Container for liquid, method and device for forming such a container

Abstract

The container (20) for liquid food or pharmaceutical liquid (22) comprises a tube (21) made of plastic material geometrically defined, at least at its mouth, for the outside of the tube, by generatrices of a cylinder or of a cone that are referred to as "outer generatrices" and, for the inside of the tube, by generatrices of a cylinder or of a cone that are referred to as "inner generatrices", this tube having a longitudinal axis (27) of rotational symmetry, this tube containing said liquid, this tube being moulded in a mould. The tube comprises, in its side wall, a barrier label (24) comprising a material which is more impervious to at least one gas than is the plastic material of the tube, this barrier label being present in the mould during the moulding of the wall of the tube.

Description

[0001] LIQUID CONTAINER, METHOD AND DEVICE FOR PRODUCING SUCH A CONTAINER

[0002] CONTAINER

[0003] TECHNICAL FIELD OF THE INVENTION

[0004] The present invention relates to a liquid container, a method and a device for constituting such a container. It applies, in particular, to the constitution of doses of medicines and drinkable products, for example food supplements or energy drinks.

[0005] STATE OF THE ART

[0006] Traditionally, containers for liquid medication and dietary supplement doses are cylindrical glass ampoules with two tips. Their advantages include their ability to contain a single material, i.e., a uniform material, the impermeability of glass to both gases and liquids, and their low cost. However, double-tipped glass ampoules have disadvantages. First, glass is a brittle and heavy material, which therefore imposes significant logistical constraints. In addition, once opened by breaking one of their tips, these ampoules can cause cuts to the user's skin. There is also a risk, when opening by breaking a tip, that glass fragments will accompany the liquid and be swallowed by the user, with the risk of cutting their digestive system.Glass also does not allow for printing or decoration other than monochrome and low resolution. An evolution of this two-pointed bulb is the cylindrical glass "bottle" bulb with a single point. This bulb has the same disadvantages as the two-pointed bulb. In addition, its manufacture is more expensive than that of the two-pointed bulb.

[0007] Synthetic material bottles have also been used. These are single-dose containers made of synthetic material with screw caps. These bottles have the advantage of being robust and non-brittle, can be filled individually, and can be decorated in four-color printing by applying a label. On the other hand, their synthetic material does not constitute a barrier for atoms or molecules, which can lead to deterioration of their contents, or even the formation of undesirable or dangerous molecules, for example through oxidation or penetration of atoms or molecules from the glue or dyes in the label. In addition, these bottles cannot be sterilized and their production cost is high.

[0008] Unicadose® have the advantages of being robust and sterilizable, but with risks of deformation and leakage. They have the following main disadvantages. Their material does not constitute a barrier for atoms or molecules, particularly in their breakable zone, which is particularly thin (of the order of a few hundredths of a millimeter thick) which aggravates the porosity to oxygen. Their sealing is obtained by interlocking, they present risks of leakage and the presence of liquid in the assembled part. Their cost price is high. Their breakability is not controlled, because the reduced material thickness at the opening varies with the wear of the mold. Their filling is collective or semi-collective, implying a very heterogeneous dosage with a significant risk of non-compliant filling. Their decoration is necessarily monochrome.

[0009] Sticks® are flexible aluminum containers. They offer the advantages of being robust and unit-fillable. They can be decorated in four colors, and their walls act as barriers to atoms and molecules, particularly oxygen. However, they cannot be sterilized, which requires the use of preservatives. They have a small capacity and are difficult for the average user to open.

[0010] SUBJECT OF THE INVENTION

[0011] The present invention aims to overcome all or part of the drawbacks of the prior art set out above. To this end, according to a first aspect, the invention aims at a container for food or pharmaceutical liquid comprising a plastic tube geometrically defined, at least at its mouth, for the outside of the tube, by generatrices of a cylinder or a cone called "external" and, for the inside of the tube, by generatrices of a cylinder or a cone called "internal", this tube having a longitudinal axis of rotational symmetry, this tube comprising said liquid, this tube being molded in a mold, container in which the tube comprises, in its side wall, a barrier label comprising a material more impermeable to at least one gas than the plastic material of the tube, this barrier label being present in the mold during the molding of the wall of the tube.

[0012] This barrier label, integrated into the wall of the tube, reduces or prevents the passage of gas through this wall and thus protects the contents of the tube.

[0013] In embodiments, the label is made of an oxygen-tight material. Since the aluminum of the seal is also oxygen-tight, oxidation of the contents of the tube is reduced.

[0014] In embodiments, the label and the seal together cover at least 80% of the total surface area of ​​the container. Preferably, this ratio is greater than 90%. The capacity for gas passage through the wall of the tube is thus greatly reduced.

[0015] In embodiments, the plastic material of the tube wall is "crystal" polypropylene without additives. There is therefore no risk of contamination of the contents of the tube by a component present in the tube material.

[0016] In embodiments, the barrier label comprises a multi-layer cast polypropylene film, the successive layers comprising polypropylene, ethylene vinyl alcohol EVOH and polypropylene. Preferably, the barrier label has a thickness of between 50 microns and 80 microns. The inventor has discovered that these characteristics ensure very good sealing of the barrier label to oxygen.

[0017] According to a second aspect, the invention relates to a container for food or pharmaceutical liquid comprising:

[0018] - a plastic tube geometrically defined, at least at its mouth, for the outside of the tube, by generatrices of a cylinder or a cone called "external" and, for the inside of the tube, by generatrices of a cylinder or a cone called "internal", this tube having a longitudinal axis of rotational symmetry, this tube comprising said liquid, and

[0019] - a seal welded onto the mouth of the tube, this seal extending, towards the outside of the tube, beyond said external generatrices; container in which the weld of this seal onto the tube comprises a meniscus on the internal wall of the tube inside the volume defined by the internal generatrices, the volume of this meniscus being at least twice the volume of any meniscus on the external wall of the tube outside the volume defined by the external generatrices.

[0020] This ensures good adhesion of the seal to the tube, while avoiding the formation of an unsightly external edge that could injure the consumer's lip when consuming the liquid.

[0021] In embodiments, before welding the cover, the last section of the mouth of the tube perpendicular to the axis of rotational symmetry is separated from the external generatrices by a distance, measured on an axis of this section passing through the axis of rotational symmetry, at least equal to one fifth of the distance between the internal generatrices and the external generatrices, the surface area of ​​the section of the tube perpendicular to the axis of rotational symmetry being reduced, compared to sections of the tube perpendicular to the axis of rotational symmetry further from the mouth. This reduction in section at the mouth may be sufficient to obtain the advantages of the second aspect of the invention.

[0022] In embodiments, the tube has, before welding the seal, at least one external shoulder near the mouth, this shoulder reducing, at the mouth, the surface of the section of the tube perpendicular to the axis of rotational symmetry, compared to sections of the tube perpendicular to the axis of rotational symmetry further from the mouth. Such a shoulder is easy to mold and its distance from the mouth makes it possible to calibrate the respective movement of the sealing punch and the tube during the melting of the tube material.

[0023] In embodiments, the tube has, before welding the seal, at least one conical shape reducing, at the mouth, the surface of the section of the tube perpendicular to the axis of rotational symmetry, compared to sections of the tube perpendicular to the axis of rotational symmetry further from the mouth. Such a conical shape is easy to mold and its geometry makes it possible to calibrate the respective movement of the sealing punch and the tube during the melting of the tube material.

[0024] In embodiments, before welding the seal, the length, parallel to the axis of rotational symmetry, of the area in which the surface area of ​​the section of the tube perpendicular to the axis of rotational symmetry is reduced, compared to sections of the tube perpendicular to the axis of rotational symmetry further from the mouth, is less than two millimeters. Thus, a very small distance is sufficient to obtain the advantages of the second aspect of the invention.

