FR3085295A1 - SYSTEM AND METHOD FOR PRODUCING ELASTOMERIC COMPOSITES VIA A MIXTURE OF LIQUIDS - Google Patents

Description

SYSTEM AND METHOD FOR PRODUCING

ELASTOMER COMPOSITES VIA A MIXTURE OF LIQUIDS

TECHNICAL AREA

The present invention relates to the use of methods for mixing liquids and the corresponding systems in the production of elastomeric composites for use in finished and semi-finished elastomeric products such as tires.

CONTEXT

It is known to obtain a masterbatch by mixing liquids continuously.

In such a case, in the production of elastomeric composites, the passage of a liquid mixture (for example a mixture of an elastomer emulsion and a filler suspension or filler) into a viscoelastic solid is carried out by coagulation (as used here, the terms "charge" and "agent of charge" are interchangeable). Obtaining a coagulum is conditioned by the nature of the emulsion and the bulking agent brought into contact, by the nature of the target bulking agent and by the coagulation used. For example, a concentrated suspension will decrease setting time and also limit the volume of water to be extracted and treated. Various methods exist for producing elastomeric composites, examples of which are set out in US document 6,048,923 and 6,075,084 as well as in Japanese document No. JP5139610.

Following the fixing of the filler in the elastomer matrix and this phase corresponds to a state of "coagulation" between the two liquids. For example, in mixtures using a silica suspension in an elastomeric emulsion, the tendency of the silica particles to re-agglomerate after mixing is due to the lack of affinity with Γ elastomer. A concentrated suspension can thus reduce setting time as well as limit the volume of water to be extracted and treated. To form a mixture of elastomers, the masterbatch is introduced into a kneading tool in order to introduce the vulcanization additives, thereby producing the final elastomer composite ready to be incorporated into a rubber product such as a tire.

Elastomeric composites derived from the liquid mixing processes must have a performance shift compared to the mass mixture. This

2/5 offset results from an improved distribution of the bulking agent in the elastomer matrix. The known industrial processes are intended for carbon black which, unlike silica, has a natural affinity with natural rubber. With silica, it is therefore necessary to use a personalized process to produce a masterbatch with valid material properties.

Since this liquid mixture is expensive and complex and since multiple mixtures and types of elastomer masterbatch compositions are taken into account during the production of a tire, the invention adapts the production structure of a masterbatch using a liquid mixture for the specific treatment of silica.

ABSTRACT

The present invention relates to a system for producing an elastomeric composite based on a selected rubber compounding recipe. The system includes a coagulum preparation facility comprising an emulsion storage facility having an emulsion reservoir storing an elastomeric emulsion; a suspension storage facility having a suspension tank storing a suspension comprising an aqueous solution of bulking agent particles; a flow mixer in fluid communication with both the emulsion tank and the suspension tank; a continuous kneading plant having predefined coagulum production zones through which the composite is transported so that a residence time of the composite in each production zone is regulated before transporting the composite to a production zone next coagulum; and a saline storage facility having a saline tank from which a precise volume of saline solution is supplied to the continuous kneading facility. The system also includes a mixing plant having an extruder disposed in operation in a corresponding barrel having a predetermined length along which multiple predefined composite coagulum production areas are provided before ending in an outlet extension out of which the elastomeric composite is discharged.

In certain embodiments, the coagulum production zones of the continuous kneading installation include:

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- a homogenization zone having a homogenizer with a helical homogenization agitator of predetermined length arranged so as to be able to rotate inside a homogenization chamber having an inlet extension which establishes fluid communication between the mixer flow and the homogenizer and an opposite output extension which establishes a fluid communication between the homogenizer and a kneading zone,

- a kneading zone comprising a kneading and transport agitator of predetermined length arranged so as to be able to rotate inside a kneading chamber having an inlet extension disposed next to the outlet extension of the chamber homogenization and an opposite outlet extension located near an entrance to a wringing zone, the kneading and transport agitator having a transport section and a kneading section facilitating the complementary processes in the kneading; and

- a wringing zone comprising a wringing agitator of predetermined length arranged so as to be able to rotate inside a wringing chamber having an inlet extension arranged near the outlet extension of the chamber kneading and an opposite outlet extension from which the elastomeric composite is discharged in the form of a coagulum, the spin agitator comprising both a texturing section and a spin section facilitating the complementary processes in the area spin.

In certain embodiments, the composite production zones of the mixing installation include:

- a feeding zone along which the elastomeric composite is brought directly to the extruder;

- A drying zone defined downstream of the feeding zone and along which the extruder eliminates in a controlled manner the residual water leaving the elastomer composition; and

- a mixing zone defined intermediate between the drying zone and the outlet extension and along which the extruder advances the composite in the direction of the outlet extension to discharge it

4/5 outside the mixing facility.

For some of these embodiments, the system comprises an additive metering device disposed at an additive metering position in the mixing zone at which the composite reaches a predefined target temperature for the introduction of one or more of several additives. For some of these embodiments, the system also includes a steam extractor which evacuates the residual water out of the elastomeric composite, the steam extractor being disposed upstream of the additive metering device near a terminal extension of the drying area. For some of these embodiments, the additive (s) include silane.

In certain embodiments, the composite production zones of the mixing installation also include a cooling zone defined intermediate between the mixing zone and the outlet extension and along which the temperature of the elastomeric composite is reduced to a target temperature when discharging the mixing plant.

In certain embodiments, the flow mixer has a feed section in which the flow mixer receives the incoming flows of the elastomeric emulsion and the suspension, a parallel effluent section disposed downstream of the feed section and a mixing section arranged further downstream both of the supply section and of the effluent section, the flows of the elastomeric emulsion and of the suspension being maintained at low pressure during mutual contact in said mixing section .

In some embodiments, the extruder includes a twin screw extruder.

In certain embodiments, the system also comprises a cooling installation disposed downstream of the mixing installation and comprising cooling means for reducing a temperature of the elastomeric composite discharged from the mixing installation; and a drying installation arranged downstream of the cooling installation and having a drying device for reducing a water content of the elastomeric composite. For some of these embodiments, the system comprises a press disposed downstream of the drying installation which converts the composite into one or more bales. For some of these embodiments, the system includes

5/5 also a plasticizing installation which regulates the viscosity of the elastomeric composite, the plasticizing installation being arranged intermediate between the drying installation and the press.

Other aspects of the disclosed invention will become apparent from the following detailed description.

BRIEF DESCRIPTION OF DRAWINGS

The nature and various advantages of the invention presented here will become more clearly apparent from the following detailed description, taken in conjunction with the accompanying drawings in which similar references everywhere refer to similar parts and in which:

Figure 1 illustrates a schematic view of a system performing continuous mixing of liquid during a masterbatch production cycle.

FIG. 2 illustrates a schematic view of an example of a coagulum preparation installation of the system of FIG. 1.

FIG. 3 illustrates a cross-sectional view of an example of a mixer used in the coagulum preparation installation of FIG. 2.

FIG. 4 illustrates a sectional view of an example of a homogenization tool used with the coagulum preparation installation of FIG. 2.

FIG. 5 illustrates a sectional view of an example of a transport tool used with the coagulum preparation installation of FIG. 2.

