JP2013138697A - Laminated gasket - Google Patents
Laminated gasket Download PDFInfo
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- JP2013138697A JP2013138697A JP2011289523A JP2011289523A JP2013138697A JP 2013138697 A JP2013138697 A JP 2013138697A JP 2011289523 A JP2011289523 A JP 2011289523A JP 2011289523 A JP2011289523 A JP 2011289523A JP 2013138697 A JP2013138697 A JP 2013138697A
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- gasket
- syringe
- annular rib
- resin film
- sliding
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- -1 polytetrafluoroethylene, ethylenetetrafluoroethylene Polymers 0.000 claims description 13
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- UPZFLZYXYGBAPL-UHFFFAOYSA-N 2-ethyl-2-methyl-1,3-dioxolane Chemical compound CCC1(C)OCCO1 UPZFLZYXYGBAPL-UHFFFAOYSA-N 0.000 description 1
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 101100334009 Caenorhabditis elegans rib-2 gene Proteins 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
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- 229920000089 Cyclic olefin copolymer Polymers 0.000 description 1
- 239000004713 Cyclic olefin copolymer Substances 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 1
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920000459 Nitrile rubber Polymers 0.000 description 1
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- 229920002367 Polyisobutene Polymers 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
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- 125000003700 epoxy group Chemical group 0.000 description 1
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- 125000001033 ether group Chemical group 0.000 description 1
- 229920006244 ethylene-ethyl acrylate Polymers 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical group FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004388 gamma ray sterilization Methods 0.000 description 1
- 238000013023 gasketing Methods 0.000 description 1
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
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- 238000003780 insertion Methods 0.000 description 1
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- 238000010884 ion-beam technique Methods 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 229920003049 isoprene rubber Polymers 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
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- 230000008018 melting Effects 0.000 description 1
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
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- 229920003052 natural elastomer Polymers 0.000 description 1
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- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
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- 229920002647 polyamide Polymers 0.000 description 1
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- 229920000728 polyester Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920013716 polyethylene resin Polymers 0.000 description 1
- 239000011116 polymethylpentene Substances 0.000 description 1
- 229920000306 polymethylpentene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
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- 238000007493 shaping process Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
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- 239000011734 sodium Substances 0.000 description 1
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- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 229920006163 vinyl copolymer Polymers 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
- A61M5/00—Devices for bringing media into the body in a subcutaneous, intra-vascular or intramuscular way; Accessories therefor, e.g. filling or cleaning devices, arm-rests
- A61M5/178—Syringes
- A61M5/31—Details
- A61M5/315—Pistons; Piston-rods; Guiding, blocking or restricting the movement of the rod or piston; Appliances on the rod for facilitating dosing ; Dosing mechanisms
- A61M5/31511—Piston or piston-rod constructions, e.g. connection of piston with piston-rod
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
- A61M2207/00—Methods of manufacture, assembly or production
- A61M2207/10—Device therefor
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- Health & Medical Sciences (AREA)
- Vascular Medicine (AREA)
- Engineering & Computer Science (AREA)
- Anesthesiology (AREA)
- Biomedical Technology (AREA)
- Heart & Thoracic Surgery (AREA)
- Hematology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Gasket Seals (AREA)
- Sealing Devices (AREA)
- Infusion, Injection, And Reservoir Apparatuses (AREA)
Abstract
Description
本発明は、不活性樹脂フィルムで積層されたガスケット、特に薬液が注射器に充填されたプレフィルドシリンジに関する。 The present invention relates to a gasket laminated with an inert resin film, and more particularly to a prefilled syringe in which a drug solution is filled in a syringe.
近年 使用時の簡便性に優れ、誤用を無くす意味において、予め薬液が注射器に充填されたプレフィルドシリンジの使用が拡大している。これらのプレフィルドシリンジのゴム部材は使用されるまで薬液と直接、接するため、耐薬品性、耐ガス透過性、耐水蒸気透過性、耐老化性が優れたブチルゴム系のガスケットやノズルキャップが多用されている。 In recent years, the use of prefilled syringes in which a liquid medicine is preliminarily filled in a syringe has been expanded in the sense that it is easy to use and eliminates misuse. These prefilled syringe rubber members are in direct contact with chemicals until they are used, so butyl rubber gaskets and nozzle caps with excellent chemical resistance, gas permeation resistance, water vapor permeation resistance, and aging resistance are often used. Yes.
しかしながら、バイオ製剤等の薬剤によっては、ゴム材質の原料ゴム、配合剤由来の溶出物、およびコート剤の脱落等の相互作用により、悪影響を受けることがある。たとえば、ブチル系ゴム部材では、ガスケットの摺動性改善、ノズルキャップの固着防止の目的で、シリンジ内壁、ガスケット、ノズルキャップのゴム表面に潤滑剤として、オイルタイプまたは硬化タイプのシリコーンが塗布されているため、製剤の種類によって、バレル内壁、ゴム部材からシリコーンコート剤が脱落して異物となり、製剤品質に重大な悪影響を与える場合がある。特にシリンジ内壁にはガスケットより多量のシリコーンコート剤が塗布されており、製剤との接液面積からもその影響は大きい。 However, some drugs such as biopharmaceuticals may be adversely affected by interactions such as the rubber material rubber, the eluate derived from the compounding agent, and the dropping of the coating agent. For example, in the case of butyl rubber members, oil type or hardened type silicone is applied as a lubricant to the syringe inner wall, gasket, and nozzle cap rubber surface for the purpose of improving gasket slidability and preventing nozzle cap sticking. Therefore, depending on the type of the preparation, the silicone coating agent may fall off from the inner wall of the barrel and the rubber member to become a foreign substance, which may have a serious adverse effect on the preparation quality. In particular, a larger amount of silicone coating agent is applied to the inner wall of the syringe than the gasket, and the influence is great from the area of contact with the preparation.
