WO2023124825A1 - 吸附剂的选择方法、变压吸附方法及其系统 - Google Patents

吸附剂的选择方法、变压吸附方法及其系统 Download PDF

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WO2023124825A1
WO2023124825A1 PCT/CN2022/136912 CN2022136912W WO2023124825A1 WO 2023124825 A1 WO2023124825 A1 WO 2023124825A1 CN 2022136912 W CN2022136912 W CN 2022136912W WO 2023124825 A1 WO2023124825 A1 WO 2023124825A1
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adsorbent
slope
adsorption
target
pressure swing
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PCT/CN2022/136912
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English (en)
French (fr)
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张胜中
乔凯
张延鹏
范得权
杨阳
胡方舟
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中国石油化工股份有限公司
中石化（大连）石油化工研究院有限公司
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Publication of WO2023124825A1 publication Critical patent/WO2023124825A1/zh

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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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials

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  • the embodiments of the present invention relate to the technical field of adsorption separation, in particular to a method for selecting an adsorbent, a pressure swing adsorption method and a system thereof.
  • Pressure swing adsorption technology can be used for the purification of hydrogen, helium, nitrogen and other gases, and can also be used for industrial processes such as carbon dioxide capture and recovery of low-carbon hydrocarbons.
  • the selected adsorbent can absorb the impurities that need to be removed, or the products that need to be produced.
  • the impurities or products adsorbed by the adsorbent are called adsorbates.
  • Adsorbent, control process and equipment are the key to the application of pressure swing adsorption technology in production.
  • pressure swing adsorption realizes continuous production through the sequential switching of no less than two towers.
  • Each tower is filled with the same type and equal weight of adsorbent, and a certain amount of adsorbent is filled in one adsorption tower.
  • the product recovery rate can be improved by prolonging the adsorption cycle; if the loading amount of the adsorbent is reduced, the product recovery rate can be ensured by shortening the adsorption cycle and the equipment footprint can be reduced.
  • the corresponding adsorbent is mainly selected through experience. Therefore, it is usually necessary to load an excessive amount of adsorbent and set a longer adsorption period to achieve the purpose of sufficient adsorption.
  • the purpose of the present invention is to provide a method for selecting an adsorbent, a pressure swing adsorption method and its system, which can be based on the slope of the adsorption isotherm at the initial pressure and the adsorption of the adsorbent to the target adsorbate at a specific temperature and a specific pressure
  • the target adsorbent is selected, thereby reducing the operation and production costs of the pressure swing adsorption.
  • the first aspect of the present invention provides a method for selecting an adsorbent, the selection method includes: obtaining the slope of the adsorption isotherm of each adsorbent on the target adsorbate at the initial pressure of a plurality of adsorbents , wherein, the adsorption isotherm is a curve of the adsorption amount varying with pressure at a specific temperature; the adsorption amount of each adsorbent on the target adsorbate at the specific temperature and specific pressure is obtained; and according to The slope and the adsorption capacity of each adsorbent are selected from the plurality of adsorbents for adsorbing the target adsorbate.
  • the selection of the target adsorbent for adsorbing the target adsorbate from the plurality of adsorbents includes: determining the pressure swing adsorption of each adsorbent according to the slope of each adsorbent The shortest time of each decomposition step in the cycle period; according to the determined shortest time, select a specific adsorbent from the plurality of adsorbents, wherein the shortest time corresponding to the specific adsorbent is less than or equal to the preset setting time; determining the product of the slope and the adsorption capacity of the specific adsorbent; and selecting the adsorbent corresponding to the largest product as the target adsorbent.
  • said determining the shortest time of each decomposition step in said cycle of pressure swing adsorption for each adsorbent comprises: when a slope of an adsorbent is greater than the first slope and less than or equal to the second slope Under the circumstances, the shortest time corresponding to the adsorbent is greater than or equal to the first shortest time; when the slope of an adsorbent is greater than the second slope and less than or equal to the third slope, the corresponding to the adsorbent The shortest time is greater than or equal to the second shortest time; when the slope of an adsorbent is greater than the third slope and less than or equal to the fourth slope, the shortest time corresponding to the adsorbent is greater than or equal to the third shortest time; Or when the slope of an adsorbent is greater than the fourth slope and less than or equal to the fifth slope, the shortest time corresponding to the adsorbent is greater than or equal to the fourth shortest time, wherein the first slope, the The second
  • the first slope is 1, the second slope is 10, the third slope is 20, the fourth slope is 30, and the fifth slope is 50, the second A shortest time is 0.05s, the second shortest time is 3s, the third shortest time is 9s and the fourth shortest time is 24s.
