WO2018135164A1 - ガス分離回収方法及び設備 - Google Patents
ガス分離回収方法及び設備 Download PDFInfo
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- WO2018135164A1 WO2018135164A1 PCT/JP2017/043776 JP2017043776W WO2018135164A1 WO 2018135164 A1 WO2018135164 A1 WO 2018135164A1 JP 2017043776 W JP2017043776 W JP 2017043776W WO 2018135164 A1 WO2018135164 A1 WO 2018135164A1
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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
- 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
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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
- 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
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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
- 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
- B01D53/0407—Constructional details of adsorbing systems
- B01D53/0446—Means for feeding or distributing gases
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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
- 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
- B01D53/0476—Vacuum pressure swing adsorption
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/40—Carbon monoxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/50—Carbon dioxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/106—Silica or silicates
- B01D2253/108—Zeolites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/504—Carbon dioxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
- B01D2259/40028—Depressurization
- B01D2259/4003—Depressurization with two sub-steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
- B01D2259/40028—Depressurization
- B01D2259/40032—Depressurization with three sub-steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
- B01D2259/40028—Depressurization
- B01D2259/40033—Depressurization with more than three sub-steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
- B01D2259/40043—Purging
- B01D2259/4005—Nature of purge gas
- B01D2259/40056—Gases other than recycled product or process gas
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
Definitions
- the present invention relates to a gas separation and recovery method by a pressure swing adsorption method (PSA method) and equipment suitable for its implementation.
- PSA method pressure swing adsorption method
- PSA method Pressure Swing Adsorption method
- PSA method is a separation method that utilizes the fact that the amount of gas component adsorbed on the adsorbent varies depending on the gas species and its partial pressure.
- the step of adsorbing the gas component on the adsorbent In order to increase the adsorption rate of gas components, a process of supplying a part of the desorbed gas desorbed by other adsorption towers as a cleaning gas (cleaning process), and desorbing the adsorbed gas components from the adsorbent and recovering the gas A process (desorption process).
- cleaning process a process of supplying a part of the desorbed gas desorbed by other adsorption towers as a cleaning gas
- desorption process desorbing the adsorbed gas components from the adsorbent and recovering the gas A process
- the PSA method has a pressurization method using a pressure difference between pressurization and normal pressure, and a suction method using a pressure difference between normal pressure (or slight pressurization) and depressurization.
- the latter is a VSA method (Vacuum Swing Adsorption) Sometimes called.
- the PSA method requires a large amount of power for gas separation, it is necessary to reduce the power consumption in the PSA method in order to reduce the gas separation cost.
- the power consumption of the gas compressor for increasing the adsorption pressure in the adsorption process and in the suction method PSA method, the power consumption of the vacuum pump in the desorption process is the power consumption required for gas separation. It accounts for a major proportion of them.
- These power consumptions increase as the amount of gas for adsorption and desorption increases.
- the concentration of the recovered gas becomes low.
- the concentration of the recovered gas can be increased.
- the desorption gas is adsorbed again on the adsorbent. Since it is sent to the desorption process, the amount of gas to be desorbed increases and the power consumption also increases.
- the object of the present invention is to solve the above-mentioned problems of the prior art, and to increase the concentration of the recovered gas without performing a cleaning process.
- An object of the present invention is to provide a gas separation and recovery method and equipment capable of separating and recovering components.
- gas adsorbents have different adsorption / desorption characteristics corresponding to adsorption force and pressure depending on the gas type, and there is a desorption timing difference depending on the gas type in the desorption process, and this desorption timing difference is used.
- a new gas separation and recovery method has been devised in which the desorbed gas is recovered in two or more time zones to selectively separate and recover a high concentration target gas component. That is, the gist of the present invention for solving the above problems is as follows.
- an adsorption step in which the gas component is adsorbed by an adsorbent packed in an adsorption tower, and the adsorbent adsorbed in the adsorption step
- a gas separation and recovery method in which the gas is divided into zones and the desorbed gas is collected separately for each time zone.
- the adsorption tower in which the raw material gas is introduced from one end side and the raw material off-gas is discharged from the other end side during the adsorption step, A gas separation and recovery method that discharges desorbed gas from the end side.
- the adsorption tower is a vertical adsorption tower in which the gas flows in the vertical direction, and the gas flow direction in the process in which the gas flow velocity becomes maximum during operation is directed downward Gas separation and recovery method.
- a pressure release valve for reducing the pressure in the adsorption tower is provided in the adsorption tower, and before the pressure in the adsorption tower is reduced by a vacuum pump in the desorption process. And a gas separation and recovery method in which the pressure release valve is opened to lower the pressure in the adsorption tower.
- the gas in the desorption process, the gas is obtained by reducing the pressure in the adsorption tower with a vacuum pump in one or more time zones from the start of the process.
