JP3543466B2 - Biaxially stretched blow molded article and method for producing the same - Google Patents
Biaxially stretched blow molded article and method for producing the same Download PDFInfo
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Description
【０００１】
【発明の属する技術分野】
本発明は、射出延伸ブロー成形に適したポリエチレン系樹脂からなる二軸延伸ブロー成形品およびその製造方法に関するものである。さらに詳しくは、衝撃強度、剛性等の諸物性はもとより、表面光沢、表面平滑性にも優れる二軸延伸成形品を射出延伸ブロー成形するのに適したポリエチレン系樹脂からなる二軸延伸ブロー成形品およびその製造方法に関するものである。
【０００２】
【従来の技術】
従来二軸延伸ボトル等の二軸延伸成形品は、塩化ビニリデン、ポリカーボネート、ポリエチレンテレフタレート等を使用して製造されている。ポリエチレンは二軸延伸しない通常のボトルには多用されているものの、二軸延伸成形品については、従来から種々検討はなされてきたが、実用化が困難であった。
【０００３】
最近は金型の設計技術や成形技術等の進歩により、ポリエチレンの射出延伸ブロー成形に要求される有底パリソンの高温離型が可能となり、ポリエチレンの射出延伸ブロー成形も注目されるようになった。
【０００４】
ところで二軸延伸しない通常の中空成形用グレードの高密度ポリエチレンは、中空成形品を成形する場合、溶融パリソンが自重で垂れ下る現象（ドローダウン）による偏肉や、メルトフラクチャーによる肌荒れを生じ易いので、従来これを防止するためにＭＦＲ ２．０ｇ／１０ｍｉｎ以下で、かつ分子量分布の広い樹脂が用いられてきた。
しかしながら、このような樹脂を使用した場合、成形品の表面光沢や表面平滑性が乏しく、商品としては不十分の感があった。さらに射出延伸ブロー成形用のポリエチレン樹脂としても最適な樹脂は見出されてはおらず、従来の通常の中空成形用のグレードが使用されるため、二軸延伸ボトルに対する世の中のニーズである表面光沢や表面平滑性に優れる射出延伸ブロー成形品は得られていなかった。
【０００５】
【発明が解決しようとする課題】
本発明は、かかる事情に鑑み、衝撃強度、剛性等のポリエチレン樹脂に特有の諸特性のほかに表面光沢、表面平滑性にも優れる二軸延伸成形品を成形するのに適した射出延伸ブロー成形用ポリエチレン系樹脂からなる二軸延伸ブロー成形品およびその製造方法を提供することを目的とする。
【０００６】
【課題を解決するための手段】
本発明は、次の二軸延伸ブロー成形品およびその製造方法である。
（１） 密度０．９４０〜０．９６８ｇ／ｃｍ3、ＭＦＲ ０．３〜１０ｇ／１０ｍｉｎ、流動比１５以上３０未満であるエチレン単独重合体、エチレン・α−オレフィン共重合体またはこれらのブレンド物を含むポリエチレン系樹脂を射出延伸ブロー成形してなる二軸延伸ブロー成形品。
（２） ポリエチレン系樹脂が密度０．９４０〜０．９６８ｇ／ｃｍ3のエチレン単独重合体および／またはエチレン・α−オレフィン共重合体を含む上記（１）記載の二軸延伸ブロー成形品。
（３） ポリエチレン系樹脂が密度０．９２５ｇ／ｃｍ3以下の高圧法ポリエチレンを５〜２５重量％含む上記（１）または（２）記載の二軸延伸ブロー成形品。
（４） 密度０．９４０〜０．９６８ｇ／ｃｍ 3 、ＭＦＲ ０．３〜１０ｇ／１０ｍｉｎ、流動比１５以上３０未満であるエチレン単独重合体、エチレン・α−オレフィン共重合体またはこれらのブレンド物を含むポリエチレン系樹脂を射出延伸ブロー成形する二軸延伸ブロー成形品の製造方法。
【０００７】
本発明において、ＭＦＲはＡＳＴＭ Ｄ１２３８に準拠し、温度１９０℃、荷重２．１６ｋｇで測定した値である。また流動比はＡＳＴＭ Ｄ１２３８に準拠し、温度１９０℃において、荷重１１２０４ｇの時のＭＦＲと、荷重１１２０ｇの時のＭＦＲとの比である。
