EP3384219B1 - Stopper for a container for use in freeze-drying - Google Patents

Description

The invention relates to a stopper for a container for use in freeze drying, also referred to as lyophilization. In a method for producing a freeze-dried product, as is often used in the field of medical diagnostics, chemical analysis, the food and / or pharmaceutical industry, for example to produce diagnostics and / or pharmaceuticals, a solution with appropriate ingredients is first produced and this solution then dried in a freeze dryer. The solvent used to prepare the solution is typically water and the solution is accordingly an aqueous solution. In principle, other solvents or their mixtures with aqueous systems can also be used, for example an alcohol, in particular ethanol, or an organic solvent. The solution is usually first filled into a container, for example a glass cuvette or glass bottle, for the purpose of freeze-drying. In order to prevent contamination of the solution or the interior of the container during the freeze-drying process and / or after the freeze-drying, Usually a stopper is inserted into the container in order to partially or completely close it for the purpose of freeze-drying or after the freeze-drying.

The stopper is designed in such a way that gas exchange between the interior of the container and the environment is possible during the freeze-drying process. This can be achieved, for example, in that in a drying position the stopper is only partially inserted into the container during the freeze-drying process, and thus the container is not yet tightly closed. In this way, the solvent, in particular water, can be removed from the solution during the freeze-drying process in order to dry the ingredients of the solution. Following the freeze-drying process, the stopper is typically pushed further into the container with the aid of a device embodied in the freeze-drying system, so that the stopper is in the sealing position in which the stopper closes the container in a fluid-tight manner. The term “fluid” is used below as a common term for gases and for liquids. The term "fluid-tight" is accordingly understood to mean that in the sealing position, penetration of gases and / or liquids, in particular water vapor or oxygen, into the interior of the container and escape of substances from the interior of the container is prevented. Often a safety lock is attached to the container afterwards to secure the stopper. This safety lock can be, for example, a crimp cap or a screw lock. Such plugs are usually made in one piece.

A one-piece stopper for use in a freeze-drying process is for example from the document DE 20 2011 050 413 U1 known. The piston plug has a top and a bottom, the bottom facing the top in an axial direction. In the area of the underside, the piston stopper has at least one outwardly open recess for gas exchange during freeze-drying, which recess is open in an axial direction downwards and in a radial direction.

From the U.S. 4,306,357 A is a cap assembly for a vessel for freeze drying known, wherein the cap arrangement has a one-piece sealing plug for insertion into an opening of a vessel for freeze drying, the plug being formed with ribs on its shaft, so that in a drying position of the plug when a cap flange is at a distance from a vessel flange, the Ribs with an inner surface of the flange of the vessel form ventilation channels in order to enable fluid communication, in particular gas exchange with regard to freeze-drying, between the interior of the vessel and the outside.

Another stopper for use in freeze drying is from the U.S. 5,596,814 A known.

From the U.S. 5,689,895 A a device for positioning a measuring probe in a container for use in freeze drying is known. The measuring probe is used to measure the physical parameters, such as temperature, during freeze drying. The device comprises a one-piece stopper, a guide tube being arranged in a central opening of the stopper penetrating the stopper, this guide tube extending into the container interior when the stopper is inserted into a container opening. The guide tube is used to accommodate the measuring probe in order to arrange it centrally and at a certain height in the interior of the container. Furthermore, the stopper has at least one further opening which passes through the stopper and which enables a gas exchange between the container interior and the container environment when the stopper is inserted into the container. The at least one further opening is preferably designed such that the gas exchange when the stopper is inserted into the container is similar or identical to a gas exchange of a conventional freeze-drying stopper in a drying position of the freeze-drying stopper. Due to the intended use and the design of the stopper of the device for positioning a measuring probe, however, the device or the stopper of the device is not intended and also not suitable for sealing the container in a fluid-tight manner after the freeze-drying.

The stoppers currently used in the field of freeze-drying, also known as lyophilization stoppers or freeze-drying stoppers, are usually made of a butyl rubber, also known as butyl rubber, for example bromobutyl rubber or chlorobutyl rubber. The production of the stopper as a molded rubber part is relatively costly, because on the one hand the material costs are relatively high and the rubber mixture must also be fully vulcanized in a heated mold, which means that the cycle times and the energy required during production are relatively high.

From the FR 1 479 255 A a stopper is known which comprises an element or a central core made of a rigid material which is opaque, transparent or translucent, such as glass, which element or the central core comprises a head and an axial body. The stopper also has a sleeve-shaped element made of plastic, the sleeve-shaped element enclosing the axial body. The sleeve-shaped plastic element has on its circumferential surface at least one bead or a sealing rib for contacting the inner surface of a container neck of the container to be closed. The bead or the sealing rib is designed such that it can be freely deformed during the closing process.

Freeze-drying stoppers are also known which are designed in two parts, the two parts of the stopper being made of different materials. Such a stopper, which has the features of the preamble of claim 1, is from the document DE 1 942 347 A known. The stopper has an insertion portion that can be inserted into the container, the insertion portion having a side surface and a bottom surface, the bottom surface being formed opposite a top surface of the stopper in an axial direction of the stopper. The insertion section in turn has a sealing section for the fluid-tight closing of the container in relation to the surroundings of the container in a sealing position of the stopper and an abutment section axially adjoining the sealing section from the top surface in the direction of the bottom surface for holding the stopper in a drying position of the stopper during freeze-drying, wherein the contact section has at least one passage opening for gas exchange between an interior of the container and the surroundings of the container during freeze-drying, this passage opening extending from the side surface into the bottom surface. Furthermore, the stopper has a sealing body and a Base on which are connected to each other.

