EP4453488B1 - Vorrichtung und verfahren zur verflüssigung eines gases - Google Patents

Vorrichtung und verfahren zur verflüssigung eines gases

Info

Publication number
EP4453488B1
EP4453488B1 EP22840192.3A EP22840192A EP4453488B1 EP 4453488 B1 EP4453488 B1 EP 4453488B1 EP 22840192 A EP22840192 A EP 22840192A EP 4453488 B1 EP4453488 B1 EP 4453488B1
Authority
EP
European Patent Office
Prior art keywords
refrigerant
dihydrogen
circuit
gas
closed
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
EP22840192.3A
Other languages
English (en)
French (fr)
Other versions
EP4453488C0 (de
EP4453488A1 (de
Inventor
Rémi LINOTTE
Florian JALIA
Hamza FILALI
Davide DURI
Loïc PENIN
Pierre CHABERNAUD
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.)
ArianeGroup SAS
Engie SA
Original Assignee
ArianeGroup SAS
Engie SA
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 ArianeGroup SAS, Engie SA filed Critical ArianeGroup SAS
Publication of EP4453488A1 publication Critical patent/EP4453488A1/de
Application granted granted Critical
Publication of EP4453488C0 publication Critical patent/EP4453488C0/de
Publication of EP4453488B1 publication Critical patent/EP4453488B1/de
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/0002—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the fluid to be liquefied
    • F25J1/0005—Light or noble gases
    • F25J1/001—Hydrogen
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0047—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using an "external" refrigerant stream in a closed vapor compression cycle
    • F25J1/005—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using an "external" refrigerant stream in a closed vapor compression cycle by expansion of a gaseous refrigerant stream with extraction of work
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0047—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using an "external" refrigerant stream in a closed vapor compression cycle
    • F25J1/0052—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using an "external" refrigerant stream in a closed vapor compression cycle by vaporising a liquid refrigerant stream
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/006—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the refrigerant fluid used
    • F25J1/0062—Light or noble gases, mixtures thereof
    • F25J1/0067—Hydrogen
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/006—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the refrigerant fluid used
    • F25J1/007—Primary atmospheric gases, mixtures thereof
    • F25J1/0072—Nitrogen
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0203—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a single-component refrigerant [SCR] fluid in a closed vapor compression cycle
    • F25J1/0204—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a single-component refrigerant [SCR] fluid in a closed vapor compression cycle as a single flow SCR cycle
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0203—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a single-component refrigerant [SCR] fluid in a closed vapor compression cycle
    • F25J1/0205—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a single-component refrigerant [SCR] fluid in a closed vapor compression cycle as a dual level SCR refrigeration cascade
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0221—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using the cold stored in an external cryogenic component in an open refrigeration loop
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
    • F25J1/0244—Operation; Control and regulation; Instrumentation
    • F25J1/0245—Different modes, i.e. 'runs', of operation; Process control
    • F25J1/0249—Controlling refrigerant inventory, i.e. composition or quantity
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
    • F25J1/0244—Operation; Control and regulation; Instrumentation
    • F25J1/0245—Different modes, i.e. 'runs', of operation; Process control
    • F25J1/0249—Controlling refrigerant inventory, i.e. composition or quantity
    • F25J1/025—Details related to the refrigerant production or treatment, e.g. make-up supply from feed gas itself
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
    • F25J1/0257—Construction and layout of liquefaction equipments, e.g. valves, machines
    • F25J1/0262—Details of the cold heat exchange system
    • F25J1/0264—Arrangement of heat exchanger cores in parallel with different functions, e.g. different cooling streams
    • F25J1/0265—Arrangement of heat exchanger cores in parallel with different functions, e.g. different cooling streams comprising cores associated exclusively with the cooling of a refrigerant stream, e.g. for auto-refrigeration or economizer
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
    • F25J1/0279—Compression of refrigerant or internal recycle fluid, e.g. kind of compressor, accumulator, suction drum etc.