【０００８】
本発明で使用されるポリエチレン系樹脂は、エチレンをモノマーの主体とする重合体であり、エチレン単独重合体、エチレン・α−オレフィン共重合体、エチレン単独重合体および／またはエチレン・α−オレフィン共重合体のブレンド物などが挙げられる。
【０００９】
エチレン単独重合体としては、チーグラー・ナッタ触媒による低圧法、フイリップス法等の中圧法等により得られる密度０．９４０〜０．９６８ｇ／ｃｍ3の高密度ポリエチレンが使用できる。ブレンド物として用いる場合は、ブレンド物の密度等が前記範囲に入る限り、密度０．９２５ｇ／ｃｍ 3 以下の高圧法ポリエチレンを一成分として配合することができる。
【００１０】
本発明で用いるエチレン・α−オレフィン共重合体は、エチレンと炭素数３〜２０、好ましくは３〜１２のα−オレフィンとの共重合体であり、α−オレフィンとしては、プロピレン、ブテン−１、ペンテン−１、ヘキセン−１、４−メチルペンテン−１、４−メチルヘキセン−１、４，４−ジメチルペンテン−１、ヘプテン−１、オクテン−１、ノネン−１、デセン−１などがあげられ、これらは１種単独で、または２種以上を組合わせて共重合させることができる。
エチレン・α−オレフィン共重合体中のα−オレフィン含有量は０．１〜２０重量％、好ましくは０．１〜１０重量％であり、密度は０．９４０〜０．９６８ｇ／ｃｍ 3 のものが好ましい。
【００１１】
本発明の射出延伸ブロー成形用ポリエチレン系樹脂は、密度が０．９４０〜０．９６８ｇ／ｃｍ3、好ましくは０．９５０〜０．９６０ｇ／ｃｍ3、ＭＦＲが０．３〜１０ｇ／１０ｍｉｎ、好ましくは０．５〜３ｇ／１０ｍｉｎ、流動比が１５以上３０未満、好ましくは１５〜２９、より好ましくは２０〜２９である。これらの特性値は、１種類の樹脂を射出延伸ブロー成形用として用いる場合は、使用する樹脂単独で満足する値であるが、複数種の樹脂をブレンド物として使用する場合は、ブレンド物として上記特性値を満足すればよく、個々の成分は上記値の範囲外のものでもよい。
【００１２】
このような範囲外の樹脂として、例えば前述のように、密度０．９２５ｇ／ｃｍ3以下の高圧法ポリエチレンを用いることができる。この高圧法ポリエチレンは、エチレンの単独重合体またはエチレンと炭素数３〜２０のα−オレフィンとの共重合体であり、１０００〜２０００気圧、２００〜３００℃でラジカル重合して得られ、密度は０．９２５ｇ／ｃｍ3以下であって、高圧法低密度ポリエチレンとも呼ばれるものである。上記の共重合体の場合のα−オレフィンの含有量は通常０．１〜２０重量％、好ましくは０．１〜１０重量％とされる。
【００１３】
本発明では射出延伸ブロー成形用樹脂として用いられる単体樹脂またはブレンド物が前記密度を有し、かつＭＦＲが０．３〜１０ｇ／１０ｍｉｎであることにより、ドローダウンが生じなくなり、かつサメ肌的にならず、成形品の表面光沢、表面平滑性が改善される。
【００１４】
また流動比が１５以上であることにより、有底パリソンの表面にフローマークが発生せず、成形後の成形品の表面状態が良好となり、流動比が３０未満であることにより成形品の表面光沢が低下せず、表面光沢、表面平滑性に優れた成形品が得られる。
【００１５】
本発明において、エチレン単独重合体とエチレン・α−オレフィン共重合体の組成物を用いる場合、前記特性値を満足する限り、両者の配合比は任意であるが、重量比で２０／８０〜８０／２０とするのが好ましい。エチレン単独重合体同士、またはエチレン・α−オレフィン共重合体同士の組成物の場合の配合比は、前記特性値を満足する限り任意である。
【００１６】
特性値が前記範囲外の成分の配合割合は樹脂成分全体の２５重量％以下、好ましくは１０重量％以下が望ましい。密度０．９２５ｇ／ｃｍ3以下の高圧法低密度ポリエチレンを配合する場合は、その配合割合は樹脂成分全体の５〜２５重量％とするのが好ましく、これにより表面光沢および表面平滑性が改善される。
【００１７】
本発明のポリエチレン系樹脂には、本発明の目的を損わない範囲で、その他の樹脂、耐熱安定剤、耐候安定剤、改質剤、滑剤、着色剤、充填剤などを配合することができる。
