CN114950068A - Method and system for separating mixed gas by temperature and pressure swing adsorption - Google Patents
Method and system for separating mixed gas by temperature and pressure swing adsorption Download PDFInfo
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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
- B01D53/0462—Temperature 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
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
-
- 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
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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
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/042—Purification by adsorption on solids
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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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Abstract
The invention relates to the field of mixed gas adsorption separation, and discloses a mixed gas temperature and pressure swing adsorption separation method and a mixed gas temperature and pressure swing adsorption separation system. The method comprises the following steps: (a) contacting the mixed gas with an adsorbent under a pressurization condition, wherein the adsorbent selectively adsorbs impurities in the mixed gas to be converted into a spent adsorbent, and a purified product gas is obtained; (b) using a plurality of strands of regeneration gas with different temperatures to perform segmented purging on the spent catalyst, so that the spent catalyst is subjected to segmented regeneration to obtain a regenerant; returning the regenerant to step (a) as part of the adsorbent, and repeating steps (a) and (b) to effect separation of the mixed gas. The method solves the problems of incomplete regeneration of an adsorbent, low purity of product gas and low recovery rate in the process of temperature and pressure swing adsorption separation of mixed gas, particularly separation and extraction of high-purity hydrogen from petroleum refining gas or coal chemical industry byproduct gas with the hydrogen content of at least 50-99.9 volume percent.
Description
Technical Field
The invention relates to the field of mixed gas adsorption separation, in particular to a mixed gas temperature and pressure swing adsorption separation method and a system for implementing the method.
Background
The mixed gas can be subjected to pressure swing adsorption to remove impurity components in the mixed gas, so that the purity of the product gas is improved. Pressure swing adsorption utilizes the difference of adsorption characteristics such as equilibrium adsorption capacity, adsorption speed and adsorption force of adsorbates on an adsorbent and the characteristic that the adsorption capacity changes along with pressure change, realizes the alternation of adsorption and desorption processes through periodic pressure change, belongs to a physical process, and can be realized at normal temperature.
CN105817117A discloses a high-efficiency pressure swing adsorption gas separation method, which utilizes a group of adsorption beds filled with one or more adsorbents to physically separate a mixed gas containing a strong adsorption component and a weak adsorption component, adsorbs the strong adsorption component at a higher pressure, desorbs the strong adsorption component at a lower pressure, continuously outputs the weak adsorption component as a separator at a higher pressure, continuously outputs the strong adsorption component as a product at a lower pressure, and each adsorption bed continuously produces a cyclic process comprising an adsorption step of raw material feeding, an equalization pressure drop step, a forward discharge step of providing regenerated gas, a reverse discharge step of reverse pressure discharge, a flushing step of flushing regeneration, an equalization pressure rise step corresponding to the equalization pressure drop step, and a final charge step of final pressure rise, and is characterized in that: the group of adsorption beds comprises at least 10 adsorption beds, the cyclic process of each adsorption bed comprises 5-12 flushing steps and 1-2 sequential discharging steps, and comprises 1 or 2 uniform pressure drop steps and a regeneration gas providing step, or the 1 st reverse discharging step provides the regeneration gas simultaneously, or the 2 uniform pressure drop steps provide the regeneration gas simultaneously and the 1 st reverse discharging step provides the regeneration gas simultaneously.
CN1330973A discloses a multi-tower pressure swing adsorption gas separation method, each adsorption tower sequentially undergoes the steps of adsorption (a), multiple pressure equalization reduction (E1D, E2D …), forward or reverse pressure release (PP/D), vacuum pumping (V1, V2 …), multiple pressure equalization rise (E1R, E2R …), final charging (FR) and the like in one cycle, and the evacuation step of each adsorption tower is divided into several stages (V1, V2 …).
