EP3934791A1 - Procédé et dispositif pour séparer un mélange gazeux renfermant du diborane et de l'hydrogène - Google Patents

Procédé et dispositif pour séparer un mélange gazeux renfermant du diborane et de l'hydrogène

Info

Publication number
EP3934791A1
EP3934791A1 EP20706647.3A EP20706647A EP3934791A1 EP 3934791 A1 EP3934791 A1 EP 3934791A1 EP 20706647 A EP20706647 A EP 20706647A EP 3934791 A1 EP3934791 A1 EP 3934791A1
Authority
EP
European Patent Office
Prior art keywords
heat exchanger
diborane
coolant
gas mixture
gas
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.)
Pending
Application number
EP20706647.3A
Other languages
German (de)
English (en)
Inventor
Friedhelm Herzog
Joachim Barbe
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.)
Messer SE and Co KGaA
Original Assignee
Messer SE and Co KGaA
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 Messer SE and Co KGaA filed Critical Messer SE and Co KGaA
Publication of EP3934791A1 publication Critical patent/EP3934791A1/fr
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/506—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification at low temperatures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
    • C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
    • C01B6/10—Monoborane; Diborane; Addition complexes thereof
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0204—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the feed stream
    • F25J3/0223—H2/CO mixtures, i.e. synthesis gas; Water gas or shifted synthesis gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0252—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of hydrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/16—Hydrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/90—Odorous compounds not provided for in groups B01D2257/00 - B01D2257/708