FIG. 6 illustrates a sectional view of an example of a kneading tool used with the coagulum preparation installation of FIG. 2.

FIG. 7 illustrates a sectional view of an example of a shearing tool used with the coagulum preparation installation of FIG. 2.

FIG. 8 illustrates a sectional view of a dewatering tool used with the coagulum preparation installation of FIG. 2.

FIG. 9 illustrates a schematic view of an example of a mixing installation of the system of FIG. 1 and of an example of states in which the mixing installation operates during a masterbatch production cycle.

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DETAILED DESCRIPTION

Referring now more specifically to the figures in which similar numbers identify similar elements, Figure I illustrates an example of a composite preparation system (or "system") which performs multiple mixing operations to produce an elastomeric composite. In a given production cycle, a composite (or "composition") is obtained by following a recipe selected from a plurality of recipes for mixing elastomers. The elastomeric composite is intended, for example, for the manufacture of tires and semi-finished products for tires (including but not limited to profiled products such as soles).

As used herein, the term "composite" refers to the rubber blend produced in the invention exhibited during an entire production cycle. A “composite” here refers to an intermediate coagulum, to a granulated material (which may be wet granules or dry granules and which may be called “granules” or “metered granules”), to an extradate, to a film or to a rubber band and any equivalent finished or semi-finished product derived from System 10. A "composite" refers to an elastomeric composite, an elastomeric composition, a masterbatch composition or simply a "composition "

Still with reference to FIG. 1 as well as with reference to FIG. 2, the system 10 comprises a coagulum preparation system 12 carrying out a continuous flow process for producing a masterbatch composition. As used herein, the terms "elastomer masterbatch", "masterbatch" and "masterbatch" are interchangeable.

The coagulum preparation system 12 includes equipment in which multiple separate coagulum production areas are established. The equipment maintains the rate of production of a masterbatch composition by controlling the residence time of an intermediate composite (i.e. a coagulum) in each production zone established before transporting the composite to a next production area. Therefore in a given masterbatch production cycle, a masterbatch composition recipe is selected from a plurality of masterbatch composition recipes. Coagulum properties are checked not only by controlling the ingredients selected by a given coagulum but also by controlling the duration

7/5 during which the ingredients stay in a given production area during a production cycle in order to control the texture or viscosity of the coagulum. This check includes checking the time at which the composite enters and leaves each production zone (or "length of stay"). The movement of the composite through the coagulum preparation system 12 is thus carried out at a constant and regulated speed.

Still with reference to FIGS. 1 and 2, there is, among the equipment provided with a coagulum preparation system 12, an emulsion storage installation 14 having an emulsion reservoir 14a equipped with an agitator 14b. The emulsion reservoir 14a stores an elastomeric (or latex) emulsion 14c. The elastomer is selected from the group consisting of natural rubber, various synthetic elastomers (eg SBR, BR, etc.) and various mixtures of elastomers. The examples provided here refer to mixtures using natural rubber.

The coagulum preparation system 12 also includes a suspension storage installation 16 having a suspension tank 16a equipped with an agitator 16b. The suspension tank 16a stores a suspension 16c in which the bulking agent particles are dispersed in water. The bulking agent is selected from the group consisting of one or more known materials, including, but not limited to, carbon black, silica, kaolin, chalk, synthesized organic bulking agents, agents natural organic filler materials (eg wood fibers, cellulose fibers, etc.) and their equivalents and combinations thereof. It will be understood that a suspension can be carried out continuously via an online dispersion of T bulking agent in T water.

The agitator 14b maintains a low level of turbulence ensuring sufficient dispersion of the particles in the emulsion. The agitator 16b preferably performs strong turbulence in order to prevent settling. It will be understood that an equivalent means of agitation can be substituted for one or both agitators. In order to avoid settling, it is possible to incorporate a microfluidifier of the Microfluideizer * 'type which fragments any aggregates of bulking agent remaining in the dispersion. The microfluidifier of Microfluideizer ¹ ® 'type can be arranged upstream or downstream of the suspension tank 16a (for example, between the suspension tank and a peristaltic pump 16d as described and illustrated here).

It is also possible to incorporate a grinder and a high pressure homogenizer to guarantee a greater dispersion of the bulking agent.

Still with reference to FIGS. 1 and 2 as well as with reference to FIG. 3, the coagulum preparation system 12 also includes a flow mixer 18 in fluid communication both with the emulsion tank 14a and with the suspension tank 16a. The flow mixer 18 as described here can be replaced by other equivalent and suitable mixing devices.

An emulsion conduit 18a with a predetermined diameter, used in conjunction with a peristaltic pump (or a series of pumps) 14d disposed intermediate between the emulsion conduit and the emulsion reservoir 14a, carries a precise volume of the emulsion 14c from the emulsion reservoir 14a to a flow mixer 18. Similarly, a suspension conduit 18b of predetermined diameter D, used in conjunction with a peristaltic pump (or a series of pumps) 16d disposed intermediate between the conduit of suspension and the suspension tank 16a, transports a precise volume of the suspension 16c from the suspension tank to the flow mixer 18. It will be understood that one or more peristaltic pumps 14d, 16d can be replaced by one or more equivalent devices, comprising , but not limited to, one or more. positive displacement (eg eccentric rotor pumps, diaphragm pumps, piston pumps, etc.).

A respective mass flow meter 14e, 16e can be arranged in operation with respect to the emulsion conduit 18a and the suspension conduit 18b so as to directly measure the mass and density of the emulsion and of the suspension transported. Each mass flow meter 14e, 16e can be a Coriolis flowmeter positioned downstream of a corresponding peristaltic pump, even if it is understood that an equivalent device may be substituted for it.

As illustrated again in FIG. 3, the flow mixer 18 receives the emulsion 14c and the suspension 16c and carries out from there a continuous process for preparing and discharging a composite in the form of a dispersion loading agent in the elastomeric matrix (or "dispersion"). As used here, the "continuous" process identifies a process or any part of a process in which all of the steps can be performed without interruption. The continuous process eliminates the need for intermediate steps and thus supports various industrial applications (for example the production of various rubber compounds for the production of tires). An example of a flow mixer 18 as described and illustrated here is set out in the application published by the applicant no. WO2017 / 021219.

The flow mixer 18 includes a feed section 18c, a parallel effluent section 18d disposed downstream and a mixing section 18e disposed further downstream of both the feed section and the effluent section. During a coagulation preparation cycle, the emulsion 14c and the suspension 16c are simultaneously brought to the mixing section 18e. The feed rate for each element among the emulsion and the suspension can be precisely measured so as to preserve a continuous flow process and to avoid the presence of free latex and uncoagulated filler when discharging out of the coagulum preparation system 12.

Referring again to Figure 3, the flow mixer 18 receives the incoming flows from the emulsion conduit 18a and the suspension conduit 18b in the corresponding supply section 18c. Along a convergence portion 18c ’of the supply section 18c, the emulsion conduit 18a transports the emulsion from the emulsion reservoir 14a to the flow mixer 18 (see arrow A in FIG. 3). In this convergence part, the emulsion conduit 18a penetrates the distribution channel of the suspension conduit 18b going from the suspension reservoir 16a to the flow mixer 18 (see arrow B in FIG. 3). The emulsion conduit 18a and the suspension conduit 18b remain coaxial until the effluent section 18d, having a predetermined length H, ends at a discharge extension 18a 'of the emulsion conduit 18a.

