FORM 2
THE PATENTS ACT, 1970
(39 of 1970)
As amended by the Patents (Amendment) Act, 2005
&
The Patents Rules, 2003
As amended by the Patents (Amendment) Rules, 2006
COMPLETE SPECIFICATION
(See section 10 and rule 13)
TITLE OF THE INVENTION
METHOD AND INSTALLATION FOR DEALKALIZING GLASS
CONTAINERS USING LIQUID
APPLICANT
SGD S.A., a French company, having its address at 14 bis Terrasse Bellini,
92800 PUTEAUX, France
PREAMBLE TO THE DESCRIPTION
The following specification particularly describes the nature of this invention and
the manner in which it is to be performed:
2
METHOD AND INSTALLATION FOR DEALKALIZING GLASS
CONTAINERS USING LIQUID
TECHNICAL FIELD
The present invention relates to the general technical field of methods and
5 installations for the treatment of glass containers, and more specifically the
technical field of methods and installations for dealkalization treatment of the inner
wall of glass containers.
PRIOR ART
In the field of pharmaceutical glass primary packaging, the purpose is to propose
10 containers, in particular of the vial type, that have an excellent chemical
compatibility with the product or preparation they are intended to contain. Indeed,
the aim is to prevent any harmful interaction between a species from the glass
forming the container and the product contained by the latter. In this respect, it is
known to subject glass containers, before their use, to a dealkalization treatment
15 that consists in extracting, over a depth of several dozens of nanometres, the
alkaline ions – and in particular the sodium ions – present in the vicinity of the
surface of the inner wall of the container, and evacuating them, in order to avoid as
much as possible the elution of the alkaline ions over time into the product
contained by the container. Such a treatment is generally carried out by introducing
20 into a glass container to be treated a solid or gaseous reactive substance that is
capable, under the action of heat, to generate an acid gas likely to chemically react
with the alkaline ions present in the glass of the container.
A dealkalization treatment method is known, which consists in introducing into a
hot glass container ammonium sulphate (NH4)2SO4 in solid form, for example in
25 the form of a crystalline powder or tablets, through a dispenser positioned above
the containers. Under the effect of heat, the ammonium sulphate sublimates and
3
forms a gas that reacts with the sodium contained in the glass in the immediate
vicinity of the inner surface of the container treated. The sodium so extracted from
the glass is then deposited at the surface of the inner wall of the container in the
form of a residual powder compound of sodium sulphate Na2SO4, which can then
5 be removed by washing. It is also known, according to a similar reaction principle,
a dealkalization treatment method that consists in introducing into a glass container,
while the latter is upstream from or within the annealing arch, sulphur dioxide SO2
or sulphur trioxide SO3 in gaseous form.
Such known methods nevertheless have a number of drawbacks. Indeed, if the use
10 of a powder reactive substance allows glass containers to be treated at a relatively
high rate, thanks to a continuous dispensing of a powder reactive substance into
containers in motion on a conveyor, there exists a significant risk of deposition and
reaction of the reactive substance on the outer wall of the container, and in particular
on the ring of the latter, which leads to aesthetic defects, or even to a local
15 weakening of the container. Moreover, it is difficult to accurately control the dose
of reactive substance really introduced into the container, unless oversizing the
quantity of reactive substance dispensed, which is not without economical and
environmental consequences. The use of a solid reactive substance in tablet form
generally allows a more accurate dispensing of the reactive substance into the
20 containers. However, it is often difficult, or even impossible, to efficiently treat that
way containers of small volume and/or small ring diameter, and especially at high
rates. On the other hand, the implementation of sulphur dioxide SO2 or sulphur
trioxide SO3 in gaseous form poses significant health, environmental and technical
problems, given the toxic and corrosive nature of these gases. Moreover, the
25 dealkalization treatment of the glass wall is not always carried out in a sufficiently
uniform and repeatable manner, and the level of chemical (or hydrolytic) resistance
of the treated container remains perfectible.
DISCLOSURE OF THE INVENTION
4
The objects assigned to the present invention therefore aim to remedy the different
drawbacks listed hereinabove, and to propose a new dealkalization method, as well
as a corresponding installation, which allow treating in a particularly efficient
manner glass containers of any size and capacity, and that at very high rates.
5 Another object of the invention aims to propose a new dealkalization method, as
well as a corresponding installation, which allow treating glass containers in a
particularly reliable and repeatable manner.
Another object of the invention aims to propose a new dealkalization method, as
well as a corresponding installation, which allow treating efficiently glass
10 containers without degrading the mechanical strength thereof.
Another object of the invention aims to propose a new dealkalization method, as
well as a corresponding installation, which allow obtaining glass containers having
an excellent hydrolytic resistance.
Another object of the invention aims to propose a new dealkalization method, as
15 well as a corresponding installation, whose implementation is particularly simple
and economical.
The objects assigned to the invention are achieved by means of a method for
dealkalizing the inner face of the wall of a glass container, such as a vial, which
wall delimits an accommodation cavity for a product and an opening providing
20 access to said accommodation cavity, said method comprising:
− a step of supplying a glass container, the inner face of the wall of which is
at a temperature of at least 350°C, and
− a step of introducing into said accommodation cavity, with said inner face
being at a temperature of at least 350°C, a treatment liquid containing a
25 treatment substance designed to react under the effect of the heat from the
inner face of the container wall to bring about dealkalization of the glass,
5
said introduction step comprising at least one operation of injecting, using an
injection head located at a distance from the opening of the container and outside
the latter, a predetermined dose of said treatment liquid as a spray cone that is
narrow enough relative to the opening of the container for substantially all of said
5 predetermined dose to end up inside the cavity of the container.
The objects assigned to the invention are also achieved by means of an installation
for dealkalizing the inner face of the wall of a glass container, such as a vial, which
wall delimits an accommodation cavity for a product and an opening providing
access to said accommodation cavity, said installation comprising
10 − a means for supplying a glass container whose inner face is at a temperature
of at least 350°C, and
− a means for introducing into said accommodation cavity, with said inner
face being at a temperature of at least 350°C, a treatment liquid containing
a treatment substance designed to react under the effect of the heat from the
15 inner face of the container wall to bring about dealkalization of the glass,
said means for introducing the treatment liquid comprising at least one injection
head, designed to be located at a distance from the opening of the container and
outside the latter, and to inject a predetermined dose of said treatment liquid as a
spray cone that is narrow enough relative to the opening of the container for
20 substantially all of said predetermined dose to end up inside the cavity of the
container.