Definitions

  • the invention relates to a method for separating diborane from a diborane-hydrogen mixture, in which a diborane and hydrogen-containing mixture
  • diborane The separation of a gas mixture consisting of diborane and hydrogen is required, for example, as a process step in some synthesis processes for diborane.
  • One way of producing diborane is the acidolysis of sodium borohydride with methanesulfonic acid. The synthesis takes place according to the following chemical reaction:
  • the sodium borohydride is metered into concentrated methanesulfonic acid as fine granules.
  • the reaction takes place spontaneously, producing a gas mixture of diborane and hydrogen in a volume ratio of 1: 2 proportions.
  • Nitrogen with a temperature of -196 ° C are added.
  • the diborane freezes out in the cold atmosphere that forms inside the vessel.
  • the still gaseous hydrogen is then drawn off from the vessel by means of a vacuum pump.
  • the vessel is then heated to a temperature above the boiling point of diborane and the diborane is recondensed into smaller vessels, which in turn are cooled with liquid nitrogen.
  • the diborane is kept in these vessels in a cooling device at a temperature of approx. -20 ° C in order to counteract decomposition and the associated undesired formation of higher boranes.
  • a method for separating hydrogen from a gas mixture containing diborane and hydrogen by cooling a storage container to -196 ° C. is mentioned in DE 1 094 248 B, for example.
  • the invention is therefore based on the object of providing a continuously or almost continuously operable method for separating a diborane and
  • the diborane and hydrogen-containing gas mixture in the first heat exchanger comes into indirect thermal contact with a liquefied gas, which is kept at a pressure such that the diborane is liquefied by the thermal contact with the coolant without to freeze out.
  • the liquefied diborane is then discharged from the first heat exchanger and fed to a storage tank.
  • the temperature of the liquefied gas on the heat exchanger surfaces of the first heat exchanger is therefore kept at a value at which the diborane on the one hand does not freeze to ice on the heat exchanger surfaces and which on the other hand is below the dew point of the diborane present in the first heat exchanger, the value for the dew point in turn depends on the respective pressure in the first heat exchanger.
  • Methanesulfonic acid is restricted. Rather, the method according to the invention can be used in all processes in the course of which the task occurs of separating a gas mixture containing diborane and hydrogen. If further substances are present in the original mixture in addition to diborane and hydrogen, further separation stages may be required before and / or after the process described here in order to separate these substances.
  • a particularly advantageous embodiment of the invention provides for the remaining gas mixture of diborane and hydrogen to be fed to a second heat exchanger (hereinafter also referred to as "freezer") after passing through the first heat exchanger, in which the remaining gas mixture is fed to a second coolant that is temperature-controlled that any diborane still present in the gas mixture freezes out on the heat exchanger surfaces of the second heat exchanger.
  • a second heat exchanger hereinafter also referred to as "freezer”
  • Most of the diborane contained in the original gas mixture for example 95% or more, is already removed by condensation in the first heat exchanger.
  • the gas mixture is cooled even more deeply to a temperature below the freezing temperature of diborane, due to which most of the remaining diborane from the gas mixture freezes out on the heat exchanger surfaces of the second heat exchanger. Since only a small amount of diborane is left in the gas mixture when it enters the second heat exchanger, the resulting ice layer only grows slow and only requires defrosting of the heat exchanger surfaces at longer intervals.
  • Capacitor can be connected and is operated alternately with the first freezer, while the other freezer is being defrosted. Alternatively, continuous operation can be ensured in that the (single) freezer is briefly heated during operation, either by heating the gas mixture flowing into the freezer by means of a meat processor or by
  • Heat exchanger used coolant is removed.
  • it is liquid nitrogen.
  • this is kept at a lower pressure in the second heat exchanger than in the first heat exchanger and is therefore at a correspondingly lower temperature, namely at a temperature below the freezing point of the diborane in the second heat exchanger.
  • the coolant in the second heat exchanger must be at such a low temperature that diborane from the gas mixture freezes onto the heat exchanger surfaces in the second heat exchanger.
  • the diborane in the storage tank is also preferably kept at a temperature at which it condenses; it is particularly preferably kept at a temperature at which it remains in the liquid state.
  • a liquefied gas is also used, in particular the same liquefied gas as in the first and / or the second heat exchanger, in particular liquid nitrogen, which is kept at a corresponding pressure to control the temperature of the diborane in such a way that the temperature is sufficient to generate the diborane to keep in the liquid state.
  • the object of the invention is also achieved with a device for separating diborane from a diborane-hydrogen mixture, which is equipped with a first heat exchanger which has a feed and an outlet for a diborane and hydrogen-containing gas mixture and a coolant feed for a coolant used liquefied gas and a gas discharge line for discharging coolant evaporated on heat exchange surfaces of the first heat exchanger on heat contact with the gas mixture, and which is characterized in that the first heat exchanger is equipped with a discharge line for diborane which is liquefied during heat exchange with the coolant and which is equipped with a Storage container for storing the liquefied diborane is flow-connected, and the gas discharge of the first heat exchanger with a device for
  • diborane contained in the supplied gas mixture condenses on the heat exchanger surfaces by indirect heat exchange with the refrigerant to form liquid diborane.
  • the liquefied gas functioning as a refrigerant for example liquid nitrogen
  • a refrigerant for example liquid nitrogen
  • a corresponding regulation and control device is advantageously provided, which sets the pressure of the refrigerant in such a way that the diborane condenses in the first heat exchanger to form liquid diborane, but does not freeze out.
  • the remaining gas mixture consisting predominantly of hydrogen, is discharged from the first heat exchanger and can be fed to a further purification stage or some other use. The one to drain the liquid diborane from the first
