JPH05140392A - Polystyrenic resin composition, sheet and containers composed of the same - Google Patents
Polystyrenic resin composition, sheet and containers composed of the sameInfo
- Publication number
- JPH05140392A JPH05140392A JP33400391A JP33400391A JPH05140392A JP H05140392 A JPH05140392 A JP H05140392A JP 33400391 A JP33400391 A JP 33400391A JP 33400391 A JP33400391 A JP 33400391A JP H05140392 A JPH05140392 A JP H05140392A
- Authority
- JP
- Japan
- Prior art keywords
- sheet
- resin composition
- slipperiness
- compound
- cup
- 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.)
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Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、ポリスチレン系樹脂組
成物、それからなるシート及び容器類に関し、更に詳し
くは、成形が良好で、且つ滑り性(アイスクリーム、プ
リン等の固形内容物の易取り出し性、スタッキング特性
等)及び炭酸飲料の発泡抑制効果に優れたポリスチレン
系樹脂組成物、それからなるシート及び容器類に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polystyrene resin composition, sheets and containers made of the same, and more particularly, it has good molding properties and slipperiness (easy removal of solid contents such as ice cream and pudding). Properties, stacking characteristics, etc.) and a foaming-suppressing effect of a carbonated beverage, and a sheet and containers made of the same.
【0002】[0002]
【従来の技術】従来、容器用材料としては、例えば特開
平1−26440号公報に、紙等の基材と、該基材上に
積層された樹脂層とからなる積層材料が記載されてい
る。この積層材料は樹脂層に工夫が加えられているた
め、炭酸飲料の発泡抑制効果に優れ、且つベンディング
マシンにおけるスタッキング特性にも優れたものである
が、成形性が必ずしも充分でなく、特に紙基材を用いた
場合には、真空成形や圧空成形により一挙にカップに成
形するということができない憾みがある。2. Description of the Related Art Conventionally, as a material for a container, for example, Japanese Patent Laid-Open No. 1-264040 describes a laminated material composed of a base material such as paper and a resin layer laminated on the base material. .. Since this laminated material has been devised in the resin layer, it is excellent in the effect of suppressing the foaming of carbonated beverages and also in the stacking characteristics of a bending machine, but it does not always have sufficient moldability, and it is particularly difficult to use paper-based materials. When a material is used, there is a problem that it cannot be formed into a cup at once by vacuum forming or pressure forming.
【0003】[0003]
【発明が解決しようとする課題】本発明はかかる実情に
鑑み、真空成形や圧空成形及び射出成形が容易に行え、
且つ滑り性及び発泡抑制効果に優れた樹脂組成物、シー
ト及び容器類を提供するものである。In view of the above situation, the present invention can easily perform vacuum forming, pressure forming and injection molding.
Further, it is intended to provide a resin composition, a sheet and containers which are excellent in slipperiness and foaming suppression effect.
【0004】[0004]
【課題を解決するための手段】即ち、本発明の第1は、
ポリスチレン系樹脂にシリコーン化合物を0.1〜1
0.0重量%含有させてなる、成形加工性、滑り性及び
炭酸飲料の発泡抑制効果に優れた樹脂組成物を、本発明
の第2は、上記樹脂組成物からなるシートを、本発明の
第3は、第2の発明のシートをポリスチレン系樹脂から
なる基材上に積層してなるシートを、本発明の第4は、
第1の発明の樹脂組成物を成形してなる容器類を、本発
明の第5は、第2又は第3の発明のシートを成形してな
る容器類を、それぞれ内容とするものである。That is, the first aspect of the present invention is to:
0.1 to 1 of silicone compound in polystyrene resin
A second aspect of the present invention is a resin composition containing 0.0% by weight, which is excellent in molding processability, slipperiness and foaming suppression effect of carbonated beverages, and a second aspect of the present invention is a sheet comprising the resin composition. The third is a sheet obtained by laminating the sheet of the second invention on a base material made of polystyrene resin, and the fourth of the invention is
A container formed by molding the resin composition of the first invention, and a fifth container of the present invention include containers formed by molding the sheet of the second or third invention.
