EP3538626A1 - Nouveau dispositif de separation gaz liquide pour equiper les reacteurs en lit fluidise triphasique tels que ceux utilises dans le procede h-oil - Google Patents
Nouveau dispositif de separation gaz liquide pour equiper les reacteurs en lit fluidise triphasique tels que ceux utilises dans le procede h-oilInfo
- Publication number
- EP3538626A1 EP3538626A1 EP17791104.7A EP17791104A EP3538626A1 EP 3538626 A1 EP3538626 A1 EP 3538626A1 EP 17791104 A EP17791104 A EP 17791104A EP 3538626 A1 EP3538626 A1 EP 3538626A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- liquid
- gas
- zone
- separation device
- diameter
- 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.)
- Withdrawn
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/0042—Degasification of liquids modifying the liquid flow
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/0042—Degasification of liquids modifying the liquid flow
- B01D19/0052—Degasification of liquids modifying the liquid flow in rotating vessels, vessels containing movable parts or in which centrifugal movement is caused
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
- B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G49/00—Treatment of hydrocarbon oils, in the presence of hydrogen or hydrogen-generating compounds, not provided for in a single one of groups C10G45/02, C10G45/32, C10G45/44, C10G45/58 or C10G47/00
- C10G49/22—Separation of effluents
Definitions
- the invention is part of the improvement of the design of the upper part of the solid liquid gas reactors used in the H-Oil process in order to obtain a better gas / liquid separation in said upper zone often called "recycle cup".
- the Anglo-Saxon terminology of "recycle cup” will be translated in this text by the phrase “liquid recycling zone” or simply recycling zone.
- the Anglo-Saxon term “spiral riser” will be translated in this text by the phrase gas / liquid separation device.
- the H-Oil process is a process for the hydroconversion of heavy hydrocarbon fractions, of the vacuum gas oil type or residues, which thus brings into contact the liquid hydrocarbon phase, the hydrogen gas phase dispersed in the form of bubbles, and the catalyst itself. even dispersed in the form of particles of a size typically between 0.2 and 2 millimeters.
- the H-Oil process is therefore a three-phase fluidized process that uses a specific reactor, said reactor being equipped with a liquid gas separation device located in the upper part of the reactor so as to allow the recycling of the liquid which is returned after separation into the reactor. the reaction zone of the reactor.
- liquid recycling rate defined as the ratio of the recycled liquid flow rate to the incoming liquid feed rate, which is generally in the range of 1 to 10.
- the present invention can be defined as an improved liquid gas separation device for H-Oil reactors which allows the reintroduction of the majority of the liquid without gas to the reaction zone, and the evacuation of the gas (which may still contain a minority of liquid) out of the reactor.
- the present device achieves greater gas / liquid separation efficiencies than the "riser spiral" of the prior art.
- Figure 1 shows a diagram of a three-phase fluidized bed reactor used in the H-Oil process.
- This figure makes it possible to visualize the reaction zone (22) corresponding to the three-phase fluidized bed containing the catalyst, the zone situated above the catalytic zone called the liquid gas separation zone (29) which allows the liquid to be recycled to the lower part of the reactor by means of the recycling pump (20).
- the solid gas separation devices are represented by the elements (27) and (28), some elements having their lower end located in the zone (29), and other elements having their lower end located on the conical surface of the "Recycle cup” (39). It is these separation elements which are the subject of the present invention, the rest of the reactor not being modified with respect to the prior art.
- FIG. 2 represents a more detailed schematic view of the upper part of the reactor called liquid recycling zone since it ends with an internal conduit (25) which, after gas / liquid separation, brings the liquid back to the lower part of the reactor via the recycling pump (20).
- the liquid gas separation devices are located along the conical surface (30) of the recycling zone. The entry of the gas / liquid mixture is via the ducts (75). The gas / liquid separation takes place in the devices (42).
- Each separating device (42) is capped by an upper cap (50) comprising an upper end (55) for evacuation of the gas, and a lower duct (70) forming an annular space around the intake duct (75) .
- the liquid is recovered by the downward outlet pipes along the arrow (45), and the gas is discharged through the upper duct (55).
- the gas leaves the reactor through the outlet duct in the direction of the boom (67).
- Figure 3 supports the information for sizing separation devices according to the invention (27) and (28). Note in particular the angles alpha and beta, and the gamma angle of the helical spiral (42) with the horizontal.
