JPH069860A - Polyester resin composition - Google Patents
Polyester resin compositionInfo
- Publication number
- JPH069860A JPH069860A JP26636991A JP26636991A JPH069860A JP H069860 A JPH069860 A JP H069860A JP 26636991 A JP26636991 A JP 26636991A JP 26636991 A JP26636991 A JP 26636991A JP H069860 A JPH069860 A JP H069860A
- Authority
- JP
- Japan
- Prior art keywords
- resin composition
- polyester resin
- polyethylene terephthalate
- melt viscosity
- melt
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、耐吸湿特性、溶融安定
性、耐熱性、機械的特性等に優れ、低比重であるポリエ
ステル樹脂組成物、特にポリエチレンテレフタレートを
主成分とするポリエステル樹脂に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polyester resin composition which has excellent moisture absorption resistance, melt stability, heat resistance, mechanical properties and the like and has a low specific gravity, and particularly to a polyester resin containing polyethylene terephthalate as a main component.
【０００２】[0002]
【従来の技術】ポリエチレンテレフタレートを主成分と
するポリエステル樹脂組成物は、機械的特性、電気的特
性、耐薬品特性を有する樹脂として知られている。2. Description of the Related Art A polyester resin composition containing polyethylene terephthalate as a main component is known as a resin having mechanical properties, electrical properties and chemical resistance.
【０００３】しかしながら、従来のポリエチレンテレフ
タレートを主成分とするポリエステル樹脂組成物は、溶
融安定性が低く耐吸湿特性が不充分であるという問題を
有している。本明細書において溶融安定性が高いとは、
後に詳述するように、キャピログラフで測定した溶融粘
度について、該キャピログラフでの滞留時間が長い場合
の溶融粘度が滞留時間が短い場合の溶融粘度に比べて充
分に高いことをいう。溶融安定性が低いと、樹脂組成物
の成形の際いわゆるばりが生じ易く成形品の外観が損な
われるばかりでなく、成形品の寸法および重量にばらつ
きが生じる原因にもなる。次に、耐吸湿特性が優れると
は、水分率の高い（例えば水分率０．０５％）ペレット
を使用して成形された成形品の強度保持率が、低水分率
（例えば０．０２％以下）のペレットにより成形された
成形品の強度に対して充分に高く、かつ、高水分率のペ
レットを使用した場合でも溶融粘度が高いことをいう。
ポリエチレンテレフタレートは吸湿した状態での成形に
難点があるので、ポリエチレンテレフタレートを主成分
とするポリエステル樹脂組成物において、耐吸湿特性の
向上は重要な課題である。However, the conventional polyester resin composition containing polyethylene terephthalate as a main component has a problem that the melt stability is low and the moisture absorption resistance is insufficient. In the present specification, high melt stability means that
As will be described later in detail, with respect to the melt viscosity measured by a capillograph, the melt viscosity when the residence time is long in the capillograph is sufficiently higher than the melt viscosity when the residence time is short. When the melt stability is low, so-called burrs are liable to occur during molding of the resin composition, which not only impairs the appearance of the molded product but also causes variations in the size and weight of the molded product. Next, that the moisture absorption resistance is excellent means that the strength retention of the molded article formed by using the pellets having a high water content (for example, water content of 0.05%) has a low water content (for example, 0.02% or less). It means that the strength of the molded product molded from the pellets of 1) is sufficiently high, and that the melt viscosity is high even when the high moisture content pellets are used.
Since polyethylene terephthalate has a difficulty in molding in a moisture-absorbed state, it is an important issue to improve the moisture absorption resistance in a polyester resin composition containing polyethylene terephthalate as a main component.
【０００４】[0004]
【発明が解決しようとする課題】本発明は、優れた機械
的特性を備えると共に、耐吸湿特性および溶融安定性を
著しく改良した低温金型成形が可能である、ポリエチレ
ンテレフタレートを主成分とするポリエステル樹脂組成
物を提供することを目的とする。DISCLOSURE OF THE INVENTION The present invention provides a polyester containing polyethylene terephthalate as a main component, which has excellent mechanical properties and is capable of low temperature mold molding with significantly improved moisture absorption resistance and melt stability. An object is to provide a resin composition.