    • F25J1/0292—Refrigerant compression by cold or cryogenic suction of the refrigerant 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/82—Processes or apparatus using other separation and/or other processing means using a reactor with combustion or catalytic reaction
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • 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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/04—Compressor cooling arrangement, e.g. inter- or after-stage cooling or condensate removal
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/14—External refrigeration with work-producing gas expansion loop
    • F25J2270/16—External refrigeration with work-producing gas expansion loop with mutliple gas expansion loops of the same refrigerant

Definitions

  • the present invention relates to a device for liquefying a gas and a method for liquefying a gas. It is applicable, in particular, to the field of liquefying a dihydrogen stream.
  • the liquefaction of dihydrogen is an energy-intensive process with a theoretical minimum energy consumption of 3.9 kWh per kilogram of liquid hydrogen produced.
  • Industrial cycles currently in operation consume between 11 and 13 kWh/ kgLH2 .
  • dihydrogen is used as a coolant or refrigerant, more than half of the energy consumption can be attributed to its compression. Improving the energy efficiency of hydrogen compressors is therefore essential to reducing the overall cost of hydrogen liquefaction.
  • Dihydrogen exists naturally in two forms depending on the spin number of its two protons: orthohydrogen (o-H2) and parahydrogen (p-H2).
  • the equilibrium composition of dihydrogen changes with temperature, as shown in figure 1 In the figure 1
  • the x-axis (110) represents temperature in Kelvin
  • the y-axis (105) represents the percentage of parahydrogen in the hydrogen.
  • dihydrogen is composed of 75% orthohydrogen and 25% parahydrogen (this composition is subsequently called normal hydrogen), while around 20 K, the liquefaction temperature, it is almost 100% parahydrogen. If normal hydrogen is liquefied and stored, a slow conversion to the parahydrogen form occurs (over several days). The heat generated by this conversion vaporizes some of the stored liquid, resulting in a loss.
  • the composition of dihydrogen when used as a refrigerant depends directly on the state of conversion of the hydrogen stream to be liquefied, and this composition does not vary over time. Indeed, the hydrogen recycled in the cycle has a composition of 99% parahydrogen and mixes in a fixed proportion over time with the dihydrogen to be liquefied, which has a normal composition.
  • Open hydrogen liquefaction cycles solve the problem of hydrogen composition evolution through the conversion step of the hydrogen to be liquefied. However, these cycles exhibit low energy efficiency.
  • the present invention aims to remedy all or part of these drawbacks.
  • the present invention relates to a device according to claim 1.
  • the hydrogen liquefaction cycle controls the composition of the hydrogen used as a refrigerant, for example by involving at least one catalytic reactor in the refrigeration cycle placed at a chosen temperature, in order to optimize the properties of the refrigerant and reduce the energy consumption of the device by having an operating equilibrium composition different from the natural equilibrium composition.
  • the closed refrigeration circuit is configured so that the refrigerant hydrogen at the inlet of the catalytic reactor has a temperature essentially equal to the average temperature of the refrigerant hydrogen in the closed circuit.
  • the catalytic reactor is positioned on a hot branch of the closed cooling circuit.
  • the catalytic reactor is configured to operate at a temperature between 31 K and 184 K. These embodiments allow for optimal energy efficiency of the device.
  • the maintenance means is configured to maintain the proportion of parahydrogen in the internal composition of the refrigerant dihydrogen stream between 27% and 96%. These embodiments allow for optimal energy efficiency of the device.
  • the holding means includes a bypass of the catalytic reactor configured to operate a predetermined flow ratio between the flow through the reactor and the flow through the bypass.
  • the closed circuit of refrigerant dihydrogen is configured to maintain an average dihydrogen temperature refrigerant temperature between 31 K and 184 K. These embodiments allow for optimal energy efficiency of the device.
  • the device of the present invention includes a pre-cooling circuit for the gas to be liquefied, said pre-cooling circuit comprising a heat exchanger between a pre-cooling fluid stream and the refrigerant hydrogen stream.
  • the gas to be liquefied is a stream consisting essentially of dihydrogen.
