EP3113867B1 - Verfahren und vorrichtung zur dispersion von gas in einer flüssigkeit - Google Patents

Verfahren und vorrichtung zur dispersion von gas in einer flüssigkeit Download PDF

Info

Publication number
EP3113867B1
EP3113867B1 EP15714025.2A EP15714025A EP3113867B1 EP 3113867 B1 EP3113867 B1 EP 3113867B1 EP 15714025 A EP15714025 A EP 15714025A EP 3113867 B1 EP3113867 B1 EP 3113867B1
Authority
EP
European Patent Office
Prior art keywords
liquid
gas
tube
plate
mixing chamber
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
EP15714025.2A
Other languages
English (en)
French (fr)
Other versions
EP3113867A1 (de
Inventor
Sylvie Baig
Pedro Fonseca
François LE QUESNE
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Suez International SAS
Original Assignee
Suez International SAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Suez International SAS filed Critical Suez International SAS
Publication of EP3113867A1 publication Critical patent/EP3113867A1/de
Application granted granted Critical
Publication of EP3113867B1 publication Critical patent/EP3113867B1/de
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20Mixing gases with liquids
    • B01F23/23Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
    • B01F23/236Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids specially adapted for aerating or carbonating beverages
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20Mixing gases with liquids
    • B01F23/23Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
    • B01F23/232Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids using flow-mixing means for introducing the gases, e.g. baffles
    • B01F23/2323Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids using flow-mixing means for introducing the gases, e.g. baffles by circulating the flow in guiding constructions or conduits
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20Mixing gases with liquids
    • B01F23/23Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
    • B01F23/231Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids by bubbling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20Mixing gases with liquids
    • B01F23/23Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
    • B01F23/2319Methods of introducing gases into liquid media
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20Mixing gases with liquids
    • B01F23/23Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
    • B01F23/232Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids using flow-mixing means for introducing the gases, e.g. baffles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20Mixing gases with liquids
    • B01F23/23Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
    • B01F23/234Surface aerating
    • B01F23/2341Surface aerating by cascading, spraying or projecting a liquid into a gaseous atmosphere
    • B01F23/23412Surface aerating by cascading, spraying or projecting a liquid into a gaseous atmosphere using liquid falling from orifices in a gaseous atmosphere, the orifices being exits from perforations, tubes or chimneys
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20Mixing gases with liquids
    • B01F23/23Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
    • B01F23/237Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media
    • B01F23/2376Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media characterised by the gas being introduced
    • B01F23/23762Carbon dioxide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/30Injector mixers
    • B01F25/31Injector mixers in conduits or tubes through which the main component flows
    • B01F25/314Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit
    • B01F25/3142Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction
    • B01F25/31423Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction with a plurality of perforations in the circumferential direction only and covering the whole circumference
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40Static mixers
    • B01F25/42Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/433Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
    • B01F25/4334Mixers with a converging cross-section
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20Mixing gases with liquids
    • B01F23/23Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
    • B01F23/237Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media
    • B01F23/2376Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media characterised by the gas being introduced
    • B01F23/23761Aerating, i.e. introducing oxygen containing gas in liquids
    • B01F23/237611Air
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20Mixing gases with liquids
    • B01F23/23Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
    • B01F23/237Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media
    • B01F23/2376Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media characterised by the gas being introduced
    • B01F23/23761Aerating, i.e. introducing oxygen containing gas in liquids
    • B01F23/237612Oxygen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/20Mixing gases with liquids
    • B01F23/23Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
    • B01F23/237Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media
    • B01F23/2376Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids characterised by the physical or chemical properties of gases or vapours introduced in the liquid media characterised by the gas being introduced
    • B01F23/23761Aerating, i.e. introducing oxygen containing gas in liquids
    • B01F23/237613Ozone

