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Definitions

• the present invention relates to a process for the production of hydrogen with capture of CO 2 produced simultaneously.
• the hydrogen is supplied from reforming with hydrocarbon vapor, more particularly methane (SMR).
• SMR methane
• the reformed gas is usually sent to a “shift” reactor (Water gas shift reactor) to produce more hydrogen.
• the "water gas shift reaction” is a reaction between carbon monoxide and water to form carbon dioxide and water.
• the gas produced generally has the following characteristics:
• H 2 Temperature close to room temperature (after cooling), - Composition in molar percentage H 2 : between 60 and 80%; CO 2 : between 15 and 25%; CO: between 0.5 and 5%; CH4: between 3 and 7%; N 2 : between 0 and 6%, saturated with water,
• Such a gas is then usually sent directly to a PSA (Pressure Swing Adsorption) hydrogen to produce high purity hydrogen (99% to 99.9999 mol%).
• PSA Pressure Swing Adsorption
• the residual PSA contains all the CO 2 , the great majority of CH4 and CO, a large part of the N 2 and hydrogen in an amount depending on the PSA unit yield (from 75 to 90% depending on the desired efficiency). ).
• This residual, with the CO 2 content, is burned at the steam reforming furnace.
• the waste gas from this unit is vented after recovering some of the available heat.
• EP 0 341 879 B1 treats the PSA H 2 waste to extract the CO 2 via a PSA and a refrigeration.
• WO 2006/054008 also treats the PSA H 2 waste via a PSA and a cryogenic unit.
• US 5,026,406 discloses the production of two high purity fractions using a PSA.
• Example 2 corresponds in part to the problem that arises here.
• a fraction rich in CO 2 (99.7 mol%) and a fraction containing approximately 90 mol% of H 2 are obtained.
• this fraction will have to be treated in a second unit, for example PSA type PSA H 2 , to obtain an H 2 purity of 99%.
• the use of vacuum pumps and / or recycling is necessary to achieve the intended performance.
• the document FR2884304 describes an adsorption unit operating at a maximum pressure of 10 bar absolute, producing a gas enriched in CO 2 which is sent to a cryogenic unit which enriches this gas to a minimum of 80 mol%.
• the CO 2 depleted gas of the adsorption unit is expanded, after cooling or not, to provide the cooling capacity of the cryogenic unit.
• At least a portion of the CO 2 -cooled gas of the cryogenic unit is recycled to the PSA, after or without expansion.
• At least a portion of the low CO 2 gas of the cryogenic unit is used as fuel.
• Said adsorption unit may be a VSA, a VPSA or a PSA
• PSA as described in FR2884304 is effectively not suitable a priori when it is desired to extract CO 2 in a high pressure gas such as synthesis gas when it is also desired to recover as a priority the majority of one of the least adsorbable constituents.
• a high pressure gas such as synthesis gas
• a moderate partial pressure of the order of the bar
• the use of a high pressure does not contribute anything to the cessation of CO 2 but is unfavorable when it is desired to keep under pressure components such as hydrogen.
• This last component adsorbs very weakly, it is mainly present in the adsorber in the gas phases, whether it is the porous volumes of the adsorbent, the intergranular volume or dead volumes at the inlet and outlet. At a given volume, the loss of hydrogen is then proportional to the pressure. In such an application, it is normal to rather consider treating the PSA H 2 waste to sequester CO 2 knowing that it is a low-pressure flow, enriched in CO2 and depleted of hydrogen.
• WO 2006/054008 and EP 0 341 879 B1 are based on these considerations.
• a problem is to provide a process capable of economically producing hydrogen with CO2 capture and without significant loss of hydrogen.
• a solution of the invention is a process for producing hydrogen from a gaseous mixture 21 comprising hydrogen (H2), carbon dioxide (CO2), carbon monoxide (CO), methane ( CH4) and water (H2O), implementing a CO2 PSA unit 30, a cryogenic unit 40 and a PSA H2 unit 50, wherein: a) introducing said gaseous mixture 21 into a PSA unit CO 2 30, producing a fraction 32 enriched in CO 2 and a fraction 31 depleted in CO 2 ; b) introducing the fraction 32 rich in CO 2 into a cryogenic unit 40, producing a fraction 41 enriched in CO2 and a fraction 43 enriched in H2; c) the fraction 43 enriched in H2 is recycled upstream of the PSA H2 50 unit; and d) introducing the fraction 31 depleted in CO2 PSA unit H2 50, producing a stream 51 enriched with hydrogen and a waste gas 52.