CN108211648A discloses a gas adsorption separation device, which comprises an adsorption function module and other function modules, the main functional part of the adsorption functional module is an adsorption sequence consisting of more than two adsorption units which are arranged in sequence, the adsorption sequence comprises a head end and a tail end, the gas to be separated passes through the adsorption sequence from the head end to the tail end, when the adsorption unit at the head end finishes the saturated adsorption of the adsorbate gas, the adsorption unit is separated from the adsorption sequence and enters other functional modules comprising a desorption device, and re-enter the adsorption sequence from the tail end in sequence after other process treatments including desorption treatment are completed, the adsorption unit is an adsorption fixed bed which is composed of an adsorbent and a mechanical support structure and has proper mechanical strength and good permeability, the adsorption unit which completes saturated adsorption is called a saturated adsorption unit, and the adsorption unit which completes desorption regeneration is called a regeneration adsorption unit. The device can give consideration to both high concentration ratio and low discharge concentration. Different adsorption and desorption modes can be adopted, and the adsorption and desorption modes mainly comprise temperature swing adsorption, pressure swing adsorption or temperature swing and pressure swing adsorption. Temperature swing adsorption generally refers to low temperature adsorption and high temperature desorption. The temperature and pressure swing adsorption is generally low temperature and high pressure adsorption and high temperature and low pressure desorption.
In the pressure swing adsorption process, the regeneration energy consumption and the regeneration time of the desorption (desorption or regeneration) process of the adsorbent become factors restricting the development of the separation process, and even influence the upsizing of the gas separation process. There is therefore a need in the art to consider improvements in the regeneration process of adsorbents.
Disclosure of Invention
The invention aims to solve the problem that the yield, the product gas purity and the recovery efficiency of the technical process are influenced by the regeneration process of an adsorbent in the prior gas separation technology, and provides a method and a system for temperature and pressure swing adsorption separation of mixed gas.
In order to achieve the above object, a first aspect of the present invention provides a method for mixed gas temperature and pressure swing adsorption separation, comprising:
(a) contacting the mixed gas with an adsorbent under a pressurization condition, wherein the adsorbent selectively adsorbs impurities in the mixed gas to be converted into a spent adsorbent, and a purified product gas is obtained;
(b) using a plurality of strands of regeneration gas with different temperatures to perform segmented purging on the spent catalyst, so that the spent catalyst is subjected to segmented regeneration to obtain a regenerant;
returning the regenerant to step (a) as part of the adsorbent, and repeating steps (a) and (b) to effect separation of the mixed gas.
In a second aspect, the present invention provides a mixed gas temperature and pressure swing adsorption separation system, including: the system comprises an air inlet subsystem, an exhaust subsystem, a regenerated gas subsystem and a main separation subsystem; wherein the content of the first and second substances,
the main ion separation system comprises more than two adsorption towers which are arranged in parallel and filled with adsorbents in a layered mode, and more than two regeneration gas pipelines are arranged in each adsorption tower along the axial direction of the adsorption tower and used for performing segmented regeneration on the adsorbents by using regeneration gases with different temperatures.
According to the technical scheme, the mixed gas separation method provided by the invention aims at the problem that different impurities are adsorbed by an adsorbent to be converted into segmented spent agents containing different impurities, the regeneration temperatures corresponding to the spent agents adsorbing different impurities are determined, the spent agents are subjected to segmented regeneration by using the regenerated gases with different temperatures, and then part of product gas is preferably used as the regenerated gas, so that the problems of incomplete regeneration of the adsorbent, low product gas purity and low recovery rate in the process of mixed gas temperature and pressure swing adsorption separation, particularly separation and extraction of high-purity hydrogen from a petroleum refining gas-producing or coal chemical gas-producing pair with at least 50-99.9 volume% of hydrogen content are solved.
Drawings
FIG. 1 is a schematic view of a process flow for mixed gas temperature and pressure swing adsorption separation provided by the present invention;
FIG. 2 is a schematic flow chart of a process for separating mixed gas temperature and pressure swing adsorption of the present invention, which comprises two absorption columns filled with adsorbents in three stages according to an embodiment of the present invention;
FIG. 3 is a graph of the variation trend of the regeneration time and the regeneration temperature of methane in an embodiment of the present invention;
FIG. 4 shows a view of a view point of example C of the present invention 3 A hydrocarbon regeneration time versus regeneration temperature trend curve;
FIG. 5 is a graph showing the penetration of the mixture in the example of the present invention;
FIG. 6 is a schematic diagram of a process flow of mixed gas temperature and pressure swing adsorption separation in the prior art, which comprises two absorption towers, and adsorbents in the towers are filled in three sections without regeneration gas with different temperatures.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For numerical ranges, each range between its endpoints and individual point values, and each individual point value can be combined with each other to give one or more new numerical ranges, and such numerical ranges should be construed as specifically disclosed herein.