[0025] In embodiments, the seal is made of coextruded metal with a layer of the same plastic material as the tube. Preferably, said metal is aluminum and said plastic material is polypropylene. Thus, the adhesion of the molten material of the tube to the seal is improved.

[0026] According to a third aspect, the invention relates to a container for food or pharmaceutical liquid comprising a plastic tube comprising, in its side wall, a barrier label comprising a material more impermeable to at least one gas than the plastic material of the tube, this barrier label being present in a mold during the molding of the wall of the tube and a seal welded onto the tube, said liquid being a liquid without preservative, the tube and this liquid undergoing a sterilization or tyndallization heat treatment. Thus, the liquid contained in the tube does not require a preservative. In addition, the barrier label limits the passage of gas through the wall of the tube, which increases the shelf life of the liquid.

[0027] In embodiments, the container has an axis of rotational symmetry, and a dimension parallel to the axis of rotational symmetry greater than five times its maximum diameter. This elongated shape increases the ratio of surface area of ​​the container having the barrier label to the total surface area of ​​the container. In addition, handling of the container is improved with such a length to diameter ratio. Finally, transporting containers is facilitated by this elongated shape.

[0028] According to a fourth aspect, the invention relates to a method for manufacturing a container for food or pharmaceutical liquid, which comprises:

[0029] - a step of molding an empty tube in a mold with a molten plastic material, during which a barrier label comprising a material more impermeable to at least one gas than the molten plastic material is held in the mold during the injection of the molten plastic material,

[0030] - a tube filling step and

[0031] - a step of sealing the tube, by welding a seal on the mouth of the tube.

[0032] Advantages, aims and particular characteristics of this method being similar to those of the container which is the subject of the first aspect of the invention, they are not recalled here.

[0033] In embodiments, during the tube molding step, the barrier label is held in position by suction through the outer wall of the mold. The barrier label is thus located on the outer surface of the tube wall, which facilitates reading of the decoration and the inscriptions or codes it carries.

[0034] In embodiments, during the tube molding step, the suction holding the barrier label in position is performed via at least one suction channel whose smallest empty dimension is between 5 and 15 microns. The molten material in the mold cannot therefore enter the suction channel, in particular when this material is polypropylene.

[0035] In embodiments, during the tube molding step, the suction holding the barrier label in position is performed by means of at least one annular suction channel located in a plane perpendicular to an axis of rotational symmetry of the outer wall of the mold, the channel having a dimension measured parallel to this axis, between 5 and 15 microns. The annular arrangement of the suction channel ensures the position of the label on the outer surface of the tube, around the entire circumference of the tube.

[0036] In embodiments, during the tube molding step, at least two annular suction channels are used, positioned near the ends of the tube to be molded. These two annular channels are sufficient to retain the entire surface of the label on the external surface of the wall of the tube being molded.

[0037] In embodiments, during the tube molding step, the annular channels are formed in an interposed manner between a bezel and a die, each bezel being movable relative to the die, between a position distant from the die, implemented during a step of introducing the label into the mold and a position closer to the die, implemented during the injection of the molten plastic material into the mold. The suction of the label towards the external wall of the mold is thus greater before injection, which guarantees optimal positioning of this label.

[0038] In embodiments, during the tube molding step, a stripper carrying a spindle is used, the movement of the stripper causing the glasses and the matrix to come together. The narrowing of the section of each suction channel is thus automatic.

[0039] In embodiments, during the tube molding step, the mouth of the tube is molded into an annular groove of a stripper. This facilitates removal of the molded tube from one side of the mold and from the stripper on the other side.

[0040] According to a fifth aspect, the invention relates to a method for manufacturing a container for food or pharmaceutical liquid, which comprises:

[0041] - a step of molding an empty tube having, at least at its mouth, a longitudinal axis of rotational symmetry, the tube having, at this mouth, a sectional surface perpendicular to the axis of rotational symmetry, reduced compared to sections of the tube perpendicular to the axis of rotational symmetry further from the mouth,

[0042] - a tube filling step and

[0043] - a step of sealing the tube, by welding a seal on the mouth of the tube.

[0044] Advantages, aims and particular characteristics of this method being similar to those of the container which is the subject of the second aspect of the invention, they are not recalled here.

[0045] In embodiments, during the sealing step, the tube is sealed by magnetic induction and pressurizing the seal onto the mouth of the tube. Thanks to this induction, only the seal heats up directly. This avoids heating of the air trapped in the tube and a risk of the seal coming loose.

[0046] In embodiments, during the sealing step, a sealing machine is used that is configured so that the magnetic induction flux is reduced, facing the inside of the tube, relative to the magnetic induction flux facing the wall of the tube. Thus, heating is focused on the portion of the seal in contact with the wall of the tube, which further reduces heating of the air inside the tube. In embodiments, during the sealing step, a sealing machine is used that is configured so that the magnetic induction flux is higher facing the inner wall of the mouth of the tube than facing the outer wall of the mouth of the tube. Thus, the material of the tube melts more quickly on the inside of the tube, which promotes the formation of the internal meniscus mentioned above.

[0047] In embodiments, during the sealing step, a sealing punch is used to pressurize the seal, and, once the magnetic induction is complete, the punch is kept under pressure on the seal. Thus, the seal and the molten material of the tube are rapidly cooled by the punch.

[0048] In embodiments, during the sealing step, the punch is cooled by injecting air through a channel in the punch used to suction the seal before it is placed on the mouth of the tube. Thus, the design, manufacture and operation of the punch are simplified and the efficiency of its cooling is improved.

[0049] In embodiments, during the tube molding step, the mouth of the tube is molded into an annular groove of a stripper. This facilitates removal of the molded tube from one side of the mold and from the stripper on the other side.

[0050] According to a sixth aspect, the invention relates to a method for constituting a container of a food or pharmaceutical liquid without preservative, which comprises:

[0051] - a step of molding a tube made of synthetic material provided with a barrier label molded together with the tube,

[0052] - a step of filling this container with the preservative-free liquid,

[0053] - a step of sealing this filled container by placing a lid, and

[0054] - a step of sterilization or tyndallization of the liquid.

[0055] Advantages, aims and particular characteristics of this method being similar to those of the container which is the subject of the third aspect of the invention, they are not recalled here.

[0056] In embodiments, the sterilization or tyndallization step is a tyndallization step carried out in an autoclave by heat treatment with a temperature below 100°C and a duration of at least one hour reproduced three times at 24-hour intervals.

[0057] In embodiments, the tyndallization step comprises, three times at 24-hour intervals:

[0058] - a preheating step of a double wall of the autoclave,

[0059] - an initial step of vacuuming the autoclave chamber, to extract the maximum amount of air from the chamber,

[0060] - a moderate steam injection step while the vacuum continues to replace all the air initially present in the chamber with saturated steam,

[0061] - a step of heating the container by more powerful injection of steam to obtain a predetermined temperature and a predetermined pressure, - a step of maintaining the temperature and pressure of the chamber, by controlling the pressure of the chamber by balancing the injection of steam and the evacuation of the atmosphere, in such a way that the temperature is regulated,

[0062] - a final step of vacuuming the autoclave chamber.

[0063] Inactivation of pathogens potentially present in the container is thus sufficient. In embodiments, the predetermined temperature is between 70°C and 75°C.

[0064] The particular characteristics of the containers which are the subject of the first three aspects and the particular steps of the methods which are the subject of the fourth to sixth aspects of the invention are intended to be combined to form other embodiments of the container and the method which are the subject of the invention.