  • the determination of the shortest time t of each decomposition step in the cycle period of the pressure swing adsorption of each adsorbent includes: Wherein, T is the preset longest step time, the unit is s; and k 0 is the slope of each adsorbent.
  • T is less than or equal to 40.
  • the selection method further includes: determining the determined shortest time as the adsorption time; and according to the amount of the target adsorbate introduced into the adsorption tower within the adsorption time and the adsorption amount of the target adsorbent, Determine the amount of the target sorbent.
  • the step of obtaining the slope of the adsorption isotherm of each of the plurality of adsorbents for the target adsorbate at the initial pressure is performed under a preset precondition, wherein the preset precondition Including: at each pressure, the absolute value of the difference between the adsorption capacity of the target adsorbate on the adsorption isotherm and the desorption isotherm of each adsorbent is less than or equal to the preset ratio of the adsorption capacity of the adsorption isotherm, wherein , the desorption isotherm is a curve of desorption amount varying with pressure at the specified temperature.
  • the preset precondition further includes: at each pressure, the adsorption capacity of each adsorbent on the adsorption isotherm of the target adsorbate is less than or equal to the adsorption capacity of the desorption isotherm.
  • the specific temperature is 10°C to 40°C.
  • the initial pressure is less than or equal to 10kPa.
  • the adsorbent is selected from: microporous molecular sieves; MOFs; carbon molecular sieves; or silica gel.
  • the present invention is creatively based on the slope of the adsorption isotherm of each of the multiple adsorbents for the target adsorbate at the initial pressure and the adsorption rate of each adsorbent at the specific temperature and specific pressure.
  • the adsorption amount of the target adsorbate by the agent is selected from the plurality of adsorbents for adsorbing the target adsorbate, so that in the process of pressure swing adsorption, the cycle of pressure swing adsorption can be optimized to reduce the amount of adsorbent The dosage, thereby reducing the operating and production costs of pressure swing adsorption.
  • the second aspect of the present invention provides a pressure swing adsorption method, said pressure swing adsorption method comprising: said adsorbent selection method, selecting a target adsorbent for adsorbing one or more target adsorbates; and using said The target adsorbent performs pressure swing adsorption on the one or more target adsorbates.
  • the pressure swing adsorption method further includes: when the slope of the adsorption isotherm of the target adsorbent at the initial pressure point is greater than the first preset slope and less than or equal to the second preset slope, using the integrated Rotary valve controls the process sequence of pressure swing adsorption; or when the slope of the adsorption isotherm of the target adsorbent at the initial pressure point is greater than the second preset slope and less than or equal to the third preset slope, a program-controlled valve is used Controlling the process sequence of pressure swing adsorption.
  • the pressure swing adsorption method further includes: grading the multiple target adsorbents, and using the target adsorbent to The one or more target adsorbates performing pressure swing adsorption at a specific temperature include: using the graded multiple target adsorbents to perform pressure swing adsorption on the one or more target adsorbates at the specific temperature .
  • the pressure swing adsorption method further includes: setting each cycle of the pressure swing adsorption according to the slope of the adsorbent having the largest slope of the adsorption isotherm at the initial pressure among the plurality of target adsorbents. The minimum time to break down the sequence.
  • the selection method of the adsorbent select the target adsorbent for adsorbing one or more target adsorbates, and then use the target adsorbent to specify the one or more target adsorbates Pressure swing adsorption at low temperature, thus, the operation and production costs of pressure swing adsorption can be reduced by reducing the amount of adsorbent and optimizing the pressure swing adsorption cycle.
  • the third aspect of the present invention provides an adsorbent selection system, the selection system includes: a memory for storing the adsorption isotherm of each adsorbent in a plurality of adsorbents for a target adsorbate; and a processor configured to In order to perform the following operations: obtain the slope of the adsorption isotherm of each adsorbent for the target adsorbate at the initial pressure, wherein the adsorption isotherm is a curve of the adsorption amount varying with pressure at a specific temperature; obtain The adsorption capacity of each adsorbent on the target adsorbate at the specific temperature and specific pressure; and according to the slope and adsorption capacity of each adsorbent, select from the plurality of adsorbents to use A target adsorbent for adsorbing the target adsorbate.
  • the fourth aspect of the present invention provides a pressure swing adsorption system
  • the pressure swing adsorption system includes: the adsorbent selection system, used to select the target adsorbent for adsorbing one or more target adsorbates; and adsorption A device for performing pressure swing adsorption at a specific temperature on the one or more target adsorbates with the target adsorbent.
