EP2206654B1 - Vial rubber-stopper - Google Patents

Vial rubber-stopper Download PDF

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Publication number
EP2206654B1
EP2206654B1 EP08838829.3A EP08838829A EP2206654B1 EP 2206654 B1 EP2206654 B1 EP 2206654B1 EP 08838829 A EP08838829 A EP 08838829A EP 2206654 B1 EP2206654 B1 EP 2206654B1
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EP
European Patent Office
Prior art keywords
flange
vial
cylindrical leg
ring
rubber stopper
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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Application number
EP08838829.3A
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German (de)
English (en)
French (fr)
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EP2206654A4 (en
EP2206654A1 (en
Inventor
Tsuyoshi Koshidaka
Masamichi Sudo
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.)
Daikyo Seiko Ltd
Original Assignee
Daikyo Seiko Ltd
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Publication date
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Publication of EP2206654A1 publication Critical patent/EP2206654A1/en
Publication of EP2206654A4 publication Critical patent/EP2206654A4/en
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D39/00—Closures arranged within necks or pouring openings or in discharge apertures, e.g. stoppers
    • B65D39/0005—Closures arranged within necks or pouring openings or in discharge apertures, e.g. stoppers made in one piece
    • B65D39/0023—Plastic cap-shaped hollow plugs
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
    • A61J1/00—Containers specially adapted for medical or pharmaceutical purposes
    • A61J1/14—Details; Accessories therefor
    • A61J1/1468—Containers characterised by specific material properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D2539/00—Details relating to closures arranged within necks or pouring openings or in discharge apertures, e.g. stoppers
    • B65D2539/001—Details of closures arranged within necks or pouring opening or in discharge apertures, e.g. stoppers
    • B65D2539/003—Details of closures arranged within necks or pouring opening or in discharge apertures, e.g. stoppers provided with sealing flanges or ribs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D2539/00—Details relating to closures arranged within necks or pouring openings or in discharge apertures, e.g. stoppers
    • B65D2539/001—Details of closures arranged within necks or pouring opening or in discharge apertures, e.g. stoppers
    • B65D2539/008—Details of closures arranged within necks or pouring opening or in discharge apertures, e.g. stoppers with coatings or coverings