The incoming flows from the emulsion pipe 18a and the suspension pipe 18b maintain a low pressure by mutual contact in the mixing section 18e. The discharge extension 18a ’of the emulsion conduit 18a and a discharge extension 18b’ of the suspension conduit 18b together delimit the boundaries of the mixing section 18e having a predetermined length L.

It will be understood that the conduits 18a, 18b establish a relationship among the supply section 18c, the effluent section 18d and the mixing section 18e preserving stable and effective coagulation. The length and diameter of each conduit are adjustable according to the composition of masterbatch selected as long as the established relationship is respected among the sections of the flow mixer 18. For example, this example illustrates the conduit

10/5 suspension 18b with an internal diameter D larger than the internal diameter d of the emulsion conduit 18a. Those skilled in the art will understand that the reverse configuration can also be used (i.e. the emulsion conduit 18a has the largest diameter) while maintaining the functional relationship between the supply section 18c, the effluent section 18d and mixing section 18th.

The discharge extension 18b ’of the suspension conduit 18b also provides an outlet for the free discharge of the composite from the flow mixer 18 to a continuous kneading plant 20 transporting the composite for further processing. In order to carry out the spread of nanocoagulation at the macro level, the continuous kneading installation 20 must transport the composite without distributing the instantaneous flow. The functional structure is therefore produced so as to delimit the multiple distinct coagulum production zones (or "production zones") while ensuring continuous controlled progression of the composite within each production zone. An example of a continuous kneading installation 20 as described and illustrated here is set out in the request by the applicant PCT / EP2018 / 062475.

Referring again to FIG. 1 as well as to FIG. 4, the coagulum preparation system 12 comprises a continuous kneading installation 20. The flow mixer 18 discharges the composite in a homogenization zone 22 of the continuous kneading plant 20 in which the particles of bulking agent (for example silica) are dispersed more finely. In the homogenization zone 22, an example of a homogenizer 22a is provided which includes a helical homogenization stirrer 22b of predetermined length arranged so as to be able to rotate inside a generally annular homogenization chamber 22c. It will be understood that the homogenization chamber 22c can take any geometric shape in cross section enabling the invention to be implemented.

The homogenization chamber 22c has an inlet extension 22c 'arranged near a discharge end of the flow mixer 18 (and more particularly next to the discharge extension 18b' of the suspension conduit 18b) and a opposite outlet extension 22c ”located near an inlet to a kneading zone 24 of the continuous kneading installation 20 (described in more detail here). The fluid communication established between the discharge end of the flow mixer 18 and the inlet extension 22b ’of the chamber

11/5 homogenization 22c supports the uninterrupted discharge of the composite, generally at atmospheric pressure or at a pressure close to it and typically due to gravity. The homogenizer 22a can be selected from the group consisting of a variety of commercially available devices.

In the initial seconds following discharge of the composite from the flow mixer 18, the composite has not yet reacted at macro level. During homogenization, the homogenization stirrer 22b rotates in a given direction so as to generate sufficient friction between the composite thus transported and an inner wall surface of the homogenization chamber 22c. The geometric shape of the helical agitator 18b relative to that of the homogenization chamber 18c propels the composite in a controlled manner towards a next production zone (i.e. the kneading zone 24) ( see arrow C in Figure 4). The speed of rotation of the agitator, controlled by an M ₂ 2a motor, establishes the transport speed of the composite and the resulting shearing efficiency). Maintaining a given speed of rotation controls the duration of stay of the composite in the homogenization zone 22 and therefore the level of coagulation efficiency produced by the composite at its exit.

Still with reference to FIGS. 1 to 4 as well as with reference to FIG. 5, the flow mixer 18 discharges the composite into a kneading zone 24 of the continuous kneading installation 20 in which the nano-coagulums must be agglomerated in order to create a possible macrostructure in the composite. The improved efficiency of coagulation carried out inside the homogenization zone 22 allows efficient nano-distribution of the filler in the elastomer matrix inside the kneading zone 24.

In the kneading zone 24, an example of kneading and transport element comprises a kneading stirrer 24a of predetermined length arranged so as to be able to rotate inside a kneading chamber 24b. The kneading chamber 24b has an inlet extension 24b 'arranged near a discharge end of the homogenization zone 22 (and more particularly next to the outlet extension 22c ”of the homogenization chamber 22c ) and an opposite outlet extension 24b ”located near an inlet to a wringing zone 26 of the continuous kneading installation 20 (described in more detail here). It will be understood that the kneading chamber

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24b can take any geometric shape in cross section enabling the present invention to be implemented.

The kneading and transport agitator 24a comprises a transport section 25 and a kneading section 27 facilitating complementary processes in the kneading zone 24. With reference to FIG. 5, the transport section 25 comprises a transport screw 25a freely rotating arranged near the outlet extension 24b ”of the kneading zone 24. The transport screw 25a is preferably an endless screw which maintains a predetermined clearance 65 between an outermost periphery of a transport net 25a 'and an inner surface of the kneading chamber. The transport screw 25a comprises multiple transport threads 25a ’of proportional pitch distributed evenly along a predetermined extension of the kneading and transport agitator 24a. The exact number of fillets can be determined based on the composition of the masterbatch selected.

Still with reference to FIG. 6, the kneading section 27 extends between an inlet extension 24b 'of the kneading chamber 24b in the direction of the transport section 25. The kneading section 27 comprises one or more screw transport 27a arranged consecutively interrupted by a proportional number of transitional transport nets 27b arranged collinearly (see Figure 2). Each screw transport system 27a comprises a generally spiral element which maintains a predetermined clearance Cz between itself and an inner wall surface of the kneading chamber. The selection of a spiral element allows a low axial flow and a limited tangent! El drive, thus extending the residence time of the composite in the kneading zone 24 (that is to say the coagulation time).

To carry out the continuous feeding of the composite between the homogenization zone 22 and the kneading zone 24, transitional transport nets 27b comprise an introduction transport net 27b 'disposed near the inlet extension 24b 'of the kneading chamber 24b. Each transition transport net can be proportional in its structure to the threads 25a ′ of the transport screw 25. It will be understood that the exact number of screw transport systems and transport nets can be determined as a function of the mixture composition. - master selected.

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To facilitate kneading (i.e. the mechanical action which propagates the nano-coagulations) while simultaneously achieving controlled progression of the composite towards a next production step, the kneading and transport agitator 24a rotates in a given direction so as to generate sufficient friction between the composite thus transported and an inner wall surface of the kneading chamber 24b. The geometrical shape of the kneading and transport agitator 24a with respect to that of the kneading chamber 24b propels the composite in a controlled manner towards a next production zone (i.e. the zone d 'spin 26) (see arrow D in Figure 5). The speed of rotation of the kneading and transport agitator, controlled by an M _24a motor, establishes the transport speed of the composite and the resulting shearing efficiency.

So as soon as the composite comes into contact with the initial transitional transport net 27b, the composite begins to be subjected to a kneading production process. Any downtime during the transition between production steps (i.e., homogenization and kneading) is thus eliminated. Different volumes of composite, including lower volumes, therefore offer the advantage of maintaining a given rotation speed so as to control the duration of stay of the composite in the kneading zone 24.