The first aspect of the invention provides a method for temperature and pressure swing adsorption separation of mixed gas, which comprises the following steps:
(a) contacting the mixed gas with an adsorbent under a pressurization condition, wherein the adsorbent selectively adsorbs impurities in the mixed gas to be converted into a spent adsorbent, and a purified product gas is obtained;
(b) using a plurality of strands of regeneration gas with different temperatures to perform segmented purging on the spent catalyst, so that the spent catalyst is subjected to segmented regeneration to obtain a regenerant;
returning the regenerant to step (a) as part of the adsorbent, and repeating steps (a) and (b) to effect separation of the mixed gas.
In some embodiments of the present invention, preferably, the spent reagent comprises a plurality of spent reagent subsections containing different impurities, and the spent reagent subsections are regenerated by regeneration gas with different temperatures.
In some embodiments of the present invention, preferably, the temperature of the regeneration gas is determined according to the action between the adsorbent and the impurities contained in the spent adsorbent subsections and the adsorption heat, corresponding to different spent adsorbent subsections. Therefore, the sectional regeneration of the spent catalyst is realized, and a better regeneration effect is obtained. The temperature of the regeneration gas may be determined in consideration of the composition of the specific mixed gas and the requirements for the specific adsorption regeneration of the adsorbent.
In some embodiments of the present invention, preferably, the regeneration gas is part of the product gas. And partial product gas is introduced as regeneration gas, so that the energy consumption for regenerating the adsorbent can be saved. Preferably, 0.5-25% by volume of the product gas is used as the regeneration gas. The regeneration gas can also use a part of gas in a pressure equalizing process. Particularly, when the number of the adsorption beds formed by the adsorbent is more than 2, the pressure equalization can be carried out for more than 1 time in the pressure swing adsorption process, so that more product gas can be recovered; at this time, if the purity of the gas after pressure equalization can meet the requirement, the non-product gas can be used as the regeneration gas, namely, the gas after pressure equalization is used as the regeneration gas.
In a specific embodiment of the invention, the invention can particularly provide a hydrogen-containing mixed gas temperature and pressure swing adsorption separation method for extracting hydrogen. Preferably, the mixed gas is petroleum refining gas or coal chemical industry by-product gas with the hydrogen content of at least 50-99.9 volume percent, and is preferably petroleum refining hydrofining or hydrocracking tail gas and coke oven gas tail gas. The method provided by the invention can help to improve the purity and efficiency of the hydrogen extracted from the gas.
In some embodiments of the present invention, preferably, the mixed gas further contains H in an amount of 0.1 to 50 vol% 2 S、SO 2 、CO、N 2 、Ar、CO 2 、C 1 -C 5 At least one of (a) and (b).
In some embodiments of the present invention, preferably, the product gas is hydrogen having a purity of 99.99 vol% or more. The invention can realize the high-efficiency separation of hydrogen and light hydrocarbon, thereby effectively improving the quality of the hydrogen, and ensuring that the hydrogen meets the quality requirements of the hydrogen for fuel cell vehicles and the concentration standards of various impurity gases meet the requirements of the hydrogen for fuel cell vehicles.
In some embodiments of the invention, preferably, the contacting temperature is from-30 ℃ to 500 ℃ and the contacting gauge pressure is from 0 to 6 MPa. In step (a) of the method provided by the invention, the contacting process is a process in which the adsorbent selectively adsorbs impurities in the mixed gas. The above conditions of the contact may be more favorable for obtaining a good effect of selective adsorption.
In some embodiments of the present invention, preferably, step (b) is preceded by: equalizing pressure drop, releasing pressure and emptying; the step (b) is followed by the steps of pressure equalization and pressure rise and final charging. The implementation process of the method is a pressure transformation process.
