Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
  • B01D53/02—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
  • B01D53/047—Pressure swing adsorption
• • 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
  • B01D53/26—Drying gases or vapours
  • B01D53/261—Drying gases or vapours by adsorption
• • 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
  • B01D53/26—Drying gases or vapours
  • B01D53/265—Drying gases or vapours by refrigeration (condensation)
• • 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
  • B01D53/34—Chemical or biological purification of waste gases
  • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
  • B01D53/75—Multi-step processes
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
  • F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES 
  • F23J15/00—Arrangements of devices for treating smoke or fumes
  • F23J15/08—Arrangements of devices for treating smoke or fumes of heaters
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
  • B01D2253/10—Inorganic adsorbents
  • B01D2253/102—Carbon
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
  • B01D2253/10—Inorganic adsorbents
  • B01D2253/104—Alumina
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
  • B01D2253/10—Inorganic adsorbents
  • B01D2253/106—Silica or silicates
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
  • B01D2253/10—Inorganic adsorbents
  • B01D2253/106—Silica or silicates
  • B01D2253/108—Zeolites
• • 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
  • B01D2256/22—Carbon dioxide
• • 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
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
  • F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES 
  • F23J2219/00—Treatment devices
  • F23J2219/60—Sorption with dry devices, e.g. beds

Definitions

• the present invention relates to a method for producing a gas enriched with CO 2 from a feed gas comprising carbon dioxide (CO 2 ), at least one of H 2 , N 2 , CH 4 , CO , O 2 and argon, water vapor - optionally NOx and / or SOx- type impurities and a solids concentration of between 0.01 and 100 mg / m, characterized in that
• the feed is at least partially dried upstream of a PSA unit so as to prevent agglomeration of the solid particles in the PSA unit.
• a technology aims to capture CO 2 emitted during the combustion of carbonaceous fuels to transport it and / or to sequester it underground. It will be noted that the capture of CO 2 in a stream also containing nitrogen, oxygen, argon, hydrogen, methane and / or carbon monoxide leads to enrich this stream in these products.
• the depleted CO 2 stream can then be used in a nearby process or recycled in the process that produced it.
• the process for producing a gas enriched with CO 2 can therefore also be seen as a deballasting process for CO 2 of the gas to be treated.
• the CO 2 problem will lead to extracting at least some of the CO 2 contained in various gases from the industry.
• Several processes will be used to capture this CO 2 .
• One of the methods is adsorption.
• the CO 2 can be trapped at high temperature, that is to say above 150 ° C. or, on the contrary, around the ambient temperature, the gas containing the CO 2 then being rather at a temperature below 60 ° C.
• the adsorption unit may be of the PSA type.
• the PSA and VPSA units have already been extensively studied for different types of separation: production of high purity hydrogen, oxygen and / or nitrogen from air, methane from CH4 / CO2 mixture, CO from synthesis gas
• These PSA are constituted from well known elementary steps: adsorption (step adsorption), balancing steps, elution gas recovery (purge providing), depressurization (blow-down) Elution (purge), recompression (repressurization), pressure sweep (rinse).
• EP 1 004 343 describes a cycle developed initially for PSA H 2 with two levels of regeneration pressure at 4 adsorbers and a balancing
• EP 1 095 689 describes a two-adsorber cycle developed for the production of oxygen from air, a cycle comprising a recompression with the non-adsorbed gas, a balancing, a final recompression with the feed gas, a production step, a decompression step in part using a vacuum pump and an elution phase;
• No. 4,840,647 describes a cycle with two adsorbers or more particularly adapted to the capture of an easily adsorbable component such as CO 2 ;
• EP 1 023 934 describes a PSA H 2 type cycle with recycling of a portion of the low pressure waste gas to the gas to be treated;
• US Pat. No. 6,287,366 describes a VSA O 2 cycle illustrating the combined steps such as simultaneous depressurization by the two sides of the adsorber, repressurization with two distinct fluids, etc.
• a majority of the cycles described in the literature are directed towards the production of the the least adsorbable gases, the most adsorbable gases constituting the residual.