  • the drainage used for the heat exchanger is geodetically directed downwards and allows the diborane to drain away under the effect of gravity. For example, it branches off from the discharge line for the gas mixture, which for this purpose likewise runs geodetically downwards, at least in a section between the condenser and the branching off of the discharge line for the liquid diborane.
  • An advantageous embodiment of the device according to the invention provides a second heat exchanger, which has a feed and a discharge line for a gas mixture consisting of diborane and hydrogen as well as a coolant feed line for a liquefied gas used as a coolant and a gas discharge line for discharging thermal contact with the gas mixture on heat exchanger surfaces of the second heat exchanger evaporated coolant from the second
  • Has heat exchanger wherein the outlet for the gas mixture of the first heat exchanger with the feed for the gas mixture of the second
  • the Heat exchanger and is cooled there in indirect thermal contact with a coolant on the heat exchanger surfaces to such an extent that diborane still contained in the gas mixture freezes out on the heat exchanger surfaces.
  • the The coolant supply to the second heat exchanger is equipped with a pressure reducer that reduces the pressure of the liquefied gas from the storage pressure in the
  • the first heat exchanger and / or the second heat exchanger is / are also preferably designed as tubular heat exchangers.
  • Outlet can be designed as a separate outlet, but a feed for the gas mixture that opens into the second heat exchanger from below can also be used in some sections as an outlet for the condensate, with an outlet connected to the storage tank branching off at a suitable point.
  • the coolant feed of the first heat exchanger and the coolant feed of the second heat exchanger are preferably connected to a source for a
  • Both coolants therefore preferably come from the same source, which is, for example, a standing tank in which the nitrogen is stored in liquefied form at a pressure that is so high that the nitrogen is present at a temperature that exceeds the freezing temperature of diborane, for example at a pressure of 14-20 bar.
  • the storage container is also expediently equipped with a cooling device in order to store the diborane in the storage container in condensed, i.e. liquid or solid, form.
  • a cooling device in order to store the diborane in the storage container in condensed, i.e. liquid or solid, form.
  • the storage container in a bath is off liquefied gas, such as liquid nitrogen, added.
  • the bath is preferably supplied from the same coolant source as the first and / or the second heat exchanger and is equipped with a device for maintaining a predetermined pressure which enables a predetermined pressure to be set
  • the storage container is also preferably provided with a separate filling line
  • Heating device is, for example, an electrical heating device or a heat exchanger, by means of which a warmer gas, for example air or gaseous nitrogen, which is at a temperature above the
  • Storage container can be brought into heat contract.
  • the discharge from the first heat exchanger is briefly blocked by means of a valve and the diborane in the storage container is heated so that it can be evaporated and discharged via the filling line.
  • An interruption of the gas separation in the first and / or second heat exchanger is not necessary during this.
  • the filling line can also be designed as a dip tube, or the filling line leads from the sump of the storage container.
  • the filling line leads from the sump of the storage container.
  • only a small proportion of diborane has to be evaporated in the storage tank in order to increase the pressure, and the diborane flows out of the storage tank, at least for the most part, in liquid form.
  • a liquid pump can of course also be used for this purpose.
  • the filling line is closed.
  • the diborane removed in liquid form from the storage container in this embodiment can then be fed in liquid form - or after evaporation - in gaseous form for filling.
  • Outlet for the gas mixture is equipped with a jet pump which is flow-connected on the drive side with the gas outlet of the first heat exchanger.
  • the increased pressure is the one from the first Heat exchanger outflowing gas, which was used there as a coolant, further used to in the discharge for the gas mixture of the first
  • Heat exchanger or the second heat exchanger to generate a negative pressure by means of which the gas mixture is withdrawn from the respective heat exchanger.
  • another gas under pressure can also be used for this purpose, for example evaporated coolant from the head space of a coolant storage container, for example a standing tank for liquid nitrogen.
  • the inventive method and the inventive device are for the separation of diborane-hydrogen gas mixtures in any
  • the invention is particularly effective at high proportions of, for example, more than 30% by volume of diborane in the im
  • Remaining gas mixture consisting predominantly of hydrogen.
  • FIG. 1 shows the circuit diagram of a device according to the invention.
  • the device 1 shown in FIG. 1 for separating diborane from a gas mixture containing diborane and hydrogen comprises a first heat exchanger, referred to below as a condenser 2, which has a feed 3 for the gas mixture.
  • a transition line 4 leads from the bottom of the condenser 2 to a second heat exchanger, here called freezer 5.
  • a gas discharge line 6, in which a suction pump 7 is arranged, leads from its headspace.
  • Condenser 2, freezer 5 and transition line 4 are equipped with walls that provide good thermal insulation.
  • Liquid discharge 8 which opens into a storage container 9. At least in its lower section it is equipped with walls with good thermal conductivity
  • Storage container 9 is received within a container 11 intended for a coolant bath.
  • the container 11 is pressure-resistant and closed and has walls that are thermally insulated towards the outside.
  • a coolant feed line 12 and a coolant outlet line 13 open into the container 11.
  • a filling line 14 leads out of the head space of the storage container 9 to a filling system, not shown here, in which, for example, mobile containers can be filled with diborane.
  • Condenser 2 and freezer 5 are designed as indirect heat exchangers and are equipped with heat exchanger surfaces 15, 16, each of which is, for example, tubes running parallel to one another or a cooling coil with walls that conduct heat well and are intended for the passage of a liquid or gaseous coolant / is.
  • heat exchanger surfaces 15, 16 are each connected to a coolant supply line 17, 18 which is connected to a
  • Coolant source in the exemplary embodiment with a nitrogen tank 19,
  • the heat exchanger surfaces 15 open on the outlet side
