WO2023242717A1 - Pressure swing adsorption device, system and method for purifying a compound of interest - Google Patents

Pressure swing adsorption device, system and method for purifying a compound of interest Download PDF

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Publication number
WO2023242717A1
WO2023242717A1 PCT/IB2023/056055 IB2023056055W WO2023242717A1 WO 2023242717 A1 WO2023242717 A1 WO 2023242717A1 IB 2023056055 W IB2023056055 W IB 2023056055W WO 2023242717 A1 WO2023242717 A1 WO 2023242717A1
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Prior art keywords
pressure
column device
kpa
further characterized
module
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PCT/IB2023/056055
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Spanish (es)
French (fr)
Inventor
Fernando Esau BASILIO OCAMPO
Jesse Yoe RUMBO MORALES
Felipe de Jesús SORCIA VÁZQUEZ
Gerardo ORTIZ TORRES
Omar Ricardo FONSECA CERVANTES
Alexis Ubaldo SALAS VILLALOBOS
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Universidad De Guadalajara
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Publication of WO2023242717A1 publication Critical patent/WO2023242717A1/en

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    • 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
    • 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
    • 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
    • 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
    • B01D53/02—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
    • B01D53/053—Pressure swing adsorption with storage or buffer vessel

Definitions

  • the present invention is related to systems for the purification of compounds, more particularly it is related to a pressure swing adsorption device, system and method for the purification of a compound of interest.
  • Pressure swing adsorption is a widely known separation process for the separation and purification of gas streams containing undesirable component concentrations.
  • the method has been developed and adapted for a wide range of feed gases, operating conditions, purity and product recovery.
  • Many pressure swing adsorption systems use two or more adsorbent columns operating in a cyclic sequence to maintain a constant product flow rate while the selected beds undergo several stages including: adsorption, depressurization, evacuation, purging, equalization pressure, repressure and other related stages.
  • multiple columns using numerous process steps are required to achieve high purity and/or recovery of valuable gaseous products such as hydrogens, carbon oxides, synthesis gases, light hydrocarbons and the like.
  • Multiple adsorbent columns using these process steps are also used to recover oxygen from air for various applications, including Portable medical oxygen concentrators recently popularized by the COVID-19 pandemic.
  • EP1029577B1 and EP1838418A4 describe pressure swing adsorption columns that exhibit in their configuration temperature sensors attached to their side walls for the purpose of detecting the temperature of the adsorbent within a selected portion of the column.
  • this configuration could be a solution, there is a problem that limits its applicability and that is that the sensors are fixed to the walls of the column, which can mean that once their useful life is over, the exchange of sensors is difficult. .
  • it cannot be ensured that the measured temperature is real since none of these sensors are located within the column where the purification process is being carried out.
  • a first aspect of the present invention refers to a pressure swing adsorption column device for the purification of a compound of interest, which comprises: an interior section; an outer section; a plurality of interchangeable temperature sensors; a lower section; and an upper section, wherein the interior section includes an interior wall that defines an interior diameter between 0.28 m and 0.32 m, the interior section comprises a plurality of interior housings for temperature sensors and is configured to allow the passage of the compound of interest, and for housing at least one interchangeable temperature sensor, wherein the outer section comprises a plurality of outer temperature sensor housings that is aligned with the plurality of inner temperature sensor housings and is configured to house each temperature sensor.
  • the plurality of interchangeable temperature sensors is configured to assemble with the plurality of exterior and interior housings and to measure the temperature at a center of the interior section, wherein the bottom section is configured to receive a vacuum inlet and a feed inlet, wherein the upper section is configured to recirculate and extract a purified product; and where the adsorption column device defines a height between 0.8 m and 1.5 m.
  • a second aspect of the present invention considers a pressure swing adsorption system, comprising: a) at least two swing adsorption column devices like the device described above; b) a plurality of valves and pipes that are connected to each column device, to at least one vacuum module, to a feed module and to a condenser module, and are configured to regulate the flow passing through each valve; c) at least one vacuum module that is connected to each column device through the plurality of valves and pipes, and is configured to generate a vacuum in the interior section of each device; d) a data acquisition module, which is connected to each sensor of the plurality of interchangeable temperature sensors and to at least one pressure gauge that measures the pressure in the interior section of each device; e) a power module that is connected to each device through the plurality of valves and pipes, and is configured to feed water vapor to the interior section of each device; and f) a condenser module that is connected to each device by the plurality of valves and pipes and is configured to receive a
  • a third aspect of the present invention considers a method to purify a compound of interest, which comprises the steps of:
  • Figure 1 illustrates a front perspective view of the pressure swing adsorption column device, in accordance with a first embodiment of the present invention.
  • Figure 2 illustrates a stainless steel mesh placed next to a lower flange of the pressure swing adsorption column device for the retention and packing of the adsorbent material, in accordance with a first embodiment of the present invention.
  • FIG.3 illustrates a diagram of the pressure swing adsorption system for the purification of a compound of interest, in accordance with a second embodiment of the present invention.
  • Figure 4 illustrates an example of the pressure swing adsorption system for the purification of bioethanol, in accordance with a second embodiment of the present invention.
  • Figure 5 illustrates the temperature profiles along the 1 m column.
  • FIG.6 Figure 6 illustrates the purity profiles from the start of the process until reaching the cyclic stable state.
  • Figure 7 illustrates the temperature profile along the column during 1 cycle of the process.
  • Figure 8 illustrates the pressure profile along the column during 1 cycle of the process.
  • the present invention involves improvements based on the pressure swing adsorption gas separation technology mentioned above, that is, in this invention almost no effective gas is lost and, furthermore, this invention does not need the complicated installations of vacuum under a suitable adsorption pressure. Therefore, the cost of equipment and energy consumption will be greatly reduced.
  • the present invention relates first of all to a pressure swing adsorption column device for the purification of a compound of interest, comprising: an inner section; an outer section; a plurality of interchangeable temperature sensors; a lower section; and an upper section, wherein the interior section includes an interior wall that defines an interior diameter between 0.28 m and 0.32 m, the interior section comprises a plurality of interior housings for temperature sensors and is configured to allow the passage of the compound of interest, and for housing at least one interchangeable temperature sensor, wherein the outer section comprises a plurality of outer temperature sensor housings that is aligned with the plurality of inner temperature sensor housings and is configured to house each temperature sensor.
  • the adsorption column device defines a height between 0.8 m and 1.5 m.
  • the adsorbent is natural or synthetic zeolite. More preferably, the zeolite is natural.
  • the upper section of the column device comprises an extraction output, an analog connection, and a digital connection; wherein the extraction outlet is configured to extract a purified product, wherein the analog connection is configured to connect to an analog pressure gauge to measure the pressure in the inner section, and wherein the digital connection is configured to connect to a digital sensor pressure sensor that sends data to a data acquisition module.
  • the lower section of the pressure swing adsorption column device additionally comprises a stainless steel mesh that is placed in a lower flange that is located in the lower section of the column device. Pressure swing adsorption, the stainless steel mesh is configured for retention and packing of the adsorbent material.
  • a second aspect of the present invention considers a pressure swing adsorption system, comprising: a) at least two swing adsorption column devices like the device described above; b) a plurality of valves and pipes that are connected to each column device, to at least one vacuum module, to a feed module and to a condenser module, and are configured to regulate the flow passing through each valve; c) at least one vacuum module that is connected to each column device through the plurality of valves and pipes, and is configured to generate a vacuum in the interior section of each device; d) a data acquisition module, comprising: a computing system and a PLC control system, the data acquisition module is connected with each sensor of the plurality of interchangeable temperature sensors and with at least one pressure gauge that measures the pressure in the interior section of each device; e) a power module that is connected to each device through the plurality of valves and pipes, and is configured to feed water vapor to the interior section of each device; and f) a condenser module that is connected to
  • the power module is a compressor or a boiler.
  • the vacuum module is a vacuum pump.
  • the capacitor module is a capacitor.
  • the data acquisition module comprises: a computing system and a PLC control system, wherein the data acquisition module is additionally connected to the plurality of valves and pipes, with the vacuum module, with the power module and with the condenser module and is configured to control the operation of each.
  • the plurality of valves and pipes comprises: an upper plurality of valves and pipes that is connected to the condenser module; and a plurality of lower valves and pipes that are connected to the vacuum module and the power module.
  • a third aspect of the present invention considers a method to purify a compound of interest, which comprises the steps of:
  • (v) repressurize the column device.
  • the flow of the compound of interest is supplied by a 175 psi compressor.
  • the compound of interest is bioethanol with 99% purity
  • the bioethanol purification conditions are the following in each of the steps of the method: (i) supply a mixture of 90% (w/w) bioethanol and 10% (w/w) water to the adsorption column device by pressure oscillation; (i) adsorb at a pressure >400 kPa and a temperature >373.15 K; (iii) depressurize the column device by decreasing the pressure to at least 50 kPa; (iv) purge the column device by decreasing the pressure from 50 kPa to 10 kPa; and (v) repressurize the column device by increasing the pressure from 10 kPa to 400 kPa.
  • the compound of interest is hydrogen with 99.9% purity
  • the hydrogen purification conditions are the following in each of the stages of the method: (i) supply a mixture that comprises: H2 at 72.2% (w/w), CH4 at 4.17% (w/w), CO at 2.03 % (w/w) and CO2 at 21.6% (w/w) to the pressure swing adsorption column device; (i) adsorb at a pressure >350 kPa and a temperature >295 K; (iii) depressurize the column device by decreasing the pressure to at least 50 kPa; (iv) purge the column device by decreasing the pressure from 50 kPa to 10 kPa; and (v) repressurize the column device by increasing the pressure from 10 kPa to 400 kPa.
  • the compound of interest is oxygen with a purity of between 95% and 99.5%;
  • the oxygen purification conditions are the following in each of the stages of the method: (i) supply a mixture that comprises: nitrogen at 74.18% (w/w), oxygen at 19.61% (w/w), carbon dioxide at 0.03% (w/w) and water vapor at 6.18% (w/w) to the pressure swing adsorption column device; (i) adsorb at a pressure >350 kPa and a temperature >298.15 K; (iii) depressurize the column device by decreasing the pressure to at least 50 kPa; (iv) purge the column device by decreasing the pressure from 50 kPa to 10 kPa; and (v) repressurize the column device by increasing the pressure from 10 kPa to 400 kPa.
  • the compound of interest is methane with a purity of between 95% and 99%;
  • the methane purification conditions are the following in each one of the steps of the method: (i) supply a mixture comprising: methane in a concentration of between 50 and 75% (w/w) and carbon dioxide in a concentration of between 25 and 45% (w/w) to the pressure swing adsorption column device; (i) adsorb at a pressure >1200 KPa and a temperature between 298 and 323 K; (iii) depressurize the column device by decreasing the pressure to at least 50 Kpa; (iv) purge the column device by decreasing the pressure from 50 kPa to 10 kPa; and (v) repressurize the column device by increasing the pressure from 10 kPa to 400 kPa.
  • FIG. 1 illustrates a pressure swing adsorption column device 1000 for the purification of a compound of interest, comprising: an inner section 1100; an outer section 1 120; a plurality of interchangeable temperature sensors 1 1 10; a lower section 1200; and an upper section 1300, wherein the interior section includes an interior wall that defines an interior diameter, the interior section comprises a plurality of interior housings for temperature sensors and is configured to allow the passage of the compound of interest, and to house each temperature sensor of the plurality of interchangeable temperature sensors 1 1 10, wherein the outer section 1 120 comprises a plurality of outer housings for temperature sensors that is aligned with the plurality of inner housings for temperature sensors and is configured to accommodate each temperature sensor of the plurality of interchangeable temperature sensors 11 10, wherein the plurality of interchangeable temperature sensors 11 10 is configured to be assembled with the plurality of exterior and interior housings and to measure the temperature at a center of the inner section, wherein the lower section 1200 is configured to receive a vacuum inlet 1220 and a feed
  • Figure 1 illustrates the upper section 1300 of the column device 1000 comprising an extraction output 1320, an analog connection 1310, and a digital connection 1330; wherein the extraction output 1320 is configured to extract a purified product, wherein the analog connection 1310 is configured to connect to an analog pressure gauge to measuring the pressure in the inner section 1 100, and wherein the digital connection 1330 is configured to connect with a digital pressure sensor that sends data to a data acquisition module (not shown).
  • Figure 2 illustrates a stainless steel mesh 1240 that is placed in a lower flange 1230 that is located in the lower section 1200 of the pressure swing adsorption column device, the stainless steel mesh 1240 It is configured for the retention and packaging of the adsorbent material, in accordance with a first embodiment of the present invention.
  • Figure 3 illustrates a pressure swing adsorption system for the purification of a compound of interest 2000, comprising: a) at least two swing adsorption column devices 1000 and 1000', b) a plurality of valves and pipes 2300 that are connected with each column device 1000,1000', with at least one vacuum module 4000, with a power module 3000 and with a condenser module 6000, and are configured to regulate the flow passing through each valve; c) at least one vacuum module 4000 that is connected to each column device through the plurality of valves and pipes 2300, and is configured to generate a vacuum in the interior section of each column device 1000, 1000'; d) a data acquisition module 5000, comprising: a computing system and a PLC control system, the data acquisition module 5000 is connected to each sensor of the plurality of interchangeable temperature sensors and with at least one manometer measuring the pressure in the interior section of each column device 1000, 1000'; e) a feed module 3000 that is connected to each column device 1000,
  • Figure 3 illustrates that the data acquisition module 5000 is additionally connected with the plurality of valves and pipes 2300, with the vacuum module 4000, with the power module 3000 and with the capacitor 6000 and is configured to control the operation of each one. Additionally, Figure 3 illustrates that the plurality of valves and pipes 2300 comprises: an upper plurality of valves and pipes 2310 that is connected to the condenser module 6000; and a plurality of lower valves and pipes 2320 that is connected to the vacuum module 4000 and to the power module 3000.