  • At least one catalytic reactor is integrated into a heat exchanger. Integrating the catalyst into a heat exchanger allows for continuous conversion during the cooling of the hydrogen to be liquefied, thus reducing the overall energy consumption of the liquefaction process.
  • this catalytic exchanger for the refrigerant dihydrogen flow eliminates the need for a catalytic reactor, thus reducing the cost and complexity of the overall process.
  • the closed refrigeration circuit includes an intercooling compression stage and at least one compression stage with a temperature below -40 °C for the refrigerant hydrogen. These arrangements limit the temperature rise of the refrigerant hydrogen and thus lower the average temperature in the cooling circuit.
  • the catalytic reactor is positioned on a cold branch of the closed refrigeration circuit. These embodiments allow for a reduction in the overall average temperature of the refrigerant flow in the closed transport circuit.
  • the closed refrigeration circuit includes at least one compressor for the ambient temperature refrigerant hydrogen and a storage tank for the liquid refrigerant hydrogen.
  • the catalytic reactor uses a catalyst comprising a member of the iron oxide family and preferably Fe2O3 .
  • the present invention relates to a method for liquefying a gas according to claim 15.
  • inventive concepts can be implemented by one or more of the methods or devices described below, several examples of which are provided here.
  • the actions or steps carried out in implementing the method or device can be ordered in any appropriate manner. Consequently, It is possible to construct embodiments in which the actions or steps are executed in a different order than illustrated, which may include the execution of some acts simultaneously, even if they are presented as sequential acts in the illustrated embodiments.
  • a and/or B when used in conjunction with open language such as “comprising”, may refer, in one embodiment, to A only (possibly including elements other than B); in another embodiment, to B only (possibly including elements other than A); in yet another embodiment, at A and B (possibly including other elements); etc.
  • the expression "at least one,” with reference to a list of one or more elements, is to be understood as meaning at least one element chosen from one or more elements in the list of elements, but not necessarily including at least one of each element specifically enumerated in the list of elements and not excluding any combination of elements in the list of elements.
  • This definition also allows for the optional presence of elements other than the elements specifically identified in the list of elements to which the expression “at least one” refers, whether or not they are related to those specifically identified elements.
  • “at least one of A and B" or, equivalently, "at least one of A”
  • At least one of A and/or B may refer, in one embodiment, to at least one, possibly including more than one, A, without B present (and possibly including elements other than B); in another embodiment, to at least one, possibly including more than one, B, without A present (and possibly including elements other than A); in yet another embodiment, to at least one, possibly including more than one, A, and at least one, possibly including more than one, B (and possibly including other elements); etc.
  • the gas 51 to be liquefied can be of any type ordinarily liquefied.
  • this gas 51 is dihydrogen.
  • the refrigerant stream is defined as containing at least some hydrogen refrigerant.
  • the proportion of hydrogen refrigerant depends on the specific application of the present invention. In some embodiments, the proportion of hydrogen refrigerant in the refrigerant stream is at least 30%. In some embodiments, the proportion of hydrogen refrigerant in the refrigerant stream is at least 50%. In some embodiments, the proportion of hydrogen refrigerant in the refrigerant stream is at least 70%. In some embodiments, the proportion of hydrogen refrigerant in the refrigerant stream is at least 90%. In some embodiments, the proportion of hydrogen refrigerant in the refrigerant stream is at least 99%. In the following description, the terms "refrigerant stream” and "hydrogen refrigerant" are used interchangeably.
  • the refrigerant dihydrogen 52 can originate from liquefied dihydrogen 51 or from a third source.
  • a "hot branch" of a closed circuit is at least a part of said circuit in which the temperature of the transported fluid decreases.
  • a "cold branch" of a closed circuit is at least a part of said circuit in which the temperature of the transported fluid increases.
  • the transport circuit 55 for example, is formed of a set of pipes configured to transport the gas 51 to be liquefied, the gas 51 originating from a source (not shown) and being transported to a fixed or mobile storage 56.
  • This transport circuit 55 is configured to transport the gas 51 through at least one heat exchanger, 201, 202, 203, 204, 205, 206, 207, 208 and/or 209.