【0005】本発明におけるポリスチレン系樹脂として
は、スチレン、α−メチルスチレン、クロロスチレン、
ジクロロスチレン、ブロモスチレン、ジメチルスチレ
ン、t−ブチルスチレン等のスチレン誘導体の単独重合
体又はそれらの組み合わせからなる共重合体、及びスチ
レン誘導体とジビニルベンゼン、メチルメタクリレート
アクリロニトリル、ブタジェン、イソプレン等との共重
合体等が挙げられる。The polystyrene resin in the present invention includes styrene, α-methylstyrene, chlorostyrene,
Homopolymers of styrene derivatives such as dichlorostyrene, bromostyrene, dimethylstyrene, and t-butylstyrene, or copolymers composed of combinations thereof, and copolymerization of styrene derivatives with divinylbenzene, methyl methacrylate acrylonitrile, butadiene, isoprene, etc. Examples include coalescence.
【0006】本発明におけるシリコーン化合物として
は、少なくとも1個の水素基を有する有機珪素化合物
と、該水素基と反応する二重結合を少なくとも1個有す
る炭素数18以上の炭化水素化合物とを反応させてなる
櫛型グラフトポリマーが特に好適に用いられる。この変
性シリコーン化合物の製造方法は、例えば特開昭63−
3076号公報に詳記されている。シリコーン化合物と
しては、他に一般のシリコーンオイル、メチルスチレン
基、メチルフェニル基等で一部を変性した変性シリコー
ンオイルや、シリコーン高分子ポリマーを汎用(GP)
ポリスチレン又はハイインパクト(HI)ポリスチレン
に高濃度に混練したシリコーンマスターバッチ等も挙げ
られる。As the silicone compound in the present invention, an organosilicon compound having at least one hydrogen group is reacted with a hydrocarbon compound having at least one double bond capable of reacting with the hydrogen group and having 18 or more carbon atoms. Comb-type graft polymers obtained from the above are particularly preferably used. A method for producing this modified silicone compound is described in, for example, JP-A-63-
It is described in detail in Japanese Patent No. 3076. As the silicone compound, general silicone oil, modified silicone oil partially modified with methylstyrene group, methylphenyl group, etc., and silicone polymer are generally used (GP).
A silicone masterbatch obtained by kneading polystyrene or high impact (HI) polystyrene at a high concentration can also be used.
【0007】本発明において、ポリスチレン系樹脂に対
するシリコーン化合物の配合割合は、0.1〜10.0
重量%の範囲である。0.1重量%未満では滑り性や発
泡抑制効果が不充分となり、10.0重量%を越えると
成形性が悪くなる。In the present invention, the blending ratio of the silicone compound to the polystyrene resin is 0.1 to 10.0.
It is in the range of% by weight. If it is less than 0.1% by weight, the slipperiness and foaming suppressing effect are insufficient, and if it exceeds 10.0% by weight, the moldability becomes poor.
【0008】上記配合物は、成形性、滑り性、発泡抑制
効果等に優れているので、飲料用、特に炭酸飲料用カッ
プや、アイスクリーム、プリン等の容器として好適で、
通常、ペレタイザーでペレット化され、シート状に押し
出され、真空成形や圧空成形によりカップや容器とされ
る。シートの厚さは0.3〜3mm程度が好適である。ま
た、このペレットを更に押出ラミネート法等によりポリ
スチレン系樹脂からなる基材上に積層することも可能で
ある。この場合のラミネート厚さは5〜30μm程度が
好適である。また本発明の樹脂組成物は射出成形により
一挙にカップや容器としてもよい。この場合、内層のみ
を本発明の配合物としてもよい。基材層を発泡層とする
こともでき、これにより断熱性が高められる。Since the above-mentioned compound is excellent in moldability, slipperiness, foam suppressing effect, etc., it is suitable as a cup for beverages, particularly carbonated beverages, and a container for ice cream, pudding, etc.