  • the column device 1000 comprises: an interior section 1100; an outer section 1 120; a plurality of interchangeable temperature sensors 1 1 10; a lower section 1200; and an upper section 1300, wherein the interior section includes an interior wall that defines an interior diameter, the interior section comprises a plurality of interior housings for temperature sensors and is configured to allow the passage of the compound of interest, and to house each temperature sensor of the plurality of interchangeable temperature sensors 1 110, wherein the outer section 1120 comprises a plurality of outer housings for temperature sensors that is aligned with the plurality of inner housings for temperature sensors and is configured to house each temperature sensor of the plurality of interchangeable temperature sensors 11 10, wherein the plurality of interchangeable temperature sensors 1 1 10 is configured to be assembled with the plurality of exterior and interior housings and to measure the temperature at a center of
  • Figure 1 illustrates the upper section 1300 of the column device 1000 comprising a draw output 1320, an analog connection 1310, and a digital connection 1330; wherein the extraction outlet 1320 is configured to extract a purified product, wherein the analog connection 1310 is configured to connect to an analog pressure gauge to measure the pressure in the inner section 1 100, and wherein the digital connection 1330 is configured to connect with a digital pressure sensor that sends data to a data acquisition module (not shown).
  • the second column device 1000' comprises the same elements as the column device 1000' indicated by the numbers 1110', 1210', 1220', 1310', 1320', and 1330' for the purification of a compound of interest in a form keep going.
  • the adsorbent used for packaging had a pretreatment that included the steps of: (i) filtering the adsorbent to eliminate impurities; (i) heat the adsorbents to a temperature of 250 °C for 150 minutes; (iii) heat a 0.1 N acid solution to its boiling point; (iv) mix the previously heated adsorbent with the boiling acid solution until completely dissolved; (v) cool the mixture to room temperature and decant the acid solution: (vi) wash the adsorbent with distilled water until all residues of the acid solution are removed; (vii) heating the adsorbent at a temperature of 250 °C for 5 hours; and (viii) cool the adsorbent to room temperature, measure the mass and repeat step (vii) until the mass is constant. Natural zeolite was used as adsorbent.
  • Valve 2321 receives the main feed from a steam boiler with a mixture of 90 wt% ethanol and 10 wt% of water. Valve 2321 is fully open (it is a digital on/off valve); Valve 2327 receives part of the feed from valve 2321.
  • This valve 2327 is proportional (analog) and has an opening of 70%, since this will allow supersaturated steam to be introduced and maintain a high pressure;
  • the 2312 valve is proportional (analog) and has a 30% opening.
  • This valve 2312 is located at the top to obtain the purified product obtained from the first column device 1000. The reason why it has a 30% opening is because it will allow the first column device 1000 not to depressurize and remain a high pressure to continue producing pure ethanol (bioethanol);
  • the valve 2314 is digital and is fully open (on/off), it receives the purified product from the first and second column devices 1000 and 1000', and sends the purified product directly to a condenser since the purified product is at high pressure and must be obtained in liquid form.
  • Valve 2323 is fully open and is a digital on/off valve, allowing the second column device to depressurize from the bottom in order to remove the water easily both in the liquid phase and the release of the zeolite active sites;
  • the valve 2324 is proportional (analog), and has an opening of 90%, this opening allows a depressurization considered to be carried out to reach 0.5 bar close to the purge pressure, this valve 2324 is located in such a way that it can be used for the first and second column devices 1000 and 1000' in the depressurization step, high concentrations of water come out of this valve (2324), this water can be reused to be introduced again into the boiler and exit in the vapor phase.
  • Valves 2321, 2326, 2312 and 2327 are enabled to perform adsorption and production using the first column device 1000', while the second column device 1000' performs the purge step by enabling valves 2323, 2325, 2324 and 2313. These steps are They have been in the same period of time for 20 seconds: Valve 2321 receives the main feed from the steam boiler with a mixture of 90% by weight of ethanol and 10% by weight of water; valve 2321 is fully open (it is a digital on/off valve); Valve 2327 receives part of the power from valve 2321.
  • This valve 2327 is proportional (analog) and has an opening of 70%, since it will allow supersaturated steam to be introduced and maintain a high pressure;
  • the valve 2312 is proportional (analog) and has a 30% opening, this valve is located at the top to obtain the purified product obtained from the first column device 1000.
  • the reason why this valve 2312 has a 30% opening % is because it will allow the first column device not to depressurize and maintain a high pressure to continue producing pure ethanol (bioethanol);
  • the 2314 valve is digital and is fully open (on/off). It receives the purified product from the first and second column devices 1000 and 1000', and sends the purified product directly to a condenser since the purified product is under high pressure and must be obtained in liquid form.
  • Valve 231 1 is proportional (analog) and has an opening of 5%, through this valve a flow passes that share the first column device 1000 towards the second column device 1000', is a purified product that carries high ethanol concentrations compared to the feed composition (90% ethanol and 20% water).
  • valve 2323 is fully open and is a digital on/off valve.
  • valve 2324 is proportional (analog), and has an opening of 25%, this opening allows a purge to be carried out with a small flow but at a high pressure, this allows all the active sites of the zeolites to be released and the second column device is regenerated 1000' and ready for the represumption step. This step is reached at a vacuum pressure of 0.25 bar. Valve 2324 is located so that it can be used for the first and second column devices 1000 and 1000' in the purge step.
  • valve 2324 High concentrations of water come out of this valve 2324, this water can be reused to be introduced into the boiler again and come out in the vapor phase;
  • the valve 2325 is completely open (it is a digital on/off valve), in this valve 2325 it is connected to a vacuum pump, which allows the vacuum to be generated that breaks the weak bond that has formed between the zeolite and the water molecule; valve 2325 is positioned that way to suck in only the water vapor and does not obstruct by gravity the liquid water passing through valve 2324.
  • Valves 2321, 2326, 2312 and 2327 are enabled to perform adsorption and production using the first column device 1000, while the second column device 1000' performs the purge step by enabling valve 231 1. These steps are carried out in the same period of time for 50 seconds. Below, the valve configuration is observed for 50 seconds in the adsorption step for the first column device 1000: Valve 2321 receives the main feed from the steam boiler with a mixture of 90% by weight of ethanol and 10% by weight of water. Valve 2321 is fully open (it is a digital on/off valve); Valve 2327 receives part of the power from valve 2321.
  • This valve is proportional (analog) and has an opening of 70%, since this will allow supersaturated steam to be introduced and maintain a high pressure;
  • the 2312 valve is proportional (analog) and has a 5% opening. This valve is located at the top to obtain the purified product obtained from the first column device 1000. The reason why it has a 5% opening is because it will allow the first column device 1000 not to depressurize and can be made equalizing pressures in the first and second column devices 1000, 1000', passing through the valve 231 1 and maintaining high pressure to continue producing pure ethanol (bioethanol);
  • the 2327 valve is digital and is fully open (on/off).
  • Valve 231 1 is proportional (analog) and has a 50% opening, this will allow more gas flow to enter towards the second column device 1000' and in turn the first column device 1000 continues to produce bioethanol, but with a lower production, this due to the reduction of the valve to 5%.
  • Valves 2312 and 2327 are enabled to perform adsorption and production using the first column device 1000, while the second column device 1000' performs the purge step by enabling valves 2321 and 2322. These steps are carried out in the same period of time. time for 80 seconds.
  • Valve 2312 is proportional (analog) and has a 30% opening. This valve 2312 is located at the top to obtain the purified product obtained from the first column device 1000. Again, valve 2321 has a 30% opening, in the first column device 1000 there is no longer a feed, only the valves are left open.
  • Valve 231 1 is digital and is fully open (on/off). It receives the purified product from the first and second column devices 1000, 1000', and sends the product purified directly to a condenser since the purified product is under high pressure and must be obtained in liquid form.
  • Valve 2321 receives the main feed from the steam boiler with a mixture of 90% by weight of ethanol and 10 % by weight of water, valve 2321 is fully open (it is a digital on/off valve); Valve 2322 receives part of the feed from valve 2321, valve 2322 is proportional (analog) and has an opening of 70%, since it will allow supersaturated steam to be introduced and maintain a high pressure. This valve 2322 allows the flow of steam that will enter the second column device 1000' until a high pressure of 4 bar is reached.
  • the composition of the bioethanol and water mixture must be close to the azeotropic point, giving as a mole fraction: 0.78 in bioethanol (90% by weight of bioethanol) and 0.22 in water (10% by weight of water).
  • the feed pressure must be at 200 kPa or above that value, in order to carry out the adsorption step on the water molecules and produce bioethanol.
  • the temperature must be at 373.15 K (100°C) or above that value, this to continue maintaining the vapor in the internal part of the column devices packed with zeolites and favor the regeneration steps of the zeolites and be able to be used again in the adsorption step.
  • FIG. 5 illustrates the temperature profiles from the start of the process until reaching a cyclic stable state. It can be seen that in node 1 (equivalent to 0.15 m) initial part of the column device, the temperature is maintained stable and at node 20 (equivalent to 1 m) the temperature decreases, this is because the steam flow enters through the first nodes of the column device, there being a decrease temperature along the axial part. It is characterized by the fact that the cyclic stable state is met after 2 h.
  • Figure 6 illustrates the purity profiles of bioethanol and water in mole fraction, where it is possible to observe how the purity of bioethanol was achieved after 2 h, with a molar composition of feeding 0.78 bioethanol and 0.22 water, until achieving a bioethanol purity of 0.985 bioethanol and 0.015 water. It is worth mentioning that two different results are shown since one test is with nominal starting values and the second test was based on the results obtained, considering optimal values that improve purity from lower compositions.
  • Figure 7 illustrates the temperature profile along the column device during 1 cycle of the process, showing how the temperature is maintained and decreased by oscillatory pressure changes.
  • Figure 8 illustrates the dynamic behavior of the internal pressure profile in the column device, when performing adsorption with a pressure of 2 bar, depressurization until reaching a pressure of 0.5 bar, which is close to vacuum. , subsequently a purge carried out with a pressure of 0.2 bar and finally a repressure that goes from 0.2 bar to 2 bar, this complies with one cycle of the process.
  • This profile is cyclic, therefore, it will be presented again until the cyclic stable state is reached and the bioethanol purity of 0.985 in mole fraction is reached, with the aim of complying with international purity standards to be able to be used as fuel.

Abstract

The present invention relates to a pressure swing adsorption device, system and method for purifying a compound of interest, said invention enabling a higher purity to be obtained in a shorter period of time, providing a device for purifying a compound of interest with temperature sensors that are easily interchangeable and coupled along the body of the column, and providing a versatile pressure swing adsorption system for purifying a compound of interest.

Description

DISPOSITIVO, SISTEMA Y MÉTODO DE ADSORCIÓN POR OSCILACIÓN DE PRESIÓN PARA LA PURIFICACIÓN DE UN COMPUESTO DE INTERÉS DEVICE, SYSTEM AND METHOD OF ADSORPTION BY PRESSURE OSCILLATION FOR THE PURIFICATION OF A COMPOUND OF INTEREST
Sector técnico Technical sector
[0001 ] La presente invención está relacionada con sistemas para la purificación de compuestos, más particularmente está relacionada con un dispositivo, sistema y método de adsorción por oscilación de presión para la purificación de un compuesto de interés. [0001] The present invention is related to systems for the purification of compounds, more particularly it is related to a pressure swing adsorption device, system and method for the purification of a compound of interest.
Técnica anterior Previous technique
[0002] La necesidad de gases de proceso con una alta pureza en las diferentes industrias ha crecido considerablemente, por ejemplo, en el recocido de acero, la fabricación de silicio, la hidrogenación de grasas y aceites, la fabricación de vidrio, el hidrocraqueo, la producción de metanol, la producción de oxoalcoholes. y procesos de isomerización. Esta creciente demanda requiere el desarrollo de procesos de separación altamente eficientes. [0002] The need for process gases with high purity in different industries has grown considerably, for example, in steel annealing, silicon manufacturing, hydrogenation of fats and oils, glass manufacturing, hydrocracking, the production of methanol, the production of oxoalcohols. and isomerization processes. This growing demand requires the development of highly efficient separation processes.
[0003] La adsorción por oscilación de presión (PSA) es un proceso de separación ampliamente conocido para la separación y purificación de corrientes de gases que contienen concentraciones de componentes indeseables. El método ha sido desarrollado y adaptado para una amplia gama de gases de alimentación, condiciones de operación, pureza y recuperación del producto. Muchos sistemas de adsorción por oscilación de presión utilizan dos o más columnas adsorbentes que operan en una secuencia cíclica para mantener una tasa de flujo de producto constante mientras que los lechos seleccionados pasan por varias etapas que incluyen: adsorción, despresuhzación, evacuación, purga, igualación de presión, represuhzación y otras etapas relacionadas. Normalmente, se requieren múltiples columnas que utilizan numerosas etapas de proceso para lograr una alta pureza y/o recuperación de productos gaseosos valiosos como hidrógenos, óxidos de carbono, gases de síntesis, hidrocarburos ligeros y similares. Las columnas adsorbentes múltiples que utilizan estos pasos del proceso también se utilizan para recuperar oxígeno del aire para diversas aplicaciones, incluidos los concentradores de oxígeno médicos portátiles recientemente popularizados por la pandemia de COVID-19. [0003] Pressure swing adsorption (PSA) is a widely known separation process for the separation and purification of gas streams containing undesirable component concentrations. The method has been developed and adapted for a wide range of feed gases, operating conditions, purity and product recovery. Many pressure swing adsorption systems use two or more adsorbent columns operating in a cyclic sequence to maintain a constant product flow rate while the selected beds undergo several stages including: adsorption, depressurization, evacuation, purging, equalization pressure, repressure and other related stages. Typically, multiple columns using numerous process steps are required to achieve high purity and/or recovery of valuable gaseous products such as hydrogens, carbon oxides, synthesis gases, light hydrocarbons and the like. Multiple adsorbent columns using these process steps are also used to recover oxygen from air for various applications, including Portable medical oxygen concentrators recently popularized by the COVID-19 pandemic.