Still with reference to Figures 1 to 6 as well as with reference to Figures 7 and. 8, the kneading and transport agitator 24a measures the composite from the kneading zone 24 to the wringing zone 26 of the continuous kneading installation 20, the macro-coagulations derived from the kneading production process being worked mechanically in a suitable form before drying. In the wiping zone 26, an example of a wiping element comprises a wiping agitator 26a of predetermined length arranged so as to be able to rotate inside a wiping chamber 26b. The spin chamber 26b has. an inlet extension 26b ’disposed near a discharge end of the kneading chamber 24b and an opposite outlet extension 26b” from which the composite is. unloaded under the. form of a coagulum. It will be understood that the wringing chamber 26b can take any geometric shape in cross section allowing the implementation of the invention.

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The wiping element 26a comprises both a texturing section 28 and a wiping section 29 facilitating complementary processes in the wiping zone 26. Still referring to FIG. 7, the texturing section 28 comprises a texturing screw 28a rotating freely disposed near the outlet extension 24b ”of the kneading chamber 24b. The texturing screw 28a is preferably an endless screw maintaining a predetermined clearance ΐ?, 8 between an outermost periphery of a cut net 28a ’and an interior surface of the spinning chamber 26b. The texturing screw 28a includes multiple contoured threads 28a ’distributed evenly along a predetermined extension of the wiper element 26a. It will be understood that the exact number of trimmed fillets can be determined according to the composition of masterbatch selected.

At least one optional transport net 28c can be included to make a continuous transition between the kneading zone 24 and the wringing zone 26 via the outlet extension 24b "of the kneading chamber 24b. For such embodiments, each transport net 28c can be proportional in its structure with the transitional transport nets 27b (including the introductory transport net 27b ') described here with respect to the kneading and mixing agitator. transport 24a.

Still with reference to FIG. 8, the wiping section 29 extends from an extension of the wiping element 26a near the outlet extension 26b ”of the wiping chamber 26b in the direction of the texturing section 28. The wiping section 29 includes a conical screw 29a having optional transport threads 29b disposed intermediate between the conical screw and the texturing section 28 (see Figure 2). These optional transport nets can be proportional in their structure to the transition transport nets 27b (comprising the introductory transport net 27b ') described here with respect to the kneading and transport agitator 24a. The conical screw 29a comprises helical threads 29c maintaining a predetermined clearance t ₂ g with respect to an interior wall surface of the wringing chamber 26b.

To facilitate spinning (that is to say the mechanical action supporting the macro-coagulation) while carrying out a controlled progression of the composite towards the discharge out of the installation for preparing coagulum 12, the element spin 26a rotates in a given direction so as to generate a

15/5 sufficient friction between the composite thus transported and the inner wall surface of the wringing chamber 26b. The geometrical shape of the wiping element relative to that of the wiping chamber propels the composite in a controlled manner towards the outlet extension 26b ”of the wiping chamber 26b and of the possible discharge out of the coagulum preparation installation 12 (see arrow E in FIG. 2). The speed of rotation of the wiping element, controlled by an M ₂ 6a motor, establishes the transport speed of the composite and the resulting shearing efficiency.

Therefore, inside the wringing zone 26, the texturing section 28 defines the coagulum size of the composite before introduction of the coagulum into the wringing section 29. The wringing section 29 purges the composite by putting the coagulum under pressure, for example, from 10 bar to 80 bar pressure. In some embodiments, a pressure of 30 bar is used.

The coagulum preparation installation 12 thus achieves the discharge of coagulum (that is to say of the composite) in the form of a generally continuous outlet simultaneously with the continuous supply of emulsion 14c and of suspension 16c in the flow mixer 18.

The coagulum preparation installation 12 is adapted to support the continuous advancement of the composite at atmospheric pressure through the kneading zone 24 and the wringing zone 26. Each element among the kneading chamber 24b and the wringing chamber 26b has a predetermined cross-sectional geometric shape preventing rotation of the composite therein (for example, each chamber may be provided as a generally annular member, or each chamber may include one of a U-shaped chamfer and a wedge U-shaped). Such a geometric shape can be combined with one or more anti-rotation accessories comprising one or more anti-rotation bars (not shown).

The coagulum preparation system 12 also includes a saline storage installation 30 having a saline tank 30a equipped with an agitator 30b (although it will be understood that an equivalent stirring means can be used from the moment where it guarantees sufficient dispersion of the particles). The saline tank 30a stores a saline solution 30c selected from the group consisting of one or more saline solutions known to be effective for managing the coagulation of rubber.

16/5 natural (for example by destabilizing a dispersion comprising silica). Such saline solutions include, but are not limited to, solutions of water-soluble chloride salts, nitrates, sulfates and acetates of sodium, potassium, calcium, magnesium, zinc and aluminum and combinations and equivalents thereof.

A saline line 30d of predetermined diameter carries, together with a peristaltic pump (or a series of pumps) 30e disposed intermediate between the saline line and the saline tank 30a, a precise volume of saline solution 30c from the saline tank at the continuous kneading plant 20 of the coagulum preparation system 12. A mass flow meter 30f can be arranged in operation with respect to the saline conduit 30d and to. the continuous kneading installation 20, said mass flowmeter possibly being a Coriolis flowmeter positioned downstream of the peristaltic pump 30e. As described here with respect to the emulsion tank 14a and the suspension tank 16c, the peristaltic pump 30e and / or the mass flow meter 30f can be replaced by one or more equivalent devices.

In the exemplary embodiment illustrated in FIGS. 1 and 2, the saline solution conduit 30d transports the saline solution along the length of the homogenization zone 22 of the continuous kneading installation 20. The Those skilled in the art will understand that the saline solution can be transported to any part of the continuous kneading plant 20 depending on the rubber mix recipe selected.

Referring again to FIG. 1, the coagulum preparation installation 12 transports the composite (that is to say the coagulum) to a dewatering installation 32. The dewatering installation 32 comprises an apparatus spin and / or drying adapted in functional communication with a granulation device arranged in series with it. An example of a suitable wringing and / or drying apparatus is illustrated here in the form of a drying device 32a which twists the coagulum and thus reduces its water content before granulation. The resulting effluent is discharged by the dewatering device for appropriate treatment (see arrow F in Figure 1). The optimal water content may vary depending on the recipe selected and the specific equipment used to coagulate, dry and dry the composite. The dewatering device 32a can be selected from the group consisting of a variety of

17/5 commercially available devices and it will be appreciated that other suitable devices may be substituted for them, including, but not limited to, extruder dryers, fluidized bed dryers, hot fair and other oven dryers and their equivalents.

The drying device 32a discharges the dehydrated coagulum towards the granulation apparatus, an example of which is illustrated in the form of a granulator 34 which converts the dehydrated coagulum into wet granules (also known as “granulated material”, “ granules "or" granules "). Granulator 34 can be selected from the group consisting of a variety of commercially available granulating devices. When discharged from the granulator 34, the composite is adapted to be dosed with one or more additives and. vulcanizing agents.