In the plug according to the aforementioned publication, the sealing body is formed by an upper part of the plug and the base body is formed by a lower part of the plug, with outer surfaces of the sealing body in the area of the sealing section forming the side surface of the insertion section and the base body in the area of the sealing section within the Sealing body is formed .. The contact section, however, is formed by the base body. Accordingly, the side surface of the insertion section in the area of the contact section and the bottom surface of the insertion section are formed by outer surfaces of the base body. In order to ensure that the stopper is securely attached and held at the specified height before and during the freeze-drying process, it is provided that the base body consists of a material that has a higher hardness than a material from which the sealing body is made. In order to keep the stopper securely in the drying position with regard to the insertion depth, locking lugs of the base body lie directly on a container wall of the container.

A plug which has the features of the preamble of claim 1 is from DE 1 942 347 A known.

The object of the present invention is to develop a stopper that has the features of the preamble of claim 1 in such a way that the stopper nevertheless has a particularly good sealing property and / or barrier property and / or chemical resistance and also has a lower material cost and less manufacturing effort has sufficient rigidity for easy and self-handling and nevertheless damage to the stopper or container when inserting the stopper into or removing the stopper from the container is avoided. The invention achieves this object by a stopper according to claim 1. The dependent claims describe optional embodiments of the invention. In particular, according to further developments, the stopper should be designed in such a way that the use of butyl rubber and thus the vulcanization of the stopper can be dispensed with.

The stopper according to the invention is designed in such a way that, in the area of the contact section, areas of the side surface of the insertion section which contact an inner surface of a container wall of the container in the drying position and / or the sealing position are formed by outer surfaces of the sealing body, the base body in the area of the contact section inside of the sealing body is formed. Accordingly, only outer surfaces of the softer sealing body come into contact with the inner surface of the container wall in the region of the insertion section.

As a result of this design of the stopper, a wall thickness of the sealing body and of the base body is reduced compared to the overall extent of the stopper. In particular, the reduction in the wall thickness of the sealing body through the formation of the base body within the sealing body leads to a reduction in the material requirement for the sealing body, which reduces production costs, since a more cost-effective material can be used for the base body compared to the material of the sealing body.

With such a design of the stopper, the sealing body can be made of a softer material, which in each case has the desired material properties, for example the necessary elasticity or sealing effect. In contrast, the base body, which due to the design of the insertion section in the area of the insertion section does not come into contact with the container wall, can be made of a harder, more cost-effective material, for example polypropylene (PP). By means of the base body arranged in the sealing body, the plug is stiffened in the area of the sealing section inside, whereby the sealing effect of the plug is almost the same or even increased despite the reduction in the wall thickness of the sealing body compared to a plug that consists of a solid material in the area of the sealing section. Since the base body is in the area of the contact section is formed within the sealing body, the contact section also has the rigidity necessary to hold the plug securely in the drying position. Due to the fact that only the softer sealing body and not the harder base body makes direct contact with the container wall, the introduction of the insertion section into the container is made easier and a secure hold is nevertheless ensured. Damage, for example a breakage or material abrasion, of the base body or the container, especially in the case of a thin-walled glass container, is avoided, as is the case with direct contact between the hard base body and the container, especially when inserting the stopper into or pulling the stopper out of the Container, could occur. Even small amounts of material abrasion from the stopper or the container that get into the interior of the container can lead to contamination of the material stored in the container, which makes the material unusable for the intended use.

In addition, due to the smaller wall thickness of the sealing body and the rigidity due to the harder base body, bulging in the sealing body when the insertion section is inserted is avoided.

Furthermore, the formation of the stopper with a base body made of a harder material and formed within the sealing body is also to be regarded as advantageous with regard to a manufacturing method of the stopper. With an appropriate choice of material for the sealing body and the base body, the stopper can be manufactured by means of a multi-component injection molding process, in particular by means of a two-component injection molding process, with the stopper being stiffened by the base body, which is harder than the sealing body, so that the stopper can be demolded from one Injection molding tool is facilitated. It is conceivable that an ejector, when demolding from an injection molding tool, does not press at least exclusively into the softer material of the sealing body, but also presses into the harder material of the base body or even acts exclusively on the base body, thereby facilitating demolding and damaging the stopper is avoided during the demolding process.

Furthermore, the safe handling of the stopper when inserting the stopper into opening the container or pulling the stopper out of the opening is facilitated, since when a force is exerted on the stopper for the purpose of inserting the stopper, excessive deformation of the stopper, especially in the area of the sealing section, is avoided due to the stiffening of the stopper by the harder base body. Such a deformation can, for example, result in the sealing section not sealing the container in a fluid-tight manner in the sealing position of the stopper or the deformation being so severe that the stopper or the container is damaged.

In particular with regard to simple manufacture and a good sealing effect, in an advantageous development, outer surfaces of the sealing body in the area of the contact section form the side surface of the insertion section.

In order to achieve particularly good stiffening of the contact section and the sealing section, the base body is preferably designed as a solid body. With regard to particularly simple manufacture, the base body is preferably essentially circular-cylindrical, at least in the area of the insertion section.

In one embodiment of the plug it is provided that the base body has an outer surface, at least a partial area of this outer surface not being covered by the sealing body in the axial direction of the plug. In such an embodiment, the base body is mechanically accessible from the outside in the axial direction, so that a force can act directly on the base body without acting directly on the sealing body. For example, an ejector of an injection molding tool can press directly on the base body in order to remove the plug from the mold.

In such an embodiment, the base body preferably protrudes in the axial direction with respect to the sealing body or the corresponding outer surface of the sealing body is flush with this outer surface of the base body. This avoids forces acting from outside in this direction acting directly on the sealing body. However, it is also entirely conceivable that the sealing body protrudes in the axial direction with respect to the base body.

It is regarded as advantageous if the outer surface of the base body forms at least a partial area of the top surface. The top surface is preferably formed exclusively by the base body.