Definitions

  • This invention relates to a rubber stopper used to seal an opened portion of vials and syringes as medical vessels which will be hereinafter simply referred to as vial and, in particular, to a rubber stopper in which stoppering properties can be improved without damaging sealing properties in the absence of silicone coating.
  • a stopper body used to seal an opened portion of chemical or medical liquid-containing vial it is required for a stopper body used to seal an opened portion of chemical or medical liquid-containing vial to meet various quality requirements such as sealing properties, gas barrier properties, chemical resistance, needling resistance, low reactivity and the like and, in general, a rubber stopper body of high elastic deformation is frequently employed as a product sufficient to satisfy these requirements, which will be hereinafter referred to as rubber stopper.
  • a syringe needle is often stuck through the rubber stopper from an upper surface thereof to suck up a chemical or medical liquid in a vial.
  • the rubber stopper should meet the quality requirement of the transfusion rubber stopper test according to the Japanese Pharmacopoeia, XV edition and, in speciality, should pass the elution test under a condition of 121°C for one hour using a heat resistant high pressure steam sterilizer.
  • thermoplastic styrene elastomers such as SEBS
  • thermoplastic elastomers mainly comprising polyisobutylene and polybutadiene and the like as a material for vial rubber stopper which meets the requirement as described above.
  • a cylindrical leg portion is protruded downward from a disc-like top portion to form a flange upward, a diameter of the leg portion being smaller than that of the disc.
  • the cylindrical leg portion of the vial rubber stopper is driven into an opened portion of the vial so that a bottom surface of the flange of the disc-like top portion is stuck firmly to an end surface of the opened portion.
  • the peripheral root portion is left as a naked rubber stock, thereby improving sealing properties of the vial, while the rubber stopper sometimes comes up to the surface after it is driven into the vial opened portion due to strong friction and repulsion of the naked rubber stock, thereby causing such problems that the stopper might be driven repeatedly plural times or is hardly to drive completely.
  • a vial rubber stopper GP as shown in Fig. 5 has been conventionally developed and used widely.
  • a wide belt-like ring protrusion R is formed on a cylindrical leg portion L to keep sealing properties of a vial opened portion, while an inactive film lamination is applied on surfaces of the ring protrusion R and a portion as a periphery of a disc-like top portion T other than a bottom surface T2 of a flange T1 as shown in Fig. 5 by a dark mesh pattern.
  • the bottom surface T2 of the flange T1 of the rubber stopper GP is not laminated to leave it as a naked rubber stock, while the upper ring protrusion R of the cylindrical leg portion L is driven into the vial opened portion as shown in Fig. 5 by a faint mesh pattern.
  • a vial rubber stopper according to the preamble of claim 1 is known from JP 5 038785 A .
  • This invention has been completed to solve conventional problems as described above and accordingly it is an object of the invention is to provide a vial rubber stopper of high sealing properties, gas barrier properties, chemical resistance and needling resistance as well as low reactivity, having improved productivity in the pharmaceutical manufacturing process and mechanical conveying properties, which is prepared without silicone coating.
  • At least one ring-like raised portion of a slightly larger diameter than that of the vial rubber stopper is formed on the outer peripheral surface of the cylindrical leg portion, which surface is laminated with an inactive synthetic resin film of low friction resistance such as fluororesins.
  • the under-flange ring portion of the cylindrical leg portion is left as a naked rubber stock, which is connected to the bottom surface of the flange arranged around the cylindrical leg portion, distance from the flange bottom surface to the nearest ring-like raised portion is in the range of 1/3 to 5 times of overall height of the ring-like raised portion.
  • the ring-like raised portion arranged nearest to the flange bottom surface is pushed against an inner peripheral surface of vial opened portion to cause a shrinkage in diameter when the cylindrical leg portion is driven into the vial opened portion, so that the under-flange ring portion as a naked rubber stock never comes in contact with the inner peripheral surface of the vial opened portion.
  • improved sealing properties and high stoppering properties can be secured by the present vial rubber stopper without applying conventional silicone coating.
  • the bottom surface in such a naked situation is firmly joined to the surface of the vial opened portion when the present vial rubber stopper is driven into the vial end portion, thereby high sealing properties being secured.
  • the upper and bottom surfaces of the disc-like top portion other than the flange bottom surface, the maximum diametral portion of the flange-peripheral surface and the surface of the cylindrical leg portion other than the under-flange ring portion are laminated with an inactive synthetic resin film such as fluororesins, thereby mutual sticking of rubber stopper being avoided to improve mechanical conveying properties thereof.
  • a vial rubber stopper 1 as an embodiment of the invention comprises a shape in which a cylindrical leg portion 3 is coaxially protruded from a bottom surface of a thick top disk portion 2, a diameter thereof being smaller than that of the than that of the disc-like top portion and a surrounding edge of the disc-like top portion 2 being overhung from upward of the cylindrical leg portion 3 to form a flange 2A.
  • An under-flange ring portion 3A is divided in a circular form of predetermined width on an upper end portion of the cylindrical leg portion 3, which is connected to a bottom surface 2A1 of the flange 2A.
  • First and second ring-like raised portions 3B and 3C are formed on a peripheral surface of the cylindrical leg portion 3 below the under-flange ring portion 3A at a predetermined interval in the vertical axial direction and extended in the circumferential direction parallel to the under-flange ring portion 3A.
