JPS6194657A - Rubber cock for vial - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

TECHNICAL FIELD The present invention relates to a rubber stopper for a vial, and more particularly to a rubber stopper for a vial that has a protective film with excellent chemical resistance on the portion of the rubber stopper that contacts the opening of the vial.

Prior Art Conventionally, a rubber stopper 21 for a vial, as shown in FIG.
A rubber stopper main body 2 including a leg portion 22b that fits into the vial opening and a flange portion 22a that contacts the upper surface of the vial opening.
2; and a protective film 23 having excellent chemical resistance, which is coated on the lower surface of the flange portion 22a and on the outer surface of the leg portion 22b and the portion 22c that contacts the vial opening. The above-mentioned protective film 23 prevents compounding agents and impurities contained in the rubber stopper 21 from being eluted into the medicinal pond in the vial 24, and conversely, components in the medicinal solution are sucked into the rubber stopper 21, causing the chemical components to be dissolved. This prevents the stability of the drug from being impaired by preventing the content from decreasing or from changing the liquid properties.

'' Comb stoppers for bipedal vials include small ones with a diameter of 13 mm on the top of the rubber stopper, medium-sized ones with a diameter of about 20 years old, and comb stoppers with a diameter of 25 to 4011111 used for infusions, etc.
There are large ones, about 1 in size. Among these, large rubber stoppers generally have longer legs than small and medium-sized rubber stoppers, so during the manufacture of comb stoppers, the protective film at the part that contacts the inner surface of the Hyal mouth part becomes white, causing cracks in the surface layer. When the cap is closed, a whisker-like hangnail may occur, causing the cap to fall into the drug in the vial.
There is a concern that it may enter the body and become an insoluble foreign substance.

The present inventors investigated conventional rubber stopper manufacturing methods in order to solve this problem with large rubber stoppers.

Conventionally, the above-mentioned comb plug has been made in two ways using the following two methods.

One method is shown in FIG. With this method,
First, a 7-carbon based resin sheet 2 is placed on the surface of the lower mold 27 where the molding recesses 27a for the legs of the rubber stopper 21 are provided.
6 and an unvulcanized rubber sheet 25 (FIG. 6(a)), and then heated and pressurized with an upper mold 33 at normal temperature and pressure to form a resin layer 26 on the lower surface. A primary molded body 34 covered with rubber material 25 on the upper surface is press-molded (FIG. 6(b)). Next, such a primary molded body 34
is passed through a canting device and canted at a predetermined location to form a large molded rubber stopper 35 (FIG. 6(C)). Then,
A layer of unvulcanized rubber sheet 29 is placed on the upper surface of the primary rubber stopper 35 fitted into the lower mold 27 as shown in FIG. 6(d).
), heated with the upper mold 28 at normal temperature and pressure,
Pressure is applied to press-form the rubber stopper 21 (Fig. 6(e)).
).

On the other hand, one method of ponding is shown in FIG.

In this method, first, a fluorine-based O (fat sheet) is preformed to match the shape of the leg of the rubber stopper main tree 22, and then the lower mold 30
(Fig. 7(a))
. Next, a protective film 23 formed by molding the above January fat sheet
Place the unvulcanized rubber sheet 31 on top of the
), the rubber stopper 21 is press-molded by heating and pressurizing the upper mold 32 and the lower mold 3°.

By the way, when we carefully examine each of the above methods, we find that in any of the above methods for manufacturing rubber plugs, the above Resin-123 is
When molded into a specific shape, it is stretched as if sheared by the lower mold, and in addition, the conventionally used Due to its poor elongation properties, especially for large rubber stoppers with long legs, the protective film on the outer circumferential surface of the leg becomes thinner than the pond area, resulting in a decrease in strength and contact with the inner circumference of the vial opening, resulting in hair-like hangnails. It turned out to be easy.

OBJECTS OF THE INVENTION Accordingly, an object of the present invention is to improve the shape and dimensions of a rubber stopper, first of all, the shape of the connecting portion between the legs of the rubber stopper body and the lower surface of the flange, and the shape of the outer peripheral corner of the lower end of the legs, and to improve the elongation characteristics. By finding a protective film material with good elasticity, and by finding an appropriate elongation rate for the protective film (Δ The goal is to prevent hair-like hangnails from forming on the skin.