- a gas separation and recovery method in which gas is desorbed by introducing purge gas into the adsorption tower without using a vacuum pump in the subsequent time zone.
- the gas desorbed in a specific time zone has a higher calorie than the gas desorbed in other time zones.
- a gas separation and recovery method in which the desorption process is divided into a plurality of time zones, and the gas desorbed in the specific time zones is recovered as a high calorie gas.
- the source gas is a mixed gas containing CO and CO 2
- the gas desorbed in a specific time zone is desorbed in another time zone.
- Gas separation and recovery method in which the desorption process is divided into a plurality of time zones so that the CO concentration is higher than that of the gas.
- an adsorption process for adsorbing the gas component to the adsorbent packed in the adsorption tower, and the adsorbent adsorbed in the adsorption process It is a facility that has a desorption process for desorbing gas components and recovering the gas, and that does not have a cleaning process for supplying a part of the desorption gas of other adsorption towers as a cleaning gas, and exhausting the desorption gas
- a gas separation / recovery facility that branches into multiple lines, and that each branch line is provided with an open / close valve so that the gas desorbed in the desorption process can be collected through different branch lines for each time zone.
- the adsorption tower is a vertical adsorption tower in which the gas flows in the vertical direction, and the gas flow direction is downward in the process in which the gas flow velocity is greatest during operation.
- a gas separation and recovery facility with a gas supply / exhaust line for the adsorption tower.
- the gas separation / recovery facility according to any one of [8] to [10], wherein the desorption gas exhaust line is provided with a vacuum pump for depressurizing the interior of the adsorption tower.
- a gas separation and recovery facility having a pressure release valve for reducing the pressure.
- the concentration of the recovered gas can be increased without performing a cleaning step, and therefore, a high concentration target gas component can be separated and recovered with less power consumption.
- FIG. 1 is an explanatory view showing an embodiment of the gas separation and recovery method and equipment of the present invention.
- FIG. 2 is a graph showing adsorption / desorption characteristics corresponding to pressure for two types of gases having different adsorption forces on the adsorbent.
- FIG. 3 is an explanatory view showing another embodiment of the gas separation and recovery method and equipment of the present invention.
- FIGS. 4-1 is explanatory drawing which shows a part of process in other embodiment of the gas separation-and-recovery method and installation of this invention.
- FIG. 4-2 is an explanatory diagram showing another part of the process in the same embodiment as FIG. 4-1.
- FIG. 5 is an explanatory view showing another embodiment of the gas separation and recovery method and equipment of the present invention.
- FIG. 6 is an explanatory diagram showing the PSA experimental apparatus used in the examples.
- the gas separation and recovery method of the present invention is a method for separating and recovering a specific gas component from a raw material gas by a pressure swing adsorption method, an adsorption step for adsorbing a gas component on an adsorbent packed in an adsorption tower, and this adsorption step And a desorption step of desorbing the gas component adsorbed by the adsorbent to recover the gas, and no cleaning step of supplying a part of the desorption gas of the other adsorption tower as a cleaning gas.
- the concentration of the recovered gas can be increased, but the amount of gas to be desorbed increases and the power consumption increases.
- the desorption process in order to increase the concentration of the collected gas without performing the cleaning process, is divided into a plurality of time zones, and the desorption gas is collected for each time zone.
- the desorption gas exhaust lines branch into a plurality of branches, and each branch line is provided with an open / close valve, and the gas desorbed in the desorption process is collected through a different branch line for each time zone. It can be so.
- FIG. 2 is a graph showing adsorption / desorption characteristics corresponding to pressure for two types of gases having different adsorption forces on the adsorbent.
- 13X zeolite used as a CO 2 adsorbent has a linear adsorption characteristic with respect to pressure for a gas species having a small adsorbing power such as N 2 or CO as in gas 1 in FIG.
- a gas species having a large adsorption force such as CO 2 has a large adsorption amount and has a non-linear adsorption characteristic with respect to pressure, like the gas 2 in FIG.
- the desorption process is divided into two time zones, and the desorption gas is divided and collected for each time zone, whereby the recovered gas having a high concentration of gas 1 is collected. It is possible to separately collect the recovered gases having high concentrations of gas 2 and gas 2.
- the present invention makes it possible to increase the concentration of the recovered gas without performing a cleaning step in this way, and to selectively separate and recover a high concentration target gas component.
- FIG. 1 is an explanatory view showing an embodiment of the gas separation and recovery method and equipment of the present invention.
- the desorption process is divided into a first time zone and a second time zone, and the desorption gas is collected separately for each time zone.
- FIG. “Process” and (b) show “desorption process: first time zone”, and (c) show “desorption process: second time zone”, respectively.