【００１８】
本発明のポリエチレン系樹脂において、ブレンド物を用いる場合のように混合が必要な場合は、各成分をバンバリーミキサー、ヘンシェルミキサー、押出機等によるドライブレンド、および／またはメルトブレンド等により混合することができる。
【００１９】
このようにして得られる射出延伸ブロー成形用ポリエチレン系樹脂は、射出延伸ブロー成形に適しており、射出延伸ブロー成形することにより、衝撃強度、剛性等のポリエチレンの諸特性のほか、表面光沢、表面平滑性に優れるボトルその他の中空成形品などの二軸延伸ブロー成形品を製造することができる。この場合、本発明の樹脂を用いて有底パリソンを射出成形し、この有底パリソンを高温離型してそのまま二軸延伸ブロー成形し、あるいは中間で有底パリソンを温調して二軸延伸ブロー成形することができるが、いずれの場合もドローダウンやメルトフラクチャーを生じることはない。そしてフローマークやサメ肌のような表面異常がなく、表面光沢、表面平滑性に優れた中空成形品が得られる。
【００２０】
【発明の効果】
本発明によれば、特定の密度、ＭＦＲ、流動比などを有するポリエチレン系樹脂を射出延伸ブロー成形することにより、成形の際にドローダウンやメルトフラクチャーがなく、衝撃強度、剛性等の諸特性はもとより、表面光沢や表面平滑性にも優れている二軸延伸ブロー成形品を得ることができる。
【００２１】
【発明の実施の形態】
次に、実施例および比較例により本発明をさらに詳細に説明するが、本発明はこれらの例によってなんら限定されるものではない。
【００２２】
実施例１〜４および比較例１〜３
表１，２に示す原料樹脂について、（株）日精ＡＳＢ製射出延伸ブロー成形機（ＡＳＢ５０ＴＨ）を用い、予備中空成形体を縦１．８倍、横１．５倍に延伸して、目付４３ｇ、口径５０ｍｍ、内容積５００ｍｌの円筒状ボトルを成形した。各例のボトルについて側壁外面の表面光沢、表面平滑性を測定した。その結果を表２に示す。
【００２３】
なお各例における特性値の測定方法は次の通りである。
１）ＭＦＲ（メルトフローレート）
ＡＳＴＭ Ｄ１２３８に準拠（１９０℃，荷重２．１６ｋｇ）
２）流動比
ＡＳＴＭ Ｄ１２３８に準拠（１９０℃）
（荷重１１２０４ｇにおけるＭＦＲ／荷重１１２０ｇにおけるＭＦＲ）
３）密度
ＡＳＴＭ Ｄ１５０５に準拠
４）表面光沢
ＡＳＴＭ Ｄ５２３に準拠
日本電色工業（株）製グロスメーター使用、入射角４５°
５）表面平滑性（目視による）
○ 表面に平滑感があり、光沢も認められる。
△ 表面にメルトフラクチャー気味の微細なシワがある。
× 表面が全体に凹凸があって肌荒れを呈し光沢もない。
【００２４】
【表１】
【表２】
表１および表２の結果より、密度、ＭＦＲおよび流動比が前記範囲内の各実施例の成形品は表面光沢および表面平滑性に優れるが、各特性、特に流動比が前記範囲外の各比較例の成形品は表面光沢および表面平滑性に劣ることがわかる。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a biaxially stretched blow-molded product made of a polyethylene resin suitable for injection stretch blow-molding and a method for producing the same. More specifically, a biaxial stretch blow molded product made of a polyethylene resin suitable for injection stretch blow molding of a biaxial stretch molded product excellent in surface gloss and surface smoothness as well as various properties such as impact strength and rigidity. And its manufacturing method .