  • the gas discharge line 21 connected to the heat exchanger surface 15 of the condenser 2 is provided with a pressure holding valve 24 which maintains the pressure in the gas discharge line 21 at a predetermined or electronically transmitted pressure value.
  • the coolant supply line 12 leading into the container 11 is via a
  • Gas line 25 is connected to the head space 26 of the nitrogen tank 19. Likewise, the one opening out at the heat exchanger surface 6 of the freezer 5 is also
  • Coolant feed line 18 is connected to the head space 26 via a gas line 27 which opens into the gas line 25. Downstream of the branching off of the gas line 27, in the gas line 25 there is a heating device 29 for heating the gaseous
  • the coolant outlet line 13 is also equipped with a pressure holding valve 28, which holds the pressure in the container 11 at a predetermined or electronically transmitted pressure value.
  • valve V1 in the feed 1 a valve V2 in the
  • valve V5 in the coolant feed line 17 a valve V6 designed as a pressure reducer in the coolant feed line 18, a valve V 7 in the Coolant supply line 12, a valve V9 in the gas line 25, downstream of the branch of the gas line 27, and a valve V9 in the gas line 27. All valves V1 -V9 are designed as remotely controllable valves and can be switched from one not shown here
  • the pressure holding valve 24 in the gas discharge line 21 ensures that a higher pressure of over 13 bar is maintained in the heat exchanger surface 15 of the condenser 2.
  • the maximum level of the pressure value predetermined by the pressure holding valve 24 is determined in the exemplary embodiment according to FIG. 1 by the operating pressure in the nitrogen tank 19, which is 14 bar, for example.
  • Condenser 2 is at a higher temperature than that in the
  • Condenser exceeds, so at a temperature of over 108.3 K. Accordingly, the diborane, which is contained in the gas mixture supplied to the condenser 2, largely, for example 95-99%, condenses in the liquid state on the heat exchanger surface 15 and continues to flow over the
  • the gas mixture still containing a remainder of diborane flows out of the condenser 2 via the transition line 4 into the freezer 5.
  • the liquid nitrogen in the heat exchanger surface 16 of the freezer 5 is at a lower pressure than the liquid nitrogen in the heat exchanger surface 16 and has a temperature of, for example 77 K. This means that the temperature on the heat exchanger surface 16 is lower than the freezing temperature of diborane.
  • the diborane still contained in the gas mixture thus freezes on the surface of the heat exchanger surface 16 and forms a layer of ice there, which, however, grows only slowly due to the small amount of diborane still present in the gas mixture. That from the freezer 5 over the
  • Gas discharge line 6 withdrawn by means of the suction pump 7 gas mixture consists predominantly of gaseous hydrogen, which is then captured in a manner not shown here and fed or diverted for further use.
  • Liquid drain 8 for example an electrical meat device 30 is provided.
  • the gas mixture in the transition line 4 is heated slightly to a temperature above the dew point temperature of the diborane / Fl2 mixture at the outlet of the condenser 2, whereby the aerosols contained therein evaporate.
  • the diborane from the aerosols then condenses in the freezer 5 and is at least largely deposited in the form of ice on the heat exchanger surface 16.
  • the diborane present in the storage container 9 is cooled by a coolant bath present in the container 11 and thus kept in the liquid state.
  • the coolant bath consists of liquid nitrogen, which flows from the nitrogen tank 19 via the coolant feed line 12 into the container 11. After the heat exchange with the storage tank 9, the liquid nitrogen evaporates and escapes via the coolant outlet line 13, whereby it is in the coolant outlet line 13 by virtue of the arranged pressure holding valve 28 is kept at a pressure of over 13 bar.
  • the liquid nitrogen in the container 11 is at a temperature which is above the freezing point of diborane, for example at 108.5 K.
  • valves V3 and V7 are first closed and the valves V4 and V9 are opened. Gaseous nitrogen flows from the head space 26 of the nitrogen tank 19 into the container 11. To a required for evaporation of the diborane in the storage tank 9
  • the nitrogen in the gas line 25 is heated by means of the heating device 29.
  • the heating device 29 can also be arranged in the container 11 or directly in the storage container 9.
  • the diborane in the storage container 9 heats up, evaporates and is fed via the filling line 14 to a filling station (not shown here).
  • Transition line 4 has accumulated, flows into the storage container 9 after the valve V3 is reopened. The removal of the diborane from the
  • Storage container 9 is thus achieved without the separating process of the
  • Gas mixture in the device 1 would otherwise have to be interrupted.
  • the heat exchanger surface 16 is heated to a temperature above the melting temperature of diborane.
  • the ice lying on the heat exchanger surface 16 thus thaws, drips into the transition line 4 and flows over the
  • valve 8 is closed again and valves V1, V2 and V6 are opened, whereby device 1 is again used to separate the hydrogen diborane Gas mixture is available. Since the vast majority of the diborane originally contained in the gas mixture has already been separated off in the condenser 2, defrosting of the freezer 5 is only necessary at longer intervals of a few days or weeks (with otherwise continuous operation of the device 1). After defrosting, V6 is opened and V8 is closed. Because the defrosting was previously done with relatively cold gas, the new cold start takes place very quickly and with little need for liquid nitrogen.
  • Defrosting can also take place during operation, accepting a briefly slightly higher diborane emission.
  • V6 is closed and V8 is opened without the supply of the gas mixture to V1 being interrupted.
  • defrosting can take place alternatively or as a support by slightly warming the gas mixture in the transition line 4 by means of the heating device 30.
  • the device 1 can also be designed in such a way that a further freezer, essentially identical in construction to the freezer 5, is used, which is connected to the transition line 4 in alternation with the freezer 5, during the defrosts the other freezer. This allows the diborane recovery rate to be increased further and excessive diborane emissions during defrosting are avoided.
  • the suction pump 7 is a jet pump which is connected on the drive side to the gas discharge line 21 or the coolant discharge line 13.
  • the pressure of the nitrogen present there, for example about 13 bar, is sufficient to build up the negative pressure required to evacuate the hydrogen from the freezer 5.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • General Chemical & Material Sciences (AREA)
  • Filling Or Discharging Of Gas Storage Vessels (AREA)