BRIEF DESCRIPTION OF THE DRAWINGS
Other features and advantages of the invention will appear in more detail upon
reading of the following description, with reference to the appended drawings,
25 given by way of purely illustrative and non-limitative examples, in which:
6
− Figure 1 schematically illustrates an example of glass container of the vial
type subjected to a step of introducing a treatment liquid into its cavity, in
accordance with the dealkalization method according to the invention;
− Figure 2 schematically illustrates, in a side view, an embodiment of a
5 dealkalization installation according to the invention;
− Figure 3 schematically illustrates, in a top view, the dealkalization
installation of Figure 2.
WAYS TO IMPLEMENT THE INVENTION
The invention relates to a method for treating a glass container 1, such as a vial,
10 comprising a wall 2 delimiting an accommodation cavity 3 for a product (or a
substance) and an opening 4 providing access to said accommodation cavity 3. The
glass wall 2 of the container 1 has a lower face 5, located facing said
accommodation cavity 3 and preferentially intended to come into direct contact
with said product, and an opposite outer face 6. Preferentially made of moulded or
15 drawn glass, and formed of a single, monolithic piece of glass, the container 1 the
invention relates to may have any shape adapted to its function, such as for example
the shape of a vial or a bottle. As illustrated by way of example in Figure 1, the wall
2 of the container 1 is advantageously formed by a glass bottom 7, a glass lateral
wall 8 that rises from the periphery of the bottom 7, and a neck 9 provided with a
20 ring 10 that delimits the opening 4 of the container 1, to allow the accommodation
cavity 3 to be put in communication with the outside. Advantageously, said opening
4 is designed so as to be able to be closed by a removable or pierceable plug or
membrane seal.
Preferably, the product intended to be received into the cavity 3 of the container 1
25 is advantageously fluid, i.e. likely to flow like, for example, a liquid, pasty (such as
a liquid with a high degree of viscosity) or powder substance. Preferably, it is a
pharmaceutical product or a substance, such as for example a medication,
potentially intended to be administered by parenteral route (general or locoregional)
7
or to be ingested or absorbed by a patient, or also a diagnostic substance, as for
example a chemical or biological reagent. By extension, the container 1 can be
designed to contain a biological substance (or body fluid), such as for example
blood, a blood product or by-product, urine, etc. Even if the application to the
5 pharmaceutical and diagnostic fields is preferred, the invention is however not
limited to pharmaceutical and diagnostic containers and may in particular also relate
to a container designed to contain a liquid, pasty or powder substance for industrial
(storage of chemical products, etc.), veterinary, food or also cosmetic use.
In the sense of the invention, the word “glass” refers to a mineral glass. It is typically
10 a glass containing at least one alkaline or alkaline-earth species, such as sodium in
particular. If the method according to the invention is particularly well suited to the
treatment of a container made of soda-lime-silica glass (“Type III” glass), it is
however also of interest for the treatment of containers made of borosilicate glass
(“Type I” glass), insofar as such a glass does contain at least one alkaline species,
15 although in lower quantity than in the case of a soda-lime-silica glass.
Preferentially, the glass constituting the wall 2 of the container 1 is transparent (or
at least translucent) in the visible domain. It may be either a colourless glass or a
coloured glass, for example to protect the fluid substance in the container against
the effects of light, in particular in certain wavelength ranges (UV, etc.).
20 More specifically, the method according to the invention is a method for
dealkalizing the inner face 5 of the wall 2 of such a glass container 1. Such a
dealkalization method aims to extract, typically over a depth of several dozens of
nanometres, the alkaline ions (and in particular the sodium ions) present in the glass
in the vicinity of the surface of the inner face 5 of the wall 2 of the container 1. At
25 the end of the method according to the invention, the glass in the vicinity of the
surface of the inner face 5 of the wall 2 of the treated container 1 is thus, preferably
significantly, depleted in alkaline and/or alkaline-earth ions.
8
Firstly, the method according to the invention comprises a step of supplying a glass
container 1 as described hereinabove, (at least) the inner face 5 of the wall 2 of
which is at a temperature of at least 350°C, preferably between 350°C and 850°C,
preferably between 350°C and 800°C, preferably between 350°C and 700°C,
5 preferably between 500°C and 700°C, and still preferably between 500°C and
650°C. As an alternative, this supply step comprises an operation of heating, using
any known suitable heating means, a pre-existing glass container as described
hereinabove and whose wall inner face is initially at a temperature close (if not
equal) to the ambient temperature, in order to heat it in such a way that the
10 temperature of at least the inner face of its wall reaches a value of at least 350°C,
preferably between 350°C and 850°C, preferably between 350°C and 800°C,
preferably between 350°C and 700°C, preferably between 500°C and 700°C, and
still preferably between 500°C and 650°C. According to another, more preferential
alternative, the step of supplying the container 1 comprises an operation of
15 collecting a glass container 1 as described hereinabove at the exit of a machine for
hot forming a glass container from a glass preform, while said container 1 is still
hot enough so that (at least) the inner face 5 of the wall 2 of said container 1 is at a
temperature of at least 350°C, preferably between 350°C and 850°C, preferably
between 350°C and 800°C, preferably between 350°C and 700°C, preferably
20 between 500°C and 700°C, and still preferably between 500°C and 650°C.
According to this preferential alternative, the method according to the invention
thus does not require the implementation of a particular heating operation, the inner
face 5 of the wall 2 of the container 1 being heated to a temperature of at least
350°C, preferably between 350°C and 850°C, preferably between 350°C and
25 800°C, preferably between 350°C and 700°C, preferably between 500°C and
700°C, and still preferably between 500°C and 650°C, as a direct consequence of a
previous forming operation of said container 1. Such a forming operation can be
carried out using any known glass container forming installation, such as for
example an IS machine in the case of a container made of moulded glass. The
30 implementation of the method according to the invention is thus simplified, in
9
particular when the latter is implemented in an industrial context of manufacture of
glass containers.
The method according to the invention also comprises a step of introducing into the
accommodation cavity 3 of the container 1 to be treated, with the inner face 5 of the
5 wall 2 of the latter being at a temperature of 350°C, preferably between 350°C and
850°C, preferably between 350°C and 800°C, preferably between 350°C and
700°C, preferably between 500°C and 700°C, and still preferably between 500°C
and 650°C, a treatment liquid containing a treatment substance (or dealkalization
substance) designed to react under the effect of the heat from the inner face 5 of the
10 wall 2 of the container 1 to bring about dealkalization of the glass, typically in the
vicinity of the surface of the inner face 5 of the wall 2. It may be a substance that,
as such, is capable of coming into direct contact with the hot inner face 5 of the wall
2 of the container 1 to react, under the effect of heat, with one or several alkaline
species present in the glass forming the wall 2 of the container 1 or also a substance
15 capable of decomposing under the effect of the heat inside the cavity 3 of the
container, due to the above-mentioned temperature to which the inner face 5 of the
wall 2 is heated, to produce one or several new chemical species or substances,
which are capable of coming into contact with the surface of the inner face 5 of the
wall 2 of the container 1 and reacting with one or several alkaline or alkaline-earth
20 species present in the glass forming said wall 2 in order to obtain the desired effect
of dealkalization.