[0004] En los procesos de PSA es habitual utilizar al menos dos columnas adsorbentes, estando una en línea mientras la otra se regenera. La despresuhzación y regeneración de una columna debe tener lugar durante el breve tiempo en que la otra columna está en línea, y una represurización rápida puede generar variaciones transitorias en los flujos de alimentación y producto que pueden afectar negativamente el funcionamiento de la planta. Uno de los principales problemas que enfrentan las columnas adsorbentes son el control de temperatura deficiente y los gradientes de calor no deseados generados en el seno de la columna. Además, las columnas usualmente son diseñadas para la purificación de un solo compuesto, limitando su aplicabilidad en procesos diferentes para los que inicialmente fueron ideadas. [0004] In PSA processes it is common to use at least two adsorbent columns, one being online while the other is regenerated. Depressurization and regeneration of one column must take place during the brief time that the other column is online, and rapid repressurization can generate transient variations in feed and product flows that can negatively affect plant operation. One of the main problems faced by adsorbent columns is poor temperature control and unwanted heat gradients generated within the column. Furthermore, columns are usually designed for the purification of a single compound, limiting their applicability in processes other than those for which they were initially designed.
[0005] Con el propósito de superar los problemas del control de temperatura en las columnas, investigaciones se han centrado en descubrir nuevas configuraciones que permitan un control más preciso de las condiciones de operación presentes dentro de las columnas. Por ejemplo, los documentos EP1029577B1 y EP1838418A4 describen columnas de adsorción por oscilación de presión que exhiben en su configuración sensores de temperatura fijados a sus paredes laterales con el propósito de detectar la temperatura del adsorbente dentro de una porción seleccionada de la columna. Si bien, esta configuración podría ser una solución, existe un problema que limita su aplicabilidad y es que los sensores son fijados a las paredes de la columna lo que se puede traducir en que una vez terminada su vida útil el intercambio de los sensores es difícil. Además, no se puede asegurar que la temperatura medida sea real pues ninguno de estos sensores se encuentra en el seno de la columna donde se está realizando el proceso de purificación. [0005] In order to overcome the problems of temperature control in the columns, research has focused on discovering new configurations that allow more precise control of the operating conditions present within the columns. For example, EP1029577B1 and EP1838418A4 describe pressure swing adsorption columns that exhibit in their configuration temperature sensors attached to their side walls for the purpose of detecting the temperature of the adsorbent within a selected portion of the column. Although this configuration could be a solution, there is a problem that limits its applicability and that is that the sensors are fixed to the walls of the column, which can mean that once their useful life is over, the exchange of sensors is difficult. . Furthermore, it cannot be ensured that the measured temperature is real since none of these sensors are located within the column where the purification process is being carried out.
[0006] Por consecuencia de lo anterior, se ha buscado suprimir los inconvenientes que presentan los dispositivos para la purificación de compuestos de interés utilizados en la actualidad, desarrollando un dispositivo, sistema y método de adsorción por oscilación de presión para la purificación de un compuesto de interés que además de permitir un control de temperatura más preciso en el seno del proceso a través de sensores de temperatura intercambiables, permita un proceso continuo y eficiente. [0006] As a consequence of the above, we have sought to eliminate the drawbacks presented by the devices for the purification of compounds of interest currently used, developing a device, system and pressure swing adsorption method for the purification of a compound. of interest that in addition to allowing more precise temperature control in the breast of the process through interchangeable temperature sensors, allowing a continuous and efficient process.
Breve descripción de la invención Brief description of the invention
[0007] Para ello, un primer aspecto de la presente invención se refiere a un dispositivo de columna de adsorción por oscilación de presión para la purificación de un compuesto de interés, que comprende: una sección interior; una sección exterior; una pluralidad de sensores de temperatura intercambiables; una sección inferior; y una sección superior, en donde la sección interior incluye una pared interior que define un diámetro interior entre 0.28 m y 0.32 m, la sección interior comprende una pluralidad de alojamientos interiores para sensores de temperatura y está configurada para permitir el paso del compuesto de interés, y para alojar por lo menos un sensor de temperatura intercambiable, en donde la sección exterior comprende una pluralidad de alojamientos exteriores para sensores de temperatura que está alineada con la pluralidad de alojamientos interiores para sensores de temperatura y está configurada para alojar a cada sensor de temperatura de la pluralidad de sensores de temperatura intercambiables, en donde la pluralidad de sensores de temperatura intercambiables está configurada para ensamblarse con la pluralidad de alojamientos exteriores e interiores y para medir la temperatura en un centro de la sección interior, en donde la sección inferior está configurada para recibir una entrada de vacío y una entrada de alimentación, en donde la sección superior está configurada para recircular y extraer un producto purificado; y en donde el dispositivo de columna de adsorción define una altura entre 0.8 m y 1 .5 m. [0007] To this end, a first aspect of the present invention refers to a pressure swing adsorption column device for the purification of a compound of interest, which comprises: an interior section; an outer section; a plurality of interchangeable temperature sensors; a lower section; and an upper section, wherein the interior section includes an interior wall that defines an interior diameter between 0.28 m and 0.32 m, the interior section comprises a plurality of interior housings for temperature sensors and is configured to allow the passage of the compound of interest, and for housing at least one interchangeable temperature sensor, wherein the outer section comprises a plurality of outer temperature sensor housings that is aligned with the plurality of inner temperature sensor housings and is configured to house each temperature sensor. of the plurality of interchangeable temperature sensors, wherein the plurality of interchangeable temperature sensors is configured to assemble with the plurality of exterior and interior housings and to measure the temperature at a center of the interior section, wherein the bottom section is configured to receive a vacuum inlet and a feed inlet, wherein the upper section is configured to recirculate and extract a purified product; and where the adsorption column device defines a height between 0.8 m and 1.5 m.
[0008] Un segundo aspecto de la presente invención considera un sistema de adsorción por oscilación de presión, que comprende: a) al menos dos dispositivos de columna de adsorción por oscilación como el dispositivo descrito anteriormente; b) una pluralidad de válvulas y tuberías que están conectadas con cada dispositivo de columna, con por lo menos un módulo de vacío, con un módulo de alimentación y con un módulo de condensador, y están configuradas para regular el flujo que pasa a través de cada válvula; c) por lo menos un módulo de vacío que está conectado a cada dispositivo de columna mediante la pluralidad de válvulas y tuberías, y está configurado para generar un vacío en la sección interior de cada dispositivo; d) un módulo de adquisición de datos, que está conectado con cada sensor de la pluralidad de sensores de temperatura intercambiables y con por lo menos un manómetro que mide la presión en la sección interior de cada dispositivo; e) un módulo de alimentación que está conectado con cada dispositivo mediante la pluralidad de válvulas y tuberías, y está configurado para alimentar con vapor de agua la sección interior de cada dispositivo; y f) un módulo de condensador que está conectado con cada dispositivo mediante la pluralidad de válvulas y tuberías y está configurado para recibir un producto purificado. [0008] A second aspect of the present invention considers a pressure swing adsorption system, comprising: a) at least two swing adsorption column devices like the device described above; b) a plurality of valves and pipes that are connected to each column device, to at least one vacuum module, to a feed module and to a condenser module, and are configured to regulate the flow passing through each valve; c) at least one vacuum module that is connected to each column device through the plurality of valves and pipes, and is configured to generate a vacuum in the interior section of each device; d) a data acquisition module, which is connected to each sensor of the plurality of interchangeable temperature sensors and to at least one pressure gauge that measures the pressure in the interior section of each device; e) a power module that is connected to each device through the plurality of valves and pipes, and is configured to feed water vapor to the interior section of each device; and f) a condenser module that is connected to each device by the plurality of valves and pipes and is configured to receive a purified product.
[0009] Un tercer aspecto de la presente invención considera un método para purificar un compuesto de interés, que comprende las etapas de: [0009] A third aspect of the present invention considers a method to purify a compound of interest, which comprises the steps of:
(i) suministrar el compuesto de interés a un dispositivo de columna de adsorción por oscilación como el descrito anteriormente, a través de un módulo de alimentación; (i) supplying the compound of interest to a swing adsorption column device as described above, through a feed module;
(¡i) adsorber el compuesto de interés controlando la presión y temperatura;(i) adsorb the compound of interest by controlling the pressure and temperature;
(iii) despresurizar el dispositivo de columna liberando el vapor residual; (iii) depressurize the column device by releasing residual vapor;
(iv) purgar el dispositivo de columna; y (iv) purge the column device; and
(v) represurizar el dispositivo de columna. (v) repressurize the column device.
Problema técnico technical problem
[0010] Teniendo en cuenta los defectos de la técnica anterior, es un objeto de la presente invención proporcionar un dispositivo, sistema y método de adsorción por oscilación de presión para la purificación de un compuesto de interés que permita obtener una pureza mayor en un menor tiempo. [0010] Taking into account the defects of the prior art, it is an object of the present invention to provide a pressure swing adsorption device, system and method for the purification of a compound of interest that allows obtaining a higher purity in a lower time.
[0011 ] Es otro objeto de la presente invención proporcionar un dispositivo para la purificación de un compuesto de interés con sensores de temperatura fácilmente intercambiables acoplados a lo largo del cuerpo de la columna. [0012] Es otro objeto de la presente invención proporcionar un sistema versátil de adsorción por oscilación de presión para la purificación de un compuesto de interés. [0011] It is another object of the present invention to provide a device for the purification of a compound of interest with easily interchangeable temperature sensors attached along the body of the column. [0012] It is another object of the present invention to provide a versatile pressure swing adsorption system for the purification of a compound of interest.
[0013] En ninguno de los trabajos reportados presentan el diseño de las columnas con sensores de temperatura que lleguen al seno de la columna. Esta configuración en el diseño de la columna permite el control real de la temperatura y no de los extremos con caídas o decrementos de temperatura. [0013] None of the reported works present the design of the columns with temperature sensors that reach the core of the column. This configuration in the column design allows real control of the temperature and not extremes with drops or decreases in temperature.
Descripción breve de las figuras Brief description of the figures
[0014] Los aspectos novedosos que se consideran característicos de la presente invención se establecerán con particularidad en las reivindicaciones anexas. Sin embargo, algunas modalidades, características y algunos objetos y ventajas de la misma, se comprenderán mejor en la descripción detallada, cuando se lea en relación con los dibujos anexos, en los cuales: [0014] The novel aspects that are considered characteristic of the present invention will be established with particularity in the attached claims. However, some embodiments, characteristics and some objects and advantages thereof will be better understood in the detailed description, when read in connection with the accompanying drawings, in which:
[0015] [Fig.1 ] La figura 1 ¡lustra una vista en perspectiva frontal del dispositivo de columna de adsorción por oscilación de presión, de conformidad con una primera modalidad de la presente invención. [0015] [Fig.1] Figure 1 illustrates a front perspective view of the pressure swing adsorption column device, in accordance with a first embodiment of the present invention.
[0016] [Fig.2] La figura 2 ¡lustra una malla de acero inoxidable colocada junto a una brida inferior del dispositivo de columna de adsorción por oscilación de presión para la retención y empaquetamiento del material adsorbente, de conformidad con una primera modalidad de la presente invención. [0016] [Fig.2] Figure 2 illustrates a stainless steel mesh placed next to a lower flange of the pressure swing adsorption column device for the retention and packing of the adsorbent material, in accordance with a first embodiment of the present invention.
[0017] [Fig.3] La figura 3 ¡lustra un diagrama del sistema de adsorción por oscilación de presión para la purificación de un compuesto de interés, de conformidad con una segunda modalidad de la presente invención. [0017] [Fig.3] Figure 3 illustrates a diagram of the pressure swing adsorption system for the purification of a compound of interest, in accordance with a second embodiment of the present invention.
[0018] [Fig.4] La figura 4 ¡lustra un ejemplo del sistema de adsorción por oscilación de presión para la purificación de bioetanol, de conformidad con una segunda modalidad de la presente invención. [0018] [Fig.4] Figure 4 illustrates an example of the pressure swing adsorption system for the purification of bioethanol, in accordance with a second embodiment of the present invention.
[0019] [Fig.5] La figura 5 ¡lustra los perfiles de temperatura a lo largo de la columna de 1 m. [0019] [Fig.5] Figure 5 illustrates the temperature profiles along the 1 m column.
[0020] [Fig.6] La figura 6 ¡lustra los perfiles de pureza desde que arranca el proceso hasta llegar al estado estable cíclico. [0021 ] [Fig.7] La figura 7 ¡lustra el perfil de temperatura a lo largo de la columna durante 1 ciclo del proceso. [0020] [Fig.6] Figure 6 illustrates the purity profiles from the start of the process until reaching the cyclic stable state. [0021] [Fig.7] Figure 7 illustrates the temperature profile along the column during 1 cycle of the process.
[0022] [Fig.8] La figura 8 ¡lustra el perfil de presión a lo largo de la columna durante 1 ciclo del proceso. [0022] [Fig.8] Figure 8 illustrates the pressure profile along the column during 1 cycle of the process.
Descripción de alguna forma de realizar la invención Description of some way of carrying out the invention
[0023] La presente invención implica mejoras basadas en la tecnología de separación de gas por adsorción por oscilación de presión mencionada anteriormente, es decir, en esta invención casi no se pierde el gas efectivo y, además, esta invención no necesita las complicadas instalaciones de vacío bajo una presión de adsorción adecuada. Por lo tanto, el costo del equipo y el consumo de energía se reducirán notablemente. [0023] The present invention involves improvements based on the pressure swing adsorption gas separation technology mentioned above, that is, in this invention almost no effective gas is lost and, furthermore, this invention does not need the complicated installations of vacuum under a suitable adsorption pressure. Therefore, the cost of equipment and energy consumption will be greatly reduced.