そこで、製剤の安定性にブチルゴムよりも優れているフッ素樹脂フィルム等をゴムに積層した製品が開発され、硝子製シリンジ又は樹脂製プレフィルドシリンジに提案されている。たとえば耐薬品性に優れたフッ素樹脂フィルムが使用され、中でも摩擦係数が最も小さいポリテトラフルオロエチレン(PTFE)が使用されている。 Therefore, a product obtained by laminating a rubber with a fluororesin film that is superior to butyl rubber in the stability of the formulation has been developed and proposed as a glass syringe or a resin prefilled syringe. For example, a fluororesin film having excellent chemical resistance is used, and polytetrafluoroethylene (PTFE) having the smallest friction coefficient is used.
しかしながら、ガスケットの接液面、シリンジ内壁と接する摺動シール部にフッ素樹脂フィルムを積層したガスケットでは、気密性と摺動抵抗が課題となる。特にスカイビング法で製造されたフィルムは表面粗さが粗く、シリンジ内壁との気密性に問題が生じ易いという問題がある。気密性を悪くする要因として、積層されたフィルムの平滑性(表面粗さ)及び、シリンジ内径に対するガスケットの圧縮率に影響するシリンジ内径バラツキが挙げられる。 However, with a gasket in which a fluororesin film is laminated on the liquid contact surface of the gasket and the sliding seal portion in contact with the syringe inner wall, airtightness and sliding resistance are problems. In particular, the film produced by the skiving method has a problem that the surface roughness is rough and a problem is likely to occur in the airtightness with the inner wall of the syringe. Factors that deteriorate the airtightness include the smoothness (surface roughness) of the laminated films and the syringe inner diameter variation that affects the compression ratio of the gasket with respect to the syringe inner diameter.
そこで、特許文献1ではPTFEのキャスティング法フィルム、UHMWPEのインフレーション法フィルムが提案されているが、特殊な製法であり実用的ではない。また、表面粗さがRa0.05μm以下のPTFEフィルムを積層しても液モレに問題が生ずることがある。これはPTFEフィルムをPTFEの融点230℃以下である成型温度170℃で積層成型したにも拘らず、積層フィルムの表面には金型表面の微細な凹凸痕が転写されてシール性に影響するためである。また、シリンジ内径に対するガスケットの圧縮率に影響するシリンジ内径バラツキも大きな問題である。樹脂製シリンジでは±0.1以内の高精度であるが、硝子シリンジでは生地管の内径バラツキが大きく、5ml以下のサイズでも内径公差は±0.15と大きくなっている。 Therefore, Patent Document 1 proposes a PTFE casting method film and a UHMWPE inflation method film, but these are special manufacturing methods and are not practical. Further, even if a PTFE film having a surface roughness of Ra 0.05 μm or less is laminated, a problem may occur in liquid leakage. This is because even though the PTFE film is laminated and molded at a molding temperature of 170 ° C., which is a melting point of PTFE of 230 ° C. or less, fine uneven marks on the mold surface are transferred to the surface of the laminated film, thereby affecting the sealing performance. It is. In addition, the syringe inner diameter variation that affects the compression ratio of the gasket with respect to the syringe inner diameter is also a big problem. Resin syringes have high accuracy within ± 0.1, but glass syringes have large inner diameter variations in the dough tube, and the inner diameter tolerance is as large as ± 0.15 even for sizes of 5 ml or less.
特許文献2では、先端環状突起の中間まで積層された形状が提案されているが、打ち抜き刃の上刃の内側に積層されていない摺動部が縮径されて入り込む特殊な方法であり、1ml用等の小サイズのガスケットでは可能であるが、大きなサイズでは抜き刃に縮径されて入る部分の肉厚が大きくなってくるので、この方法では打ち抜きが困難となり製造できない。また、上刃の研磨により短くなるのでメンテナンスが問題となる。
一方で、円柱状の環状リブを一つまたは複数設けたガスケットが提案されている。しかしながら、環状リブが円弧状の場合、摺動抵抗には優れるが、摺接面積が小さくなることから、気密性が劣るという問題がある。また、多くの先端環状リブは同一径の直線で設計されているが、シリンジ内径との圧縮率を大きくすると摺動抵抗値が高くなり、ガスケット打栓に支障する。又、圧縮率を小さく設計すると気密性の問題が生じる。この原因は、先端リブ部はムクのゴム部であり、ゴムが変形し難い状態のためである。 On the other hand, a gasket provided with one or more cylindrical annular ribs has been proposed. However, when the annular rib has an arc shape, the sliding resistance is excellent, but since the sliding contact area is small, there is a problem that the airtightness is inferior. Many end annular ribs are designed with straight lines having the same diameter. However, if the compression ratio with the syringe inner diameter is increased, the sliding resistance value is increased, which hinders gasketing. Further, when the compression rate is designed to be small, an airtight problem occurs. The reason for this is that the tip rib is a rubber part of the rubber and the rubber is difficult to deform.
