out dip dyeing treatment; To be immersed in second solution through the PVA film of described dip dyeing treatment, and extend described PVA film simultaneously, wherein said second solution comprises boric acid; And will carry out drying through extending the described PVA film of handling, form polarisation.
Wherein said carboxylic acid comprises ethane diacid, malonic acid, succinic acid, glutaric acid, hexane diacid, or heptandioic acid.
Wherein said catalyzer comprises lewis acid.Wherein said lewis acid comprises aluminium ion, zinc ion or contains aluminium ion or the salt of zinc ion or complex compound.
Wherein said staining solution comprises dichroic dye.Wherein said dichroic dye comprises iodine or organic dye molecule.
Wherein said second solution further comprises potassium iodide.
Also a kind of method of making polaroid of the present invention includes: polyvinyl alcohol (PVA) (PVA) film is provided; Described PVA film is immersed in first solution, and to carry out pre-service, wherein said first solution comprises at least a have the carboxylic acid or derivatives thereof of at least two carboxyls and the catalyzer of described carboxylic acid of at least a catalysis and the surface reaction of described PVA film; To be immersed in the staining solution through described pretreated PVA film, carry out dip dyeing treatment; To be immersed in second solution through the PVA film of described dip dyeing treatment, and extend described PVA film simultaneously, wherein said second solution comprises boric acid; To carry out drying through extending the described PVA film of handling, form polarisation; And, form polaroid with sub and at least one protective seam applying of the described polarisation of drying.
Wherein said carboxylic acid comprises ethane diacid, malonic acid, succinic acid, glutaric acid, hexane diacid, or heptandioic acid.
Wherein said catalyzer comprises lewis acid.Wherein said lewis acid comprises aluminium ion, zinc ion or contains aluminium ion or the salt of zinc ion or complex compound.
Wherein said staining solution comprises dichroic dye.Wherein said dichroic dye comprises iodine or organic dye molecule.
Wherein said second solution further comprises potassium iodide.
Wherein said protective seam comprises Triafol T (TAC) film, cellulose diacetate (DAC), polyethylene terephthalate (PET), cyclic olefin polymer (COP), cycloolefin co-polymer (COC) or polycarbonate (PC).
Description of drawings
Fig. 1 shows polaroid cross-sectional view of the prior art.
Fig. 2 shows the method for using foundation manufacturing polarisation of the present invention and the synoptic diagram of making the method for polaroid.
Fig. 3 shows the surface structure synoptic diagram of PVA film after handling through dicarboxylic acids.
Fig. 4 shows the cell body configuration schematic diagram of manufacturing polarisation of prior art.
Fig. 5 shows the tables of data according to the polarisation subsample test result of two embodiment of the present invention and three comparative example manufacturings.
Embodiment
Method according to manufacturing polarisation of the present invention comprises polyvinyl alcohol (PVA) (PVA) film is provided; The PVA film is immersed in first solution, and to carry out pre-service, wherein first solution comprises at least a have the carboxylic acid or derivatives thereof of at least two carboxyls and the catalyzer of at least a catalysis carboxylic acid and the surface reaction of PVA film; To be immersed in the staining solution through pretreated PVA film, carry out dip dyeing treatment; To be immersed in second solution through the PVA film of dip dyeing treatment, and extend the PVA film simultaneously, wherein second solution comprises boric acid; And will carry out drying through extending the PVA film of handling, form polarisation.See also Fig. 2, describe the present invention in detail with a specific embodiment.
As shown in Figure 2, show that one uses method and the further specific embodiment of making polaroid according to manufacturing polarisation of the present invention, flow process roughly is divided into several key steps, comprising:
Step 102: pre-service (pre-treatment).
Step 104: contaminate (dyeing).
Step 106: extend (stretching).
Step 108: dry (drying).
Step 110: fit (lamination).
Step 112: dry (drying).
Step 102,104,106, and 108 are key steps of the method for manufacturing polarisation of the present invention.After dip-dye or the extension, also can optionally wash once or several.When making polaroid, further on prepared polarisation, carry out the applying of step 110.After step 110, can carry out the drying program of step 112 according to need.