Definitions

  • the invention relates to a method and a device for dispersing gas in a downward flow of liquid.
  • the invention more particularly relates to a method and a dispersing device with hybrid liquid gas jet mixer and jet injector.
  • the method is intended to homogeneously disperse the gas in the form of fine bubbles in a liquid engine for contacting liquid gas or for subsequent contact with the mass of liquid in a surrounding contactor in which the device is implanted.
  • the device is composed of an injection head comprising a liquid-jet mixing chamber at the top and a vertical coaxial tube with diphasic jet at the bottom, forming a nozzle.
  • Said homogeneous liquid gas dispersion is produced for a gas retention of between 5 and 70%, preferably between 30 and 50%.
  • the invention relates more particularly to a method and a device for injecting ozone or a mixture of ozone and oxygen and / or air into a stream of water, to purify it.
  • the performance of the gas dispersion can be expressed on the one hand as a function of the size of the gas bubbles produced and on the other hand as a function of a gas / liquid volume ratio of the two-phase gas-liquid mixture resulting from the dispersion.
  • ratio related to the gas retention defined as the ratio of the volume of the gas phase relative to the total volume of the contactor equal to the sum of the volumes of gas and liquid that it contains or as the ratio of the volumetric flow rate of the gaseous phase reported the sum of the volume flow rates of gas and liquid.
  • the two-phase liquid gas contactors correspond to many industrial applications, such as liquid phase oxidation and hydrogenation or gas absorption by a liquid with or without a chemical reaction.
  • the gaseous and liquid phase contacting devices are designed to respond as efficiently as possible to the requirement to ensure the transfer of the quantities of material required, at the best cost, including furthermore notions related to the operation such as flexibility with regard to the quantities of material to be used, safety and stability of operation, speed of execution of the start-up and start-up steps, potential duration of operation (corrosion, maintenance, .... ).
  • the quantity of material exchanged within a two-phase apparatus denoted N
  • N the quantity of material exchanged within a two-phase apparatus
  • the liquid gas contactors are designed to offer the largest exchange surface compatible with hydrodynamic conditions relating to the circulating flow rates of the fluids and the physicochemical properties of the latter. It is also essential that the pressure drop on the gas side is as moderate as possible in order to avoid unacceptable energy expenditure or pressure conditions that are incompatible with the application conditions.
  • the contactors in which the gas is dispersed in the form of bubbles in a liquid cover the bubble column, mechanically stirred tank, perforated plate column, co-current tubular contactor such as static mixer, submerged jet ejector and venturi ejector. engine liquid ( M. Roustan, Gas-liquid transfers in water and waste gas treatment processes, Editions Lavoisier 2003 ; Pierre Trambouze, Chemical Reactors - Technology, J4020, Editions Techniques de l'Ingur, 1993 ). These different contactors are characterized by variable levels of fluid retention and interfacial area.
  • tubular contactors operating at co-current of gas and liquid offer the advantages of admitting a wider operating range both in gaseous dispersed phase retention (defined as the ratio of gaseous phase volume reported to the total volume of the contactor equal to the sum of the volumes of gas and liquid contained therein or as the ratio of the volume flow rate of the gaseous phase to the sum of the volume flow rates of gas and liquid) and to generate a very important interfacial area.
  • WO 2012025214 discloses a device and method for absorbing ozone in a tubular contactor for treating liquids in which the ozonated gas injection takes place in the circulating liquid stream by means of at least two static mixers spaced from contact zones .
  • WO 2013082132 relates to a method and apparatus for injecting a gas into a liquid, wherein a rotating helical helix located inside a suction tube immersed in the liquid creates a downward flow of liquid inside the tube suction nozzle fed by gas through nozzles arranged either above or below or along the helical helix.
  • the liquid is sucked into the suction tube at a superficial velocity greater than a terminal rate of rise of the gas bubbles, so as to allow undissolved gas bubbles to be entrained in the bulk of the liquid within the liquid that is sucked into the suction tube.
  • a transfer efficiency of 90% is obtained in the contactor for a gas retention of 5% in the tube of less than one meter in length.
  • EP 0 086 019 relates to a two-stage hybrid contactor combining a rain column and a bubble column for dissolving a gas in a liquid, preferably for the ozonation of water, in which the gas injection is carried out by means of a submerged tube.
  • a fraction of the liquid flow is used to inject the gas in the form of bubbles by means of a submerged tube which introduces the two-phase mixture into a downward flow of the main flow of liquid fed by runoff into the annular portion upper outer of the contactor.
  • This device thus involves a free space of significant volume runoff that promotes degassing so that the yield of dissolution of the gas is reduced. Gaseous retention in the injection tube is indicated as 13% maximum.
  • FR 2,762,232 also describes a method and a device for contacting ozone in liquids, in particular water, according to which a two-phase mixture of the partial flow of the liquid to be treated and a gas charged with ozone under pressure is formed in a downwardly co-current tube of gas and liquid optionally containing bubble shearing devices, all of which constitute part of an ozone absorption contactor in the U-shaped tube-shaped liquid as described in FR 2 545 732 .
  • the dispersion of the gas in the form of bubbles is obtained in the descending tube under the effect of the liquid velocity of about 1.5 m / s.