  • the fifth aspect of the present invention provides a computer-readable storage medium, where a computer program is stored on the computer-readable storage medium, and when the computer program is executed by a processor, the above-mentioned adsorbent selection method and/or the above-mentioned pressure change are realized Adsorption method.
  • Fig. 1 is the flowchart of the selection method of the adsorbent provided by an embodiment of the present invention
  • Fig. 2 is a flow chart of selecting a target adsorbent for adsorbing the target adsorbate from among the plurality of adsorbents provided by an embodiment of the present invention
  • Fig. 3 is the adsorption isotherm and desorption isotherm of a kind of adsorbent to certain adsorbate;
  • Fig. 4 is the slope curve of the adsorption isotherm and the slope curve of the desorption isotherm in Fig. 3;
  • Fig. 5 is the adsorption isotherm and desorption isotherm of a kind of adsorbent to certain adsorbate
  • Fig. 6 is the slope curve of the adsorption isotherm and the slope curve of the desorption isotherm in Fig. 5;
  • Fig. 7 is the adsorption isotherm and desorption isotherm of another kind of adsorbent to certain adsorbate;
  • Fig. 8 is the slope curve of the adsorption isotherm and the slope curve of the desorption isotherm in Fig. 7;
  • Fig. 9 is the adsorption isotherm and desorption isotherm of another kind of adsorbent to certain adsorbate;
  • Figure 10 is the slope curve of the adsorption isotherm and the slope curve of the desorption isotherm in Figure 9;
  • Figure 11 is an adsorption isotherm of an adsorbent for an adsorbate and a slope curve of the adsorption isotherm
  • Fig. 12 is an adsorption isotherm of an adsorbent for an adsorbate and a slope curve of the adsorption isotherm.
  • Fig. 1 is a flow chart of an adsorbent selection method provided by an embodiment of the present invention.
  • the selection method may include: step S101, obtaining the slope of the adsorption isotherm of each of the plurality of adsorbents on the target adsorbate at the initial pressure, wherein the adsorption isotherm is The curve of the adsorption amount changing with the pressure at a specific temperature; Step S102, obtaining the adsorption amount of each adsorbent on the target adsorbate at the specific temperature and specific pressure; and Step S103, according to the each The slope and the adsorption capacity of each adsorbent, and the target adsorbent for adsorbing the target adsorbate is selected from the plurality of adsorbents.
  • adsorbent type for the target adsorbate, it is possible to realize the fast-period pressure swing adsorption cycle, optimize the pressure swing adsorption process, realize the reduction of the amount of adsorbent, and effectively reduce the amount of the same production scale (the same impurity composition and content).
  • raw material gas) pressure swing adsorption device occupying an area and weight, reducing pressure swing adsorption operation and production costs.
  • step S101 the degree of coincidence between the adsorption isotherm and the desorption isotherm of each adsorbent for the target adsorbate can be obtained first, and then the degree of coincidence can be judged. If the coincidence degree is good, it indicates that the adsorbed adsorbate has been fully decomposed, and the desorption ability is strong, and step S101 is performed; otherwise, no corresponding subsequent steps need to be performed for the adsorbent.
  • the coincidence degree of the adsorption isotherm and the desorption isotherm refers to the coincidence degree of the adsorption amount of the two curves under the same pressure.
  • the adsorption isotherm refers to the static adsorption isotherm, which has the characteristics of good repeatability, easy access, and almost applicable to the performance characterization of all adsorbents;
  • the desorption isotherm refers to the adsorbent that has completed the static adsorption isotherm test. Next, start the reduced-pressure desorption to obtain the adsorption capacity isotherm.
  • the test method of the adsorption isotherm is to take the pressure as the abscissa, the unit is bar, and the adsorption amount as the ordinate, the unit is ml/g; the obtained adsorption isotherm represents the equilibrium of the adsorbent per unit mass under a certain adsorbate pressure Adsorption capacity.
  • the step of obtaining the slope of the adsorption isotherm of each of the plurality of adsorbents for the target adsorbate at the initial pressure is performed under the condition that preset preconditions are met.
  • the preset precondition may include: at each pressure, the absolute value of the difference between the adsorption isotherm and desorption isotherm of each adsorbent for the target adsorbate is less than or equal to the adsorption isotherm A preset ratio (for example, 15%) of the adsorption amount.
  • the desorption isotherm is a curve of desorption amount changing with pressure at the specific temperature.
  • the specific temperature is normal temperature (for example, 10°C to 40°C), preferably 25°C.