本発明は、Ra0.05μm以上と表面粗さが粗いスカイビングフィルムを成型しても、液密性と摺動抵抗に優れたガスケットを提供することを目的とする。 An object of the present invention is to provide a gasket excellent in liquid-tightness and sliding resistance even when a skiving film having a rough surface roughness of Ra 0.05 μm or more is molded.
本発明は、シリンジ内壁と摺接する環状リブを複数有するガスケットであって、先端環状リブの摺接部断面が略直線状であり、該直線部の長さが摺動側面部長さLに対して10〜55%であり、該直線部の最小径に対して0.1〜2.7%の範囲でシリンジ後端方向に直線状に拡径していることを特徴とする不活性樹脂フィルムで積層されたガスケットに関する。 The present invention is a gasket having a plurality of annular ribs that are in sliding contact with the inner wall of the syringe, and the cross section of the sliding contact portion of the tip annular rib is substantially linear, and the length of the linear portion is relative to the sliding side portion length L. 10 to 55%, an inert resin film characterized in that the diameter is linearly expanded in the direction of the rear end of the syringe within a range of 0.1 to 2.7% with respect to the minimum diameter of the linear portion. The present invention relates to a laminated gasket.
先端環状リブに位置するネジ上部に空洞を設けることが好ましい。 It is preferable to provide a cavity in the upper part of the screw located in the tip annular rib.
シリンジ内径に対し、先端環状リブの略直線部最小径、最大径および後端側環状リブの圧縮率が1〜5%であることが好ましい。 It is preferable that the compression rate of the substantially linear portion minimum diameter, maximum diameter, and rear end side annular rib of the front annular rib is 1 to 5% with respect to the syringe inner diameter.
不活性樹脂フィルムが、スカイビング法で製造されたポリテトラフルオロエチレン(PTFE)、エチレンテトラフルオロエチレン共重合樹脂フィルム(ETFE)、又は、超高分子量ポリエチレン(UHMWPE)であることが好ましい。 The inert resin film is preferably polytetrafluoroethylene (PTFE), ethylenetetrafluoroethylene copolymer resin film (ETFE), or ultrahigh molecular weight polyethylene (UHMWPE) produced by a skiving method.
不活性樹脂フィルムの厚さが25〜150μmであることが好ましい。 The thickness of the inert resin film is preferably 25 to 150 μm.
ガスケット成型金型の少なくとも摺動摺接部表面の中心線平均粗さがRa0.03μm以下に鏡面加工された成型金型によって成型されることが好ましい。 The gasket molding die is preferably molded by a molding die that is mirror-finished so that the center line average roughness of at least the sliding sliding contact portion surface is Ra 0.03 μm or less.
ガスケット基材がブチル系ゴムまたは熱可塑性エラストマーであり、J1S A硬さが 50〜70度、圧縮永久ひずみが20%以下であることが好ましい。 It is preferable that the gasket base material is butyl rubber or thermoplastic elastomer, the J1SA hardness is 50 to 70 degrees, and the compression set is 20% or less.
本発明のシリンジ内壁と摺接する環状リブを複数有する不活性フィルムで積層されたガスケットでは、先端環状リブの摺接部断面が略直線状であり、該直線部の長さが摺動側面部長さLに対して10〜55%であり、該直線部の最小径に対して0.1〜2.7%の範囲でシリンジ後端方向に直線状に拡径しているため、生産性に優れる簡便な一段成型により液密性と摺動抵抗に優れたガスケットを提供することができる。また、シリンジ内壁およびガスケットに使用されているシリコーン等の潤滑コート剤を完全に無くす、または製剤品質へ悪影響を与えない程度の極微量に低減することが可能となる。 In the gasket laminated with an inert film having a plurality of annular ribs that are in sliding contact with the syringe inner wall of the present invention, the sliding contact section of the tip annular rib is substantially linear, and the length of the linear portion is the length of the sliding side surface. It is 10 to 55% with respect to L, and the diameter is linearly expanded in the direction of the rear end of the syringe within a range of 0.1 to 2.7% with respect to the minimum diameter of the linear portion, so that productivity is excellent. A gasket having excellent liquid-tightness and sliding resistance can be provided by simple one-step molding. Further, it becomes possible to completely eliminate the lubricant coating agent such as silicone used for the syringe inner wall and the gasket, or to reduce it to a very small amount so as not to adversely affect the quality of the preparation.
以下に実施形態を掲げ、本発明を詳細に説明するが、本発明はこれらの実施形態のみに限定されるものではない。 The present invention will be described in detail below with reference to embodiments, but the present invention is not limited only to these embodiments.
本発明のシリンジ内壁と摺接する環状リブを複数有するガスケットは、先端環状リブの摺接部断面が略直線状であり、該直線部の長さが摺動側面部長さLに対して10〜55%であり、該直線部の最小径に対して0.1〜2.7%の範囲でシリンジ後端方向に略直線状に拡径していることを特徴とする。図1(a)〜(d)には、本発明のガスケットの断面図を示す。1が先端環状リブ、2が環状リブ、3が空洞である。
ここで、図1(a)に示すように、摺動側面部長さLとは先端環状リブの角よりロッド挿入後端部までの最短長さをいい、側面に沿った長さではない。なお、後端部の密着防止突起は含まない長さをいう。該直線部の長さは摺動側面部長さLに対しては、10〜55%が好ましい。
In the gasket having a plurality of annular ribs that are in sliding contact with the inner wall of the syringe of the present invention, the sliding contact section of the tip annular rib is substantially linear, and the length of the linear portion is 10 to 55 with respect to the sliding side surface length L. %, And the diameter is expanded in a substantially linear shape in the direction of the rear end of the syringe in the range of 0.1 to 2.7% with respect to the minimum diameter of the straight line portion. 1A to 1D are sectional views of the gasket of the present invention. Reference numeral 1 denotes a tip annular rib, 2 an annular rib, and 3 a cavity.