It has been observed that the fact to introduce the treatment substance, what’s more
in liquid phase, into a container 1 already heated to the treatment temperature (i.e.
a temperature included in the above-mentioned temperature ranges) makes it
25 possible to obtain far better performances, in particular in terms of homogeneity of
the dealkalization treatment of the inner face 5 of the wall 2 of the container 1 and
of hydrolytic resistance of the so-treated container 1, than when the same treatment
substance is introduced into a cold container 1 before the latter is heated to the
treatment temperature to make said treatment substance react under heat.
10
Preferably, said treatment substance comprises a sulphur compound, and still
preferably a compound containing sulphur combined with oxygen, in solution or in
suspension in a volatile liquid, i.e. in a liquid likely to evaporate under the effect of
heat, and at least at temperatures of at least 350°C, preferably between 350°C and
5 850°C, preferably between 350°C and 800°C, preferably between 350°C and
700°C, preferably between 500°C and 700°C, and still preferably between 500°C
and 650°C. Advantageously, this volatile liquid can be a solvent of said compound.
Still more preferentially, said sulphur compound is an ammonium sulphate, and
said volatile liquid is preferably water. It is then preferentially in this case
10 demineralised water or, still more preferentially, ultra-pure water. The ammonium
sulphate is then advantageously at least partially (and preferably totally) dissolved
in water, in a predefined concentration. Apart from the fact that the production, the
storage and the implementation of such a treatment liquid are relatively easy, safe
and inexpensive, it has been observed that excellent results in terms of hydrolytic
15 resistance of the glass can further be obtained using such a treatment liquid formed
of ammonium sulphate dissolved in water. In particular, very good results have
been obtained for glass containers 1 the inner face 5 of the wall 2 of which is at a
temperature preferentially between 500°C and 700°C, and more preferentially
between 500°C and 650°C, during the step of introducing the treatment liquid.
20 These results could be explained by a phenomenon of absorption of the water
molecules evaporated under the effect of heat, which facilitates or improves the
dealkalization treatment of the glass by the ammonium sulphate. However, the
invention is of course not limited to this example of treatment substance and volatile
liquid, and other substances and volatile liquids can actually be used to obtain the
25 desired effect of dealkalization by reaction with the glass under the effect of heat.
For example, the treatment substance may comprise a sulphur compound formed of
gaseous sulphur dioxide or trioxide, which would then be dissolved in the liquid
solvent (volatile liquid), or also a mixture of a sulphur compound and a fluorine
compound. In these cases also, the volatile liquid may advantageously be water
30 (preferably, demineralised water and, still more preferentially, ultra-pure water),
11
both for practicality and safety of implementation and for questions of treatment
efficiency, as mentioned above.
According to the invention, the step of introducing the treatment liquid into the
accommodation cavity 3 of the container 1 to be treated comprises at least one
5 operation of injecting, into said cavity 3, a predetermined dose of said treatment
liquid, using an injection head (or nozzle) 11, which is located at a distance from
the opening 4 of the container 1 to be treated and outside said container 1. Thus, the
injection head 11 does not enter the cavity 3 of the container 1 during, or for the
purpose of, said injection operation. In a preferential embodiment, and as
10 schematically illustrated in Figure 1, said injection head 11 is thus located facing
the opening 4 of the container 1, and above said opening 4, the container 1 being
positioned vertically, with its bottom 7 directed towards the ground. Said
predetermined dose of treatment liquid advantageously corresponds to an also
predetermined and known dose of treatment substance, insofar as, on the one hand,
15 the volume of the predetermined dose of treatment liquid sprayed by the injection
head 11, and on the other hand, the (mass or molar) concentration of treatment
substance in the treatment liquid, are known. Thus, according to the quantity of
treatment substance required to obtain the desired level of dealkalization
(advantageously characterized by a measurement of the hydrolytic resistance HR
20 of the container glass according to the usual measurement protocols) for a container
1 of given size, it is advantageously possible either to modulate the volume of the
predetermined dose for a fixed and known concentration of treatment substance, or
on the contrary to modulate the concentration of treatment substance for a known
and fixed volume of the predetermined dose, or also, as will be seen hereinafter, to
25 repeat the injection operation.
According to the invention, said injection operation is carried out in such a way as
to inject said predetermined dose of treatment liquid as a spray cone C that is narrow
enough relative to the opening 4 of the container 1 for substantially all of said
predetermined dose to end up inside the cavity 3 of the container 1 at the end of
12
said injection operation. When the injection head 11 is located facing and at a
distance from the opening 4 of the container 1, the spray cone C hence
advantageously has a cross-section, included in a plane in which the opening 4 of
the container 1 is inscribed, whose size is lower than that of said opening 4 of the
5 container 1 in said plane. As schematically illustrated in Figure 1, the spray cone C
generated by the injection head 11 can then advantageously have a (dummy) base
of size lower, and preferably far lower, than that of the opening 4 of the container
1, in such a way that all of the predetermined dose of treatment liquid (to within the
potential unavoidable but nevertheless negligible losses) can be injected into the
10 cavity 3 of the container 1, and hence with substantially no dispersion of treatment
liquid next to the container 1 or on the outer face 6 of the wall 2 and the ring 10 of
the latter. It will be noted that, in the context of the invention, “spray cone” is not
to be considered according to a strict mathematical definition of the term “cone",
but preferentially mean a dummy envelope (whether conical, frustoconical, or even
15 ideally substantially cylindrical) inside which is contained substantially all the
predetermined dose of treatment liquid sprayed by the injection head 11 towards
the cavity 3 of the container 1, as illustrated in dotted line in Figure 1.
The particular combination of the feature of temperature of the inner face 5 of the
wall 2 of the container 1 to be treated, on the one hand, and the features of the
20 above-described step of introducing the treatment liquid into the cavity 3 of the
container 1 thus advantageously makes it possible to dealkalize glass containers 1
in a particularly efficient manner, whatever their size and capacity, and that at very
high rates when the method according to the invention is applied successively to a
plurality of glass containers 1. Indeed, it is not necessary to proceed to cycles of
25 insertion and removal of the injection head 11 into, and from, the cavity 3 of
containers 1 to be treated, in order to treat a plurality of containers successively
brought facing the injection head 11. Moreover, the method according to the
invention is particularly economical, clean and environmentally friendly because it
allows avoiding any overdose of treatment substance and the useless dispersion of
30 a quantity of this treatment substance outside the container to be treated.
