JPH0465095B2 - - Google Patents
Info
- Publication number
- JPH0465095B2 JPH0465095B2 JP26357087A JP26357087A JPH0465095B2 JP H0465095 B2 JPH0465095 B2 JP H0465095B2 JP 26357087 A JP26357087 A JP 26357087A JP 26357087 A JP26357087 A JP 26357087A JP H0465095 B2 JPH0465095 B2 JP H0465095B2
- Authority
- JP
- Japan
- Prior art keywords
- film
- polarizing plate
- triacetate film
- triacetate
- resin
- 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.)
- Expired
Links
- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 claims description 29
- 239000011248 coating agent Substances 0.000 claims description 21
- 238000000576 coating method Methods 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 15
- 239000004925 Acrylic resin Substances 0.000 claims description 11
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 5
- 239000011347 resin Substances 0.000 description 9
- 229920005989 resin Polymers 0.000 description 9
- 239000004973 liquid crystal related substance Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 235000010724 Wisteria floribunda Nutrition 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- -1 acrylate ester Chemical class 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 230000003678 scratch resistant effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 210000001685 thyroid gland Anatomy 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Landscapes
- Polarising Elements (AREA)
- Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)
- Laminated Bodies (AREA)
Description
産業上の利用分野：
本発明は、耐擦傷性、耐薬品性、防眩性にすぐ
れたトリアセテートフイルムに関するものであ
る。当該トリアセテートフイルムの利用分野とし
ては偏光板、写真・印刷物の保護、OHPシート
など広汎に可能であるが、とくに沃素及び、もし
くは二色性染料系偏光フイルムに貼合するトリア
セテートフイルムとして使用すれば、耐擦傷性、
耐薬品性、防眩性のきわめてすぐれた偏光板を作
ることができる。該偏光板を用いて液晶表示体を
構成すると、偏光板に対する保護板や保護フイル
ムが不要となり、軽量で厚みが薄く視認性の高い
表示体が得られる。
液晶表示体は、電卓、時計、ポケツトテレビ、
パーソナルコンピユーター、車載用計器などの各
種表示に広く利用されつつあり、画面の大型化に
ともない、表示体の薄型化・軽量化が高画質化、
カラー化とともに開発の重要目標となつている。
本発明のトリアセテートフイルムは、このよう
な液晶表示体の薄型化・軽量化に大きく寄与する
ものである。
従来の技術とその問題点：
従来の液晶表示体では、通常の偏光板が耐擦傷
性に耐薬品性に劣るために、表示体画面の最表面
には、ガラスもしくは透明プラスチツク板を設
け、偏光板を保護しなければならなかつた。この
ため、成形された偏光板（偏光フイルムとトリア
セテートフイルムなどの透明プラスチツクフイル
ムを接着剤で貼合したもの）にポリエステルアク
リレート系樹脂、（メタ）アクリル酸エステル系
樹脂、ポリエステルアクリレート系樹脂、アクリ
ルウレタン樹脂などによる硬化塗膜を設け、耐擦
傷性、耐薬品性を付与する工夫がなされてきた
が、その性能は不十分なものであつた。
問題点を解決するための手段：
本発明者らは、皮膜硬度、耐薬品性にすぐれる
紫外線硬化型エポキシアクリレート系樹脂が、未
ケン化のトリアセテートフイルムに対しては、密
着性の良好な塗膜を形成することを見出し本発明
を完成するに至つた。通常、偏光板の成形時に
は、トリアセテートフイルムは偏光フイルムとの
貼合前に接着性を上げるためにケン化処理を受け