Here, as shown in FIG. 1 (a), the sliding side surface portion length L is the shortest length from the corner of the tip annular rib to the rod insertion rear end portion, not the length along the side surface. It should be noted that the length does not include the rear end protrusion prevention protrusion. The length of the straight part is preferably 10 to 55% with respect to the sliding side part length L.
本発明のガスケットは、シリンジ内壁と摺接する環状リブを複数有する。複数とは、2つ以上有することであり、2以上であれば特に限定されない。図1(a)〜(c)には環状リブが2つの態様を、図1(d)には環状リブが3つの態様を示す。 The gasket of the present invention has a plurality of annular ribs that are in sliding contact with the syringe inner wall. “Multiple” means to have two or more, and is not particularly limited as long as it is two or more. 1A to 1C show two embodiments of the annular rib, and FIG. 1D shows three embodiments of the annular rib.
一般に、従来のゴム単身のガスケットと比べて、フィルムを積層したガスケットでは、気密性と摺動性を両立させる設計が難しく、本発明では下記の設計要素とすることで可能となる。
ガスケットの打栓性(シワ、斜め打栓)、液密性、摺動性の機能性を両立させる方法として、先端環状リブが、バレル内径に対する圧縮率が1〜5%であり、複数の環状リブの内、先端側環状リブが略直線であり、略直線の長さが摺動側面部長さLに対して、10〜55%、先端環状リブの直線部最小径に対し、シリンジ後端方向に略直線状に0.1〜2.7%拡径しており、ガスケット環状リブ径が5〜40mmのガスケットの場合、略直線部の長さを1〜6mmとしたガスケット形状である。さらに、ネジ上部に空洞を設けることで、機能性が向上される。
In general, compared with a conventional gasket having a single rubber, it is difficult to design a gasket in which films are laminated to achieve both airtightness and slidability. In the present invention, the following design elements are possible.
As a method for making gaskets pluggable (wrinkled, diagonally plugged), liquid-tight, and slidable, the tip annular rib has a compression ratio of 1 to 5% with respect to the inner diameter of the barrel. Of the ribs, the tip-side annular rib is substantially straight, the length of the substantially straight line is 10 to 55% with respect to the sliding side surface length L, and the syringe rear-end direction with respect to the straight-line minimum diameter of the tip annular rib In the case of a gasket having a diameter of 0.1 to 2.7% in a substantially linear shape and a gasket annular rib diameter of 5 to 40 mm, the length of the substantially linear portion is 1 to 6 mm. Furthermore, functionality is improved by providing a cavity above the screw.
直線部の長さは摺動側面部長さLに対して、10〜55%であるが、13〜50%が好ましく、15〜45%であることがより好ましい。また、略直線部の長さは、ガスケット環状リブ径が5〜40mmのガスケットの場合、1〜6mmが好ましく、1.5〜4.5mmがより好ましい。 The length of the straight portion is 10 to 55% with respect to the sliding side portion length L, but is preferably 13 to 50%, and more preferably 15 to 45%. Moreover, in the case of a gasket with a gasket annular rib diameter of 5 to 40 mm, the length of the substantially straight portion is preferably 1 to 6 mm, and more preferably 1.5 to 4.5 mm.
先端環状リブは、略直線部の最小径に対して0.1〜2.7%でシリンジ後端方向に直線状に拡径していることが好ましく、0.15〜2.5%で拡径していることがより好ましい。 The distal end annular rib is preferably 0.1 to 2.7% of the minimum diameter of the substantially straight portion and linearly expanded in the direction of the rear end of the syringe, and is expanded to 0.15 to 2.5%. More preferably, it has a diameter.
先端環状リブに位置するネジ上部には、先端環状リブの最大径部が内方向に撓むことにより、摺動抵抗値が低下するという理由で、空洞を設けることが好ましい。空洞の形状は特に限定されないが、ネジ部山径より小さい円柱状または環状に設けることができる。空洞は1つでも、複数設けても良い。図1(c)では空洞を1つ設けた態様を、図1(d)では空洞を環状に設けた態様を示す。 It is preferable to provide a cavity in the upper part of the screw located in the tip annular rib because the sliding resistance value is lowered by bending the maximum diameter portion of the tip annular rib inward. The shape of the cavity is not particularly limited, but can be provided in a columnar shape or an annular shape smaller than the thread crest diameter. One or more cavities may be provided. FIG. 1C shows an embodiment in which one cavity is provided, and FIG. 1D shows an embodiment in which the cavity is provided in an annular shape.
環状リブの圧縮率は、シリンジ内径に対して1〜5%が好ましく、2〜4%がより好ましい。1%未満では、液密性、気密性が劣り、5%を超えると、バレルへの打栓が困難となり、環状リブ表面のフィルムにシワが発生し液密性が劣る、又、摺動抵抗も高くなる傾向がある。 The compression rate of the annular rib is preferably 1 to 5% and more preferably 2 to 4% with respect to the syringe inner diameter. If it is less than 1%, the liquid tightness and air tightness are inferior. If it exceeds 5%, it is difficult to plug into the barrel, wrinkles occur on the film on the surface of the annular rib, resulting in poor liquid tightness, and sliding resistance. Tend to be higher.