Still with reference to FIG. 1 as well as with additional reference to FIG. 9, the stripping installation 32 transports the wet granules via a conduit 36 going from the granulator 34 to a mixing installation 40 in communication with it (see arrow G in Figure 9). In certain embodiments, this transport is carried out by a programmable pneumatic device (not illustrated) measuring the granules at a predetermined speed. The transfer can also be carried out by one or more transport systems comprising one or more transfer belts as known in the art.

The mixing installation 40 comprises a wet granule metering system having a discharge hopper 42 and a motorized transport system 44. An unregulated screw transport system (not illustrated) allows the discharge of granules into the discharge hopper 42 at a fixed speed according to the flow rate setpoint. A monitoring system (not illustrated) having at least one sensor can detect one or more filling speeds at which the granules are transported to the hopper, a current filling height of the granules in the hopper and. a current weight of the granulated material in the hopper (for example as determined from the detection of the filling speed and the current filling height). The monitoring system can generate one or more signals indicating a predetermined filling height and / or weight. Monitoring can be continuous or intermittent so that control signals can adjust in real time.

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At the mixing installation 40, the hopper 42 discharges all or part of the granulated material discharged in the form of a predetermined dosage (that is to say metered granules) to the motorized transport system 44. The motorized transport system 44 may comprise at least one mass sensor or equivalent means for weighing the metered granules before dispensing them to a mixer 46. When detecting the weight of the metered granules, the motorized transport system 44 checks the behavior with the prescriptions of the recipe. Distribution to the mixer 46 is generally carried out at atmospheric pressure or at a pressure approaching it and typically under the effect of gravity.

Still with reference to Figures 1 and 9, the motorized transport system 44 delivers the granulated material discharged to the mixer 46 via a feed hopper 46a (see arrow H in Figures 1 and 9). The feed hopper 46a brings the granulated material to an extruder 48 of the mixer 46. As illustrated and described here, the extruder 48 is a twin screw extruder with corotation allowing a controlled flow of all the elements transported and the reproducibility of the duration of stay. The rotating screws are arranged inside a barrel 49 inside which the granulated material advances in a controlled manner towards a barrel outlet 49d from which the mixer 46 discharges the composite. Twin screw extrusion is appreciated for its regularity and increased productivity due to continuous processing. If a twin screw extruder is matched with the weight dosing capacity of the motorized transport system 44, a target feed speed can be set and maintained throughout an entire production cycle. The twin screw extruder can use a variety of known screw and barrel configurations to process a wide range of raw materials depending on the recipe selected. As used herein, the term "twin screw extruder" also means "twin conical extruder", "twin screw roller head extruder", "twin screw discharge extruder", "twin screw rolling mill", " kneader "," co-rotating mixer "," continuous processing device "and any other equivalent nomenclature commonly used and understood in the art to refer to similar rubber equipment and its equivalent.

The barrel 49 comprises multiple zones 49a, 49b, 49c in which the temperature of the composite is specified for each zone. During a cycle of

19/5 production, the time at which the composite enters and leaves each zone ("length of stay") is also specified. System 10 thus carries out the chemical reactions necessary to obtain a mixture of elastomers having target rheological properties. These properties are variable and adaptable depending on the optimal implementation of the mixture of elastomers. For example, for mixtures intended for the manufacture of tires, the resulting tire should exhibit target performance properties (for example reduced roll resistance, improved wear resistance, comparable grip in dry and wet conditions, etc.).

Among the zones specified in the barrel 49, a feeding zone 49a is provided in which the mixer 46 receives the granulated material (that is to say the metered granules) from the motorized transport system 44.

Inside the feed zone 49a, the closely related rotation of the extruder 48 propels the composite in a controlled manner in the form of an extradate having a target temperature at the outlet out of the feed zone. This target temperature is typically in a range from about 120 ° C to about 180 ° C, and preferably from about 140 ° C to about 150 ° C.

The extradate enters a drying zone 49b of the barrel 49 along which the residual water is again removed from the extrudate. Along the drying zone 49b, the barrel 49 maintains a constant temperature as the composite is transported all along. The drying zone 49b ends at a steam extractor 50 evacuating the water extracted from the extrudate at a predetermined speed (see arrow I in FIGS. 1 and 9). The steam extractor 50 can be selected from the group consisting of a variety of commercially available devices, including, but not limited to, those having vacuum means or any other means for removing water vapor and any inherent particulate matter.

A mixing zone 49c is defined along a part of the barrel 49 between the steam extruder 50 and the barrel outlet 49d. Along the mixing zone 49c, the additional elastomer (s) and the necessary additives are brought into the extruder 48, with the complementary ingredients forming the crosslinking system.

Inside the mixing zone 49c, the extruder 48 advances the elastomeric material towards an additive dispenser 52 introducing one or more

20/5 several additives 52a in the mixing zone 49c. The additive dispenser 52 is placed in an additive metering position of the mixing zone 49c in which the extrudate reaches a predefined target temperature for the introduction of the additives 52a. The preset temperature is defined according to the selected recipe. The additive dispenser 52 can comprise at least one element from a volumetric dispenser and a gravimetric dispenser so that the additives 52a can be introduced both in liquid and powder form according to the needs of the selected recipe.

Additives introduced into the elastomeric material in the additive metering position can include, but are not limited to, one or more oils, one or more complementary elastomers, one or more recycled materials, one or more protective agents, and one or more antioxidants.

In certain embodiments, the silane is introduced into the mixture in the additive metering position. After reaction, the silanes which are coupling silanes produce a covalent bond between the elastomer and the silica. In the manufacture of tires and semi-finished products for tires, the silanization technology of silica is known for use in green tires so as to give the resulting tire product the properties of improved abrasion resistance, reduced roll resistance and improved fuel economy.

After the introduction of the additives 52a, the extruder 48 advances the elastomeric material downstream of the additive dispenser 52 in the direction of an additional additive dispenser 54 which introduces one or more additional additives 54a into the mixing zone 49c . The additional additive dispenser 54c is arranged in an additional dosing position of the mixing zone 49c in which the extrudate reaches a predefined target temperature for the introduction of the additional additives 54a. The preset temperature is defined according to the selected recipe.

At least one element among the additive dispenser 52 and the additional additive dispenser 54 may comprise at least one element among a volumetric dispenser and a gravimetric dispenser so that the additives 52a, 54a can be introduced both in liquid form as powder according to the needs of the selected recipe. The nature of the additive (i.e. whether it is in the form of a liquid or powder) can determine the dosing device to be used

21/5 (for example a powder weighing system and a positive displacement pump for the liquid).

Referring to Figures 1 and 9, the extruder 48 discharges the resulting extradate out of the outlet extension 49d in the form of an elastomeric composition. In certain embodiments, at the exit from the mixing zone 49c and before the discharge from the exit extension 49d, T extruder 48 propels the mixture in a controlled manner downstream of the mixing zone towards a cooling zone 49e. In the cooling zone 49e, the temperature of the mixture is reduced to a target temperature before discharging out of the outlet extension 49d. For certain recipes, such cooling may be desirable before the transfer of the elastomeric composition towards an apparatus or a downstream installation forming the composition.

