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  • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
  • C07C7/00—Purification; Separation; Use of additives
  • C07C7/005—Processes comprising at least two steps in series
• • 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
  • B01D53/02—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 adsorption, e.g. preparative gas chromatography
  • B01D53/04—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 adsorption, e.g. preparative gas chromatography with stationary adsorbents
  • B01D53/0462—Temperature swing adsorption
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  • 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
  • B01D53/22—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 diffusion
  • B01D53/225—Multiple stage diffusion
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  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
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  • B01D53/22—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 diffusion
  • B01D53/225—Multiple stage diffusion
  • B01D53/226—Multiple stage diffusion in serial connexion
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  • 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
  • B01D53/22—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 diffusion
  • B01D53/229—Integrated processes (Diffusion and at least one other process, e.g. adsorption, absorption)
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  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F11/00—Treatment of sludge; Devices therefor
  • C02F11/02—Biological treatment
  • C02F11/04—Anaerobic treatment; Production of methane by such processes
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• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
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• • C—CHEMISTRY; METALLURGY
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  • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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  • 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
  • F25J3/0209—Natural gas or substitute natural gas
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  • 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
  • F25J3/0233—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 CnHm with 1 carbon atom or more
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  • 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
  • F25J3/0257—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 nitrogen
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  • 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
  • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
• • 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
  • B01D2256/24—Hydrocarbons
  • B01D2256/245—Methane
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2257/00—Components to be removed
  • B01D2257/10—Single element gases other than halogens
  • B01D2257/102—Nitrogen
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  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2257/00—Components to be removed
  • B01D2257/10—Single element gases other than halogens
  • B01D2257/104—Oxygen
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  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
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• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
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  • B01D2257/50—Carbon oxides
  • B01D2257/504—Carbon dioxide
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  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2257/00—Components to be removed
  • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
  • B01D2257/708—Volatile organic compounds V.O.C.'s
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  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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  • B01D2257/80—Water
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
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  • B01D2258/05—Biogas
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2259/00—Type of treatment
  • B01D2259/40—Further details for adsorption processes and devices
  • B01D2259/402—Further details for adsorption processes and devices using two beds
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  • B01D2259/416—Further details for adsorption processes and devices involving cryogenic temperature treatment
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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  • 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
  • B01D53/02—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 adsorption, e.g. preparative gas chromatography
  • B01D53/04—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 adsorption, e.g. preparative gas chromatography with stationary adsorbents
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  • 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
  • F25J2200/00—Processes or apparatus using separation by rectification
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  • F25J2200/00—Processes or apparatus using separation by rectification
  • F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
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  • 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
  • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
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  • F25J2205/00—Processes or apparatus using other separation and/or other processing means
  • F25J2205/80—Processes or apparatus using other separation and/or other processing means using membrane, i.e. including a permeation step
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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  • F25J2210/00—Processes characterised by the type or other details of the feed stream
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  • F25J2210/00—Processes characterised by the type or other details of the feed stream
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  • F25J2220/62—Separating low boiling components, e.g. He, H2, N2, Air
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  • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
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• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
  • Y02C20/00—Capture or disposal of greenhouse gases
  • Y02C20/40—Capture or disposal of greenhouse gases of CO2
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E50/00—Technologies for the production of fuel of non-fossil origin
  • Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel

Definitions

• the invention relates to a process for producing bio methane by biogas purification, for example biogas from non-hazardous waste storage facilities (ISDND). It also relates to an installation for implementing the method.
• ISDND non-hazardous waste storage facilities
• the present invention relates to a method of treatment by coupling a membrane permeation and a cryogenic distillation of a gaseous stream containing at least methane, carbon dioxide, air gases (nitrogen and oxygen) and pollutants (H 2 S and volatile organic compounds (VOCs)).
• the objective is to produce a gaseous stream rich in methane whose methane content is in line with the needs of its use and to limit as much as possible the impact of CH 4 discharges into the atmosphere (high greenhouse gas) ).
• the invention relates in particular to the purification of biogas from non-hazardous waste storage facilities, hereinafter ISDND (Non-Hazardous Waste Storage Facility), with the aim of producing biomethane in accordance with the injection into a natural gas system or in local use as a vehicle fuel.
• ISDND Non-Hazardous Waste Storage Facility
• ISDNDs The anaerobic digestion of organic wastes in ISDNDs produces a significant amount of biogas throughout ISDND's lifetime and even several years after shutdown and closure of ISDND.
• methane and carbon dioxide - biogas is a powerful greenhouse gas; At the same time, it constitutes a significant source of renewable energy in the context of the scarcity of fossil fuels.
• Biogas contains several polluting compounds and must be purified to allow commercial development. There are several processes for recovering and purifying biogas.