- gas 1 and gas 2 shown in FIG. 2 in the following description, gas 1 has a linear adsorption characteristic with respect to pressure, and is desorbed in the process of depressurization from a high pressure state.
- the gas 2 has a non-linear adsorption characteristic with respect to the pressure, hardly desorbs in the high pressure state, and indicates a gas that is rapidly desorbed when the pressure is reduced to the low pressure state. The same applies to the other embodiments shown in FIGS.
- the adsorption tower 1 is a vertical adsorption tower in which gas flows in the vertical direction, and is filled with an adsorbent having different linearity of adsorption isotherm depending on the gas species as shown in FIG.
- One end side (lower end side) of the adsorption tower 1 is connected to a supply / exhaust pipe 2 for introducing a source gas and exhausting a desorption gas, and the supply / exhaust pipe 2 is configured to supply a source gas introduction line 4.
- the pipe and the exhaust pipe constituting the desorption gas exhaust line 5 are connected to each other.
- the other end side (upper end side) of the adsorption tower 1 is connected to an exhaust pipe constituting an exhaust line 3 for raw material off gas.
- the exhaust line 5 is provided with a vacuum pump 6 and its downstream side (pump discharge side) branches into branch lines 50a and 50b.
- on-off valves 7a and 7b are provided on the branch lines 50a and 50b.
- 8 is an open / close valve (shutoff valve) provided in the introduction line 4
- 9 is an open / close valve (shutoff valve) provided in the exhaust line 3.
- the open on-off valve is in an open state
- the black on-off on-off valve is in a closed state.
- the raw material gas is introduced into the adsorption tower 1 through the introduction line 4 and the raw material off-gas is discharged from the exhaust line 3.
- the desorption process is performed by depressurizing the inside of the adsorption tower 1 with the vacuum pump 6 without performing the cleaning process.
- the desorption gas (recovered gas A) is recovered through the branch line 50b for the purpose of recovering the gas 2 as shown in FIG. 1 (c). Gas B) is recovered.
- the on-off valves 7a and 7b are appropriately opened and closed (the same applies to the embodiments in FIGS. 3 to 5).
- the gas 1 has a linear adsorption characteristic with respect to pressure and is desorbed in the process of depressurization from a high pressure state
- the gas 2 has a non-linear adsorption characteristic with respect to pressure. Since it is a gas that is hardly desorbed in the high pressure state and is rapidly desorbed when the pressure is reduced to the low pressure state, the recovered gas A having a high concentration of gas 1 is obtained in the first time zone, and in the second time zone. A recovered gas B having a high concentration of the gas 2 is obtained.
- the target gas component for example, recovery gas A
- the time zone between the first time zone and the second time zone can be determined according to the adsorption / desorption characteristics of the adsorbent as shown in FIG. 2, the target concentration, heat quantity, target yield, etc. of the target gas component. Good.
- gas adsorbents have different adsorption / desorption characteristics (linearity of adsorption isotherm) corresponding to the adsorption force and pressure depending on the gas species as shown in FIG. 2, and such adsorbents may be used in the present invention. Therefore, there are no particular restrictions on the type of adsorbent, but particularly suitable adsorbents include ZSM-5 zeolite and NaA zeolite in addition to the 13X zeolite described above. 13X zeolite differs in the linearity of the adsorption isotherm especially for CO 2 and CO and N 2 . Also, ZSM-5 zeolite has different linearity of adsorption isotherm especially for CO 2 and CO (for example, Fig.
- Non-Patent Document 1 NaA zeolite has an adsorption isotherm especially for CO 2 and CH 4.
- the linearity is different (for example, Fig. 7 of Non-Patent Document 2).
- the type of adsorbent may be appropriately selected according to the gas type to be separated.
- the desorption process is divided into two time zones. However, depending on the type of adsorbent and the type of gas to be separated and recovered, the desorption step is divided into three or more time zones, and the desorption gas is separated. You may make it collect
- FIG. 3 is an explanatory view showing an embodiment of such a gas separation and recovery method and facility of the present invention.
- the desorption process is divided into a first time zone and a second time zone, and the desorption gas is collected separately for each time zone.
- FIG. , And (b) show “desorption process: first time zone”, and (c) show “desorption process: second time zone”, respectively.
- the adsorption tower 1 is a vertical adsorption tower in which gas flows in the vertical direction, and is filled with an adsorbent having different linearity of adsorption isotherm depending on the gas species as shown in FIG.
- a supply pipe constituting the source gas introduction line 4 is connected to one end side (upper end side) of the adsorption tower 1.
- the other end side (lower end side) of the adsorption tower 1 is connected to an exhaust pipe 10 for exhausting the raw material offgas and exhausting the desorbed gas.
- the pipe and the exhaust pipe constituting the desorption gas exhaust line 5 are connected to each other.