  • Each heat exchanger, 201, 202, 203, 204, 205, 206, 207, 208 and/or 209, may belong to a pre-cooling and/or cooling circuit.
  • the number and arrangement of heat exchangers, 201, 202, 203, 204, 205, 206, 207, 208 and/or 209, depends on the desired configuration for device 200, the desired specifications for gas 51 at the outlet of this device 200 and the desired energy performance for device 200.
  • Storage 56 can be a temporary storage for separating the evaporation gas and the liquefied gas 51.
  • the feed stream consists of normal hydrogen (25% parahydrogen and 75% orthohydrogen) at a pressure of 21 bar, a temperature of 298 K (25 °C), and a mass flow rate of 0.116 kg/s.
  • the stream is first cooled to 83 K (-190 °C) by two heat exchangers. This stream then enters a catalytic heat exchanger, which performs the first stage of the ortho-to-para conversion.
  • the stream exits the pre-cooling section at a temperature of 80 K (-193 °C) with a composition of 49% parahydrogen.
  • the feed stream 51 reaches a temperature of 22 K (-251 °C) and a composition of 99% parahydrogen through a series of six catalytic heat exchangers.
  • the final liquefaction stage is carried out with a pressure-reducing valve that lowers the pressure to 2 bar.
  • the liquid portion of the stream (98%) exits the device, and the remaining gaseous portion is conveyed to an exhaust gas management system.
  • Each heat exchanger is, for example, a plate heat exchanger between a so-called “hot” fluid and a so-called “cold” fluid.
  • the gas 51 to be liquefied acts as the hot fluid.
  • the cold fluid depends on the implementation variants.
  • the heat exchangers in the cooling section use hydrogen refrigerant as the cold fluid
  • the heat exchangers in the pre-cooling section use hydrogen refrigerant and a pre-cooling fluid.
  • the refrigeration circuit 210 is formed of a A set of pipes configured to transport the refrigerant hydrogen 52.
  • This transport circuit 210 is configured to transport the refrigerant hydrogen 52 through at least one heat exchanger, 201, 202, 203, 204, 205, 206, 207, 208 and/or 209.
  • the configuration of the refrigeration circuit 210 depends on the desired performance of the device 200 and the operating conditions expected for this device 200.
  • the refrigerant dihydrogen 52 is configured to have a temperature between 171 K and 22 K, this dihydrogen 52 refrigerant being configured to cool the gas 51 to be liquefied.
  • the 410 refrigeration circuit is a closed circuit, similar to the 210 refrigeration circuit as shown in figure 2 , in which the holding means 415 comprises two catalytic reactors, 420 and 421, located on either side of the fourth heat exchanger 404 along the hot branch.
  • the catalytic reactor 820 is positioned on a cold branch of the closed refrigeration circuit 810.
  • the closed refrigeration circuit 810 comprising at least one compressor 817 of the refrigerant dihydrogen at ambient temperature and a tank 819 for storing the liquid refrigerant dihydrogen.
  • the closed circuit, 210, 310, 410, 510, 610, 710 and/or 810, of refrigerant dihydrogen is configured to maintain an average temperature of the refrigerant dihydrogen between 31 K and 184 K.
  • the closed circuit 210 includes a means 215 for maintaining the internal composition of the dihydrogen.
  • a maintenance means 215 includes, for example, at least one catalytic reactor 220 configured to promote a predetermined ratio of parahydrogen to orthohydrogen. This ratio is selected so as to be lower or higher than the same ratio in a natural equilibrium state of a closed circuit 210 without a maintenance means 215. Increasing the relative proportion of parahydrogen in the composition of the dihydrogen improves the performance of the dihydrogen in the heat exchanges taking place within the device 100.
  • the catalytic reactor 220 is positioned on a hot branch of the closed circuit 210.
  • the catalytic reactor 320 is positioned on a cold branch of the closed circuit 310.
  • the holding means 415 comprises two catalytic reactors, 420 and 421, positioned on a hot branch of the closed circuit 210. These two catalytic reactors, 420 and 421, are positioned, for example, on either side of a heat exchanger with the flow 51 of gas to be liquefied.