In the event that the sealing body covers the base body in the axial direction, it is considered to be particularly advantageous if the covering region of the sealing body has a relatively small axial dimension. A ratio of this axial dimension to a radial dimension of the sealing section, in particular the diameter of the sealing section, is preferably between 0.02 and 0.10, in particular between 0.02 and 0.06.

Outer surfaces of the sealing body form the side surface and the bottom surface of the insertion section. With such a design of the stopper, the sealing body, which comes into contact with the container and the contents of the container, can be made of a material that has the desired material properties, for example the necessary elasticity, chemical resistance and / or barrier properties with respect to the in the substance stored in the container or the substances stored in the container and / or the solvent used in the solution. In contrast, the base body can be made of a different material. For example, a material can be selected for the sealing body that has a good barrier effect and / or chemical resistance to substances stored in the interior of the container or the solvent used, and a material, which is generally less expensive, is selected for the base body, which has a less good barrier effect and / or has chemical resistance to these substances or the solvent used, since these substances or the solvent do not come into direct contact with the base body.

In a preferred embodiment, the sealing body is pot-shaped or essentially pot-shaped.

In particular, the sealing body is designed as a hollow cylinder or essentially as a hollow cylinder with a preferably closed bottom surface in the region of the insertion section.

Furthermore, through a suitable choice of the material combination of material of the sealing body and material of the base body, the blocking effect of the stopper can be easily adapted to the substances to be stored in the container and / or the solvent used and / or the ambient atmosphere. For example, a material can be selected for the sealing body that has a good blocking effect and / or chemical resistance to substances stored in the interior of the container, for example an organic solvent, and a material can be selected for the base body that has a good blocking effect and / or chemical Has resistance to substances in the vicinity of the container, for example oxygen or water. This allows a corresponding Material selection a contamination of the contents of the container by substances from the environment, such as oxygen, avoided or at least reduced.

The sealing body and the base body are preferably connected directly to one another. It is therefore not necessary in this embodiment to glue them to one another by means of an additional adhesive. In particular, the sealing body and the base body are directly materially connected to one another. As a result of this direct, in particular direct material connection between the sealing body and the base body, these are inextricably connected to one another, as a result of which the plug is virtually in one piece. The quasi one-piece design of the stopper makes it easier to use the stopper, in particular with regard to an automated freeze-drying process in which the mechanical insertion of the stopper is automated. The quasi one-piece design prevents the sealing body from becoming detached from the base body in the event of a mechanical load on the plug, for example for the purpose of opening or closing the container and, for example, the sealing body remaining in the container during the process of opening the container or when the container is inserted Stopper by a movement of the sealing body relative to the base body, a bulge is formed on the sealing body, which has a disadvantageous effect on the sealing effect of the plug.

It is also conceivable to weld the sealing body to the base body.

The material connection preferably takes place without an additional process step, in that the sealing body is molded onto the base body or the base body is molded onto the sealing body by means of an injection molding process.

In one embodiment, a cross section of the stopper with a circular outer contour is formed in the area of the sealing section perpendicular to the axial direction of the stopper. In the case of a container with a correspondingly shaped circular opening, the sealing section in the sealing position comes to rest all the way around the inner surface of the container wall delimiting the opening in this area and seals the container.

In particular with regard to a reduction in the material of the sealing body while the plug still has good sealing properties, it is considered particularly advantageous if the sealing body has an annular cross-section in the area of the sealing section perpendicular to the axial direction of the plug. A ratio of an outer radius of the circular ring to an inner radius of the circular ring is preferably 1.1 to 2.5.
In order to improve the blocking effect of the stopper against the substances to be stored in the container and / or the atmosphere outside the container, a preferred embodiment of the stopper provides for the stopper to have a blocking body or a barrier layer. By means of the blocking body or the blocking layer, for example, oxygen diffusion through the stopper into the interior of the container can be prevented or at least reduced. The material of the barrier body or barrier layer can be, for example, a plastic, for example vinyl alcohol copolymer (EVOH), or aluminum, in particular an aluminum foil.

It is entirely conceivable that the barrier layer and / or the barrier body forms the top surface. However, the blocking body and / or the blocking layer is preferably formed between the base body and the sealing body. As a result, the barrier layer or the barrier body is particularly well protected against damage from external forces.

In this context, it is considered to be particularly advantageous if the blocking body or the blocking layer is materially connected to the base body and / or materially connected to the sealing body.

In a preferred embodiment of the plug, an outer surface of the base body forms the top surface of the plug, the top surface covering the sealing body in the axial direction. As a result, handling of the stopper is made easier by the cover surface, which is harder than the sealing body, and the effective outer surface of the stopper is reduced, since the area of the sealing body that comes into contact with the ambient air is reduced by the cover by means of the cover surface of the base body is, whereby with a suitable choice of the material of the base body in combination with the choice of the material of the sealing body diffusion of substances from the environment into the container and / or diffusion of substances from the container into the environment can at least be reduced.

It is considered particularly advantageous if the stopper has a cover section adjoining the insertion section in the axial direction, in particular the cover section has the top surface, and wherein a radial dimension of the cover section is at least as large, in particular larger, than the radial dimension of the insertion section.

In particular, the embodiment of the cover section with a larger radial dimension is to be regarded as advantageous in that the cover section limits the insertion depth of the stopper into the container in the sealing position of the stopper. When inserting the stopper with a cover section larger than the insertion section, the area of the cover section protruding from the insertion section comes into contact with an outer surface of the container wall of the container facing the cover section, which prevents the stopper from being pushed further into the container.

Furthermore, a cover section with a larger radial dimension makes it easier to remove the stopper from the container, since the cover section forms an easily accessible contact surface on the stopper.

The cover section can definitely be designed as a circumferential flange.