- Figure 4 is a visualization of the efficiency of liquid gas separation resulting from a 3D simulation performed using Fluent TM software. EXAMINATION OF THE PRIOR ART
- recycle cup corresponds to the upper part of the reactor which, after separation of the gas and the liquid, allows the return of the liquid to the reaction zone of the reactor, and the evacuation of the gas via a dedicated pipe.
- zone of recycling we will use in the rest of the text the terminology upper zone of recycling of the liquid or more simply, zone of recycling, for "recycle cup”.
- the present invention can be defined as a liquid gas separation device implanted in the recycling zone of three-phase fluidized reactors used in the hydroconversion processes of heavy hydrocarbon cuts in the presence of hydrogen under high pressure, a process which we will call a type process. H-Oil.
- the present device can be used in any type of triphasic fluidized bed reactor requiring a liquid gas separation.
- a three-phase fluidized bed process is understood to mean a process in which three phases are present in the reaction zone; a liquid phase, generally constituting the charge to be treated, a gas phase under high pressure generally of hydrogen, and a solid phase corresponding to the catalyst divided into solid particles, most often of a diameter of between 0.2 and 2 mm and preferably between 0.7 and 1.5 mm.
- particle diameter indications do not constitute a limitation of the present invention since it relates to the separation of gas and liquid, the solid phase being upstream of the gas-liquid separation zone.
- the separation device consists of a plurality of separating elements (27) and (28) operating in parallel and vertically implanted from the conical surface (30) of the recycling zone (39).
- the recycling zone (39) decomposes into an upper part (39 v) corresponding to the gas, and a lower part (39 I) corresponding to the liquid. These two zones are, during operation, separated by a liquid gas interface (24).
- Each separating element (27) and (28) is equipped with a helical spiral (42) located in the upper part of the intake duct (75) bringing the liquid gas mixture from the zone (29) into each of said elements separation (27) and (28).
- Each separating element (27) and (28) is capped with an upper cap (50) which comprises at its upper end a gas evacuation pipe (53), and at its lower end a vertical pipe (70) substantially concentric to the inlet duct (75) allowing the return of the separated liquid to the reaction zone by the general return duct (25).
- Each separating element (27) and (28) therefore consists of the intake duct (75), the upper cap (50), the liquid return duct (70), and a conical transition zone (47). ) connecting the upper cap (50) to the liquid return line (70).
- the upper part of each separating element (27) and (28) is situated above the liquid gas interface (24). This liquid gas interface (24) is established during operation substantially at the slots (65) fitted to the lower part of the gas discharge pipe (40).
- the annular zone between the intake duct (75) and the vertical liquid return duct (70) contains the recycled liquid to a certain level noted (25) in FIG. 3. This liquid level (25) must remain separate from the liquid gas interface (24).
- the diameter of the intake duct (75) is generally between 0.02 m and 0.5 m, preferably between 0.05 m and 0.4 m, and more preferably between 0.1 m and 0 , 3 m.
- the liquid gas separation device according to the present invention contains inside each separating element (27) and (28) a helical spiral (42) forming an angle ⁇ with the horizontal between 10 ° and 80 ° of meadow. between 20 ° and 70 ° and preferably between 35 ° and 60 °.
- the helical spiral (42) contained in each separating element (27) and (28) performs a number of rotations between 0.5 and 4, each rotation corresponding to 1 complete revolution (360 preferably between 0.5 and 2 turns when passing from the lower part to the upper part of each separating element.
- the ratio of the diameter of the upper cap (50) which covers the intake duct (75) in its upper part, to the diameter of said intake duct (75) is generally between 1 and 6, preferably between 1, 5 and 5, and preferably between 2 and 4.
- the ratio of the diameter of the gas discharge pipe (55) at the upper end of the separating members (27) and (28) to the diameter of said separating element (75) is generally between 0.3 and 5, preferably between 0.5 and 4, and preferably between 0.6 and 3.
- the height H1 defined as the distance separating the upper end of the spirals (42), the gas outlet (55) of the separation elements (27) and (28) taken at its lower end, has a ratio H1 / diameter of the elements of separation (27) and (28) between 0.5 and 6, preferably between 0.7 and 5, and preferably between 1 and 4.
- the angle a of the gas outlet duct (55) with respect to the vertical is generally between 0 ° and 135 °, preferably between 10 ° and 120 ° and preferably between 30 ° and 90 °.