13
It is desirable that the injection head 11 is not located too close to the container 1 to
be treated during the operation of injecting said predetermined dose of treatment
liquid, in order in particular to avoid the injection head 11 to be damaged by the
heat from the container 1. On the other hand, it is preferable that the injection head
5 11 is not either located at a too great distance d from the opening 4 of the container
1, in order in particular not to degrade the accuracy of the injection operation and
to facilitate the practical implementation thereof. Finally, it is advisable to choose
the distance d between the injection head 11 and the opening 4 of the container 1 in
such a way as to limit the risk of evaporation of the treatment liquid, under the effect
10 of the heat from the container 1, even before the dose has been able to fully enter
the cavity 3 of the container 1. As such, during the operation of injecting said
predetermined dose of treatment liquid, the injection head 11 may be
advantageously located substantially facing the opening 4 of the container 1 (as
contemplated hereinabove) and at a distance d preferentially between 1 cm and 20
15 cm, and still more preferentially between 1 cm and 5 cm, from said opening 4 during
the injection step. This distance d is here preferentially understood as the average
distance measured in straight line between, on the one hand, the outlet 12 of the
injection head 11 (through which the predetermined dose of treatment liquid exits
from the injection head 11) and a plane containing the opening 4 of the container 1,
20 as illustrated in Figure 1.
In order to facilitate the injection, in accordance with the above, of all the
predetermined dose of treatment liquid into the cavity 3 of the container 1 to be
treated, the spray cone C of said predetermined dose of treatment liquid is formed,
by the injection head 4, in such a way as to preferentially have an apex angle (or
25 opening angle) θ substantially between 0° and 5°. Still more preferentially, the apex
angle θ of the spray cone is substantially between 0° and 1°, in such a way that the
predetermined dose of treatment liquid is advantageously injected into the cavity 3
of the container 1 as a cylindrical or almost-cylindrical dummy envelope. Thus, if,
at the exit of the injection head 11, the predetermined dose of the treatment liquid
30 is for example in the form of a plurality of treatment liquid droplets, more or less
14
distinct from each other, these latter can then form, between the injection head 11
and the cavity 3 of the container 1, a substantially rectilinear trickle or jet of
treatment liquid.
Preferentially, the treatment liquid has a predefined concentration of said treatment
5 substance in solution that it close (if not equal) or just below the saturation
concentration. In other words, the treatment liquid contains said treatment
substance, which is substantially totally dissolved in a liquid, and preferably a
volatile liquid as mentioned hereinabove, in a quantity close or just below the
maximum quantity able to be dissolved in the considered liquid for a chosen
10 temperature of implementation of the treatment liquid. The predetermined
concentration thus advantageously corresponds to the highest possible
concentration of treatment substance, without exceeding the saturation
concentration. Typically, the predefined concentration is hence substantially
between about 70 % and 100 % of the saturation concentration, preferably between
15 about 80 % and 100 % of the saturation concentration, still preferably between
about 90 % and 100 % of the saturation concentration for a chosen temperature of
implementation of the treatment liquid. That way, it is possible to introduce into the
container 1 a predetermined dose of treatment liquid that contains an optimum
quantity of treatment substance in the smallest possible volume of predetermined
20 dose. That way, the quality of the dealkalization treatment is optimized while
limiting the risk of damage to the container 1 by thermal shock when the treatment
liquid enters into contact with the hot inner face 5 of the wall 2 of the container 1.
Maintaining a concentration of treatment substance lower than or equal to the
saturation concentration advantageously makes it possible to guarantee an excellent
25 reproducibility of the quantity of treatment substance introduced into the container
1, and also to limit the risk of clogging of the injection head 11 when the treatment
substance is a solid substance, dissolved in a volatile liquid to form the treatment
liquid (risk of precipitation). For example, when the treatment liquid comprises a
ammonium sulphate (treatment substance) dissolved in water (volatile liquid), as
30 already contemplated hereinabove, the predefined concentration of ammonium
15
sulphate in the treatment liquid may generally be between about 0.1 g/mL and about
1 g/mL, according in particular to the temperature of implementation of the
treatment liquid and the desired level of hydrolytic resistance. However, in view of
the above, it is therefore more advantageous that the predefined concentration of
5 dissolved ammonium sulphate in the treatment liquid is between about 0.5 g/mL
and about 0.8 g/mL for a temperature of the treatment liquid between about 0°C
and about 40°C, and preferably between about 10°C and about 40°C. The
predefined concentration of dissolved ammonium sulphate in the treatment liquid
could go up to about 1 g/mL for a temperature of the treatment liquid of about 90°C.
10 Preferentially, the volume of the predetermined dose of treatment liquid injected by
the injection head 11 is chosen substantially between 5 µL and 50 µL, and
preferably between 5 µL and 30 µL, which advantageously makes it possible to
limit the risk of damage to the container 1 by thermal shock when the treatment
liquid enters into contact with the hot inner face 5 of the wall 2 of the container 1.
15 Moreover, the choice of such a limited volume of treatment liquid helps to facilitate
the injection of all the predetermined dose of treatment substance into the cavity 3
of the containers 1 to be treated, and that even at very high rates.
Although the method according to the invention can be of interest for treating a
container 1 that remains stationary relative to the injection head 11 during the
20 injection operation, the injection operation of the method according to the invention
is advantageously carried out while the container 1 to be treated is in motion relative
to the injection head 11, preferably at a speed of at least 25 m per minute, still
preferably at least 30 m per minute, and still preferably up to 40 m per minute, so
that in particular a plurality of containers 1 can be treated using the injection head
25 11 at a particularly high rate. According to an alternative, the injection head 11
moves, during the injection operation, relative to the container 1 to be treated, which
is itself held stationary (in the earth reference system). According to another, more
preferential alternative, the injection head 11 is on the contrary held stationary (in
the earth reference system), while the container 1 to be treated moves relative to the
16
injection head 11, for example on a conveyor positioned under and facing the
injection head 11.
In the particular case in which the injection operation of the method according to
the invention is hence advantageously carried out while the container 1 to be treated
5 is in motion relative to the injection head 11, the method according to the invention
preferentially comprises a step of detecting the presence of the container 1 upstream
from the injection head 11 (considering the direction of relative movement of the
injection head 11 and the container 1), previously to the injection operation, to
synchronize the triggering of the injection operation with the arrival of the container
10 1 at the injection head 11, and preferably facing the outlet 12 of the latter. Indeed,
knowing the speed of movement of the container 1 relative to the injection head 11,
and on the basis of a detection signal, generated during the detection step, of the
presence of the container 1 at a known distance downstream from the injection head
11, it is hence advantageously possible to trigger the injection of the predetermined
15 dose by the injection head 11 at the precise moment when the container 1 is
positioned facing the outlet 12 of the injection head 11, and preferably just in
alignment therewith.