るが、ケン化処理されたトリアセテートフイルム
に対しては、紫外線硬化型エポキシアクリレート
系樹脂は著しく塗膜密着性が劣る。ケン化処理を
うけたトリアセテートフイルムに対し該樹脂の硬
化塗膜が密着の悪い原因は明確ではないが、ケン
化後のトリアセテートフイルム表面に吸着した水
分が該樹脂と一部反応するためではないかと考え
られる。
本発明のトリアセテートフイルムを偏光板の構
成材料として利用するには、該樹脂の硬化塗膜を
設けたトリアセテートフイルムのもう一方の面に
ケン化処理を施した後、通常の成形工程を経て偏
光板とすればよい。
偏光板に防眩性をさらに付与するには、該樹脂
に無定形シリカ粉末を必要料配合した組成液を未
ケン化のトリアセテートフイルムに塗工し硬化皮
膜を設けたフイルムを上述の貼合工程で使用すれ
ば、耐擦傷性、耐薬品性、防眩性を合わせもつ偏
光板を得ることができる。
従来の偏光板に硬化塗膜を設ける方法に較べ、
本発明のトリアセテートフイルムに硬化塗膜を設
けた後に偏光板に成形すると製品歩留まりも高く
経済的に著しく有利である。
さらに、本発明のトリアセテートフイルムで成
形された偏光板を用い液晶表示体を構成すると、
該アセテートフイルムの耐擦傷性、耐薬品性、防
眩性がすぐれているために、偏光板の保護材料を
必要とせず、液晶表示体の厚みを薄く、かつ軽く
することができる。
本発明のトリアセテートフイルムは、偏光板の
構成材料としてのみでなく、その耐擦傷性、耐薬
品性、防眩性のすぐれていることを生かし、種々
の用途に使用可能である。たとえば、写真、印刷
物の表面保護のためにその表面に貼付するなどの
用途が考えられ、とくに偏光板の構成材料として
の用途のみに限定されない。
実施例：
以下に本発明を実施例、比較例に基づいて詳細
に説明する。本発明は、これに限定されるもので
はない。
実施例 １
未ケン化のトリアセテートフイルム（富士写真
フイルム(株)製FTUV；厚み80μ）の一方の面に紫
外線硬化型エポキシアクリレート系樹脂（エポキ
シアクリレートをオリゴマーとし、これに反応性
希釈剤、光反応開始剤などを添加したもの）を塗
工厚が5μとなるように塗工したのち差外線照射
（UV出力44W／cm）し、塗膜を硬化した。
比較例 １
アルカリ溶液によりケン化処理したトリアセテ
ートフイルムを用いる他は実施例１と同様にし
て、硬化皮膜を有するトリアセテートフイルムを
得た。
実施例 ２
無定形シリカ粉末（富士デヴインソン化学社製
サイロイド244）のトルエン分散液を液と同重量
のガラスビーズとともに30分間、約1500回転の速
度で攪拌した。その後、固型分重量比が98.5：
1.5となるように紫外線硬化型エポキシアクリレ
ート系樹脂とサイロイド244分散液を混合した
（固型分濃度75％）。この混合液を塗工厚が5μと
なるように未ケン化のトリアセテートフイルムに
塗工した後実施例１と同様に紫外線により硬化し
試料とした。
比較例 ２
未ケン化のトリアセテートフイルムの一方の面
に非紫外線硬化型アクリル系樹脂とシリカ粉末か
らなる組成物による硬化皮膜を設けた。第１表に
測定結果を示す。
Industrial Application Field: The present invention relates to a triacetate film with excellent scratch resistance, chemical resistance, and antiglare properties. The triacetate film can be used in a wide range of fields, including polarizing plates, protection of photographs and printed matter, and OHP sheets, but especially when used as a triacetate film laminated to iodine and/or dichroic dye-based polarizing films, Scratch resistance,
A polarizing plate with excellent chemical resistance and anti-glare properties can be made. When a liquid crystal display is constructed using the polarizing plate, a protective plate or protective film for the polarizing plate becomes unnecessary, and a display that is lightweight, thin, and highly visible can be obtained. Liquid crystal displays are used in calculators, watches, pocket televisions,
It is becoming widely used for various displays such as personal computers and in-vehicle instruments, and as screens become larger, display bodies become thinner and lighter, resulting in higher image quality.