【０００５】[0005]
【課題を解決するための手段】本発明者は前記課題を解
決すべく鋭意研究を続けた結果、ポリエチレンテレフタ
レートに一定量のポリオレフィンを添加することによっ
て、ポリエチレンテレフタレートの前記本来の性質を損
なうことなく、耐吸湿特性、溶融安定性が著しく改良さ
れることを見出して本発明を完成することに至った。す
なわち、本発明は、本質的にポリエチレンテレフタレー
トおよびポリオレフィンからなり、該ポリエチレンテレ
フタレートとポリオレフィンの比を９５：５〜８０：２
０とすることを特徴とするポリエステル樹脂組成物であ
る。Means for Solving the Problems The inventors of the present invention have conducted extensive studies to solve the above problems, and as a result, by adding a certain amount of polyolefin to polyethylene terephthalate, the original properties of polyethylene terephthalate are not impaired. The inventors have completed the present invention by finding that the moisture absorption resistance and the melt stability are remarkably improved. That is, the present invention consists essentially of polyethylene terephthalate and a polyolefin, and the ratio of the polyethylene terephthalate to the polyolefin is 95: 5 to 80: 2.
It is a polyester resin composition characterized by being 0.
【０００６】本発明に用いるポリエチレンテレフタレー
トは、少なくとも約０．４の固有粘度を有するものを用
いるのが好ましく、約１．２までの固有粘度を有するも
のを用いるのが好ましい。The polyethylene terephthalate used in the present invention preferably has an intrinsic viscosity of at least about 0.4, and preferably has an intrinsic viscosity of up to about 1.2.
【０００７】本発明でいうポリオレフィンには、ポリエ
チレン、ポリプロピレン、および他のポリオレフィン：
グリシジルメタアクリレートで変性したポリオレフィン
及びオレフィンとビニル化合物及び／またはアクリル化
合物との共重合体又はグラフト重合体が含まれるが、特
にポリプロピレンを用いるのが適当である。ポリプロピ
レンを用いる場合には、メルトインデックスが（ＡＳＴ
ＭＤ１２３８）が０．１〜５０ｇ／１０分、特に０．５
〜２０ｇ／分のものを用いるのが好ましい。ポリオレフ
ィンの配合量は、得られる成形品の物性を考慮して定め
られるが、ポリエチレンテレフタレート対ポリオレフィ
ンの比を９５：５〜８０：２０の範囲とする。ポリオレ
フィンの配合量は、本組成物全体に対しては１〜３０重
量％が好ましく、２〜１５重量％であることがより好ま
しい。２重量％以下ではポリオレフィンによる充分な耐
吸湿特性と溶融安定性を得にくく、１５重量％以上では
得られる成形品の耐熱性及び機械的特性の低下の原因と
なりやすい。The polyolefins referred to in this invention include polyethylene, polypropylene, and other polyolefins:
Polyolefins modified with glycidyl methacrylate and copolymers or graft polymers of olefins with vinyl compounds and / or acrylic compounds are included, with polypropylene being particularly suitable. If polypropylene is used, the melt index (AST
MD1238) is 0.1 to 50 g / 10 minutes, especially 0.5
It is preferable to use one having a content of up to 20 g / min. The blending amount of polyolefin is determined in consideration of the physical properties of the obtained molded product, and the ratio of polyethylene terephthalate to polyolefin is set to 95: 5 to 80:20. The polyolefin content is preferably 1 to 30% by weight, more preferably 2 to 15% by weight, based on the entire composition. If it is 2% by weight or less, it is difficult to obtain sufficient moisture absorption resistance and melt stability due to the polyolefin, and if it is 15% by weight or more, heat resistance and mechanical properties of the obtained molded product tend to be deteriorated.