It is considered to be advantageous if an outer surface of the sealing body forms a support surface of the cover section facing away from the cover surface. This bearing surface comes into contact with the outer surface of the container when the stopper is inserted into the container, whereby this bearing surface contributes to the sealing effect of the stopper.

In a preferred embodiment of the plug, the base body has a first projection formed in the radial direction in the region of the cover section, the first projection in particular as a circumferential first projection is trained. This projection can serve to hold the stopper in an additional closure that can be attached to the container. This closure can be, for example, a crimp cap or a screw closure. Typically, such an additional closure is applied to the container following the freeze drying process to secure the stopper. It is entirely conceivable that the stopper is completely inserted into the container by attaching the closure to the container.

The stopper can be held in the closure, for example, in that a partial area of the closure engages behind the first projection on the side facing the container, for example the first projection is arranged in an undercut of the closure. The connection between the closure and the stopper ensures that the stopper is pulled out of the container when the closure is removed from the container, for example when a closure designed as a twist lock is unscrewed.

With regard to the connection between the stopper and the closure, it is entirely conceivable that the closure is already connected to the stopper before the freeze-drying process.

In order to further reduce the effective outer surface of the plug, in an advantageous embodiment of the plug the base body at least partially covers the sealing body in the area of the cover section radially on the outside. For this purpose, in a preferred embodiment, the base body has in the area of the cover section a radially outwardly formed second projection extending from the top surface in the direction of the bottom surface, the second projection at least partially covering the sealing body in the area of the cover section radially outside. The sealing body is preferably radially enclosed by the second projection.

In an advantageous development of the plug, a partial area of the sealing body extending from the bottom surface in the direction of the top surface is radially enclosed by the base body. This increases the contact area between the sealing body and the base body, which has an advantageous effect on the stability of the connection between these affects.

It is considered to be particularly advantageous if the base body has a through-channel extending from the top surface in the direction of the bottom surface. This through-channel makes it possible, for example, by means of a syringe or the like to remove the contents from the container without removing the stopper from the container. For this purpose, a needle or the like can be inserted into the through-channel, the bottom surface of the sealing body being pierced in the area adjoining the through-channel and the contents of the container thus becoming accessible.

It is entirely conceivable and preferred that a partial area of the sealing body extending from the bottom surface in the direction of the top surface is formed in the through channel.

The design of the base body with a through channel is also to be regarded as advantageous with regard to the production of the stopper by means of injection molding. For example, a base body with a through-channel can first be injection-molded and then the sealing body can be injection-molded onto the base body through the through-channel from the side facing the cover surface. As a result, the required tool technology is significantly simplified and the tool becomes more cost-effective, more robust and has a longer service life. It is considered to be particularly advantageous if the through-channel is formed centrally in the base body, as a result of which shape tolerances, in particular with regard to the roundness of the sealing body, can be reduced.

It is considered to be particularly advantageous if the insertion section, in particular the sealing body, has at least one recess, the at least one recess forming the at least one passage opening for gas exchange. Such a recess is open in the axial direction towards the bottom surface and open in the radial direction. It is entirely conceivable that an outer surface of the insertion section delimiting the recess is at least partially formed by the base body.

Since in the drying position such a plug with a recess does not lie circumferentially on the inner surface of the container wall, but only a partial area of the inner surface adjoining the contact section contacts the sealing body, it is considered useful with regard to a secure hold of the plug in the drying position if in the drying position, a proportion of this sub-area in the area of the inner surface of the container which adjoins the contact section is at least 20%, in particular at least 40%.

The sealing body is preferably made of a material that has a hardness of Shore A 40 to 80, preferably a hardness of Shore A 50 to 70, in accordance with the DIN ISO 7619-1: 2010 standard and / or the sealing body is made of a thermoplastic elastomer (TPE).

With regard to the base body, it is considered particularly advantageous if the base body consists of a material that has a hardness of Shore D 30 to 100, preferably a hardness of Shore D 40 to 85 in accordance with DIN ISO 7619-1: 2010 and / or the base body is made of polypropylene (PP) or high-density polyethylene (HDPE).

The contact section is preferably free of areas protruding outward in the radial direction relative to the sealing section. Accordingly, the contact section does not have any areas protruding from the sealing section, such as locking lugs, beads or the like, which in the drying position bear against the container wall in the axial direction in order to hold the stopper at a certain insertion depth in the drying position. In such an embodiment, the stopper is only held in that the contact section contacts the inner surface of the container wall. Due to the softer material of the sealing body compared to the base body, which forms the areas of the side surface of the insertion section which contact the inner surface of the container wall in the drying position and / or the sealing position, and the harder base body which is arranged inside the sealing body and consequently stiffens the contact section , a secure hold in the drying position is also possible without locking lugs or the like. In contrast to stoppers with locking lugs or the like, the transfer of a stopper configured in this way from the drying position into the sealing position with less effort, since no protruding parts have to be deformed. Plugs with locking lugs, beads or the like also have the disadvantage that, due to the strong deformation in the area of the locking lugs or beads, when the stopper is moved into the sealing position of the plug, these protruding areas or the container itself are damaged. The pulling out of the stopper is also made more difficult by locking lugs or the like, since the locking lugs or beads are deformed in a direction opposite to the deformation during insertion. Due to the opposite load, there is in turn the risk of damage or even of the locking lugs or beads being sheared off.

In an advantageous development of the plug, the base body and / or the sealing body and / or the plug is symmetrical, in particular radially symmetrical, with respect to an axis of symmetry and / or plane of symmetry running in the axial direction.

The stopper is preferably a stopper manufactured by means of a multi-component injection molding process, preferably by means of a two-component or a three-component injection molding process.