  • This heat exchanger is, for example, the fourth heat exchanger 404 in a general sequence of a pre-cooling section with three heat exchangers, which corresponds to the first heat exchanger in the cooling section.
  • the 520 catalytic reactor is a so-called “short” reactor positioned on a hot branch of the closed 510 circuit.
  • the maintenance means 615 comprises a catalytic reactor 620 and a bypass 616 of the reactor 620, positioned on a hot branch of the closed circuit 610.
  • the bypass 616 is, for example, a valve mounted on a pipe whose inlet is located upstream of reactor 620 and whose outlet is located downstream of reactor 620. This valve can be controlled in flow rate to the flow rate through reactor 620.
  • the 616 bypass is associated with a control unit, such as a PLC, configured to issue activation or deactivation commands to the 616 bypass according to predetermined activation criteria.
  • a control unit such as a PLC
  • the maintenance means 1115 comprises at least one catalytic reactor 1120 integrated into a heat exchanger 204.
  • the catalytic reactor 1120 can be integrated into any heat exchanger, 202, 203, 204, 205, 206, 207, 208 or 209, of the closed circuit 52.
  • the reactor, 220, 320, 420, 520, 620, 720 and/or 820 catalytic is configured to operate at a temperature between 31 K and 184 K.
  • the maintenance means, 215, 315, 415, 515, 615, 715 and/or 815 is configured to maintain the proportion of parahydrogen in the internal composition of the refrigerant dihydrogen stream between 27% and 96%.
  • the cooling loop is a dual-pressure loop, known as a "Claude loop," and the refrigerant used is hydrogen.
  • the refrigerant fluid 52 is first compressed to 29 bar by a multi-stage compressor 213.
  • the temperature of the fluid 52 at the outlet of the compressor 213 is approximately 171 K (-102 °C).
  • the fluid 52 is cooled to 80 K (-193 °C) with two heat exchangers, 202 and 203, by exchange with a pre-cooling fluid, such as nitrogen.
  • the fluid 52 then enters a cooling section and is cooled to 69 K (-204 °C) in the first cooling heat exchanger 204.
  • the hydrogen stream 52 passes through a catalytic conversion reactor 220 where the hydrogen reaches an equilibrium composition for the operating temperature considered.
  • the hydrogen is, for example, composed of 58% parahydrogen and 42% orthohydrogen.
  • the hydrogen is thus slightly heated to between 0.1 K and 0.5 K in steady state.
  • the refrigerant is then separated, and 89% of the total flow is expanded, by means of an expansion valve 214, to 18.5 bar and reaches 60 K (-213 °C).
  • the flow 52 is then cooled to 51 K (-222 °C) in a heat exchanger 206, and then expanded with a two-stage expansion valve 216 to 4.5 bar to reach 31.5 K (-241.5 °C).
  • the flow 52 is used as a refrigerant in the cooling heat exchangers 207, 206, 205, and 204.
  • the remaining portion (11%) is cooled to 26 K through four heat exchangers, 205, 206, 207, and 208.
  • This portion is then expanded with an expansion valve 211 to 1.5 bar to reach 22 K.
  • the liquid refrigerant cools the supply stream to 22 K in two two-phase heat exchangers, 209 and 208, and four multi-flow heat exchangers, 207, 206, 205, and 204.
  • the two refrigerant streams at 4.5 and 1.5 bar exit the cooling section at 78 K (-195 °C).
  • the low-pressure stream is compressed to 4.5 bar in a first compressor 212.
  • the stream from the first compressor 212 is then mixed with the medium-pressure stream before entering the second compressor 213.
  • the closed refrigeration circuit, 210, 310, 410, 510, 610, 710 and/or 810 is configured so that the flow 52 of refrigerant dihydrogen has, at the inlet of the catalytic reactor, 220, 320, 420, 520, 620, 720 and/or 820, a temperature essentially equal to the average temperature of the refrigerant dihydrogen 52 in the closed circuit, 210, 310, 410, 510, 610, 710 and/or 810.