• This type of cycle can nevertheless be used for CO 2 capture.
• the PSA will for example be adjusted to the CO 2 content in the light gases. Indeed, produce at low pressure a fraction enriched in CO 2 is to produce at the adsorption pressure a fluid depleted in CO 2 .
• US 2007/0261551 relating to the CHVCO 2 separation gives, as an example, a PSA H 2 type cycle with a high pressure adsorption phase, 2 equilibrations, a co-current decompression with elution gas recovery, a final depressurization , a low pressure elution step with the previously recovered gas and product gas and a final recompression with the feed gas and product gas.
• This type of cycle can possibly be improved with the addition of more specific steps for the production of the most adsorbable gas, that is to say here the CO 2 .
• These additional steps are essentially steps for recycling part of the gas resulting from the decompression, recycling into the feed or directly into another adsorber.
• the recycling towards the food generally consists of taking the fraction (s) least rich in CO 2 from the gas of the PSA of the steps of decompressions in countercurrent or of elution (purge) in order to obtain a residual richer in CO2 .
• elution purge
• 4,077,779 describes a cycle with 4 or 6 adsorbers comprising the recycling of a portion of the decompression gas to carry out a recycling step in the feed or directly in another adsorber, as well as an elution step with a gas external to the feed.
• PSA elution step with a gas external to the feed.
• the literature also describes cycles for extracting CO from a synthesis gas. In this case, CO is the most easily adsorbable gas on an adsorbent that is specific to it. This type of cycle can be transposed directly to stopping CO 2 contained in essentially less adsorbable gases after adsorbents have been changed.
• CO 2 sequestration will be used primarily on units producing large flows of CO 2 -rich gas.
• waste gases from power plants producing carbonaceous fuels in particular oxyfuel combustion, cement gases, gases from iron and steel processes, or synthesis gases obtained by partial oxidation. or steam reforming of carbonaceous fuels.
• These gases have in common in addition to their CO 2 content to contain water vapor and dust.
• the amount of dust contained in the gas as well as the particle size distribution can be obtained by any of the known methods which are not developed here. Then, when we talk about particle size, expressed in microns, we will refer to the main dimension of the particle (length if it is an elongated cylindrical shape, diameter of the circumscribed sphere if it is a particle of essentially sheric or cubic form). The percentages given refer to the number of particles having a particle size smaller or larger than a specified value. It appeared that the fine residual dust - that is to say after filtration or any primary trapping - that in the absence of liquid water can pass without any particular problem the different equipment of the PSA unit, being easily transported by gas, agglomerates and settles when there is moisture.
• agglomerates may eventually cover the particles of adsorbents or at least clog their pores, plug the various instrumentation outlets, lodge in essential equipment including valves in particular. A loss of tightness of the latter causes a malfunction of the PSA, in particular a decrease of perfo nuances even a blockage of the system. It is the same if the adsorbent is partially damaged.
• the thermal effects may be less significant at the level of the adsorbent beds themselves due to less pressure effect than in a PSA but condensation is likely at the level of the vacuum pump since that we recompress the gas rich in CO 2 .
• the PSA N 2 , the PSA H 2 and the PSA supplying the air instrument directly treat a wet feed gas. This is also the case of PSAs producing CO2 and simultaneously hydrogen relatively close to the PSAs mentioned here. This can be found in Douglas Ruthven and Garlic, "Pressure Swing Adsorption" where it is taught that water is stopped by a first series of adsorbent beds.
• the washing techniques and the number of washing stages can be improved to get rid of all the residual dust or at least to obtain residual contents sufficiently low that even their agglomeration during one or more years in or on the equipment presents little inconvenience.
• a simple calculation of the quantities of dust entering the system leads to acceptable residual values of less than about ten micrograms per Nm 3 of gas to be treated, preferably of the order of one microgram per Nm. Both of these techniques can be used in series. Direct (investment) and indirect costs (pressure drop on gas, pumping energy, etc.) are very expensive.
• Another solution is to operate the adsorption unit at a sufficiently high temperature to remain in all circumstances beyond the condensation both in the adsorber and in the ancillary equipment.