Structure of the Invention In order to achieve the above object, the present inventors have repeatedly conducted experiments and have found that the following is a prerequisite.

■For large rubber stoppers, in order to ensure that the legs of the rubber stopper are inserted into the vial opening when the automatic stopper is used to close the opening of the vial, it is necessary to attach a certain axis to the leg. A direction length dimension is required, and this minimum length dimension is 311
It is said to be about 1111.

The thickness of the protective film formed on the 0 leg portion must be at least 15 μII+ in order to prevent whisker-like hangnails from occurring.

The inventors of the present invention took these points into consideration when determining the axial length, shape, etc. of the legs. A detailed explanation will be given below according to FIGS. 1 to 5.

The rubber stopper 4 according to the present invention consists of a rubber stopper body 1 and a protective film 2, as shown in FIG.

The rubber stopper main body 1 integrally includes a cylindrical leg portion 1b that fits into the mouth portion 3a of the vial 3, and a flange portion 1a whose lower surface is in contact with the mouth portion upper surface 3b of the vial 3. The rubber plug body 1 is coated with a protective film 2 made of ethylene-tetrafluoroethylene copolymer resin on the periphery of the lower leg of the flange and on the outer surface of the leg b, thereby forming the rubber plug 4. .

The rubber stopper body 1 is made of an elastic material such as natural rubber or synthetic rubber such as bunal rubber. In FIG. 2, the diameter W of the upper surface of this rubber stopper body 1 is 25 to 4
It should be about 0 mm. The axial length of the leg portion 1b of the rubber stopper body 1 is 3 to 8tIIIfi. The outer peripheral surface of the leg portion 1b is a concave curved peripheral surface 1 connected to the lower surface of the flange portion 1a.
c, a convex curved circumferential surface 1d connected to the lower leg surface 1g, and a portion outer surface 1 connecting the Nissin circumferential surface 1c and the convex curved curved surface 1d.
This peripheral wall surface 1" is in close contact with the inner peripheral surface of the vial opening during capping. The radius of curvature R1 of the concave curved peripheral surface 1c connected to the lower surface of the flange portion 1a is 0.5+am or more, preferably l , (1m+a or more. Hota,
Radius of curvature R2 of the convex curved peripheral surface 1d connected to the lower leg surface 1ε
is 0, 5111111 or more, preferably ], 5+
It shall be n+n or more.

In addition, the protective film 2 has an elongation rate with respect to A (the fat sheet (in the conventional example, the note indicated by 26 in FIG. 6(a)), that is, the concave curved peripheral surface 1c and the lower surface of the flange. The distance from the contact point A to the contact point B between the lower end surface 1g of the leg and the convex curved circumferential surface 1d is the sum of the two radii of curvature (R1 + Rz)
[=? The elongation rate divided by r=] is 3.5 or less, preferably 3 or less.

Here, rl represents the distance from the center of the rubber stopper to point A, and r2 represents the distance from the center of the rubber stopper to point B. More specifically, tj (the thickness of the fat sheet is 50 to 15
The thickness of the protective film 2 shall be 15 μm or more.

The rubber stopper according to the present invention is manufactured by conventional press molding as shown in FIG. 6.7.

In addition, as shown in FIG. 13, the present invention forms an annular projection 1e on the lower surface of the flange portion 1a of the rubber stopper body 1, and
may be brought into close contact with the vial opening 3a and upper surface 3b, and furthermore, as shown in FIG. good.

Effects and Effects of the Invention According to the above configuration, the material of the protective film is ethylene-↓fluorinated ethylene/copolymer resin, so the protective film has excellent chemical resistance compared to the conventional example. Above, 58! It has good elongation properties at high temperatures during the coating process, and therefore has the advantage of being resistant to tearing, without causing pinholes when coating the legs.