Employed carboxylic acid or derivatives thereof with at least two carboxyls can be and have two carboxyls (organic acid or derivatives thereof COOH), for example ethane diacid, malonic acid, succinic acid, glutaric acid, hexane diacid, heptandioic acid, and the derivant of aforesaid compound.As long as that is to say carboxylic acid or derivatives thereof, all can use for the present invention with at least two carboxyls.Also can use its esters, but must further add acid, make first solution become acidity.
Wherein, be example with the hexane diacid, be dicarboxylic acids, (molecular formula is HOOC (CH to have 6 carbon atoms altogether
2)
4COOH), so different configuration (configuration) is spatially arranged.Consider molecular characterization, obtain the source, reach the factors such as solubleness to water, hexane diacid is to be applicable to one of the present invention person.
Have the amount of carboxylic acid or derivatives thereof in first solution of at least two carboxyls, there is no particular restriction, as long as can form bond with the surface reaction of PVA film, and can dissolve fully under the temperature of first solution that sets and get final product.In the general assembly (TW) of first solution, the amount of dicarboxylic acids can be for example about 1 to 4 weight %, is preferably 2 to 3 weight %.The groove temperature of pretreatment tank can be adjusted according to need, does not have strict restriction, in a specific embodiment of the present invention, can be between 25 and 40 ℃, is preferably between 30 and 40 ℃.
Employed catalyzer can be lewis acid (Lewis acid), for example aluminium ion (Al
3+), zinc ion (Zn
2+).All Al that provides
3+Or Zn
2+Salt or the misfit thing (complex compound, compound complexes) all can use, for example aluminium sulphate, aluminum chloride, zinc chloride, zinc sulfate or the like.Because the configuration of the size of pretreatment tank, the concentration of carboxylic acid, roller, pretreatment tank groove temperature etc. all belong to transformable parameter, so catalyst concentration and unrestricted, as long as catalyst concentration enough makes carboxylic acid and PVA reaction.If carboxylic acid and PVA produce reaction, the ductility that then can obviously observe the PVA film promotes, thus originally traditional manufacture process the extension ratio that can't reach, can reach easily by this manufacture process.If with 18 hydrazine aluminum sulfates as Al
3+The source, in the general assembly (TW) of first solution, about 0.01 to 5 weight %, 0.01 to 3 weight % more preferably, and most preferably be 0.01 to 1 weight %.
Please consult Fig. 3 simultaneously, it shows the surface structure synoptic diagram through the pretreated PVA film 53 of step 102.To add hexane diacid is example, all has one of them carboxylic acid group of carboxylic acid group's hexane diacid molecule esterification (esterification) to take place with the water wettability hydroxy 62 on PVA film surface at the strand two ends, produces chemical bonded refractory structure 64.Or esterifications (esterification) take place with the hydroxy 62 on PVA film surface respectively in two carboxylic acid groups of hexane diacid molecule, produce chemical bonded refractory structure 65.
This pre-treatment step is to carry out before the dyeing of PVA film, therefore need not contain expensive potassium iodide composition in first solution in pretreatment tank.And before carrying out pre-service, also can not be immersed in the pure water with swelling extending (un-stretched) PVA film earlier.
Carry out the dip-dye of step 104 through the pretreated PVA film 53 of step 102, for example soak in the Biodine prescription 54, make PVA film 53 absorption iodine at dye solution.Biodine prescription 54 comprises molecular iodine and potassium iodide, and wherein the weight percent concentration of iodine (comprising iodine molecule and iodide ion) is about about 0.01 weight % to 1 weight %.Also can further contain boric acid in the dye solution.
In the present invention, be not limited to make the iodine polarizing sheet, therefore, in the dip-dye program of step 104, the dyestuff that is used to dye can be dichroic dye, and it also can be organic dye molecule and fellow thereof except iodine.
Then,, after contaminating and before the extension program, place first rinsing bowl to wash the PVA film, wherein contain the aqueous solution of boric acid and potassium iodide in first rinsing bowl optionally as common conventional art.