成型に用いる不活性樹脂フィルムの厚さは、25〜150μmが好ましく、50〜100μmがより好ましい。25μm未満では、成型時のフィルム破れが多く発生する傾向があり、150μmを超えると、成型品の寸法安定性及びコストアップとなり経済的でなくなる傾向がある。 25-150 micrometers is preferable and, as for the thickness of the inactive resin film used for shaping | molding, 50-100 micrometers is more preferable. If the thickness is less than 25 μm, many film tears tend to occur at the time of molding, and if it exceeds 150 μm, the dimensional stability and cost of the molded product tend to increase, which tends to be uneconomical.
不活性樹脂フィルムを構成する樹脂としては特に限定されないが、良好な耐薬品性が得られるという点から、テトラフルオロエチレン・エチレン共重合体(ETFE)、ポリテトラフルオロエチレン(PTFE)、ポリクロロテトラフルオロエチレン(PCTFE)からなる群より選択される少なくとも1種のフッ素樹脂、及び/又はオレフィン系樹脂が好ましい。また、医療用容器の滅菌法として、蒸気滅菌、エチレンオキサイドガス滅菌、ガンマ線滅菌が行われるが、PTFEはガンマ線に対する耐性が低い。よって、ガンマ線滅菌に対する耐性が高いETFE、変性ETFE、PCTFEが特に好ましい。 Although it does not specifically limit as resin which comprises an inactive resin film, From the point that favorable chemical-resistance is acquired, tetrafluoroethylene-ethylene copolymer (ETFE), polytetrafluoroethylene (PTFE), polychlorotetra At least one fluororesin selected from the group consisting of fluoroethylene (PCTFE) and / or an olefin resin is preferred. Further, as a sterilization method for medical containers, steam sterilization, ethylene oxide gas sterilization, and gamma ray sterilization are performed, but PTFE has low resistance to gamma rays. Therefore, ETFE, modified ETFE, and PCTFE, which have high resistance to gamma sterilization, are particularly preferable.
ここで、ETFEとは、エチレンとテトラフルオロエチレンを30/70〜70/30のモル比で共重合したものであり、改質目的でさらに他の成分を共重合した変性ETFEがある。他の成分としては、フッ素含有オレフィンや炭化水素系オレフィンが挙げられる。具体的には、プロピレン、部点などのα−オレフィン、ヘキサフルオロプロピレン、フッ化ビニリデン、パーフルオロブチルエチレン、トリフルオロクロロエチレンなどの含フッ素オレフィン、エチレンビニルエーテル、パーフルオロメチルビニルエーテル、パーフルオロプロピルビニルエーテルなどのビニルエーテル類、含フッ素アクリレート類などがあり、2〜10モル%程度共重合されて、ETFEを改質する。 Here, ETFE is a copolymer of ethylene and tetrafluoroethylene in a molar ratio of 30/70 to 70/30, and there is a modified ETFE obtained by copolymerizing other components for the purpose of modification. Examples of other components include fluorine-containing olefins and hydrocarbon olefins. Specifically, propylene, α-olefin such as part point, hexafluoropropylene, vinylidene fluoride, perfluorobutylethylene, trifluorochloroethylene and other fluorinated olefins, ethylene vinyl ether, perfluoromethyl vinyl ether, perfluoropropyl vinyl ether There are vinyl ethers such as fluorinated acrylates and the like, and 2 to 10 mol% is copolymerized to modify ETFE.
変性ETFEとしては、接着性を付与する官能基を有するETFEを好適に使用することができ、該官能基としては、カルボキシル基、無水カルボキシル基、エポキシ基、水酸基、イソシアネート基、エステル基、アミド基、アルデヒド基、アミノ基、シアノ基、炭素−炭素二重結合、スルホン酸基、エーテル基などが挙げられる。また、変性ETFEの市販品としては、旭硝子(株)製のフルオンAH−2000などが挙げられる。 As the modified ETFE, ETFE having a functional group imparting adhesiveness can be suitably used. Examples of the functional group include a carboxyl group, an anhydrous carboxyl group, an epoxy group, a hydroxyl group, an isocyanate group, an ester group, and an amide group. Aldehyde group, amino group, cyano group, carbon-carbon double bond, sulfonic acid group, ether group and the like. Moreover, as a commercial item of modified ETFE, Asahi Glass Co., Ltd. full-on AH-2000 etc. are mentioned.