[0024] Por lo tanto, la presente invención se refiere en primer lugar a un dispositivo de columna de adsorción por oscilación de presión para la purificación de un compuesto de interés, que comprende: una sección interior; una sección exterior; una pluralidad de sensores de temperatura intercambiables; una sección inferior; y una sección superior, en donde la sección interior incluye una pared interior que define un diámetro interior entre 0.28 m y 0.32 m, la sección interior comprende una pluralidad de alojamientos interiores para sensores de temperatura y está configurada para permitir el paso del compuesto de interés, y para alojar por lo menos un sensor de temperatura intercambiable, en donde la sección exterior comprende una pluralidad de alojamientos exteriores para sensores de temperatura que está alineada con la pluralidad de alojamientos interiores para sensores de temperatura y está configurada para alojar a cada sensor de temperatura de la pluralidad de sensores de temperatura intercambiables, en donde la pluralidad de sensores de temperatura intercambiables está configurada para ensamblarse con la pluralidad de alojamientos exteriores e interiores y para medir la temperatura en un centro de la sección interior, en donde la sección inferior está configurada para recibir una entrada de vacío y una entrada de alimentación, en donde la sección superior está configurada para recircular y extraer un producto purificado; y en donde el dispositivo de columna de adsorción define una altura entre 0.8 m y 1 .5 m. [0025] Preferiblemente, el adsorbente es zeolita natural o sintética. Más preferiblemente, la zeolita es natural. [0024] Therefore, the present invention relates first of all to a pressure swing adsorption column device for the purification of a compound of interest, comprising: an inner section; an outer section; a plurality of interchangeable temperature sensors; a lower section; and an upper section, wherein the interior section includes an interior wall that defines an interior diameter between 0.28 m and 0.32 m, the interior section comprises a plurality of interior housings for temperature sensors and is configured to allow the passage of the compound of interest, and for housing at least one interchangeable temperature sensor, wherein the outer section comprises a plurality of outer temperature sensor housings that is aligned with the plurality of inner temperature sensor housings and is configured to house each temperature sensor. of the plurality of interchangeable temperature sensors, wherein the plurality of interchangeable temperature sensors is configured to assemble with the plurality of exterior and interior housings and to measure the temperature at a center of the interior section, wherein the bottom section is configured to receive a vacuum inlet and a feed inlet, wherein the upper section is configured to recirculate and extract a purified product; and where the adsorption column device defines a height between 0.8 m and 1.5 m. [0025] Preferably, the adsorbent is natural or synthetic zeolite. More preferably, the zeolite is natural.
[0026] En una modalidad de la presente invención, la sección superior del dispositivo de columna comprende una salida de extracción, una conexión analógica, y una conexión digital; en donde la salida de extracción está configurada para extraer un producto purificado, en donde la conexión analógica está configurada para conectarse a un manómetro analógico para medir la presión en la sección interior, y en donde la conexión digital está configurada para conectarse con un sensor digital de presión que envía datos a un módulo de adquisición de datos. [0026] In one embodiment of the present invention, the upper section of the column device comprises an extraction output, an analog connection, and a digital connection; wherein the extraction outlet is configured to extract a purified product, wherein the analog connection is configured to connect to an analog pressure gauge to measure the pressure in the inner section, and wherein the digital connection is configured to connect to a digital sensor pressure sensor that sends data to a data acquisition module.
[0027] En otra modalidad de la presente invención, la sección inferior del dispositivo de columna de adsorción por oscilación de presión comprende adicionalmente una malla de acero inoxidable que es colocada en una brida inferior que está ubicada en la sección inferior del dispositivo de columna de adsorción por oscilación de presión, la malla de acero inoxidable está configurada para la retención y empaquetamiento del material adsorbente. [0027] In another embodiment of the present invention, the lower section of the pressure swing adsorption column device additionally comprises a stainless steel mesh that is placed in a lower flange that is located in the lower section of the column device. Pressure swing adsorption, the stainless steel mesh is configured for retention and packing of the adsorbent material.
[0028] Un segundo aspecto de la presente invención considera un sistema de adsorción por oscilación de presión, que comprende: a) al menos dos dispositivos de columna de adsorción por oscilación como el dispositivo descrito anteriormente; b) una pluralidad de válvulas y tuberías que están conectadas con cada dispositivo de columna, con por lo menos un módulo de vacío, con un módulo de alimentación y con un módulo de condensador, y están configuradas para regular el flujo que pasa a través de cada válvula; c) por lo menos un módulo de vacío que está conectado a cada dispositivo de columna mediante la pluralidad de válvulas y tuberías, y está configurado para generar un vacío en la sección interior de cada dispositivo; d) un módulo de adquisición de datos, que comprende: un sistema de cómputo y un sistema de control PLC, el módulo de adquisición de datos está conectado con cada sensor de la pluralidad de sensores de temperatura intercambiables y con por lo menos un manómetro que mide la presión en la sección interior de cada dispositivo; e) un módulo de alimentación que está conectado con cada dispositivo mediante la pluralidad de válvulas y tuberías, y está configurado para alimentar con vapor de agua la sección interior de cada dispositivo; y f) un módulo de condensador que está conectado con cada dispositivo mediante la pluralidad de válvulas y tuberías y está configurado para recibir un producto purificado. [0028] A second aspect of the present invention considers a pressure swing adsorption system, comprising: a) at least two swing adsorption column devices like the device described above; b) a plurality of valves and pipes that are connected to each column device, to at least one vacuum module, to a feed module and to a condenser module, and are configured to regulate the flow passing through each valve; c) at least one vacuum module that is connected to each column device through the plurality of valves and pipes, and is configured to generate a vacuum in the interior section of each device; d) a data acquisition module, comprising: a computing system and a PLC control system, the data acquisition module is connected with each sensor of the plurality of interchangeable temperature sensors and with at least one pressure gauge that measures the pressure in the interior section of each device; e) a power module that is connected to each device through the plurality of valves and pipes, and is configured to feed water vapor to the interior section of each device; and f) a condenser module that is connected to each device by the plurality of valves and pipes and is configured to receive a purified product.
[0029] Preferiblemente, el módulo de alimentación es un compresor o una caldera. [0029] Preferably, the power module is a compressor or a boiler.
[0030] Preferiblemente, el módulo de vacío es una bomba de vacío. [0030] Preferably, the vacuum module is a vacuum pump.
[0031 ] Preferiblemente, el módulo de condensador es un condensador. [0031] Preferably, the capacitor module is a capacitor.
[0032] En una modalidad de la presente invención, el módulo de adquisición de datos comprende: un sistema de cómputo y un sistema de control PLC, en donde el módulo de adquisición de datos está conectado adicionalmente con la pluralidad de válvulas y tuberías, con el módulo de vacío, con el módulo de alimentación y con el módulo de condensador y está configurado para controlar el funcionamiento de cada uno. [0032] In one embodiment of the present invention, the data acquisition module comprises: a computing system and a PLC control system, wherein the data acquisition module is additionally connected to the plurality of valves and pipes, with the vacuum module, with the power module and with the condenser module and is configured to control the operation of each.
[0033] En una modalidad adicional de la presente invención, la pluralidad de válvulas y tuberías comprende: una pluralidad de válvulas y tuberías superior que está conectada con el módulo de condensador; y una pluralidad de válvulas y tuberías inferior que está conectada con el módulo de vacío y con el módulo de alimentación. [0033] In a further embodiment of the present invention, the plurality of valves and pipes comprises: an upper plurality of valves and pipes that is connected to the condenser module; and a plurality of lower valves and pipes that are connected to the vacuum module and the power module.
[0034] Un tercer aspecto de la presente invención considera un método para purificar un compuesto de interés, que comprende las etapas de: [0034] A third aspect of the present invention considers a method to purify a compound of interest, which comprises the steps of:
(i) suministrar el compuesto de interés a un dispositivo de columna de adsorción por oscilación como el descrito anteriormente, a través de un módulo de alimentación; (i) supplying the compound of interest to a swing adsorption column device as described above, through a feed module;
(¡i) adsorber el compuesto de interés controlando la presión y temperatura;(i) adsorb the compound of interest by controlling the pressure and temperature;
(iii) despresurizar el dispositivo de columna liberando el vapor residual; (iii) depressurize the column device by releasing residual vapor;
(iv) purgar el dispositivo de columna; y (iv) purge the column device; and
(v) represurizar el dispositivo de columna. [0035] En una modalidad de la presente invención, el flujo del compuesto de interés es suministrado mediante un compresor de 175 psi. (v) repressurize the column device. [0035] In one embodiment of the present invention, the flow of the compound of interest is supplied by a 175 psi compressor.
[0036] Preferiblemente, el compuesto de interés es bioetanol con un 99% de pureza; las condiciones de purificación del bioetanol son las siguientes en cada una de las etapas del método: (i) suministrar una mezcla de bioetanol al 90 % (p/p) y agua al 10% (p/p) al dispositivo de columna de adsorción por oscilación de presión; (¡i) adsorber a una presión >400 kPa y una temperatura >373.15 K; (iii) despresurizar el dispositivo de columna disminuyendo la presión a al menos 50 kPa; (iv) purgar el dispositivo de columna disminuyendo la presión de 50 kPa a 10 kPa; y (v) represuhzar el dispositivo de columna aumentando la presión de 10 kPa a 400 kPa. [0036] Preferably, the compound of interest is bioethanol with 99% purity; The bioethanol purification conditions are the following in each of the steps of the method: (i) supply a mixture of 90% (w/w) bioethanol and 10% (w/w) water to the adsorption column device by pressure oscillation; (i) adsorb at a pressure >400 kPa and a temperature >373.15 K; (iii) depressurize the column device by decreasing the pressure to at least 50 kPa; (iv) purge the column device by decreasing the pressure from 50 kPa to 10 kPa; and (v) repressurize the column device by increasing the pressure from 10 kPa to 400 kPa.
[0037] Preferiblemente, el compuesto de interés es hidrogeno con un 99.9% de pureza; las condiciones de purificación del hidrogeno son las siguientes en cada una de las etapas del método: (i) suministrar una mezcla que comprende: H2 al 72.2 % (p/p), CH4 al 4.17% (p/p), CO al 2.03% (p/p) y CO2 al 21.6% (p/p) al dispositivo de columna de adsorción por oscilación de presión; (¡i) adsorber a una presión >350 kPa y una temperatura >295 K; (iii) despresurizar el dispositivo de columna disminuyendo la presión a al menos 50 kPa; (iv) purgar el dispositivo de columna disminuyendo la presión de 50 kPa a 10 kPa; y (v) represuhzar el dispositivo de columna aumentando la presión de 10 kPa a 400 kPa. [0037] Preferably, the compound of interest is hydrogen with 99.9% purity; The hydrogen purification conditions are the following in each of the stages of the method: (i) supply a mixture that comprises: H2 at 72.2% (w/w), CH4 at 4.17% (w/w), CO at 2.03 % (w/w) and CO2 at 21.6% (w/w) to the pressure swing adsorption column device; (i) adsorb at a pressure >350 kPa and a temperature >295 K; (iii) depressurize the column device by decreasing the pressure to at least 50 kPa; (iv) purge the column device by decreasing the pressure from 50 kPa to 10 kPa; and (v) repressurize the column device by increasing the pressure from 10 kPa to 400 kPa.
[0038] Preferiblemente, el compuesto de interés es oxígeno con una pureza de entre 95% y 99.5%; las condiciones de purificación del oxígeno son las siguientes en cada una de las etapas del método: (i) suministrar una mezcla que comprende: nitrógeno al 74.18% (p/p), oxígeno al 19.61 % (p/p), dióxido de carbono al 0.03% (p/p) y vapor de agua al 6.18% (p/p) al dispositivo de columna de adsorción por oscilación de presión; (¡i) adsorber a una presión >350 kPa y una temperatura >298.15 K; (iii) despresurizar el dispositivo de columna disminuyendo la presión a al menos 50 kPa; (iv) purgar el dispositivo de columna disminuyendo la presión de 50 kPa a 10 kPa; y (v) represuhzar el dispositivo de columna aumentando la presión de 10 kPa a 400 kPa. [0038] Preferably, the compound of interest is oxygen with a purity of between 95% and 99.5%; The oxygen purification conditions are the following in each of the stages of the method: (i) supply a mixture that comprises: nitrogen at 74.18% (w/w), oxygen at 19.61% (w/w), carbon dioxide at 0.03% (w/w) and water vapor at 6.18% (w/w) to the pressure swing adsorption column device; (i) adsorb at a pressure >350 kPa and a temperature >298.15 K; (iii) depressurize the column device by decreasing the pressure to at least 50 kPa; (iv) purge the column device by decreasing the pressure from 50 kPa to 10 kPa; and (v) repressurize the column device by increasing the pressure from 10 kPa to 400 kPa.
[0039] Preferiblemente, el compuesto de interés es metano con una pureza de entre 95% y 99%; las condiciones de purificación del metano son las siguientes en cada una de las etapas del método: (i) suministrar una mezcla que comprende: metano en una concentración de entre 50 y 75% (p/p) y dióxido de carbono en una concentración de entre 25 y 45% (p/p) al dispositivo de columna de adsorción por oscilación de presión; (¡i) adsorber á una presión >1200 KPa y una temperatura de entre 298 y 323 K; (iii) despresurizar el dispositivo de columna disminuyendo la presión a al menos 50 Kpa; (iv) purgar el dispositivo de columna disminuyendo la presión de 50 kPa a 10 kPa; y (v) represurizar el dispositivo de columna aumentando la presión de 10 kPa a 400 kPa. [0039] Preferably, the compound of interest is methane with a purity of between 95% and 99%; The methane purification conditions are the following in each one of the steps of the method: (i) supply a mixture comprising: methane in a concentration of between 50 and 75% (w/w) and carbon dioxide in a concentration of between 25 and 45% (w/w) to the pressure swing adsorption column device; (i) adsorb at a pressure >1200 KPa and a temperature between 298 and 323 K; (iii) depressurize the column device by decreasing the pressure to at least 50 Kpa; (iv) purge the column device by decreasing the pressure from 50 kPa to 10 kPa; and (v) repressurize the column device by increasing the pressure from 10 kPa to 400 kPa.