Usually, it is pelletized by a pelletizer, extruded into a sheet shape, and formed into a cup or a container by vacuum forming or pressure forming. The thickness of the sheet is preferably about 0.3 to 3 mm. Further, the pellets can be further laminated on a base material made of polystyrene resin by an extrusion laminating method or the like. In this case, the laminate thickness is preferably about 5 to 30 μm. Further, the resin composition of the present invention may be formed into a cup or a container by injection molding. In this case, only the inner layer may be the composition of the present invention. The base material layer may be a foamed layer, which enhances heat insulation.
【0009】積層は、押出ラミネート、ドライラミネー
ト、ウエットラミネート、接着等の公知の方法が全て使
用されるが、特に押出ラミネート(共押出)が生産効率
の面から好適である。For the lamination, known methods such as extrusion lamination, dry lamination, wet lamination and adhesion are all used, but extrusion lamination (coextrusion) is particularly preferable from the viewpoint of production efficiency.
【0010】[0010]
【実施例】以下、実施例に基づいて本発明を更に詳細に
説明するが、本発明の範囲はかかる実施例のみに限定さ
れるものではない。尚、以下の記載において「部」、
「%」はそれぞれ「重量部」、「重量%」を意味する。 参考例 ポリメチルハイドロジェンシロキサン(P=600、M
W=44000)56部、α−オレフィン「ダイヤレン
−30」、(三菱化成株式会社製、炭素数:28〜5
2)44部、0.1%H2 PtCl6 ・6H2 Oのイソ
プロピルアルコール溶液3部を反応器に仕込み、120
℃で5時間付加反応させ、次いで更に0.1%H2 Pt
Cl6 ・6H2 Oのイソプロピルアルコール溶液3部を
加え、更にプロピレン0.5部を反応器に仕込み、12
0℃で3時間反応させた。反応生成物はアセトンで3回
洗浄し、精製乾燥した。得られた剥離剤のシリコーン含
有率は56%であった。The present invention will be described in more detail based on the following examples, but the scope of the present invention is not limited to these examples. In the following description, "part",
"%" Means "part by weight" and "% by weight", respectively. Reference example Polymethyl hydrogen siloxane (P = 600, M
W = 44000) 56 parts, α-olefin “Dialene-30”, (manufactured by Mitsubishi Kasei Co., Ltd., carbon number: 28-5)
2) 44 parts, 3 parts of 0.1% H 2 PtCl 6 .6H 2 O in isopropyl alcohol was charged into the reactor, and 120
Addition reaction at ℃ for 5 hours, then add 0.1% H 2 Pt
3 parts of Cl 6 .6H 2 O in isopropyl alcohol was added, and 0.5 part of propylene was charged into the reactor.
The reaction was carried out at 0 ° C for 3 hours. The reaction product was washed 3 times with acetone, purified and dried. The silicone content of the obtained release agent was 56%.
【0011】実施例1 スチレン−ブタジエンブロックコポリマー「K−RES
IN KR05」(フィリップス石油株式会社製、MI
=8.0g/10min 、密度=1.01g/cm3 )99.5
%に対し参考例の合成物0.5%を添加し、ペレタイザ
ーによりダイス温度180℃でシート用樹脂を作製し
た。このフィルム用樹脂をTダイ押出し機よりダイス温
度200℃で押出しシートを作製した。得られたシート
の厚さは、800μmであった。このシートを用いて、
常法により圧空成形を行い、カップ(9オンス)を作製
した。得られたシート又はカップの泡立ちテスト及び滑
り性、成形加工性の測定結果を表1に示した。Example 1 Styrene-butadiene block copolymer "K-RES"
IN KR05 "(Made by Philips Oil Co., Ltd., MI
= 8.0 g / 10 min, density = 1.01 g / cm 3 ) 99.5
% Of 0.5% of the synthetic material of Reference Example was added, and a sheet resin was produced at a die temperature of 180 ° C. by a pelletizer. This resin for film was extruded from a T-die extruder at a die temperature of 200 ° C. to prepare an extruded sheet. The thickness of the obtained sheet was 800 μm. With this sheet,
A cup (9 ounces) was produced by pressure forming by a conventional method. The foaming test of the obtained sheet or cup and the measurement results of the slipperiness and the moldability are shown in Table 1.