Advantageously, the step of introducing the treatment liquid into the
accommodation cavity 3 of the container 1 may comprise a plurality of successive
20 operations of injection of said predetermined dose of said treatment liquid. Indeed,
it may be necessary, according to the size of the glass container 1 to be treated, to
implement a significant quantity of treatment substance to achieve the desired
dealkalization level, without having to use for that purpose predetermined doses of
treatment liquid of significant volumes, which could lead to a high risk of thermal
25 shocks detrimental to the mechanical strength of the container 1. If it is conceivable,
as discussed hereinabove, to increase the quantity of treatment substance by playing
on the concentration of the latter in the treatment liquid, it may thus also be
advantageously contemplated (as a complement or as an alternative) to subject
several times a same glass container 1 to the injection operation of the method
17
according to the invention by implementing, at each iteration, a predetermined dose
of treatment liquid of limited volume (for example, between 5 µL and 50 µL, and
preferably between 5 µL and 30 µL, as mentioned hereinabove). In such a case,
said injection operation can then be carried out, for example, using a single and
5 same injection head 11, the container 1 then remaining preferentially stationary (at
least temporarily) facing the injection head 11. As an alternative, said injection
operation could be carried out using a plurality of distinct injection heads 11,
positioned for example one after the other along a path of movement of the
container 1.
10 In order to further improve the repeatability and the reliability of the dealkalization
treatment, by taking into account potential variations of weather conditions, the
method according to the invention preferably comprises, previously to the step of
introducing a treatment liquid into the cavity 3 of the container 1, an operation of
regulating and controlling the temperature of the treatment liquid in order to make
15 sure that this temperature remains substantially constant over time, and
advantageously equal to a predefined setpoint temperature. Therefore, the
predetermined dose of treatment liquid is injected into the cavity 3 of the container
1 at an advantageously predefined temperature, which is then substantially identical
for each container 1 to be treated according to the method of the invention.
20 As an alternative or as a complement, the method according to the invention may
comprise, previously to the step of introducing the treatment liquid into the cavity
3 of the container 1, an operation of preheating the treatment liquid (typically to a
temperature higher than the ambient temperature), in such a way as to reduce the
difference between the temperature of the predetermined dose of treatment liquid
25 injected during the injection operation and the temperature of the inner face 5 of the
wall 2 of the container 1 to be treated. This makes it possible in particular to further
reduce the risk of thermal shock during the treatment of the container 1, and hence
the risk of damage to the latter.
18
The method according to the invention may advantageously comprise, after the step
of introducing the treatment liquid into its cavity 3, a step of transferring the sotreated container 1 to a glass container annealing device, such as a conventional
industrial annealing arch.
5 The invention also relates, as such, to an installation 13 for treating a glass container
1, advantageously intended to implement the method according to the invention.
More specifically, the installation 13 according to the invention is an installation
for dealkalizing the inner face 5 of the wall 2 of such a glass container 1, which
wall 2 delimits an accommodation cavity 3 for a product and an opening 4 providing
10 access to said accommodation cavity 3. The installation 13 in question is
advantageously an installation for implementing a dealkalization method in
accordance with the invention, so that the above description related to the method
according to the invention remains valid and applicable, mutatis mutandis, to the
present installation 13, and vice versa. It is preferentially an industrial installation,
15 advantageously automated. Still more preferentially, said installation 13 is designed
to treat in a substantially uninterrupted manner a large number of containers 1. An
embodiment of the installation 13 according to the invention is schematically
illustrated by way of example in Figures 2 and 3.
The installation 13 according to the invention comprises a means 14 for supplying
20 a glass container 1, as described hereinabove, (at least) the inner face 5 of the wall
2 of which is at a temperature of at least 350°C, preferably between 350°C and
850°C, preferably between 350°C and 800°C, preferably between 350°C and
700°C, preferably between 500°C and 700°C, and still preferably between 500°C
and 650°C. According to an alternative, this supply means comprises a heating
25 means, of any known suitable type (for example, of the arch or oven type), designed
to heat a pre-existing glass container as described hereinabove and the inner face of
the wall of which is initially at a temperature close (if not equal) to the ambient
temperature, in such a way that the temperature of at least the inner face of the
container wall reaches a value of at least 350°C, preferably between 350°C and
19
850°C, preferably between 350°C and 800°C, preferably between 350°C and
700°C, preferably between 500°C and 700°C, and still preferably between 500°C
and 650°C. According to another, more preferential alternative, the means 14 for
supplying the container 1 comprises a system 15 for collecting a glass container 1
5 as described hereinabove at the exit of a machine 16 for hot forming a glass
container from a glass preform, while said container 1 is still hot enough so that (at
least) the inner face 5 of the wall 2 of said container 1 is at a temperature of at least
350°C, preferably between 350°C and 850°C, preferably between 350°C and
800°C, preferably between 350°C and 700°C, preferably between 500°C and
10 700°C, and still preferably between 500°C and 650°C. According to this
preferential alternative, the installation 13 according to the invention thus
advantageously does not comprise a specific heating means for heating the
container 1,the inner face 5 of the wall 2 of the container 1 being heated to a
temperature of at least 350°C, preferably between 350°C and 850°C, preferably
15 between 350°C and 800°C, preferably between 350°C and 700°C, preferably
between 500°C and 700°C, and still preferably between 500°C and 650°C, as a
direct consequence of a previous forming operation of said container 1 by said
forming machine 16. As mentioned hereinabove in relation with the method
according to the invention, this machine or installation 16 for forming glass
20 containers may be of any known forming type, such as for example an IS machine
in the case of a container made of moulded glass. The collecting system 15 may,
for example, comprise an arm, advantageously robotic, and/or a conveyor 17 (for
example, of the belt or roll type), designed, arranged and sized to collect a glass
container 1 at the exit of a forming machine 16, close enough to the latter so that
25 (at least) the inner face 5 of the wall 2 of the container 1 is still at a temperature of
at least 350°C, preferably between 350°C and 850°C, preferably between 350°C
and 800°C, preferably between 350°C and 700°C, preferably between 500°C and
700°C, and still preferably between 500°C and 650°C.
The installation 13 according to the invention also comprises a means (or station)
30 18 for introducing into the accommodation cavity 3 of the container 1 to be treated,
20
with the inner face 5 of the wall 2 of the latter being at a temperature of 350°C,
preferably between 350°C and 850°C, preferably between 350°C and 800°C,
preferably between 350°C and 700°C, preferably between 500°C and 700°C, and
still preferably between 500°C and 650°C, a treatment liquid containing a treatment
5 substance (or dealkalization substance) designed to react under the effect of the heat
from the inner face 5 of the wall 2 of the container 1 to bring about dealkalization
of the glass, typically in the vicinity of the surface of the inner face 5 of the wall 2.