[0040] Haciendo referencia ahora a la figura 1 , que ¡lustra un dispositivo de columna 1000 de adsorción por oscilación de presión para la purificación de un compuesto de interés, que comprende: una sección interior 1100; una sección exterior 1 120; una pluralidad de sensores de temperatura intercambiables 1 1 10; una sección inferior 1200; y una sección superior 1300, en donde la sección interior incluye una pared interior que define un diámetro interior, la sección interior comprende una pluralidad de alojamientos interiores para sensores de temperatura y está configurada para permitir el paso del compuesto de interés, y para alojar a cada sensor de temperatura de la pluralidad de sensores de temperatura intercambiables 1 1 10, en donde la sección exterior 1 120 comprende una pluralidad de alojamientos exteriores para sensores de temperatura que está alineada con la pluralidad de alojamientos interiores para sensores de temperatura y está configurada para alojar a cada sensor de temperatura de la pluralidad de sensores de temperatura intercambiables 11 10, en donde la pluralidad de sensores de temperatura intercambiables 11 10 está configurada para ensamblarse con la pluralidad de alojamientos exteriores e interiores y para medir la temperatura en un centro de la sección interior, en donde la sección inferior 1200 está configurada para recibir una entrada de vacío 1220 y una entrada de alimentación 1210, en donde la sección superior 1300 está configurada para recircular y extraer un producto purificado. [0040] Referring now to Figure 1, which illustrates a pressure swing adsorption column device 1000 for the purification of a compound of interest, comprising: an inner section 1100; an outer section 1 120; a plurality of interchangeable temperature sensors 1 1 10; a lower section 1200; and an upper section 1300, wherein the interior section includes an interior wall that defines an interior diameter, the interior section comprises a plurality of interior housings for temperature sensors and is configured to allow the passage of the compound of interest, and to house each temperature sensor of the plurality of interchangeable temperature sensors 1 1 10, wherein the outer section 1 120 comprises a plurality of outer housings for temperature sensors that is aligned with the plurality of inner housings for temperature sensors and is configured to accommodate each temperature sensor of the plurality of interchangeable temperature sensors 11 10, wherein the plurality of interchangeable temperature sensors 11 10 is configured to be assembled with the plurality of exterior and interior housings and to measure the temperature at a center of the inner section, wherein the lower section 1200 is configured to receive a vacuum inlet 1220 and a feed inlet 1210, wherein the upper section 1300 is configured to recirculate and extract a purified product.
[0041 ] Adicionalmente, la figura 1 ¡lustra la sección superior 1300 del dispositivo de columna 1000 que comprende una salida de extracción 1320, una conexión analógica 1310, y una conexión digital 1330; en donde la salida de extracción 1320 está configurada para extraer un producto purificado, en donde la conexión analógica 1310 está configurada para conectarse a un manómetro analógico para medir la presión en la sección interior 1 100, y en donde la conexión digital 1330 está configurada para conectarse con un sensor digital de presión que envía datos a un módulo de adquisición de datos (no mostrado). [0041] Additionally, Figure 1 illustrates the upper section 1300 of the column device 1000 comprising an extraction output 1320, an analog connection 1310, and a digital connection 1330; wherein the extraction output 1320 is configured to extract a purified product, wherein the analog connection 1310 is configured to connect to an analog pressure gauge to measuring the pressure in the inner section 1 100, and wherein the digital connection 1330 is configured to connect with a digital pressure sensor that sends data to a data acquisition module (not shown).
[0042] Ahora, la figura 2, ¡lustra una malla de acero inoxidable 1240 que es colocada en una brida inferior 1230 que está ubicada en la sección inferior 1200 del dispositivo de columna de adsorción por oscilación de presión, la malla de acero inoxidable 1240 está configurada para la retención y empaquetamiento del material adsorbente, de conformidad con una primera modalidad de la presente invención. [0042] Now, Figure 2 illustrates a stainless steel mesh 1240 that is placed in a lower flange 1230 that is located in the lower section 1200 of the pressure swing adsorption column device, the stainless steel mesh 1240 It is configured for the retention and packaging of the adsorbent material, in accordance with a first embodiment of the present invention.
[0043] Finalmente, la figura 3 ¡lustra un sistema de adsorción por oscilación de presión para la purificación de un compuesto de interés 2000, que comprende: a) al menos dos dispositivos de columna 1000 y 1000’ de adsorción por oscilación, b) una pluralidad de válvulas y tuberías 2300 que están conectadas con cada dispositivo de columna 1000,1000’, con por lo menos un módulo de vacío 4000, con un módulo de alimentación 3000 y con un módulo de condensador 6000, y están configuradas para regular el flujo que pasa a través de cada válvula; c) por lo menos un módulo de vacío 4000 que está conectado a cada dispositivo de columna mediante la pluralidad de válvulas y tuberías 2300, y está configurado para generar un vacío en la sección interior de cada dispositivo de columna 1000, 1000’; d) un módulo de adquisición de datos 5000, que comprende: un sistema do cómputo y un sistema de control PLC, el módulo de adquisición de datos 5000 está conectado con cada sensor de la pluralidad de sensores de temperatura intercambiables y con por lo menos un manómetro que mide la presión en la sección interior de cada dispositivo de columna 1000, 1000’; e) un módulo de alimentación 3000 que está conectado con cada dispositivo de columna 1000, 1000’ mediante la pluralidad de válvulas y tuberías 2300, y está configurado para alimentar con vapor de agua la sección interior de cada dispositivo de columna 1000, 1000’; y f) un módulo de condensador 6000 que está conectado con cada dispositivo de columna 1000, 1000’ mediante la pluralidad de válvulas y tuberías 2300 y está configurado para recibir un producto purificado. [0043] Finally, Figure 3 illustrates a pressure swing adsorption system for the purification of a compound of interest 2000, comprising: a) at least two swing adsorption column devices 1000 and 1000', b) a plurality of valves and pipes 2300 that are connected with each column device 1000,1000', with at least one vacuum module 4000, with a power module 3000 and with a condenser module 6000, and are configured to regulate the flow passing through each valve; c) at least one vacuum module 4000 that is connected to each column device through the plurality of valves and pipes 2300, and is configured to generate a vacuum in the interior section of each column device 1000, 1000'; d) a data acquisition module 5000, comprising: a computing system and a PLC control system, the data acquisition module 5000 is connected to each sensor of the plurality of interchangeable temperature sensors and with at least one manometer measuring the pressure in the interior section of each column device 1000, 1000'; e) a feed module 3000 that is connected to each column device 1000, 1000' through the plurality of valves and pipes 2300, and is configured to feed steam to the inner section of each column device 1000, 1000'; and f) a condenser module 6000 that is connected to each column device 1000, 1000' by the plurality of valves and pipes 2300 and is configured to receive a purified product.
[0044] Además, la figura 3 ¡lustra que el módulo de adquisición de datos 5000 está conectado adicionalmente con la pluralidad de válvulas y tuberías 2300, con el módulo de vacío 4000, con el módulo de alimentación 3000 y con el módulo de condensador 6000 y está configurado para controlar el funcionamiento de cada uno. Adicionalmente, la figura 3 ¡lustra que la pluralidad de válvulas y tuberías 2300 comprende: una pluralidad de válvulas y tuberías superior 2310 que está conectada con el módulo de condensador 6000; y una pluralidad de válvulas y tuberías inferior 2320 que está conectada con el módulo de vacío 4000 y con el módulo de alimentación 3000. [0044] Furthermore, Figure 3 illustrates that the data acquisition module 5000 is additionally connected with the plurality of valves and pipes 2300, with the vacuum module 4000, with the power module 3000 and with the capacitor 6000 and is configured to control the operation of each one. Additionally, Figure 3 illustrates that the plurality of valves and pipes 2300 comprises: an upper plurality of valves and pipes 2310 that is connected to the condenser module 6000; and a plurality of lower valves and pipes 2320 that is connected to the vacuum module 4000 and to the power module 3000.
[0045] La presente invención será mejor entendida a partir de los siguientes ejemplos, los cuales se presentan únicamente con fines ilustrativos para permitir la comprensión cabal de las modalidades preferidas de la presente invención, sin que por ello se implique que no existen otras modalidades no ¡lustradas que puedan llevarse a la práctica con base en la descripción detallada arriba realizada. [0045] The present invention will be better understood from the following examples, which are presented solely for illustrative purposes to allow a full understanding of the preferred embodiments of the present invention, without implying that there are no other embodiments. Illustrated ideas that can be put into practice based on the detailed description above.
Ejemplos Examples
[0046] Se realizó un ensayo para la purificación de biometano a partir del sistema de adsorción por oscilación de presión de conformidad con la presente invención. [0046] A test was carried out for the purification of biomethane from the pressure swing adsorption system in accordance with the present invention.
[0047] Para la purificación se utilizó un arreglo de dos dispositivos de columna 1000 y 1000’ empacados con un adsorberte como el que se muestra en la figura 4 controlados e interconectadas a través de una pluralidad de válvulas y tuberías superior 2310 e inferior 2320, donde el dispositivo de columna 1000 comprende: una sección interior 1100; una sección exterior 1 120; una pluralidad de sensores de temperatura intercambiables 1 1 10; una sección inferior 1200; y una sección superior 1300, en donde la sección interior incluye una pared interior que define un diámetro interior, la sección interior comprende una pluralidad de alojamientos interiores para sensores de temperatura y está configurada para permitir el paso del compuesto de interés, y para alojar a cada sensor de temperatura de la pluralidad de sensores de temperatura intercambiables 1 110, en donde la sección exterior 1120 comprende una pluralidad de alojamientos exteriores para sensores de temperatura que está alineada con la pluralidad de alojamientos interiores para sensores de temperatura y está configurada para alojar a cada sensor de temperatura de la pluralidad de sensores de temperatura intercambiables 11 10, en donde la pluralidad de sensores de temperatura intercambiables 1 1 10 está configurada para ensamblarse con la pluralidad de alojamientos exteriores e interiores y para medir la temperatura en un centro de la sección interior, en donde la sección inferior 1200 está configurada para recibir una entrada de vacío 1220 y una entrada de alimentación 1210, en donde la sección superior 1300 está configurada para recircular y extraer un producto purificado. Adicionalmente, la figura 1 ¡lustra la sección superior 1300 del dispositivo de columna 1000 que comprende una salida de extracción 1320, una conexión analógica 1310, y una conexión digital 1330; en donde la salida de extracción 1320 está configurada para extraer un producto purificado, en donde la conexión analógica 1310 está configurada para conectarse a un manómetro analógico para medir la presión en la sección interior 1 100, y en donde la conexión digital 1330 está configurada para conectarse con un sensor digital de presión que envía datos a un módulo de adquisición de datos (no mostrado). El segundo dispositivo de columna 1000’ comprende los mismos elementos que el dispositivo de columna 1000’ señalados por los números 1110’, 1210’, 1220’, 1310’, 1320’, y 1330’ para la purificación de un compuesto de interés de forma continua. [0047] For purification, an arrangement of two column devices 1000 and 1000' packed with an adsorbent as shown in Figure 4 controlled and interconnected through a plurality of upper 2310 and lower 2320 valves and pipes was used. wherein the column device 1000 comprises: an interior section 1100; an outer section 1 120; a plurality of interchangeable temperature sensors 1 1 10; a lower section 1200; and an upper section 1300, wherein the interior section includes an interior wall that defines an interior diameter, the interior section comprises a plurality of interior housings for temperature sensors and is configured to allow the passage of the compound of interest, and to house each temperature sensor of the plurality of interchangeable temperature sensors 1 110, wherein the outer section 1120 comprises a plurality of outer housings for temperature sensors that is aligned with the plurality of inner housings for temperature sensors and is configured to house each temperature sensor of the plurality of interchangeable temperature sensors 11 10, wherein the plurality of interchangeable temperature sensors 1 1 10 is configured to be assembled with the plurality of exterior and interior housings and to measure the temperature at a center of the section interior, where The lower section 1200 is configured to receive a vacuum inlet 1220 and a feed inlet 1210, wherein the upper section 1300 is configured to recirculate and extract a purified product. Additionally, Figure 1 illustrates the upper section 1300 of the column device 1000 comprising a draw output 1320, an analog connection 1310, and a digital connection 1330; wherein the extraction outlet 1320 is configured to extract a purified product, wherein the analog connection 1310 is configured to connect to an analog pressure gauge to measure the pressure in the inner section 1 100, and wherein the digital connection 1330 is configured to connect with a digital pressure sensor that sends data to a data acquisition module (not shown). The second column device 1000' comprises the same elements as the column device 1000' indicated by the numbers 1110', 1210', 1220', 1310', 1320', and 1330' for the purification of a compound of interest in a form keep going.
[0048] El adsorbente utilizado para el empaquetamiento tuvo un pretratamiento que comprendió las etapas de: (i) filtrar el adsorbente para eliminar impurezas; (¡i) calentar el adsorbentes a una temperatura de 250 °C durante 150 minutos; (iii) calentar una solución ácida al 0.1 N hasta su punto de ebullición; (iv) mezclar el adsorbente previamente calendado con la solución ácida en ebullición hasta su total disolución; (v) enfriar la mezcla a temperatura ambiente y decantar la solución ácida: (vi) lavar el adsorbente con agua destilada hasta eliminar todos los residuos de la solución ácida; (vii) calentar el adsorbente a una temperatura de 250 °C durante 5 horas; y (viii) enfriar el adsorbente a temperatura ambiente, medir la masa y repetir el paso (vii) hasta que la masa sea constante. Como adsorbente se utilizó zeolita natural. [0048] The adsorbent used for packaging had a pretreatment that included the steps of: (i) filtering the adsorbent to eliminate impurities; (i) heat the adsorbents to a temperature of 250 °C for 150 minutes; (iii) heat a 0.1 N acid solution to its boiling point; (iv) mix the previously heated adsorbent with the boiling acid solution until completely dissolved; (v) cool the mixture to room temperature and decant the acid solution: (vi) wash the adsorbent with distilled water until all residues of the acid solution are removed; (vii) heating the adsorbent at a temperature of 250 °C for 5 hours; and (viii) cool the adsorbent to room temperature, measure the mass and repeat step (vii) until the mass is constant. Natural zeolite was used as adsorbent.