[0065] BRIEF DESCRIPTION OF THE FIGURES

[0066] Other advantages, aims and characteristics of the invention will emerge from the description which follows, given for explanatory and in no way limiting purposes with regard to the appended drawings, in which:

[0067] Figure 1 represents, in axial section, a particular embodiment of a closed container which is the subject of the invention,

[0068] Figure 2 represents a section marked in Figure 1, of the container illustrated in Figure 1,

[0069] Figure 3 shows, in top view, a temperature distribution on the circular surface of a lid during the sealing of a container,

[0070] Figures 4 to 6 represent, in section, three variants of a mouth part, before sealing, of the container illustrated in Figures 4 to 7,

[0071] Figure 7 shows, in section, the mouthpiece part illustrated in one of Figures 8 to 10, after sealing,

[0072] Figures 8 to 12 schematically represent five stages of a particular molding of a container in a molding machine,

[0073] Figures 13 and 14 schematically represent a capping machine before welding and during welding of a lid on a container,

[0074] Figure 15 represents a timing diagram for activating components of a sealing machine implemented in a particular embodiment of the method which is the subject of the invention,

[0075] Figure 16 represents, in the form of a flowchart, steps in a process for manufacturing a container,

[0076] Figures 17 to 20 are photographs taken respectively on the first, third, sixth and eighth days of a comparative stability monitoring, and

[0077] Figure 21 is a photograph of the mouths of a tube to be capped, a capped tube and a tube after removal of the cap.

[0078] DESCRIPTION OF EMBODIMENTS

[0079] Throughout the description, the following terms are used: - “Monodose”: a single-dose container made of synthetic material.

[0080] - “Unit filling”: action of filling the single-dose unit by unit, controlling the quantity of liquid inserted into the single-dose.

[0081] - “Collective filling”: action of filling single doses collectively.

[0082] - “Sterilization”: heat treatment at a temperature above 100°C and lasting between 12 and 30 min.

[0083] - “Tyndallization”: heat treatment at a temperature below 100°C (generally 70°C) for a duration of 60 mm, repeated 3 times at 24-hour intervals (Used for heat-sensitive raw materials and active ingredients).

[0084] - “Barrier”: term used to describe the absence of porosity to oxygen in materials.

[0085] In Figure 1, we observe a container 20 (also called “monodose” below), according to a section BB identified in Figure 2. This monodose 20 comprises a tube 21 containing a liquid 22. The tube 21 is geometrically defined, at least at its mouth, for the outside of the tube, by generatrices of a cylinder or a cone called “external” and, for the inside of the tube, by generatrices of a cylinder or a cone called “internal”. The tube 21 has a longitudinal axis 27 of rotational symmetry.

[0086] The lower opening of the tube 21 is closed by a molded wall 23. The upper opening of the tube 21 is closed by a cover 25 which a consumer can remove without tools to consume the liquid 22. The cover 25 protrudes, towards the outside of the tube 21, the external generatrices of the tube 21. The wall of the tube 21 contains a barrier label 24. Preferably, the label 24 and the cover 25 jointly cover at least 80% of the surface of the container.

[0087] 20 and, even more preferably, at least 90% of this surface.

[0088] Figure 2 represents the section AA identified in Figure 1, of the single-dose 20. The barrier label 24 supports a “decoration” representing, in particular, the mandatory legal information on a container of consumable foodstuff. In this particular embodiment, and preferably, the label 24 is an IML label (acronym for “InMould Labeling”), which allows a four-color decoration to be obtained. Thanks to this type of label 24, the tube 21 can be molded in “crystal” polypropylene, therefore without additives, which constitutes a significant qualitative advantage for a container of consumable foodstuff. This IML label 24 makes it possible, since it is manufactured with a “barrier” support, to solve the problem of porosity of polypropylene containers, which can lead, among other things, to oxidation of the components of the liquid 22. Preferably, in order to limit the problems of sealing, the tube

[0089] 21 is relatively long (more than 100 millimeters) and narrow (less than 20 millimeters and preferably less than 17 millimeters), for a liquid volume 22 of 15 ml.

[0090] The manufacturing of 15 ml single-dose containers in pharmaceutical grade polypropylene sealed using a co-extruded aluminum seal with a polypropylene layer is described below. The assembly of these materials ensures the perfect seal of the container, despite the stress due to the sterilization process, while allowing tool-free opening for the consumer, and respecting production rate constraints. Note that the use of a direct thermal head is impossible on a filled container, because the heat necessary for the fusion of the materials spreads to all parts near the punch, i.e. the moving part of the thermal head which comes into contact with the seal. This punch combines the functions of cutting the co-extruded aluminum ribbon with a polypropylene layer, during passage through the die, transporting the seal in contact with the container and maintaining it during sealing and cooling.Note that this punch is the only part that is in contact with the seal, outside of the container.

[0091] With a thermal head, heating the residual air chamber below the seal causes an increase in pressure in the tube, which in turn generates a thrust on the seal during heating. When the punch is removed from the head, while the polypropylene is still molten, this thrust causes the seal to detach. A seal cannot therefore be obtained.

[0092] In the embodiment detailed here, an induction sealing head is used. With this technology, the seal becomes the hot part. The induction field is directed primarily towards the peripheral parts of the seal that are opposite the thickness of the tube at its mouth, in order to focus the heat generation on these parts. This has the effect of limiting the heating of the air chamber inside the tube. To obtain this local heating, the magnetic field lines are opposed in the center of the seal, with a part of low relative magnetic permeability, a diamagnetic part or a magnet whose field lines are opposite the electrically induced magnetic field. Alternatively, two parallel magnetic fields of opposite directions are induced on the central part of the seal, for example with two coaxial coils of different diameters traversed by currents in opposite directions.

[0093] Furthermore, once the fusion, and therefore the assembly, has been carried out, the induction is stopped and the head punch preferably remains under pressure until the polypropylene cools and hardens. Since the polypropylene is no longer molten when the punch is withdrawn, and the relative air pressure inside the tube is almost zero, the risk of disturbing the connection between the tube and the seal is thus eliminated. The resulting seal is thus controlled.

[0094] In addition, the use of this induction sealing technology allows for a higher throughput and eliminates the need for temperature management (preheating, cooling and heating control throughout production) required by other technologies.

[0095] In Figure 13, a sealing machine 80 is shown schematically in its rest configuration, before cutting a seal and welding this seal onto a container 21. The machine 80 comprises a punch 81, movable in translation along a vertical axis 88 and provided, on its axis, with a channel 82, for suction to retain a cut seal 25, or for blowing air to cool the punch 81. In its vertical translation movement, the punch 81 is guided by a punch guide 83. Between this punch guide 83 and a cutting die 84, a film 85 of metal coextruded with a layer of the same plastic material as the tube 21 moves in horizontal translation. Preferably, this metal is aluminum and the coextruded plastic material is polypropylene. The aluminum is on the upper side of this film.This film 85 moves by a step corresponding to a little more than the diameter of the cover 25, each time the punch 81 is in its rest configuration illustrated in figure 13.

[0096] Below the die 84 are successively a support 86 and an inductor 87. A tube 21, containing the liquid 22 and provided with the label 24, is positioned below the support 86. During the descent of the punch 81, it cuts a cover 25 in the film 85 and makes it descend to bear on the tube 21 which remains fixed, as illustrated in figure 14. The inductor 87 causes heating of the cover 25 in its contact zone with the mouth of the tube 21. This heating causes the melting of the material of the tube 21 and the welding of the cover 25 on this mouth. During this melting, the tube 21 is kept under pressure on the cover 25 to ensure the formation of the meniscus 34.

[0097] The welding of the cover 25 on the tube 21 thus comprises a meniscus 34 on the internal wall of the tube 21 inside the volume defined by the internal generatrices of the tube 21. The volume of this meniscus 34 is at least twice the volume of any meniscus on the external wall of the tube 21, outside the volume defined by the external generatrices of the tube 21.