Then, will carry out step 106, the extension of PVA film just (stretching) manufacture process through the PVA film of contaminating 55.Make PVA film 55 in containing the extension slot solution 56 of boric acid and potassium iodide, carry out the extension of film, for example unidirectional extension (uniaxiallystretching).Wherein, the weight percent concentration of boric acid can be the employed concentration of prior art, for example is about about 1 weight % to 10 weight %.The concentration of potassium iodide can be the employed concentration of prior art, for example about 1 to 10 weight %.Contained boric acid and potassium iodide in the employed extension slot solution often needs its content of periodic monitoring in manufacture process.In the present invention, it is quantitatively easy, does not have problem.
PVA film after the extension can optionally further be washed, and for example can utilize second rinsing bowl of normal use in the prior art to wash.Then, also can optionally further in soaper, carry out fixation.Solution in second rinsing bowl and the soaper can contain boric acid and potassium iodide, the visual demand of concentration and adjusting, preferred each independently be 1 to 5 weight %, the ratio content ratio with interior boric acid of extension slot and potassium iodide usually is approximately identical, can further improve the character of PVA film.As still have needs, and can further wash once more, can utilize in the prior art normal the 3rd rinsing bowl that uses to wash, use frozen water (for example about 10 ℃ or more low temperature) removal earlier before dry of PVA film to be remained in the chemical constitution on PVA film surface.
Then, carry out step 108, will carry out drying, so, obtain PVA film 58, be polarisation that makes according to method of the present invention through the PVA film 57 that extends.Drying mode is not particularly limited, can be by for example mode drying such as hot-air seasoning or IR (infrared ray) oven dry.
Proceed step 110, make the PVA film 58 handled through step 108 and at least one protective seam 59 manufacture process of fitting, form three laminatings and close structure, with the manufacturing polaroid.Protective seam can comprise for example TAC, cellulose diacetate (diacetyl cellulose; abbreviation DAC), polyethylene terephthalate (polyethylene terephthalate; abbreviation PET), cyclic olefin polymer (cycloolefin polymer; abbreviation COP), cycloolefin co-polymer (cycloolefin copolymer; abbreviation COC), polycarbonate (polycarbonate is called for short PC) film and fellow thereof.
At last, carry out step 112, three laminatings of fitting are closed structure 60 impose dried, for example under about 50 to 80 ℃, carry out drying, make polaroid.Drying mode is not particularly limited, can be by for example mode drying such as hot-air seasoning or IR oven dry.
In addition, in order to increase the functional of polaroid, can on protective seam, further be coated with for example liquid crystal layer, protective seam, Bewildering resistance layer, anti-reflecting layer or scratch resistance and hinder antifouling processing layer or the like.By the combination of different functional protection layers, the Polarizer that can obtain having the different optical effect.
Below, especially exemplified by several embodiment, describe method in detail, and compare with comparative example according to manufacturing polarisation of the present invention.Method of the present invention can be switched easily with traditional manufacture process, therefore, is the cell body configuration of directly adopting prior art in an embodiment.But, only being the simplest synoptic diagram as the configuration of cell body among Fig. 4 and roller (or claiming roller), its configuration can change with actual demand.