  • the device, 200, 300, 400, 500, 600, 700 and/or 800 comprises a circuit 54 for pre-cooling the gas to be liquefied, said pre-cooling circuit comprising at least one heat exchanger, 203, 303, 403, 503, 603, 703 and/or 802, between a pre-cooling fluid flow and the 52 flow of refrigerant dihydrogen.
  • the pre-cooling circuit 54 is configured to transport nitrogen with a temperature between 298 K and 80 K.
  • the objective of such a pre-cooling circuit 54 is to cool the gas 51 to be liquefied and the refrigerant dihydrogen from 90 K to 80 K.
  • the pre-cooling circuit 54 is similar to the cooling circuit 54 shown in figures 2 to 6 , the compressor 57 being formed of a succession of compressors.
  • the refrigerant flow 54 is implemented in at least one heat exchanger 719 of the intercooled compression stage 713 and in at least one compression stage 718 at a temperature below -40°C.
  • the pre-cooling circuit 54 is an open circuit.
  • pre-cooling from 300 K (27 °C) to 80 K (-193 °C) is achieved using a closed nitrogen loop.
  • the nitrogen is first compressed from 1 bar to 50 bar by a multi-stage compressor 57. This nitrogen is then cooled to 200 K (-73 °C) in a heat exchanger 201. The nitrogen is then separated; 97% of the total flow is expanded to 1.1 bar in an expansion valve 59 and reaches 81 K (-192 °C). This nitrogen returns as refrigerant to the first pre-cooling heat exchanger 201. The remaining portion (3%) is cooled to 83 K (-190 °C).
  • This portion is then partially liquefied by an expansion valve 56, reaching 78 K (-195°C), and functions in the third heat exchanger 203 as the primary refrigerant.
  • the remaining cooling capacity of the nitrogen is used in the pre-cooling heat exchangers 202 and 201.
  • a particular composition of the refrigerant dihydrogen that is the subject of the present invention comprises 58% parahydrogen and 42% orthohydrogen, this composition not being the natural equilibrium composition. This constitutes a compromise to obtain the best match between the thermal properties of the gas both during its compression and as a refrigerant.
  • the present invention exhibits high operating performance under the following operating conditions, with regard to the device 200 shown in figure 2 : Table 1 Settings lower limit upper limit Pre-cooling temperature (K/°C) 60 / -213 150 /-123 Compression inlet temperature (K/°C) 31 / -242 250 / -23 Parahydrogen fraction (%) 27% 96% Catalysis temperature (K/°C) 31 / -232 184 / -89 Average refrigerant temperature (K) 31 / -232 184 / -89 Minimum operating time (days) 30 -
  • the catalytic reactor 320 is positioned on a return branch of the cooling loop, which shifts the cycle equilibrium according to its associated temperature.
  • a suitable position for reactor 320 is between the fifth heat exchanger 305 and the sixth heat exchanger 306.
  • the catalysis temperature is 54 K (-219 °C) (for a composition of 74% p-H2 and 26% o-H2).
  • the catalytic conversion is carried out in several catalytic reactors, 420 and 421, arranged at different temperatures, thus aiming for a stepwise conversion of the refrigerant hydrogen.
  • This is advantageous because the heat generated during the conversion increases inversely with temperature.
  • a first conversion is carried out at 80 K (-193 °C), bringing the hydrogen to a composition of 52% p-H2, and then a second conversion is carried out at 69 K (-204 °C), bringing the hydrogen to the target composition of 58% p-H2.
  • reactor 520 is sized so that the transit time or the reactivity of the catalyst does not allow for reaching thermodynamic equilibrium.
  • reactor 520 is placed at a catalysis temperature of 56 K (-217 °C), but shortening the length of reactor 520 allows the target composition of 58% p-H2 to be reached instead of the equilibrium composition of 70% p-H2 associated with the temperature of 56 K (-217 °C).
  • the target composition can be selected using a partial bypass device of reactor 620.
