JPS6285203A - Production of polarizing film - Google Patents

Production of polarizing film

Info

Publication number
JPS6285203A
JPS6285203A JP22518185A JP22518185A JPS6285203A JP S6285203 A JPS6285203 A JP S6285203A JP 22518185 A JP22518185 A JP 22518185A JP 22518185 A JP22518185 A JP 22518185A JP S6285203 A JPS6285203 A JP S6285203A
Authority
JP
Japan
Prior art keywords
film
glutaraldehyde
iodine
contg
soln
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP22518185A
Other languages
Japanese (ja)
Inventor
Hideo Kawaguchi
英夫 川口
Takashi Takayanagi
丘 高柳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fujifilm Holdings Corp
Original Assignee
Fuji Photo Film Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fuji Photo Film Co Ltd filed Critical Fuji Photo Film Co Ltd
Priority to JP22518185A priority Critical patent/JPS6285203A/en
Publication of JPS6285203A publication Critical patent/JPS6285203A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To improve the moisture and heat resistances and the polarizing property by uniaxially stretching a polyvinyl alcohol film contg. iodine, treating the stretched film with the acidic soln. of glutaraldehyde and drying it. CONSTITUTION:A PVA film is immersed in an aqueous soln. contg. iodine and potassium iodide and is uniaxially stretched 2-6 times in a wet state The stretched film is treated with the acidic soln. of 4-3pH contg. 20-1% glutaraldehyde under the tension and is dried at 75-130 deg.C. Since the film is treated with the soln. contg. glutaraldehyde, the moisture and heat resistances are improved and the degree of polarization of light at about 750nm can be increased.

Description

【発明の詳細な説明】 〔発明の分野〕 本発明は偏光フィルムの製造方法に関するものである。[Detailed description of the invention] [Field of invention] The present invention relates to a method for manufacturing a polarizing film.

偏光フィルムはサングラス、反射防止板、液晶を組合せ
て電卓、時計、OA機器、自動車用表示機器など広く使
用され、今後も更に広い分野へ使用されつつある。この
様に使用分野が拡がるにつれて、偏光膜に対する要求性
能もきびしくなり、耐湿耐熱性があり、かつ偏光度の大
きい偏光フィルムが必要とされてきている。
Polarizing films are widely used in combination with sunglasses, antireflection plates, and liquid crystals, such as calculators, watches, office automation equipment, and automobile display equipment, and will continue to be used in even wider fields. As the fields of use have expanded in this way, the performance requirements for polarizing films have become stricter, and there has been a need for polarizing films that are resistant to moisture and heat and have a high degree of polarization.

本発明は耐湿耐熱性がすぐれ、偏光性の大きな偏光フィ
ルムの製造方法に関するものである。
The present invention relates to a method for producing a polarizing film with excellent moisture and heat resistance and high polarization properties.

〔従来技術〕[Prior art]

現在一般に使用されている偏光膜は、ポリビニルアルコ
ール(以下PVAと略す)フィルムに二色性染料又はヨ
ードを含浸させ一軸に延伸させるか、あるいはPVAを
一軸に延伸後二色性染料又はヨードを含浸させホウ酸で
架橋させて作られる。
Polarizing films commonly used at present are made by impregnating a polyvinyl alcohol (hereinafter abbreviated as PVA) film with a dichroic dye or iodine and stretching it uniaxially, or by impregnating a dichroic dye or iodine after stretching the PVA film uniaxially. It is made by crosslinking with boric acid.

しかし、かくして得られ次偏光模は湛度ざo ’C1相
対湿度10%のような高温高湿の雰囲気中におくと偏光
度は数日のうちに劣化して浸用にたえなくなる。
However, if the thus obtained polarized light pattern is placed in a high temperature and high humidity atmosphere such as a relative humidity of 10%, the degree of polarization deteriorates within a few days, making it unsuitable for immersion.