Embodiment
Please refer to the cell body configuration schematic diagram of prior art shown in Figure 4, with width is that 650mm and thickness are that the not extension PVA film 50 of 75 μ m utilizes roller to carry, swelling in 28 ℃ of pure water in groove 68 is carried out pre-service then in as the about 30 ℃ of aqueous solution in the groove 70 of pretreatment tank earlier.Contain the hexane diacid of 2.25 weight % and the aluminum sulfate hydrate class (Al of 0.3 weight % in the aqueous solution of groove 70
2(SO
4)
316～18H
2O).After this pre-service, in 30 ℃ the iodine solution (containing iodine concentration is 0.033 weight %, and boric acid concentration is 0.95 weight %, and potassium iodide concentration is 0.6 to 0.8 weight %) of groove 72, contaminate.To in the extension slot 74 of 51 ℃ of groove temperature, extend through the PVA film of contaminating, extend liquid and contain the boric acid of 3.35 weight % and the potassium iodide of 3.01 weight %.Then, wash in second rinsing bowl 76, the water lotion temperature is 40 ℃, contains the boric acid of 3.27 weight % and the potassium iodide of 4.19 weight %.Carry out fixation again in soaper 78, its solution is 40 ℃, contains the boric acid of 3.14 weight % and the potassium iodide of 3.86 weight %.Further in 10 ℃ of water of the 3rd rinsing bowl 80, clean.Obtain polarisation 60 ℃ of following dryings at last.With the polarisation that obtained measure extension ratio, fabric width (mm), thickness (μ m), penetrance (Ys, %), (V, %), and form and aspect b value, the result is as shown in the table of Fig. 5 for degree of polarization.
Embodiment 2
Carry out the manufacturing of polarisation as embodiment 1 described mode, but with the groove temperature of groove 70 be adjusted into 35 ℃, and the groove temperature drop of extension slot be 46.5 ℃.With the polarisation that obtained measure extension ratio, fabric width (mm), thickness (μ m), penetrance (Ys, %), (V, %), and form and aspect b value, the result is as shown in the table of Fig. 5 for degree of polarization.
Comparative example 1
Please refer to Fig. 4, with width is that 650mm and thickness are that the not extension PVA film 50 of 75 μ m utilizes roller to carry, in groove 68, be immersed in as the swelling groove carry out swelling in 30 ℃ the pure water and handle after, as 30 ℃ of iodine solutions in the groove 70 of staining trough (contain the iodine of 0.048 weight %, about 1 weight % boric acid, and the potassium iodide of about 1.5 weight %) in contaminate.To handle in the water lotion in as the groove 72 of first rinsing bowl through the PVA film of contaminating, the water lotion temperature is 35 ℃, contains the boric acid of 3 weight % and the potassium iodide of 3 weight %.Then, in the extension slot 74 of 53 ℃ of groove temperature, extend, extend boric acid, and the potassium iodide of 4 weight % of zinc chloride, the 1 weight % of hexane diacid that liquid contains 3 weight %, 0.14 weight %.Then, wash in second rinsing bowl 76, the water lotion temperature is 30 ℃, contains the boric acid of 3 weight % and the potassium iodide of 4 weight %.Carry out fixation again in soaper 78, its solution is 30 ℃, contains the boric acid of 3 weight % and the potassium iodide of 4 weight %.In 10 ℃ of water of the 3rd rinsing bowl 80, clean again.Obtain polarisation 60 ℃ of following dryings at last.With the polarisation that obtained measure extension ratio, fabric width (mm), thickness (μ m), penetrance (Ys, %), (V, %), and form and aspect b value, the result is as shown in the table of Fig. 5 for degree of polarization.
Comparative example 2
Please refer to Fig. 4, with width is that 650mm and thickness are that the not extension PVA film 50 of 75 μ m utilizes roller to carry, in groove 68, be immersed in as the swelling groove carry out swelling in 30 ℃ of pure water and handle after, groove 70 as staining trough, is contaminated in 30 ℃ of iodine solutions in groove 70.Groove 72 as first rinsing bowl, will be handled in the water lotion of groove 72 through the PVA film of contaminating, and the water lotion temperature is 35 ℃, contains the boric acid of 3 weight % and the potassium iodide of 3 weight %.Then, in the extension slot 74 of 53 ℃ of groove temperature, extend.Extend zinc chloride, and the potassium iodide of 4 weight % of boric acid, the 0.14 weight % of hexane diacid that liquid contains 3 weight %, 1 weight %.Then, wash in second rinsing bowl 76, the water lotion temperature is 30 ℃, contains the boric acid of 3 weight % and the potassium iodide of 4 weight %.Carry out fixation again in soaper 78, its solution is 30 ℃, contains the boric acid of 3 weight % and the potassium iodide of 4 weight %.In 10 ℃ of water of the 3rd rinsing bowl 80, clean again, obtain polarisation 60 ℃ of following dryings at last.With the polarisation of gained measure extension ratio, fabric width (mm), thickness (μ m), penetrance (Ys, %), (V, %), and form and aspect b value, the result is as shown in the table of Fig. 5 for degree of polarization.