  • the height of the contactor is between 20 and 35 m. This type of contactor involves operating with a gas retention of less than 20% to control the two-phase water and gas mixture ( Degrémont, Memento Technique of water, Editions Lavoisier, 2005 ).
  • US6001247 still exposes a contactor composed of a diffusion compartment equipped with a submerged vertical tube cocurrent descending ozonated gas and water to uniformly introduce the gas.
  • the inside of the tube contains coaxial porous elements to distribute the ozonated gas in the form of bubbles in the water flowing through it.
  • the device comprises a radial inlet of the gas in the annular distributing chamber, from a gas pipe extending beyond the radial inlet for possible venting to the atmosphere.
  • venting is particularly advantageous, in particular because it improves the safety during the operation of such a device, in particular during a stop sequence of the device.
  • a sequence stopping it typically begins by evacuating the gas contained in the device by replacing it with outside air, through the extension, or vent pipe, of said gas pipe.
  • a vent valve is gradually opened so as to introduce outside air into the mixing chamber through this vent pipe, and then a gas inlet valve is closed so as to interrupt the arrival. of gas in the mixing chamber through said gas conduit.
  • the venting thus makes it possible to avoid any phenomenon of implosion of the device.
  • venting makes it possible to comply with such safety constraints, particularly when the device performs an injection of gas into a water level situated at a relatively low altitude relative to the altitude of the injection head. , that is to say when said downward vertical tube has a relatively long length before submersion, for example 10 meters.
  • venting also makes it possible to improve the flexibility of the device during a start-up sequence during which a liquid is injected into the mixing chamber via said inlet duct for the liquid to be treated.
  • the vent valve is opened, allowing at least a portion of the gas present in the mixing chamber to be evacuated. Venting also allows the gas supply to be closed until the desired hydraulic speed is achieved. The gas inlet is then opened and the vent valve is closed.
  • the cross section of the vertical tube is at least equal to the total surface of the holes of the plate, and at most equal to twice the same surface, and is preferably between 1.2 and 1.5 times the total surface of the orifices. of the plate.
  • the length of the descending tube may be between 1 and 30 meters, and is preferably between 1 and 15 meters.
  • the convergent of the mixing chamber may be frustoconical, the angle of inclination of the generatrices of the truncated cone relative to the axis being between 15 ° and 45 °.
  • the injection system which is the subject of the invention is a dispersion system with a hybrid liquid gas jet mixer and a jet injector.
  • Said system is composed of an injection head comprising a liquid-jet mixing chamber at the top and a vertical coaxial tube with diphasic jet at the bottom, forming a nozzle. Its function is to homogeneously disperse the gas in the form of fine bubbles in the engine liquid as a liquid gas contactor or for subsequent contact with the mass of liquid in a surrounding contactor.
  • Said liquid gas dispersion is produced for a gas retention of between 5 and 70%, preferably between 30 and 50%.
  • the injection head is designed to pre-mix the liquid and the gas upstream of the nozzle, the mixture being made homogeneous along the descent into the nozzle.
  • the gas and the liquid may be those involved in any operation requiring the formation of a liquid gas dispersion.
  • the injected gas will be selected from air, oxygen, ozone, carbon dioxide, these gases being injected alone or in mixtures.
  • the liquid will be aqueous including natural fresh or saline water, wastewater and more generally aqueous effluents, industrial process water in the industry including the drinking water production sector.
  • the injection head is fed by the liquid discharged by a pumping system and the gas from the distribution system is at a pressure equal to or greater than atmospheric pressure.
  • the injection head performs a premixing of the liquid and the gas under the effect of one to several turbulent streams of liquid emitted into the radially admitted gas stream.
  • the jets of liquid are produced by means of a liquid distribution member in the form of jets at high speed, typically between 4 and 10 m / s, preferably between 6 and 8 m / s.
  • the dispensing member is preferably an orifice distribution plate.
  • a mixing chamber located below the dispenser member has the shape of the section of the dispensing plate as an upper section.
  • the mixing chamber is tulip-shaped or frustoconical convergent or cylindrical or parallelepipedal.
  • the turbulence of the jets is demonstrated by Reynolds numbers greater than 10 5 .
  • the emission of the liquid jets produces an interfacial friction rate in the gas, which can thus reach more than 0.3 m / s, ie a speed greater than the terminal gas bubble speed of the order of 3 mm.
  • a liquid flow diagram shows the liquid flow lines and highlights the areas of liquid recirculation within the mixing chamber also filled with gas.
  • the high speed liquid jets thus shear the gas and suck up the produced gas pockets towards the down tube.
  • the liquid jets initiate the transfer of liquid gas material. Considering an average contact time of the liquid jets of 0.15 s, the transfer coefficient is of the order of 1.10 -4 m / s according to the nature of the gas.
  • the exchange potential is equal to the equilibrium concentration between the gas and the liquid.
  • the quantity The amount of carbon dioxide transferred is 0.3 kg / s.
  • the mixing chamber is followed downstream of a preferably cylindrical coaxial tube.
  • the section of the tube is at least equal to the total emission surface of the liquid jets in the mixing chamber and at most equal to twice the same surface.