In an exemplary embodiment, the mixture is discharged from the mixing installation 40 in the form of a granulated material (also known as “granules” or “granules”) having the bulking agent and the additives necessary for industrial application. The granulated material is then transported to a cooling installation 60 at which the temperature of the elastomeric composition is further reduced (see arrow J in FIG. 1). The cooling installation 60 comprises a cooling means (such as a cooling bath 60a) known in the art for reducing the temperature of an elastomeric composition, thus preparing it for its subsequent treatment and / or storage.

Still with reference to FIG. 1, the system 10 transports the elastomer composition from the cooling installation 60 to a drying installation 62 having a drying device which reduces the water content of the elastomer composition and discharges the resulting effluent for appropriate treatment. The drying device can be selected from the group consisting of a variety of commercially available devices and it will be understood that other suitable devices can replace it, including, but not limited to, extruder driers, driers fluidized bed, hot air and other kiln dryers and their equivalents.

The system 10 discharges the elastomer composition from the drying installation 62 and transports it towards a press 64. The press 64 converts the dehydrated composition in one or more bales 66 from which various and diverse

22/5 kinds, grades, species, batches and groups of elastomers are generated. Press 64 can be selected from the group consisting of a variety of commercially available presses and equivalent devices. Elements can be generated from such bullets, as known in the art. When discharged from the press 64, the elastomeric composition is therefore suitable for use as a masterbatch composition.

In certain embodiments of the system 10, the system may include a plasticizing installation 68 which performs a step of adjusting the viscosity of the elastomeric material as a function of its optimal use (for example as a masterbatch or as a mixture). In such embodiments, the elastomeric material discharged from the drying installation 62 is then brought to the plasticization installation 68. To control the viscosity of the material, the plasticization can be carried out by mechanical treatment or by addition of chemical plasticizer , as known in the art. One or more additional additives can be introduced into the mixture at the level of the plasticizing installation 68 (such as additives comprising, for example, one or more additives described here with respect to the mixing zone 49c). During the discharge from the plasticizing installation 68, the elastomeric material is transferred to the press 64 (for example by a transport system 70 or by equivalent means) in order to prepare one or more bales 66 therein. A plasticizer used at the plasticizing facility 68 may be selected from the group consisting of a variety of commercially available plasticizers, including, but not limited to, a thumbscrew, a continuous mixer (e.g. cylindrical tool) or a batch mixer (for example an internal mixer).

Referring now to Figures 1 and 9, an exemplary method is described implemented by the system 10 to create an elastomeric composition intended for use in one or more tires and / or in one or more tire products. All the positions are indicated relative to a longitudinal extension of the barrel 49 of the mixing installation 40. All the figures and all the numbers are, provided by way of example only and do not limit the invention to particular values. Those skilled in the art will understand that various modifications and variants can be applied without it being necessary to carry out experiments and without departing from the scope of the invention described.

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EXAMPLE

The following example illustrates an example of states in which system 10 operates.

The following Table 1 illustrates three states in which the coagulum preparation system 12 implements a continuous flow process to produce a masterbatch composition. These states are carried out with two examples of silica suspension as identified below.

1 2 3 Type HA latex emulsion / Silica suspension * (selected from highly dispersible silicas having a CTAB specific surface of 160 m ² / g (*) Mg ²⁺ doped (**) and P200) / saline solution Plantation latex emulsion / Silica suspension (selected from highly dispersible silicas with a CTAB specific surface of 160 m ² / g (*) Mg ²⁺ doped (**) and P200) / saline solution HA latex emulsion / eSBR1500 latex emulsion / silica suspensi on (selected from highly dispersible silicas having a CTAB specific surface of 160 m ² / g (*) Mg ²⁺ doped (**) and P200) / saline solution Minimum mass concentrations (%) 9/9/5 35/23/5 61 / 24.5 / 14/9 Flow rates (kg / h) 27.6 / 162/23 78.2 / 90/33 17 / 10.6 / 80.2 / 18 Crusher (rpm) / Injection pressure (bar) 2000/300 2000/300 2000/300 Homogenization / Wise kneading / Texturing / Pre-drying (rpm) 400/30/20/30 560/40/5/30 400/30/20/30

(*) Selected from highly dispersible silicas with a specific surface

CT AB of 160 m ² / g Mg ² doped (* *) commercially available under the name Solvay under the brand ZEOSIL® 1165 MP and. amorphous precipitated silica having a CT AB specific surface of 200 m ² / g Mg ² 'doped commercially available under the name Solvay under the brand ZEOSIL® Premium 200MP.

(**) As described in patent application, collective WO2013 / 053733

TABLE 1

24/5 • A recipe is selected to make, in the coagulum preparation system 12, a mixture of natural rubber and silica containing 75 PHR of bulking agent.

• The emulsion tank 14a brings a 60% concentrated latex to the flow mixer 18 at a speed of 30 kg / h.

• The suspension tank 16a brings a suspension of concentrated silica at 9% to the flow mixer 18 at a speed of 135 kg / h.

• The saline tank 30a supplies a saline solution to the homogenizer 22a at a speed of 18 kg / h.

• The mixture of the emulsion and the suspension produces a coagulum containing 75 PHR of bulking agent at a rate of 31.5 kg / h (18 kg / h + 13.5 kg / h = 31.5 kg / h) with an initial concentration of 19% by weight (concentration of the coagulum = 31.5 / (135 + 30) = 19% by weight)

The coagulation, spinning and drying stages gradually eliminate the water content of the composite, as illustrated below:

State of matter Initial Coagulum Wet pellets Pellets dry Content water (%) 81 80 40 0 Mass flow (kg / h) 165 165 44 29 Temperature (° C) 35 60 60 150

TABLE 2 * The discharge hopper 42 brings the wet granules (having a water content of 40%) to the feed zone 49a of the mixing installation at a speed of 44 kg / h (position C0).

* The extruder 48 advances at a speed of 250 rpm (positions C0 to C l 1).

* The steam extractor 50 operates at a steam discharge rate of 18 kg / h (position C6).

* For the selected recipe, the dosages of each additive are regulated as follows:

o Maximum flow of antioxidant 6PPD introduced by the additive doser 52: 0.22 kg / h (position C7) o Maximum flow of silane introduced by the additive doser: 2.25 kg / h (position C10) * The mass flows of the different elements are calculated according to the selected recipe. So for the following recipe, the flows of the different ingredients are regulated as follows, respecting the working temperatures of each additive:

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Ingredients Masterbatch Silane Antioxidant Share (PHR) 175 15 1.5 Mass flow (kg / h) 26.4 2.25 0.22 Maximum temperature (° C) 180 ° C 160 ° C 180 ° C

TABLE 3 * So in order to carry out the necessary chemical reactions producing a mixture having the intended rheological properties, the following extradate temperatures are obtained in each zone from the feeding zone 49a, the drying zone 49b and the mixing zone 49c (see figure 9):

Position C0-C2 C3-C5 C6 C7 C8-C9 Cl 0-11 Function Food Drying Steam discharge (drying) Formulation Cooled surely Lamination Temperature (° C) 140 140 140 120 100 100 Type of area pump kneaded ssag e pump mixed pump kneading

TABLE 4 • From the steam extractor 50 to the mixing zone 49c, the extruder 48 eliminates the water content of the extradate so that the extradate has a relative humidity of approximately 0-2% (positions C6 to Cl 1).