【０００８】上記の各成分を配合した組成物にさらにガ
ラス繊維、マイカ、ウィスカーなどの無機強化物質また
は難燃剤を、該組成物１００重量部に対して５〜１５０
部配合することができる。これら無機強化物質等を配合
した組成物から得られる成形品は、溶融安定性、耐吸湿
特性に優れるほか、耐熱性、剛性、機械的強度にも優れ
たものとなる。Inorganic reinforcing substances such as glass fiber, mica and whiskers or flame retardants are further added to the composition containing the above components in an amount of 5 to 150 parts by weight per 100 parts by weight of the composition.
Parts can be compounded. A molded article obtained from a composition containing these inorganic reinforcing substances and the like is excellent not only in melt stability and moisture absorption resistance, but also in heat resistance, rigidity and mechanical strength.
【０００９】さらに、本発明のポリエステル樹脂組成物
は、低温金型成形性を向上させるため、核剤を含有する
ことが好ましい。核剤としては、ナトリウム化合物およ
び／またはカリウム化合物を用いることができる。これ
らナトリウム化合物およびカリウム化合物の一部または
全部をタルクで置き換えても良い。この他各種の核剤も
使用することができる。また、本発明の主成分であるポ
リエステルの一部または全部を、末端がナトリウムまた
はカリウム化したポリエチレンフタレートで置き換えて
も良い。この末端処理したポリエチレンフタレートは、
米国特許第４，４２５，４７０号明細書に記載されたも
のであり、同明細書に記載の方法で製造することができ
る。この末端がナトリウムまたはカリウム化したポリエ
チレンフタレートを使用すれば、核剤を別に添加しなく
てもよい場合もある。Further, the polyester resin composition of the present invention preferably contains a nucleating agent in order to improve the low temperature moldability. As the nucleating agent, a sodium compound and / or a potassium compound can be used. Part or all of these sodium compounds and potassium compounds may be replaced with talc. Various nucleating agents can also be used. Further, a part or all of the polyester, which is the main component of the present invention, may be replaced with polyethylene phthalate having a terminal sodium or potassium. This end-treated polyethylene phthalate is
It is described in U.S. Pat. No. 4,425,470 and can be produced by the method described therein. If polyethylene phthalate whose terminal is sodium or potassium is used, the nucleating agent may not be added separately in some cases.
【００１０】本発明の組成物は可塑剤を特に添加しなく
ても良好な溶融粘度を示すが、可塑剤を添加して溶融粘
度を調節してもよい。この他、本発明の組成物には、酸
化防止剤および安定剤等種々の添加剤を添加することが
できる。The composition of the present invention exhibits a good melt viscosity without adding any plasticizer, but the melt viscosity may be adjusted by adding a plasticizer. In addition, various additives such as an antioxidant and a stabilizer can be added to the composition of the present invention.
【００１１】本発明のポリエステル樹脂組成物を製造す
るには、溶融混練する方法が用いられ、一般に使用され
ているバンバリーミキサー、押出し機、各種のニーダー
等の混練装置を用いることができる。また、本発明のポ
リエステル樹脂組成物を製造する際の混練順序について
は、各成分を一度に混練しても良く、また、ポリオレフ
ィンをサイドフィーダーから供給してもよい。In order to produce the polyester resin composition of the present invention, a method of melt kneading is used, and a kneading device such as a Banbury mixer, an extruder and various kneaders which are generally used can be used. Regarding the kneading order when the polyester resin composition of the present invention is produced, the respective components may be kneaded at once, or the polyolefin may be supplied from a side feeder.
【００１２】本発明のポリエステル樹脂組成物は、溶融
安定性が高いので、成形時にばりが生じにくくなり外観
が良好であり且つ寸法および重量のばらつきも少ない優
れた成形品を得ることができる。また、本発明のポリエ
ステル樹脂組成物は、耐吸湿性が良好なので、紙バッグ
を開いた直後ポリエチレンテレフタレートペレットを乾
燥なしに成形しても成形性は良好でありしかも強度が高
く外観等にも優れた成形品を与える。Since the polyester resin composition of the present invention has high melt stability, it is possible to obtain an excellent molded product which is less likely to cause flash during molding, has a good appearance, and has less variation in size and weight. Further, since the polyester resin composition of the present invention has good moisture absorption resistance, the polyethylene terephthalate pellets can be molded immediately after opening the paper bag without drying, and the moldability is good, and the strength and the appearance are excellent. Give a molded article.