• the adsorption capacity is too much reduced by raising the temperature and such units would not be efficient. Vacuum pumping of hot gas would also be very expensive in investment and energy.
• a problem that arises is to propose a process for producing a gas enriched in CO 2 implementing a PSA unit, in which the agglomeration of the solid particles within the PSA unit is reduced.
• a solution of the invention is a process for producing a gas enriched with CO 2 from a feed gas comprising from 10 to 75 mol% of carbon dioxide (CO 2 ), water vapor at least one constituent selected from hydrogen, CO, methane, nitrogen, oxygen, argon, and solid particles, implementing a unit PSA, characterized in that the feed gas is at least partially dried upstream of the PSA unit and enters said PSA unit with a solids concentration of between 0.01 and 100 mg / m.
• CO 2 carbon dioxide
• particles organic or inorganic constituents in the solid state under the conditions of pressure and temperature of the gas to be treated.
• These particles may be fragments of the base materials used in the upstream process and which have not reacted (for example coal dust) or driven reaction products ... They may contain metals, in particular heavy metals . It can be soot ... Generally, we talk about them "dust”.
• the process according to the invention may have one of the following characteristics: the feed gas also contains at least one impurity among the nitrogen oxides
• NOx including nitric oxide and nitrogen dioxide and sulfur oxides (SOx) including sulfur dioxide
• the concentration of solid particles of the feed gas entering said PSA unit is between 0.1 to 50 mg / m, preferably between 1 and 20 mg / m; the majority of the solid particles have a particle size of less than 20 microns, more generally less than 5 microns; by majority is meant at least 50% by number of solid particles;
• the feed gas is at least partially dried until a relative humidity of less than or equal to 50%, preferably less than 10%, is obtained;
• the feed gas is at least partially dried until a water content of less than 10 molar ppm, preferably less than lppm molar, is obtained;
• the feed gas is dried by passing through a TSA type adsorption unit;
• the adsorption unit of the TSA type comprises one or more adsorbents chosen from a type 3 A molecular sieve, undoped activated alumina and silica gel; the dried feed gas is compressed upstream of the PSA unit;
• the PSA unit has a first adsorbent layer chosen from activated aluminas, silica gels and activated carbon;
• the feed gas is compressed before being dried; said compression may be at least partially adiabatic type, that is to say that there is not systematically cooling the compressed gas at each compression stage.
• the compressed gas may be cooled and the condensed water is preferably separated from the stream fed to the dryer.
• the feed gas is a waste gas from a power generation plant from fuel, a cement gas, a synthesis gas or a gas from a steelmaking process.
• adsorbents that do not trap CO 2 , for example 3A sieve, undoped activated alumina or silica gel. It will be possible to regenerate at a pressure equal to or close to the adsorption pressure if necessary to avoid the effects of depressurization or desorption. It will also be possible, if necessary, to use thermal insulations internal or external to the adsorber to prevent thermal losses.
• This unit will be dimensioned so that there is no water condensation thereafter in the PSA unit CO 2 and if necessary in the treatment unit (s) complementary to the CO 2 rich stream from the PSA CO 2 , for example in compressors.
• a partial cold spot drying with a water exchanger / separator system may be sufficient to avoid the condensation of water in the PSA unit and / or the associated equipment. This will be the case, for example, for PSAs operating with limited pressure ratios (or pressure differences) between adsorption and regeneration, for example with an adsorption pressure of less than 10 bar absolute and a regeneration around atmospheric pressure.
• An adsorbent with capacity limited CO 2 adsorption, for example silica gel may be less likely to cause the appearance of cold point than a zeolitic adsorbent. Partial drying may also be sufficient if the CO 2 rich gas produced by the PSA is not recompressed and cooled below its saturation point in water.
• cold point drying it is called cold point drying to cool the gas to be treated with a temperature Tl, for example 40 ° C., to a substantially cooler temperature T2, for example 8 ° C., to eliminate the condensed water. and heating the gas to a temperature close to its initial temperature Tl, for example here 35 ° C or at least substantially greater than T2, for example up to 20 ° C.
