JP2001198189A - Plug body for transfusion - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a plug body with improved sealing performance and collapse resistance and to provide a plug body for transfusion requiring no special process in manufacturing the plug body and a membrane required in the conventional structure, with a low manufacturing cost. SOLUTION: The plug body is formed of a rubber plug and a plastic support body with the rubber plug fitted in its inside and having no membrane. The plug body for the transfusion is so formed that both sides of a part or the whole of the rubber plug surface are laminated with a fluororesin film with its both sides surface-treated and a contact part between the rubber plug and the plastic support body is substantially closely stuck together.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a plug for infusion, and more particularly, to a plug for infusion which has sufficient performance in practical use and is particularly excellent in safety and economy.

[0002]

2. Description of the Prior Art A plug for infusion is generally a cylindrical rubber stopper 10 which has a self-sealing function at the time of infusion and after a needle is inserted, as shown in a sectional view of FIG. And a plastic support 11 serving to connect with the backing bag.

In these plugs, simply a rubber plug 1 is used.
A plastic support having a plastic diaphragm 12 in order to improve the safety of the contact surface of the bag with the drug, in addition to a plug consisting of the plastic support 11 and the plastic support 11 (Japanese Patent Application Laid-Open No. 61-232851). Gazette). Further, there is a method in which a rubber stopper is laminated with a plastic film which can be thermally fused with a plastic support, and then fitted and fused with the plastic support to produce a stopper (Japanese Patent No. 02582134).

[0004] Social demands on the safety of drugs and medical devices are increasing day by day, and even in medical rubber stoppers, in order to avoid direct contact between the drug and the rubber stopper, a more hygienic plastic material than a rubber stopper material is used. A diaphragm is required. As a material for a diaphragm of a medical rubber stopper, a fluororesin film that is chemically most stable and has been used in the medical field has been tried in the past. On the other hand, the diaphragm in the plug forms a part of the plastic support as shown in FIG. 6, and is formed as a single piece when the plastic support is formed. Usually, a polyolefin resin is used for the plastic support, and a polyolefin resin is used for the diaphragm, and the diaphragm is also composed of the polyolefin resin. When the medicine is taken out by the syringe with the stopper having such a diaphragm structure, the medicine remains in the space between the diaphragm 12 and the rubber stopper 10, which may further cause contamination.

On the other hand, in a method of manufacturing a plug by laminating a rubber plug with a plastic film, a PE or PP polyolefin resin is generally used as a plastic support for the plug. For example, in Japanese Patent No. 02582134, a polyolefin-based resin film is used as a laminate film of a rubber stopper in order to improve thermal fusion with a plastic support. In general, a laminated rubber stopper is manufactured by disposing a plastic film on an upper surface and / or a lower surface of an unvulcanized rubber sheet and laminating the rubber in a mold simultaneously with vulcanization of the rubber. Here, the vulcanization of rubber varies depending on the material, but is usually 140 to 1
A condition of about 10 minutes at a temperature of 80 ° C. is generally used. However, since the softening point and melting point of the polyolefin-based film are lower than the rubber vulcanization temperature, the plastic film softens during vulcanization, and there is a problem that desirable vulcanization conditions cannot be adopted in order to form a homogeneous laminate.
In order to solve this problem, (i) the vulcanization temperature of the rubber stopper is lowered. (Ii) A vulcanized molded sheet is produced from an unvulcanized rubber sheet, and a laminate with a polyolefin film is produced again. (Iii) The production of a laminated sheet using a calender roll of an unvulcanized rubber sheet and a polyolefin film may be employed, but the cost increase factor is large due to the manufacturing process, the defective rate and the like.

For example, lowering the vulcanization temperature is economically disadvantageous, such as increasing the amount of a vulcanizing agent and vulcanization aid or extending the vulcanization time. Cannot be achieved, and a rubber stopper with good properties cannot be obtained.

Therefore, it is necessary to prepare a rubber plug-molded sheet from an unvulcanized sheet under ordinary vulcanization conditions, and to again laminate the polyolefin film at a temperature lower than the rubber vulcanization conditions. In addition, in order to eliminate the problem of deformation and melting of the polyolefin film due to the temperature of the rubber vulcanizing mold, there is a method of producing a sheet in which an unvulcanized rubber sheet and a polyolefin film are sufficiently laminated in advance and vulcanizing the sheet. Requires a step of producing a laminate sheet. Nevertheless, there are basic problems such as perforation and tearing of the laminated film due to partial melting of the film caused by vulcanization at the same or higher temperature as the softening point and melting point of the polyolefin film.