[0049] Una vez listo el sistema, la primera etapa para la purificación de bioetanol, comprendió: [0049] Once the system was ready, the first stage for bioethanol purification included:
[0050] -Adsorción en un primer dispositivo de columna 1000 y despresuñzación en un segundo dispositivo de columna 1000’. Las válvulas 2321 , 2326, 2312 y 2327 fueron habilitadas para realizar la adsorción y producción utilizando el primer dispositivo de columna 1000, mientras el segundo dispositivo de columna realiza el paso de despresuñzación habilitando las válvulas 2323 y 2325. Estos pasos se llevan en el mismo periodo de tiempo durante 80 segundos. A continuación, se describe la configuración de las válvulas por 80 segundos en el paso de adsorción para el primer dispositivo de columna 1000: La válvula 2321 recibe la alimentación principal proveniente de una caldera de vapor con una mezcla de 90% en peso de etanol y 10 % en peso de agua. La válvula 2321 está totalmente abierta (es una válvula digital on/off); La válvula 2327 recibe parte de la alimentación de proveniente de la válvula 2321. Esta válvula 2327 es proporcional (analógica) y tiene una apertura del 70%, ya que esto permitirá introducir vapor sobresaturado y mantener una presión elevada; La válvula 2312 es proporcional (analógica) y tiene una apertura del 30%. Esta válvula 2312 está ubicada en la parte superior para obtener el producto purificado obtenido del primer dispositivo de columna 1000. El motivo por el cual está tiene una apertura del 30% es porque permitirá que el primer dispositivo de columna 1000 no se despresurice y se mantenga una presión elevada para seguir producción etanol puro (bioetanol); la válvula 2314 es digital y tiene está totalmente abierta (on/off), esta recibe el producto purificado del primer y segundo dispositivos de columna 1000 y 1000’, y manda el producto purificado directamente a un condensador ya que el producto purificado está a alta presión y debe de obtenerse de manera líquida. Luego, para la etapa de despresuhzación en el segundo dispositivo de columna 1000’: La válvula 2323 está totalmente abierta y es una válvula digital on/off, permitiendo que el segundo dispositivo de columna se despresurice por la parte inferior con el objetivo de retirar el agua fácilmente tanto en fase liquida como la liberación de los sitios activos de zeolita; la válvula 2324 es proporcional (analógica), y tiene una apertura del 90%, está apertura permite que se realice una despresurización considerada para llegar a los 0.5 bar cercana a la presión de purga, esta válvula 2324 se encuentra ubicada de tal manera que pueda ser utilizada para el primer y segundo dispositivos de columna 1000 y 1000’ en el paso de despresuhzación, de esta válvula (2324) salen concentraciones de agua elevadas, esta agua se puede reutilizar para nuevamente ser introducida en la caldera y salga en fase vapor. [0050] -Adsorption in a first column device 1000 and depressurization in a second column device 1000'. Valves 2321, 2326, 2312 and 2327 were enabled to perform adsorption and production using the first column device 1000, while the second column device performs the depressurization step by enabling valves 2323 and 2325. These steps are carried out in the same period of time for 80 seconds. Next, it describes the valve configuration for 80 seconds in the adsorption step for the first column device 1000: Valve 2321 receives the main feed from a steam boiler with a mixture of 90 wt% ethanol and 10 wt% of water. Valve 2321 is fully open (it is a digital on/off valve); Valve 2327 receives part of the feed from valve 2321. This valve 2327 is proportional (analog) and has an opening of 70%, since this will allow supersaturated steam to be introduced and maintain a high pressure; The 2312 valve is proportional (analog) and has a 30% opening. This valve 2312 is located at the top to obtain the purified product obtained from the first column device 1000. The reason why it has a 30% opening is because it will allow the first column device 1000 not to depressurize and remain a high pressure to continue producing pure ethanol (bioethanol); The valve 2314 is digital and is fully open (on/off), it receives the purified product from the first and second column devices 1000 and 1000', and sends the purified product directly to a condenser since the purified product is at high pressure and must be obtained in liquid form. Then, for the depressurization step in the second column device 1000': Valve 2323 is fully open and is a digital on/off valve, allowing the second column device to depressurize from the bottom in order to remove the water easily both in the liquid phase and the release of the zeolite active sites; The valve 2324 is proportional (analog), and has an opening of 90%, this opening allows a depressurization considered to be carried out to reach 0.5 bar close to the purge pressure, this valve 2324 is located in such a way that it can be used for the first and second column devices 1000 and 1000' in the depressurization step, high concentrations of water come out of this valve (2324), this water can be reused to be introduced again into the boiler and exit in the vapor phase.
[0051 ] -Adsorción en el primer dispositivo de columna 1000 y purga en el segundo dispositivo de columna 1000’. Las válvulas 2321 , 2326, 2312 y 2327 están habilitadas para realizar la adsorción y producción utilizando el primer dispositivo de columna 1000’, mientras el segundo dispositivo de columna 1000’ realiza el paso de purga habilitando las válvulas 2323, 2325, 2324 y 2313. Estos pasos se llevan en el mismo periodo de tiempo durante 20 segundos: La válvula 2321 recibe la alimentación principal proveniente de la caldera de vapor con una mezcla de 90% en peso de etanol y 10 % en peso de agua; la válvula 2321 está totalmente abierta (es una válvula digital on/off); la válvula 2327 recibe parte de la alimentación proveniente de la válvula 2321. Esta 2327 válvula es proporcional (analógica) y tiene una apertura del 70%, ya que permitirá introducir vapor sobresaturado y mantener una presión elevada; la válvula 2312 es proporcional (analógica) y tiene una apertura del 30%, esta válvula se ubica en la parte superior para obtener el producto purificado obtenido del primer dispositivo de columna 1000. El motivo por el cual esta válvula 2312 tiene una apertura del 30% es porque permitirá que el primer dispositivo de columna no se despresurice y se mantenga una presión elevada para seguir la producción etanol puro (bioetanol); la válvula 2314 es digital y tiene está totalmente abierta (on/off). Esta recibe el producto purificado del primer y segundo dispositivos de columna 1000 y 1000’, y manda el producto purificado directamente a un condensador ya que el producto purificado está a alta presión y debe de obtenerse de manera líquida. Luego, la configuración de las válvulas por 20 segundos en el paso de purga para el segundo dispositivo de columna 1000’ consiste en: La válvula 231 1 es proporcional (analógica) y tiene una apertura del 5%, por esta válvula pasa un flujo que comparten el primer dispositivo de columna 1000 hacia el segundo dispositivo de columna 1000’, es un producto purificado que lleva concentraciones de etanol elevado en comparación con la composición de alimentación (90% etanol y 20% agua). El motivo por el cual se tiene es apertura tan pequeña es para hacer pasar o recircular un flujo gaseoso con una pureza mayor a la de la alimentación, de tal manera que cuando se pasa por el segundo dispositivo de columna 1000’ se recircula y realiza la purga, pero por un corto tiempo de 20 segundos, esto permitirá que cuando se represuñce ya exista etanol elevado en pureza para ser producido por el segundo dispositivo de columna 1000’, otro de los motivos por el cual se tiene esa apertura del 5 % es para que no exista una caída de presión en el primer dispositivo de columna 1000 y todo el producto purificado se pierda en el primer dispositivo de columna 1000; la válvula 2323 está totalmente abierta y es una válvula digital on/off. Esta válvula permite que el segundo dispositivo de columna 1000’ se purgue por la parte inferior, esto con el objetivo retirar el agua fácilmente tanto en fase liquida como, permitiendo liberar los sitios activos de las zeolitas; la válvula 2324 es proporcional (analógica), y tiene una apertura del 25%, está apertura permite que se realice una purga con un flujo pequeño pero a una elevada presión, esto permite que todos los sitios activos de las zeolitas se liberen y quede regenerado el segundo dispositivo de columna 1000’ y listo para el paso de represuñzación. Este paso se llega a una presión de vacío de 0.25 bar. La válvula 2324 está ubicada de tal manera que pueda ser utilizada para el primer y segundo dispositivos de columna 1000 y 1000’ en el paso de purga. De esta válvula 2324 salen concentraciones de agua elevadas, esta agua se puede reutilizar para nuevamente ser introducida en la caldera y salga en fase vapor; la válvula 2325 está totalmente abierta (es una válvula digital on/off), en esta válvula 2325 está conectada a una bomba de vacío, el cual permite que se genere ese vacío que rompe el enlace débil que se ha formado entre la zeolita y la molécula de agua; la válvula 2325 está colocada de esa manera para succionar solo el vapor de agua y no obstruya por gravedad el agua líquida que pasa a través de la válvula 2324. [0051] -Adsorption in the first column device 1000 and purge in the second column device 1000'. Valves 2321, 2326, 2312 and 2327 are enabled to perform adsorption and production using the first column device 1000', while the second column device 1000' performs the purge step by enabling valves 2323, 2325, 2324 and 2313. These steps are They have been in the same period of time for 20 seconds: Valve 2321 receives the main feed from the steam boiler with a mixture of 90% by weight of ethanol and 10% by weight of water; valve 2321 is fully open (it is a digital on/off valve); Valve 2327 receives part of the power from valve 2321. This valve 2327 is proportional (analog) and has an opening of 70%, since it will allow supersaturated steam to be introduced and maintain a high pressure; The valve 2312 is proportional (analog) and has a 30% opening, this valve is located at the top to obtain the purified product obtained from the first column device 1000. The reason why this valve 2312 has a 30% opening % is because it will allow the first column device not to depressurize and maintain a high pressure to continue producing pure ethanol (bioethanol); The 2314 valve is digital and is fully open (on/off). It receives the purified product from the first and second column devices 1000 and 1000', and sends the purified product directly to a condenser since the purified product is under high pressure and must be obtained in liquid form. Then, the configuration of the valves for 20 seconds in the purge step for the second column device 1000' consists of: Valve 231 1 is proportional (analog) and has an opening of 5%, through this valve a flow passes that share the first column device 1000 towards the second column device 1000', is a purified product that carries high ethanol concentrations compared to the feed composition (90% ethanol and 20% water). The reason why there is such a small opening is to pass or recirculate a gas flow with a purity greater than that of the feed, in such a way that when it passes through the second column device 1000' it is recirculated and performs the purge, but for a short time of 20 seconds, this will allow that when reprising there is already high purity ethanol to be produced by the second column device 1000', another reason why there is that 5% opening is so that there is no pressure drop in the first column device 1000 and all of the purified product is lost in the first column device 1000; valve 2323 is fully open and is a digital on/off valve. This valve allows the second column device 1000' to be purged from the bottom, this in order to easily remove the water both in the liquid phase and, allowing the active sites of the zeolites to be released; valve 2324 is proportional (analog), and has an opening of 25%, this opening allows a purge to be carried out with a small flow but at a high pressure, this allows all the active sites of the zeolites to be released and the second column device is regenerated 1000' and ready for the represumption step. This step is reached at a vacuum pressure of 0.25 bar. Valve 2324 is located so that it can be used for the first and second column devices 1000 and 1000' in the purge step. High concentrations of water come out of this valve 2324, this water can be reused to be introduced into the boiler again and come out in the vapor phase; The valve 2325 is completely open (it is a digital on/off valve), in this valve 2325 it is connected to a vacuum pump, which allows the vacuum to be generated that breaks the weak bond that has formed between the zeolite and the water molecule; valve 2325 is positioned that way to suck in only the water vapor and does not obstruct by gravity the liquid water passing through valve 2324.
[0052] -Adsorción en el primer dispositivo de columna 1000 e igualación en el segundo dispositivo de columna 1000’. Las válvulas 2321 , 2326, 2312 y 2327 están habilitadas para realizar la adsorción y producción utilizando el primer dispositivo de columna 1000, mientras el segundo dispositivo de columna 1000’ realiza el paso de purga habilitando la válvula 231 1. Estos pasos se llevan en el mismo periodo de tiempo durante 50 segundos. A continuación, se observa la configuración de las válvulas por 50 segundos en el paso de adsorción para el primer dispositivo de columna 1000: La válvula 2321 recibe la alimentación principal proveniente de la caldera de vapor con una mezcla de 90% en peso de etanol y 10% en peso de agua. La válvula 2321 está totalmente abierta (es una válvula digital on/off); La válvula 2327 recibe parte de la alimentación proveniente de la válvula 2321 . Esta válvula es proporcional (analógica) y tiene una apertura del 70%, ya que estos permitirán introducir vapor sobresaturado y mantener una presión elevada; La válvula 2312 es proporcional (analógica) y tiene una apertura del 5%. Esta válvula está ubicada en la parte superior para obtener el producto purificado obtenido del primer dispositivo de columna 1000. El motivo por el cual está tiene una apertura del 5% es porque permitirá que el primer dispositivo de columna 1000 no se despresurice y se pueda hacer la igualación de presiones en el primer y segundo dispositivos de columna 1000, 1000’, pasando por la válvula 231 1 y manteniendo una presión elevada para seguir producción etanol puro (bioetanol); la válvula 2327 es digital y tiene está totalmente abierta (on/off). Esta recibe el producto purificado del primer y segundo dispositivos de columna 1000, 1000’, y manda el producto purificado directamente a un condensador ya que el producto purificado está a alta presión y debe de obtenerse de manera líquida. Luego, en la configuración de las válvulas por 50 segundos en el paso de igualación para el segundo dispositivo de columna 1000’: La válvula 231 1 es proporcional (analógica) y tiene una apertura del 50%, esto permitirá que entre más flujo de gas hacia el segundo dispositivo de columna 1000’ y que a su vez el primer dispositivo de columna 1000 siga produciendo bioetanol, pero con una producción menor, esto por la reducción de la válvula al 5%. Esta es una gran ventaja ya que se está introduciendo etanol puro en una columna regenerada, por lo tanto, al entrar al segundo dispositivo de columna 1000’ permitirá purificar más el etanol, este paso es cíclico por lo tanto también se presentará para el primer dispositivo de columna 1000, dando como resultado elevar la pureza del producto purificado obtenido. [0052] -Adsorption in the first column device 1000 and equalization in the second column device 1000'. Valves 2321, 2326, 2312 and 2327 are enabled to perform adsorption and production using the first column device 1000, while the second column device 1000' performs the purge step by enabling valve 231 1. These steps are carried out in the same period of time for 50 seconds. Below, the valve configuration is observed for 50 seconds in the adsorption step for the first column device 1000: Valve 2321 receives the main feed from the steam boiler with a mixture of 90% by weight of ethanol and 10% by weight of water. Valve 2321 is fully open (it is a digital on/off valve); Valve 2327 receives part of the power from valve 2321. This valve is proportional (analog) and has an opening of 70%, since this will allow supersaturated steam to be introduced and maintain a high pressure; The 2312 valve is proportional (analog) and has a 5% opening. This valve is located at the top to obtain the purified product obtained from the first column device 1000. The reason why it has a 5% opening is because it will allow the first column device 1000 not to depressurize and can be made equalizing pressures in the first and second column devices 1000, 1000', passing through the valve 231 1 and maintaining high pressure to continue producing pure ethanol (bioethanol); The 2327 valve is digital and is fully open (on/off). It receives the purified product from the first and second column devices 1000, 1000', and sends the purified product directly to a condenser since the purified product is under high pressure and must be obtained in liquid form. Then, in setting the valves for 50 seconds in the equalization step for the second column device 1000': Valve 231 1 is proportional (analog) and has a 50% opening, this will allow more gas flow to enter towards the second column device 1000' and in turn the first column device 1000 continues to produce bioethanol, but with a lower production, this due to the reduction of the valve to 5%. This is a great advantage since pure ethanol is being introduced into a regenerated column, therefore, entering the second column device 1000' will allow further purification of the ethanol, this step is cyclic therefore it will also be presented for the first device of column 1000, resulting in increasing the purity of the purified product obtained.