[0098] The heating and temperature control concerns the seal 25 and the punch 81. In fact, the punch 81 is cooled during periods of inactivity of the inductor 87, with the help of an injection of compressed air. This prevents the punch 81 from tending to heat up during the sealing process of thousands of containers 20.

[0099] Figure 15 illustrates, on a timing diagram 50, the operating phases of different members of the machine 80, over a cycle of placing a cover 25 on a tube 21 to form a container 20. Curve 51 represents, on the one hand, the instants during which the punch 81 is in the rest position, curve 51 taking its high value there, and, on the other hand, the instants during which the punch is moving or in its low position, curve 51 taking its low value there. Curve 52 represents the instants during which the air cooling of the punch 81 is activated, curve 52 taking its high value there. Curve 53 represents the instants during which the cover 25 is cut and moved, curve 53 taking its high value there. Curve 54 represents the instants during which the suction of the cover 25 is carried out via the channel 82, curve 54 taking its high value there.Curve 55 represents the instants during which the seal 25 is moved until it comes into contact with the tube 21, curve 55 taking its high value there. Curve 56 represents the instants during which the seal 25 is in contact with the tube 21, curve 56 taking its high value there. Curve 57 represents the instants during which the inductor 87 is activated, curve 57 taking its high value there. It is observed that, for a duration 58, the seal 25 is kept in contact with the tube 21 and in contact with the punch 81, while the inductor 87 is inactive. This duration 58 allows the cooling of the seal 25 and the molten material of the tube 21, by the punch 81, which remains at a temperature lower than the melting temperature of this material. For example, the heating time of the cover 25 by the inductor 87 is about 0.7 seconds for a three-second cycle. Thus, up to 2.3 seconds of a cycle are devoted to cooling.The punch 81 thus quickly acquires its optimum temperature, after approximately two or three cycles. Preferably, during these two or three initial cycles, the values ​​of the parameters increasing the heating of the seal 25 are slightly increased, to compensate for the lower temperature of the punch 81, and to avoid discarding the first sealed containers 20 at the start of production.

[0100] The management of the values ​​of the power and duration parameters of the phases, combined with air cooling during the intermediate phases between two induction phases during each cycle, makes it possible to guarantee the reproducibility of the operations throughout the production period with very high precision. More precisely, the cooling of the cover 25 and the punch 81 is done by injecting air through the punch 81 during the intermediate phases between two induction phases.

[0101] The air injection is carried out through the channel 82 of the punch 81 used for the suction of the seal 25, which makes it possible to keep the seal 25 perfectly centered during the movement of the punch 81 between the die 84 and the mouth of the tube 21 to be sealed.

[0102] Preferably, during heat sealing, the direction of diffusion of the material of the container is controlled, after melting. This prevents the creation of excess material outside the volume defined by the generatrices of the cylindrical or conical tube. Indeed, these excess materials can rise up onto the seal by capillarity. They therefore risk causing a significant increase in the outside diameter of the tube, a coarse result and a risk of cutting the lips of the consumer who brings the mouth of the container 20 to his lips. In addition, these excess materials would increase the sealing surface of the seal and, consequently, significant difficulties for the consumer to open the container.

[0103] In the container 20 detailed here, the quantity of material at the periphery of the container is preferentially reduced before heat sealing, as illustrated in figure 4: the internal diameter of the tube is, before sealing, identical over the entire length of the tube 21, including its mouth, but the external diameter of the tube 21 is reduced near the mouth.

[0104] In geometric terms, the last section of the mouth of the tube 21 perpendicular to the axis 27 of rotational symmetry, is separated from the external generatrices of the mouth of the tube 21, by a distance, measured on an axis of this section passing through the axis of rotational symmetry, at least equal to one fifth of the distance between the internal generatrices and the external generatrices, i.e. the thickness of the tube 21. Consequently, the surface area of ​​the section of the tube 21 perpendicular to the axis 27 of rotational symmetry is reduced, compared to sections of the tube perpendicular to the axis 27 of rotational symmetry further away from this mouth.

[0105] In Figure 4, the reduction in the external diameter, in the form of a shoulder 30, is 0.5 millimeters. The thickness of the tube 21 thus goes from 1.00 millimeters to 0.75 millimeters over the last half-millimeter of the tube 21 preceding its upper end. More generally, the longitudinal dimension of the part having a reduced external diameter is preferably less than two millimeters and this reduction in diameter is less than half the thickness of the tube. The external shoulder 30 located near the mouth of the tube 21 reduces, at this mouth, the surface area of ​​the section of the tube 21 perpendicular to the axis 27 of rotational symmetry, compared to sections of the tube 21 perpendicular to the axis 27 further away from the mouth.

[0106] In other embodiments, the reduction in diameter at the mouth is progressive, for example in the form of several successive shoulders 31 and 32, as illustrated in Figure 5, or in the form of a cone 33 forming, in section, a bevel on each edge of the tube 21, as illustrated in Figure 6. The conical shape 33 reduces, at the mouth, the surface area of ​​the section of the tube 21 perpendicular to the axis 27 of rotational symmetry, compared to sections of the tube 21 perpendicular to the axis 27 further from the mouth. Preferably, the length, parallel to the axis 27, of the zone in which the surface area of ​​the section of the tube 21 perpendicular to the axis 27 is reduced, compared to sections of the tube 21 perpendicular to the axis 27 further from the mouth, is less than two millimeters.

[0107] As illustrated in Figure 7, thanks to the reduction in the external diameter of the tube 21 at its mouth, during induction heating, a meniscus, or bead, of material 34 is created inside the tube 21, which adheres to the cover 25. On the outside of the tube 21, the material of the tube which melts does not exceed, or very little, the generatrices of the cylinder or cone defining the tube 21. This provides good adhesion of the cover 25 to the tube 21 while avoiding the formation of an unsightly external edge likely to injure the consumer's lip when consuming the liquid 22.

[0108] In figure 21, a photograph shows, from left to right, the mouths of a tube 21 to be capped, of a capped tube and of a tube after removal of the cap 25. There we see the shoulder 30, at the mouth of the tube 21 to be capped, and the meniscus 34, at the mouth of the tube after removal of the cap, by hand, without tools.

[0109] As can be understood from reading the preceding description, the reduction in diameter of the tube 21 at its mouth makes it possible to absorb the excess molten material while remaining within the outer perimeter of the generatrices of the tube 21, cylindrical or conical.

[0110] The induction flow is oriented so that the melting takes place preferentially on the seal facing the internal wall of the tube 21, the part of the seal facing the external wall of the tube receiving a lower induction flow and therefore heating up less. Figure 3 shows, in top view, a temperature distribution on the circular surface of a seal during the sealing of a container. The circular dashed line 26 represents the initial contact surface of the wall of the tube 21 with the seal 25. The material, for example polypropylene, is therefore softer on the internal wall of the mouth of the tube 21 and is therefore pushed towards the inside of the tube 21, while the external wall of the mouth of the tube, which is more rigid, does not deform beyond the generatrices of the tube 21.

[0111] Each of the sealing measures set out above makes it possible to increase the contact surface between the tube 21 and the seal 25 for better sealing, without degrading the ease of use of the seal 25 during opening. Finally, the use of this peripheral induction technology reduces space requirements and allows the multiplication of workstations on industrial equipment.

[0112] We will now describe, with reference to figures 8 to 11, a molding machine 40 and the steps of molding the tube 21 comprising, in its thickness, the IML label 24. It is noted that these steps lead to the production of a tube 21 oriented in the opposite direction to its representation in figures 1 to 7, that is to say with its mouth at the bottom.