- Other configurations are the same as those in the embodiment of FIG. 1, and thus the same reference numerals are given and detailed descriptions thereof are omitted.
- the gas adsorption amount distribution in the adsorption tower 1 when the raw material gas is introduced is such that the gas 2 having a large adsorption force is adsorbed in a region near the raw material gas introduction port, and the gas 1 having a small adsorption force is disposed in a region far from the raw material gas introduction port. Adsorbs. This is due to a continuous change in the gas composition when the source gas flows through the adsorption tower 1. In the adsorption tower 1 in which such a gas adsorption amount distribution is generated, if the desorption gas is discharged from the same side as the raw material gas introduction side as in the embodiment of FIG. 1, a gas separation effect due to the difference in gas desorption timing can be obtained.
- the gas 1 having a small adsorption force when desorbed for the first time, it passes through the region where the gas 2 having a large adsorption force is adsorbed, so that the partial pressure of the gas 2 is reduced and the gas 2 is partially desorbed. As a result, the gas separation effect is reduced accordingly.
- the gas adsorption amount distribution in the adsorption tower 1 is as shown in FIG. 3A by discharging the desorption gas from the side opposite to the raw material gas introduction side as in this embodiment.
- the gas 1 having a low adsorption force is desorbed without passing through the region where the gas 2 having a high adsorption force is adsorbed, as shown in FIG. 3B. Therefore, the gas 2 is not partially desorbed, and the gas separation efficiency is improved as compared with the embodiment of FIG.
- the raw material gas is introduced into the adsorption tower 1 through the introduction line 4, and the raw material off-gas is discharged from the exhaust pipe 10 and the exhaust line 3.
- the desorption process is performed by depressurizing the inside of the adsorption tower 1 with the vacuum pump 6 without performing the cleaning process.
- the purpose is to recover the gas 1 as shown in FIG.
- the desorption gas (recovered gas A) is recovered through the branch line 50b for the purpose of recovering the gas 2 in the second time zone of the subsequent desorption process.
- Gas B) is recovered.
- the adsorption tower is a vertical adsorption tower in which the gas flows in the vertical direction as in the embodiment of FIG. 3, and the gas flow direction in the process in which the gas flow velocity is the largest during operation is downward.
- the deterioration of the adsorbent due to fluidization can be suppressed.
- a gas supply / exhaust line for the adsorption tower is provided so as to realize such a gas flow.
- the present invention uses the gas adsorption amount distribution in the adsorption tower 1, it is preferable to use a vertical adsorption tower in which gas flows in the vertical direction.
- the vertical adsorption tower has the same adsorbent filling amount. Since the sectional area of the tower is smaller than that of a horizontal adsorption tower or the like, the flow velocity of the gas flowing in the adsorbent packed bed is increased. In such an adsorption tower having a high gas flow rate, there is a concern that the adsorbent may be fluidized to promote deterioration of the adsorbent.
- the gas flow rate increases at the start of the adsorption process after depressurizing the adsorption tower 1 (at the start of the introduction of the raw material gas).
- the gas flow rate increases at the start of the gas release pressure after the adsorption process (a pressure release process as shown in FIG. 4B described later).
- the adsorption tower 1 is a vertical adsorption tower in which the gas flows in the vertical direction.
- the gas flow direction in the process is downward.
- FIG 3 shows the gas flow direction that satisfies such a condition.
- the movement of the adsorbent is constrained by a metal mesh or the like that supports the adsorbent. Deterioration can be prevented.
- the adsorption tower is provided with a pressure release valve for reducing the pressure in the tower, and before the pressure in the adsorption tower is reduced by a vacuum pump in the desorption process, the pressure relief valve is opened to reduce the pressure in the adsorption tower.
- FIG. 4 is an explanatory view showing an embodiment of such a gas separation and recovery method and facility of the present invention.
- FIG. 4 is a generic name of FIGS. 4-1 and 4-2.
- the desorption process is divided into a first time zone and a second time zone, and the desorption gas is collected separately for each time zone.
- FIG. , And (b) show a "pressure releasing step",
- (c) shows a "desorption step: first time zone”, and
- (d) shows a "desorption step: second time zone", respectively.
- the adsorption tower 1 is a vertical adsorption tower in which gas flows in the vertical direction, and is filled with an adsorbent having a different linearity of the adsorption isotherm depending on the gas type as shown in FIG. 2.
- a supply pipe constituting the source gas introduction line 4 is connected to one end side (upper end side) of the adsorption tower 1.
- the other end side (lower end side) of the adsorption tower 1 is connected to an exhaust pipe 10 for exhausting the raw material offgas and exhausting the desorbed gas.
- a pipe and an exhaust pipe constituting the desorption gas exhaust line 5 are connected to each other, and a pressure relief pipe 11 including a pressure relief valve 12 is connected.