In some embodiments of the invention, the adsorbent can be selected according to different impurities contained in the mixed gas, so that the adsorption pertinence is improved, and meanwhile, the regeneration effect of the adsorbent can be effectively improved by implementing the targeted regeneration temperature on the to-be-regenerated agent converted after different impurities are adsorbed. Preferably, for the above-mentioned mixed gas containing hydrogen (such as the above-mentioned petroleum refinery gas or coal chemical by-product gas), the adsorbent to be selected is discriminated with respect to impurities possibly contained therein, and different regeneration temperatures are defined. Preferably, the impurity contained in the mixed gas is CO 2 、CH 4 、Ar、H 2 S、SO 2 When at least one of the above-mentioned (B) is selected, the described adsorbent is active carbon, and the sectional regeneration temp. is 0-40 deg.C;
the mixed gas contains CO and/or N as impurities 2 When the adsorbent is a molecular sieve, the temperature of sectional regeneration is 0-40 ℃;
the mixed gas contains CO as impurity 2 、H 2 S、SO 2 When at least one of the above-mentioned (B) is selected, the described adsorbent is active carbon supported adsorbent, and the sectional regeneration temp. is 25-150 deg.C; wherein, the activated carbon supported adsorbent can contain a load which is conventional in the field;
the mixingThe gas contains H as impurity 2 When O is needed, the adsorbent is selected from at least one of activated alumina, silica gel adsorbent and 13X, and the temperature of sectional regeneration is 0-250 ℃;
the mixed gas contains C as impurity 2 When hydrocarbon is produced, the adsorbent is activated carbon and/or silica gel adsorbent, and the temperature of sectional regeneration is 25-150 ℃;
the mixed gas contains C as impurity 3 When hydrocarbon is produced, the adsorbent is activated carbon and/or silica gel adsorbent, and the temperature of sectional regeneration is 25-200 ℃;
the mixed gas contains C as impurity 4 When hydrocarbon is produced, the adsorbent is activated carbon and/or silica gel adsorbent, and the temperature of sectional regeneration is 25-300 ℃;
the mixed gas contains C as impurity 5 When the hydrocarbon is used, the adsorbent is activated carbon and/or silica gel adsorbent, and the temperature of sectional regeneration is 25-500 ℃.
In the present invention, C 2 The hydrocarbon means a compound containing carbon having a carbon number of 2 and hydrogen, for example, at least one of ethane, ethylene, and acetylene. C 3 Hydrocarbons, C 4 Hydrocarbons and C 5 The above hydrocarbons are also analogous carbon and hydrogen compounds.
In some embodiments of the present invention, a plurality of adsorbents can be selected to form an adsorption bed layer to be filled in the adsorption tower. The selected multiple adsorbents and the filling mode in the adsorption bed layer can realize the separation of the mixed gas to be treated, and the product gas with expected purity and yield can be obtained. The spent adsorbent obtained by the contact can contain impurities adsorbed by different adsorbents filled in corresponding adsorption bed layers in sections to form subsections of the spent adsorbent, and further can adopt section regeneration. When the multi-strand regeneration gas with different temperatures meets the requirements of sectional regeneration, the regeneration of different agent sections to be regenerated is carried out at different sectional regeneration temperatures. For example, the mixed gas is the above-mentioned mixed gas containing hydrogen, and the product gas obtained by separation is hydrogen having a purity of 99.99 vol% or more. The impurities contained in the mixed gas can be considered, the multiple adsorbents are selected, and the formed adsorption bed layer is contacted to form a plurality of sections of spent adsorbent containing different impurities for sectional regeneration.
In some embodiments of the present invention, preferably, the method further comprises: prior to step (a), analyzing the impurity composition of said gas mixture to select a corresponding adsorbent; single component breakthrough and regeneration experiments were then performed on the selected sorbent to determine the optimum regeneration temperature for the selected sorbent. This step is used to determine the dynamic adsorption capacity of the selected adsorbent. The single component breakthrough test refers to passing the mixed gas through an adsorption bed containing a single selected adsorbent, and then performing composition analysis on the obtained tail gas to determine the dynamic adsorption capacity of the adsorbent for a certain impurity, as shown in fig. 5.