【００１３】[0013]
【実施例】本発明を以下の実施例及び比較例により更に
詳細に説明するが、本発明はこれらの実施例にのみ限定
されるものではない。次の表に示す通りの成分を含有す
る実施例１〜３および比較例１の組成物を調製し、同表
に示す通りの物性値の測定結果を得た。 実施例１ 実施例２ 実施例３ 比較例１ ＰＥＴ 59 55 48 63 ＰＰ 4 8 15 0 ナトリウム塩 4 4 4 4 ガラス繊維 30 30 30 30 乾燥時溶融粘度(pascal sec) 215 180 176 251 滞留時溶融粘度(pascal sec) 192 178 182 204 吸湿時溶融粘度(pascal sec) 83.5 89.1 95.3 94.5 滞留時溶融粘度保持率（％） 89.3 98.9 100 81.3 吸湿時溶融粘度保持率（％） 38.8 49.5 54.2 37.6 引っ張り強度 乾燥時 1440 1320 1010 1590 （Kg／ cm 2 ） 吸湿時 1340 1300 1060 1380 引っ張り伸び率 乾燥時 3.49 3.70 3.21 3.27 （％） 吸湿時 2.80 3.44 3.16 2.46 曲げ強度 乾燥時 2230 2100 1670 2450 （Kg／ cm 2 ） 吸湿時 2090 2060 1780 2070 アイゾット衝撃強さ 乾燥時 99.2 93.7 78.3 101 （Kg-cm ／cm） 吸湿時 63.6 85.6 69.7 47.9The present invention will be described in more detail with reference to the following examples and comparative examples, but the present invention is not limited to these examples. The compositions of Examples 1 to 3 and Comparative Example 1 containing the components shown in the following table were prepared, and the measurement results of physical properties shown in the table were obtained. Example 1 Example 2 Example 3 Comparative Example 1 PET 59 55 48 63 PP 4 8 15 0 Sodium salt 4 4 4 4 Glass fiber 30 30 30 30 Dry melt viscosity (pascal sec) 215 180 176 251 Melt viscosity at residence (pascal sec) 192 178 182 204 Melt viscosity when absorbing moisture (pascal sec) 83.5 89.1 95.3 94.5 Melt viscosity retention rate at retention (%) 89.3 98.9 100 81.3 Melt viscosity retention rate at moisture absorption (%) 38.8 49.5 54.2 37.6 Tensile strength Drying 1440 1320 1010 1590 (Kg / cm 2 ) Moisture absorption 1340 1300 1060 1380 Tensile elongation dry 3.49 3.70 3.21 3.27 (%) Moisture absorption 2.80 3.44 3.16 2.46 Bending strength dry 2230 2100 1670 2450 (Kg / cm 2 ) When absorbing moisture 2090 2060 1780 2070 Izod impact strength When drying 99.2 93.7 78.3 101 (Kg-cm / cm) When absorbing moisture 63.6 85.6 69.7 47.9
【００１４】これらの実施例および比較に於ては下記の
成分を使用した。ポリエチレンテレフタレート（ＰＥ
Ｔ）は、デュポン社製のもので、固有粘度は約０．６７
〜０．５８である。ポリオレフィンとしてはポリポロピ
レン（ＰＰ）を使用した。これは、チッソ社製のポリポ
ロピレンＫ１００８であり、メルトインデックスは１０
ｇ／１０分である。ナトリウム塩としてはデュポン社製
サ−リン８９２０を用いた。各組成物試料には、この
他、可塑剤および酸化剤も添加した。The following components were used in these examples and comparisons. Polyethylene terephthalate (PE
T) is manufactured by DuPont and has an intrinsic viscosity of about 0.67.
Is 0.58. Polypropylene (PP) was used as the polyolefin. This is Polysoporene K1008 manufactured by Chisso Co., and has a melt index of 10
g / 10 minutes. As a sodium salt, DuPont Sarlin 8920 was used. In addition, a plasticizer and an oxidizer were also added to each composition sample.