[0053] -Adsorción en el primer dispositivo de columna 1000 y represuhzación en el segundo dispositivo de columna 1000’. Las válvulas 2312 y 2327 están habilitadas para realizar la adsorción y producción utilizando el primer dispositivo de columna 1000, mientras el segundo dispositivo de columna 1000’ realiza el paso de purga habilitando las válvulas 2321 y 2322. Estos pasos se llevan en el mismo periodo de tiempo durante 80 segundos. A continuación, se observa la configuración de las válvulas por 80 segundos en el paso de adsorción para el primer dispositivo de columna 1000: La válvula 2312 es proporcional (analógica) y tiene una apertura del 30%. Esta válvula 2312 está ubicada en la parte superior para obtener el producto purificado obtenido del primer dispositivo de columna 1000. Nuevamente tiene una apertura del 30% la válvula 2321 , en el primer dispositivo de columna 1000 ya no hay alimentación, se dejan solamente abiertas las válvulas 2312 y 2313 para que todo el gas que suba se vaya purificando, para este caso solo el etanol subirá ya que tiene un punto de ebullición menor al del agua, por lo tanto, el agua quedara adsorbida y en la parte inferior de la columna; La válvula 231 1 es digital y tiene está totalmente abierta (on/off). Esta recibe el producto purificado del primer y segundo dispositivos de columna 1000, 1000’, y manda el producto purificado directamente a un condensador ya que el producto purificado está a alta presión y debe de obtenerse de manera líquida. Luego, en la configuración de las válvulas por 50 segundos en el paso de represuhzación para el segundo dispositivo de columna 1000’: La válvula 2321 recibe la alimentación principal proveniente de la caldera de vapor con una mezcla de 90% en peso de etanol y 10 % en peso de agua, la válvula 2321 está totalmente abierta (es una válvula digital on/off) ; La válvula 2322 recibe parte de la alimentación de proveniente de la válvula 2321 , la válvula 2322 es proporcional (analógica) y tiene una apertura del 70%, ya que permitirá introducir vapor sobresaturado y mantener una presión elevada. Esta válvula 2322 permite el flujo de vapor que ingresará al segundo dispositivo de columna 1000’ hasta llegar una presión elevada de 4 bar. [0053] -Adsorption in the first column device 1000 and repressure in the second column device 1000'. Valves 2312 and 2327 are enabled to perform adsorption and production using the first column device 1000, while the second column device 1000' performs the purge step by enabling valves 2321 and 2322. These steps are carried out in the same period of time. time for 80 seconds. Below is the valve configuration for 80 seconds in the adsorption step for the first column device 1000: Valve 2312 is proportional (analog) and has a 30% opening. This valve 2312 is located at the top to obtain the purified product obtained from the first column device 1000. Again, valve 2321 has a 30% opening, in the first column device 1000 there is no longer a feed, only the valves are left open. valves 2312 and 2313 so that all the gas that rises is purified, in this case only the ethanol will rise since it has a lower boiling point than water, therefore, the water will be adsorbed and at the bottom of the column ; Valve 231 1 is digital and is fully open (on/off). It receives the purified product from the first and second column devices 1000, 1000', and sends the product purified directly to a condenser since the purified product is under high pressure and must be obtained in liquid form. Then, in the valve configuration for 50 seconds in the repressure step for the second column device 1000': Valve 2321 receives the main feed from the steam boiler with a mixture of 90% by weight of ethanol and 10 % by weight of water, valve 2321 is fully open (it is a digital on/off valve); Valve 2322 receives part of the feed from valve 2321, valve 2322 is proportional (analog) and has an opening of 70%, since it will allow supersaturated steam to be introduced and maintain a high pressure. This valve 2322 allows the flow of steam that will enter the second column device 1000' until a high pressure of 4 bar is reached.
[0054] La composición de la mezcla bioetanol y agua debe de estar cerca del punto azeotrópico, dando como fracción molar: 0.78 en bioetanol (90% en peso de bioetanol) y 0.22 en agua (10% en peso de agua). La presión de alimentación debe de estar en 200 kPa o arriba de ese valor, con el fin de llevar a cabo el paso de adsorción sobre las moléculas de agua y producir bioetanol. La temperatura debe de estar en 373.15 K (100°C) o arriba de ese valor, esto para seguir manteniendo el vapor en la parte interna de los dispositivos de columna empacados con zeolitas y favorecer los pasos de regeneración de las zeolitas y poder ser utilizadas nuevamente en el paso de adsorción. Para inyectar el flujo de vapor, es necesario la implementación de una caldera de vapor de 3 BPH (45 kg/h) o de más potencia a través de la válvula 2321 . Los dispositivos de columnas produjeron 40 kg/h de bioetanol con la alimentación de 45 kg/h. Además, el tiempo es más corto en comparación a otros procesos, los dispositivos de columnas empiezan a producir una pureza del 99% después de 2 h. [0054] The composition of the bioethanol and water mixture must be close to the azeotropic point, giving as a mole fraction: 0.78 in bioethanol (90% by weight of bioethanol) and 0.22 in water (10% by weight of water). The feed pressure must be at 200 kPa or above that value, in order to carry out the adsorption step on the water molecules and produce bioethanol. The temperature must be at 373.15 K (100°C) or above that value, this to continue maintaining the vapor in the internal part of the column devices packed with zeolites and favor the regeneration steps of the zeolites and be able to be used again in the adsorption step. To inject the steam flow, it is necessary to implement a 3 BPH (45 kg/h) steam boiler or more power through valve 2321. The column devices produced 40 kg/h of bioethanol with the feed of 45 kg/h. In addition, the time is shorter compared to other processes, column devices begin to produce 99% purity after 2 h.
[0055] Como parte de los controles de monitoreo se registraron los valores de temperatura y presión a lo largo del proceso. En la figura 5, se ¡lustran los perfiles de temperatura desde el arranque del proceso hasta llegar a un estado estable cíclico, se puede apreciar que en el nodo 1 (equivalente a 0.15 m) parte inicial del dispositivo de columna, la temperatura se mantiene estable y en el nodo 20 (equivalente a 1 m) la temperatura decae, esto es debido a que el flujo de vapor entra por los primeros nodos del dispositivo de columna, existiendo un decremento de temperatura a Io largo de la parte axial. Se caracteriza por que el estado estable cíclico se cumple después de 2 h. [0055] As part of the monitoring controls, the temperature and pressure values were recorded throughout the process. Figure 5 illustrates the temperature profiles from the start of the process until reaching a cyclic stable state. It can be seen that in node 1 (equivalent to 0.15 m) initial part of the column device, the temperature is maintained stable and at node 20 (equivalent to 1 m) the temperature decreases, this is because the steam flow enters through the first nodes of the column device, there being a decrease temperature along the axial part. It is characterized by the fact that the cyclic stable state is met after 2 h.
[0056] Por otro lado, en la figura 6, se ¡lustran los perfiles de pureza de bioetanol y agua en fracción molar, donde se logra observar como la pureza de bioetanol se logró a partir de las 2 h, con una composición molar de alimentación de 0.78 de bioetanol y 0.22 de agua, hasta lograr una pureza de bioetanol de 0.985 de bioetanol y 0.015 de agua. Cabe mencionar que se muestran dos resultados diferentes ya que una prueba es con valores nominales de arranque y la segunda prueba fue bajo los resultados obtenidos, considerando valores óptimos que mejoren la pureza a partir de composiciones más bajas. La figura 7 ¡lustra el perfil de temperatura al largo del dispositivo de columna durante 1 ciclo del proceso, donde se muestra como la temperatura se mantiene y decrece por los cambios oscilatorios de presión. [0056] On the other hand, Figure 6 illustrates the purity profiles of bioethanol and water in mole fraction, where it is possible to observe how the purity of bioethanol was achieved after 2 h, with a molar composition of feeding 0.78 bioethanol and 0.22 water, until achieving a bioethanol purity of 0.985 bioethanol and 0.015 water. It is worth mentioning that two different results are shown since one test is with nominal starting values and the second test was based on the results obtained, considering optimal values that improve purity from lower compositions. Figure 7 illustrates the temperature profile along the column device during 1 cycle of the process, showing how the temperature is maintained and decreased by oscillatory pressure changes.
[0057] La figura 8 ¡lustra el comportamiento dinámico del perfil de la presión interna en el dispositivo de columna, al realizar la adsorción con una presión de 2 bar, una despresuhzación hasta llegar a una presión de 0.5 bar, está es cercana al vació, posteriormente una purga realizándola con una presión de 0.2 bar y por último una represuhzación que va de 0.2 bar a 2 bar, esto cumple con un ciclo del proceso. Este perfil es cíclico, por lo tanto, se presentará nuevamente hasta llegar al estado estable cíclico y alcanzado la pureza de bioetanol de 0.985 en fracción molar, con el objetivo de cumplir con las normas internacionales de pureza para poder ser utilizado como carburante. [0057] Figure 8 illustrates the dynamic behavior of the internal pressure profile in the column device, when performing adsorption with a pressure of 2 bar, depressurization until reaching a pressure of 0.5 bar, which is close to vacuum. , subsequently a purge carried out with a pressure of 0.2 bar and finally a repressure that goes from 0.2 bar to 2 bar, this complies with one cycle of the process. This profile is cyclic, therefore, it will be presented again until the cyclic stable state is reached and the bioethanol purity of 0.985 in mole fraction is reached, with the aim of complying with international purity standards to be able to be used as fuel.
[0058] En consecuencia, del ejemplo anterior es evidente para un técnico en la materia la disposición de las válvulas para la configuración de un sistema continuo que utiliza más de dos dispositivos de columnas. [0058] Consequently, from the previous example it is evident to a person skilled in the art the arrangement of the valves for the configuration of a continuous system that uses more than two column devices.
[0059] De conformidad con lo anteriormente descrito, será evidente para cualquier experto en la materia que las modalidades del sistema y del dispositivo de columna de adsorción por oscilación de presión que utilicen sensores de temperatura intercambiables acoplados al cuerpo de la columna, así como la configuración del sistema según se describió anteriormente e ¡lustró en los dibujos que se acompañan, son únicamente ilustrativas más no limitativas de la presente invención, ya que son posibles numerosos cambios de consideración en sus detalles sin apartarse del alcance de la invención. [0059] In accordance with the above, it will be evident to any person skilled in the art that the modalities of the pressure swing adsorption column system and device that use interchangeable temperature sensors coupled to the body of the column, as well as the system configuration as described above and illustrated in the accompanying drawings, are solely illustrative and not limiting of the present invention, since numerous considerable changes in its details are possible without departing from the scope of the invention.
[0060] Por lo tanto, la presente invención no deberá considerarse como restringida excepto por lo que exija la técnica anterior y por el alcance de las reivindicaciones anexas. [0060] Therefore, the present invention should not be considered restricted except as required by the prior art and by the scope of the appended claims.

Claims

Reivindicaciones Claims
[Reivindicación 1 ] i Un dispositivo de columna de adsorción por oscilación de presión para la purificación de un compuesto de interés, caracterizado porque comprende: una sección interior; una sección exterior; una pluralidad de sensores de temperatura intercambiables; una sección inferior; y una sección superior, en donde la sección interior incluye una pared interior que define un diámetro interior entre 0.28 m y 0.32 m, la sección interior comprende una pluralidad de alojamientos interiores para sensores de temperatura y está configurada para permitir el paso del compuesto de interés, y para alojar por lo menos un sensor de temperatura intercambiable, en donde la sección exterior comprende una pluralidad de alojamientos exteriores para sensores de temperatura que está alineada con la pluralidad de alojamientos interiores para sensores de temperatura y está configurada para alojar a cada sensor de temperatura de la pluralidad de sensores de temperatura intercambiables, en donde la pluralidad de sensores de temperatura intercambiables está configurada para ensamblarse con la pluralidad de alojamientos exteriores e interiores y para medir la temperatura en un centro de la sección interior, en donde la sección inferior está configurada para recibir una entrada de vacío y una entrada de alimentación, en donde la sección superior está configurada para recircular y extraer un producto purificado; y en donde el dispositivo de columna de adsorción define una altura entre 0.8 m y 1 .5 m. [Claim 1] i A pressure swing adsorption column device for the purification of a compound of interest, characterized in that it comprises: an interior section; an outer section; a plurality of interchangeable temperature sensors; a lower section; and an upper section, wherein the interior section includes an interior wall that defines an interior diameter between 0.28 m and 0.32 m, the interior section comprises a plurality of interior housings for temperature sensors and is configured to allow the passage of the compound of interest, and for housing at least one interchangeable temperature sensor, wherein the outer section comprises a plurality of outer temperature sensor housings that is aligned with the plurality of inner temperature sensor housings and is configured to house each temperature sensor. of the plurality of interchangeable temperature sensors, wherein the plurality of interchangeable temperature sensors is configured to assemble with the plurality of exterior and interior housings and to measure the temperature at a center of the interior section, wherein the bottom section is configured to receive a vacuum inlet and a feed inlet, wherein the upper section is configured to recirculate and extract a purified product; and where the adsorption column device defines a height between 0.8 m and 1.5 m.