• the process according to the invention may have one or more of the following characteristics: the fraction enriched in H2 represents more than 90% of the quantity of hydrogen contained in fraction 32 rich in CO2.
• step a) the fraction 32 enriched with CO2 is compressed at a pressure greater than the pressure of the gaseous mixture 21.
• the PSA CO2 comprises at least one adsorber with at least one adsorbent and in that said adsorber is subjected to a pressure cycle comprising a step of sweeping the adsorbent by a portion of the fraction 32 enriched in CO2 and compressed.
• fraction 32 enriched with CO2 is at least partially dried using a dryer 35.
• the gaseous mixture 21 is at least partially dried using a dryer 25.
• step a) the gaseous mixture 21 is at least partially dried using a dryer 25 and in step c) the following substeps are carried out: at least a part of the fraction enriched in H2 is reheated in a heater 44; said portion of the heated fraction 43 is used to regenerate the dryer or dryer 25, then said portion of the fraction 43 is recycled upstream of the PSA unit H2 50 after refrigeration and separation of the condensed water.
• step c) at least a portion of the fraction enriched in H2 is recycled upstream of the PSA CO 2 unit 30.
• the waste gas 52 is partly recycled upstream of the PSA H 2 50; PSA H 2 50 is regenerated at a pressure less than or equal to atmospheric pressure.
• the fraction 41 enriched in CO 2 comprises more than 90% CO 2 , preferably more than 97% CO 2 , more preferably more than 99% CO 2 .
• the fraction 41 enriched in CO2 is packaged in a bottle or tank or feeds a CO2 line for industrial use or storage in the basement, or is produced in liquid form.
• the subject of the invention is also an installation for producing hydrogen from a gaseous mixture 21 comprising hydrogen H 2, carbon dioxide C 2, carbon monoxide CO, methane CH 4 and water H 2 O , characterized in that said installation comprises a PSA CO 2 and PSA H 2 50 in series, the PSA CO 2 30 being upstream of the PSA H 2 50 and combined with a cryogenic unit 40.
• the installation may have at least one of the following characteristics:
• the PSA CO 2 comprises at least 5 adsorbers comprising at least silica gel as adsorbent; in each adsorber of the PSA CO 2 30, the silica gel represents at least 50% of the total volume of adsorbent and a zeolite of type A or X at most 25% of the total volume;
• the cryogenic unit comprises a stripping device of at least a portion of the fraction 32 of CO 2 , previously liquefied, to extract hydrogen, and generally incondensable, dissolved in said fraction.
• FIG. 1 represents an installation according to the invention with different options for recycling flows from the cryogenic unit.
• the natural gas (or, more generally, the hydrocarbons) 1 and the vapor 2 are introduced into the reforming unit 10.
• the reformed gas comprising hydrogen (H 2 ), carbon dioxide (CO 2 ), carbon dioxide carbon monoxide (CO), methane (CH4), optionally argon (Ar) and nitrogen (N 2 ), and water (H 2 O) is shifted in a shift reactor 20, wherein at least a portion of the carbon monoxide reacts with at least a portion of the water to form hydrogen and carbon dioxide.
• the gas thus reformed and shifted corresponds to the gaseous mixture 21.
• the gaseous mixture 21 feeds the PSA CO 2 30.
• the fluid 32 is the rich residue CO 2 of the PSA CO 2 30.
• This fluid is at low pressure, that is, to say at a pressure less than 3 bar abs, usually around atmospheric pressure. Being compressed to feed the cryogenic unit 40, this fluid could be found in slight depression (for example 0.9 bar abs) without departing from the teaching of the invention.