- Other configurations are the same as those of the embodiment of FIGS. 1 and 3, and thus the same reference numerals are given and detailed description thereof is omitted.
- the desorption process is performed by depressurizing the inside of the adsorption tower 1 with a vacuum pump, and during that time, the depressurization speed is controlled by the control of the vacuum pump.
- the depressurization speed is controlled by the control of the vacuum pump.
- a pressure release step (FIG. 4B) is provided between the adsorption step (FIG. 4A) and the desorption step (FIG. 4C), and the pressure in the adsorption tower 1 is increased.
- the desorption process is performed after reducing the above.
- the raw material gas is introduced into the adsorption tower 1 through the introduction line 4, and the raw material off gas is discharged from the exhaust pipe 10 and the exhaust line 3.
- the pressure in the adsorption tower 1 is reduced by opening the pressure release valve 12 as shown in FIG. 4B without performing a washing process (pressure release process).
- the pressure release valve 12 is closed, and the desorption process is performed by reducing the pressure in the adsorption tower 1 with the vacuum pump 6. That is, in the first time zone of the desorption process, as shown in FIG.
- the desorption gas (recovered gas A) is collected through the branch line 50a for the purpose of collecting the gas 1, and the second time zone of the subsequent desorption process.
- the desorbed gas (recovered gas B) is recovered through the branch line 50b for the purpose of recovering the gas 2.
- the pressure release gas in the pressure release step is lower in concentration of the gas 1 than the recovered gas A, but since the gas 1 is a gas concentrated to some extent, it may be recovered and used for a specific application.
- the gas in the desorption process, is desorbed by depressurizing the inside of the adsorption tower with a vacuum pump in one or more time zones from the start of the process, and the vacuum pump is used in the subsequent time zones.
- the gas can be desorbed by introducing the purge gas into the adsorption tower.
- a purge gas introduction line for introducing the purge gas for gas desorption into the adsorption tower is provided.
- the gas 2 may be desorbed by circulating the purge gas without using a vacuum pump and discharged together with the purge gas.
- the purge gas nitrogen or the like is usually used, but is not limited thereto.
- FIG. 5 is an explanatory view showing an embodiment of such a gas separation and recovery method and equipment of the present invention.
- the desorption process is divided into a first time zone and a second time zone, and the desorption gas is collected separately for each time zone, and FIG. , And (b) show “desorption process: first time zone”, and (c) show “desorption process: second time zone”, respectively.
- the adsorption tower 1 is a vertical adsorption tower in which gas flows in the vertical direction, and is filled with an adsorbent having different linearity of adsorption isotherm depending on the gas type as shown in FIG. 2.
- a supply pipe constituting the source gas introduction line 4 is connected to one end side (upper end side) of the adsorption tower 1.
- a supply pipe 13 for introducing purge gas is connected to the line 4 portion, and an on-off valve 14 (shutoff valve) is provided in the supply pipe 13.
- the other end side (lower end side) of the adsorption tower 1 is connected to an exhaust pipe 10 for exhausting the raw material offgas and exhausting the desorbed gas.
- the pipe and the exhaust pipe constituting the desorption gas exhaust line 5 are connected to each other.
- Other configurations are the same as those of the embodiment of FIGS. 1 and 3, and thus the same reference numerals are given and detailed description thereof is omitted.
- the raw material gas is introduced into the adsorption tower 1 through the introduction line 4, and the raw material off-gas is discharged from the exhaust pipe 10 and the exhaust line 3.
- the desorption process is performed without performing the cleaning process.
- the vacuum pump 6 depressurizes the inside of the adsorption tower 1 to recover the gas 1 as shown in FIG.
- the desorption gas recovered gas A
- the on-off valve 14 is opened and the purge gas is introduced into the adsorption tower 1 from the supply pipe 13 as shown in FIG.
- the gas is desorbed with the purge gas, and the desorbed gas (recovered gas B) is recovered together with the purge gas through the branch line 50b.
- the mixed gas of the recovered gas B + purge gas may be diffused into the atmosphere, or may be used for a specific application as a gas having a high gas 2 concentration.
- the mixed gas serving as the raw material gas is not particularly limited as long as it is composed of at least two or more gas components.
- the target gas component can be separated and recovered from the source gas for various purposes.
- the gas desorbed at a specific time zone in the desorption process is divided into a plurality of time zones so that the amount of heat is higher than the gas desorbed in other time zones, and the gas desorbed in the specific time zones is recovered as a high calorie gas.
- the gas desorbed in a specific time zone has a CO concentration higher than the gas desorbed in other time zones.
- the desorption process is divided into a plurality of time zones so as to be high, and the gas desorbed in the specific time zone is recovered as a high calorie gas.