Along with colorization, this has become an important development goal. The triacetate film of the present invention greatly contributes to making such liquid crystal displays thinner and lighter. Conventional technology and its problems: In conventional liquid crystal displays, ordinary polarizing plates have poor scratch resistance and chemical resistance, so a glass or transparent plastic plate is provided on the top surface of the display screen to polarize I had to protect the board. For this reason, a molded polarizing plate (a polarizing film and a transparent plastic film such as triacetate film bonded together with an adhesive) is coated with polyester acrylate resin, (meth)acrylate ester resin, polyester acrylate resin, acrylic urethane resin, etc. Efforts have been made to provide a hardened coating film made of resin or the like to provide scratch resistance and chemical resistance, but the performance has been insufficient. Means for Solving the Problem: The present inventors have discovered that an ultraviolet curable epoxy acrylate resin with excellent film hardness and chemical resistance has good adhesion to unsaponified triacetate film. They discovered that a film can be formed and completed the present invention. Normally, when forming a polarizing plate, triacetate film is saponified to improve adhesion before being laminated with the polarizing film. Resin has significantly poor coating adhesion. The reason why the cured coating film of this resin has poor adhesion to the saponified triacetate film is not clear, but it may be because the water adsorbed on the surface of the triacetate film after saponification partially reacts with the resin. Conceivable. In order to use the triacetate film of the present invention as a constituent material of a polarizing plate, the other side of the triacetate film provided with the cured coating of the resin is saponified, and then the polarizing plate is formed through a normal molding process. And it is sufficient. In order to further impart anti-glare properties to the polarizing plate, a composition liquid in which the resin is mixed with amorphous silica powder is applied to an unsaponified triacetate film, a cured film is formed, and the film is then subjected to the above lamination process. If used in , it is possible to obtain a polarizing plate that has scratch resistance, chemical resistance, and anti-glare properties. Compared to the conventional method of applying a cured coating to a polarizing plate,
If the triacetate film of the present invention is formed into a polarizing plate after being provided with a cured coating, the product yield will be high and it will be economically advantageous. Furthermore, when a liquid crystal display is constructed using a polarizing plate formed from the triacetate film of the present invention,
Since the acetate film has excellent scratch resistance, chemical resistance, and antiglare properties, a protective material for the polarizing plate is not required, and the thickness of the liquid crystal display can be made thin and light. The triacetate film of the present invention can be used not only as a constituent material of a polarizing plate, but also for various purposes, taking advantage of its excellent scratch resistance, chemical resistance, and antiglare properties. For example, it may be applied to the surface of photographs or printed matter to protect the surface thereof, and is not particularly limited to use as a constituent material of a polarizing plate. Examples: The present invention will be described in detail below based on Examples and Comparative Examples. The present invention is not limited to this. Example 1 One side of an unsaponified triacetate film (FTUV manufactured by Fuji Photo Film Co., Ltd.; thickness 80 μm) was coated with an ultraviolet curable epoxy acrylate resin (an oligomer of epoxy acrylate, which was treated with a reactive diluent and a photoreactive material). After applying a coating with a coating thickness of 5 μm (adding an initiator, etc.), the coating film was cured by differential external ray irradiation (UV output: 44 W/cm). Comparative Example 1 A triacetate film having a cured film was obtained in the same manner as in Example 1, except that a triacetate film saponified with an alkaline solution was used. Example 2 A toluene dispersion of amorphous silica powder (Syroid 244 manufactured by Fuji Devinson Chemical Co., Ltd.) was stirred with glass beads of the same weight as the liquid for 30 minutes at a speed of about 1500 revolutions. After that, the solid content weight ratio is 98.5:
The UV-curable epoxy acrylate resin and Thyroid 244 dispersion were mixed so that the solid content was 1.5% (solid content concentration 75%). This mixed solution was coated on an unsaponified triacetate film to a coating thickness of 5 μm, and then cured with ultraviolet rays in the same manner as in Example 1 to prepare a sample. Comparative Example 2 A cured film made of a composition consisting of a non-ultraviolet curable acrylic resin and silica powder was provided on one side of an unsaponified triacetate film. Table 1 shows the measurement results.