• the cryogenic unit 40 makes it possible on the one hand to supply the CO 2 at the required purity (41) for its use (sequestration, injection into oil or gas wells, chemistry, food, etc.) and secondly to recycle 43 the essential (more than 90%, pref over 95, preferably still more than 99%) of the hydrogen contained in the stream 32.
• the cryogenic unit 40 may optionally produce a methane-enriched stream 42 which will be recycled to unit 1 or used elsewhere. Fraction 43 enriched in H 2 can be recycled at various locations of unit 1:
• hydrogen - or if there is also a need for impure hydrogen - all or part of the hydrogen-enriched stream 43 may be used in another unit or mixed with the production. principal of hydrogen 51.
• a complementary treatment 60 for example permeation or catalysis (methanation ..), can be envisaged to adapt the purity of this flow to needs.
• the flows 46 and / or 48 may be mixed with the main feed streams, respectively 21 and 31 or constitute a second feed.
• Streams 47 and / or 49 may be used internally to the PSAs, for example to perform all or part of the purge or repressurization.
• this flow would be injected at the PSA other than as a main or secondary feed, at a pressure lower than the adsorption pressure, it is possible to insert a permeation unit to enrich part of the flow of hydrogen. .
• the fraction 31, produced by the PSA CO 2 30, is depleted in CO 2 and feeds the PSA H2 50.
• the waste 52 of the PSA H 2 can be recycled in total at the reformer 10, as a fuel and / or as a reagent 71 after compression in the compressor 70. It is also possible to recycle a portion of this waste at the PSA H 2 level. even, or even use all or part of this flow in an outdoor unit. These variants, which do not alter the spirit of the invention, are not shown in FIG.
• the process according to the invention uses a unit for capturing CO 2 by adsorption of PSA type, that is to say not using a vacuum regeneration, coupled to a cryogenic unit which allows both to obtain the required purity for the CO 2 and to recycle the majority of the hydrogen contained in the CO 2 fraction 32 from the PSA CO 2 30 to the reformed gas line.
• the hydrogen extracted at the level of the PSA CO 2 is reinjected into the high pressure circuit going from the feed of the SMR to the hydrogen production, that is to say at a pressure of about fifteen bars abs. at 40 bar maximum.
• Coupling with a cryogenic unit thus makes it possible to compensate for the average performance of the PSA (compared with a unit using vacuum regeneration) thanks to further purification of CO 2 and improved recycling of incondensables.
• Incondensable means H 2 , N 2 , CH 4, CO, Ar. It turns out that the modifications made to the cryogenic unit - as compared to a conventional unit for purification and production of CO 2 - such as the choice of a high operating pressure suitable for recycling, a partial re-boiling of the liquid CO 2 in order to expel the dissolved hydrogen, a partial expansion of the liquid CO 2 to recover the vapor fraction rich in incondensables ...
• cryogenic units associated with PSA making it possible to obtain the performance required both for capturing CO 2 and for recycling incondensables, more particularly hydrogen.
• the cryogenic unit will be supplied at a pressure greater than the pressure of the hydrogen production, in practice always greater than 15 bar abs and will preferably comprise a so-called "stripping" device of the hydrogen contained in the CO 2 - and more generally incondensable: N 2 , CH 4, CO, Ar-device involving a pressure drop and / or reheating and / or injection of gas in a liquefied fraction of CO 2 .
• Figure 2 corresponds to a preferred installation of the invention.
• the fraction 32 enriched in CO 2 and supplying the cryogenic unit 40 will be compressed via the compressor 34 at a pressure greater than the pressure of the gaseous mixture 21 so as to be able to recycle the hydrogen-rich gas 43 without any other compression means.
• this fluid rich in CO 2 from the PSA CO 2 containing water vapor, this fluid will be at least partially dried before or after compression and cooling (or at the outlet of an intermediate compression stage after cooling).
• the residual water content will be compatible with the proper functioning of the cryogenic unit, the correct use of the retained materials (corrosion) and the specification of CO2 purity.
• FIG. 2 for the sake of clarity, only the post-compression position 34 has been shown for said desiccation 35.
• the regeneration of said drying unit may be carried out with a fraction of the dried fluid 32, or with an external fluid such as nitrogen, or with the residue of the PSA H2 50, but preferably with all or part of the hydrogen-rich recycled fraction 43.