- the method of the present invention not only separates and collects high-calorie gas, but also separates and collects gas using, for example, a mixed gas of two or more kinds of gases having low calorific values (both non-combustible gases) as a raw material gas. Needless to say, it can be applied to cases.
- a demonstration experiment of the present invention was performed using a PSA experimental apparatus having an adsorption tower having an inner diameter of 40 mm and a height of 200 mm (height of the adsorbent packed bed is 190 mm) as shown in FIG.
- Commercially available 13X zeolite was used as the adsorbent.
- the test conditions were an adsorption pressure of 50 kPaG, a desorption pressure of -95 kPaG, and a cycle time of 351 seconds.
- a mixed gas having a gas composition of N 2 : 49 vol%, CO 2 : 22 vol%, CO: 24 vol%, H 2 : 5 vol% is used as the raw material gas, and a flow rate of 3 L / min with a mass flow controller (MFC) with respect to the adsorption tower. Controlled and supplied.
- MFC mass flow controller
- the adsorption process, the pressure release process, and the desorption process were sequentially performed.
- the recovered gas A was recovered in the first time zone
- the recovered gas B was recovered in the second time zone.
- the time distribution of each process was as follows: adsorption process t 1 : 243 sec, pressure release process t 2 : 6 sec, first time zone t 3 : 5 sec of desorption process, and second time zone t 4 : 97 sec of desorption process.
- raw material off-gas, release gas, recovered gas A, and recovered gas B were sampled, and the collected gas was subjected to composition analysis by gas chromatography. Table 1 shows the composition analysis results of the source gas and sampling gas.
- the composition of the raw material off-gas in the adsorption process is mainly due to CO 2 adsorption.
- the recovered gas A CO having a relatively smaller adsorption power than that of CO 2 is concentrated to 41.7 vol%, and with respect to the recovered gas B, CO 2 having a larger adsorbing power is reduced to 99.0 vol%. It can be confirmed that the gas separation effect according to the present invention is obtained.
- the pressure release gas although the CO concentration is lower than that of the recovered gas A, it is concentrated up to 32.3 vol%, and further the amount of CO 2 mixed is small, so that the pressure release gas can also be used as the CO separation gas. Is possible.
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Abstract
Description
一般に、PSA運転サイクルが吸着工程と脱着工程の2工程のみであれば電力消費量は抑制できるが、回収ガスの濃度は低くなる。一方、脱着ガスを一部洗浄ガスとして別の吸着塔へ循環供給する洗浄工程を行う運転方法では、回収ガスの濃度は高くすることができるが、一方で脱着ガスを再度吸着剤へ吸着させて脱着工程に送るため、脱着を行うガス量が増加し、電力消費量も増加してしまう。