[0113] In Figure 8, in the molding machine 40, we observe a fixed part comprising an injection module 41, a bezel 42, a “Venturi” suction channel 43 between the bezel 42 and a die 44 and a “Venturi” suction channel 45 between the die 44 and a bezel 45. Below this fixed part is shown a label 24 held by a cylindrical removal tool (not shown) to have a diameter smaller than the diameter of a cavity 49 of the fixed part passing through the bezels 42 and 45 and the die 44 and ending under the injection module 41. Below the label 24 is shown a stripper 48 carrying a pin 47. As shown by the arrows in Figure 8, the label 24 and the pin 47 are intended to penetrate into the cavity 49. The difference in radius between the pin 47 and the cavity 49 thus corresponds to the thickness of the tube to be molded.

[0114] In Figure 8, the mold comprising the die 44 and the glasses 42 and 45 is in the open position and the label 24 is waiting to be introduced into the cavity 49 of the mold. The glasses 42 and 45 are spaced from the die 44 so as to create a gap of two millimeters for the suction channels 43 and 46. The stripper 48 is in the open position.

[0115] The positioning of the label 24 in the cavity 49 is carried out by a Cartesian robot (not shown). This robot will retrieve the label 24 from a distribution magazine (not shown). The label 24 is wrapped around the cylindrical installation tool (for example with a diameter of 15 mm). The label 24 is held on this removal tool by vacuum. The width of the label 24 and the diameter of the removal tool are linked. The diameter of the removal tool must necessarily be less than the diameter of the cavity. The label must be held over its entire surface, therefore its width must be less than or equal to the perimeter of the removal tool: if its width were greater than the perimeter of the removal tool, the additional label, called "overlap", would come into contact with the cavity 49 of the mold when the label 24 is introduced.

[0116] The robot then presents itself in front of the mold cavity 49 when the latter is in the open position. The removal tool introduces the label 24 into the mold cavity 49 (for example, with a diameter of 16.9 mm). Once the label 24 has arrived in position, the depression exerted by the removal tool is stopped and replaced by an injection of air to detach the label 24 from the removal tool and press it against the wall of the cavity 49. The label 24 is then held in place using the two suction channels 43 and 46 positioned near the ends of the cavity 49. These venturis are obtained by breaking down the cavity 49 into three parts. The bottom part, the injection module 41, which supports the injection nozzle, is fixed. The central part, which is conical and perfectly smooth, corresponds to the die 44. The lower part is cylindrical. The depression is created using channels 43 and 46 which are formed at the junction of these three parts.However, the second and third parts are slightly movable. When the mold is open, each of these parts is spaced 2 mm from the previous one, so that the suction power is maximum. Once the label 24 is in place, the removal tool is removed and the mold can close. When it closes, the mold compresses the second and third parts to reduce the size of the venturi channels to a minimum (between 5 and 13 microns). In the case of polypropylene injection, the dimension of 13 microns is the maximum size that allows for suction to hold the label without allowing the polypropylene to be sucked in and clog the channels 43 and 46 after a few injections.

[0117] In Figure 9, the label 24 is positioned in the cavity 49 of the mold and the mold is being closed. The suction channels 43 and 46 are still in the open position. The suction they provide holds the label 24 in a cylindrical configuration against the wall of the cavity 49. This prevents the distance between the label 24 and the wall of the cavity 49 from varying according to the parts of the label 24. The stripper 48 is in the closed position. It presses on a cone of the spindle 47 to ensure its perfect centering and prevent the thickness of the tube to be molded from varying according to the angle around its longitudinal axis.

[0118] In Figure 10, the stripper 48 has inserted the pin 47 into the cavity 49. The suction channels 43 and 46 are closed by the thrust of the stripper 48, so that each channel 43 and 46 has an opening, measured parallel to the axis of the cavity, limited to a value between five and fifteen microns, typically eight or nine microns. The injection of the material begins to be carried out by the injection module 41.

[0119] In Figure 11, the mold is still closed and in the same configuration as in Figure 10. The injection is complete. The die 44 and the spindle 47 are cooled by internal circulation of a refrigerated fluid. In Figure 11, for explanatory purposes, the tube 21 is shown in dashed lines.

[0120] Once cooling is complete, the stripper 48 and the mold return to the position illustrated in Figure 1, as illustrated in Figure 12. It can be seen in Figure 12 that the tube 21 is detached from the spindle 47 by sliding the spindle 47 downwards in the stripper 48. Once the tube 21 is removed from the spindle 47, the cycle begins again with the positioning of a label 24 opposite the cavity 49, as illustrated in Figure 1. The complete cycle lasts approximately ten seconds. It can also be seen in Figure 12 that the shoulder 30 has been molded into an annular cylindrical groove 59 of the stripper 48. This particular characteristic has, among other advantages, that the label 24, held in position in the cavity 49, is moved away from the molded sealing zone in the stripper.

[0121] The tube 21 is conical, with a generatrice angle of 0.2 degrees to 0.4 degrees relative to the longitudinal axis of the tube 21. This is a physical requirement for the molded parts. Technically, this is a draft. This draft allows the moving parts of the mold to very quickly no longer be in contact with the molded part when the mold is opened. Without this draft, the frictional stresses would be too high and the damage to the molded parts too. The thickness is almost constant over the entire length of the tube, for example, approximately 0.8 millimeters. However, approximately 14 millimeters from the end of the tube 21, the draft is abandoned to change to a cylindrical profile. Thus, a thickness of one millimeter is obtained at the rim of the container, before the shoulder 30. These geometric characteristics have several advantages.On the one hand, the thickness of one millimeter is preferable to obtain the quantity of material necessary for sealing the cover 25. In addition, it is the surface on which the stripper 48 rests to detach the tube 21 from the pin 47 when opening the mold shown in figure 12. The fact of going to 0.8 millimeters, outside this zone defined to meet these constraints, makes it possible to save weight of material injected into the mold.

[0122] The molded wall 23 is the material injection part. The profile of this part is very technical. The "skirt" which protrudes from the wall 23 of the tube 21 is a so-called "thief" bottom.

[0123] The objective of implementing the elements shown in figures 8 to 12 is to enable the positioning and maintenance of the label 24. This also allows the injection flow of the material to meet the label 24 perpendicularly in order to press the start of the label against the wall of the cavity 49 of the mold.

[0124] As understood from reading the description given with regard to figures 8 to 12, preferably, a mold is used which holds the label 24 using air suction ("Venturi"). Since the label 24 does not cover the entire circumference of the tube 21, each annular channel 43 and 46 of each venturi must be wide enough to allow the passage of air and ensure a sufficient suction effect, without however allowing the suction of material which would block this channel 43 or in the event of absence or lack of integrity of the label 24 during injection. Preferably, the longitudinal dimension of each annular channel 43 and 46 is between 5 and 15 microns. At least two venturi suction channels are arranged on each external mold, near the ends of the internal cavity 49 of this mold.

[0125] The moving part of the mold that closes is made up of the pin 47, which determines the internal profile of the tube 21 of the single-dose, and the stripper 48 which is the last part of the mold (as far as the parts in contact with the molded part are concerned). This stripper 48 has several functions. The positioning of the label 24 is done with a small offset to prevent the removal tool from coming into conflict with the bottom (at the top in figure 9) of the cavity 49. The stripper 48 makes it possible to push the label 24 to the bottom of the cavity 49 and its precise positioning.

[0126] It is also the stripper 48 which creates the particular profile of the rim (material removal shoulder to allow the sealing of the cover 25 without material overflow). The stripper 48 also allows the pin 47 to be precisely centered during injection. Finally, it allows the tube 21 to be detached from the pin 47 when the mold is opened.