  • the ratio of these surfaces is preferably between 1.2 and 1.5.
  • the dispersion device according to the invention makes the two-phase mixture homogeneous during the downward co-flow flow in the coaxial tube to the liquid distributor, as has been observed for a 40% gas retention. %.
  • the length of the down tube can reach 30 meters to promote the transfer of material inside the tube and possibly in the surrounding contactor whose height corresponds to the useful height of the dispersion system.
  • the height is preferably between 1 and 25 m.
  • a gas retention in the two-phase volume equal to 50% corresponds to the compact stack of the gas inclusions in the liquid. Therefore, the attainment of a homogeneous bubble size in the descending tube requires shearing again the volume of gas sucked under the effect of the turbulence of the mixture while the frequency of coalescence of the bubbles is all the more important than the gas retention is high.
  • the turbulence of the mixture is demonstrated by Reynolds number levels of the diphasic mixture greater than 10 4 .
  • This turbulence is maintained by applying a relative liquid velocity equal to the liquid velocity of the distribution jets in the mixing chamber for the best continuity of flow, ie typically between 4 and 10 m / s.
  • This velocity tends to decrease slightly during the descent under the effect of the compression of the gas under the effect of the column of liquid and under the effect of the transfer of material which takes place.
  • the regime is established in the area of bubble flow from the top of the tube. The quality of the mixture at the beginning of the descending tube determines the pressure required for the injected gas.
  • the pressure of the liquid gas mixture is a function of the outlet pressure of the nozzle (mainly a function of the immersion height), the pressure drops and the weight of the liquid column in the injection system (which can be considered as the static component). It turns out that an annular liquid film type flow regime such as that observed in the first meters of a tube equipped with a nozzle and without premixing of the gas and liquid operating with gaseous retention of 40% prevents the transmission of static pressure downwards.
  • the loss of liquid height is reflected directly by the need to increase the pressure of the gas injection.
  • the device of the invention allows on the contrary a regular transmission of the pressure because it provides a good quality of dispersion from the beginning of the descent into the tube.
  • the size of the bubbles produced is correlated with the dissipated energy itself, which is dependent on the local retention rates and on the physicochemical properties of the fluids composing the dispersion.
  • a dispersion of oxygen in water at 40% gas is characterized by bubbles of average diameter equal to 2.5 mm at the end of the tube 10 m in length.
  • the highly concentrated two-phase jet of dissolved gas produced at the outlet of the tube can then be dispersed in a surrounding contactor or relaxed towards the outlet of the reactor according to the contact time necessary for the absorption and possibly the reaction involved in the application.
  • the surrounding contactor may be any contactor known from the state of the art with a gas updraft.
  • the dispersing device D comprises two sets: an injection head H and a jet dispersion tube P, forming a nozzle.
  • the injection head H is the structure that connects the liquid and gas inlets, mixes these fluids and directs the resulting mixture into the down tube P.
  • the injection head H is connected to the inlet pipe 1 of liquid and comprises a compartment B with, in the lower part, a liquid distribution member, preferably a horizontal distribution plate 2 for the liquid, pierced with orifices. 2a.
  • the liquid flows vertically below the plate, following jets schematized by arrows A on Fig.2 .
  • An inlet pipe 4 of the gas to be injected is connected, by a radial box 4a, to an annular chamber 5 located under the plate 2, the lower periphery of which it surrounds.
  • a wall E limiting radially inwards the chamber 5 comprises nozzles or openings O of gas distribution in centripetal radial directions represented by arrows F on Fig.2 .
  • a mixing chamber 3 is located under the plate 2.
  • the mixing chamber 3 is preferably convergent tulip or frustoconical shape, but could be of cylindrical or parallelepipedal shape.
  • the inclination of the generatrices of the convergent with respect to the geometric axis is preferably between 15 ° and 45 °.
  • the chamber 3 provides the connection to the downward vertical tube P, preferably coaxial and cylindrical.
  • a venting system 6 for the start-up phase is provided at the end of the pipe 4 beyond the connection with the annular chamber 5.
  • a vent valve, not shown, is provided in the system 6, and a gas inlet valve not shown.
  • the jet dispersion tube P is hydraulically described as a straight vertical pipe length.
  • the operation of the device is as follows.
  • the device is capable of responding correctly to abrupt changes in conditions. , resulting, for example, from a power failure or any other event that could lead to an unscheduled shutdown.
  • This device makes it possible to ensure an eminently variable gaseous engagement of between 0.01 and 2 (if expressed in relation to gas and liquid flow rates), at the best cost under the effect of the necessary pressure reduction, to produce a homogeneous dispersion of gas in the liquid suitable for transferring the quantities of material required.
  • This device solves the disadvantages of the systems described in the state of the prior art and is also capable of replacing all or part of the gas injection and diffusion systems of the bubble column contactors, injection systems of gas and agitation of the agitated contactors.
  • the resulting contactors are much more efficient both technically and economically.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Accessories For Mixers (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)