【表】【table】
【表】
測定方法は次の通り行なつた。（番号は第１表
中の番号と対応する）
(1) ２mm口の切りこみを塗膜に入れた後にセロテ
ープでひきはがし塗膜の残つているマス目の数
を％で表示。
(2) １Kg／cm2の荷重を塗膜にかけながら、スチー
ルウール＃0000で100往復する前、後でのヘイ
ズ度の差を％で表示。小さい程、耐擦傷性が良
い。
(3) 日本電色工業製曇度計ND−H67により測
定。
(4) 日立分光々度計330（60φ積分球）を使用し、
試料ホルダーのスペーサー（10゜）有無により
その差から算出。
(5) 各溶剤を塗膜面に滴下１分後にふきとり、そ
の表面の変化の有無を観察した。
（○は変化なし、×は変化あり。）
実施例１では、比較例１に較べ塗膜密着度が良
好であり、このため耐擦傷性も良好である。
実施例２は適度の防眩性（塗膜表面での光の乱
反射により正反射率が低下し、ヘイズ度が実施例
１に較べ上がる。）を有しながら、耐擦傷性、耐
薬品性がすぐれている。
発明の効果：
本発明の硬化塗膜を有するトリアセテートフイ
ルムは、紫外線硬化型エポキシアクリレート系樹
脂単独もしくは同樹脂と無定形シリカとからなる
組成物からなる硬化塗膜を未ケン化のトリアセテ
ートフイルム上に設けることにより、きわめてす
ぐれた耐擦傷性、耐薬品性、防眩性を有するトリ
アセテートフイルムであり、その効果を列挙する
と以下の通りである。
(1) 未ケン化のトリアセテートフイルムの一方の
面に紫外線硬化型エポキシアクリレート系樹脂
単独もしくは同樹脂と無定形シリカとからなる
組成物の硬化塗膜を設けることにより塗膜の密
着性が向上し、耐擦傷性も向上する。
(2) 紫外線硬化エポキシアクリレート系樹脂を主
とする硬化塗膜により、すぐれた耐薬品性が得
られる。
(3) 本発明のトリアセテートフイルムを偏光板の
構成材料として使用すれば、耐擦傷性、耐薬品
性、防眩性を有する偏光板の製品歩留まりが向
上する。
(4) 本発明の耐擦傷性、耐薬品性、防眩性を有す
るトリアセテートフイルムを構成材料とした偏
光板を液晶表示体に使用すれば、偏光板の保護
板が不要となり、表示体の薄型化、軽量化が実
現できる。[Table] The measurement method was as follows. (The numbers correspond to the numbers in Table 1) (1) After making a 2 mm cut into the paint film, peel it off with cellophane tape and indicate the number of squares remaining in the paint film as a percentage. (2) The difference in haze degree is expressed as a percentage before and after 100 reciprocations with #0000 steel wool while applying a load of 1 kg/cm 2 to the coating film. The smaller the value, the better the scratch resistance. (3) Measured using Nippon Denshoku Kogyo haze meter ND-H67. (4) Using Hitachi spectrophotometer 330 (60φ integrating sphere),
Calculated from the difference between the presence and absence of a spacer (10°) on the sample holder. (5) After dropping each solvent onto the coating surface for 1 minute, it was wiped off and the presence or absence of any change in the surface was observed. (○ indicates no change, × indicates change.) In Example 1, the coating film adhesion was better than in Comparative Example 1, and therefore the scratch resistance was also good. Example 2 has moderate anti-glare properties (specular reflectance decreases due to diffuse reflection of light on the coating surface, and the degree of haze increases compared to Example 1), but also has good scratch resistance and chemical resistance. It is excellent. Effect of the invention: The triacetate film having a cured coating film of the present invention is produced by applying a cured coating film made of an ultraviolet curable epoxy acrylate resin alone or a composition consisting of the same resin and amorphous silica onto an unsaponified triacetate film. This triacetate film has extremely excellent scratch resistance, chemical resistance, and anti-glare properties, and its effects are listed below. (1) By providing a cured coating film of an ultraviolet curable epoxy acrylate resin alone or a composition consisting of the same resin and amorphous silica on one side of an unsaponified triacetate film, the adhesion of the coating film is improved. , abrasion resistance is also improved. (2) Excellent chemical resistance is achieved by the cured coating film, which is mainly made of UV-curable epoxy acrylate resin. (3) When the triacetate film of the present invention is used as a constituent material of a polarizing plate, the product yield of the polarizing plate having scratch resistance, chemical resistance, and antiglare properties is improved. (4) If a polarizing plate made of the scratch-resistant, chemical-resistant, and anti-glare triacetate film of the present invention is used in a liquid crystal display, a protective plate for the polarizing plate becomes unnecessary, and the display becomes thinner. It can be made lighter and lighter.