[0127] The mechanical part which supports the removal tool, on its front face, is equipped with a gripper, on its rear face. When the mold is opened again, this gripper catches the molded tube 21, previously detached from the pin 47 as shown with reference to figure 12. The actions of removing the label 21 and recovering the molded tube 21 are therefore carried out simultaneously, while the mold is opening. This step only lasts 2 to 3 seconds. The injection and cooling steps last 7 to 8 seconds, with 5 to 6 seconds only for cooling.

[0128] Below are some possible technical specifications for the IML label: barrier material, multi-layer cast polypropylene (CPP) film (Polypropylene / Ethylene-vinyl alcohol EVOH / Polypropylene), with a thickness between 50 microns and 80 microns, for example 65 microns.

[0129] In embodiments and as illustrated in FIG. 16, the method 60 for constituting a container 20 for packaging a preservative-free liquid comprises:

[0130] - the manufacture of a container made of synthetic material provided with an IML label, step 61, preferably as set out with regard to figures 8 to 12,

[0131] - filling this container, step 62,

[0132] - the sealing of this filled container, step 63, preferably by induction and more particularly by peripheral induction as explained with regard to figures 3 to 7 and 13 to 15, and

[0133] - sterilization or tyndallization of the contents (in particular by autoclave), step 64.

[0134] Preferably, this method 60 for manufacturing a container 20 of food or pharmaceutical liquid 22, comprises:

[0135] - a step 61 of manufacturing an empty tube 21 having, at least at its mouth, a longitudinal axis 27 of rotational symmetry, the tube having, at this mouth, a sectional surface perpendicular to the axis of rotational symmetry, reduced compared to sections of the tube perpendicular to the axis of rotational symmetry further from the mouth, and / or

[0136] - a step 61 of molding an empty tube 21 in a mold 41 to 46 with a molten plastic material, during which, a barrier label 24 comprising a material more impermeable to at least one gas than the molten plastic material is maintained in the mold during the injection of the molten plastic material.

[0137] Preferably, during the sealing step 63, the tube 21 is sealed by magnetic induction and pressure applied to the seal on the mouth of the tube.

[0138] Preferably, during the sealing step 63, a sealing machine 80 is used, configured so that the magnetic induction flux is reduced, facing the inside of the tube 21, compared to the magnetic induction flux facing the wall of the tube. Preferably, during the sealing step 63, a sealing machine 80 is used, configured so that the magnetic induction flux is higher facing the inner wall of the mouth of the tube 21 than facing the outer wall of the mouth of the tube. Preferably, during the sealing step 63, a sealing punch 81 is used, pressurized on the seal 25, and, once the magnetic induction is complete, the punch is kept under pressure on the seal.Preferably, during the sealing step 63, the cooling of the punch 81 is done by injecting air through a channel 82 of the punch used for the suction of the cover 25 before it is placed on the mouth of the tube 21.

[0139] Preferably, during step 61 of manufacturing the tube 21, the mouth of the tube is molded in an annular groove 59 of a stripper 48.

[0140] Preferably, during step 61 of molding the tube 21, the suction holding the barrier label 24 in position is carried out by means of at least one suction channel 43, 46 whose smallest empty dimension is between 5 and 15 microns.

[0141] Preferably, during step 61 of molding the tube 21, the suction holding the barrier label 24 in position is carried out by means of at least one annular suction channel 43, 46 located in a plane perpendicular to an axis 27 of rotational symmetry of the external wall of the mold, channel whose dimension measured parallel to this axis is between 5 and 15 microns. Preferably, during step 61 of molding the tube 21, at least two annular suction channels 43, 46 are used, positioned near the ends of the tube 21 to be molded.

[0142] Preferably, during step 61 of molding the tube 21, the annular channels 43, 46 are formed in an interposed manner between a bezel 42, 45 and a die 44, each bezel being movable relative to the die, between a position distant from the die, implemented during a step of introducing the label 24 into the mold 41 to 46 and a position closer to the die, implemented during the injection into the mold of the molten plastic material. Preferably, during step 61 of molding the tube 21, a stripper 48 carrying a spindle 47 is used, the movement of the stripper causing the bezels 43, 46 and the die 44 to come together.

[0143] Preferably, during step 61 of molding the tube 21, the mouth of the tube is molded in an annular groove 59 of a stripper 48.

[0144] Preferably, the sterilization or tyndallization step 64 is a tyndallization step. Tyndallization is a heat treatment carried out by an autoclave using a time / temperature exposure ratio. This heat treatment is carried out with a temperature below 100°C and, for example, a duration of at least one hour reproduced three times at 24-hour intervals.

[0145] Preferably, step 64 of tyndallization comprises, three times at 24-hour intervals:

[0146] - a preheating step of a double wall of the autoclave,

[0147] - an initial step of vacuuming the autoclave chamber, to extract the maximum amount of air from the chamber,

[0148] - a moderate steam injection step while the vacuum continues to replace all the air initially present in the chamber with saturated steam,

[0149] - a step of heating the container 20 by more powerful injection of steam to obtain a predetermined temperature and a predetermined pressure, - a step of maintaining the temperature and pressure of the chamber, by controlling the pressure of the chamber by balancing the injection of steam and the evacuation of the atmosphere, in such a way that the temperature is regulated,

[0150] - a final step of vacuuming the autoclave chamber.

[0151] Preferably, the predetermined temperature is between 70°C and 75°C.

[0152] In the manufacturing unit, empty tubes are loaded in bulk by an operator at the line entrance and the filled tubes, sealed and stored on a support of multitudes of tubes, are received by this operator at the exit. The production line includes:

[0153] - automatic feeding of empty tubes (unpicking, grouping on a motorized conveyor with suction, positioning in packaging buckets),

[0154] - the filling,

[0155] - the sealing, and

[0156] - placing on a support for sterilization or tyndallization.

[0157] Regarding sterilization or tyndallization, autoclaves are preferably used. These are rectangular tunnels with a sealed door on each side. The load is introduced on one side and removed on the other. They have a volume of several cubic meters. For operation, the goal is to apply a precise and controlled temperature to each container (several tens of thousands for a load) for a variable duration depending on the chosen temperature; this is the time / temperature exposure ratio mentioned above.

[0158] There are two types of treatment: those with a temperature below 100°C (minimum 70°C) which are called "tyndallization" and those above 100°C (maximum 121°C) which are called "sterilization";

[0159] The first steps are the same for both types.

[0160] 1 - Preheating the double wall.

[0161] 2 - Initial vacuum which aims to extract the maximum amount of air from the chamber (typically 90%).

[0162] 3 - Vacuum and moderate steam injection to improve the quality of the chamber atmosphere. Steam is injected while the vacuum continues in the lower part of the chamber. In fact, all the cold air at the bottom of the chamber is extracted and eventually replaced by saturated steam. This will be important for maintaining the temperature during the plateau phase.

[0163] 4 - Heating the load by powerful injection of steam. The aim is to obtain the desired temperature at the same time as the desired pressure.

[0164] 5 - Treatment tray. This is the effective part of the cycle that allows us to obtain the result of reducing the initial bacterial load (Reduction by a factor of 10 to the power of 12 for a 12-minute cycle at 121°C).

[0165] To obtain the regularity of the plateau, we only play on the pressure of the chamber by balancing the injection of steam and the vacuum. It is the law of ideal gases, PV=nRT, which allows a regulation to the tenth of a degree in a very large volume, whatever the desired temperature (pressure below the relative pressure for 70°C, 0.34 bar in absolute, and higher for sterilization, 2.049 bars for 121°C according to the Régnault table) and the initial temperature of the injected steam (around 170°C in our case).