• At the outlet extension 49d, the mixing installation 40 discharges the masterbatch composite out of the barrel 49 in the form of dry granules at the discharge speed of 29 kg / h. The dry granules have a product temperature of around 150 ° C.

· The dry granules are cooled to a temperature of 80 ° C. at the level of the cooling installation 60 and then dried at the level of the drying installation 62. The composite is finally plasticized at the level of the plasticization installation 68 and transported to press 64 to form one or more bales 66.

EXAMPLE

Using system 10, several masterbatches (MB) are produced in liquid form according to the following compositions:

26/5

MB "L" MB "M" MB "G" MB "H" MB "K" Natural rubber 100 100 100 100 100 Silica 160MP 62 64 74 ”7 ^ 74 Si69 7.0 Si75 7 2 OCTEO * 8.5 6PPD 1.5 L5 1.5 1.5 1.5

* The silica coating agent commercially available under the name Degussa under the brand DYNASYLAN® OCTEO

TABLE 5

The masterbatches are then subjected to standard mixing in an internal mixer and finalized (for example with the introduction of one or more vulcanizing agents such as sulfur and one or more accelerators) in an external mixer (for example a rolling mill) according to the following formulas:

Comparative examples of mixing Formulation (parts in mass) I 2 3 4 5 MB "L" 163.50 MB "M" 172.46 MB "G" 175.50 MB "H" 180.73 MB "K" 183.96 N234 3 3 3 3 3 Si69 * 6.74 8.04 8.04 DPG 0.67 0.70 0.80 0.78 0.80 6PPD 2.5 2.5 2.5 2.5 2.5 Paraffin 6266 1 1 1 1 1 Stearic acid 2.5 2.5 2.5 2.5 2.5 ZnO 1 I 1 I 1 CTP 0.15 0.15 0.15 0.15 0.15

27/5

2H sulfur solution ** 1.6 1.58 1.46 2.34 1.46 CB S 2.05 2.05 2.05 2.05 2.05

Where applicable, Si69 is added to the internal mixer.

TABLE 6 • As shown in the table below, after 1 month, it is observed that the presence of silane in the masterbatches delays the consumption of 6PPD and significantly reduces the Mooney viscosity.

Masterbatches <: L " MB "M" MB "G" MB "H" MB "K" Ball MS0.04 (5 + 10) > 220 94 > 220 148 128 Level 6PPD (%) 0.27 0.70 0.24 0.87 0.48

TABLE 7 • The reduction in Mooney viscosity facilitates the use of additives and the efficiency of their incorporation in the internal mixer.

Comparative examples of mixing I 2 3 4 5 MFTR.23T (kcycles) 171.2 235.0 23.9 248.7 131.5 σ _Η 2 60-c (MPa) 22.1 21.5 16.4 22.4 21.9 CCH2 60 ° C (%) 516.4 521.7 365.9 597.8 516.0 Fdz ioo ° c (MPa) 63.6 64.2 39.2 70.9 60.4 OlDZ! 00 ° C ( ^{: i /} o) 262.2 271.0 151.8 318.6 217.2 G * oj% _a jter6o ° c (MPa) 4.4 3.6 8.6 6.4 5.8 G * 50% 60 c (MPa) 1.9 1.7 2.8 2.0 2 2 G * o, l% return (MPa) 3.9 3.3 6.7 5.6 4.9 AG * 6o’c (MPa) 2.0 1.57 3.97 3.55 2.75 G _œax 60 ° c (MPa) 0.38 0.31 0.79 0.67 0.53 tan (Ô) niax return 60 ° C 0.137 0.129 0.180 0.192 0.160 Note Z 86 88 62 86 85

28/5

dm av CETR (mg) 28.3 25.2 30.0 24.7 30.4

TABLE 8

The presence of silane in the masterbatches increases the resistance to fatigue and reduces the non-linearity in the final mixture. In the case where the silane is a binding agent (mixtures 2 and 5), its presence in the composite also reduces the mass part on CETR, thus indicating an improvement in the wear resistance of the mixture.

In certain methods, at the outlet of the internal mixer, the temperature drop of the initial rubber compounding composition does not exceed 180 ° C. and at the outlet of the external mixer, the outlet temperature of the initial compound initial rubber mixture does not exceed 120 ° C.

Test measurement

Fatigue MFTR (“MFTRA” test)

The fatigue strength, expressed in number of cycles or in relative units (ru), is measured in a known manner on an unscored test specimen subjected to low frequency tensile deformations repeated up to an elongation of 20% , using a Monsanto machine (type “MFTR”) until the test specimen breaks, in accordance with French standard NF T46021.

Tear resistance

The tear resistance indices are measured at 100 ° C. In particular, the force to be exerted in order to obtain the rupture (FRD, in MPa) is determined on a test specimen with dimensions of 10 ^x 105 x 2.5 mm notched in the center of its length to a depth of 5 mm to allow the test specimen to break.

Viscosity

Mooney viscosity, also known as viscosity or plasticity, characterizes, in a known manner, solid substances. A consistometer

29/5 oscillating as described in ia standard ASTM D1646 (1999) is used. This plasticity measurement is carried out according to the following principle: the sample analyzed in a green state (that is to say, before hardening or before crosslinking) is molded (formed) in a cylindrical chamber heated to a given temperature (by example 35 ° C or 100 ° C). After one minute of preheating, the rotor turns inside the specimen at 2 rpm and the torque necessary to maintain this movement is measured during 4 minutes of rotation. The Mooney viscosity (ML 1 + 4) is expressed in "Mooney unit" (with 1UM = 0.83 Nm) and corresponds to the value obtained at the end of the 4 minutes.

H2 break

The rupture measurements are carried out at 60 ° C and according to French standard

NF T 46-002 of September 1988. The rupture specimens are of the H2 type as described in the standard NF ISO 37 of I ^e1 March 2012, except the thickness which is 2.5 cm. The force to be exerted to obtain the rupture (tensile stress in MPa (in N / mm)) is determined and the elongation at rupture is measured (in%).

Water content :

The Karl-Fisher method is used.

Dispersion

In known manner, the dispersion of bulking agent in an elastomeric matrix can be represented by the result Z measured, after crosslinking, according to the method described by S. Otto and Al in Kautschuk Gummi Kunststoffe, 58 Jahrgang, NR 7-8 / 2005, in accordance with ISO 11345 (literal translation of the french magazine KGK: plastics, rubber eraser, ^58th year, No. 7- 8/2005).

The calculation of the result Z is carried out on the basis of the percentage of area in which the bulking agent is not dispersed (“area not dispersed in%”), as measured by the device “disperGRADER +” supplied with its operating mode and its software "disperDATA" supplied by the company Dynisco according to the equation:

Z ^::: 100 - (area not dispersed in%) /0.35

30/5

The percentage of non-dispersed surface is measured by a camera observing the surface of the sample under incident light at 30 °. Clear dots are associated with the bulking agent and agglomerates, while dark dots are associated with the rubber matrix; digital processing transforms the image into a black and white image and makes it possible to determine the percentage of non-dispersed surface, as described by S. Otto in the above-mentioned document.