The treatment liquid and substance implemented by the installation, as well as the
reaction principles associated therewith, are advantageously consistent with the
10 treatment liquid and substance described hereinabove in relation with the method
according to the invention. The means 18 for introducing the treatment liquid
comprises at least one injection head (or nozzle or valve) 11, designed to be located
(and held) at a distance from the opening 4 of the container 1 and outside the latter,
and to inject (while the injection head 11 is located that way) a predetermined dose
15 of the treatment liquid as a spray cone C that is narrow enough relative to the
opening 4 of the container 1 for substantially all of said predetermined dose to end
up inside the cavity 3 of the container 1. In other words, the introduction means 18
is designed to hold the injection head 11 in such a way that the latter does not enter
the cavity 3 of the container 1 when the injection head 11 is in operation and injects
20 said predetermined dose of treatment liquid into the cavity 3 of the container 1. The
injection head 11 is designed to generate, at an outlet (opening) 12, said
predetermined dose of treatment liquid, and to inject it, to spray it as a spray cone
C having a (dummy) base of size lower, and preferably far lower, than that of the
opening 4 of the container 1, as shown in Figure 1 and described hereinabove in
25 relation with the method according to the invention.
The particular combination of the features of the means 14 for supplying the
container 1, on the one hand, and the features of the means 18 for introducing the
treatment liquid into the cavity 3 of the container 1 thus makes the installation 13
according to the invention advantageously capable of carrying out a particularly
30 efficient dealkalization treatment of glass containers 1, whatever their size and
21
capacity, and that at very high rates when the installation according to the invention
is implemented to treat successively a plurality of glass containers 1. Moreover, the
installation 13 according to the invention is particularly economical, clean and
environmentally friendly because it allows avoiding any overdose of treatment
5 substance and the useless dispersion of a quantity of this treatment substance
outside the container to be treated.
In a preferential embodiment, and as schematically illustrated in Figure 2, the
means 14 for supplying the glass container 1 to be treated is designed to bring the
container 1 to the introduction means 18 in such a way that the container 1 is
10 positioned vertically, with its bottom 7 directed towards the ground, and the
introduction means 18 is designed in such a way that the injection head 11 can be
located facing the opening 4 of the container 1 and above said opening 4.
Advantageously, the introduction means 18 may comprise an adjustable support for
adapting, preferably automatically, the position (or altitude) of the injection head
15 11 as a function of the size of the container(s) 1 to be treated.
Preferably, and for the reasons and advantages explained hereinabove in relation
with the method according to the invention, the introduction means 18 is designed
to position, and also preferably to hold, the injection head 11 substantially facing
the opening 4 of the container 1 and at a distance d between 1 cm and 20 cm, and
20 preferably between 1 cm and 5 cm, from said opening 4, when the injection head
11 is in operation, that is to say when it forms the predetermined dose and sprays it
towards the cavity 3 of the container 1. This distance d is here too preferentially
understood as the average distance measured in straight line between, on the one
hand, the outlet 12 of the injection head 11 and a plane containing the opening 4 of
25 the container 1, as illustrated in Figure 1.
Preferentially, the injection head 11 is designed to generate a spray cone C of said
predetermined dose of treatment liquid having an apex angle θ substantially
between 0° and 5°. Still more preferentially, the injection head 11 is designed to
22
generate a spray cone C of said predetermined dose of treatment liquid with an
angle θ substantially between 0° and 1°, in such a way that the predetermined dose
can be advantageously injected into the cavity 3 of the container 1 as a substantially
cylindrical or almost-cylindrical dummy envelope.
5 In order to limit the risk of damage to the container 1 by thermal shock when the
treatment liquid enters into contact with the hot inner face 5 of the wall 2 of the
container 1, but also to advantageously facilitate the injection of all the
predetermined dose of treatment liquid into the cavity 3 of the containers 1 to be
treated, and that even at very high rates, the injection head 11 is preferentially
10 designed in such a way that the volume of said predetermined dose of said treatment
liquid is between 5 µL and 50 µL, and preferably between 5 µL and 30 µL.
According to a preferential embodiment, the injection head 11 comprises an
electromechanical actuator driven by a piezoelectric device, to allow the dosing and
the injection of volumes of liquid between 5 µL and 50 µL, and preferably between
15 5 µL and 30 µL, in response to an electric control signal. As an alternative, and in
particular for higher volumes of treatment liquid to be dosed and injected, the
injection head 11 may comprise, for example, an electromechanical actuator driven
by a solenoid device.
Although the installation 13 according to the invention can be of interest for treating
20 a container 1 that remains stationary relative to the injection head 11 during the
operation of the latter, the installation 13 is preferentially designed to allow a
dealkalization treatment of one or several glass containers 1 in motion relative to
the injection head 11, preferably at a speed of at least 25 m per minute, still
preferably at least 30 m per minute, and still preferably up to 40 m per minute, so
25 that in particular a plurality of containers 1 can be treated using the injection head
11 at a particularly high rate. According to an alternative, the installation 13
comprises, on the one hand, means for moving the injection head 11 during its
operation, preferably at the above-mentioned speed, relative to the container 1,
23
which itself remains stationary (in the earth reference system). According to a more
preferential alternative, and as schematically illustrated in Figures 2 and 3, the
installation 13 preferably comprises a conveyor 19 (for example of the belt or roll
type), or any other suitable known means, designed to, adapted to, put the
5 container(s) 1 to be treated in motion relative to the injection head 11, which is held
stationary (in the earth reference system, for example “through a frame fixed to the
ground”), preferably at a speed of at least 25 m per minute, still preferably at least
30 m per minute, and still preferably up to 40 m per minute. In this case, and as
illustrated by way of example in Figure 2, the conveyor 19 can then be preferentially
10 positioned under and facing the injection head 11, with the container 1 positioned
vertically, with its bottom 7 resting on the conveyor 19 and its opening 4 directed
upward, in such a way that said opening 4 comes under (and preferably in alignment
with) the outlet 12 of the injection head 11. Potentially, the conveyor 19 may be the
same as the conveyor 17 comprised, in the example proposed hereinabove, in the
15 system 15 for collecting the glass container 1 at the exit of a forming machine 16.
Preferentially, the installation 13 according to the invention comprises a means 20
for detecting the presence of the container 1 upstream from the injection head 11,
and a control unit 21 connected, mechanically or electrically, on the one hand to the
detection means 20, and on the other hand to the injection head 11, to synchronize
20 the triggering of the operation of the injection head 11 with the arrival of the
container 1 at the injection head 11, and preferably facing the outlet 12 of the latter,
as contemplated hereinabove in relation with the method according to the invention.