In the case of an arrangement of a container and a stopper for use of the arrangement in the case of freeze-drying, it is provided that the stopper is inserted into an opening of the container. The stopper has an insertion portion inserted into the container, the insertion portion having a side surface and a bottom surface, the bottom surface being formed opposite a top surface of the stopper in an axial direction of the stopper. The insertion section in turn has a sealing section for the fluid-tight closing of the container in relation to the surroundings of the container in a sealing position of the stopper and an abutment section axially adjoining the sealing section from the top surface in the direction of the bottom surface for holding the stopper in a drying position of the stopper during freeze-drying, wherein the contact section has at least one passage opening for a gas exchange between an interior of the container and the surroundings of the container during freeze drying, this passage opening extending from the side surface into the Floor area extends. Furthermore, the stopper has a sealing body and a base body which are connected to one another. The base body consists of a material that has a higher hardness than a material of which the sealing body is made. The base body is formed in the area of the sealing section within the sealing body. Outer surfaces of the sealing body form the side surface of the insertion section in the area of the sealing section.

In the drying position of the stopper, the sealing section is arranged outside the container and the contact section contacts an inner surface of a container wall of the container, the at least one passage opening opening into the interior of the container and into the environment, whereby a gas exchange between the interior during the freeze-drying process of the container and the environment is possible.

In the sealing position of the stopper, the stopper is inserted further into the container compared to the drying position and the sealing section is arranged inside the container, the sealing section making circumferential contact with the inner surface of the container wall, whereby the sealing section closes the container in a fluid-tight manner.

In the area of the contact section, areas of the side surface of the insertion section which contact the inner surface of the container wall of the container in the drying position and / or the sealing position are formed by outer surfaces of the sealing body, and the base body is formed in the area of the contact section within the sealing body.

Due to the fact that only the softer sealing body and not the harder base body makes direct contact with the container wall, the introduction of the insertion section into the container is made easier and a secure hold is nevertheless ensured. Damage, for example breakage or material abrasion, to the base body or the container, especially in the case of a thin-walled glass container, is avoided, as could occur with direct contact between the hard base body and the container. Even slight material abrasion of the stopper or the container, which can get into the interior of the container lead to contamination of the substance stored in the container, which makes the substance unusable for the intended use.

The stopper of the arrangement can also be designed according to the embodiments described with respect to the stopper as such. In particular, the stopper of the arrangement is designed according to the features of one or more of claims 1 to 14.

It is considered to be particularly advantageous if, in the sealing position of the stopper, the side surface of the sealing section lies flat against the inner surface of the container wall.

Further features of the invention are shown in the subclaims, the description of the figures and the figures themselves, it being noted that all individual features and all combinations of individual features are essential to the invention.

In the figures, the invention is shown on the basis of exemplary embodiments, without being restricted thereto.

Fig. 1

eine erste Ausführungsform eines Stopfens und einen Behälter in einer Anordnung, in der der Stopfen teilweise in den Behälter eingeführt ist, in einer Seitenansicht,

Fig. 2

der Stopfen und der Behälter gemäß Fig. 1 in einer Anordnung, in der der Stopfen maximal weit in den Behälter eingeführt ist, in einer Seitenansicht,

Fig. 3

der Stopfen gemäß Fig. 1 in einer Ansicht gemäß dem Pfeil III in Fig. 6,

Fig. 4

der Stopfen in einer Ansicht gemäß dem Pfeil IV in Fig. 3,

Fig. 5

der Stopfen in einer Ansicht gemäß dem Pfeil V in Fig. 3,

Fig. 6

der Stopfen in einer Schnittansicht gemäß der Linie VI-VI in Fig. 3,

Fig. 7

der Stopfen in einer Schnittansicht gemäß der Linie VII-VII in Fig. 3,

Fig. 8

eine zweite Ausführungsform des Stopfens in einer Ansicht gemäß dem Pfeil VIII in Fig. 9,

Fig. 9

der Stopfen in einer Schnittansicht gemäß der Linie IX-IX in Fig. 8,

Fig. 10

eine dritte Ausführungsform des Stopfens in einer Ansicht gemäß dem Pfeil X in Fig. 11,

Fig. 11

der Stopfen in einer Schnittansicht gemäß der Linie XI-XI in Fig. 10,

Fig. 12

eine vierte Ausführungsform des Stopfens in einer Ansicht gemäß dem Pfeil XII in Fig. 13,

Fig. 13

der Stopfen in einer Schnittansicht gemäß der Linie XIII-XIII in Fig. 12,

Fig. 14

der Stopfen in einer Ansicht gemäß dem Pfeil XIV in Fig. 13

Fig. 15

eine nicht zur Erfindung gehörende Ausführungsform eines Stopfens in einer Ansicht gemäß dem Pfeil XV in Fig. 16,

Fig. 16

der Stopfen in einer Schnittansicht gemäß der Linie XVI-XVI in Fig. 15,

Fig. 17

eine nicht zur Erfindung gehörende Ausführungsform eines Stopfens in einer Ansicht gemäß dem Pfeil XVII in Fig. 18,

Fig. 18

der Stopfen in einer Schnittansicht gemäß der Linie XVIII-XVIII in Fig. 17,

Fig. 19

eine siebte Ausführungsform des Stopfens in einer Ansicht gemäß dem Pfeil XIX in Fig. 20,

Fig. 20

der Stopfen in einer Schnittansicht gemäß der Linie XX-XX in Fig. 19,

Fig. 21

der Behälter gemäß Fig. 1 in einer Schnittansicht gemäß der Linie XXI-XXI in Fig. 22,

Fig. 22

der Behälter in einer Ansicht gemäß dem Pfeil XXII in Fig. 21.