- the ratio of the diameter of the lower duct (70) returning the liquid after separation to the recycle line (31), to the diameter of the intake duct (75) is generally between 1 and 5, preferably between 1, 1 and 4, and more preferably between 1, 5 and 3.
- the length of the liquid return conduit (70) must be greater than the distance between the interfaces (24) and (25) to create a "plug" of liquid in said conduit (70), to prevent the gas from descending to the liquid zone 39L.
- the conical part (47) which connects the upper cap (50) to the lower part (70), which cover the separating elements (27) and (28) has an angle ⁇ relative to the vertical generally between 90 ° and 270 ° preferably between 100 ° and 200 ° and preferably between 120 ° and 150 °.
- the liquid gas separation device according to the invention generally has a density of the separation elements (27) and (28) of between 5 and 70 units per m2 of empty barrel reactor surface.
- the present invention can also be defined as a process for hydroconversion of heavy hydrocarbon cuts in three-phase fluidized bed using the liquid gas separation device according to the characteristics given above, said method operating under the following operating conditions:
- the superficial velocity of the upward flow taken inside each intake duct (75) is generally between 0.1 and 20 m / s, preferably between 0.2 and 15 m / s, and more preferably between 0.3 and 10 m / s.
- FIG. 1 is a representative diagram showing the main elements of an H-Oil reactor according to the prior art.
- This reactor is specifically designed with suitable materials to process reactive liquids, liquid-solid slurry, (ie liquids containing fine solid particles dispersed therein), solids and gases at high temperature and pressure with a preferred application for the treatment of liquid hydrocarbon cuts with hydrogen at high temperature and high pressure, i.e.
- the H-Oil type reactor (10) is designed with a suitable inlet duct (12) for the injection of a heavy hydrocarbon feed ( 1 1) and a gas (13) containing hydrogen.
- the outlet ducts are positioned in the upper part of the reactor (10).
- the outlet duct (40) is designed to draw off vapors that may contain a certain amount of liquid, and optionally the duct (24) allows mainly liquid to be withdrawn.
- the reactor also contains a system for introducing and withdrawing catalyst particles schematically shown by the conduit (15) for introducing the fresh catalyst (16), and the conduit (17) for withdrawing the spent catalyst (14). ).
- the heavy hydrocarbon feed is introduced through the conduit (1 1), while the hydrogen-containing gas is introduced through the conduit (13).
- the feed mixture and hydrogen gas is then introduced into the reactor (10) through the conduit (12) in the lower part of the reactor.
- Incoming fluids pass through a tray (18) containing suitable dispensers.
- "bubble cap” type distributors (19) are shown, but it is understood that any distributor known to those skilled in the art to distribute the fluids from the conduit (12) over the entire surface of the reactor 10 , and this in the most homogeneous way possible, can be used.
- the liquid / gas mixture flows upwards and the catalyst particles are entrained in a bubbling bed motion by the gas flow and the liquid flow induced by the recirculation pump (20) which may be internal or external to the reactor (10).
- the upward flow of liquid delivered by the pump (20) is sufficient for the mass of catalyst in the reaction zone or catalytic bed (22) to expand by at least 10%, preferably from 20% to 100% by relative to the static (i.e., at rest) volume of the catalyst bed, thereby allowing the flow of gas and liquid through the reactor (10), as shown by the direction arrows (21).
- the bed of catalyst particles reaches a high level of expansion while the liquid and the lighter gas continues to travel up the reactor (10) beyond this solid level.
- the maximum expansion level of the catalyst corresponds to the interface (23).
- the catalytic reaction zone (22) which extends from the grid (18) to the level (23).
- the interface (23) is a zone (39) containing only gas and liquid.
- the catalyst particles in the reaction zone (22) are in random movement in the fluidized state, which is why the reaction zone (22) is called a three-phase fluidized zone.
- the zone (29) with low catalyst concentration above level (23) is filled with liquid and entrained gas.
- the gas is separated from the liquid in the upper portion of the so-called "recycle cup” (30) to collect and recycle most of the liquid through the central conduit (25). It is important that the recycled liquid through the central pipe (25) contain as little gas as possible, or no gas at all, to avoid cavitation of the pump (20).
- the liquid products remaining after the liquid gas separation can be withdrawn through the conduit (24).
- the conduit (40) is used for gas withdrawal.
- the enlarged portion at the upper end of the conduit (25) forms the 39V and 39L liquid recycle zone.