[0166] 6 - Either cooling with injection of cold purified water then draining for sterilization, or final vacuum for tyndallization. Safety and legislation do not allow opening the autoclave if the internal temperature is higher than a limit temperature, for example 90°C. Sterilization generally lasts between 15 and 30 minutes (for example, for food supplements, 115°C can be applied for 20 minutes).

[0167] Tyndallization lasts 60 minutes and the cycle must be repeated three times at 24-hour intervals. The goal is to alternate periods of heat stress and rest for the bacteria, which have the ability to protect themselves in the event of an attack. They cannot change states several times. Therefore, the first pass stresses them and they can no longer protect themselves during the second pass. The third secures everything. Tyndallization is used for products whose active ingredients are heat-sensitive so that they are not destroyed during heat treatment (royal jelly or vitamins, for example).

[0168] STABILITY TESTS

[0169] Tests were carried out to compare the behavior of a packaged product:

[0170] - in 15 mL yellow glass ampoule,

[0171] - in single-dose PPS® 10 mL,

[0172] - in 15 mL single dose containing a colored IML label,

[0173] - in 15 mL single dose containing a white IML label,

[0174] - in single dose 15 mL without IML label.

[0175] These tests were carried out on Taurine Zinc Royal Jelly. The purpose of this study is to present the results in order to see the evolution of the product's color over time depending on the type of container. In order to avoid any microbiological risk that could alter the study, the manufacturing of the Taurine Zinc Royal Jelly and the filling into the different containers were carried out on the same day.

[0176] Five different containers were used for this study, namely:

[0177] - a 15 ml yellow glass ampoule. This is a container used on the market and known to be permeable to oxygen.

[0178] - a 10 ml PPS® single-dose container. This is a container available on the market and known not to be permeable to oxygen (the material used is not an oxygen barrier).

[0179] - the 15 ml single-dose containing a colored IML label, called “single-dose teaser”,

[0180] - the 15 ml single-dose containing a white IML label,

[0181] - the 15 ml single-dose without IML label.

[0182] The 15mL single-dose containers are composed of a PPMH350 polypropylene tube with or without an IML label and a coextruded aluminum and polypropylene seal. It should be noted that the In-Mould Labeling (IML) label allows for four-color decoration. It systematically has a white backing and has the advantage of being an oxygen barrier. The different samples underwent tyndallization at 70°C for one hour, and this for three successive days. All the containers were then inserted into cases and placed in an oven (oven temperature between 60°C and 75°C). Stability monitoring was carried out every two working days with a visual check of the color. Only the PPS® single-dose containers, opaque, were checked when a difference in color was observed between the other containers. Test procedure.

[0183] In terms of manufacturing, for technical and ergonomic reasons, two 750 mL preparations were produced:

[0184] - Manufacturing 1 = Test 1 A,

[0185] - Manufacturing 2 = Tests 1 B.

[0186] To avoid any cross-contamination, precautionary measures were put in place with bench cleaning between each test. All raw materials used were present in stock at the warehouse and had been released compliantly by the Quality Control laboratory. No anomalies were encountered during this stage.

[0187] Regarding filling, in order to avoid any microbiological risk, the filling and sealing of the containers were carried out on the same day as manufacturing. For the 15 mL yellow glass ampoules, the filling of these ampoules was carried out under a vacuum bell jar and the welding was carried out using a torch gun. 16 15 mL ampoules were filled. For the PPS® unit-doses, their filling was carried out manually using a pipette. 16 10 mL PPS® unit-doses were filled. For the 15 mL single-doses, their filling was carried out in accordance with good manufacturing practices. The single-doses were filled and sealed. The values ​​used for the adjustment parameters for sealing are presented below:

[0188] Ten single-dose containers with a colored IML label, ten single-dose containers with a white label, and ten single-dose containers without labels were filled. The filling steps were completed successfully; no anomalies occurred.

[0189] Regarding the heat treatment, as specified above, the different samples underwent tyndallization (70°C for 1 hour three days in a row). The heat treatment took place in a production environment governed by Good Manufacturing Practices. All applicable rules, described in the laboratory procedures, for heat treatment were applied for these stability tests. This heat treatment was carried out in an autoclave. No anomalies were encountered during this phase. For single-dose containers, a leak test by passing through a vacuum bell was carried out for verification.

[0190] Regarding stability and stability monitoring, the different cases were placed in the oven, in order to mimic accelerated stability conditions and thus be able to observe the behavior of the single-dose containers under the effect of heat (oven temperature between 60°C and 75°C). Stability monitoring was carried out with a visual check of the color on all the containers. It should be remembered that, since the PPS® single-dose container is opaque, it is only checked when a color difference is observed between the different containers.

[0191] The analysis of the results is given below. The stability monitoring for this study was carried out over 7 days. The results obtained are presented in relation to Figures 17 to 20. JO results: Figure 17, with, from left to right: ampoule 91, PPS® single-dose 92, teaser single-dose 93, white-label single-dose 94, IML unlabeled single-dose 95. No significant visual difference in color was observed between the different containers.

[0192] Results D+2: figure 18, with from left to right: ampoule 91, single-dose without IML label 95, single-dose teaser 93, single-dose white label 94. No significant visual difference in color was observed between the different containers.

[0193] Results D+5: figure 19, with, from left to right: ampoule 91, single-dose teaser 93, single-dose white label 94, single-dose without IML label 95, single-dose PPS® 92. Initial color differences were observed during these checks at D+5.

[0194] The results show:

[0195] - that the contents of the PPS® 92 single-dose containers are much darker than those of the other containers. This observation highlights that the material that makes up the PPS® 92 single-dose containers is very porous and does not protect the product. In fact, under the effect of heat, the product oxidizes much more quickly in this type of container.

[0196] - that the contents of the single-dose containers without an IML label are darker than the contents of the single-dose containers with a label, but are not as dark as the contents of the PPS® 92 single-dose containers. This observation highlights the fact that the IML label plays an extremely important role in protecting the product against external conditions. No significant visual difference in color was observed between the ampoule and the single-dose containers with an IML label.

[0197] Results D+7: Figure 20, with, from left to right: ampoule 91, single-dose teaser 93, single-dose white label 94, single-dose without IML label 95. The observations noted during the checks at D+7 are quite similar to those at D+5. There is little difference in color between the ampoule and the single-doses with IML label.

[0198] Stability studies have shown that the color changes faster in the single-dose container than in the ampoule, without having any impact on the organoleptic and physicochemical characteristics. Depending on the type of container selected, the evolution of the product over time is different. The PPS® single-dose container, although offering many advantages, is porous to air. The product, under the effect of heat, changes much faster than in the ampoule and / or the single-dose container. The single-dose container without an IML label is also porous to air. The presence of an IML label is important for the protection of the product against external conditions. The ampoule is the container that shows a slower color evolution than the single-dose container. However, it is useful to specify that the color evolution observed in the single-dose container with an IML label does not interfere with the organoleptic and physicochemical characteristics.

Claims

CLAIMS 1. Container (20) of food or pharmaceutical liquid (22) comprising a tube (21) made of plastic material geometrically defined, at least at its mouth, for the outside of the tube, by generatrices of a cylinder or a cone called "external" and, for the inside of the tube, by generatrices of a cylinder or a cone called "internal", this tube having a longitudinal axis (27) of rotational symmetry, this tube comprising said liquid, this tube being molded in a mold, characterized in that the tube comprises, in its side wall, a barrier label (24) comprising a material more impermeable to at least one gas than the plastic material of the tube, this barrier label being present in the mold during the molding of the wall of the tube.

2. Container (20) according to claim 1, wherein the label (24) is made of oxygen-tight material.

3. Container (20) according to one of claims 1 or 2, in which the label (24) and the seal (25) jointly cover at least 80% of the total surface area of ​​the container.