Claims (13)

  1. Verfahren zur Dispersion von Gas in einem abwärts fließenden Flüssigkeitsstrom, bei welchem:
    - die Flüssigkeit als mindestens ein nach unten gerichteter Strahl (A), vorzugsweise als mehrere Strahlen, verteilt wird,
    - das Gas radial (F) in Richtung des Flüssigkeitsstrahls oder der - strahlen verteilt wird, um von der Flüssigkeit mitgenommen zu werden,
    - und die Flüssigkeit/Gas-Mischung in ein abwärts gerichtetes vertikales Strömungsrohr (P) geleitet wird,
    wobei das Verfahren mittels einer Vorrichtung durchgeführt wird, welche aufweist:
    - eine Einlassleitung (1) für die zu behandelnde Flüssigkeit;
    - im oberen Bereich, einen Einspritzkopf (H), der mit der Einlassleitung verbunden ist und eine Flüssigkeitsstrahl-Mischkammer (3) aufweist;
    - und im unteren Bereich, ein vertikales, vorzugsweise koaxiales Zweiphasenströmungsrohr (P),
    - wobei der Einspritzkopf (H) einen Raum (B) aufweist, der im unteren Bereich eine horizontale Flüssigkeitsverteilungsplatte (2) aufweist, welche von mindestens einer Öffnung (2a) durchsetzt ist, und eine ringförmige Verteilungskammer (5) aufweist, die unter der Platte (2) an deren Umfang vorgesehen ist, und mit einer Öffnung zur Gasverteilung in eine zentripetale radiale Richtung (F) versehen ist,
    - eine unterhalb der Platte befindliche Mischkammer (3),
    dadurch gekennzeichnet, dass die Mischkammer als Sammler für den Anschluss an das abwärts gerichtete vertikale Rohr (P) ausgebildet ist,
    und dass die Vorrichtung einen radialen Gaseinlass (4a) in die ringförmige Verteilungskammer (5) aufweist, welcher sich von einer Gasleitung (4) ausgehend über den radialen Einlass hinaus erstreckt (6), um eine Belüftung zu ermöglichen.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass das Gas unter einem Druck von weniger als 2 bar, vorzugsweise weniger als 1,5 bar verteilt wird.
  3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die Geschwindigkeit des Flüssigkeitsstrahls oder der -strahlen (A) zwischen 4 und 10 m/s, vorzugsweise zwischen 6 und 8 m/s beträgt.
  4. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass der Querschnitt des vertikalen Rohres (P) mindestens gleich der Gesamtemissionsfläche der Flüssigkeitsstrahlen (A) ist, und höchstens gleich dem 2-fachen dieser Fläche ist, wobei der genannte Querschnitt vorzugsweise zwischen dem 1,2- und dem 1,5-fachen der Gesamtemissionsfläche der Strahlen beträgt.
  5. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass:
    - die Flüssigkeit oberhalb der horizontalen Platte (2), die mehrere Öffnungen (2a) im Inneren einer Zone aufweist, gerichtet wird, um als ein oder mehrere Flüssigkeitsstrahlen abwärts zu strömen,
    - das Gas radial unterhalb und in Richtung des Inneren der Zone der Öffnungen für die Flüssigkeit verteilt wird,
    - die Flüssigkeit/Gas-Mischung entlang eines Abschnitts geleitet wird, der sich verjüngt, bis er das abwärts gerichtete vertikale Strömungsrohr (P) erneut erreicht.
  6. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Flüssigkeit/Gas-Mischung für mindestens 0,2 Sekunden in das abwärts gerichtete vertikale-Rohr (P) geleitet wird.