In addition, the outer peripheral surface of the leg was configured to include a curved peripheral surface connected to the lower surface of the flange and a convex curved surface connected to the lower surface of the leg. The whole body can be stretched uniformly and smoothly without any localized shear stretching phenomenon, and the axial length of the leg can be suppressed to 8111 m or less, and the elongation rate of the protective film with respect to the resin notebook can be kept at 3. Since it is suppressed to 5 or less, the protective film is given appropriate elongation I), and therefore, the generation of whisker-like hangnails on the protective film is effectively prevented.

S1 +j+ fat sheet with thickness dimension 100μm, (R, +R2
) is 1.0+1. o=2.0+o+n rubber stopper body (
Sample (a)), 1. (1+1.5"2.5mm rubber stopper body (sample (b)) and I, 5+1.5-'3.Omm
When forming a protective film by press molding on each rubber stopper body (sample (C)), the axial length of the leg is 4, S
, 6, 7, 8, 9, and 1011 m, whisker-like hangnails occur when the elongation rate ε of each protective film and the four operations of plugging, uncorking, plugging, and uncorking are performed. I did an experiment on whether or not it was possible. The results are shown in Table 1.

In Table 1, the - mark means that the occurrence of whisker-like hangnails is not observed, and the + mark means that the occurrence of whisker-like hangnails is observed.6 From the above results, the sample (R1+R+)=2.0m+n (
), the axial length of the leg IJ14~5■, 1
When the application rate ξ is 2.6 to 3.1, b, (R, +821
= 2, 5 + nh+ sample (1)), the axial length of the leg is 4 to 71 planes, and the elongation rate ε is 2.2 to 71 planes.
3. - When ↓, and (R1 + R2) = 3.0 sample (ci, when the axial length of the leg is 4-81 cotton and the elongation E is 1.9-3.3) , it can be seen that sink-like hangnails do not occur in each case.Therefore, the elongation rate ε
It can be seen that the occurrence of whisker-like hangnails can be effectively prevented if the size is set to 3.5 or less and the dimension is set to 8cm or less.

[Brief explanation of the drawing]

Figures 1 and 2 are a schematic cross-sectional view of the rubber plug according to the present invention and a cross-sectional explanatory view of the main part of the rubber plug body, and Figures 3 and 4 are respectively the first and second cross-sectional views.
A schematic sectional view showing a modification of the figure, FIG. 5 is a sectional view of a conventional rubber stopper, FIGS. 6(,) to (e), and FIG. 7(a),
(b) is an explanatory diagram showing a conventional rubber plug forming method. 1...Rubber stopper body, 1a...flange part, 1b...
・Leg δ inhibition 1c... Nissin curved circumferential surface, ]d... Convex curved circumferential surface, 2... Hold! Membrane, 3... Vial, 4... Rubber stopper. Figure 2 Figure 5 Figure 7 (a)

Claims (1)

[Claims] (1) A rubber stopper body comprising a cylindrical leg that fits into the mouth of the vial and a flange that contacts the upper surface of the mouth of the vial; the entire lower surface of the flange or the area around the leg on the lower surface of the flange. and a protective film made of ethylene-tetrafluoroethylene copolymer resin that covers the outer surface of the leg; and the protective film is coated on the rubber stopper body by press molding a resin sheet. In the rubber stopper for a vial, the outer circumferential surface of the leg has a concave curved circumferential surface connected to the lower surface of the flange, a convex curved circumferential surface connected to the leg lower surface, and the concave curved circumferential surface and the convex curved circumferential surface. A rubber stopper for a vial, characterized in that it consists of an outer surface of a cylinder connected to a peripheral surface, and satisfies the following conditions [1] and [2]. [1] Axial length L of the leg; 8 mm or less [2]
Elongation rate ε of the protective film: 3.5 or less, provided that the elongation rate ε of the protective film is expressed by the following formula. ε=■■/(R_1+R_2) Here, R_1; radius of curvature of the concave curved circumferential surface; R_2;
The radius of curvature of the convex curved circumferential surface, ■■; The radius of curvature R_1
The distance from the point of contact A between the concavely curved circumferential surface and the lower surface of the flange to the point of contact B between the lower end surface of the leg and the convexly curved circumferential surface with the radius of curvature R_2.