4. Container (20) according to one of claims 1 to 3, in which the plastic material of the wall of the tube (21) is "crystal" polypropylene without additive.

5. Container (20) according to one of claims 1 to 4, in which the barrier label (24) comprises a multi-layer cast polypropylene film, the successive layers comprising polypropylene, ethylene-vinyl alcohol EVOH and polypropylene.

6. Container (20) according to one of claims 1 to 5, in which the barrier label (24) has a thickness of between 50 microns and 80 microns.

7. Container (20) according to one of claims 1 to 6, which further comprises a seal (25) welded onto the mouth of the tube, this seal extending, towards the outside of the tube, beyond said external generatrices, the weld of this seal onto the tube comprising a meniscus (34) on the internal wall of the tube inside the volume defined by the internal generatrices, the volume of this meniscus being at least twice the volume of any meniscus on the external wall of the tube outside the volume defined by the external generatrices.

8. Container (20) according to claim 7, in which, before welding the cover (25), the last section of the mouth of the tube (21) perpendicular to the axis (27) of rotational symmetry, is separated from the external generatrices, by a distance, measured on an axis of this section passing through the axis of rotational symmetry, at least equal to one fifth of the distance between the internal generatrices and the external generatrices, the surface area of ​​the section of the tube perpendicular to the axis of rotational symmetry being reduced, compared to sections of the tube perpendicular to the axis of rotational symmetry further from the mouth.

9. Container (20) according to one of claims 7 or 8, in which the tube (21) has, before welding the cover (25), at least one external shoulder (30) near the mouth, this shoulder reducing, at the mouth, the surface area of ​​the section of the tube perpendicular to the axis of rotational symmetry, relative to sections of the tube perpendicular to the axis of rotational symmetry further from the mouth.

10. Container (20) according to one of claims 7 to 9, in which the tube (21) has, before welding the cover (25), at least one conical shape (33) reducing, at the mouth, the surface area of ​​the section of the tube perpendicular to the axis (27) of rotational symmetry, compared to sections of the tube perpendicular to the axis of rotational symmetry further from the mouth.

11. Container (20) according to one of claims 8 to 10, in which, before welding of the lid (25), the length, parallel to the axis (27) of rotational symmetry, of the zone in which the surface of the section of the tube perpendicular to the axis of rotational symmetry is reduced, compared to sections of the tube perpendicular to the axis of rotational symmetry further from the mouth, is less than two millimeters.

12. Container (20) according to one of claims 7 to 11, in which the cover (25) is made of coextruded metal with a layer of the same plastic material as the tube.

13. The container (20) of claim 12, wherein said metal is aluminum and said plastic material is polypropylene.

14. Container (20) according to one of claims 1 to 13, in which the liquid is a preservative-free liquid, the tube and this liquid undergoing a sterilization or tyndallization heat treatment.

15. Container (20) according to claim 14, wherein the dimension parallel to the axis of rotational symmetry of the container is greater than five times its maximum diameter.

16. Method (60) for manufacturing a container (20) of food or pharmaceutical liquid (22), characterized in that it comprises: - a step (61) of molding an empty tube (21) in a mold (41 to 46) with a molten plastic material, during which a barrier label (24) comprising a material more impermeable to at least one gas than the molten plastic material is held in the mold during the injection of the molten plastic material, - a step (62) of filling the tube and - a step (63) of sealing the tube, by welding a cover (25) onto the mouth of the tube.

17. Method (60) according to claim 16, wherein, during the step (61) of molding the tube (21), the barrier label (24) is held in position by suction through the external wall of the mold (41 to 46).

18. Method (60) according to claim 17, in which, during the step (61) of molding the tube (21), the suction holding the barrier label (24) in position is carried out by means of at least one suction channel (43, 46) whose smallest empty dimension is between 5 and 15 microns.

19. Method (60) according to one of claims 17 or 18, in which, during the step (61) of molding the tube (21), the suction holding the barrier label (24) in position is carried out by means of at least one annular suction channel (43, 46) located in a plane perpendicular to an axis (27) of rotational symmetry of the external wall of the mold, channel whose dimension measured parallel to this axis is between 5 and 15 microns.

20. Method (60) according to claim 19, in which, during the step (61) of molding the tube (21), at least two annular suction channels (43, 46) positioned near the ends of the tube (21) to be molded are used.

21. Method (60) according to one of claims 19 or 20, in which, during the step (61) of molding the tube (21), the annular channels (43, 46) are formed in an interposed manner between a bezel (42, 45) and a die (44), each bezel being movable relative to the die, between a position distant from the die, implemented during a step of introducing the label (24) into the mold (41 to 46) and a position closer to the die, implemented during the injection of the molten plastic material into the mold.

22. Method (60) according to claim 21, in which, during the step (61) of molding the tube (21), a stripper (48) carrying a spindle (47) is used, the movement of the stripper causing the glasses (43, 46) and the matrix (44) to come together.

23. Method (60) according to one of claims 16 to 22, in which, during the step (61) of molding the tube (21), the mouth of the tube is molded in an annular groove (59) of a stripper (48).

24. Method (60) according to one of claims 16 to 23, in which, at the end of the molding step (61), the empty tube (21) has, at least at its mouth, a longitudinal axis (27) of rotational symmetry, the tube having, at this mouth, a sectional surface perpendicular to the axis of rotational symmetry, reduced compared to sections of the tube perpendicular to the axis of rotational symmetry further away from the mouth.

25. Method (60) according to one of claims 16 to 24, in which, during the sealing step (63), the tube (21) is sealed by magnetic induction and pressurizing the seal on the mouth of the tube.

26. Method (60) according to claim 25, in which, during the sealing step (63), a sealing machine (80) is used, configured so that the magnetic induction flux is reduced, facing the interior of the tube (21), compared to the magnetic induction flux facing the wall of the tube.

27. Method (60) according to one of claims 25 or 26, in which, during the sealing step (63), a sealing machine (80) is used, configured so that the magnetic induction flux is higher opposite the internal wall of the mouth of the tube (21) than opposite the external wall of the mouth of the tube.

28. Method (60) according to one of claims 25 to 27, in which, during the sealing step (63), a sealing punch (81) is used, put under pressure on the cover (25), and, once the magnetic induction is finished, the punch is kept under pressure on the cover.

29. Method (60) according to claim 28, in which, during the sealing step (63), the cooling of the punch (81) is done by injecting air through a channel (82) of the punch used for suction of the seal (25) before it is placed on the mouth of the tube (21).

30. Method (60) according to one of claims 16 to 29, in which, during the step (62) of filling the tube, the liquid is a preservative-free liquid, a method which further comprises, after the step (63) of sealing this filled tube by welding a cover (25), a step (64) of sterilization or tyndallization of the liquid.

31. Method (60) according to claim 30, in which the sterilization or tyndallization step (64) is a tyndallization step carried out in an autoclave by heat treatment with a temperature lower than 100°C and a duration of at least one hour reproduced three times at 24 hour intervals.

32. Method (60) according to claim 31, in which the tyndallization step (64) comprises, three times at 24-hour intervals: - a preheating step of a double wall of the autoclave, - an initial step of vacuuming the autoclave chamber, to extract the maximum amount of air from the chamber, - a moderate steam injection step while the vacuum continues to replace all the air initially present in the chamber with saturated steam, - a step of heating the container (20) by more powerful injection of steam to obtain a predetermined temperature and a predetermined pressure, - a stage of maintaining the temperature and pressure of the chamber, by controlling the pressure of the chamber by balancing the injection of steam and the evacuation of the atmosphere, in such a way that the temperature is regulated, - a final step of vacuuming the autoclave chamber.

33. The method (60) of claim 32, wherein the predetermined temperature is between 70°C and 75°C.

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