【0012】実施例2 実施例1において、参考例の合成物の添加量を3.0%
に変えた以外は実施例1と同じ方法でシート及びカップ
を作製した。得られたシート又はカップの泡立ちテスト
及び滑り性、成形加工性の測定結果を表1に示した。Example 2 In Example 1, the addition amount of the synthetic compound of Reference Example was 3.0%.
A sheet and a cup were produced by the same method as in Example 1 except that The foaming test of the obtained sheet or cup and the measurement results of the slipperiness and the moldability are shown in Table 1.
【0013】実施例3 実施例1において、参考例の合成物の添加量を10.0
%に変えた以外は実施例1と同じ方法でシート及びカッ
プを作製した。得られたシート又はカップの泡立ちテス
ト及び滑り性、成形加工性の測定結果を表1に示した。Example 3 In Example 1, the amount of the reference compound added was 10.0.
Sheets and cups were produced in the same manner as in Example 1 except that the percentage was changed. The foaming test of the obtained sheet or cup and the measurement results of the slipperiness and the moldability are shown in Table 1.
【0014】実施例4 スチレン−ブタジエンブロックコポリマー「K−RES
IN KR05」94%と、シリコーンマスターバッチ
「シリコーンコンセントレート・BY27−003」
(東レ・ダウコーニング・シリコーン株式会社製、シリ
コーン含有量50%、GPPS50%)6%とをドライ
ブレンドして実施例1と同じ方法でシート及びカップを
作製した。得られたシート又はカップの泡立ちテスト及
び滑り性、成形加工性の測定結果を表1に示した。Example 4 Styrene-butadiene block copolymer "K-RES"
IN KR05 "94% and Silicone Masterbatch" Silicone Concentrate BY27-003 "
6% (manufactured by Toray Dow Corning Silicone Co., Ltd., silicone content 50%, GPPS 50%) was dry blended to prepare a sheet and a cup in the same manner as in Example 1. The foaming test of the obtained sheet or cup and the measurement results of the slipperiness and the moldability are shown in Table 1.
【0015】比較例1 実施例1において、参考例の合成物を添加せず、スチレ
ン−ブタジエンブロックコポリマー「K−RESIN
KR05」のみとした以外は実施例1と同じ方法でシー
ト及びカップを作製した。得られたシート又はカップの
泡立ちテスト及び滑り性、成形加工性の測定結果を表1
に示した。Comparative Example 1 In Example 1, the styrene-butadiene block copolymer "K-RESIN" was added without adding the synthetic material of Reference Example.
A sheet and a cup were produced in the same manner as in Example 1 except that only "KR05" was used. The foaming test of the obtained sheet or cup and the measurement results of slipperiness and moldability are shown in Table 1.
It was shown to.
【0016】比較例2 実施例1において、参考例の合成物の添加量を12.0
%に変えた以外は実施例1と同じ方法でシート及びカッ
プを作製した。得られたシート又はカップの泡立ちテス
ト及び滑り性、成形加工性の測定結果を表1に示した。Comparative Example 2 In Example 1, the addition amount of the synthetic material of Reference Example was 12.0.
Sheets and cups were produced in the same manner as in Example 1 except that the percentage was changed. The foaming test of the obtained sheet or cup and the measurement results of the slipperiness and the moldability are shown in Table 1.
【0017】尚、泡立ちテスト、滑り性及び成形加工性
は、以下の方法により実施した。The foaming test, slipperiness and moldability were carried out by the following methods.
【0018】泡立ちテスト:得られたカップ(9オン
ス)(1)に、図1に示す如く、液温7℃の炭酸飲料
(「コカコーラ」)(2)を190ml/6secの注入
スピードで注入し、その時の泡(3)のカップ内壁に接
した最高位置と液面との距離(L)を測定し、更にその
泡が液面より消失するまでの時間を測定した。Foaming test: The resulting cup (9 ounces) (1) was infused with a carbonated beverage (“Coca-Cola”) (2) at a liquid temperature of 7 ° C. at an injection speed of 190 ml / 6 sec as shown in FIG. The distance (L) between the liquid level and the highest position of the bubble (3) in contact with the inner wall of the cup was measured, and the time until the bubble disappeared from the liquid level was measured.