Then, a simulated gas having the same composition as the mixed gas is used to conduct a breakthrough test on the adsorbent bed containing the selected adsorbent, and the position where the adsorbent bed introduces the regeneration gas having a different temperature is determined. When the step is used for determining the adsorption beds for sectional regeneration, the regeneration gas with the corresponding temperature is introduced into the adsorption beds at which position to obtain better sectional regeneration effect. As illustrated in fig. 1.
In some embodiments of the present invention, the adsorbent used for the mixed gas temperature and pressure swing adsorption separation may comprise one or more of the above-mentioned adsorbents capable of adsorbing various impurities in the mixed gas correspondingly. When plural kinds of adsorbents are packed in the adsorbent bed, the amount of each adsorbent used may be determined by analyzing the composition of the mixed gas, or plural kinds of adsorbents may be packed in equal amounts.
In a second aspect, the present invention provides a mixed gas temperature and pressure swing adsorption separation system, as shown in fig. 1, including: the system comprises an air inlet subsystem, an exhaust subsystem, a regenerated gas subsystem and a main separation subsystem; wherein the content of the first and second substances,
the main ion separation system comprises more than two adsorption towers which are arranged in parallel and filled with adsorbents in a layered mode, and more than two regeneration gas pipelines are arranged in each adsorption tower along the axial direction of the adsorption tower and used for performing segmented regeneration on the adsorbents by using regeneration gases with different temperatures.
The multiple adsorption towers can alternately perform adsorption and sectional regeneration, for example, a main ion separation system comprises two adsorption towers which are connected in parallel, one adsorption tower is used as an adsorption bed to perform mixed gas adsorption, the other adsorption tower is subjected to an adsorption process, an adsorbent in the adsorption tower is converted into a spent adsorbent containing impurities to be subjected to a regeneration process, and regeneration gas with different temperatures is introduced to perform sectional regeneration.
In some embodiments of the present invention, preferably, the regeneration gas subsystem comprises more than two regeneration gas buffer tanks and heat exchangers, and is communicated with the regeneration gas pipeline for providing regeneration gas with different temperatures to the main separation ion system.
In some embodiments of the present invention, preferably, the exhaust subsystem comprises a product gas pipeline, an exhaust gas discharge pipeline, a product gas buffer tank; the product gas pipeline is communicated with the product gas buffer tank, the main ion separating system and the regeneration gas subsystem and is used for discharging the product gas obtained by separating the main ion separating system into the product gas buffer tank and introducing part of the product gas into the regeneration gas subsystem as regeneration gas.
In some embodiments of the present invention, preferably, the gas inlet subsystem is communicated with the main separation subsystem for introducing a mixture gas into the main separation subsystem.
In some embodiments of the present invention, preferably, the main separation subsystem comprises 1 to 12 adsorption towers, and each adsorption tower is communicated with the air intake subsystem, the air exhaust subsystem and the regeneration gas subsystem through a pipeline provided with a valve; the valve is set to be in an on/off state, so that the absorption tower is alternately in an adsorption state and a sectional regeneration state.
The step of separating and extracting the high-purity hydrogen from the hydrogen-containing mixed gas (such as petroleum refining produced gas or coal chemical industry byproduct gas with the hydrogen content of at least 50-99.9 vol%) provided by the invention can comprise the following steps:
the locations at which the adsorbent beds can introduce regeneration gas at different temperatures, and the different temperatures of the regeneration gas, are determined. Then, as shown in FIG. 1,
1-adsorption: the mixed gas is pressurized by the gas inlet subsystem and then enters the adsorption tower of the main separation subsystem, wherein the regeneration and pressure boosting steps are completed. Under certain temperature and pressure conditions, impurities in the mixed gas are selectively adsorbed, weakly adsorbed components serving as product gas enter a product gas buffer tank from the top of an adsorption tower, and part of the product gas is shunted and enters a regeneration gas tank for heat exchange; when the mixed gas contains more than one kind of impurities, the acting forces of different impurities and the adsorbent are relatively strong and weak, the impurities with relatively strong adsorption can replace the weakly adsorbed impurities occupying the adsorption sites, so that different impurity enrichment regions appear along the axial direction of the adsorption tower, and the impurity enrichment regions are related to the acting forces between the adsorbent and the impurities and the layered filling types of the adsorbent in the adsorption tower.