[0002]
[Prior art]
Conventionally, biaxially stretched molded products such as biaxially stretched bottles have been manufactured using vinylidene chloride, polycarbonate, polyethylene terephthalate and the like. Although polyethylene is often used for ordinary bottles which are not biaxially stretched, various studies have been made on biaxially stretched molded products, but practical use has been difficult.
[0003]
Recent advances in mold design and molding techniques have made possible the high-temperature release of bottomed parisons required for polyethylene injection stretch blow molding, and polyethylene injection stretch blow molding has also attracted attention. .
[0004]
By the way, high-density polyethylene of ordinary hollow molding grade which is not biaxially stretched tends to cause uneven wall thickness due to a phenomenon (drawdown) in which a molten parison hangs down by its own weight and rough surface due to melt fracture when molding a hollow molded article. Conventionally, to prevent this, a resin having an MFR of 2.0 g / 10 min or less and a wide molecular weight distribution has been used.
However, when such a resin is used, the surface gloss and surface smoothness of the molded product are poor, and there is an unsatisfactory feeling as a commercial product. Furthermore, no optimal resin has been found as a polyethylene resin for injection stretch blow molding.Since conventional grades for ordinary hollow molding are used, surface gloss and gloss, which are public needs for biaxially stretched bottles, are required. An injection-stretch blow-molded article having excellent surface smoothness has not been obtained.
[0005]
[Problems to be solved by the invention]
In view of such circumstances, the present invention is directed to injection stretch blow molding suitable for molding biaxially stretched molded products having excellent surface gloss and surface smoothness in addition to various characteristics unique to polyethylene resins such as impact strength and rigidity. It is an object of the present invention to provide a biaxially stretch blow-molded article made of a polyethylene resin for use and a method for producing the same.
[0006]
[Means for Solving the Problems]
The present invention relates to the following biaxially stretch blow-molded article and a method for producing the same.
(1) Ethylene homopolymer, ethylene / α-olefin copolymer or a blend thereof having a density of 0.940 to 0.968 g / cm 3 , an MFR of 0.3 to 10 g / 10 min, and a flow ratio of 15 or more and less than 30 A biaxially stretched blow-molded product obtained by injection-stretching blow-molding of a polyethylene resin containing.
(2) The biaxially stretch blow-molded article according to the above (1), wherein the polyethylene resin contains an ethylene homopolymer and / or an ethylene / α-olefin copolymer having a density of 0.940 to 0.968 g / cm 3 .
(3) The biaxially stretched blow-molded article according to the above (1) or (2), wherein the polyethylene resin contains 5 to 25% by weight of a high pressure polyethylene having a density of 0.925 g / cm 3 or less.
(4) Density 0.940 to 0.968 g / cm 3 , MFR Biaxial stretch blow molding for injection stretching blow molding of a polyethylene-based resin containing an ethylene homopolymer, an ethylene / α-olefin copolymer or a blend thereof having a flow rate of 0.3 to 10 g / 10 min and a flow ratio of 15 to less than 30. Product manufacturing method .
[0007]
In the present invention, the MFR is a value measured at a temperature of 190 ° C. and a load of 2.16 kg in accordance with ASTM D1238. The flow ratio is a ratio of the MFR under a load of 11204 g and the MFR under a load of 1120 g at a temperature of 190 ° C. in accordance with ASTM D1238.
[0008]
The polyethylene resin used in the present invention is a polymer containing ethylene as a main monomer, and is composed of an ethylene homopolymer, an ethylene / α-olefin copolymer, an ethylene homopolymer and / or an ethylene / α-olefin copolymer. Blends of polymers and the like can be mentioned.
[0009]
As the ethylene homopolymer, high-density polyethylene having a density of 0.940 to 0.968 g / cm 3 obtained by a low-pressure method using a Ziegler-Natta catalyst, a medium-pressure method such as a Phillips method, or the like can be used. When used as a blend, high pressure polyethylene having a density of 0.925 g / cm 3 or less can be blended as one component as long as the density of the blend falls within the above range.