For example, the detection means 20 may be of the optical barrier type and comprise
either a light beam emitter (for example, of the infrared type) positioned opposite a
25 photoelectric cell, or a detection cell 22 comprising both a light beam emitter (for
example, of the infrared type) and a photoelectric cell and a light reflector 23
positioned opposite a photoelectric cell, as in the example illustrated in Figure 3.
The detection cell 22 and the reflector 23 are advantageously positioned on either
side of the path of movement of the container 1, at a known distance from the
30 injection head 11. In the absence of container 1, the detection cell 22 emits a light
24
beam (represented in dotted line in Figure 3), which is reflected by the reflector 23
and detected by the photoelectric cell of the detection cell 22. In this case, the
control unit 21 controls the stop of the operation of the injection head 11. In the
presence of a container 1, the light beam is interrupted (or at least disturbed) by the
5 container 1, in such a way that the photoelectric cell does not detect the light beam
(or detects a disturbed light beam), which signs the presence of a container 1. In
this case, the control unit 21 controls, with a time delay defined according to the
known speed of movement of the container 1, the triggering of the operation of the
injection head 11. In a particularly advantageous manner, such a detection means
10 20 of the optical barrier type may be designed and arranged in such a way that the
light beam emitted is interrupted by the neck 9 or the ring 10 of a container 1, and
not by the body of the latter, in order to allow a finer synchronization of the
operation of the injection head 11, and hence a more accurate injection of the
predetermined dose of treatment liquid into the cavity 3 of the container 1, when
15 the latter arrives at the injection head 11. Of course, other known and suitable
detection means, not necessarily optical, may be contemplated.
Advantageously, the means 18 for introducing the treatment liquid may comprise a
plurality of injection heads 11, or a single injection head 11 provided with a
plurality of outlets 12, in order to allow the injection of a predetermined dose of
20 treatment liquid simultaneously into the cavity 3 of a plurality of glass containers 1
(whether these latter are then in motion or not relative to the injection heads 11),
and/or to allow the successive injection of several predetermined doses into the
cavity 3 of a same container 1. The introduction means 18 can then comprise, for
example, a plurality of distinct injection heads 11, mounted one after the other along
25 the path of relative movement of the injection heads and the container(s) 1. As an
alternative and/or a complement, the introduction means 18 may comprise a
plurality of distinct injection heads 11 mounted next to each other in a direction
transverse to the path of relative movement of the injection heads and the
container(s) 1, in order to allow the treatment of glass containers 1 arranged in rows.
25
As a complement or alternative to such a means 20 for detecting the presence of the
container 1 upstream from the injection head 11, the installation 13 advantageously
comprises, when it is provided to treat successively or simultaneously a plurality of
glass containers 1, a means for controlling the relative position and aligning the
5 containers, upstream from the injection head(s) 11, in order to further improve the
accuracy of injection of the predetermined dose of treatment liquid into the cavity
3 of the containers 1 to be treated. Such means for controlling the relative position
and aligning the containers are known as such in the field of glass container
treatment, so that it is not necessary to describe them here in more detail.
10 Advantageously, the installation 13 comprises a system 24 for preparing and/or
storing the treatment liquid, upstream from the injection head 11 of the introduction
means 18. This preparation and/or storage system 24 can advantageously comprise
a system 25 for mixing the treatment substance and the volatile liquid, to obtain
and/or preserve a perfectly homogeneous treatment liquid. In order to further
15 improve the repeatability and the reliability of the dealkalization treatment, by
taking into account potential variations of weather conditions, the installation 13
according to the invention preferably comprises, and for example at the abovementioned system 24 for preparing and/or storing the treatment liquid, a heat
regulation system 26 for holding the treatment liquid at a constant predefined
20 temperature before the latter is injected into the cavity 3 of the container 1 by the
injection head 11. Advantageously, the introduction means 18 may comprise, and
for example at said system 24 for processing and/or storing the treatment liquid, a
system 27 for pressurizing the treatment liquid upstream from or within the
injection head 11, for example at a relative pressure comprised between 0.5 bar and
25 4 bar.
The installation 13 according to the invention may advantageously comprise,
downstream from the means 18 for introducing the treatment liquid into the cavity
3 of the container 1, and preferably above the opening 4 of the container 1, one or
several extraction hoods 28 to efficiently extract and evacuate the off-gases
26
resulting from the glass dealkalization reaction. The installation 13 according to the
invention may advantageously comprise, downstream from the means 18 for
introducing the treatment liquid into the cavity 3 of the container 1, a means 29 for
transferring the treated container 1 to the entry of a glass container annealing device
5 30, such as a conventional industrial annealing arch 30. The transfer means 29 may,
for example, comprise an arm, advantageously robotic, and/or a conveyor 31 (for
example, of the belt or roll type), designed, arranged and sized to collect the treated
glass container 1 at, or downstream from, the introduction means 18 and to bring it
to the entry of the annealing device 30.
10 As understood from the above detailed description, the method and installation
according to the invention can advantageously be directly integrated to industrial
glass container production methods and line, wherein the installation according to
the invention can be positioned in a production line, between a glass container
forming machine and a device for annealing these latter.
15 Advantageously, the method and installation according to the invention allow the
dealkalization of the inner face of the wall of a large number of glass containers, at
a rate that may be higher than 400 vials / minute in single row (a single injection
head) or 800 vials / minute in dual row (two parallel rows of containers on the
conveyor, two injection heads), in particular for containers of rated capacity of 5
20 mL to 50 mL, and that, while achieving a better hydrolytic resistance level of the
treated containers than that usually achieved using known methods and installations
of dealkalization by a solid or gaseous treatment substance.
POSSIBILITY OF INDUSTRIAL APPLICATION
The invention finds its application in the field of methods and installations for the
25 treatment of glass containers, and more specifically the technical field of methods
and installations for the dealkalization treatment of the inner wall of glass
27
containers, such as for example containers forming pharmaceutical glass primary
packaging.
28
WE CLAIM:
1. A method for dealkalizing the inner face (5) of the wall (2) of a glass
container (1), such as a vial, which wall (2) delimits an accommodation
cavity (3) for a product and an opening (4) providing access to said
5 accommodation cavity (3), said method comprising
- a step of supplying a glass container (1), the inner face (5) of the wall
(2) of which is at a temperature of at least 350°C, and
- a step of introducing into said accommodation cavity (3), with said
inner face (5) being at a temperature of at least 350°C, a treatment liquid
10 containing a treatment substance designed to react under the effect of
the heat from the inner face (5) of the wall (2) of the container (1) to
bring about dealkalization of the glass,
said introduction step comprising at least one operation of injecting, using
an injection head (11) located at a distance from the opening (4) of the
15 container (1) and outside the latter, a predetermined dose of said treatment
liquid as a spray cone (C) that is narrow enough relative to the opening (4)
of the container (1) for substantially all of said predetermined dose to end
up inside the cavity (3) of the container (1).