2-average pressure drop: and when the impurity adsorption in the adsorption tower is close to saturation, closing the inlet of the adsorption tower. The adsorption tower is connected with the adsorption tower which is regenerated in other parallel adsorption towers, and the pressure equalizing and reducing step is carried out. After the pressure equalization drop, the pressure of the adsorption tower is reduced, the adsorbed impurities are partially desorbed, and the impurities further move forward along the adsorption tower.
3-pressure relief and emptying: after the pressure equalization is finished, opening a vent valve at the gas inlet end of the adsorption tower to discharge residual gas-phase mixed gas in the system, and at the moment, because the pressure of the system is reduced, adsorbing part of impurities in the desorbed gas phase is vented.
4-sectional temperature-changing regeneration purging: after the adsorption tower is emptied, part of impurities can not be completely desorbed, and the spent catalyst in the adsorption tower is completely regenerated by adopting a sectional hot purging method. Connecting the top end of the adsorption tower with a normal-temperature regeneration gas buffer tank, wherein gas enters the adsorption tower from the tower top and is discharged from a discharge port at the tower bottom; then, the regeneration gas with different temperatures is distributed into the adsorption tower along the axial direction of the adsorption tower and passes through the spent adsorbent from top to bottom, different temperature sections from top to bottom are formed in the adsorption tower, and the temperature required by complete desorption of different spent adsorbent subsections formed by adsorbing different types of impurities is provided; the desorbed gas is discharged from a discharge port at the bottom of the tower; the spent adsorbent is regenerated in a segmented mode, heat loss is reduced to the maximum extent, the using amount of regenerated gas is reduced, and the utilization efficiency of the adsorbent is improved.
5-pressure equalization rise: and after the adsorption tower completes regeneration, the adsorption tower is connected with other adsorption towers in the main separation subsystem to perform pressure equalization and increase, so that the pressure of the adsorption tower is increased.
6-final pressurization; and finally pressurizing the system by adopting part of product gas to ensure that the adsorption bed reaches the adsorption pressure, and starting the next cycle.
As illustrated in fig. 1, the main separation subsystem has two adsorption columns, one in adsorption mode and one in staged regeneration mode. The regeneration gas subsystem heats part of product gas to different temperatures (T1, T2 and T3), then the product gas is used as regeneration gas with different temperatures to be introduced into an adsorption tower in a segmented regeneration state (wherein the adsorbent already contains impurities to be converted into spent adsorbent, the segments contain different impurities (C1, C2, C3-C5) to become spent adsorbent subsections), and the regeneration gas with different temperatures is introduced from different positions of the adsorption tower along the axial direction to carry out segmented regeneration. The other subsystems are corresponding to the adsorption state or the sectional regeneration state of different adsorption towers and correspondingly switched through the connecting pipeline and the valve arranged on the connecting pipeline.
The present invention will be described in detail below by way of examples.
Example 1
The mixed gas temperature and pressure swing adsorption separation system is shown in figure 2. The method comprises 2 adsorption towers (adsorption tower-1 and adsorption tower-2), wherein each adsorption tower is sequentially filled with three sections of adsorbents from bottom to top: the adsorbent A, the adsorbent B and the adsorbent C (the adsorbent A is macroporous silica gel, the adsorbent B is B-type silica gel, the adsorbent C is activated carbon, the loading amounts of the three adsorbents are the same) are provided with a regeneration gas subsystem, and regeneration gases with different temperatures are provided.
The mixed gas is refinery gas and comprises the following components in percentage by weight: h 2 92.75 vol.%, CH 4 2.15 vol.%, C 2 Hydrocarbon 2.63 vol%, C 3 Hydrocarbon 1.68 vol%, C 4 The hydrocarbon was 0.69 vol%. Extracting high-purity hydrogen.