The higher the Z result, the better the dispersion of the bulking agent in the elastomer matrix (a Z result of 100 corresponds to perfect dispersion and a Z result of 0 to poor dispersion). We will consider that a result Z greater than or equal to 80 corresponds to a surface having a very good dispersion of the bulking agent in the elastomer matrix.

Dynamic properties

The dynamic properties including tan (δ) max, representing hysteresis, are measured on a viscoanalyzer (Metravib VA4000), according to standard ASTM D 5992-96. The response of a sample of the vulcanized composition (cylindrical specimens each having a thickness of 2.8 mm and a cross-sectional area of 78 mm), subjected to a sinusoidal stress according to a single alternating shear, at a frequency of 10 Hz , at a temperature of 60 ° C, is recorded. A voltage amplitude sweep is performed from 0.1% to 50% peak to peak (forward cycle), then from 50% to 0.1% peak to peak (return cycle). The exploited results are the complex dynamic shear modulus (G *) and the loss factor tan (δ). For the forward cycle, the maximum value of tan (δ) observed is called tan (δ) max. For the return cycle, the module G * at 50% deformation is called G * 50%.

A system implementing a process for creating a composite in the form of a coagulum can be summarized as comprising the following elements:

- the use of a mechanical coagulator to achieve heterocoagulation with high levels of bulking agent,

31/5

- the controlled dosing of the granules of natural rubber / silica composites at the entrance to the mixing plant 40 to guarantee the resulting silane / silica ratio;

- the dosage of injection of the silane into the mixing installation 40 after drying to guarantee the exceptional distribution of the bulking agent in the matrix, preventing re-agglomeration of the bulking agent;

- the use of a co-rotating twin screw extruder regulating the residence time of the composite, thus respecting the energy level, the temperature and the dosage of the additives;

- the availability of a plasticizer after mixing and cooling to allow recovery of the masterbatch during a traditional mixing process (i.e. a mixing process using an internal mixer and an external mixer).

As used herein, the term "process" or "method" may include one or more steps performed at least using an electronic or computer device having a processor to execute the instructions performing the steps.

The terms "at least one" and "one or more" are used interchangeably. The ranges described here as "between a and b" include, the values for "a" and "b".

Even if these are particular embodiments of the exposed apparatus which have been illustrated and described, it will be understood that various changes, additions and modifications can be made without departing from the spirit and scope of this description. Consequently, no limitation is applied to the scope of the invention set out here, except that of the appended claims.

Claims (12)

1. System (10) for producing an elastomeric composite according to a selected rubber compounding recipe, comprising: a coagulum preparation installation (12) comprising: an emulsion storage facility (14) having an emulsion reservoir (14a) storing an elastomeric emulsion (14c); a suspension storage installation (16) having a suspension tank (16a) storing a suspension (16c) comprising an aqueous solution of bulking agent particles, a flow mixer (18) in fluid communication with each of the elements emulsion tank and suspension tank; a continuous kneading installation (20) having predefined coagulum production zones through which the composite is transported so that a residence time of the composite in each production zone is regulated before transporting the composite to a zone next coagulum production; and a saline storage installation (30) having a saline tank (30a) out of which a precise volume of saline solution is transported to the continuous kneading installation (20); and a mixing installation (40) comprising an extruder (48) disposed in operation in a corresponding barrel (49) having a predetermined length along which multiple predefined composite production zones (49a, 49b, 49c) are provided before ending in an outlet extension (49d) from which the elastomeric composite is discharged. 2. System according to claim 1, in which the coagulum production zones of the continuous kneading installation (20) comprise: a homogenization zone (22) having a homogenizer (22a) with a helical homogenization agitator (22b) of predetermined length arranged so as to be able to rotate inside a homogenization chamber (22c) having an extension inlet (22b ') which establishes fluid communication between the flow mixer (18) and the homogenizer and an outlet extension (22b ”) 33/5 opposite which establishes a fluid communication between the homogenizer and a kneading zone (24); a kneading zone (24) comprising a kneading and transport agitator (24a) of predetermined length arranged so as to be able to rotate inside a kneading chamber (24b) having an inlet extension (24b ') arranged next to the outlet extension of the homogenization chamber and an opposite outlet extension (24b ”) placed near an inlet to a wringing area (26), the kneading and mixing agitator transport having a transport section 25 and a kneading section 27 facilitating the complementary processes in the kneading zone, and a wringing zone (26) comprising a wringing agitator (26a) of predetermined length arranged so as to be able to rotate inside a wringing chamber (26b) having an inlet extension (26b ') arranged near the outlet extension of the kneading chamber and an outlet extension (26b ”) opposite outside from which the elastomeric composite is discharged in the form of a coagulum, the wringing agitator comprising both a texturing section (28) and a wringing section (29) facilitating the complementary processes in the area of spinning. 3. System according to claim 1 or 2, in which the composite production zones of the mixing installation (40) comprise: a feeding zone (49a) along which the elastomeric composite is brought directly to the extruder (48); a drying zone (49b) defined downstream of the feeding zone and along which the extruder eliminates in a controlled manner the residual water out of the elastomer composition; and a mixing zone (49c) defined intermediate between the drying zone and the outlet extension (49d) and along which the extruder (48) advances the composite towards the outlet extension for discharge from the mixing plant. 4. The system of claim 3, further comprising an additive metering device (52) disposed in an additive metering position of the mixing zone (49c) in which the composite reaches a predefined target temperature for 34/5 the introduction of one or more additives (52a). 5. The system of claim 4, further comprising a steam extractor (50) which discharges the residual water out of the elastomeric composite, the steam extractor being disposed upstream of the additive metering device (52) near a terminal extension of the drying zone (49b). 6. The system of claim 4 or claim 5, wherein the additive (s) comprise silane. 7. System according to any one of claims 3 to 6, in which the composite production zones of the mixing installation (40) further comprise a cooling zone (49e) defined intermediate between the mixing zone (49c) and the outlet extension (49d) and along which the temperature of the elastomeric composite is reduced to a target temperature when discharged from the mixing plant (40). 8. System according to any one of the preceding claims, in which the flow mixer (18) comprises a feed section (18c) in which the flow mixer receives the incoming flows of the elastomeric emulsion (14c) and of the suspension (16c), a parallel effluent section (18d) disposed downstream of the feed section and a mixing section (18e) disposed further downstream of both the feed section and the d section effluent, the flows of the elastomeric emulsion and the suspension being maintained at low pressure during mutual contact in said mixing section. 9. System according to any one of the preceding claims, in which the extruder (48) comprises a twin screw extruder. 10. System according to any one of the preceding claims, further comprising: a cooling installation (60) arranged downstream of the mixing installation (40) and comprising a cooling means making it possible to reduce the temperature of the elastomeric composite discharged from the mixing installation; 35/5 and a drying installation (62) arranged downstream of the cooling installation and having a drying device for reducing a water content of the elastomeric composite. 11. The system of claim 10, further comprising a press (64) disposed downstream of the drying installation which converts the composite into one or more bales (66). 12. The system of claim 11, further comprising a plasticizing installation (68) which adjusts a viscosity of the elastomeric composite, the plasticizing installation being arranged intermediate between the drying installation (62) and the press (64 ).