It shows:

Fig. 1

a first embodiment of a stopper and a container in an arrangement in which the stopper is partially inserted into the container, in a side view,

Fig. 2

the stopper and the container according to Fig. 1 in an arrangement in which the stopper is inserted as far as possible into the container, in a side view,

Fig. 3

the plug according to Fig. 1 in a view according to arrow III in Fig. 6 ,

Fig. 4

the stopper in a view according to arrow IV in Fig. 3 ,

Fig. 5

the plug in a view according to the arrow V in Fig. 3 ,

Fig. 6

the plug in a sectional view along the line VI-VI in Fig. 3 ,

Fig. 7

the plug in a sectional view along the line VII-VII in Fig. 3 ,

Fig. 8

a second embodiment of the plug in a view according to arrow VIII in Fig. 9 ,

Fig. 9

the plug in a sectional view along the line IX-IX in Fig. 8 ,

Fig. 10

a third embodiment of the plug in a view according to the arrow X in Fig. 11 ,

Fig. 11

the plug in a sectional view along the line XI-XI in Fig. 10 ,

Fig. 12

a fourth embodiment of the plug in a view according to the arrow XII in Fig. 13 ,

Fig. 13

the plug in a sectional view along the line XIII-XIII in Fig. 12 ,

Fig. 14

the stopper in a view according to arrow XIV in Fig. 13

Fig. 15

an embodiment of a stopper not belonging to the invention in a view according to arrow XV in FIG Fig. 16 ,

Fig. 16

the plug in a sectional view along the line XVI-XVI in Fig. 15 ,

Fig. 17

an embodiment of a plug not belonging to the invention in a view according to arrow XVII in FIG Fig. 18 ,

Fig. 18

the plug in a sectional view along the line XVIII-XVIII in Fig. 17 ,

Fig. 19

a seventh embodiment of the plug in a view according to the arrow XIX in Fig. 20 ,

Fig. 20

the plug in a sectional view along the line XX-XX in Fig. 19 ,

Fig. 21

the container according to Fig. 1 in a sectional view along the line XXI-XXI in Fig. 22 ,

Fig. 22

the container in a view according to arrow XXII in Fig. 21 .

The Figs. 1 and 2 illustrate the upper end of a container 18 and a first embodiment of a stopper 1 for use in a freeze-drying process, the stopper being inserted into an opening 23 of the container 18 which is formed in the region of a container neck 19.

In the Figures 1 and 2 the container is cut and the stopper is shown uncut.

In the Fig. 1 an arrangement of the container 18 and the stopper 1 is shown in which an insertion section 2 of the stopper 1 is partially inserted into the neck 19 of the container 18. This position of the stopper 1 corresponds to a drying position of the stopper 1.

The Fig. 2 shows an arrangement of the container 18 and the stopper 1 in which the insertion section 2 of the stopper 1 is completely inserted into the container neck 19 of the container 18 and a cover section 10 of the stopper 1 adjoining the insertion section 2 in an axial direction Z of the stopper 1 an outer surface 20 of the container neck 19 rests. This position of the stopper 1 corresponds to a sealing position of the stopper 1.

The insertion section 2 has a side face 3 and a bottom face 4, the bottom face 4 being formed opposite a top face 5 of the plug 1 formed in the area of the cover section 10 in the axial direction Z of the plug 1.

The insertion section 2 has a sealing section 16 for the fluid-tight closing of the container 18 in relation to the surroundings of the container 18 in the sealing position of the plug 1 and an abutment section 17 axially adjoining the sealing section 16 from the top surface 5 in the direction of the bottom surface 4 for holding the plug 1 in the drying position of the plug 1 during freeze-drying, the abutment section 17 having four passage openings 6, the passage openings 6 are identical and each in the form of a recess 6. The respective recess 6 extends from the side surface 3 into the bottom surface 4 and enables gas exchange between an interior space 22 in the drying position of the plug, thus in a state in which the insertion section 2 of the plug 1 is only partially inserted into the container 18 of the container 18 and the environment. This state is in the Fig. 1 The contact section 17 of the stopper 1 is partially formed outside the container neck 19, the sub-area of the contact section 17 located outside the container 18 having a sub-area of the respective passage opening 6 which is open in a radial direction X, Y and in this way a gas exchange between the container interior 22 and the environment is made possible. Hence, in the, in the Fig. 1 shown drying position of the stopper 1 a freeze-drying of a solution stored in the container 18 is possible.

In the drying position of the stopper 1, only a partial area of the inner surface 21 adjoining the contact section 17 makes contact with the sealing body 7. In the present case, the tangential extension of the respective recess is approximately 45 °. Consequently, the proportion of the contacting partial area in the area of the inner surface of the container which adjoins the contact section is approximately 50%.

The insertion section 2 has an essentially circular-cylindrical outer contour, the contact section 17 being free of regions protruding in the radial direction X, Y with respect to the sealing section 16.

In the in the Fig. 1 In the state shown, partial areas of the side surface 3 of the contact section 17 rest on an inner surface 21 of the container neck 19, whereby the stopper 1 is held in its partially pushed-in position, and for further insertion of the stopper 1 a force is exerted on the stopper 1 in the axial direction Z in Direction of the container 18 is necessary.

The stopper 1 has a sealing section 16 adjoining the contact section 17 in the direction of the top surface 5, the sealing section 16 lying circumferentially on the inner surface 21 of the container neck 19 in a state in which the insertion section 2 is completely inserted into the container 18 and thus sealingly closes the container 18.

As in particular the sectional view of the Fig. 6 As can be seen, the stopper 1 has a sealing body 7 and a base body 8, with outer surfaces of the sealing body 7 in the area of the sealing section 16 and the contact section 17 forming the side surface 3 of the insertion section 2 and the bottom surface 4 of the insertion section 2.

In the present case, the sealing body 8 is essentially pot-shaped.