  • a vial rubber stopper 1 shown in Fig. 2 as a modified example of the embodiment of Fig. 1 there are formed a cutaway portion 3E on the cylindrical leg portion 3 and a separate-type raised portion 3D on the outer peripheral surface thereof.
  • the cutaway portion 3E is formed by cutting the cylindrical leg portion 3 upwardly from a tip side opposed to the under-flange ring portion 3A to a line between the first and the second ring-like raised portions 3B and 3C in the axial direction at a predetermined interval.
  • the cutaway portion 3E is shown only one in Fig. 2 but may be formed plurally and, in the case of plurality, each one may be the same size and opposing each other, or may be random size and arranged randomly.
  • the separate-type raised portion 3D is formed below the second ring-like raised portion 3C parallel thereto and divided in the circumferentially direction, which cross-sectional shape is, for example, nearly triangle to keep stability.
  • Cross-sectional shape of the first ring-like raised portion 3B arranged above the cutaway portion 3E and the second ring-like raised portion 3C cut off by the cutaway portion 3E may be semicircular, semi-oval, triangle, rectangular, trapezoid or any others.
  • Those potions 3B and 3C shown in Fig. 1 may also be shaped similarly.
  • the first ring-like raised portion 3B arranged above the cutaway portion 3E may be not only one but formed plurally.
  • a maximum outer diameter of the first and the second ring-like raised portions 3B and 3C shown in Fig. 1 and that of similar portions 3B and 3C shown in Fig. 2 are slightly larger, and more definitely about 1 % to 30 % larger, than a caliber of a vial B opened portion shown in Fig. 4 , i.e., diameter of an opened inner peripheral portion B1.
  • An increase in maximum outer diameter as described above makes it possible to secure high sealing properties and stoppering properties when the vial rubber stopper is driven into the vial B opened portion.
  • Such the increase in diameters of the first and the second ring-like raised portions 3B and 3C varies depending on elasticity of a rubber stock to be used for the rubber stopper 1 and a material of the vial B (glass or synthetic resins) and is not necessarily fixed, although it is desirable to increase diameters thereof in the range of about 1 % to 30 % compared with a caliber of the vial B when elasticity of a synthetic resin used as a material of the vial B is about 2 to 2.5 GPa and Shore A hardness of a rubber stock used as the rubber stopper 1 is about 15 to 45.
  • the uppermost first ring-like raised portion 3B is preferably arranged to be fallen in a length range from 1/3 to 5 times of overall height thereof in the downward direction from an upper edge of the under-flange ring portion 3A which coincides in arrangement with the bottom surface 2A1 of the flange 2A. That is to say, the shortest interval of the nearest first ring-like raised portion 3B from the bottom surface 2A1 of the flange 2A is preferably fallen in the range from 1/3 to 5 times of overall height thereof.
  • the rubber stock of the under-flange ring portion 3A comes in contact with the inner peripheral surface B1 of the vial B opened portion, thereby causing failure in stoppering and loosing sealing properties of the vial B.
  • An optimum location of the first ring-like raised portion 3B varies depending on hardness and size of the rubber stopper 1.
  • Hardness (Shore A) of a rubber stock within the optimum designed value is about 15 to 45 and size of the rubber stopper 1 is about 5 to 50 mm in diameter.
  • the bottom surface 2A1 of the flange 2A is left as a naked rubber stock. Further, the bottom surface 2A1 is molded to adhere to an edge surface B2 of the opened portion of the vial B shown in Fig. 4 .
  • the edge surface B2 of the opened portion is generally shaped into flat and, accordingly, the bottom surface 2A1 of the flange 2A is preferably flat.
  • the upper surface of the disc-like top portion 2 including the upper surface of the flange 2A, the maximum diametral portion 2A2 of the peripheral surface of the flange 2A, the bottom surface of the disc-like top portion 2 arranged in the cylindrical leg portion 3 and the surface including the outer and inner peripheral surfaces of the cylindrical leg portions 3 other than the under-flange ring portion 3A are laminated with a synthetic resin film as shown in Fig. 1 or Fig. 2 (see, mesh patterns drawn therein).
  • the bottom surface 2A1 of the flange 2A and the surface of the under-flange ring portion 3A of the cylindrical leg portion 3 are left as a naked rubber stock.
  • An upper edge of the synthetic resin film laminated on the outer peripheral surface of the cylindrical leg portion 3 is fit upward over the first ring-like raised portion 3B, which the nearest location to the bottom surface 2A1 of the flange 2A, so that the under-flange ring portion 3A is divided between the upper edge and the bottom face 2A1.
  • the upper edge of the synthetic resin film is preferably fit downward of the bottom surface 2A1 of the flange 2A at an interval of 0.5 mm or more so as to leave vertical width of 0.5 mm or more for the under-flange ring portion 3A.
  • the cutaway portion 3E formed on the cylindrical leg portion 3 of the vial rubber stopper 1 shown in Fig. 2 is effective as will be described in the following.
  • a solvent or water component in a medical liquid charged in the vial B shown in Fig. 4 should be removed, the vial B with the medical liquid charged therein is placed in an appropriate device such as vacuum dryer while keeping the vial rubber stopper 1 in a half-driven situation.
  • the solvent or water component contained in the vial B is evaporated and suctioned out through the cutaway portion 3E when the vacuum dryer is operated, the medical liquid being thus vacuum dried.
  • Such a half-driven situation of the vial rubber stopper 1 can be kept satisfactorily by means of the separate-type raised portion 3D which is separated in the circumferential direction and has a triangle cross-section.
  • Fig. 3 is an illustration of vial rubber stopper 1 shown in Figs. 1 and 2 in which the rubber stopper 1 is placed in a mold in the course of molding.
  • the cylindrical leg portion 3 is subjected to press molding to monolithically mold (laminate) with a synthetic resin film (drawn as mesh patterns in Fig. 3 ), punched out and set in a bottom force (not shown).