[0008]

SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problems, and has a needle piercing property, a re-sealing property, a coring property, etc. which are basic characteristics of a rubber stopper itself. Provided is a plug having improved sealing and depressing resistance as a plug by improving adhesion and adhesion of a support. In particular, all fluorine-based resins have a melting point of 200 ° C. or higher, and melt at a normal rubber vulcanization temperature.
Does not soften. Therefore, there is provided a plug for infusion, which does not require a special step in manufacturing a plug of a laminated rubber plug made of a fluororesin film and does not require a diaphragm in a conventional structure, and which has a low production cost.

[0009]

According to the present invention, there is provided a plug comprising a rubber plug and a plastic support without a diaphragm in which the rubber plug is inserted. This is a transfusion plug which is laminated with a surface-treated fluororesin film, and in which the rubber plug and the plastic support joint portion are substantially adhered.

Here, the fluororesin film is made of polytetrafluoroethylene, tetrafluoroethylene / ethylene copolymer, tetrafluoroethylene / perfluoroalkylvinyl ether copolymer, chlorotrifluoroethylene / ethylene copolymer, polychlorotrifluoro. It is a film of ethylene, polyvinyl fluoride, or the like.

As a method for treating the surface of the film, corona discharge, glow discharge and arc discharge are used.

[0012]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS As shown in the sectional view of FIG. 1, a plug for infusion according to the present invention comprises a cylindrical rubber plug 3 and a plastic support 4 into which the rubber plug 3 is fitted. Be composed. Here, it is preferable that concave portions 3a are formed on both sides of the central portion of the rubber stopper 3 so that the injection needle can be easily inserted. And the plastic support 4 is a rubber stopper 3
And a pair of upper and lower inner flanges 4a, 4b for holding the infusion and an outer flange 4c for connecting to the infusion bag, and more preferably, a rubber stopper is provided on one side of the flange in contact with the rubber stopper. A projection 7 for preventing detachment is formed.

The rubber stopper of the present invention is partially or entirely laminated with a film of a fluororesin whose both surfaces are surface-treated in order to make the bonding with the plastic support adherent. . Although FIG. 1 shows that the laminated film 8 is laminated on the entire surface of both sides of the rubber stopper 3, as shown in FIG. 2, one side can be laminated only on the side in contact with the medicine.

The fluororesin used in the present invention is, for example, polytetrafluoroethylene (PTFE), tetrafluoroethylene / perfluoroalkylvinyl ether copolymer (PFA), tetrafluoroethylene / hexafluoropropylene copolymer (FEP) , Tetrafluoroethylene / ethylene copolymer (ETFE), polychlorotrifluoroethylene (PCTFE), chlorotrifluoroethylene / ethylene copolymer (ECTFE),
There are polyvinylidene fluoride (PVDF), polyvinyl fluoride (PVF) and the like.

The surface of the fluororesin film can be treated by a conventional technique, for example, by corona discharge, glow discharge or arc discharge. The thickness of the film is preferably in the range of 10 to 500 μm.

The surface-treated film is laminated on the unvulcanized rubber plug composition sheet, and is subjected to normal vulcanization conditions, for example, a temperature of 140 ° C. to 180 ° C. and a pressure of 3 to 15 MPa.
Vulcanization is carried out simultaneously with molding by a vacuum press under the conditions of 5 to 30 minutes to produce a rubber stopper laminated with a film.
The molded laminated rubber stopper is fitted so that the rubber stopper 3 is in close contact with the plastic support 4 as shown in FIG.

Next, as the rubber component used for the rubber stopper in the present invention, isoprene rubber, butadiene rubber, styrene-butadiene rubber, butyl rubber, ethylene-propylene rubber, ethylene-propylene-diene rubber, acrylonitrilo rubber and the like are used alone or in combination. These are used as a mixture.
Here, as the rubber component, it is preferable to use a diene rubber, particularly butadiene rubber or isoprene rubber as a main component.

A styrene-conjugated diene block copolymer elastomer or a hydrogenated styrene-conjugated diene block copolymer elastomer with respect to the rubber component;
Furthermore, modified such as epoxidation and carboxylation,
These block copolymer elastomers can be appropriately blended.