すなわち、上記課題を解決するための本発明の要旨は以下のとおりである。
[3]上記[1]又は[2]のガス分離回収方法において、吸着塔がガスが上下方向に流れる縦型吸着塔であり、運転時に最もガス流速が大きくなる工程でのガス流れ方向を下向きとするガス分離回収方法。
[4]上記[1]~[3]のいずれかのガス分離回収方法において、吸着塔に塔内圧力を低下させるための放圧弁を設け、脱着工程において真空ポンプで吸着塔内を減圧する前に、前記放圧弁を開放して吸着塔内の圧力を低下させるガス分離回収方法。
[6]上記[1]~[5]のいずれかのガス分離回収方法において、脱着工程において、特定の時間帯に脱着されるガスが、他の時間帯に脱着されるガスよりも熱量が高くなるように、脱着工程を複数の時間帯に区分けし、前記特定の時間帯において脱着されるガスを高カロリーガスとして回収するガス分離回収方法。
[7]上記[6]のガス分離回収方法において、原料ガスがCOとCO2を含む混合ガスであり、脱着工程において、特定の時間帯に脱着されるガスが、他の時間帯に脱着されるガスよりもCO濃度が高くなるように、脱着工程を複数の時間帯に区分けするガス分離回収方法。
[9]上記[8]のガス分離回収設備において、吸着工程の際に一端側から原料ガスが導入され、他端側から原料オフガスが排出される吸着塔において、脱着工程では吸着塔の前記他端側から脱着ガスが排出されるように、脱着ガスの排気ラインが設けられたガス分離回収設備。
[11]上記[8]~[10]のいずれかのガス分離回収設備において、脱着ガスの排気ラインに吸着塔内を減圧するための真空ポンプが設けられた設備であって、吸着塔内の圧力を低下させるための放圧弁を有するガス分離回収設備。
[12]上記[8]~[11]のいずれかのガス分離回収設備において、脱着ガスの排気ラインに吸着塔内を減圧するための真空ポンプが設けられた設備であって、ガス脱着用のパージガスを吸着塔内に導入するためのパージガス導入ラインを有するガス分離回収設備。
ここで、図2に示されるガス1、ガス2と同様、以下の説明において、ガス1とは、圧力に対して線形な吸着特性を有し、高圧状態から減圧する過程で脱着されるガスを指し、また、ガス2とは、圧力に対して非線形な吸着特性を有し、高圧状態ではほとんど脱着せず、低圧状態まで減圧された時点で急激に脱着されるガスを指す。なお、図3~図5に示す他の実施形態においても同様である。
ここで、白抜きの開閉弁は開状態にあることを、黒く塗りつぶした開閉弁は閉状態にあることを、それぞれ示している。なお、図3~図5に示す他の実施形態においても同様である。
ここで、第1時間帯と第2時間帯の時間区分は、図2に示すような吸着剤の吸着・脱着特性と、目的ガス成分の目標濃度や熱量、目標収率などに応じて決めればよい。
吸着剤の種類によって、吸着等温線の線形性が異なるガス種は異なるので、分離するガス種に応じて吸着剤の種類を適宜選択すればよい。
なお、本実施形態では、脱着工程を2つの時間帯に区分けしたものであるが、吸着剤の種類や分離回収するガス種によっては、脱着工程を3つ以上の時間帯に区分け、脱着ガスを前記各時間帯毎に分けて回収するようにしてもよい。
本発明では、吸着工程の際に一端側から原料ガスが導入され、他端側から原料オフガスが排出される吸着塔において、脱着工程では吸着塔の前記他端側(原料ガス導入側と反対側)から脱着ガスを排出することにより、ガス分離効率を高めることができる。図3は、そのような本発明のガス分離回収方法及び設備の一実施形態を示す説明図である。この実施形態も脱着工程を第1時間帯と第2時間帯に区分けし、脱着ガスを前記各時間帯毎に分けて回収するようにしたものであり、図1の(a)は「吸着工程」、(b)は「脱着工程:第1時間帯」、(c)は「脱着工程:第2時間帯」をそれぞれ示している。
図4は、そのような本発明のガス分離回収方法及び設備の一実施形態を示す説明図である。なお、図4は、図4-1と図4-2とを総称したものである。この実施形態も脱着工程を第1時間帯と第2時間帯に区分けし、脱着ガスを前記各時間帯毎に分けて回収するようにしたものであり、図4の(a)は「吸着工程」、(b)は「放圧工程」、(c)は「脱着工程:第1時間帯」、(d)は「脱着工程:第2時間帯」をそれぞれ示している。
なお、放圧工程での放圧ガスは、回収ガスAよりもガス1の濃度は低いが、ガス1がある程度濃縮されたガスであるため、回収して特定の用途に利用してもよい。
パージガスとしては、通常、窒素などが用いられるが、これに限定されない。
本発明では、種々の目的で原料ガスから目的ガス成分を分離回収することができるが、原料ガスから高カロリーガスを分離回収する場合には、脱着工程において、特定の時間帯に脱着されるガスが、他の時間帯に脱着されるガスよりも熱量が高くなるように、脱着工程を複数の時間帯に区分けし、前記特定の時間帯において脱着されるガスを高カロリーガスとして回収する。したがって、例えば、原料ガスがCOとCO2を含む混合ガスである場合には、脱着工程において、特定の時間帯に脱着されるガスが、他の時間帯に脱着されるガスよりもCO濃度が高くなるように、脱着工程を複数の時間帯に区分けし、前記特定の時間帯において脱着されるガスを高カロリーガスとして回収する。
ただし、本発明法は、高カロリーガスの分離回収だけでなく、例えば、熱量が低い2種類以上のガス(いずれも非可燃性ガス)の混合ガスを原料ガスとしてガスの分離回収を行うような場合などにも適用できることはいうまでもない。
2 給排気管
3 排気ライン
4 導入ライン
5 排気ライン
6 真空ポンプ
7a,7b 開閉弁
8 開閉弁
9 開閉弁
10 排気管
11 放圧管
12 放圧弁
13 供給管
14 開閉弁
50a,50b 分岐ライン
Claims (12)
- 圧力スイング吸着法により原料ガスから特定のガス成分を分離回収する方法において、
吸着塔に充填された吸着剤にガス成分を吸着させる吸着工程と、
該吸着工程で吸着剤に吸着させたガス成分を脱着させてガスを回収する脱着工程を有するとともに、