これ全改良する目的でPVAの代りポリエステルやナイ
ロンを用いること(特開昭II−/2100コ、特開昭
5r−a+りOコ、特開昭to−/!tμO/)、PV
At−脱水処理したポリビニレンを用いること(特公昭
tO−/Aり03、特公昭60−/λ3t7)、一部ポ
リエン化し次ポリ塩化ビニルを用いること(特公昭!タ
ー≠2tコロ)などが検討されているがこれらは耐湿性
は改良されるものの現行のPVA−ヨード系よりなる偏
光フィルムと比較する時それに対応する十分な偏光度が
得られていない。
For the purpose of completely improving this, polyester or nylon is used instead of PVA (JP-A Show II-/2100, JP-A Show 5r-a+ri-O, JP-A-Sho to-/!tμO/), PV
Consideration is being given to using At-dehydrated polyvinylene (Tokuko Sho tO-/Ari 03, Tokko Sho 60-/λ3t7), and using partially polyenized polyvinyl chloride (Tokuko Sho! Tar ≠ 2t Colo). However, although these films have improved moisture resistance, they do not have a sufficient degree of polarization when compared with current PVA-iodine polarizing films.

〔発明の目的〕[Purpose of the invention]

本発明は、これらの点を改良し、耐湿耐熱性があり、し
かも現行偏光フィルムと同等以上の偏光性含有す偏光フ
ィルムの製造方法に関するものである。
The present invention improves these points and relates to a method for producing a polarizing film that has moisture and heat resistance and has a polarizing property equivalent to or higher than that of current polarizing films.

〔発明の構成〕[Structure of the invention]

本発明によればPVAにヨード金含浸させたのち−Ni
lに延伸し7少くともグルタルアルデヒドを含有する酸
性4液で処理し乾燥することにより目的が達せられるこ
とがわかった。同じアルデヒド系でもホルマリン、アセ
トアルデヒド、グリオキザールは効果少なく、グルタル
アルデヒドが非常に効果のあることがわかった。
According to the present invention, after impregnating PVA with gold iodide, -Ni
It has been found that the object can be achieved by stretching the film to a length of 7 liters, treating it with an acidic solution containing at least glutaraldehyde, and drying. Even among aldehydes, formalin, acetaldehyde, and glyoxal were found to be less effective, while glutaraldehyde was found to be extremely effective.

PVAにヨードを含浸させるにはヨード及びヨウ化カリ
ウムの水溶液中にPVAt−浸漬すればよい。浸漬後ウ
ェット状態で/軸方向に2倍ないし2倍に延伸する。延
伸後緊張下で少くともグルタルアルデヒドを含む溶液で
処理をする。グルタルアルデヒド溶液中のグルタルアル
デヒドの謎、度は該PVAの処理時間に依存するが20
%から7%がよい。グルタルアルデヒド浴液ばpHμ以
下好ましくは3以下がよく、この溶液の中にはヨウ化カ
リなど加えても支障はない。
PVA can be impregnated with iodine by dipping the PVA in an aqueous solution of iodine and potassium iodide. After immersion, the film is stretched in a wet state/axially by a factor of 2 to 2 times. After stretching, the film is treated under tension with a solution containing at least glutaraldehyde. The mystery of glutaraldehyde in glutaraldehyde solution, the degree depends on the processing time of the PVA20
% to 7% is good. The pH of the glutaraldehyde bath solution should be less than μ, preferably less than 3, and there is no problem even if potassium iodide is added to this solution.

酸としては例えば塩酸、硝酸、硫酸の無機酸、橘酸、酢
酸、などの有機酸などを用いることができる。
Examples of acids that can be used include inorganic acids such as hydrochloric acid, nitric acid, and sulfuric acid, and organic acids such as citrus acid and acetic acid.

グルタルアルデヒドの酸性溶液で処理後、過剰のグルタ
ルアルデヒドを除去するため水洗してもよい。
After treatment with an acidic solution of glutaraldehyde, washing with water may be performed to remove excess glutaraldehyde.

処理後の乾燥け7よ0c以上i3o 0c以下が好まし
い。乾燥は初期、乾燥は低温で、後乾燥で部属にするな
どしても伺ら支障はない。
The drying temperature after treatment is preferably 7 to 0 c or more and i3 to 0 c or less. There is no problem in drying in the initial stage, drying at low temperature, and post-drying to separate parts.

グルタルアルデヒドを含有する@液で処理することによ
り耐湿耐熱性が向上するばかりでなく、おどろくべきこ
とに長波長側、特に7.rOnm近傍の光の偏光度が向
上することがわかった。
Treatment with @solution containing glutaraldehyde not only improves moisture and heat resistance, but also surprisingly improves resistance to long wavelengths, especially 7. It was found that the degree of polarization of light near rOnm was improved.