【0019】滑り性:滑り性については、得られたシー
トの表面とクラフト紙(坪量=73g/m2)にLDPE
「ミラソン16SP」(三井石油化学工業株式会社製、
MI=4.5g/10min 、密度=0.923g/cm3 )を
ミラーロールを使ってラミネートしたラミ面との静
(動)摩擦係数を測定した。測定条件は圧力1.67Kg
f/cm2 、引張り速度30mm/minとした。Lubricity: Regarding the lubricity, LDPE was applied to the surface of the obtained sheet and kraft paper (basis weight = 73 g / m 2 ).
"Mirason 16SP" (Mitsui Petrochemical Industry Co., Ltd.,
The static (dynamic) friction coefficient between the laminated surface of MI = 4.5 g / 10 min and density = 0.923 g / cm 3 ) laminated with a mirror roll was measured. The measurement condition is pressure 1.67Kg
The f / cm 2 and the pulling speed were 30 mm / min.
【0020】加工性:Tダイ押出し機を使用してシート
成形を実施する時の加工性を評価した。 ○:シートの成膜が容易である。 ×:シートの成膜が困難である。Workability: The workability when forming a sheet using a T-die extruder was evaluated. ◯: The film formation on the sheet is easy. X: It is difficult to form a film on the sheet.
【0021】[0021]
【表1】 [Table 1]
【0022】実施例5 ハイインパクトポリスチレン「IT−40」(出光石油
化学株式会社製、MI=7g/10min 、密度=1.05
g/cm3 )96%に対し、参考例の合成物4%を添加した
組成物(I)と、「IT−40」100%(II)とを、
常法により共射出成形して、アイスクリーム用容器を成
形した。ここにおいて、組成物(I)を容器の内容とな
るようにし、かつ、組成物(I)の厚さを100μm 、
(II)の厚さを200μm とした。得られた容器の内容
物易取り出し性及び射出成形加工性の評価結果を表2に
示した。Example 5 High-impact polystyrene "IT-40" (manufactured by Idemitsu Petrochemical Co., Ltd., MI = 7 g / 10 min, density = 1.05)
g / cm 3 ) 96%, composition (I) in which 4% of the synthetic product of Reference Example was added, and “IT-40” 100% (II),
A container for ice cream was molded by co-injection molding by a conventional method. Here, the composition (I) is made to have the content of the container, and the thickness of the composition (I) is 100 μm.
The thickness of (II) was set to 200 μm. Table 2 shows the evaluation results of the easy removal of the contents and the injection molding processability of the obtained container.
【0023】比較例2 実施例5において、参考例の合成物を添加せず、「IT
−40」のみを射出成形して、厚さ300μm のアイス
クリーム用容器を成形した。得られた容器の内容物易取
り出し性及び射出成形加工性の評価結果を表2に示し
た。Comparative Example 2 In Example 5, the compound of Reference Example was not added, and "IT
Only "-40" was injection-molded to form a 300 μm thick container for ice cream. Table 2 shows the evaluation results of the easy removal of the contents and the injection molding processability of the obtained container.
【0024】尚、内容物易取り出し性及び射出成形加工
性については、以下の方法により評価した。The ease of taking out the contents and the injection molding processability were evaluated by the following methods.
【0025】内容物易取り出し性:得られた容器に、深
さの8%までに水を張り冷凍室で凍らせた後、冷凍室よ
り取り出し、20℃の恒温室に5分間放置する。その
後、容器を倒立させ、中の氷が完全に容器から滑り落ち
るまでの時間を測定した。Ease of taking out contents: The obtained container is filled with water to a depth of 8% and frozen in a freezing room, then taken out from the freezing room and left in a thermostatic chamber at 20 ° C. for 5 minutes. Then, the container was turned upside down, and the time until the ice in the container completely slipped down from the container was measured.