他の吸着塔の脱着ガスの一部を洗浄ガスとして供給する洗浄工程を有しないガス分離回収方法であり、
脱着工程を複数の時間帯に区分けし、脱着ガスを前記各時間帯毎に分けて回収するガス分離回収方法。 - 吸着工程の際に一端側から原料ガスが導入され、他端側から原料オフガスが排出される吸着塔において、
脱着工程では吸着塔の前記他端側から脱着ガスを排出する請求項1に記載のガス分離回収方法。 - 吸着塔がガスが上下方向に流れる縦型吸着塔であり、運転時に最もガス流速が大きくなる工程でのガス流れ方向を下向きとする請求項1又は2に記載のガス分離回収方法。
- 吸着塔に塔内圧力を低下させるための放圧弁を設け、
脱着工程において真空ポンプで吸着塔内を減圧する前に、前記放圧弁を開放して吸着塔内の圧力を低下させる請求項1~3のいずれかに記載のガス分離回収方法。 - 脱着工程において、工程開始時からの1つ以上の時間帯では、真空ポンプで吸着塔内を減圧することによりガスを脱着し、その後の時間帯では、真空ポンプを用いることなく吸着塔内にパージガスを導入することによりガスを脱着する請求項1~4のいずれかに記載のガス分離回収方法。
- 脱着工程において、特定の時間帯に脱着されるガスが、他の時間帯に脱着されるガスよりも熱量が高くなるように、脱着工程を複数の時間帯に区分けし、前記特定の時間帯において脱着されるガスを高カロリーガスとして回収する請求項1~5のいずれかに記載のガス分離回収方法。
- 原料ガスがCOとCO2を含む混合ガスであり、脱着工程において、特定の時間帯に脱着されるガスが、他の時間帯に脱着されるガスよりもCO濃度が高くなるように、脱着工程を複数の時間帯に区分けする請求項6に記載のガス分離回収方法。
- 圧力スイング吸着法により原料ガスから特定のガス成分を分離回収する設備において、
吸着塔に充填された吸着剤にガス成分を吸着させる吸着工程と、
該吸着工程で吸着剤に吸着させたガス成分を脱着させてガスを回収する脱着工程を有するとともに、
他の吸着塔の脱着ガスの一部を洗浄ガスとして供給する洗浄工程を有しないガス分離回収を行う設備であり、
脱着ガスの排気ラインが複数に分岐するとともに、各分岐ラインに開閉弁が設けられ、脱着工程で脱着されるガスを時間帯毎に異なる分岐ラインを通じて回収できるようにしたガス分離回収設備。 - 吸着工程の際に一端側から原料ガスが導入され、他端側から原料オフガスが排出される吸着塔において、
脱着工程では吸着塔の前記他端側から脱着ガスが排出されるように、脱着ガスの排気ラインが設けられた請求項8に記載のガス分離回収設備。 - 吸着塔がガスが上下方向に流れる縦型吸着塔であり、運転時に最もガス流速が大きくなる工程でのガス流れ方向が下向きとなるように、吸着塔に対するガスの給排気ラインが設けられた請求項8又は9に記載のガス分離回収設備。
- 脱着ガスの排気ラインに吸着塔内を減圧するための真空ポンプが設けられた設備であって、
吸着塔内の圧力を低下させるための放圧弁を有する請求項8~10のいずれかに記載のガス分離回収設備。 - 脱着ガスの排気ラインに吸着塔内を減圧するための真空ポンプが設けられた設備であって、
ガス脱着用のパージガスを吸着塔内に導入するためのパージガス導入ラインを有する請求項8~11のいずれかに記載のガス分離回収設備。
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- 2017-12-06 EP EP17892777.8A patent/EP3549657A4/en active Pending
- 2017-12-06 WO PCT/JP2017/043776 patent/WO2018135164A1/ja unknown
- 2017-12-06 CN CN201780083910.2A patent/CN110198775B/zh active Active
- 2017-12-06 US US16/478,562 patent/US11083990B2/en active Active
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See also references of EP3549657A4 |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2022270439A1 (ja) * | 2021-06-24 | 2022-12-29 | Jfeスチール株式会社 | ガス分離設備およびガス分離方法 |
JP7207626B1 (ja) * | 2021-06-24 | 2023-01-18 | Jfeスチール株式会社 | ガス分離設備およびガス分離方法 |
WO2023042535A1 (ja) * | 2021-09-16 | 2023-03-23 | Jfeスチール株式会社 | ガス分離方法 |
JPWO2023042535A1 (ja) * | 2021-09-16 | 2023-03-23 |
Also Published As
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US20200047108A1 (en) | 2020-02-13 |
KR20190102288A (ko) | 2019-09-03 |
US11083990B2 (en) | 2021-08-10 |
EP3549657A1 (en) | 2019-10-09 |
JP2018114464A (ja) | 2018-07-26 |
CN110198775B (zh) | 2022-04-19 |
CN110198775A (zh) | 2019-09-03 |
EP3549657A4 (en) | 2020-01-01 |
JP6677181B2 (ja) | 2020-04-08 |
BR112019014398A2 (pt) | 2020-02-11 |
KR102292143B1 (ko) | 2021-08-20 |
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