- a plurality of vertically oriented separating elements (27) and (28) creates the link between the liquid gas zone ( 29) and the recycling zone (39).
- the liquid gas mixture flows upwardly through the conduits of the separating members (27) and (28).
- a portion of the separated liquid is then directed to the recycle pump (20) in the direction of the boom (31) through the central conduit (25), and is thus recycled to the lower portion of the reactor (10) below. of the grid (18).
- the gas separated from the liquid flows to the upper part of the reactor (10) and is withdrawn through the upper conduit (40).
- the withdrawn gas is then treated in a conventional manner to recover as much hydrogen as possible so that the latter is recycled to the reactor through the conduit (13).
- the general organization of the flow of fluids is not modified in the present invention with respect to the prior art as just described. Only are modified the geometry of the separating elements (27) and (28) and the dimensioning of the recycling zone (39).
- FIG 2 is a more specific diagram of the recycling zone (39) shown in Figure 1.
- the gas and the liquid have an upward flow shown by the direction arrow (41) and are introduced through the intake ducts (75) where they come into contact with a helical spiral (42) contained within each ducts (75) which induces a tangential velocity to the two fluids.
- the helical coil (42) causes a centrifugal separation where the liquid which has a higher density than the gas is plated on the inner wall of the cap (50), while the gas (53) is directed through the conduit (55). ) to a gas phase zone (39 v) delimited by the liquid level (24).
- the level (24) separates the upper part (39 V) mainly containing the gas separated from the lower part (39L) mainly containing the recycled liquid.
- the different separated liquids (45) from the different separating elements (27) and (28) flow downwards through the conical wall (30), and are collected by the central recycling duct (25). to be taken up by the recycling pump (20).
- the duct (40) generally has slots (65) at its lower end which allow the height of the liquid-gas interface (24) to be fixed.
- Figure 3 shows the design of a liquid gas separation device according to the invention in more detail, and shows the geometric dimensions important for the dimensioning of said device.
- the diameter of the intake duct (75) of each separating element (27) and (28) is generally between 0.02 m and 0.5 m, preferably between 0.05 m and 0.4 m, and preferred between 0.1 m and 0.3 m.
- the superficial liquid velocity of the upward flow represented by the direction arrow (41) is generally between 0.1 and 20 m / s, preferably between 0.2 m / s and 15 m / s, and so preferred between 0.3 m / s and 10 m / s.
- the helical spiral (42) forms an angle ⁇ with the horizontal between 10 ° and 80 °, preferably between 20 ° and 70 ° and preferably between 35 ° and 60 °.
- the spiral rotates between 0.5 and 4 full turns (one full turn equals one rotation of 360 e ), preferably between 0.5 and 2 complete turns, when passing from its lower end to its upper end.
- the ratio of the diameter of the upper cap (50) to the diameter of the intake duct (75) is generally between 1 and 6, preferably between 1.5 and 5, and preferably between 2 and 4.
- the ratio of the diameter of the gas discharge duct (55) to the diameter of the intake duct (75) is generally between 0.3 and 5, preferably between 0.5 and 4, and preferably between 0 and 4. , 6 and 3.
- the height H1 is defined as the distance separating the upper end of the helical spirals (42) from the lower end of the gas discharge ducts (55).
- the ratio of the length H1 to the diameter of the intake duct (75) is generally between 0.5 and 6, preferably between 0.7 and 5, and preferably between 1 and 4.
- the angle ⁇ of the gas outlet duct (55) with respect to the vertical is generally between 0 ° and 135 °, preferably between 10 ° and 120 ° and preferably between 30 ° and 90 °.
- the ratio of the diameter of the lower duct (70) surrounding the intake duct (75) to the diameter of said intake duct (75) is generally between 1 and 5, preferably between 1, 1 and 4, and preferably preferred between 1, 5 and 3.
- the conical transition (47) which connects the upper cap (50) to the lower part (70) of the separating elements (27) and (28) has an angle ⁇ relative to the vertical generally between 90 ° and 270 ° Preferably between 100 ° and 200 ° and preferably between 120 ° and 150 °.
- Equations 1 and 2 The gas and liquid separation efficiencies are defined by Equations 1 and 2 below.
- a 3D CFD simulation of the invention was performed using the Fluent software An Eulerian approach is used for each phase (liquid and gas) with a resolution of conservation equations of mass and momentum.