Comparative example 3
Please refer to Fig. 4, is that 650mm and thickness are that the not extension PVA film 50 of 75 μ m utilizes roller to carry with width, is immersed in 28 ℃ of pure water with after carrying out swelling and handling in the groove 68 as the swelling groove, contaminates in the iodine solution as the groove 70 of staining trough.Use groove 72 as treatment trough, will through in 39 ℃ the aqueous solution of PVA film immersion in treatment trough of dip-dye to handle.Contain the hexane diacid of 2.5 weight %, the aluminum sulfate hydrate class (Al of 0.3 weight % in the aqueous solution of groove 72
2(SO
4)
316～18H
2O), reach the potassium iodide of 3.3 weight %.Then treated PVA film is extended in the extension slot 74 of 52 ℃ of groove temperature, extend liquid and contain the boric acid of 3.49 weight % and the potassium iodide of 4.13 weight %.Then, wash in second rinsing bowl 76 in regular turn, the water lotion temperature is 40 ℃, contain the boric acid of 3.29 weight % and the potassium iodide of 3.81 weight %, carry out fixation again in soaper 78, its solution is 40 ℃, contains the boric acid of 3.8 weight % and the potassium iodide of 4.3 weight %.Further in 10 ℃ of water of the 3rd rinsing bowl 80, clean.Obtain polarisation 60 ℃ of following dryings at last.With the polarisation that obtained measure extension ratio, fabric width (mm), thickness (μ m), penetrance (Ys, %), (V, %), and form and aspect b value, the result is as shown in the table of Fig. 5 for degree of polarization.
By in the table of Fig. 5 as can be known, with embodiment 1 and 2 and comparative example 1,2, and 3 relatively, fabric width and extension multiplying power do not increase, and thickness is thicker, make in manufacture process not easy fracture, optical properties such as degree of polarization and penetrance are good, and the b value then is greatly improved to 1.781 and 1.831.Use method as can be known, polarisation that can obtain to have more superior b value easily according to manufacturing polarisation of the present invention.Further embodiment 1 and embodiment 2 are compared, under identical extension ratio, change for example extension slot temperature or the like of other parameter as can be known, still can obtain polarisation that can not fade, that is to say according to the manufacture process elasticity of method of the present invention big.
Above-mentioned according to embodiments of the invention 1 and 2 in, be before the dyeing of PVA film, to use the tank liquor that contains hexane diacid to handle the PVA film, because the PVA surface has a large amount of-OH base, so under heating and interpolation appropriate amount of catalysts, can form ester bond on the PVA surface, because hexane diacid spatially is free, therefore have chemical bonded refractory structure 64 and 65 two kind of bond structure generation.The hexane diacid of one end bond can further increase the tackness of PVA film when follow-up and protective seam are fitted, and the hexane diacid of both-end bond then makes the ductility of PVA film significantly increase, so the powerful extension of tolerable and easy fracture not.The lifting of stock utilization is being represented in powerful extension, passes through the auxiliary of mechanisms such as roller, expansion wheel simultaneously, also can obtain wideer, thinner polarisation.
Yet, with traditional crosslinking chemical boric acid relatively, the use of hexane diacid makes PVA film ductility improve, but it is lower than boric acid to opposing the benefiting of aspect of fading.In comparative example 1 and 2, hexane diacid and catalyzer be added in the extension slot use simultaneously with boric acid, the PVA film is extended under the effect of boric acid and hexane diacid simultaneously.And from the result of comparative example 1 and 2 as can be known, though this kind manufacture process can reach high extension ratio and extremely wide fabric width, polarisation as the above-mentioned situation about seriously fading that has that produce, optical property is relatively poor.And in comparative example 3, hexane diacid and catalyzer are added on use in extension slot washing one groove (as pretreatment tank) before, make the PVA film after process dyeing, effect by hexane diacid earlier increases ductility, carry out crosslinkedly again through the boric acid in the extension slot, make the iodine easy to leak more not in the PVA film.This kind manufacture process has extra advantage, that is to say owing to use extra pretreatment tank to carry out the reaction of hexane diacid and PVA, so the switching between traditional manufacture process and this manufacture process is comparatively easy, can effectively saves and change the cost that tank liquor causes.Yet this manufacture process still has the phenomenon that fades when passing through last washing manufacture process.