• Biogas mainly contains methane (CH 4 ) and carbon dioxide (CO 2 ) in varying proportions depending on the method of production.
• the gas also contains a proportion of air gases (nitrogen and oxygen) and, to a lesser extent, water, hydrogen sulphide, and volatile organic compounds (VOCs).
• air gases nitrogen and oxygen
• VOCs volatile organic compounds
• the proportions of the biogas components differ.
• the biogas comprises, on dry gas, 30 to 60% of methane, 15 to 50% of CO2, 0 to 30% of nitrogen, 0 to 6% of oxygen, 0 to 1% of hosts and a few tens to thousands of milligrams per normal cubic meters of VOCs and a number of other trace impurities.
• Biogas is valued in different ways. It may, after partial treatment, be recovered near the production site to provide heat, electricity or both (cogeneration). The high content of carbon dioxide and nitrogen reduces its calorific value, increases the compression and transport costs and limits the economic interest of its valuation to this use of proximity.
• Biomethane thus completes the natural gas resources with a renewable part produced in the heart of the territories. It is usable for exactly the same uses as natural gas of fossil origin. It can feed a natural gas network, a filling station for vehicles.
• the modes of valorization of the biomethane are determined according to the local contexts: local energy needs, possibilities of valorization as biomethane fuel, existence close to networks of distribution or transport of natural gas in particular. Creating synergies between the different actors working on a territory (farmers, industrialists, public authorities), the production of biomethane helps the territories to acquire a greater energy autonomy.
• the document US Pat. No. 8,221,524 B2 describes a process for enriching a gas with CH 4 by up to 88% by different recycling steps.
• the process consists of compressing the gas stream and then passing it over an adsorbent to remove VOCs.
• the gas stream is then subjected to a membrane separation step and then to a pressure swing adsorption step (PSA).
• PSA pressure swing adsorption step
• the adsorbent used in the PSA is of the CMS (carbon molecular sieve) type and makes it possible to eliminate the nitrogen and a small part of the oxygen.
• EP1979446 discloses a biogas purification process of removing hhS, compressing the gas, filtering it to remove particles. The gas is then subjected to a membrane separation step to remove CO2 and GO2, from drying by passing through a PSA then in different filters and finally again in a PSA to eliminate nitrogen. The gas is finally liquefied.
• US2004 / 0103782 discloses a biogas purification process of eliminating gas compression, filtering it to remove particles, subjecting it to a pressure swing adsorption (PSA) step to remove VOCs, and then membrane separation to remove most of the CO2 as well as a fraction of the oxygen.
• PSA pressure swing adsorption
• US5964923 and US5669958 disclose a method of treating a gaseous effluent comprising dehydrating the gas, condensing it through an exchanger, subjecting the gas to membrane separation, and then cryogenic separation.
• US2010 / 077796 discloses a purification process of subjecting the gaseous stream to a membrane separation, treating the permeate in a distillation column, and then mixing the methane gas from the column, after vaporization, with the retentate obtained at room temperature. the outcome of membrane separation.
• EP0772665 describes the use of a cryogenic distillation column for the separation of mine gas composed mainly of CFI 4 , CO2 and nitrogen.
• One of the problems that the invention proposes to solve is that of providing a biogas purification process complying with the above constraints, that is to say a process that is safe, with optimal yield, producing a biomethane high quality substitutable for natural gas and which meets environmental standards including the destruction of polluting compounds such as VOCs and compounds with strong greenhouse effect such as CFI 4 .
• the gas thus produced can be recovered in gaseous form either by injection into a gas network or for mobility applications.
• the CO2 is mainly removed on the membrane step. This imperfect separation leaves in the purified gas a CO2 content frequently between 0.5 mol% and 1.5 mol%. It is possible to reduce the content of CO2 in the purified gas by sizing the unit of separation (involving consumption more important of the compressor). In all cases the CO2 content in the purified gas can never be much lower (same order of magnitude of concentration).
• This purified gas containing, among others, the remainder of CO2, methane, a little oxygen and nitrogen (between 1% and 20% mol) is then treated in a cryogenic unit.
• the temperatures reached in this unit are of the order of -100 ° C. or even lower, which at low pressure (between Patm and about thirty bar) leads to solidification of the CO2 contained in the gas to be treated.
• a frequently used solution is to use a purification step based on adsorption technology (TSA, Temperature Swing Adsorption).
• TSA Temperature Swing Adsorption
• This technology makes it possible to reach very low levels of CO2 (for example 50ppmv in the case of a liquefied natural gas). At these levels, the CO2 does not solidify at the temperatures considered even at low pressure because it is still soluble in methane.