  • a material of the disc-like top portion 2 is placed on the cylindrical leg portion 3 in the above mentioned situation, while a synthetic resin film is put on the stock which is then press-molded by means of a force (not shown) . Accordingly, press molding of the disc-like top portion 2, lamination of the disc-like top portion 2 with the synthetic resin film and unification of the disc-like top portion 2 and the cylindrical leg portion 3 are conducted at the same time.
  • the laminated disc-like portion 2 is drawn by mesh patterns in Fig. 3 and implies a continuous surface ranging from the upper surface of the disc-like top portion 2, which includes the upper surface of the flange 2A, and the maximum diametral portion 2A2 of the peripheral surface of the flange 2A.
  • the synthetic resin film used to laminate the cylindrical leg portion 3 and that of used to laminate the maximum diametral portion 2A2 of the peripheral surface of the flange 2A may be the same or different.
  • a fluororesin film is preferably used either in the case of same or different, and different fluororesin films are preferably selected in the case of different.
  • An Ultra High Molecular Weight polyethylene resin film is also used preferably as a synthetic resin film other than a fluororesin form standpoints of thermal resistance, chemical resistance, etc.
  • each rubber stock does not exert any bad influence upon their unification, if the same or different rubber stock useful for unifying these two portions 2 and 3 is used even when the synthetic resin film to be laminated is the same or different.
  • the rubber stock for comprising the disc-like top portion 2 and the cylindrical leg portion 3 of the present vial rubber stopper 1 is not restricted to a specific one, if the material is tough and has appropriate hardness, impact resilience and other excellent properties such as thermal resistance, aging resistance, chemical resistance, gas barrier properties, low eluting properties and low reactivity.
  • Rubber stocks used in the present invention include, for example, butyl rubber, i.e., isoprene-isobutylene copolymer, halogenated butyl rubber prepared by chlorinating or brominating butyl rubber, acrylonitrile-butadiene copolymer rubber, isoprene terpolymer, isoprene rubber, butadiene rubber, styrene-butadiene rubber, ethylene-propylene rubber, ethylene-propylene-diene rubber, chloro-sulfonated polystyrene, ethylene-vinyl acetate copolymer, styrene-ethylene-butylene-styrene (SEBS) thermoplastic elastomer, thermoplastic elastomer comprising polyisobutylene and polybutadiene as a main component, and a rubber stock in which synthetic rubber such as styrene-isoprene rubber or natural rubber is used as a main component and
  • butyl rubber, halogenated butyl rubber, and thermoplastic elastomer comprising polyisobutylene or polybutadiene as a main component are preferable rubber stocks not only for a reason that they meet the requirements as described above but from a standpoint of their high gas-impermeability, ozone resistance, aging resistance and adhesive properties.
  • a fluororesin film is preferably used as a synthetic resin film for laminating the present vial rubber stopper 1, which can be laminated on the rubber stock as an inactive synthetic resin film and has high thermal resistance and chemical resistance as well as lower frictional resistance compared with that of the rubber stock.
  • the fluororesin includes, for example, tetrafluoroethylene resin (PTFE), tetrafluoroethylen-perfluoroethylene copolymer (PFA), tetrafluoroethylene-hexafluoroethylene copolymer (FEP), tetrafluoroethylene-ethylene copolymer (ATFE), polytrichlorotrifluoroethylene (PCTFE), polyfluorinated vinylidene (PVDF), polyfluorinated vinyl (PVF), etc.
  • PTFE tetrafluoroethylene resin
  • PFA tetrafluoroethylen-perfluoroethylene copolymer
  • FEP tetrafluoroethylene-hexafluoroethylene copolymer
  • ATFE tetrafluoroethylene-ethylene copolymer
  • PCTFE polytrichlorotrifluoroethylene
  • PVDF polyfluorinated vinylidene
  • PVF polyfluorinated vinyl
  • Tetrafluoroethylene resin which will be hereinafter referred to as PTFE, is especially preferable by the following reasons.
  • PTFE is considerably stable so that it does not solve or swell almost all chemicals, and is one of the most thermally resistant organic materials, simply results in transparent gel but does not exhibit melt-flow characteristics when it is melted at the melting point of 327 °C and has so high continuous working temperature as about 260 °C, while its surface is extremely hydrophobic, oil-repellent and non-adhesive and exhibits low frictional resistance and high sliding properties. Because of intrinsic advantages as described above, PTFE is sufficiently resistant to high temperature sterilizing treatments in the course of pharmaceutical and other processes.
  • PTFE laminated on the vial rubber stopper 1 comes in contact with chemicals charged in the vial for a long period of time, the laminated material does not absorb the chemicals and nothing is eluted from the lamination, thereby proving chemical stability thereof.
  • PTFE is sufficiently slidable to pressingly drive the rubber stopper into the vial after charging chemicals therein, so that it possesses characteristics to meet physical and chemical properties to be expected as a surface laminating film material, which is used to laminate sealing stoppers for sealing vial containers.
  • An Ultra High Molecular Weight polyethylene resin film may also be preferably used as a laminating material other than the fluororesin film from a standpoint of thermal resistance, chemical resistance, etc.
  • the Ultra High Molecular Weight polyethylene refers to those polyethylene polymers of about 100 million to 700 million in molecular weight.
  • Thickness of the inactive synthetic resin film such as the above mentioned fluororesin film is preferably about 0.001 to 0.3 mm, more preferably 0.01 to 0.2 mm and most preferably 0.02 to 0.15 mm, and the thickness fallen in this range lowers voids of thin film, thereby reducing the defectiveness level of products with advantage.
  • An excessively thinner film makes it difficult to yield the products and would cause processing failure and inadequate certification of products, while excessively thicker one raises rigidity of the film extremely so that sealing properties and needling resistance of a completed rubber stopper deteriorate inadequately.