As shown in FIGS. 3 and 4, are methane and C 3 Purge curves at different temperatures of the hydrocarbons. The adsorbent, regeneration temperature, regeneration time, and regeneration gas introduction location were confirmed. Figures 3 and 4 show that the regeneration time is significantly reduced with increasing temperature. Of mixed gasesThe breakthrough plot, shown in FIG. 5, illustrates methane (C) 1 Hydrocarbon) first breakthrough, C 4 The hydrocarbons eventually penetrate the adsorbent bed. The three sectional regeneration temperatures are sequentially selected, and the regeneration gases with different temperatures (realized by a regeneration gas subsystem and meeting the sectional regeneration temperatures required by each spent catalyst subsection) are introduced from the bottom to the top of the adsorption tower and from 1/3 to 2/3 at the bottom of the tower. Wherein, the regeneration gas is part of product gas, and the amount of the regeneration gas is about 25 volume percent of the product gas.
The system operating conditions are as follows: the adsorption pressure (contact pressure) is 3MPa, and the adsorption temperature (contact temperature) is room temperature; temperature of the staged regeneration: t1 (corresponding to adsorbent a layer): 25 ℃, T2 (corresponding to adsorbent B layer): 150 ℃, T3 (corresponding to adsorbent C layer): at 300 ℃.
The product hydrogen was obtained with a purity of 99.992% and a hydrogen recovery of 68.2%, the results are shown in table 1.
Comparative example 1
In the pressure swing adsorption separation process shown in fig. 6 having two adsorption columns, there is no regeneration gas subsystem that provides regeneration gas at different temperatures.
The composition, adsorption temperature and adsorption pressure of the mixed gas are the same as those of the example 1, the regeneration temperature is 25 ℃, and the regeneration gas with different temperatures in different sections is subjected to sectional regeneration.
The hydrogen yield was 63.5% and the hydrogen purity was 99.5%, the results are shown in Table 1.
TABLE 1
| Numbering | Purity of hydrogen | Yield of |
| Example 1 | 99.992％ | 68.2％ |
| Comparative example 1 | 99.5％ | 63.5％ |
It can be seen from the results in table 1 that the method provided by the present invention is used to perform the staged regeneration of the spent catalyst with the regeneration gas at different temperatures, the hydrogen yield obtained in example 1 is high, and the product purity is significantly better. And part of product gas is used as regeneration gas, so that the product purity can be improved.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (13)
1. A method for separating mixed gas by temperature and pressure swing adsorption comprises the following steps:
(a) contacting the mixed gas with an adsorbent under a pressurization condition, wherein the adsorbent selectively adsorbs impurities in the mixed gas to be converted into a spent adsorbent, and a purified product gas is obtained;
(b) using a plurality of strands of regeneration gas with different temperatures to perform segmented purging on the spent catalyst, so that the spent catalyst is subjected to segmented regeneration to obtain a regenerant;
returning the regenerant to step (a) as part of the adsorbent, and repeating steps (a) and (b) to effect separation of the mixed gas.
2. The method according to claim 1, wherein the spent agent comprises a plurality of spent agent subsections containing different impurities, and the spent agent subsections are regenerated by regeneration gases with different temperatures;
preferably, the temperature of the regeneration gas is determined according to the action between the adsorbent and the impurities contained in the spent adsorbent subsection and the adsorption heat corresponding to different spent adsorbent subsections.
3. The process of claim 1 or 2, wherein the regeneration gas is part of the product gas.
4. The method according to any one of claims 1 to 3, wherein the mixed gas is a petrochemical off-gas or a coal chemical by-product gas having a hydrogen content of at least 50 to 99.9 vol%, preferably a hydrofinished or hydrocracked tail gas of a petrochemical, a coke oven gas tail gas;
preferably, the gas mixture further contains H in an amount of 0.1 to 50 vol% 2 S、SO 2 、CO、N 2 、Ar、CO 2 、C 1 -C 5 At least one of the hydrocarbons of (a);
preferably, the product gas is hydrogen having a purity of 99.99% by volume or more.
5. The process of any one of claims 1-4, wherein the contacting temperature is from-30 ℃ to 500 ℃ and the contacting gauge pressure is from 0 to 6 MPa.