グルタルアルデヒド処理し乾燥した該偏光フィルムはセ
ルローストリアセテート、セルロースアセテートブチレ
ート、−軸延伸ポリエチレンテレフタレート、ポリエー
テルスルホンなどのフィルム?保護としてラミネートし
て使用することは何ら支障はない。
The polarizing film treated with glutaraldehyde and dried is a film of cellulose triacetate, cellulose acetate butyrate, -axially oriented polyethylene terephthalate, polyether sulfone, etc. There is no problem in laminating and using it for protection.

以下に実施例を記述するが、実施例中の測定及び評価は
次の方法で行つfc。
Examples will be described below, and measurements and evaluations in the examples will be performed using the following methods.

〔偏光度〕二分光々度計を用い、二枚の偏光フィルムを
同一配向方向に重ねて測定し定時の最大吸収波長での透
過率のIi!i、kToとし配向方向を互に直角にして
重ねて測定し友時の最大吸収波長での透過率をT2Oと
して次式で計算した。
[Degree of polarization] Using a two-spectrum photometer, measure two polarizing films stacked in the same orientation direction, and measure the transmittance Ii at the maximum absorption wavelength at a given time! i, kTo, the orientation directions were set at right angles to each other, and the transmittance at the maximum absorption wavelength was calculated using the following formula as T2O.

更に波長fz7jOnmにした時の夫々の透過率より同
様に計ばしたf[f全7jOnmでの偏光度とした。
Furthermore, the degree of polarization at f [f total 7j Onm was calculated in the same manner from the respective transmittances when the wavelength was set to fz7j Onm.

〔耐湿耐熱性〕:@度ro 0c、相対湿間?O%の雰
囲気中に弘!時間放置し、その後の偏光度?測定し、初
期の偏光度に対しての低下が!チ以内のもの金A1 !
チル20%までのもの金B1コ0係以上低下したものを
Cとした。
[Humidity and heat resistance]: @degrees RO 0C, relative humidity? Hiro in the atmosphere of O%! Leave it for a while and then the degree of polarization? Measure and see the decrease in the initial degree of polarization! Money within 1 A1!
A case where the temperature decreased by more than a factor of 0 with gold B1 up to 20% was classified as C.

実施例/ 厚さ75μのPVAフィルム(クラレ■製光学用フィル
ム)をヨード/%(wt)、ヨウ化カリウム2%(Wt
)の水溶液に7分間浸漬後、ウェット状幅で3倍に延押
し次。緊張状聾の互まグルタルアルデヒド!%(wt)
、塩酸0.3j%(wt)の水gQ(pI−(/ 、 
3o )中に7分間浸漬し700 °Cで70分間乾燥
し、偏光フィルムとした。この偏光フィルムの両面に保
護膜として10μのセルローストリアセテートをラミネ
ートし、サンプル(1)とした。
Example/ A PVA film (optical film made by Kuraray ■) with a thickness of 75μ was prepared by adding iodine/% (wt) and potassium iodide 2% (wt).
) After soaking in an aqueous solution for 7 minutes, the sample was stretched to 3 times its width in a wet state and then pressed. Glutaraldehyde for catatonic deafness! %(wt)
, hydrochloric acid 0.3j% (wt) water gQ (pI-(/,
3o) for 7 minutes and dried at 700°C for 70 minutes to obtain a polarizing film. A 10 μm cellulose triacetate film was laminated as a protective film on both sides of this polarizing film to obtain a sample (1).

比較例/ 実施例/と同様なPVAフィルムをヨード/%(w t
 )、ヨウ化カリウム2%(w t )の水溶液に7分
間浸漬した後、ウェット状ゆで3@に延伸した。緊張状
的のままグリオキザール2.2チ(wt)、塩酸0.3
よ%(wt )の水溶液中に7分間浸漬し、10o 0
cで70分間乾燥し偏光フィルムとした。実施例(1)
と同様な保護膜をラミネートしサンプル(2)とした。
A PVA film similar to Comparative Example/Example/was prepared with iodine/% (w t
), immersed in an aqueous solution of 2% (w t ) potassium iodide for 7 minutes, then wet-boiled and stretched to 3@. Glyoxal 2.2 t (wt), hydrochloric acid 0.3 while in a nervous state
% (wt) aqueous solution for 7 minutes, and
The film was dried at c for 70 minutes to obtain a polarizing film. Example (1)
A similar protective film was laminated to prepare sample (2).