  • a surface of the synthetic resin film is preferably cleaned or treated by means of, primer treatment, corona discharge, plasma discharge, glow discharge, arc discharge, sputtered etching and the like, thereby adhesion between the film and the rubber stock being strengthened.
  • the preferred adhesive strength is about 1 to 30 kg/cm.
  • the present vial rubber stopper 1 is molded in the following manner.
  • the cylindrical leg portion 3 which has been laminated by press molding in advance, is set in the bottom force (not shown).
  • a molding stock of the disc-like top portion 2 and a laminating synthetic resin film are placed on the upper surface of the leg portion 3, followed by press molding of the synthetic resin film and the molding stock by means of a force (not shown) .
  • Molding of the disc-like top portion 2, lamination of the synthetic resin film on the leg portion 2 and unification of the cylindrical leg portion 3 are conducted simultaneously.
  • the laminating synthetic resin film is placed on the bottom force (not shown) for molding the cylindrical leg portion 3 first of all, on which an uncured rubber stock to be used to mold the cylindrical leg portion 3 is placed.
  • the cylindrical leg portion 3 is molded and cured by means of press molding and, at the same time, a continuous surface covering over the inner peripheral surface of the cylindrical leg portion 3 and the outer peripheral surface thereof is laminated, the outer peripheral surface including the first ring-like raised portion 3B, the second ring-like raised portion 3C and the separate-type raised portion 3D.
  • the bottom force is opened to take out the cylindrical leg portion 3 which is laminated by the synthetic resin film and cut into a predetermined shape.
  • the thus laminated and cut cylindrical leg portion 3 is cleaned and set in a bottom force (not shown), while the uncured rubber stock to be used for molding the disc-like top portion 2 is placed thereon, and then the laminating synthetic resin film is put on the upper surface of the rubber stock, followed by clamping by means of a force (not shown) and press-molding under pressure of about 50 to 150 kg/cm 2 at temperature ob about 150 to 200 °C.
  • molding of the disc-like top portion 2 and lamination thereof are conducted by means of the molding tool for molding the disc-like top portion 2, but there may be used the bottom force for molding the cylindrical leg portion 3 in another embodiment.
  • each rubber stock to be used for molding the cylindrical leg portion 3 and the disc-like top portion 2 may either be the same composition or different one as described above, if each rubber stock can be unified.
  • FIG. 4 An applied example of the present vial rubber stopper 1 is shown in Fig. 4 .
  • the cylindrical leg portion 3 of the present vial rubber stopper 1 is inserted and driven into the opened portion of the vial B along the inner peripheral surface B1 to adhere the bottom surface 2A1 of flange 2A of the disc-like top portion 2 to the edge surface B2 of the opened portion.
  • the disc-like top portion 2 is covered with an aluminum cap A to caulk around the opened portion of the vial B and seal it. Complete seal of the vial B is thus secured.
  • a plate stock of uncured rubber composition shown in Table 1 was used as a rubber stock for molding the cylindrical leg portion 3 and the disc-like top portion 2.
  • PTFE inactive synthetic resin
  • Table 1 Composition of Rubber Stock Parts by Weight butyl rubber 100 wet water-containing silica (1) 30 zinc oxide (2) 1.5 1,1-bis(t-butylperoxide)-3,3,5-trimethylhexane (3) 2 (1) Nipushiiru ER; available from Nippon Sirika Kogyo (2) Active Chinese White AZO; available from Seido Kagaku Kogyo (3) Perhexane 3M-40; available from NOF Corporation
  • maximum outer diameters (maximum height of the raised portions) of the first and the second ring-like raised portions 3B and 3C as well as the separate-type raised portion 3D are sums of doubled dimensions of their overall height shown in Table 2 and diameter of the cylindrical leg portion 3 as shown in Table 2, respectively.
  • the plate stock of uncured rubber composition shown in Table 1 and the laminating synthetic resin film were placed thereon and then press molding of the disc-like top portion 2, lamination of the synthetic resin and unification of the disc-like top portion 2 and the cylindrical leg portion 3 were conducted at the same time under the same pressure and temperature condition as described above, followed by opening of the bottom force, cutting as shown in Fig. 3 by the line "x" and washing.
  • the thus yielded vial rubber stopper 1 was driven into the opened portion of commercial vials B and it was found that every tested rubber stopper 1 was fitted therein satisfactorily.
  • the vials B were charged with water and kept in a half-stoppered situation with the rubber stopper 1, followed by drying in a vacuum dryer under pressure of 0.5 kg/cm 2 and at temperature of 25 °C for 24 hours.
  • a conventional vial rubber stopper GP shown in Fig. 5 was used to repeat a stoppering test and a vacuum drying test in a similar manner as described above. As a result, it was found that a stoppering process was performed unsatisfactorily in the stoppering test because of considerable frictional resistance caused by rubber stock used as a wide belt ring-like raised portion R, while in the vacuum drying test, vacuum drying itself was performed favorably but the stoppering process after vacuum drying was not proceeded successfully.
  • the present vial rubber stopper is conveniently applicable to various vials provided with an opened portion of different calibers. Further, the present stopper can be applied not only to embodiments in which an injection needle pierces the top portion but to those cases in which no needle pierces the top portion.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Medical Preparation Storing Or Oral Administration Devices (AREA)
  • Closures For Containers (AREA)
EP08838829.3A 2007-10-18 2008-10-20 Vial rubber-stopper Active EP2206654B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2007270871 2007-10-18
PCT/JP2008/069393 WO2009051282A1 (ja) 2007-10-18 2008-10-20 バイアル用ゴム栓