Abstract

Pour séparer le diborane contenu dans un mélange gazeux renfermant du diborane et de l'hydrogène, un refroidissement du mélange gazeux est habituellement réalisé dans un contenant de stockage au moyen d'azote liquide, ce qui entraîne la séparation du diborane par congélation. L'objectif de cette invention est de pouvoir réaliser une séparation, qui soit continue dans une large mesure, du diborane contenu dans le mélange gazeux. À cet effet, dans un échangeur de chaleur, le mélange gazeux est mis en contact thermique avec un gaz liquéfié dont la pression est maintenue de manière que le diborane soit liquéfié par contact thermique avec l'agent réfrigérant, le diborane liquéfié étant ensuite évacué du premier échangeur de chaleur et introduit dans un contenant de stockage. Dans un deuxième échangeur de chaleur monté en aval, le diborane resté dans le mélange gazeux peut ensuite subir un processus de séparation par congélation.
EP20706647.3A 2019-03-02 2020-02-13 Procédé et dispositif pour séparer un mélange gazeux renfermant du diborane et de l'hydrogène Pending EP3934791A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102019001497.9A DE102019001497B3 (de) 2019-03-02 2019-03-02 Verfahren und Vorrichtung zum Trennen eines Diboran und Wasserstoff enthaltenden Gasgemisches
PCT/EP2020/053702 WO2020177998A1 (fr) 2019-03-02 2020-02-13 Procédé et dispositif pour séparer un mélange gazeux renfermant du diborane et de l'hydrogène

Publications (1)

Publication Number Publication Date
EP3934791A1 true EP3934791A1 (fr) 2022-01-12

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EP20706647.3A Pending EP3934791A1 (fr) 2019-03-02 2020-02-13 Procédé et dispositif pour séparer un mélange gazeux renfermant du diborane et de l'hydrogène

Country Status (6)

Country Link
US (1) US20220144633A1 (fr)
EP (1) EP3934791A1 (fr)
KR (1) KR20220002276A (fr)
CN (1) CN113518656B (fr)
DE (1) DE102019001497B3 (fr)
WO (1) WO2020177998A1 (fr)

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CN114593560A (zh) * 2022-03-11 2022-06-07 苏州金宏气体股份有限公司 脱除no中no2、n2o的纯化装置及纯化方法

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DE102017006910A1 (de) * 2017-07-20 2019-01-24 Linde Aktiengesellschaft Vorrichtung zur Zerlegung des Produktstroms einer Alkan-Dehydrierung

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DE102019001497B3 (de) 2020-03-05
US20220144633A1 (en) 2022-05-12
CN113518656B (zh) 2024-02-23
KR20220002276A (ko) 2022-01-06
WO2020177998A1 (fr) 2020-09-10
CN113518656A (zh) 2021-10-19

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