【0026】射出成形加工性:射出成形時の加工性を評
価した。 ○:容器成形が容易で、偏肉がない。 ×:容器成形が困難で、偏肉がある。Injection molding processability: The processability during injection molding was evaluated. ◯: Container formation is easy and there is no uneven thickness. X: Molding of the container is difficult and uneven thickness is present.
【0027】[0027]
【表2】 [Table 2]
【0028】[0028]
【発明の効果】叙上の通り、本発明の樹脂組成物及びシ
ートは成形加工性、滑り性及び発泡抑制効果に優れてい
るので、飲料用、特に炭酸飲料用カップ、アイスクリー
ム、プリン等用の各種容器として好適である。As described above, since the resin composition and sheet of the present invention are excellent in molding processability, slipperiness and foaming suppressing effect, they are used for beverages, especially carbonated beverage cups, ice creams, puddings, etc. It is suitable as various containers.
【図面の簡単な説明】[Brief description of drawings]
【図1】泡立ちテストの方法を示す概略図である。FIG. 1 is a schematic view showing a method of a foaming test.
1 カップ 2 炭酸飲料 3 泡 1 cup 2 carbonated drinks 3 bubbles
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 FI 技術表示箇所 C08L 83:10) 8319−4J ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 5 Identification code Internal reference number FI technical display area C08L 83:10) 8319-4J
Claims (6)
を0.1〜10.0重量%含有させてなる、成形加工
性、滑り性及び炭酸飲料の発泡抑制効果に優れた樹脂組
成物。1. A resin composition comprising a polystyrene resin containing a silicone compound in an amount of 0.1 to 10.0% by weight, which is excellent in moldability, slipperiness, and the effect of suppressing foaming of carbonated beverages.
水素基を有する有機珪素化合物と、該水素基と反応する
二重結合を少なくとも1個有する炭素数18以上の炭化
水素化合物とを反応させてなる櫛型グラフトポリマーで
ある請求項1記載の組成物。2. A silicone compound is obtained by reacting an organosilicon compound having at least one hydrogen group with a hydrocarbon compound having at least one double bond that reacts with the hydrogen group and having 18 or more carbon atoms. The composition according to claim 1, which is a comb-type graft polymer.
物からなるシート。3. A sheet made of the polystyrene resin composition according to claim 1.
系樹脂からなる基材上に積層してなるシート。4. A sheet obtained by laminating the sheet according to claim 3 on a base material made of polystyrene resin.
物を成形してなる容器類。5. Containers formed by molding the polystyrene resin composition according to claim 1.
なる容器類。6. A container formed by molding the sheet according to claim 3 or 4.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP33400391A JPH05140392A (en) | 1991-11-22 | 1991-11-22 | Polystyrenic resin composition, sheet and containers composed of the same |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP33400391A JPH05140392A (en) | 1991-11-22 | 1991-11-22 | Polystyrenic resin composition, sheet and containers composed of the same |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH05140392A true JPH05140392A (en) | 1993-06-08 |
Family
ID=18272412
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP33400391A Withdrawn JPH05140392A (en) | 1991-11-22 | 1991-11-22 | Polystyrenic resin composition, sheet and containers composed of the same |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH05140392A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20120100266A1 (en) * | 2010-10-20 | 2012-04-26 | Pepsico., Inc. | Control of bubble size in a carbonated liquid |
JP2013544300A (en) * | 2010-11-11 | 2013-12-12 | ザ プロクター アンド ギャンブル カンパニー | Nacreous container |
-
1991
- 1991-11-22 JP JP33400391A patent/JPH05140392A/en not_active Withdrawn
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20120100266A1 (en) * | 2010-10-20 | 2012-04-26 | Pepsico., Inc. | Control of bubble size in a carbonated liquid |
US9327462B2 (en) | 2010-10-20 | 2016-05-03 | Pepsico, Inc. | Control of bubble size in a carbonated liquid |
US10501259B2 (en) | 2010-10-20 | 2019-12-10 | Pepsico, Inc. | Control of bubble size in a carbonated liquid |
JP2013544300A (en) * | 2010-11-11 | 2013-12-12 | ザ プロクター アンド ギャンブル カンパニー | Nacreous container |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 19990204 |