[0010]
The ethylene / α-olefin copolymer used in the present invention is a copolymer of ethylene and an α-olefin having 3 to 20 carbon atoms, preferably 3 to 12 carbon atoms. Examples of the α-olefin include propylene and butene-1. Pentene-1, hexene-1, 4-methylpentene-1, 4-methylhexene-1, 4,4-dimethylpentene-1, heptene-1, octene-1, nonene-1, decene-1 and the like. These can be copolymerized alone or in combination of two or more.
The α-olefin content in the ethylene / α-olefin copolymer is 0.1 to 20% by weight, preferably 0.1 to 10% by weight, and the density is 0.940 to 0.968 g / cm 3 . Are preferred.
[0011]
The polyethylene resin for injection stretch blow molding of the present invention has a density of 0.940 to 0.968 g / cm 3 , preferably 0.950 to 0.960 g / cm 3 , and an MFR of 0.3 to 10 g / 10 min, preferably Is 0.5 to 3 g / 10 min, and the flow ratio is 15 or more and less than 30, preferably 15 to 29, more preferably 20 to 29. These characteristic values are values that are satisfied by the resin used alone when one type of resin is used for injection stretch blow molding, but when a plurality of types of resins are used as a blend, It suffices to satisfy the characteristic values, and the individual components may be outside the above-mentioned range.
[0012]
As the resin out of such a range, for example, as described above, high-pressure polyethylene having a density of 0.925 g / cm 3 or less can be used. This high-pressure polyethylene is a homopolymer of ethylene or a copolymer of ethylene and an α-olefin having 3 to 20 carbon atoms, and is obtained by radical polymerization at 1000 to 2000 atm and 200 to 300 ° C. It is 0.925 g / cm 3 or less and is also called a high-pressure low-density polyethylene. The content of the α-olefin in the case of the above copolymer is usually 0.1 to 20% by weight, preferably 0.1 to 10% by weight.
[0013]
In the present invention, since the single resin or the blend used as the resin for injection stretch blow molding has the above density and the MFR is 0.3 to 10 g / 10 min, drawdown does not occur and shark skin is reduced. In addition, the surface gloss and surface smoothness of the molded product are improved.
[0014]
When the flow ratio is 15 or more, no flow mark is generated on the surface of the bottomed parison, and the surface condition of the molded product after molding becomes good. When the flow ratio is less than 30, the surface gloss of the molded product is improved. , And a molded article excellent in surface gloss and surface smoothness can be obtained.
[0015]
In the present invention, when a composition of an ethylene homopolymer and an ethylene / α-olefin copolymer is used, as long as the above characteristic values are satisfied, the mixing ratio of both is arbitrary, but the weight ratio is 20/80 to 80/80. / 20 is preferable. The composition ratio of the composition of ethylene homopolymers or of ethylene / α-olefin copolymers is arbitrary as long as the above characteristic values are satisfied.
[0016]
The compounding ratio of the component whose characteristic value is out of the above range is desirably 25% by weight or less, preferably 10% by weight or less of the whole resin component. When a high-pressure low-density polyethylene having a density of 0.925 g / cm 3 or less is blended, the blending ratio is preferably 5 to 25% by weight of the entire resin component, whereby the surface gloss and surface smoothness are improved. You.
[0017]
In the polyethylene resin of the present invention, other resins, heat stabilizers, weather stabilizers, modifiers, lubricants, coloring agents, fillers, and the like can be blended within a range that does not impair the purpose of the present invention. .
[0018]
In the polyethylene resin of the present invention, when mixing is required as in the case of using a blend, each component may be mixed by a dry blend using a Banbury mixer, a Henschel mixer, an extruder, and / or a melt blend. it can.
[0019]
The polyethylene resin for injection stretch blow molding obtained in this way is suitable for injection stretch blow molding . Injection stretch blow molding provides various properties of polyethylene such as impact strength and rigidity, as well as surface gloss and surface Biaxially stretched blow molded articles such as bottles and other hollow molded articles having excellent smoothness can be produced. In this case, a bottomed parison is injection-molded using the resin of the present invention, and the bottomed parison is released at a high temperature and biaxially stretch blow-molded as it is, or biaxially stretched by controlling the temperature of the bottomed parison in the middle. Blow molding can be performed, but no drawdown or melt fracture occurs in any case. Then, a hollow molded article having no surface abnormality such as flow mark or shark skin and excellent in surface gloss and surface smoothness can be obtained.