• this purification unit is relatively expensive and requires the use of a so-called regeneration gas to be able to evacuate the stopped CO2.
• the gas frequently used is either the nitrogen that has been separated in the cryogenic stage or the methane product at the outlet of NRU. If nitrogen is used, it may be necessary to degrade the efficiency of the unit or add nitrogen to achieve the required flow rate. If production methane is used, CO2 concentration peaks associated with desorption may appear to make the gas out of specification.
• the gas from a landfill or a biogas production unit contains oxygen (typical value between 0% and 1% mol of oxygen, but potentially more).
• This oxygen is partially removed in the pretreatment steps including that of the membranes which consists in removing the CO2. During this stage, the amount of oxygen in absolute value decreases but its concentration increases or remains constant.
• the oxygen entering the cryogenic part may concentrate in certain places such as the distillation column. Indeed, the volatility of oxygen is between that of nitrogen and that of methane. It is therefore quite possible to create zones of concentration of oxygen in the distillation column. This concentration, if not controlled, can reach values that are likely to to cause an inflammation, to see an explosion of the gas mixture. This is a security risk of major importance that the inventors of the present invention sought to minimize.
• the inventors of the present invention have then developed a solution to solve the problems raised above.
• the subject of the present invention is a method for producing biomethane by purifying a biogas feed stream, comprising the following steps:
• the columns to be distilled have a cylindrical shape, their height is always very large compared to their diameter. Most used are equipped with trays.
• the plates of a column aim to put in contact the liquid, which falls down by gravity, with the rising vapor. They include an active area pierced with holes, possibly equipped with valves or bells, a dam to retain on the plateau a certain thickness of liquid, a weir for bringing the liquid of the plateau considered to the lower plate .
• the solution that is the object of the present invention is therefore not to further reduce the CO2 content at the outlet of the membrane step while ensuring a sufficient solubility of the CO2 in the gas to be treated (mainly methane) in order to avoid a crystallization and that at any point of the process.
• the TSA stage for slaughtering the majority of CO2 is therefore removed.
• the gas that supplies the cryogenic section therefore contains between 0.3 mol% and 2 mol% of CO2.
• the solution that is the subject of the present invention makes it possible to limit the risk related to the presence of oxygen during the distillation.
• the subject of the invention is also:
• distillation column comprises n real trays, n being an integer between 8 and 100 and characterized in that said stream or gaseous mixture from step a) depleted in CO2 implemented in step b) is introduced into the distillation column at a plateau between the plate n-4 and the plate n, the plate n being the highest plateau in said column.
• step a) further comprises a step of purifying the compressed gaseous gas stream at pressure P1.
• step b) A process as defined above, characterized in that said gaseous stream from step a) depleted of CO2 implemented in step b) comprises between 0.3 mol% and 2 mol% of CO2.
• step a) the separation of CO2 and oxygen from the feed gas stream is performed by a unit comprising at least two stages of separating membranes.
• step c) A method as defined above, characterized in that the pressure P2 of step c) is greater than 40 bar abs.
• step b the gaseous stream depleted in CO2 from step a) undergoes expansion to a pressure P3 between 15 bar abs and 40 bar abs before entering said distillation column.
• P3 is greater than 25 bar abs.
• step b A process as defined above, characterized in that the gaseous stream depleted of CO2 from step a) is at least partially condensed in a countercurrent heat exchanger of the CH 4 enriched stream from step c) and at least a portion of the nitrogen stream separated in step b).
• the subject of the invention is also:
• a pretreatment unit for removing all or part of the VOCs, water, sulfur compounds from the gas stream to be treated
• a compressor capable of compressing said gaseous flow at a pressure of between 25 and 100 bar;
• distillation column comprises n trays and the level of introduction of the stream to be treated in said column depends on the oxygen concentration of said stream to be treated, n being an integer between 8 and 100.
• the heat exchanger may be any heat exchanger, unit or other arrangement adapted to allow the passage of a number of flows, and thus allow a direct or indirect heat exchange between one or more lines of refrigerant, and a or multiple feed streams.
• the gas to be treated is thus cooled partially or totally liquefied in the exchange line. It is then expanded to the distillation pressure.
• the partially or totally liquefied gas is expanded and then injected into the distillation column. This injection is carried out either directly at the head of one of the 4 trays head of the column.
• the reference refers to a liquid flow and the pipe that carries it, the pressures considered are absolute pressures and the percentages considered are molar percentages.
• the plant comprises a source of biogas to be treated (1), a pretreatment unit (5) comprising a compression unit (2) and a CO2 and Ü2 purification unit (23), a VOC purification unit and water (3), a cryodistillation unit (4), and finally a unit for recovering methane gas (6). All devices are interconnected by pipes.