• the equipment of the said dryer exchanger, water / gas separator
• groups of adsorbers for example groups of 2.3 or 4 adsorbers, which then operate in parallel.
• a PSA CO 2 cycle which would have 6 phases and could thus operate with 6 very large adsorbers would in practice consist of 12 or 18 small adsorbers.
• 2 groups of two adsorbers can for example be simultaneously in the adsorption phase.
• the PSA H 2 can operate in said degraded mode, that is to say with a reduced number of adsorbers, it is easy to develop for the CO 2 PSA degraded steps to operate in case of problems on one or more adsorbers (this is usually valve problems).
• the PSA CO 2 adsorbents will have to be adapted to this process. They will generally comprise several successive layers of adsorbents of different characteristics. The majority adsorbent will generally be silica gel (40 to 80% by volume).
• This adsorbent is as follows: Chemical composition: SiO 2 > 96% by weight, Al 2 O 3 ⁇ 4% by weight, specific surface area (BET): 550/775 m 2 / g, internal porous volume: 0.3 / 0.5 ml / g, Density in bulk bed: 550/800 kg / m.
• BASF Sorbead silica gel LE-32 recommended for this application in the commercial brochure and whose average characteristics are: Chemical composition: SiO 2 approx 99.5% wt, Al 2 O 3 approx 0.5% wt, Specific Surface (BET): 750 m 2 / g, Internal pore volume: 0.45 ml / g, Density in bulk bed: 600 kg / m 3 .
• BET Specific Surface
• the operating conditions and the desired performances in particular the content of CO 2 in the gas produced under pressure and the purity of the CO 2 in the off-gas, it will be used differently.
• adsorbents before and after the silica gel bed activated alumina and / or doped activated alumina, silica gel with properties different from those of the main bed such as silica gel made to withstand the presence of liquid water such as BASF Sorbead WS, activated charcoal (chemically or steam), that is to say characterized by a large pore volume (> 0.6 ml / g), a large average pore diameter (> 15 Angstrom) and / or low density ( ⁇ 450 kg / m 3 ).
• the upper layers may consist of a denser active carbon (density> 450 kg / m3) such as NORIT RB, and / or zeolite type A, Y or X (or LSX) such as the commercial products of UOP (NaY, HP 13X, APG, APG II, APG III ....), CECA (G5, G5DC, G5CO2M, G5CO2MLZ, G5CO2 LZ ...), ZEOCHEM (Z10-02, Z 10-02 ND, 7), GRACE DAVISON (Sylobead MS C ....), CWK etc.
• a denser active carbon density> 450 kg / m3
• zeolite type A, Y or X or LSX
• UOP NaY, HP 13X, APG, APG II, APG III ....
• CECA G5, G5DC, G5CO2M, G5CO2MLZ, G5CO2 LZ
• ZEOCHEM
• active carbon adsorbents of various and more or less activated origin, alumina, silica gel of varied porosity, optionally exchanged zeolites of type A, Y, X - commercially available can be defined through many other properties relating to their adsorption capacity of the different gases involved, their thermal ... and this under standard conditions or operating conditions .... It is not the purpose of this application to include here this type of data. It is the same for the kinetics of these adsorbents which can be defined by various measurements in the laboratory and then for example related to the cycle time of PSA CO 2 .
• the kinetics is controlled by the size of the adsorbent particles and those skilled in the art will adapt the diameter of the balls or the equivalent diameter of the particles to the process. retained. Generally, the equivalent diameter will be between 1 and 4mm.
• optimization parameters such as the choice of the duration of the steps, the choice of certain cutoff pressures (example: balancing end and start pressure). blow-down).
• These simulators can be coupled to an optimization engine that will modify a certain number of parameters left free (for example the processed flow rate, the intermediate pressure, the phase time .%) under different constraints (for example purity. ..) in order to optimize a parameter (the CO2 extraction efficiency for example) or a function (separation specific energy for example).
• a parameter the CO2 extraction efficiency for example
• a function separation specific energy for example
• the duration of the adsorption stage will generally be between 30 seconds and 3 minutes.