The base body 8 is formed in the area of the insertion section 2 within the sealing body 7, whereby only the sealing body 7 comes into contact with the inner surface 21 of the container 18 and the interior of the container 18. The sealing body 7 and the base body 8 are materially connected to one another. Due to the material connection, the sealing body 7 and the base body 8 are inextricably connected to one another, so that the plug 1 is designed as a single piece. The material connection is preferably produced by a multi-component injection molding process, in particular a two-component injection molding process.

The base body 8 and the sealing body 7 are made of different materials, the base body 8 being made of a material that has a higher hardness than a material of which the sealing body 7 is made.

The sealing body 7 has an annular cross-section in the area of the sealing section 16, an outer radius R of the circular ring being approximately twice an inner radius r of the circular ring.

The sealing body 7 and the base body 8 are partially formed in the cover section 10, with an outer surface of the base body 8 forming the top surface 5 and the top surface 5 covering the sealing body 7 in the axial direction Z.

In order to limit the insertion depth of the stopper 1 in the axial direction Z and to improve the sealing effect of the stopper 1 and to facilitate the removal of the stopper 1 from the container 18, the cover section 10 has a radial dimension which is larger than a radial dimension of the insertion section 2. When the stopper 1 is completely inserted into the container 18, a bearing surface 11 of the cover section 10 facing away from the cover surface 5 rests on the outer surface 20 of the container 18. This bearing surface 11 of the cover section 10 is formed by an outer surface of the sealing body 7.

Both the base body 8 and the sealing body 7 of the stopper 1 are designed to be radially symmetrical to an axis of symmetry 18 of the stopper 1 running in the axial direction Z.

The base body 8 is essentially circular-cylindrical both in the area of the insertion section 2 and essentially circular-cylindrical in the area of the cover section 10, the base body 8 having a larger diameter in the area of the cover section 10 than in the area of the insertion section 2.

The base body 8 furthermore has, in the area of the cover section 10, a circumferential first projection 12 formed in the radial direction X, Y. This first projection 12 can serve, for example, to hold the stopper 1 in an additional closure that can be attached to the container 18.

In order to further reduce the effective outer surface of the plug 1, the base body 8 covers the in the Figs. 8-11 The second exemplary embodiment shown of the plug 1 partially removes the sealing body 7 in the area of the cover section 10 radially on the outside. For this purpose, the base body 8 in the area of the cover section 10 has a radially outwardly formed, circumferential second projection 13 extending from the top surface 5 in the direction of the bottom surface 4, the second projection 13 holding the sealing body 7 in the area of the cover section 10 radially on the outside partially covers.

That in the Figures 10 and 11 The third embodiment of the plug 1 shown differs from that in FIG Fig. 8 and 9 The embodiment shown essentially in that the plug 1 has a blocking body 9 in the form of a blocking layer 9 formed between the base body 8 and the sealing body 7 in order to improve the blocking effect of the plug 1, for example against oxygen diffusion. The barrier layer 9 and / or the barrier body 9 can consist, for example, of ethylene-vinyl alcohol copolymer (EVOH) or aluminum. The blocking body 9 and / or the blocking layer 9 is preferably materially connected to the base body 8 and / or materially connected to the sealing body 7. Such a stopper 1 can be produced, for example, by means of a three-component injection molding process. However, it is also entirely conceivable that the blocking body 9 and / or the blocking layer 9 is held between the base body 8 and the sealing body 7 in a clamping or form-fitting manner.

That in the Figures 12-14 The fourth exemplary embodiment of the plug 1 shown here differs from the first exemplary embodiment essentially in that the base body 8 has a central through-channel 15 extending from the top surface 5 in the direction of the bottom surface 4, with a central passage channel 15 extending from the bottom surface 4 in the direction of the top surface 5 extending sub-area 14 of the sealing body 7 is formed in the through-channel 15, whereby the base body 8 radially encloses this sub-area 14 of the sealing body 7. The through channel 15 enables the contents of the container to be removed without removing the stopper 1 from the container 18, for example by inserting a needle into the through channel 15 and piercing the sealing body 7 in the insertion area of the needle.

Furthermore, such an embodiment of the plug 1 can be produced particularly easily and inexpensively by first producing the base body 8, for example by means of an injection molding process, and then injecting the sealing body 7 onto the base body 8, with the sealing body 7 being injected through the through-channel 15 of the base body 8 takes place. Through the centrally formed through channel 15 and the consequent central injection molding of the sealing body 7 onto the base body 8, shape tolerances of the plug 1 are also reduced.

That in the Figures 15 and 16 The fifth exemplary embodiment of the plug 1 shown here differs from the first exemplary embodiment essentially in that the base body 8 has an outer surface, a portion of this outer surface not being covered by the sealing body 7 in the axial direction Z of the plug 1. In the present case, this outer surface of the base body 8 forms a sub-area of the bottom surface 4, the corresponding outer surface of the sealing body 7, which also forms a sub-area of the bottom surface 4, flush with this outer surface of the base body 8 in the axial direction Z. In addition, in contrast to the first exemplary embodiment of the plug 1, the top surface 5 is formed by the sealing body 7.

That in the Figures 17 and 18 The illustrated sixth exemplary embodiment of the plug 1 differs from the first exemplary embodiment essentially in that the base body 8 has an outer surface, a portion of this outer surface not being covered by the sealing body 7 in the axial direction Z of the plug 1. In the present case, this outer surface of the base body 8 forms a sub-area of the cover surface 5, the corresponding outer surface of the sealing body 7, which also forms a sub-area of the cover surface 5, flush with this outer surface of the base body 8 in the axial direction Z.