オレフィン系樹脂としては、ポリエチレン、エチレン−プロピレン共重合体、エチレン−プロピレン−非共役ジエン共重合体、エチレン−ブテン共重合体、エチレン−ヘキセン共重合体、エチレン−オクテン共重合体、エチレン−酢酸ビニル共重合体、エチレン−ビニルアルコール共重合体、エチレン−エチルアクリレート共重合体、塩素化ポリエチレン等のポリエチレン系樹脂、ポリプロピレン、プロピレン−エチレンランダム共重合体、プロピレン−エチレンブロック共重合体、塩素化ポリプロピレン等のポリプロピレン系樹脂、ポリブテン、ポリイソブチレン、ポリメチルペンテン、環状オレフィンの共重合体等が挙げられ、ポリエチレン(特に超高分子量ポリエチレン(UHMWPE))が好ましい。また、オレフィン系樹脂は、フッ素を含んでいてもよい。 Examples of the olefin resin include polyethylene, ethylene-propylene copolymer, ethylene-propylene-nonconjugated diene copolymer, ethylene-butene copolymer, ethylene-hexene copolymer, ethylene-octene copolymer, ethylene-acetic acid. Vinyl copolymers, ethylene-vinyl alcohol copolymers, ethylene-ethyl acrylate copolymers, polyethylene resins such as chlorinated polyethylene, polypropylene, propylene-ethylene random copolymers, propylene-ethylene block copolymers, chlorinated Examples thereof include polypropylene resins such as polypropylene, polybutene, polyisobutylene, polymethylpentene, and cyclic olefin copolymers, and polyethylene (particularly, ultrahigh molecular weight polyethylene (UHMWPE)) is preferable. The olefin resin may contain fluorine.
不活性フィルム115は、ゴム等との接着性を高める処理を行うことが好ましい。接着性を高める処理としては、化学処理法、フィルムの表面を粗面化する処理や、これらを組み合わせたものが挙げられ、具体例としては、ナトリウム処理、グロー放電処理、大気圧下又は真空下でのプラズマ処理(放電処理)、エキシマレーザー処理(放電処理)、イオンビーム処理が挙げられる。 The inert film 115 is preferably subjected to a treatment for improving the adhesion with rubber or the like. Examples of the treatment for improving the adhesion include chemical treatment, treatment for roughening the surface of the film, and combinations thereof. Specific examples include sodium treatment, glow discharge treatment, under atmospheric pressure or under vacuum. And plasma treatment (discharge treatment), excimer laser treatment (discharge treatment), and ion beam treatment.
ガスケット基材の弾性材料としては特に限定されず、例えば、天然ゴム、ブチルゴム、イソプレンゴム、ブタジエンゴム、スチレン−ブタジエンゴム、シリコーンゴム、エピクロルヒドリンゴム、エチレンプロピレンゴム、ニトリルゴムのような各種ゴム材料や、ポリウレタン系、ポリエステル系、ポリアミド系、オレフィン系、スチレン系等の各種熱可塑性エラストマーなどが挙げられる。これらの弾性材料は、単独でも複数の成分をブレンドして使用することもできる。なかでも、加硫により、弾性が得られる材料が好ましい。また、加硫材料の場合、硫黄などの加硫剤、加硫促進剤など、ゴム工業の公知の配合剤を適宜添加できる。 The elastic material of the gasket base material is not particularly limited, and examples thereof include various rubber materials such as natural rubber, butyl rubber, isoprene rubber, butadiene rubber, styrene-butadiene rubber, silicone rubber, epichlorohydrin rubber, ethylene propylene rubber, and nitrile rubber. And various thermoplastic elastomers such as polyurethane, polyester, polyamide, olefin, and styrene. These elastic materials can be used alone or by blending a plurality of components. Among these, a material that can obtain elasticity by vulcanization is preferable. In the case of a vulcanized material, a known compounding agent in the rubber industry such as a vulcanizing agent such as sulfur or a vulcanization accelerator can be appropriately added.
ガスケット基材のJ1S A硬さは特に限定されないが、50〜70度が好ましく、55〜65度がより好ましい。50度未満では、摺動時のガスケットの変形による漏れや、吸引時にプランジャーロッドがガスケットからはずれる場合がある。一方、70度を超えると、成型圧力を高くする必要があり、フィルムが破れ易く、脱型が困難になる傾向がある。
また、圧縮永久ひずみも特に限定されないが、20%以下が好ましく、15%以下がより好ましい。20%を超えると、打栓、滅菌及び保管中に環状リブが縮径して圧縮率不足となり、バレル内壁との液密性、気密性を保つことが出来なくなる傾向がある。
ここで、圧縮永久歪とは、25%圧縮、70±1℃、22時間の条件で測定したときの値である。
Although J1SA hardness of a gasket base material is not specifically limited, 50-70 degree | times is preferable and 55-65 degree | times is more preferable. If the angle is less than 50 degrees, leakage due to deformation of the gasket during sliding or the plunger rod may come off from the gasket during suction. On the other hand, when it exceeds 70 degrees, it is necessary to increase the molding pressure, the film is easily broken, and it tends to be difficult to remove the mold.
Further, the compression set is not particularly limited, but is preferably 20% or less, and more preferably 15% or less. If it exceeds 20%, the diameter of the annular rib is reduced during plugging, sterilization and storage, the compression rate becomes insufficient, and there is a tendency that liquid tightness and airtightness with the inner wall of the barrel cannot be maintained.
Here, the compression set is a value when measured under conditions of 25% compression, 70 ± 1 ° C., and 22 hours.
本発明のガスケットは、密封式混練機、オープンロール混練機などを用いて、所定配合比で配合材料を混練した混練物を、カレンダーまたはシート成型機で未加硫ゴムシートを作製し、次に、一定重量、サイズの未加硫ゴムシートと不活性フィルムを重ねて金型に置き、真空プレスで成型することにより、積層ガスケットの成型シートを得ることができる。 The gasket of the present invention is a kneaded product obtained by kneading compounded materials at a predetermined compounding ratio using a sealed kneader, an open roll kneader, etc., and producing an unvulcanized rubber sheet with a calendar or a sheet molding machine. A laminated gasket molded sheet can be obtained by stacking an unvulcanized rubber sheet of a constant weight and size and an inert film, placing them in a mold, and molding them with a vacuum press.