Publications (3)

Publication Number Publication Date
EP2206654A1 EP2206654A1 (en) 2010-07-14
EP2206654A4 EP2206654A4 (en) 2011-01-05
EP2206654B1 true EP2206654B1 (en) 2015-07-08

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EP08838829.3A Active EP2206654B1 (en) 2007-10-18 2008-10-20 Vial rubber-stopper

Country Status (7)

Country Link
US (1) US20100206836A1 (ja)
EP (1) EP2206654B1 (ja)
JP (1) JP5479104B2 (ja)
DK (1) DK2206654T3 (ja)
ES (1) ES2545204T3 (ja)
HU (1) HUE026463T2 (ja)
WO (1) WO2009051282A1 (ja)

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JP6243096B2 (ja) 2011-11-16 2017-12-06 株式会社大協精工 バイアル用ゴム栓
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ITMI20121793A1 (it) * 2012-10-23 2014-04-24 Copan Italia Spa Elemento di chiusura di un contenitore per fluidi biologici
KR101262963B1 (ko) 2013-03-15 2013-05-09 (주)효선전기 기밀 패킹구조를 갖는 마개
DE102013214102A1 (de) * 2013-07-18 2015-02-19 Bayerische Motoren Werke Aktiengesellschaft Klebehilfe und Verfahren zum Verkleben von Bauteilen
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HUE026463T2 (en) 2016-05-30
JPWO2009051282A1 (ja) 2011-03-03
EP2206654A4 (en) 2011-01-05
US20100206836A1 (en) 2010-08-19
DK2206654T3 (en) 2015-08-24
WO2009051282A1 (ja) 2009-04-23
EP2206654A1 (en) 2010-07-14
ES2545204T3 (es) 2015-09-09
JP5479104B2 (ja) 2014-04-23

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