In other words, if after the PVA film is through dip-dye, just use dicarboxylic acids to handle the situation of PVA film as crosslinking chemical, because dicarboxylic acids is lower than boric acid to opposing the benefiting of aspect of fading, so in the follow-up impregnation process of PVA film, make easily dye in the staining trough into iodide leak, make that its optical property of polarisation of output is destroyed.
In the present invention, be the problem of avoiding fading, be before treatment step with dicarboxylic acids is advanced to staining trough, pretreatment tank (tank liquor comprises dicarboxylic acids and catalyzer) is set before staining trough, make PVA before dyeing, handle the ductility of improving PVA through carboxylic acid or derivatives thereof earlier with at least two carboxyls, then according to manufacture process of the prior art dye, in the extension slot (containing boric acid and potassium iodide) extend, (containing boric acid and potassium iodide) fixation in the soaper, and in rinsing bowl, clean with clear water, drying obtains polarisation more at last.According to method of the present invention, kept the advantage that is easy to switch traditional manufacture process and this manufacture process, and because be before dyeing, earlier to handle the PVA film, so the phenomenon that can cause polarisation to fade not because of the minimizing in boric acid processing time with carboxylic acid or derivatives thereof with at least two carboxyls.In addition, because the lifting of PVA film ductility, so in the extension process of extension slot, the extension slot temperature can effectively reduce and avoid making the soup volatilization too fast because of the groove temperature is high.Yet, because the effect of hexane diacid is not to implement in extension or before extending, thus less to the ductility lifting amplitude of PVA film, so the sub-fabric width of the polarisation of output is less, thickness is thicker.But because used the problem of boric acid, so but output optical property polarisation preferably to avoid fading.In addition, extension ratio also can further promote by the adjustment (for example pretreatment tank temperature, roller configuration, extension parameter configuration or the like) of other parameter.Therefore, still PVA is carried out crosslinked step according to method of the present invention, and many advantages and effect are arranged because of having before dyeing.
The above only is the preferred embodiments of the present invention, and every equalization of doing according to claim of the present invention changes and modifies, and all should belong to covering scope of the present invention.
The main element symbol description
10 polaroids, 12 polarization matrix layers
14 protective layers, 16 protective layers
18 pressure sensing adhesive layer, 20 fractal films
22 diaphragms 50 do not extend the PVA film
52 first solution 53PVA films
54 Biodines prescription 55PVA film
56 extension slot solution 57PVA films
60 3 laminatings close structure 62 hydroxys
64 chemical bonded refractory structures, 65 chemical bonded refractory structures
68 grooves, 70 grooves
72 grooves, 74 extension slots
76 second rinsing bowls, 78 soapers
80 the 3rd rinsing bowls
102,104,106,108,110,112 steps
Claims (10)
1. method of making polarisation includes:
Polyvinyl alcohol (PVA) (PVA) film is provided;
Described PVA film is immersed in first solution, and to carry out pre-service, wherein said first solution comprises at least a have carboxylic acid, or derivatives thereof and the described carboxylic acid of at least a catalysis of at least two carboxyls and the catalyzer of described PVA film surface reaction;
To be immersed in the staining solution through described pretreated PVA film, carry out dip dyeing treatment;
To be immersed in second solution through the PVA film of described dip dyeing treatment, and extend described PVA film simultaneously, wherein said second solution comprises boric acid; And
To carry out drying through extending the described PVA film of handling, form polarisation.
2. method according to claim 1, wherein said carboxylic acid comprises ethane diacid, malonic acid, succinic acid, glutaric acid, hexane diacid, or heptandioic acid.