成型条件は特に限定されず、適宜設定すればよいが、成型温度は、好ましくは155〜200℃、より好ましくは165〜180℃であり、成型時間は、好ましくは1〜20分間、より好ましくは3〜15分間、さらに好ましくは5〜10分間である。 The molding conditions are not particularly limited and may be set as appropriate. The molding temperature is preferably 155 to 200 ° C, more preferably 165 to 180 ° C, and the molding time is preferably 1 to 20 minutes, more preferably 3 to 15 minutes, more preferably 5 to 10 minutes.
使用する金型は、褶動面形成部の鏡面仕上げにより、該当部のカットオフ値0.08mmで測定した算術平均粗さRaが0.03μm以下の平滑な金型表面が形成されていることが好ましい。このような金型を使用することによって、積層成型されたゴム部材は、元のフィルムの表面粗さより小さい成型品を得ることができる。Raは、好ましくは0.02μm以下、より好ましくは0.015μm以下である。なお、本発明において、算術平均粗さ(Ra)は、JIS B0601−2001に準拠して測定される。 The mold to be used has a smooth mold surface with an arithmetic average roughness Ra of 0.03 μm or less measured at a cutoff value of 0.08 mm of the corresponding part by mirror finishing of the sliding surface forming part. Is preferred. By using such a mold, the laminated rubber member can obtain a molded product smaller than the surface roughness of the original film. Ra is preferably 0.02 μm or less, more preferably 0.015 μm or less. In the present invention, the arithmetic average roughness (Ra) is measured according to JIS B0601-2001.
この後、ガスケットの成型品から不要部分を、切断・除去した後、洗浄、滅菌、乾燥および外観検査を行ってガスケットの完成品を得る。 Thereafter, unnecessary portions are cut and removed from the molded product of the gasket, and thereafter, cleaning, sterilization, drying, and appearance inspection are performed to obtain a finished product of the gasket.
以下、実施例に基づいて本発明を具体的に説明するが、本発明はこれらのみに限定されるものではない。 EXAMPLES Hereinafter, although this invention is demonstrated concretely based on an Example, this invention is not limited only to these.
実施例で使用したフッ素樹脂フィルムの内容を以下に示す。
不活性樹脂フィルム
変性PTFEスカイビング法フィルム:日本バルカー工業(株)製 商品名「ニューバルフロン」(フィルム厚さ70μm、中心線平均表面粗さ0.11μm)
ガスケット基材
塩素化ブチルゴム材質 (JIS A 硬さ58度)
The contents of the fluororesin film used in the examples are shown below.
Inert resin film modified PTFE skiving method film: Nippon Valqua Industries, Ltd. Trade name “New VALFLON” (film thickness 70 μm, centerline average surface roughness 0.11 μm)
Gasket base material chlorinated butyl rubber (JIS A Hardness 58 degrees)
実施例1〜3および比較例1〜2
塩素化ブチルゴム製未加硫ゴムシートに、PTFEフィルム(スカイビング法、厚さ70μ、片面接着処理)に未加硫ゴムシートを重ねて成型金型上に置き、真空プレスで175℃10分成型し加硫接着させた。得られたガスケット(5mL用COP樹脂シリンジ用、バレル内径12.45mm)を用いて以下の試験を行った。
Examples 1-3 and Comparative Examples 1-2
A non-vulcanized rubber sheet made of chlorinated butyl rubber, a PTFE film (skiving method, thickness 70μ, single-sided adhesive treatment) and an unvulcanized rubber sheet are placed on a molding die and molded at 175 ° C for 10 minutes using a vacuum press. Vulcanized and bonded. The following tests were conducted using the obtained gasket (for 5 mL COP resin syringe, barrel inner diameter 12.45 mm).
(シリンジ打栓性)
ガスケットネジ部に一定長さの冶具を嵌めた状態で、接液側を上にして置き、シリンジを真直ぐに挿入して打栓した。次にノズルより、メチレンブルーで着色した水5ml充填した後、15時間放置し、ガスケットの斜め打栓状況、及び先端環状リブのシワ発生状況を確認した。n=20として評価し、判定した。
先端環状リブのシワ発生状況は、接液面の斜め打栓状況を目視で確認し、先端環状リブ部を10倍に拡大して観察した。
○:斜め打栓、シワの発生が10%以下
△:斜め打栓、シワ発生率が10〜20%
×:斜め打栓又はシワ発生率20%以上
(Syringe plugging)
In a state where a fixed-length jig was fitted to the gasket thread portion, the wetted side was placed up, and the syringe was inserted straight and plugged. Next, 5 ml of methylene blue-colored water was filled from the nozzle, and then left for 15 hours to confirm the oblique plugging state of the gasket and the wrinkle generation state of the tip annular rib. Evaluation was made with n = 20.
As for the wrinkle generation state of the tip annular rib, the oblique plugging state of the wetted surface was visually confirmed, and the tip annular rib portion was observed by magnifying 10 times.
○: Diagonal plugging and wrinkle generation is 10% or less. Δ: Diagonal plugging and wrinkle generation rate is 10 to 20%.