• the flow 43 may be cyclically heated in the exchanger 44 (electric, steam, heat recovery on a hot fluid) and then cooled in the exchanger 45 with evacuation of condensed water. This flow 46 is then reintroduced into the reformed gas.
• the dryer may be of any type, but preferably TSA type as indicated above.
• the adsorbers may be cylindrical type vertical axis, cylindrical horizontal axis or radial type for larger flow rates.
• the technology of the radial adsorbers may be that used for the overhead treatment in front of the cryogenic air separation units or that of the VSA 02.
• the waste 32 of the PSA CO2 can also feed a gasometer 33 or a buffer capacity before being compressed and then dried. This storage then has the double effect of homogenizing the composition of the waste and regulating its flow rate.
• the reformed and shifted gas 21 is mixed with the gas 46 enriched in H2 and derived from the cryogenic unit which contains all the hydrogen contained in the CO2-rich fraction (32), CO2 - as a function of the thermodynamic equilibria achieved in the Cryonic methane unit, carbon monoxide and possibly nitrogen and argon. These levels depend essentially on the required purity for CO 2 .
• the fraction 31 depleted in CO 2 , resulting from PSA CO 2 30 has a residual CO 2 content generally in the range from 0.5 to 7.5 mol%, more generally from 1.5 to 3.5%.
• PSA H 2 50 purifies said gas with CO 2 , CH 4 , CO, N 2 ... and produces pure hydrogen 51, that is to say with a purity greater than 98% and generally between 99 and 99.9999%.
• the PSA H 2 low pressure waste stream 52 is generally used as a fuel (SMR furnace) and / or as a feedstock of the SMR after compression.
• this recycling can be mixed with the main feed (31) or constitute a second feed.
• PSA CO 2 as a means of drying the reformed gas before supplying PSA H 2 is one of the advantages of this process. Since the waste 52 of PSA H 2 is dry, it is possible to envisage, at reduced costs, improving the performance of said PSA not only via recycling as described above but also by lowering the pressure of this waste. In fact, in the case of a conventional PSA H 2 , the PSA waste is sent to the furnace burners of the SMR. The adjustment means and the pressure drops in the pipes and accessories make the low pressure of the PSA cycle is of the order of
• the cryogenic unit is conventional, of the partial condensation type as used for the production of liquid CO 2 for industrial or food use.
• a first example is given in EP 0341 879 B1.
• a more complex example is shown in FIG. 6 of document FR 2 884 304.
• document WO 2006/054008 describes variations of cryogenic unit.
• the unit may comprise a device enabling to extract the dissolved hydrogen in the liquid CO 2 in order to make the losses negligible. This device may consist in partially boiling off liquid CO 2 , the light constituents then being preferentially in the gas phase.
• This cryogenic unit will therefore be characterized by its operating pressure greater than or equal to the pressure of the shifted gas, that is to say in practice always greater than 15 bar abs and by a recycling in hydrogen greater than 90%, preferably greater than 95. %, still more preferably equal to or greater than 99% of the hydrogen contained in the waste 32 of the PSA CO2.
• the HP 43 recycle containing hydrogen is used to regenerate the dryer after passing through the heater 44 to provide the water desorbing energy. This fluid is then cooled 45 for removal of the condensed water and injection into the main stream 21.
• the PSA CO2 30 can operate in a PSA H 2 type cycle.
• the PSA CO 2 30 comprises at least two equilibria, preferably still 3 or 4 equilibrations, and is capable of producing under pressure a hydrogen-rich gas containing from 0.5 to 7.5% CO 2 , preferably from 1.5 to 3.5 mol% CO 2 , 0.5 to 7% CO, 3 to 10% CH 4 , 0 to 10% N 2 .
• This gas is essentially dry, that is to say it contains on average less than 1 ppm of water.
• the waste gas 32 produced at low pressure is rich in CO 2 (from 80 to 95 mol%), the remainder consisting of H 2 , CO, CH 4 , optionally nitrogen. This gas also contains water vapor.
• the overall extraction rate of CO 2 is in a range of approximately 70 to 98%, preferably around 85 to 90%.