  • the final composition corresponds to the average of the output compositions of reactor 620 and bypass 616 weighted by the respective flow rates passing through them.
  • cryogenic compression with intermediate cooling i.e. cooling the refrigerant fluid between each stage.
  • the placement of the catalytic reactor 820 is configured so that compression takes place at ambient temperature. If the average temperature of the refrigerant dihydrogen remains below 184 K (-89 °C), as is the case, for example, if a liquid hydrogen buffer storage is used after valve 53, then in this embodiment, increasing the parahydrogen content reduces the natural conversion in the liquid buffer storage, thereby reducing and shifting some of the losses associated with the process to a location less sensitive to heat release.
  • the present invention is particularly suitable for the production of liquid hydrogen in excess of five tonnes per day because the reduction in investment requirements and the stability of the process in operation allow for savings on the final cost of hydrogen liquefaction.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
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Claims (15)

  1. Vorrichtung (200, 300, 400, 500, 600, 700, 800, 1100) zum Verflüssigen eines Gases (51), umfassend:
    - einen Transportkreislauf (55) für das zu verflüssigende Gas, der mindestens einen Wärmetauscher (204, 304, 404, 504, 604, 704, 804) zwischen dem zu verflüssigenden Gas (51) und einem Kältemittelstrom (52),
    der mindestens das Kältemittel Dihydrogen enthält,
    - einen geschlossenen Kühlkreislauf (210, 310, 410, 510, 610, 710, 810) zum Transportieren des Kältemittelstroms,
    dadurch gekennzeichnet, dass der geschlossene Kühlkreislauf ein Mittel (215, 315, 415, 515, 615, 715, 815, 1115) zum Aufrechterhalten einer inneren Zusammensetzung des Kältemittels Dihydrogen in einem Verhältnis von Parahydrogen zu Orthohydrogen, das geringer oder größer ist als das Verhältnis, das einer natürlichen Gleichgewichtszusammensetzung im geschlossenen Kältemittelkreislauf entspricht, wobei das Mittel einen katalytischen Reaktor (220, 320, 420, 520, 620, 720, 820, 1120) umfasst, der so konfiguriert ist, dass er einen Teil des Orthowasserstoffs des Kältemitteldihydrogenstroms in Parahydrogen umwandelt oder umgekehrt.
  2. Vorrichtung (200, 400, 500, 600, 700, 800, 1100) nach Anspruch 1, wobei der geschlossene Kühlkreislauf (210, 310, 410, 510, 610, 710, 810) so konfiguriert ist, dass das Kältemittel Dihydrogen am Eingang des katalytischen Reaktors (220, 320, 420, 520, 620, 720, 820) im Wesentlichen der gleichen Temperatur wie die durchschnittliche Temperatur des Kältemittels Dihydrogen im geschlossenen Kreislauf aufweist.
  3. Vorrichtung (200, 400, 500, 600, 1100) nach einem der Ansprüche 1 oder 2, wobei der katalytische Reaktor (220, 420, 520, 620) an einem heißen Strang des geschlossenen Kreislaufs (210, 410, 510, 610) positioniert ist.
  4. Vorrichtung (200, 300, 400, 500, 600, 700, 800, 1100) nach einem der Ansprüche 1 bis 3, wobei der Reaktor (220, 320, 420, 520, 620, 720, 820) so konfiguriert ist, dass er bei einer Temperatur zwischen 31 K und 184 K betrieben werden kann.
  5. Vorrichtung (200, 300, 400, 500, 600, 700, 800, 1100) nach einem der Ansprüche 1 bis 4, wobei das Mittel (215, 315, 415, 515, 615, 715, 815) so konfiguriert ist, dass es den Anteil an Parawasserstoff in der inneren Zusammensetzung des Kältemittels Dihydrogen zwischen 27 % und 96 % hält.
  6. Vorrichtung (600) nach einem der Ansprüche 1 bis 5, wobei das Mittel (615) einen Bypass (616) des katalytischen Reaktors umfasst, der so konfiguriert ist, dass er ein vorbestimmtes Durchflussverhältnis zwischen dem durch den Reaktor (620) strömenden Durchfluss und dem durch den Bypass strömenden Durchfluss herstellt.