Claims (1)
面に、紫外線硬化型エポキシアクリレート系樹脂
からなる硬化塗膜を設けたことを特徴とする耐擦
傷性、耐薬品性にすぐれたトリアセテートフイル
ム。 ２ 硬化塗膜が、紫外線硬化型エポキシアクリレ
ート系樹脂と無定形シリカを含む組成物からなる
ことを特徴とする、特許請求の範囲第１項記載の
耐擦傷性、耐薬品性、防眩性にすぐれたトリアセ
テートフイルム。[Scope of Claims] 1. A triacetate with excellent scratch resistance and chemical resistance, characterized in that a cured coating film made of an ultraviolet curable epoxy acrylate resin is provided on one side of an unsaponified triacetate film. film. 2. The scratch resistance, chemical resistance, and anti-glare properties of claim 1, wherein the cured coating film is made of a composition containing an ultraviolet curable epoxy acrylate resin and amorphous silica. Excellent triacetate film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26357087A JPH01105738A (en) | 1987-10-19 | 1987-10-19 | Triacetate film with scratch resistance, chemical resistance and glare resistance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26357087A JPH01105738A (en) | 1987-10-19 | 1987-10-19 | Triacetate film with scratch resistance, chemical resistance and glare resistance |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01105738A JPH01105738A (en) | 1989-04-24 |
| JPH0465095B2 true JPH0465095B2 (en) | 1992-10-19 |
Family
ID=17391384
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26357087A Granted JPH01105738A (en) | 1987-10-19 | 1987-10-19 | Triacetate film with scratch resistance, chemical resistance and glare resistance |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01105738A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020170784A1 (en) | 2019-02-22 | 2020-08-27 | パナソニックＩｐマネジメント株式会社 | High frequency heating apparatus |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2530537B2 (en) * | 1991-12-13 | 1996-09-04 | 日本製紙株式会社 | Hard coat film |
| JP2967474B2 (en) * | 1997-03-27 | 1999-10-25 | 株式会社巴川製紙所 | Anti-glare material and polarizing film using the same |
| EP2233605B1 (en) | 2000-12-12 | 2012-09-26 | Konica Corporation | Optical film comprising an anti-reflection layer |
| US8304086B2 (en) | 2005-05-26 | 2012-11-06 | Eastman Chemical Company | Crosslinkable, cellulose ester compositions and films formed therefrom |
| KR101281878B1 (en) | 2005-08-30 | 2013-07-03 | 코니카 미놀타 어드밴스드 레이어즈 인코포레이티드 | Liquid crystal display |
| JPWO2007026545A1 (en) | 2005-08-31 | 2009-03-05 | コニカミノルタホールディングス株式会社 | Plasma discharge treatment apparatus and method for producing gas barrier film |
| JP5089312B2 (en) * | 2007-09-28 | 2012-12-05 | 日揮触媒化成株式会社 | Base material with hard coat film and coating liquid for forming hard coat film |
-
1987
- 1987-10-19 JP JP26357087A patent/JPH01105738A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020170784A1 (en) | 2019-02-22 | 2020-08-27 | パナソニックＩｐマネジメント株式会社 | High frequency heating apparatus |
| EP3929490A4 (en) * | 2019-02-22 | 2022-04-20 | Panasonic Intellectual Property Management Co., Ltd. | High frequency heating apparatus |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01105738A (en) | 1989-04-24 |
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| EXPY | Cancellation because of completion of term |