比較例コ 実施例1と同様なPVAフィルムをりo ’Cに加熱し
一町に3倍延伸し、/弘o ’Cで70分間熱処理した
。このフィルムを緊張状態のままヨード3%(wt )
、ヨウ化カリウムjチ(w t )、グルタルアルテビ
ド7%(wt)、塩酸0 、 j J−チ(wt)の水
溶液(pH=/ 、 4!j )に2分間浸漬し100
0Cで乾燥し偏光フィルムとした。
Comparative Example A PVA film similar to that of Example 1 was heated to 100°C, stretched 3 times in one direction, and heat treated at 200°C for 70 minutes. This film was kept under tension with 3% iodine (wt)
, potassium iodide (wt), glutarartebide 7% (wt), hydrochloric acid (0%), jJ-chi (wt) for 2 minutes immersed in an aqueous solution (pH=/, 4!j) of 100
It was dried at 0C to form a polarizing film.

実施例il+と同様な保護膜をラミネートしサンプル(
3)とした。
A protective film similar to that of Example il+ was laminated and a sample (
3).

比較例3 実施例(1)と同様fZPVktヨー )”/ % (
wt )、ヨウ化カリウム2%(wt )の水溶液に1
分間浸漬後、3倍に延伸し、緊張状態のままホウ酸≠チ
(wt )の水溶液中に1分間浸漬し、1000Cでi
o分間乾燥して偏光フィルムとし次。
Comparative Example 3 Same as Example (1) fZPVkt Yaw )”/% (
wt ), 1 in an aqueous solution of 2% (wt ) potassium iodide.
After immersion for 1 minute, it was stretched 3 times, immersed for 1 minute in an aqueous solution of boric acid≠thi(wt) under tension, and then heated at 1000C for i.
Dry for o minutes to form a polarizing film.

実施例(1)と同様な保護膜をラミネートしサンプル(
4)とし念。
A protective film similar to that in Example (1) was laminated and the sample (
4) Reminder.

以上のサンプルについて偏光度及び耐湿耐熱をしらべた
。結果を第1表に示す。本発明の方法がもつともすぐれ
ていることがわかる。
The degree of polarization and moisture resistance and heat resistance of the above samples were examined. The results are shown in Table 1. It can be seen that the method of the present invention is also superior.

第7表Table 7

Claims (1)

【特許請求の範囲】[Claims] ヨードを含有するポリビニルアルコールフィルムを一軸
延伸する偏光フィルムの製造方法において、ヨード含有
ポリビニルアルコールフィルムを一軸に延伸したのち、
グルタルアルデヒドの酸性溶液で処理し、乾燥すること
を特徴とする偏光フィルムの製造方法。
In a method for producing a polarizing film in which an iodine-containing polyvinyl alcohol film is uniaxially stretched, after the iodine-containing polyvinyl alcohol film is uniaxially stretched,
A method for producing a polarizing film, which comprises treating with an acidic solution of glutaraldehyde and drying.
JP22518185A 1985-10-09 1985-10-09 Production of polarizing film Pending JPS6285203A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP22518185A JPS6285203A (en) 1985-10-09 1985-10-09 Production of polarizing film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP22518185A JPS6285203A (en) 1985-10-09 1985-10-09 Production of polarizing film

Publications (1)

Publication Number Publication Date
JPS6285203A true JPS6285203A (en) 1987-04-18

Family

ID=16825228

Family Applications (1)

Application Number Title Priority Date Filing Date
JP22518185A Pending JPS6285203A (en) 1985-10-09 1985-10-09 Production of polarizing film

Country Status (1)

Country Link
JP (1) JPS6285203A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0259336A (en) * 1988-08-24 1990-02-28 Mitsubishi Monsanto Chem Co Polarizing film
US5087985A (en) * 1988-07-12 1992-02-11 Toray Industries, Inc. Polarizer for visible light
JPH07104126A (en) * 1993-10-05 1995-04-21 Kuraray Co Ltd Production of polarizing film

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5087985A (en) * 1988-07-12 1992-02-11 Toray Industries, Inc. Polarizer for visible light
JPH0259336A (en) * 1988-08-24 1990-02-28 Mitsubishi Monsanto Chem Co Polarizing film
JPH07104126A (en) * 1993-10-05 1995-04-21 Kuraray Co Ltd Production of polarizing film

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