X: Diagonal plugging or wrinkle incidence 20% or more
(摺動抵抗)
プランジャーロッド及び注射針23Gを装着し、オートグラフでスピード100mm/分で吐出した。n=10で測定し、評価した。
○:10N以下でノッキングせずにスムーズに摺動
△:15N以下で摺動
×:15N以上
(Sliding resistance)
A plunger rod and an injection needle 23G were attached, and the autograph was discharged at a speed of 100 mm / min. Measurements were made at n = 10 and evaluated.
○: Sliding smoothly without knocking at 10N or less Δ: Sliding at 15N or less ×: 15N or more
(液漏れ)
「滅菌済み注射筒基準」平成10年12月11日医薬発1079号厚生省医薬***長通知に準ずる。
5ml用ガスケットサンプル、ノズルキャップ、5ml用注射筒、プランジャーを準備する。ガスケットネジ部にネジより長い冶具を嵌めた状態で、接液面を上にして置き、シリンジを真直ぐに挿入して打栓した。次にノズルより、メチレンブルーで着色した水を公称容量目盛りの3/4の位置まで充填した。ノズルキャップ、プランジャーを取り付け、注射筒を下に向けてプランジャーに343Kpaの圧力を10秒間かける。n20で評価した。
10倍に拡大し、ガスケット谷部(先端環状リブと後端環状の谷部)への漏れを観察する。
○:漏れを認めない。
△:筋状の微小な漏れを認める。
×:明らかに漏れを認める。
(Liquid leak)
“Sterilized syringe standards”, according to the notification from the Pharmaceutical Safety Bureau of the Ministry of Health and Welfare No. 1079 on December 11, 1998.
Prepare a 5 ml gasket sample, nozzle cap, 5 ml syringe barrel and plunger. In a state where a jig longer than the screw was fitted to the gasket thread portion, the wetted surface was placed up, and the syringe was inserted straight and plugged. Next, the nozzle was filled with water colored with methylene blue to a position of 3/4 of the nominal volume scale. A nozzle cap and a plunger are attached, and a pressure of 343 Kpa is applied to the plunger for 10 seconds with the syringe barrel facing downward. Evaluation was made at n20.
Magnify 10 times and observe leakage to gasket valleys (tip annular rib and rear end annular valley).
○: No leakage is recognized.
(Triangle | delta): A streaky minute leak is recognized.
X: Leakage is clearly recognized.
評価結果を表1に示す。
従来のガスケットである比較例1および2のガスケットでは、特に打栓性に問題があり、その結果、摺動性と液漏れに影響を及ぼしている。一方、本発明のガスケットでは、先端環状リブの摺接部断面が略直線状であり、該直線部の長さがガスケット全長に対して、10〜55%であり、該直線部の最小径に対して0.1〜2.7%の範囲でシリンジ後端方向に直線状に拡径しているため、実施例1〜3に示されるように、ガスケット打栓性、摺動抵抗、液漏れのいずれにおいても優れていた。 In the gaskets of Comparative Examples 1 and 2 which are conventional gaskets, there is a problem particularly in the plugging property, and as a result, the sliding property and the liquid leakage are affected. On the other hand, in the gasket of the present invention, the sliding contact section of the tip annular rib is substantially straight, and the length of the straight portion is 10 to 55% of the total length of the gasket. On the other hand, since the diameter is linearly expanded in the direction of the rear end of the syringe in the range of 0.1 to 2.7%, as shown in Examples 1 to 3, gasket plugging property, sliding resistance, liquid leakage Both were excellent.
1 先端環状リブ
2 環状リブ
3 空洞
L 摺動側面部の長さ
l 先端環状リブ摺接部の長さ
1 End
Claims (7)
先端環状リブの摺接部断面が略直線状であり、該直線部の長さが摺動側面部長さに対して10〜55%であり、該直線部の最小径に対して0.1〜2.7%の範囲でシリンジ後端方向に直線状に拡径していることを特徴とする不活性樹脂フィルムで積層されたガスケット。 A gasket having a plurality of annular ribs in sliding contact with the inner wall of the syringe,
The cross section of the sliding contact portion of the tip annular rib is substantially linear, the length of the straight portion is 10 to 55% with respect to the sliding side surface length, and 0.1 to the minimum diameter of the straight portion. A gasket laminated with an inert resin film, wherein the diameter is linearly expanded toward the rear end of the syringe within a range of 2.7%.
The gasket according to any one of claims 1 to 6, wherein the material of the gasket base material is butyl rubber or thermoplastic elastomer, the J1SA hardness is 50 to 70 degrees, and the compression set is 20% or less.
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WO2015049972A1 (en) * | 2013-10-02 | 2015-04-09 | 住友ゴム工業株式会社 | Gasket for pre-filled syringe |
JP2015146871A (en) * | 2014-02-05 | 2015-08-20 | 住友ゴム工業株式会社 | Syringe for medical treatment, gasket applied to syringe and manufacturing method of gasket |
EP2957310A1 (en) * | 2014-06-18 | 2015-12-23 | Sumitomo Rubber Industries, Ltd. | Gasket to be used for medical syringe, and medical syringe |
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JP2016132767A (en) * | 2015-01-22 | 2016-07-25 | 三菱電線工業株式会社 | Manufacturing method of rubber product |
JP2022002738A (en) * | 2013-10-28 | 2022-01-11 | ベクトン・ディキンソン・アンド・カンパニーBecton, Dickinson And Company | Leak-free stopper for syringe assembly having low breakloose and sustaining forces |
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