  7. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass das eingespritzte Gas unter Luft, Sauerstoff, Stickstoff und Kohlendioxid ausgewählt ist, wobei diese Gase allein oder in Mischungen eingespritzt werden.
  8. Verfahren nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Flüssigkeit wässrig ist, einschließlich natürliches Süß- oder Salzwasser, Brauchwasser und im Allgemeinen Abwässer, industrielles Prozesswasser, einschließlich des Sektors der Trinkwasserherstellung.
  9. Vorrichtung zum Einspritzen von Gas in eine Flüssigkeit, insbesondere zur Durchführung eines Verfahrens nach einem der vorhergehenden Ansprüche, die eine Einlassleitung (1) für die zu bearbeitende Flüssigkeit aufweist, mit:
    - im oberen Bereich, einem Einspritzkopf (H), der mit der Einlassleitung verbunden ist und eine Flüssigkeitsstrahl-Mischkammer (3) aufweist;
    - im unteren Bereich, einem vertikalen, vorzugsweise koaxialen Zweiphasenströmungsrohr (P),
    - wobei der Einspritzkopf (H) einen Raum (B) aufweist, der im unteren Bereich eine horizontale Flüssigkeitsverteilungsplatte (2) aufweist, welche von mindestens einer Öffnung (2a) durchsetzt ist, und eine ringförmige Verteilungskammer (5) aufweist, die unter der Platte (2) an deren Umfang vorgesehen ist, und mit einer Öffnung zur Gasverteilung in eine zentripetale radiale Richtung (F),
    - wobei die Mischkammer (3) unter der Platte angeordnet ist,
    dadurch gekennzeichnet, dass die Mischkammer als Sammler für den Anschluss an das abwärts gerichtete vertikale Rohr (P) ausgebildet ist,
    und dass die Vorrichtung einen radialen Gaseinlass (4a) in die ringförmige Ausgabekammer (5) aufweist, welcher sich von einer Gasleitung (4) ausgehend über den radialen Einlass hinaus erstreckt (6), um eine Belüftung zu ermöglichen.
  10. Vorrichtung nach Anspruch 9, dadurch gekennzeichnet, dass der Durchmesser der Öffnungen der Platte ausreicht, insbesondere mindestens gleich 10 mm ist, um eine Vorstopfung aufgrund von in der Flüssigkeit, insbesondere in Brauchwasser, enthaltenen Partikeln zu vermeiden.
  11. Vorrichtung nach Anspruch 9 oder 10, dadurch gekennzeichnet, dass der Querschnitt des vertikalen Rohres mindestens gleich der Gesamtfläche der Öffnungen (2a) der Platte ist, und höchstens gleich dem 2-fachen dieser Fläche ist, und dass er vorzugsweise zwischen dem 1,2- und dem 1,5-fachen der Gesamtfläche der Öffnungen (2a) der Platte ist.
  12. Vorrichtung nach einem der Ansprüche 9 bis 11, dadurch gekennzeichnet, dass die Länge des abwärts gerichteten Rohres (P) zwischen 1 und 25 Meter beträgt.
  13. Vorrichtung nach einem der Ansprüche 9 bis 12, dadurch gekennzeichnet, dass der Sammler der Mischkammer (3) kegelstumpfförmig ausgebildet ist, wobei der Neigungswinkel der Erzeugenden des Kegelstumpfs in Bezug auf die Achse zwischen 15° und 45° beträgt.
EP15714025.2A 2014-03-07 2015-03-09 Verfahren und vorrichtung zur dispersion von gas in einer flüssigkeit Active EP3113867B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1451870A FR3018206A1 (fr) 2014-03-07 2014-03-07 Procede et dispositif de dispersion de gaz dans un liquide
PCT/IB2015/051705 WO2015132773A1 (fr) 2014-03-07 2015-03-09 Procede et dispositif de dispersion de gaz dans un liquide