  7. Vorrichtung (200, 300, 400, 500, 600, 700, 800, 1100) nach einem der Ansprüche 1 bis 6, wobei der geschlossene Kühlkreislauf (210, 310, 410, 510, 610, 710, 810) so konfiguriert ist, dass er eine durchschnittliche Temperatur des Dihydrogen-Kältemittels zwischen 31 K und 184 K aufrechterhält.
  8. Vorrichtung (200, 300, 400, 500, 600, 700, 800, 1100) nach einem der Ansprüche 1 bis 7, die einen Kreislauf (54) zum Vorkühlen des zu verflüssigenden Gases umfasst, wobei der Vorkühlkreislauf einen Wärmetauscher (203, 303, 403, 503, 603, 703, 802) zwischen einem Vorkühlfluidstrom und dem Strom (52) des Kältemittels Dihydrogens umfasst.
  9. Vorrichtung (200, 300, 400, 500, 600, 700, 800, 1100) nach einem der Ansprüche 1 bis 8, wobei das zu verflüssigende Gas ein im Wesentlichen aus Dihydrogen bestehender Strom ist.
  10. Vorrichtung (1100) nach einem der Ansprüche 1 bis 9, wobei mindestens ein katalytischer Reaktor (1120) in einen Wärmetauscher (204) integriert ist.
  11. Vorrichtung (700) nach einem der Ansprüche 1 bis 10, wobei der geschlossene Kühlkreislauf (710) eine Kompressionsstufe (713) mit Zwischenkühlung und mindestens eine Kompressionsstufe (718) mit einer Temperatur unter -40 °C für das Kältemittel Dihydrogen umfasst.
  12. Vorrichtung (800) nach einem der Ansprüche 1 bis 11, wobei der katalytische Reaktor (820) an einem kalten Strang des geschlossenen Kreislaufs (810) positioniert ist.
  13. Vorrichtung (800) nach einem der Ansprüche 1 bis 12, wobei der geschlossene Kühlkreislauf (810) mindestens einen Kompressor (817) für das Kältemittel Dihydrogen bei Umgebungstemperatur und einen Speicherbehälter (819) für das flüssige Kältemittel Dihydrogen umfasst.
  14. Vorrichtung (200, 300, 400, 500, 600, 700, 800, 1100) nach einem der Ansprüche 1 bis 13, wobei der katalytische Reaktor (220, 320, 420, 520, 620, 720, 820) einen Katalysator einsetzt, der ein Mitglied der Familie der Eisenoxide und vorzugsweise Fe2O3 umfasst.
  15. Vorrichtung (1000) zum Verflüssigen eines Gases (51), umfassend:
    - einen Schritt (1005) zum Transportieren des zu verflüssigenden Gases, der mindestens einen Schritt (1010) zum Wärmeaustausch zwischen dem zu verflüssigenden Gas und einem Kältemittelstrom, der mindestens das Kältemittel Dihydrogen enthält,
    - einen Schritt (1015) zum Transportieren des Kältemittelstroms in einem geschlossenen Kühlkreislauf,
    des Kältemittelstroms, dadurch gekennzeichnet, dass der Schritt des Transports des Kältemittelstroms einen Schritt (1020) des Aufrechterhaltens einer inneren Zusammensetzung des Kältemittels Dihydrogen in einem Verhältnis von Parahydrogen zu Orthohydrogen umfasst, das geringer oder größer ist als das Verhältnis, das einer natürlichen Gleichgewichtszusammensetzung im geschlossenen Kältemittelstromkreislauf entspricht, wobei der Aufrechterhaltungsschritt einen Schritt (1025) der katalytischen Reaktion umfasst, um einen Teil des Orthowasserstoffs des Kältemittels Dihydrogen in Parahydrogen umzuwandeln oder umgekehrt.
EP22840192.3A 2021-12-21 2022-12-21 Vorrichtung und verfahren zur verflüssigung eines gases Active EP4453488B1 (de)

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