• the CO2 purification unit (23) combines, for example, two membrane separation stages.
• the membranes are chosen to allow the separation of at least 90% of the CO2 and about 50% of GO2.
• the retentate from the first separation is then directed to the second membrane separation.
• the permeate from the second membrane separation is recycled through a pipe connected to the main circuit upstream of the compressor. This step makes it possible to produce a gas (7) with less than 3% CO2 and with a CH 4 yield greater than 90%.
• the temperature of this stream is typically ambient, if necessary air or water cooling steps can be incorporated.
• the compression unit (2) is for example in the form of a piston compressor.
• the purification unit (TSA) of VOC and water (3) comprises two bottles (9, 10). They are loaded with adsorbents chosen specifically to allow the adsorption of water and VOCs, and their subsequent desorption during regeneration. The bottles work alternately in production mode and regeneration mode.
• the bottles (9, 10) are supplied with gaseous flow at their lower part.
• the pipe in which the gas flow (8) flows is split into two pipes (1 1, 12), each equipped with a valve (13, 14) and feeding the lower part respectively of the first bottle (9) and the second bottle (10).
• the valves (13, 14) will be alternately closed depending on the saturation level of the bottles.
• the valve (13) is closed and the valve (14) is opened to begin charging the second bottle (10).
• From the upper part of each of the bottles opens a pipe respectively (15 and 16).
• Each of them splits into two pipes respectively (17, 18) and (19, 20).
• the purified flow of water and VOC from the first bottle flows through the pipe (18) while the purified flow of water and VOC from the second PSA flows through the pipe (20).
• the two pipes are joined to form a single pipe (21) supplying the cryogenic unit (4).
• the cryodistillation unit (4) is fed by the pipe (21) in which circulates the gas stream (22) to be purified. It contains three elements respectively a heat exchanger (24), a reboiler (25), a distillation column (26).
• the exchanger (24) is preferably a brazed plate heat exchanger made of aluminum or stainless steel. It cools the gas stream (22) flowing in the pipe (21) by heat exchange with the flow of liquid methane (27) withdrawn from the distillation column (26). The gas stream (22) is cooled (28) to a temperature of about -100 ° C. The two-phase flow (28) resulting therefrom may alternatively ensure the reboiling of the bottom reboiler (25) of the column (26) and the heat generated (29) is transferred to the bottom of the column (26).
• the cooled fluid (28) is expanded by means of a valve (30) at a pressure for example between 20 bar absolute and 45 bar absolute bar absolute.
• the fluid then in the diphasic state or in the liquid state (31) is introduced into the column (26) at a stage E1 located in the upper part of said column (26) at a temperature, for example between -1 10 ° C and -100 ° C.
• the CO2-depleted gaseous stream (22) introduced into the column (26) at a stage E1 has an oxygen concentration equal to C1.
• the resulting gas stream (22) is introduced into the distillation column at a level E1 between the plate n-4 and the plate n, the plate n being the plate located on higher in said column.
• the gaseous stream (22) is introduced into the distillation column at a level E 1 of the plate n, the plate n being the most high in said column.
• the liquid (31) then separates in the column (26) to form a gas (32) through the condenser (33).
• the cooling of the condenser (33) may, for example be provided by a refrigerating cycle using nitrogen and or methane.
• a portion (36) of the liquid (37) exiting the distillation column vessel (26) at a temperature between -120 ° C and -90 ° C is sent to the reboiler (25) where it partially vaporizes. .
• the formed gas (29) is returned to the column vessel (26).
• the other portion (38) of the remaining liquid (37) is pumped by means of a pump (39) to form the liquid methane stream (27) which vaporizes in the exchanger (24) to form a methane product pure gas (40).
• This pumping step is carried out at a high pressure, typically above the critical pressure and above 40 bar absolute, preferably above 50 bar absolute. This level of pressure makes it possible to avoid the accumulation of CO2 in the last drop of vaporization of the exchange line.
• the dew point of the gas below the critical pressure is very low (typically below -90 ° C.).
• the injection of nitrogen into the gas to be treated so as to limit the oxygen concentration in the distillation column therefore solves the problem identified by the inventors of the present invention. Indeed, if the gas at equal oxygen concentration contains more nitrogen, the risk of concentration at the top of the column becomes lower because the oxygen is more diluted in nitrogen. A control system is therefore put in place.
• nitrogen concentration is less than t1, nitrogen is injected into the feed gas in order to obtain a mixture with a composition approaching or even exceeding t1 (typically the injection flow rate is controlled according to content in the mixture).

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• 2017
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  • 2018-12-17 US US16/954,790 patent/US20210087123A1/en not_active Abandoned
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