【００１５】前記表に示す重量部の樹脂および核剤およ
びその他の添加剤を、タンブラーで２０分間予備混合し
た後、東芝機械社製二軸押出機ＴＥＭ３５Ｂを用い２９
０℃の温度で溶融混練して樹脂組成物を得た。これらの
樹脂組成物に対して東洋精機製キャピログラフを用いて
２８０℃で剪断応力１２１６（sec--1) での溶融粘度を
測定した。ここで乾燥時溶融粘度とは、水分率が０．０
２％以下のペレットを用いて滞留時間３分で測定したと
きの溶融粘度のことである。滞留時溶融粘度とは、水分
率が０．０２％以下のペレットを用いて滞留時間３０分
で測定したときの溶融粘度のことである。また、吸湿時
溶融粘度とは水分率０．０５％のペレットを使用して測
定したときの溶融粘度のことである。滞留時溶融粘度保
持率と吸湿時溶融粘度保持率は各々以下の式で求められ
る。 滞留時溶融粘度保持率（％）＝（Ａ／Ｂ）×１００ 吸湿時溶融粘度保持率（％）＝（Ｃ／Ｄ）×１００ Ａ＝滞留時溶融粘度， Ｂ＝乾燥時溶融粘度，The resin, nucleating agent and other additives in the parts by weight shown in the above table are premixed for 20 minutes by a tumbler, and then the twin-screw extruder TEM35B manufactured by Toshiba Machine Co., Ltd. is used 29
A resin composition was obtained by melt-kneading at a temperature of 0 ° C. The melt viscosity of these resin compositions at a shear stress of 1216 (sec -1 ) was measured at 280 ° C using a Toyo Seiki Capillograph. Here, the dry melt viscosity means that the water content is 0.0
It is the melt viscosity when measured with a residence time of 3 minutes using pellets of 2% or less. The melt viscosity at the time of retention is the melt viscosity when measured with a retention time of 30 minutes using pellets having a water content of 0.02% or less. Also, the melt viscosity upon absorption of moisture is the melt viscosity measured using a pellet having a water content of 0.05%. The retention rate of melt viscosity during retention and the retention rate of melt viscosity during moisture absorption are each calculated by the following equations. Retention rate of melt viscosity during retention (%) = (A / B) × 100 Retention rate of melt viscosity during moisture absorption (%) = (C / D) × 100 A = melt viscosity during retention, B = melt viscosity during drying,
【００１６】Ｃ＝吸湿時溶融粘度（滞留時間３分），Ｄ
＝乾燥時溶融粘度（滞留時間３分）物性試験に関して
は、この樹脂組成物を１３５℃で３時間乾燥した後、成
形機を用いて２９０℃、金型温度９０℃で標準物性試験
片を作製し、この樹脂組成物の乾燥時の物性を測定し
た。試験方法は、引っ張り試験はＡＳＴＭ−６３８に準
拠し、曲げ試験はＡＳＴＭ−７９０に準拠して行なっ
た。アイゾット衝撃試験はＤ−２５６に準拠した。湿時
の物性については、水分率０．０５％のこの樹脂組成物
のペレットを用いてそれぞれの物性を測定した。水分率
は、カールフィッシャー法で測定した。C = melt viscosity when absorbing moisture (residence time 3 minutes), D
= Regarding the melt viscosity upon drying (retention time 3 minutes) physical property test, after drying this resin composition at 135 ° C for 3 hours, a standard physical property test piece was prepared at 290 ° C and a mold temperature of 90 ° C using a molding machine. Then, the physical properties of this resin composition during drying were measured. As for the test method, the tensile test was conducted according to ASTM-638, and the bending test was conducted according to ASTM-790. The Izod impact test was based on D-256. Regarding the physical properties when wet, the respective physical properties were measured using pellets of this resin composition having a water content of 0.05%. The water content was measured by the Karl Fischer method.