6. The method of any one of claims 1-5, wherein step (b) is preceded by: equalizing pressure drop, releasing pressure and emptying; the step (b) is followed by the steps of pressure equalization and pressure rise and final charging.
7. The method according to any one of claims 4 to 6, wherein the impurity contained in the mixed gas is CO 2 、CH 4 、Ar、H 2 S、SO 2 When at least one of the above-mentioned (B) is selected, the described adsorbent is active carbon, and the sectional regeneration temp. is 0-40 deg.C;
the mixed gas contains CO and/or N as impurities 2 When the adsorbent is a molecular sieve, the temperature of sectional regeneration is 0-40 ℃;
the mixed gas contains CO as impurity 2 、H 2 S、SO 2 When at least one of the above-mentioned (B) is selected, the described adsorbent is active carbon supported adsorbent, and the sectional regeneration temp. is 25-150 deg.C;
the mixed gas contains H as impurity 2 When O is needed, the adsorbent is at least one of activated alumina, silica gel adsorbent and 13X, and the temperature of the segmented regeneration is 0-250 ℃;
the mixed gas contains C as impurity 2 When hydrocarbon is produced, the adsorbent is activated carbon and/or silica gel adsorbent, and the temperature of sectional regeneration is 25-150 ℃;
the mixed gas contains C as impurity 3 When hydrocarbon is produced, the adsorbent is activated carbon and/or silica gel adsorbent, and the temperature of sectional regeneration is 25-200 ℃;
the mixed gas contains C as impurity 4 When hydrocarbon is produced, the adsorbent is activated carbon and/or silica gel adsorbent, and the temperature of sectional regeneration is 25-300 ℃;
the mixed gas contains C as impurity 5 When the hydrocarbon is used, the adsorbent is activated carbon and/or silica gel adsorbent, and the temperature of sectional regeneration is 25-500 ℃.
8. The method of claim 7, wherein the method further comprises: prior to the step (a) of the process,
analyzing the impurity composition in the mixed gas, and selecting a corresponding adsorbent; then, carrying out single-component penetration and regeneration experiments on the selected adsorbent, and determining the optimal regeneration temperature corresponding to the selected adsorbent;
a simulated gas having the same composition as the mixed gas is used to perform a breakthrough test on the adsorbent bed containing the selected adsorbent, and the location where the adsorbent bed introduces the regeneration gas having a different temperature is determined.
9. A mixed gas temperature and pressure swing adsorption separation system comprises: the system comprises an air inlet subsystem, an exhaust subsystem, a regenerated gas subsystem and a main separation subsystem; wherein the content of the first and second substances,
the main ion separation system comprises more than two adsorption towers which are arranged in parallel and filled with adsorbents in a layered mode, and more than two regeneration gas pipelines are arranged in each adsorption tower along the axial direction of the adsorption tower and used for performing segmented regeneration on the adsorbents by using regeneration gases with different temperatures.
10. The system of claim 9, wherein the regeneration gas subsystem comprises two or more regeneration gas buffer tanks and heat exchangers and is in communication with the regeneration gas conduit for providing different temperatures of regeneration gas to the main separation ion system.
11. The system of claim 9 or 10, wherein the exhaust subsystem comprises a product gas line, a tail gas vent line, a product gas surge tank;
the product gas pipeline is communicated with the product gas buffer tank, the main ion separation system and the regeneration gas subsystem and is used for discharging the product gas obtained by separating the main ion separation system into the product gas buffer tank and introducing part of the product gas into the regeneration gas subsystem to be used as regeneration gas.
12. The system of any one of claims 9-11, wherein the gas inlet subsystem communicates with the main separation subsystem for introducing a mixture of gases into the main separation subsystem.
13. The system of any one of claims 9-12, wherein the main separation subsystem comprises 1-12 adsorption towers, each adsorption tower is communicated with the air intake subsystem, the air exhaust subsystem and the regeneration air subsystem through a pipeline provided with a valve;
the valve is set to be in an on/off state, so that the absorption tower is alternately in an adsorption state and a sectional regeneration state.
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