2. The method according to the preceding claim, wherein
20 - said supply step is a step of supplying a glass container (1), the inner
face (5) of the wall (2) of which is at a temperature between 350°C and
850°C, preferably between 350°C and 800°C, still preferably between
350°C and 700°C,
- said introduction step being a step of introducing said treatment liquid
25 into said accommodation cavity (3), with said inner face (5) being at a
temperature between 350°C and 850°C, preferably between 350°C and
800°C, still preferably between 350°C and 700°C.
29
3. The method according to any one of the preceding claims, wherein the step
of supplying the container (1) comprises an operation of collecting a glass
container (1) at the exit of a machine for hot forming a glass container from
a glass preform, while said container (1) is still hot enough so that the inner
5 face (5) of the wall (2) is at a temperature of at least 350°C, preferably
between 350°C and 850°C, preferably between 350°C and 800°C, still
preferably between 350°C and 700°C.
4. The method according to any one of the preceding claims, wherein said
substance comprises a sulphur compound, in solution or in suspension in a
10 volatile liquid.
5. The method according to the preceding claim, wherein said sulphur
compound is an ammonium sulphate, said volatile liquid being preferably
water.
6. The method according to any one of the preceding claims, wherein said
15 treatment liquid has a predefined concentration of said treatment substance
in solution that it close or just below the saturation concentration.
7. The method according to any one of the preceding claims, wherein the
injection head (11) is located substantially facing the opening (4) of the
container (1) and at a distance (d) between 1 cm and 20 cm, and preferably
20 between 1 cm and 5 cm, from said opening (4) during the injection step.
8. The method according to any one of the preceding claims, wherein said spray
cone (C) has an apex angle (θ) between 0° and 5°, preferably between 0° and
1°.
9. The method according to any one of the preceding claims, wherein the
25 volume of said predetermined dose of treatment liquid is chosen substantially
between 5 µL et 50 µL, and preferably between 5 µL et 30 µL.
30
10. The method according to any one of the preceding claims, wherein said
injection operation is carried out while the container (1) is in motion relative
to the injection head (11), preferably at a speed of at least 25 m per minute,
still preferably at least 30 m per minute, still preferably up to 40 m per
5 minute.
11. The method according to the preceding claim, which comprises a step of
detecting the presence of the container (1) upstream from the injection head
(11), previously to the injection operation, to synchronize the triggering of
said injection operation with the arrival of the container (1) at the injection
10 head (11).
12. The method according to any one of the preceding claims, wherein said step
of introducing the treatment liquid into the accommodation cavity (3) of the
container (1) comprises a plurality of successive operations of injection of
said predetermined dose of said treatment liquid.
15 13. An installation (13) for dealkalizing the inner face (5) of the wall (2) of a
glass container (1), such as a vial, which wall (2) delimits an accommodation
cavity (3) for a product and an opening (4) providing access to said
accommodation cavity (3), said installation (13) comprising
- a means (14) for supplying a glass container (1) whose said inner face
20 (5) is at a temperature of at least 350°C, and
- a means (18) for introducing into said accommodation cavity, with said
inner face (5) being at a temperature of at least 350°C(3), a treatment
liquid containing a treatment substance designed to react under the
effect of the heat from the inner face (5) of the container (1) to bring
25 about dealkalization of the glass,
said means (18) for introducing the treatment liquid comprising at least one
injection head (11), designed to be located at a distance from the opening
31
(4) of the container (1) and outside the latter, and to inject a predetermined
dose of said treatment liquid as a spray cone (C) that is narrow enough
relative to the opening (4) of the container (1) for substantially all of said
predetermined dose to end up inside the cavity (3) of the container (1).
5 14. An installation (13) according to the preceding claim, wherein
- said supply means (14) is a means (14) for supplying a glass container
(1), the inner face (5) of the wall (2) of which is at a temperature
between 350°C and 850°C, preferably between 350°C and 800°C, still
preferably between 350°C and 700°C,
10 - said introduction means (18) being a means (18) for introducing said
treatment liquid into said accommodation cavity (3), with said inner
face (5) being at a temperature between 350°C and 850°C, preferably
between 350°C and 800°C, still preferably between 350°C and 700°C.
15. The installation (13) according to the preceding claim, wherein the means
15 (14) for supplying the container comprises a system (15) for collecting a
glass container (1) at the exit of a machine for hot forming a glass container
from a glass preform, while said container (1) is still hot enough so that the
inner face (5) of its wall (2) is at a temperature of at least 350°C, preferably
between 350°C and 850°C, preferably between 350°C and 800°C, preferably
20 between 350°C and 700°C.
16. The installation (13) according to any one of claims 13 to 15, wherein the
introduction means (18) is designed to position the injection head (11)
substantially facing the opening (4) of the container (1) and at a distance (d)
between 1 cm and 20 cm, and preferably between 1 cm and 5 cm, from said
25 opening (4), when the injection head (11) is in operation.
32
17. The installation (13) according to any one of claims 13 to 16, wherein the
injection head (11) is designed in such a way that said spray cone (C) has an
apex angle (θ) between 0° and 5°, preferably between 0° and 1°.
18. The installation (13) according to any one of claims 13 to 17, wherein the
5 injection head (11) is designed in such a way that the volume of said
predetermined dose of treatment liquid is between 5 µL et 50 µL, and
preferably between 5 µL et 30 µL.
19. The installation (13) according to any one of claims 13 to 18, which
comprises a heat regulation system (26) for holding the treatment liquid at a
10 constant predefined temperature before the latter is injected into the cavity
(3) of the container by the injection head (11).
20. The installation (13) according to one of claims 13 to 19, which comprises a
conveyor (20) designed to put the container (1) in motion relative to the
injection head (11), preferably at a speed of at least 25 m per minute, still
15 preferably at least 30 m per minute, and still preferably up to 40 m per
minute.
21. The installation (13) according to the preceding claim, which comprises a
means (20) for detecting the presence of the container (1) upstream from the
injection head (11), and a control unit (21) connected to said detection means
20 (20) and to the injection head (11), to synchronize the triggering of the
operation of the injection head (11) with the arrival of the container (1) at the
injection head (11).

22. The installation (13) according to any one of claims 13 to 21, wherein the
means (18) for introducing the treatment liquid comprises a plurality of
injection heads (11).