• the duration of an adsorption phase will then depend on the total number of adsorption phase of the envisaged cycle. For example a CO2 PSA having a phase time of 45 seconds and two successive stages of adsorption will have a total adsorption time of 90 seconds.
• Figure 1 depicts a simple method where the PSA CO 2 unit (11) directly produces a fraction sufficiently enriched in CO 2 to be compressed by the machine (12) and produce a fraction (4) directly usable.
• the gas to be treated (1) is dried in the TSA (10) and it is the dried fraction (2) that feeds the PSA.
• the fraction depleted in CO 2 from PSA (5) is used to regenerate TSA.
• the regeneration can be carried out with nitrogen available at the site or any other gas sufficiently dry and whose subsequent use is not compromised by the presence of water.
• the CO2 content in the gas to be treated will generally be quite high, for example between 40 and 75 mol%.
• the moisture of the feed gas will be trapped in the first layers of adsorbent and then end up in the rich fraction of CO 2 .
• FIG. 2 shows the addition of a cold box (13) for improving the CO 2 content before use (8).
• the waste of the cold box (7) is optionally recycled at the inlet of the PSA CO 2 .
• the purpose of the cold box is to preferentially condense CO 2 , the other gases present (among nitrogen, oxygen, argon, hydrogen, methane and carbon monoxide) being more "light" as carbon dioxide.
• the resulting liquid (or the corresponding gas flow if the CO 2 is vaporized) is then substantially richer in CO 2 than the fluid thus treated.
• the CO 2 content of the feed gas will generally be between 25 and 70 mol%.
• the previous remarks on particle deposition apply here as well.
• Figure 3 shows a variant of the process of Figure 1 in which the gas to be treated (1) must be compressed (17) before being dried (10).
• Final refrigeration (18) is provided with separation of the condensed water (21) in the gas / liquid separator (19).
• a washing system may be provided at the separator (19) and optionally refrigerant (18) or compressor (17).
• the condensation of water being controlled that is to say that we know that it happens in the exchanger, it is obviously possible to take effective countermeasures such as water injection, continuous or punctual. It will be understood that such solutions are not applicable when the deposits are carried out in the adsorbent or carpet large equipment surfaces (adsorber bottoms, valves ). It should also be noted that the cold point of a PSA depends on the operating conditions which can change quite regularly.
• the dryer is here regenerated by a fraction (9) of the dried feed gas (2). This gas can then be reinjected to the suction of the compressor, usually after cooling and condensation of the water present.
• the drying unit (10) may comprise two adsorbers including one in the adsorption phase and one in the regeneration phase (heating and cooling).
• adsorbent selected from activated aluminas, silica gels, activated carbon, zeolites, in particular a type 3A zeolite.
• the PSA unit (11) may also include several layers.
• the first layer or layers will consist of adsorbents taken from the group consisting of activated aluminas, silica gels and activated carbon.
• a next layer may include zeolites or MOFs (metal organic frame).
• the adsorption pressure of the TSA is preferably between 1.5 and 30 bar abs; and the pressure of the PSA unit (or VSA) is preferably between 1.3 and 30 bar abs.
• the dried gas can be optionally compressed before the PSA unit.
• the adsorbers of TSA and / or PSA may be cylindrical type vertical axis, horizontal axis or preferably the radial type when the flow rates to be treated will be large (eg greater than 150 000 Nm 3 / h).
• the TSA unit intended to dry the gas to be treated upstream of the PSA may, depending on the adsorbents used, intentionally or non-intentionally stop other constituents present in the type of gas treated. Indeed, it is known that gases from Combustion or metallurgy can indeed contain very many constituents in the form of traces.
• drying the feed gas upstream of the PSA unit can limit the use of stainless steel or expensive materials in favor of the use of ordinary carbon steel. Indeed, the condensation water saturated with CO 2 and / or NOx and SOx can be very corrosive. The presence of oxygen usually aggravates this corrosion phenomenon. The additional cost of the dryer will be at least partially offset by gains on the materials.

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