That in the Figures 19 and 20 The seventh embodiment of the plug 1 shown differs from the fifth embodiment essentially in that the side surface 3 of the insertion section 2 is not formed exclusively by outer surfaces of the sealing body 7, but only the areas of the side surface 3 of the insertion section 2 which are in the drying position and / or the sealing position contact the inner surface 21 of the container wall 24, formed by outer surfaces of the sealing body 7. Accordingly, in the drying position and / or the sealing position in the area of the insertion section 2, only outer surfaces of the softer sealing body 7 come into contact with inner surfaces 21 of the container wall 24. Subareas of the side surface 3 of the insertion section 2, in this case a subarea of the side surface 3 delimiting the respective recess 6, are formed by outer surfaces of the base body 8.

The Figures 21 and 22 show the container 18 without a stopper 1.

In order to facilitate insertion of the stopper 1, the exemplary embodiments of the stopper 1 shown in the figures have a conical outer contour in a region of the contact section 17 having the bottom surface 4.

List of reference symbols

1

Plug

2

Lead-in section

3

Side face

4th

Floor area

5

Top surface

6

Passage opening

7th

Sealing body

8th

Base body

9

Barrier body / barrier layer

10

Cover section

11

Contact surface

12

first lead

13th

second lead

14th

Section

15th

Through channel

16

Sealing section

17th

Plant section

18th

container

19th

Container neck

20th

Exterior surface

21st

Inner surface

22nd

inner space

23

opening

24

Container wall

X

radial direction

Y

other radial direction

Z

axial direction

Claims (13)

1. Stopper (1) for a container (18) for use in freeze-drying processes, wherein the stopper (1) has an insertion section (2) which can be inserted into the container (18), and the insertion section (2) has a lateral surface (3) and a bottom surface (4), wherein the bottom surface (4) is configured opposite a top surface (5) of the stopper (1) in an axial direction (Z) of the stopper (1), and the insertion section (2) has a sealing section (16) for closing the container (18) in a fluid-tight manner from the surroundings of the container (18) in a sealing position of the stopper (1) and a contact section (17) which adjoins the sealing section (16) axially from the top surface (5) in the direction of the bottom surface (4), for holding the stopper (1) in a drying position of the stopper (1) during the freeze-drying process, wherein the contact section (17) has at least one passage opening (6) for a gas exchange between an interior (22) of the container (18) and the surroundings of the container (18) during the freeze-drying process, wherein the at least one passage opening (6) extends from the lateral surface (3) into the bottom surface (4) and the stopper (1) has a sealing body (7) and a main body (8) which are connected together, wherein outer surfaces of the sealing body (7) in the region of the sealing section (16) form the lateral surface (3) of the insertion section (2) and the main body (8) is configured within the sealing body (7) in the region of the sealing section (16), wherein the main body (8) consists of a material which has a higher degree of hardness than a material which makes up the sealing body (7), characterized in that regions of the lateral surface (3) of the insertion section (2), which are able to contact an inner surface (21) of a container wall (24) of the container (18) in the drying position and/or the sealing position, are formed by outer surfaces of the sealing body (7) in the region of the contact section (17), wherein the main body (8) is configured within the sealing body (7) in the region of the contact section (17), wherein outer surfaces of the sealing body (7) form the lateral surface (3) and the bottom surface (4) of the insertion section (2).
2. Stopper (1) according to Claim 1, characterized in that outer surfaces of the sealing body (7) form the lateral surface (3) of the insertion section (2) in the region of the contact section (17).
3. Stopper (1) according to either of Claims 1 and 2, characterized in that the main body (8) has an outer surface, wherein at least a partial region of this outer surface is not covered by the sealing body (7) in the axial direction (Z) of the stopper (1).
4. Stopper (1) according to Claim 3, characterized in that the outer surface of the main body (8) forms at least a partial region of the top surface (5).
5. Stopper (1) according to one of Claims 1 to 4, characterized in that the sealing body (7) and the main body (8) are directly connected together, in particular directly connected together by a material connection.
6. Stopper (1) according to one of Claims 1 to 5, characterized in that an outer surface of the main body (8) forms the top surface (5) and the top surface (5) covers the sealing body (7) in the axial direction (Z) .
7. Stopper (1) according to one of Claims 1 to 6, characterized in that the stopper (1) has a cover section (10) adjoining the insertion section (2) in the axial direction (Z), wherein a radial dimension of the cover section (10) is larger than a radial dimension of the insertion section (2).
8. Stopper (1) according to Claim 7, characterized in that an outer surface of the sealing body (7) forms a bearing surface (11) of the cover section (10) remote from the top surface (5).
9. Stopper (1) according to one of Claims 1 to 8, characterized in that the sealing body (7) in the region of the sealing section (16) has a circular cross section perpendicular to the axial direction (Z) of the stopper (1), and preferably a ratio of an external radius (R) of the annulus to an internal radius (r) of the annulus is 1.1 to 2.5.
10. Stopper (1) according to one of Claims 1 to 9, characterized in that the insertion section (2) comprises at least one recess (6), wherein the recess (6) forms the at least one passage opening (6).
11. Stopper (1) according to one of Claims 1 to 10, characterized in that the sealing body (7) consists of a material which has a Shore A hardness of 40 to 80, preferably a Shore A hardness of 50 to 70 according to DIN ISO 7619-1:2010, and/or the sealing body (7) consists of a thermoplastic elastomer (TPE).
12. Stopper (1) according to one of Claims 1 to 11, characterized in that the main body (8) consists of a material which has a Shore D hardness of 30 to 100, preferably a Shore D hardness of 40 to 85 according to DIN ISO 7619-1:2010, and/or the main body (8) consists of polypropylene (PP) or high density polyethylene (HDPE).
13. Stopper (1) according to one of Claims 1 to 12, characterized in that the contact section (17) is free of regions protruding outwardly relative to the sealing section (16) in a radial direction (X, Y).

Images