Publications (2)

Publication Number Publication Date
EP3113867A1 EP3113867A1 (de) 2017-01-11
EP3113867B1 true EP3113867B1 (de) 2018-01-03

Family

ID=51168034

Family Applications (1)

Application Number Title Priority Date Filing Date
EP15714025.2A Active EP3113867B1 (de) 2014-03-07 2015-03-09 Verfahren und vorrichtung zur dispersion von gas in einer flüssigkeit

Country Status (6)

Country Link
US (1) US10603643B2 (de)
EP (1) EP3113867B1 (de)
CA (1) CA2939691C (de)
ES (1) ES2663342T3 (de)
FR (1) FR3018206A1 (de)
WO (1) WO2015132773A1 (de)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3018206A1 (fr) * 2014-03-07 2015-09-11 Degremont Procede et dispositif de dispersion de gaz dans un liquide
US11219871B2 (en) * 2017-03-10 2022-01-11 Pronto Concepts Inc. Liquid diffusing filter

Family Cites Families (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US805653A (en) * 1902-03-10 1905-11-28 Leon P Lowe Apparatus for cleaning manufactured gases.
US2767127A (en) * 1950-10-30 1956-10-16 Gulf Oil Corp Particle transporting method and apparatus for use in the catalytic conversion of hydrocarbons
US3440018A (en) * 1966-03-11 1969-04-22 Us Stoneware Inc Chemical treating tower
JPS53116562A (en) * 1977-03-22 1978-10-12 Akoo Kk Powdery material mixing method and apparatus therefor
EP0086019B2 (de) 1982-02-09 1989-11-29 BBC Brown Boveri AG Vorrichtung zur Begasung einer Flüssigkeit und Verfahren zum Betrieb der Vorrichtung
US4498819A (en) * 1982-11-08 1985-02-12 Conoco Inc. Multipoint slurry injection junction
FR2545732B1 (fr) 1983-05-10 1989-10-27 Lyonnaise Eaux Eclairage Appareil pour la dissolution d'ozone dans un fluide
WO1992003219A1 (en) * 1990-08-27 1992-03-05 The University Of Newcastle Research Associates Limited Aeration apparatus with diffuser
US5462351A (en) * 1994-06-20 1995-10-31 Jenike & Johanson, Inc. Conditioning vessel for bulk solids
US6001247A (en) 1996-05-01 1999-12-14 Schulz; Christopher R. Removable, in-line diffuser apparatus for ozone disinfection of water
AUPO129096A0 (en) * 1996-07-26 1996-08-22 Boc Gases Australia Limited Oxygen dissolver for pipelines or pipe outlets
FR2762232B1 (fr) 1997-04-17 1999-05-28 Degremont Procede et dispositif pour la mise en contact de l'ozone dans des fluides a traiter, notamment de l'eau
US6007055A (en) * 1997-12-29 1999-12-28 Schifftner; Kenneth C. Gas and liquid contact apparatus
FR2776942B1 (fr) 1998-04-07 2000-05-05 Roger Botton Dispositif pour disperser un gaz dans un liquide en vue d'effectuer des reactions chimiques, biochimiques ou de simples echanges physiques avec ou sans particules en suspension
DE10250707B4 (de) * 2002-10-31 2010-08-12 Roland Damann Vorrichtung zur Lösung von Gas in Flüssigkeit
DE202006002983U1 (de) * 2006-02-24 2006-04-27 Damann, Roland Vorrichtung zum Durchführen von Wellness-Bädern oder therapeutischen Bädern
DE102010035519B3 (de) 2010-08-25 2011-12-08 Itt Mfg. Enterprises, Inc. Vorrichtung und Verfahren zur Behandlung von Flüssigkeiten mittels Ozon
US9486750B2 (en) 2011-12-01 2016-11-08 Praxair Technology, Inc. Gas injection method and apparatus
FR3018206A1 (fr) * 2014-03-07 2015-09-11 Degremont Procede et dispositif de dispersion de gaz dans un liquide
DE102017011074B3 (de) * 2017-11-30 2019-01-17 Palas Gmbh Partikel- Und Lasermesstechnik Verfahren und Vorrichtung zum Verdünnen eines Aerosols

Also Published As

Publication number Publication date
FR3018206A1 (fr) 2015-09-11
CA2939691C (fr) 2020-08-04
WO2015132773A1 (fr) 2015-09-11
US20160361692A1 (en) 2016-12-15
EP3113867A1 (de) 2017-01-11
ES2663342T3 (es) 2018-04-12
CA2939691A1 (fr) 2015-09-11
US10603643B2 (en) 2020-03-31