• phase times will generally be between 20 and 120 seconds depending on the number of adsorbers used. It is recalled that the cycle time corresponds to the time T that an adsorber returns to a given state and that for a cycle with N adsorbers, the phase time is by definition equal to TYN.
• a cycle 10-3-4 will be described, which is, according to the conventionally accepted terminology, a PSA type adsorption cycle involving 10 identical adsorbers each in a cycle comprising 3 production phases and 4 balancing.
• Such a cycle can be represented according to the table below:
• Such a table means, on the one hand, that a given adsorber will chronologically follow all the steps starting from the upper left box to the lower right box and that on the other hand, at a given moment, the adsorbers will be found. in a state corresponding to a column.
• a line corresponds to a phase as defined previously. We see that each phase has several stages that correspond to special times in the control system (switching from one step to another usually involves at least one valve movement for the PSA). More particularly, the 10-3-4 cycle described herein thus comprises:
• a phase of "purge providing” that is to say producing a fraction rich in hydrogen and light component (CO, CH 4 , N 2 ) which serves as elution gas for an adsorber then in low pressure
• Such a step makes it possible to partially purge the adsorber of the hydrogen that it contains making it possible to obtain a residue that is richer in CO 2 .
• Such a step is integrated in the cycle during the depressurization and before the "Blow Down" stage. The performance improvement thus obtained is to be compared with the greater complexity of the PSA CO 2 .
• adsorbents having a compromise between the adsorption capacity and the desorption facility will have to be used since the vacuum is not used for desorption purposes.
• the use of X or A type zeolites, widely recommended for this application should be proscribed or at least limited, preferably as a final layer at the outlet of the adsorber, where the CO 2 content is reduced.
• this layer of zeolite A or X will represent less than 25% of the total volume adsorbent.
• silica gel for example the product manufactured by BASF under the reference LE 32.
• activated alumina from 5 to 25% of the total volume adsorbent
• activated carbon from 5 to 20%
• Some molecular sieves (NaY ..) having a limited affinity with CO 2 may be used to optimize performance depending on the objective of extraction of CO 2 retained.
• Recently synthesized adsorbents such as MOFs (Metal Organic Frame) also correspond to the criteria of choice.
• the geometry of the adsorbers, PSA CO 2 30, can be of varied type. Vertical cylindrical adsorbers will preferably be used for small flow rates, up to a few thousand or tens of thousands of Nm3 / h of feedstock flow, then horizontal axis cylindrical adsorbers or radial adsorbers for larger flow rates.
• the technology of the radial adsorbers may be that used for the overhead treatment in front of the cryogenic air separation units or that of the VSA 02.
• the PSA H 2 50 is a conventional PSA H 2 with distribution of the adsorbents adapted to the composition of the food. It may comprise a particular preprogrammed cycle in the event of a change in composition, for example related to the decommissioning of the CO 2 PSA.
• cycles will be used comprising several adsorbers, generally 8 and more.
• the extraction yield of hydrogen may be of the order of 90%, of the order of 92% with booster on the waste going to the burners, of the order of 92 to 95% with recycling.
• a variant shown in FIG. 3 consists of drying the synthesis gas in a unit 25 after the shift unit 20 and before the CO 2 PSA 30. This makes it possible to eliminate the dryer 35.
• the interest of such a unit 25 is that it allows the use of standard materials downstream, particularly at the PSA CO 2 , the compressor 34 (see Fig 2).
• Such a dryer 25 also makes it possible to avoid any water / CO 2 interferences at the level of the adsorbents of the PSA CO 2 and thus to facilitate the stopping of CO 2 .
• the unit 25 must process all the flow of synthesis gas.
• the choice of the basic solution or of said variant will depend on operating conditions, local economic conditions ... This choice is part of the optimization work of the person skilled in the art.
• Figure 3 shows variant in which the desiccation 25 is TSA type and is regenerated under pressure by the cyclically heated stream 43 in the exchanger 44 (up to a temperature of the order of 100 to 250 0 C) and after desorption of water retained in 25, cooled in the exchanger 45 where the condensed water is removed. The resulting stream 46 is then re-injected upstream of desiccation 25.

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