[0020]
【The invention's effect】
According to the present invention , by injection-stretch blow molding of a polyethylene resin having a specific density, MFR, flow ratio, etc., there is no drawdown or melt fracture during molding, and various properties such as impact strength and rigidity are obtained. Naturally, it is possible to obtain a biaxially stretched blow-molded article having excellent surface gloss and surface smoothness.
[0021]
BEST MODE FOR CARRYING OUT THE INVENTION
Next, the present invention will be described in more detail with reference to Examples and Comparative Examples, but the present invention is not limited to these Examples.
[0022]
Examples 1-4 and Comparative Examples 1-3
For the raw material resins shown in Tables 1 and 2, the preliminary hollow molded body was stretched 1.8 times vertically and 1.5 times horizontally using an injection stretch blow molding machine (ASB50TH) manufactured by Nissei ASB Co., Ltd. to obtain a basis weight of 43 g. A cylindrical bottle having a diameter of 50 mm and an internal volume of 500 ml was formed. The surface gloss and surface smoothness of the outer surface of the side wall of each bottle were measured. Table 2 shows the results.
[0023]
The method of measuring the characteristic value in each example is as follows.
1) MFR (melt flow rate)
Conforms to ASTM D1238 (190 ° C, load 2.16kg)
2) Flow ratio Conforms to ASTM D1238 (190 ° C)
(MFR at 11204 g load / MFR at 1120 g load)
3) Density conforms to ASTM D1505 4) Surface gloss conforms to ASTM D523 Using a gloss meter manufactured by Nippon Denshoku Industries Co., Ltd., incident angle of 45 °
5) Surface smoothness (visual)
表面 The surface is smooth and glossy.
△ There are fine wrinkles with melt fracture on the surface.
C: The surface is entirely uneven and rough, without gloss.
[0024]
[Table 1]
[Table 2]
From the results shown in Tables 1 and 2, the molded articles of Examples in which the density, the MFR and the flow ratio were within the above ranges were excellent in surface gloss and surface smoothness, but each characteristic, especially each flow ratio outside the above range was compared. It can be seen that the molded articles of the examples are inferior in surface gloss and surface smoothness.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP00859396A JP3543466B2 (en) | 1996-01-22 | 1996-01-22 | Biaxially stretched blow molded article and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP00859396A JP3543466B2 (en) | 1996-01-22 | 1996-01-22 | Biaxially stretched blow molded article and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09194534A JPH09194534A (en) | 1997-07-29 |
| JP3543466B2 true JP3543466B2 (en) | 2004-07-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP00859396A Expired - Fee Related JP3543466B2 (en) | 1996-01-22 | 1996-01-22 | Biaxially stretched blow molded article and method for producing the same |
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| Country | Link |
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| JP (1) | JP3543466B2 (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2366722A1 (en) | 2010-03-19 | 2011-09-21 | Total Petrochemicals Research Feluy | Bimodal polyethylene for injection stretch blow moulding applications. |
| EP2464675B1 (en) | 2009-11-10 | 2016-08-17 | Total Research & Technology Feluy | Use of a bimodal polyethylene for injection stretch blow moulding applications |
| CN102858812A (en) | 2010-01-28 | 2013-01-02 | 道达尔研究技术弗吕公司 | Injection Stretch Blow Moulding Containers Prepared With Polyethylene |
| EP2351781A1 (en) | 2010-01-28 | 2011-08-03 | Total Petrochemicals Research Feluy | Injection stretch blow moulding containers prepared with polyethylene |
| KR101530799B1 (en) | 2011-01-11 | 2015-06-22 | 토탈 리서치 앤드 테크놀로지 펠루이 | Injection stretch blow moulded articles |
| JP5904442B2 (en) * | 2012-05-31 | 2016-04-13 | 株式会社吉野工業所 | Molding method of high density polyethylene resin container |
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1996
- 1996-01-22 JP JP00859396A patent/JP3543466B2/en not_active Expired - Fee Related
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| JPH09194534A (en) | 1997-07-29 |
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