Similar Documents

Publication Publication Date Title
JP4725707B2 (ja) 旋回式微細気泡発生装置及び同気泡発生方法
JP3397154B2 (ja) 旋回式微細気泡発生装置
EP1866068B1 (de) Vorrichtung zum mischen und verteilen eines gases und einer flüssigkeit vor einer granulatschüttung
CA2231338A1 (fr) Dispositif de generation de mousse
WO1999033553A1 (fr) Generateur de fines bulles a turbulence
EP0459928B1 (de) Einrichtung zur einphasigen Behandlung von Flüssigkeitsströmen in einem Kontaktapparat sowie zugehöriger Rückführungsentgaser
EP3113867B1 (de) Verfahren und vorrichtung zur dispersion von gas in einer flüssigkeit
FR2905608A1 (fr) Procede et installation pour la mise en contact de l'ozone dans un flux de liquide,en particulier d'eau potable ou d'eau residuaire.
KR101125851B1 (ko) 나노버블 발생장치
JP2010155243A (ja) 旋回式微細気泡発生装置
FR2511031A1 (fr) Dispositif pour l'elaboration de milieux fluides de faible viscosite et de milieux tres visqueux, en particulier pour une fermentation de micro-organismes
WO2003084652A2 (fr) Procede et reacteur de mise en contact gaz/liquide par dispersion, et applications
EP3894060B1 (de) Vorrichtung zum einspritzen von flüssigkeit in eine flüssigkeit, verfahren zur reinigung dieser vorrichtung und abwasserbehandlungsanlage
KR20110108412A (ko) 가스 주입 장치 및/또는 배플을 갖는 하강류 혼합 장치
EP1343577A1 (de) Verfahren, modul und vorrichtung zum kontaktieren eines gases und einer flüssigkeit
JP7105446B2 (ja) 反応装置
EP2188215B1 (de) Verfahren zur flüssigkeits-/feststofftrennung in abwässern sowie dazugehörige trennvorrichtung
EP0577714B1 (de) Reaktor und Verfahren zum biologischen Reinigen von schadstoffhaltigen Flüssigkeiten
EP0122846B1 (de) Flüssigprodukt mit hohem Energieinhalt und dessen Verwendung bei der Speisung eines Reaktionsraumes mit brennbarem Material
FR2484862A1 (fr) Procede et dispositif pour le transfert de gaz dans un liquide applicable en particulier au traitement des eaux, en biotechnologie et dans l'industrie chimique
FR2825996A1 (fr) Systeme d'oxygenation d'un liquide a traiter transitant dans un bassin
FR2779660A1 (fr) Procede et installation pour le traitement d'un milieu reactionnel susceptible de provoquer un moussage expansif
CH396786A (fr) Procédé pour le traitement d'un milieu liquide par un mélange gazeux et appareil pour la mise en oeuvre de ce procédé
AU770174B2 (en) Swirling type micro-bubble generating system
EP1646444B1 (de) Ventilplatte zum verteilen einer gasförmigen phase und einer flüssigen phase

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20160810

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

AX Request for extension of the european patent

Extension state: BA ME

DAV Request for validation of the european patent (deleted)
DAX Request for extension of the european patent (deleted)
GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

INTG Intention to grant announced

Effective date: 20170721

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

Free format text: NOT ENGLISH

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

Ref country code: AT

Ref legal event code: REF

Ref document number: 959714

Country of ref document: AT

Kind code of ref document: T

Effective date: 20180115

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

Free format text: LANGUAGE OF EP DOCUMENT: FRENCH

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 602015007217

Country of ref document: DE

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 4

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2663342

Country of ref document: ES

Kind code of ref document: T3

Effective date: 20180412

REG Reference to a national code

Ref country code: NL

Ref legal event code: MP

Effective date: 20180103

REG Reference to a national code

Ref country code: LT

Ref legal event code: MG4D

REG Reference to a national code

Ref country code: AT

Ref legal event code: MK05

Ref document number: 959714

Country of ref document: AT

Kind code of ref document: T

Effective date: 20180103

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

Ref country code: NO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180403

Ref country code: HR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LV

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

Ref country code: PL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180404

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180403

Ref country code: IS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180503

Ref country code: RS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

Ref country code: AT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 602015007217

Country of ref document: DE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SM

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

Ref country code: MC

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

REG Reference to a national code

Ref country code: BE

Ref legal event code: MM

Effective date: 20180331

26N No opposition filed

Effective date: 20181005

REG Reference to a national code

Ref country code: IE

Ref legal event code: MM4A

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180309

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180309

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180331

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: TR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MK

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20180103

Ref country code: HU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO

Effective date: 20150309

Ref country code: RO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20180103

REG Reference to a national code

Ref country code: DE

Ref legal event code: R079

Ref document number: 602015007217

Country of ref document: DE

Free format text: PREVIOUS MAIN CLASS: B01F0003040000

Ipc: B01F0023200000

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20230327

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: IT

Payment date: 20230321

Year of fee payment: 9

P01 Opt-out of the competence of the unified patent court (upc) registered

Effective date: 20230601

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20230403

Year of fee payment: 9

Ref country code: CH

Payment date: 20230402

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20240327

Year of fee payment: 10

Ref country code: GB

Payment date: 20240327

Year of fee payment: 10