【００１７】上記の表に示された測定結果から明らかな
ように、本発明のポリエステル樹脂組成物は、ポリエチ
レンテレフタレートの優れた機械的特性を有し、溶融安
定性と耐吸湿特性にも優れた樹脂組成物である。As is clear from the measurement results shown in the above table, the polyester resin composition of the present invention has excellent mechanical properties of polyethylene terephthalate, and excellent melt stability and moisture absorption resistance. It is a resin composition.
【００１８】[0018]
【発明の効果】本発明のポリエステル樹脂組成物は、ポ
リエチレンテレフタレートを主成分とするポリエステル
樹脂組成物の優れた機械的特性を有し、かつ溶融安定性
および耐吸湿特性にも優れている。Industrial Applicability The polyester resin composition of the present invention has the excellent mechanical properties of the polyester resin composition containing polyethylene terephthalate as the main component, and also has excellent melt stability and moisture absorption resistance.
Claims (3)
よびポリオレフィンからなり、該ポリエチレンテレフタ
レートと該ポリオレフィンの比が９５：５〜８０：２０
であることを特徴とするポリエステル樹脂組成物。1. It consists essentially of polyethylene terephthalate and a polyolefin, the ratio of said polyethylene terephthalate to said polyolefin being 95: 5 to 80:20.
And a polyester resin composition.
る請求項１に記載のポリエステル樹脂組成物。2. The polyester resin composition according to claim 1, wherein the polyolefin is polypropylene.
１５０部の無機強化物質または難燃剤を含有する請求項
１または２に記載のポリエステル樹脂組成物。3. Further 5 to 100 parts by weight of the composition
The polyester resin composition according to claim 1 or 2, which contains 150 parts of an inorganic reinforcing substance or a flame retardant.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26636991A JPH069860A (en) | 1991-10-15 | 1991-10-15 | Polyester resin composition |
| CA 2121459 CA2121459A1 (en) | 1991-10-15 | 1992-10-13 | Polyester resin composition |
| EP92922430A EP0608351A1 (en) | 1991-10-15 | 1992-10-13 | Polyester resin composition |
| PCT/US1992/008715 WO1993008233A1 (en) | 1991-10-15 | 1992-10-13 | Polyester resin composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26636991A JPH069860A (en) | 1991-10-15 | 1991-10-15 | Polyester resin composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH069860A true JPH069860A (en) | 1994-01-18 |
Family
ID=17429989
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26636991A Pending JPH069860A (en) | 1991-10-15 | 1991-10-15 | Polyester resin composition |
Country Status (4)
| Country | Link |
|---|---|
| EP (1) | EP0608351A1 (en) |
| JP (1) | JPH069860A (en) |
| CA (1) | CA2121459A1 (en) |
| WO (1) | WO1993008233A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4339476A1 (en) * | 1993-11-19 | 1995-05-24 | Bayer Ag | Polyalkylene terephthalate injection molding compositions |
| WO2007070967A1 (en) * | 2005-12-22 | 2007-06-28 | Vip Plastic Packaging Pty Ltd. | Polymer blends |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL136859C (en) * | 1962-07-27 | 1900-01-01 | ||
| DE2139125A1 (en) * | 1971-08-05 | 1973-02-15 | Huels Chemische Werke Ag | THERMOPLASTIC MOLDING COMPOUND MADE OF POLYAETHYLENE TEREPHTHALATE |
| WO1990014391A1 (en) * | 1989-05-15 | 1990-11-29 | Eastman Kodak Company | Reinforced polyester molding compositions |
-
1991
- 1991-10-15 JP JP26636991A patent/JPH069860A/en active Pending
-
1992
- 1992-10-13 WO PCT/US1992/008715 patent/WO1993008233A1/en not_active Application Discontinuation
- 1992-10-13 CA CA 2121459 patent/CA2121459A1/en not_active Abandoned
- 1992-10-13 EP EP92922430A patent/EP0608351A1/en not_active Withdrawn
Also Published As
| Publication number | Publication date |
|---|---|
| EP0608351A1 (en) | 1994-08-03 |
| WO1993008233A1 (en) | 1993-04-29 |
| CA2121459A1 (en) | 1993-04-29 |
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