[Reivindicación 2] El dispositivo de conformidad con la reivindicación i , caracterizado además porque el adsorbente es zeolita natural o sintética. [Claim 2] The device according to claim i, further characterized in that the adsorbent is natural or synthetic zeolite.
[Reivindicación 3] El dispositivo de conformidad con la reivindicación 2, caracterizado además porque la zeolita es natural. [Claim 3] The device according to claim 2, further characterized in that the zeolite is natural.
[Reivindicación 4] El dispositivo de conformidad con la reivindicación 1 , caracterizado además porque la sección superior del dispositivo de columna comprende una salida de extracción, una conexión analógica, y una conexión digital; en donde la salida de extracción está configurada para extraer un producto purificado, en donde la conexión analógica está configurada para conectarse a un manómetro analógico para medir la presión en la sección interior, y en donde la conexión digital está configurada para conectarse con un sensor digital de presión que envía datos a un módulo de adquisición de datos. [Claim 4] The device according to claim 1, further characterized in that the upper section of the column device comprises an extraction output, an analog connection, and a digital connection; wherein the extraction outlet is configured to extract a purified product, wherein the analog connection is configured to connect to an analog pressure gauge to measure the pressure in the inner section, and wherein the digital connection is configured to connect to a digital sensor pressure sensor that sends data to a data acquisition module.
[Reivindicación 5] El dispositivo de conformidad con la reivindicación 1 , caracterizado además porque la sección inferior del dispositivo de columna de adsorción por oscilación de presión comprende adicionalmente una malla de acero inoxidable que es colocada en una brida inferior que está ubicada en la sección inferior del dispositivo de columna de adsorción por oscilación de presión, la malla de acero inoxidable está configurada para la retención y empaquetamiento del material adsorbente. [Claim 5] The device according to claim 1, further characterized in that the lower section of the pressure swing adsorption column device further comprises a stainless steel mesh that is placed in a lower flange that is located in the lower section of the pressure swing adsorption column device, the stainless steel mesh is configured for the retention and packing of the adsorbent material.
[Reivindicación 6] Un sistema de adsorción por oscilación de presión, caracterizado porque comprende: a) al menos dos dispositivos de columna de adsorción por oscilación de conformidad con la reivindicación 1 ; b) una pluralidad de válvulas y tuberías que están conectadas con cada dispositivo de columna, con por lo menos un módulo de vacío, con un módulo de alimentación y con un módulo de condensador, y están configuradas para regular el flujo que pasa a través de cada válvula; c) por lo menos un módulo de vacío que está conectado a cada dispositivo de columna mediante la pluralidad de válvulas y tuberías, y está configurado para generar un vacío en la sección interior de cada dispositivo; d) un módulo de adquisición de datos que está conectado con cada sensor de la pluralidad de sensores de temperatura intercambiables y con por lo menos un manómetro que mide la presión en la sección interior de cada dispositivo; e) un módulo de alimentación que está conectado con cada dispositivo mediante la pluralidad de válvulas y tuberías, y está configurado para alimentar con vapor de agua la sección interior de cada dispositivo; y f) un módulo de condensador que está conectado con cada dispositivo mediante la pluralidad de válvulas y tuberías y está configurado para recibir un producto purificado. [Claim 6] A pressure swing adsorption system, characterized in that it comprises: a) at least two swing adsorption column devices according to claim 1; b) a plurality of valves and pipes that are connected to each column device, to at least one vacuum module, to a feed module and to a condenser module, and are configured to regulate the flow passing through each valve; c) at least one vacuum module that is connected to each column device through the plurality of valves and pipes, and is configured to generate a vacuum in the interior section of each device; d) a data acquisition module that is connected to each sensor of the plurality of interchangeable temperature sensors and to at least one pressure gauge that measures the pressure in the interior section of each device; e) a power module that is connected to each device through the plurality of valves and pipes, and is configured to feed water vapor to the interior section of each device; and f) a condenser module that is connected to each device by the plurality of valves and pipes and is configured to receive a purified product.
[Reivindicación 7] El sistema de conformidad con la reivindicación 6, caracterizado además porque el módulo de alimentación es un compresor o una caldera. [Claim 7] The system according to claim 6, further characterized in that the power module is a compressor or a boiler.
[Reivindicación 8] El sistema de conformidad con la reivindicación 6, caracterizado además porque el módulo de vacío es una bomba de vacío. [Claim 8] The system according to claim 6, further characterized in that the vacuum module is a vacuum pump.
[Reivindicación 9] El sistema de conformidad con la reivindicación 6, caracterizado además porque el módulo de condensador es un condensador. [Claim 9] The system according to claim 6, further characterized in that the capacitor module is a capacitor.
[Reivindicación 10] El sistema de conformidad con la reivindicación 6, caracterizado además porque el módulo de adquisición de datos comprende: un sistema de cómputo y un sistema de control PLC, en donde el módulo de adquisición de datos está conectado adicionalmente con la pluralidad de válvulas y tuberías, con el módulo de vacío, con el módulo de alimentación y con el módulo de condensador y está configurado para controlar el funcionamiento de cada uno. [Claim 10] The system according to claim 6, further characterized in that the data acquisition module comprises: a computing system and a PLC control system, wherein the data acquisition module is additionally connected to the plurality of valves and pipes, with the vacuum module, with the power module and with the condenser module and is configured to control the operation of each one.
[Reivindicación 1 1 ] El sistema de conformidad con la reivindicación 6, caracterizado además porque la pluralidad de válvulas y tuberías comprende: una pluralidad de válvulas y tuberías superior que está conectada con el módulo de condensador; y una pluralidad de válvulas y tuberías inferior que está conectada con el módulo de vacío y con el módulo de alimentación. [Claim 1 1] The system according to claim 6, further characterized in that the plurality of valves and pipes comprises: an upper plurality of valves and pipes that is connected to the condenser module; and a plurality of lower valves and pipes that are connected to the vacuum module and the power module.
[Reivindicación 12] Un método para purificar un compuesto de interés, caracterizado porque comprende las etapas de: (i) suministrar el compuesto de interés a un dispositivo de columna de adsorción por oscilación de conformidad con la reivindicación 1 , a través de un módulo de alimentación; (¡i) adsorber el compuesto de interés controlando la presión y temperatura; (iii) despresurizar el dispositivo de columna liberando el vapor residual; (iv) purgar el dispositivo de columna; y (v) represurizar el dispositivo de columna. [Claim 12] A method for purifying a compound of interest, characterized in that it comprises the steps of: (i) supplying the compound of interest to a swing adsorption column device according to claim 1, through a module of feeding; (i) adsorb the compound of interest by controlling the pressure and temperature; (iii) depressurize the column device by releasing residual vapor; (iv) purge the column device; and (v) repressurize the column device.
[Reivindicación 13] El método de conformidad con la reivindicación 12, caracterizado además porque el compuesto de interés es bioetanol con un 99% de pureza. [Claim 13] The method according to claim 12, further characterized in that the compound of interest is bioethanol with 99% purity.
[Reivindicación 14] El método de conformidad con la reivindicación 13, caracterizado además porque las condiciones de purificación del bioetanol son las siguientes en cada una de las etapas del método: (i) suministrar una mezcla de bioetanol al 90 % (p/p) y agua al 10% (p/p) al dispositivo de columna de adsorción por oscilación de presión; (¡i) adsorber a una presión >400 kPa y una temperatura >373.[Claim 14] The method according to claim 13, further characterized in that the bioethanol purification conditions are the following in each of the steps of the method: (i) supplying a 90% (w/w) bioethanol mixture and 10% (w/w) water to the pressure swing adsorption column device; (i) adsorb at a pressure >400 kPa and a temperature >373.
15 K; (iii) despresurizar el dispositivo de columna disminuyendo la presión a al menos 50 kPa; (iv) purgar el dispositivo de columna disminuyendo la presión de 50 kPa a 10 kPa; y (v) represurizar el dispositivo de columna aumentando la presión de 10 kPa a 400 kPa. [Reivindicación 15] El método de conformidad con la reivindicación 12, caracterizado además porque el compuesto de interés es hidrogeno con un 99.9% de pureza. 15K; (iii) depressurize the column device by decreasing the pressure to at least 50 kPa; (iv) purge the column device by decreasing the pressure from 50 kPa to 10 kPa; and (v) repressurize the column device by increasing the pressure from 10 kPa to 400 kPa. [Claim 15] The method according to claim 12, further characterized in that the compound of interest is hydrogen with 99.9% purity.
[Reivindicación 16] El método de conformidad con la reivindicación 15, caracterizado además porque las condiciones de purificación del hidrogeno son las siguientes en cada una de las etapas del método: (i) suministrar una mezcla que comprende: H2 al 72.2 % (p/p), CH4 al 4.17% (p/p), CO al 2.03% (p/p) y CO2 al 21 .6% (p/p) al dispositivo de columna de adsorción por oscilación de presión; (¡i) adsorber a una presión >350 kPa y una temperatura >295 K; (iii) despresurizar el dispositivo de columna disminuyendo la presión a al menos 50 kPa; (iv) purgar el dispositivo de columna disminuyendo la presión de 50 kPa a 10 kPa; y (v) represurizar el dispositivo de columna aumentando la presión de 10 kPa a 400 kPa. [Claim 16] The method according to claim 15, further characterized in that the hydrogen purification conditions are the following in each of the steps of the method: (i) supplying a mixture comprising: H2 at 72.2% (w/ p), CH4 at 4.17% (w/w), CO at 2.03% (w/w) and CO2 at 21.6% (w/w) to the pressure swing adsorption column device; (i) adsorb at a pressure >350 kPa and a temperature >295 K; (iii) depressurize the column device by decreasing the pressure to at least 50 kPa; (iv) purge the column device by decreasing the pressure from 50 kPa to 10 kPa; and (v) repressurize the column device by increasing the pressure from 10 kPa to 400 kPa.
[Reivindicación 17] El método de conformidad con la reivindicación 12, caracterizado además porque el compuesto de interés es oxígeno con una pureza de entre 95% y 99.5%. [Claim 17] The method according to claim 12, further characterized in that the compound of interest is oxygen with a purity of between 95% and 99.5%.
[Reivindicación 18] El método de conformidad con la reivindicación 17, caracterizado además porque las condiciones de purificación del oxígeno son las siguientes en cada una de las etapas del método: (i) suministrar una mezcla que comprende: nitrógeno al 74.18% (p/p), oxígeno al 19.61 % (p/p), dióxido de carbono al 0.03% (p/p) y vapor de agua al 6.18% (p/p) al dispositivo de columna de adsorción por oscilación de presión; (¡i) adsorber a una presión >350 kPa y una temperatura >298.15 K; (iii) despresurizar el dispositivo de columna disminuyendo la presión a al menos 50 kPa; (iv) purgar el dispositivo de columna disminuyendo la presión de 50 kPa a 10 kPa; y (v) represurizar el dispositivo de columna aumentando la presión de 10 kPa a 400 kPa. [Claim 18] The method according to claim 17, further characterized in that the oxygen purification conditions are the following in each of the steps of the method: (i) supplying a mixture comprising: 74.18% nitrogen (w/ p), 19.61% (w/w) oxygen, 0.03% (w/w) carbon dioxide, and 6.18% (w/w) water vapor to the pressure swing adsorption column device; (i) adsorb at a pressure >350 kPa and a temperature >298.15 K; (iii) depressurize the column device by decreasing the pressure to at least 50 kPa; (iv) purge the column device by decreasing the pressure from 50 kPa to 10 kPa; and (v) repressurize the column device by increasing the pressure from 10 kPa to 400 kPa.
[Reivindicación 19] El método de conformidad con la reivindicación 12, caracterizado además porque el compuesto de interés es metano con una pureza de entre 95% y 99%. [Claim 19] The method according to claim 12, further characterized in that the compound of interest is methane with a purity of between 95% and 99%.
[Reivindicación 20] El método de conformidad con la reivindicación 19, caracterizado además porque las condiciones de purificación del metano son las siguientes en cada una de las etapas del método: (i) suministrar una mezcla que comprende: metano en una concentración de entre 50 y 75% (p/p) y dióxido de carbono en una concentración de entre 25 y 45% (p/p) al dispositivo de columna de adsorción por oscilación de presión; (¡i) adsorber a una presión >1200 KPa y una temperatura de entre 298 y 323 K; (iii) despresurizar el dispositivo de columna disminuyendo la presión a al menos 50 KPa; (iv) purgar el dispositivo de columna disminuyendo la presión de 50 kPa a 10 kPa; y (v) represurizar el dispositivo de columna aumentando la presión de 10 kPa a 400 kPa. [Claim 20] The method according to claim 19, further characterized in that the methane purification conditions are the following in each of the steps of the method: (i) supplying a mixture comprising: methane in a concentration of between 50 and 75% (w/w) and carbon dioxide in a concentration of between 25 and 45% (w/w) to the pressure swing adsorption column device; (i) adsorb at a pressure >1200 KPa and a temperature between 298 and 323 K; (iii) depressurize the column device by decreasing the pressure to at least 50 KPa; (iv) purge the column device by decreasing the pressure from 50 kPa to 10 kPa; and (v) repressurize the column device by increasing the pressure from 10 kPa to 400 kPa.
[Reivindicación 21 ] El método de conformidad con la reivindicación 12, caracterizado además porque el flujo del compuesto de interés es suministrado mediante un compresor de 175 psi. i [Claim 21] The method according to claim 12, further characterized in that the flow of the compound of interest is supplied by a 175 psi compressor. Yo
PCT/IB2023/056055 2022-06-14 2023-06-12 Pressure swing adsorption device, system and method for purifying a compound of interest WO2023242717A1 (en)

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