3. method according to claim 1, wherein said catalyzer comprises lewis acid.
4. method according to claim 3, wherein said lewis acid comprise aluminium ion, zinc ion or contain aluminium ion or the salt of zinc ion or complex compound.
5. method according to claim 1, wherein said staining solution comprises dichroic dye.
6. method according to claim 5, wherein said dichroic dye comprises iodine or organic dye molecule.
7. method according to claim 1, wherein said second solution further comprises potassium iodide.
8. method of making polaroid includes:
Polyvinyl alcohol (PVA) (PVA) film is provided;
Described PVA film is immersed in first solution, and to carry out pre-service, wherein said first solution comprises at least a have the carboxylic acid or derivatives thereof of at least two carboxyls and the catalyzer of described carboxylic acid of at least a catalysis and the surface reaction of described PVA film;
To be immersed in the staining solution through described pretreated PVA film, carry out dip dyeing treatment;
To be immersed in second solution through the PVA film of described dip dyeing treatment, and extend described PVA film simultaneously, wherein said second solution comprises boric acid;
To carry out drying through extending the described PVA film of handling, form polarisation; And
Described polarisation of drying is fitted with at least one protective seam, form polaroid.
9. method according to claim 8, wherein said carboxylic acid comprises ethane diacid, malonic acid, succinic acid, glutaric acid, hexane diacid, or heptandioic acid.
10. method according to claim 8, wherein said catalyzer comprises lewis acid.
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| CNA2007100937391A CN101281267A (en) | 2007-04-05 | 2007-04-05 | Method for preparing bias photon and method for preparing polarized light slice |
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| CNA2007100937391A CN101281267A (en) | 2007-04-05 | 2007-04-05 | Method for preparing bias photon and method for preparing polarized light slice |
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| CN102116889A (en) * | 2009-12-31 | 2011-07-06 | 第一毛织株式会社 | Polarizer, method for preparing the same, and polarizing plate provided with the same |
| CN102432899A (en) * | 2011-08-16 | 2012-05-02 | 深圳市华星光电技术有限公司 | Modified polyvinylalcohol (PVA) base film, preparation method thereof and polarizer |
| CN103163584A (en) * | 2011-12-12 | 2013-06-19 | 第一毛织株式会社 | Polarizing plate for organic light-emitting display and display device including the same |
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| US10114159B2 (en) | 2015-01-27 | 2018-10-30 | Lg Chem, Ltd. | Method for manufacturing polarizer and polarizer manufactured by the same |
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| US9290674B2 (en) | 2011-08-16 | 2016-03-22 | Shenzhen China Star Optoelectronics Technology Co. Ltd | Method for preparing a base film of modified polyvinyl alcohol polymer |
| CN102432899A (en) * | 2011-08-16 | 2012-05-02 | 深圳市华星光电技术有限公司 | Modified polyvinylalcohol (PVA) base film, preparation method thereof and polarizer |
| CN103163584A (en) * | 2011-12-12 | 2013-06-19 | 第一毛织株式会社 | Polarizing plate for organic light-emitting display and display device including the same |
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| US10114159B2 (en) | 2015-01-27 | 2018-10-30 | Lg Chem, Ltd. | Method for manufacturing polarizer and polarizer manufactured by the same |
| US11314006B2 (en) | 2015-01-27 | 2022-04-26 | Lg Chem, Ltd. | Method for manufacturing polarizer and polarizer manufactured by the same |
| CN107012699A (en) * | 2017-03-03 | 2017-08-04 | 厦门祥福兴胶粘制品有限公司 | A kind of preparation method of anti-blue light polaroid |
| CN107012699B (en) * | 2017-03-03 | 2020-05-22 | 厦门祥福兴胶粘制品有限公司 | Manufacturing method of anti-blue-light polaroid |
| CN113198438A (en) * | 2020-02-27 | 2021-08-03 | 合肥三利谱光电科技有限公司 | Method for determining regeneration time node and regeneration time node of resin for filtering extension liquid |
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