In the present invention, a vulcanizing agent, a vulcanization accelerator, an inorganic filler such as calcined clay, silica, metal oxide and carbon black, oil and the like can be appropriately blended into the rubber stopper composition.

As the material of the support used in the present invention, various plastic materials can be used, and a polyolefin resin is particularly preferably used. Here, as the polyolefin resin, for example, polyethylene, polypropylene, ethylene-propylene copolymer, α-olefin, acrylic acid, methacrylic acid, esters thereof, modified polyethylene with a copolymer such as vinyl acetate,
Alternatively, there is an ionomer which is a crosslinked product of a metal salt of a copolymer of ethylene and an unsaturated carboxylic acid.

In the present invention, various methods can be adopted for assembling the laminated rubber stopper and the plastic support.

For example, as shown in FIGS. 2 and 3, a vulcanized and molded rubber plug 3 fitted to a separately injected first support 5 is set in a mold, and the first support 5 is Is a method of insert-molding a separate second support member 6, or assembling the rubber stopper 3, the first support member 5 and the second support member 6, which are separately formed, and integrating them by heat fusion or ultrasonic fusion. Can be adopted. When the second support 6 is manufactured by insert molding, a rubber stopper set in a mold or a plastic material of the second support 6 in a molten state in the first support is injected and filled into a mold cavity. Therefore, the adhesiveness between the first support 5 and the rubber plug 3 is improved, and a plug that is sufficiently tightly integrated without any gap can be obtained.

Further, as another method of assembling the plug body of the present invention, in the structure shown in FIG. 4, a support 8 previously formed by injection molding is laminated with a film 8 vulcanized by vacuum pressing. In the structure shown in FIG. 5, there is a method of setting the vulcanized laminated rubber plug 3 in a mold and injecting and designing the support 2. .

[0024]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Manufacture of rubber stopper The composition shown in Table 1 was used as the basic composition of the rubber stopper composition used in the examples and comparative examples. As the rubber composition, two types of isoprene rubber compounding (IR compounding) and butadiene rubber compounding (BR compounding) were used.

A 50 μm-thick fluororesin film having both surfaces treated as a laminate film is laminated on both sides of a rubber sheet of the above rubber composition or on one side in contact with a drug, and is heated and pressed under vacuum to vulcanize. A laminated rubber stopper was obtained simultaneously with the molding. The materials of the used films are as follows.

(1) ETFE (tetrafluoroethylene / ethylene copolymer) Trade name: Aflex LM (Asahi Glass) (2) PFA (tetrafluoroethylene / perfluoroalkylvinyl ether copolymer) Trade name: Aflex PFA ( Asahi Glass) 2. 1. Molding of Support and Manufacture of Plug The first support 5 and the second support 5 of the plastic support 4 shown in FIG.
The supports 6 are separately injection molded. The laminated rubber plug 3 was combined with the first support 5 and the second support 6 as shown in FIG. 1, and the whole was integrated by an ultrasonic welding method to produce a plug. Here, the resin material used for the support is as follows.

(1) PE (polyethylene): Evatate D3021 (Sumitomo Chemical Co., Ltd.) (2) PP (polypropylene): Sumitomo Noprene W
531 (Sumitomo Chemical Co., Ltd.) The specifications of the plug manufactured by the above method are as follows. (I) Rubber stopper Diameter 25mmφ Thickness 5mm Central diameter Maximum diameter 5mmφ Minimum diameter 2mmφ Depth 1mm conical depression (ii) First support outer cylinder Bottom Maximum diameter (L ₁ ) 28.2mmφ Minimum diameter (L ₂ ) Within 19mmφ Tube diameter 25mmφ Side cylinder thickness Maximum part 1.4mm Minimum part 0.7mm Bottom part 0.8mm Cylindrical height (H) 10.8mm (iii) Second support body cylinder Top part maximum diameter (L ₃ ) 35mmφ Minimum diameter ( L ₄₎ 19
mmφ Inner cylinder diameter 25mmφ Side cylinder thickness 0.7mm Top part thickness 0.8mm Tube height 8.3mm 3. Performance evaluation of the plug The characteristic evaluation of the plug manufactured as described above was performed by the following method.

(1) Sealing As a method of evaluating the sealing (airtightness) of the plug, the plug is fused to a soft bag filled with a chemical solution, and the bag is hung with 1500 ml of pure water put in the bag. It was evaluated by checking the presence or absence of liquid leakage to the surface of the rubber stopper after 24 hours. A sample with no liquid leakage was rated as ○, and a sample with liquid leakage was rated as x.