- FIG. 4 shows the liquid volume fraction in the separation device according to the invention in gray variation. The higher the shade of gray, the higher the concentration in the liquid phase. It can be seen that the device according to the invention achieves an almost perfect separation of the gas and the liquid which is found along the wall (50) in downward flow. The gas fraction is found in the outlet pipe (53).
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR1660835A FR3058421B1 (fr) | 2016-11-09 | 2016-11-09 | Nouveau dispositif de separation gaz liquide pour equiper les reacteurs en lit fluidise triphasique tels que ceux utilises dans le procede h-oil |
PCT/EP2017/077848 WO2018086958A1 (fr) | 2016-11-09 | 2017-10-31 | Nouveau dispositif de separation gaz liquide pour equiper les reacteurs en lit fluidise triphasique tels que ceux utilises dans le procede h-oil |
Publications (1)
Publication Number | Publication Date |
---|---|
EP3538626A1 true EP3538626A1 (fr) | 2019-09-18 |
Family
ID=58009967
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP17791104.7A Withdrawn EP3538626A1 (fr) | 2016-11-09 | 2017-10-31 | Nouveau dispositif de separation gaz liquide pour equiper les reacteurs en lit fluidise triphasique tels que ceux utilises dans le procede h-oil |
Country Status (6)
Country | Link |
---|---|
US (1) | US20190321753A1 (fr) |
EP (1) | EP3538626A1 (fr) |
CN (1) | CN110139918A (fr) |
FR (1) | FR3058421B1 (fr) |
RU (1) | RU2019117610A (fr) |
WO (1) | WO2018086958A1 (fr) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR3094984A1 (fr) | 2019-04-12 | 2020-10-16 | IFP Energies Nouvelles | Reacteur triphasique avec coupelle de recycle de section decroissante et d’angle d’inclinaison variable |
FR3094983B1 (fr) | 2019-04-12 | 2024-01-19 | Ifp Energies Now | Reacteur triphasique avec coupelle de recycle tronconique a fort angle d’inclinaison |
CN113011114A (zh) * | 2021-03-25 | 2021-06-22 | 赣江新区澳博颗粒科技研究院有限公司 | 一种优化液-固水力旋流器分离性能的数值仿真方法 |
FR3130832A1 (fr) * | 2021-12-20 | 2023-06-23 | IFP Energies Nouvelles | Dispositif de séparation gaz-liquide avec une zone d’accompagnement du liquide en sortie, notamment pour réacteur en lit fluidisé triphasique |
US20240157274A1 (en) * | 2022-11-16 | 2024-05-16 | Chevron U.S.A. Inc. | Gas-liquid separation device for an ebullated bed reactor |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4886644A (en) | 1987-12-02 | 1989-12-12 | Texaco Inc. | Liquid degaser in an ebullated bed process |
US5066467A (en) * | 1990-10-05 | 1991-11-19 | Texaco Inc. | Liquid degasser in an ebullated bed process |
FR2826876B1 (fr) * | 2001-07-06 | 2003-09-26 | Inst Francais Du Petrole | Dispositif interne de separation d'un melange comprenant au moins une phase gazeuse et une phase liquide |
CN103769010B (zh) * | 2012-10-19 | 2016-01-20 | 中国石油化工股份有限公司 | 一种沸腾床反应器 |
CN104549065B (zh) * | 2013-10-28 | 2017-09-22 | 中国石油化工股份有限公司 | 一种浆态床环流反应器及应用和一种生产过氧化氢的方法 |
-
2016
- 2016-11-09 FR FR1660835A patent/FR3058421B1/fr not_active Expired - Fee Related
-
2017
- 2017-10-31 RU RU2019117610A patent/RU2019117610A/ru not_active Application Discontinuation
- 2017-10-31 EP EP17791104.7A patent/EP3538626A1/fr not_active Withdrawn
- 2017-10-31 US US16/348,745 patent/US20190321753A1/en not_active Abandoned
- 2017-10-31 WO PCT/EP2017/077848 patent/WO2018086958A1/fr unknown
- 2017-10-31 CN CN201780069393.3A patent/CN110139918A/zh active Pending
Also Published As
Publication number | Publication date |
---|---|
RU2019117610A (ru) | 2020-12-10 |
FR3058421A1 (fr) | 2018-05-11 |
CN110139918A (zh) | 2019-08-16 |
FR3058421B1 (fr) | 2020-07-24 |
WO2018086958A1 (fr) | 2018-05-17 |
US20190321753A1 (en) | 2019-10-24 |
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