(2) Depression resistance The evaluation is made by measuring the maximum load when the rubber is depressed from the plastic support when pressed with a stainless needle (tip diameter 2 mm) into the center recess of the rubber plug of the plug. Was. When the load at the time of the depression is 98 N or more, the result is evaluated as ○, and when the load is less than 98 N, the result is evaluated as ×.

(3) Resealability Under the same condition as the evaluation of the sealability, a plastic needle (manufactured by IS6AI Nipro) of the infusion set is inserted into the center of the rubber stopper of the stopper attached to the vial containing the sample. After leaving for 1 hour, the needle was pulled out, and then the state of liquid leakage was observed for 10 minutes. A sample with no liquid leakage was rated as ○, and a sample with liquid leakage was rated as ×.

(4) Needle piercing property A test needle (infusion set 2) is inserted into the central hollow of the rubber stopper of the stopper.
The maximum load when piercing a 00 type plastic needle (manufactured by JMS) was measured. In this evaluation method, 98N or less was evaluated as ○, and 9
Those exceeding 8N were rated as x.

(5) Coring property A rubber stopper is vertically stabbed five times with an injection needle (JMS 18G) in the same condition as the evaluation of the sealing property. Thereafter, the pure water in the soft bag is filtered by a membrane filter. Check for the presence of debris rubber on the filter. The case where there is no or very small fragment rubber is marked as “○”. When the presence of more than that was recognized, it was evaluated as x.

(6) Japanese Pharmacopoeia test A rubber stopper obtained by molding with a vacuum press was heated at 121 ° C. for 3 hours.
Hot water treatment for 0 minutes, followed by drying. Using this, the evaluation was carried out in accordance with the dissolution test of the Japanese Pharmacopoeia 13th Edition "Rubber stopper test method for infusion". Those that matched were marked with ○, and those that were not matched were marked with x.

[0034]

[Table 1]

[0035]

[Table 2]

From the evaluation results shown in Table 2, Examples 1 to 6 using a laminated film of ETFE and PFA having both surfaces treated with a special corona were more sealed than Comparative Examples 1 and 2 using a laminated film without both surfaces. It is clear that the properties and the sinking resistance are improved.

The embodiments disclosed this time are to be considered in all respects as illustrative and not restrictive. The scope of the present invention is defined by the terms of the claims, rather than the description above, and is intended to include any modifications within the scope and meaning equivalent to the terms of the claims.

[0038]

The plug of the present invention has excellent properties such as resealability and needle sticking properties, which are basic properties of the plug, because at least a part of the rubber plug is laminated with a fluororesin film treated on both sides. The adhesion and integration of the stopper and the support are improved, and as a result, a manufacturing process that avoids contamination and high cost by the rubber stopper can be realized. Further, it is possible to obtain a plug having high sealing properties and safety.

[Brief description of the drawings]

FIG. 1 is a cross-sectional view showing an example of an infusion plug according to the present invention.

FIG. 2 is a cross-sectional view showing an example of a transfusion plug according to the present invention.

FIG. 3 is a cross-sectional view showing an example of a transfusion plug according to the present invention.

FIG. 4 is a cross-sectional view showing an example of a transfusion plug according to the present invention.

FIG. 5 is a cross-sectional view showing an example of a transfusion plug according to the present invention.

FIG. 6 is a cross-sectional view of a conventional plug for infusion.

[Explanation of symbols]

1 stopper, 2,4 support, 3 rubber stopper, 5 first support, 6 second support, 8 film.

Claims (3)

[Claims] 1. A fluororesin comprising a rubber plug and a plastic support without a diaphragm in which the rubber plug is fitted, wherein a part or all of the surface of the rubber plug is surface-treated on both surfaces. Laminated with a film of
A transfusion plug having a rubber stopper and a plastic support joint portion substantially adhered to each other. 2. The fluororesin film is made of polytetrafluoroethylene, tetrafluoroethylene / ethylene copolymer, tetrafluoroethylene / perfluoroalkylvinyl ether copolymer, chlorotrifluoroethylene / ethylene copolymer, polychlorotrifluoro. 2. The plug for infusion according to claim 1, which is a film of ethylene or polyvinyl fluoride. 3. The plug for infusion according to claim 1, wherein the surface treatment is performed by corona discharge, glow discharge, or arc discharge.