  • the preset precondition may further include: at each pressure, the adsorption amount of each adsorbent on the adsorption isotherm of the target adsorbate is less than or equal to the adsorption amount of the desorption isotherm.
  • the adsorbed adsorbate can be quickly and completely desorbed.
  • Step S101 acquiring the slope at the initial pressure of the adsorption isotherm of each of the multiple adsorbents for the target adsorbate.
  • the adsorption isotherm is a curve in which the adsorption amount varies with pressure at a specific temperature.
  • the specific temperature is normal temperature (for example, 10°C to 40°C), preferably 25°C. In this article, if there is no specific value for a specific temperature, it is assumed to be 25°C by default.
  • the initial pressure is less than or equal to 10kPa.
  • the pressure value setting can be the same for different adsorbents.
  • the adsorbent is selected from: microporous molecular sieves; MOFs; carbon molecular sieves; special adsorbents filled with specific materials (for example, filled with metal materials such as Cu/Zn) in microporous molecular sieves, MOFs or carbon molecular sieves; silica gel.
  • the particle size ranges from 0.4 mm to 2.5 mm, and the shaped adsorbent can be in the form of spheres, strips, columns, or core-shells.
  • the thickness of the sorbent coating is between 50 ⁇ m and 400 ⁇ m.
  • Structured adsorbent generally refers to coating adsorbent powder on a porous carrier, which can be metal sintered porous material, alumina sintered porous material, organic glass fiber porous material, etc.
  • Step S102 obtaining the adsorption amount of each adsorbent on the target adsorbate at the specific temperature and specific pressure.
  • the adsorption amount of each adsorbent on the target adsorbate at the specific temperature and specific pressure (for example, 1 bar) can be obtained.
  • specific pressure refers to a reasonable pressure for measuring the adsorption amount, which can be reasonably set according to actual conditions, and is not limited to 1 bar.
  • Step S103 selecting a target adsorbent for adsorbing the target adsorbate from the plurality of adsorbents according to the slope and adsorption capacity of each adsorbent.
  • the selection of the target adsorbent for adsorbing the target adsorbate from the plurality of adsorbents may include the following steps S201-S204.
  • Step S201 according to the slope of each adsorbent, determine the shortest time of each decomposition step in the pressure swing adsorption cycle of each adsorbent.
  • the entire cycle period (adsorption period) can be determined.
  • the determination of the shortest time of each decomposition step in the pressure swing adsorption cycle of each adsorbent includes: when the slope of an adsorbent is greater than the first slope and In the case of less than or equal to the second slope, the shortest time corresponding to the adsorbent is greater than or equal to the first shortest time; when the slope of an adsorbent is greater than the second slope and less than or equal to the third slope, The shortest time corresponding to the adsorbent is greater than or equal to the second shortest time; when the slope of an adsorbent is greater than the third slope and less than or equal to the fourth slope, the shortest time corresponding to the adsorbent is greater than or equal to the third shortest time; or when the slope of an adsorbent is greater than the fourth slope and less than or equal to the fifth slope, the shortest time corresponding to the adsorbent is greater than or equal to the fourth shortest time.
  • first slope, the second slope, the third slope, the fourth slope and the fifth slope gradually increase; and the first shortest time, the second shortest time, The third shortest time and the fourth shortest time gradually increase.
  • the first slope is 1, the second slope is 10, the third slope is 20, the fourth slope is 30, and the fifth slope is 50, the first minimum time is 0.05s, the second shortest time is 3s, the third shortest time is 9s, and the fourth shortest time is 24s.
  • the slope of the initial pressure point of the adsorption isotherm of the adsorbent is greater than 50 for the target adsorbate, it can be judged that the adsorbent is not suitable for the continuous production process of pressure swing adsorption at room temperature.
  • the adsorbent when the slope of the initial pressure point of the adsorption isotherm of the adsorbent is less than or equal to 50, the adsorbent is suitable for the normal temperature pressure swing adsorption process, and the periodic cycle adsorption of the adsorbent can be realized within a suitable pressure swing adsorption cycle time And regeneration (ie step-down regeneration process).
  • the time of each decomposition step in the pressure swing adsorption cycle is greater than or equal to 0.05s; when the adsorption of the selected adsorbent The slope of the initial pressure point of the isotherm is 10 ⁇ k 0 ⁇ 20, and the time of each decomposition step in the pressure swing adsorption cycle is greater than or equal to 3s; when the slope of the initial pressure point of the adsorption isotherm of the selected adsorbent is 20 ⁇ k 0 ⁇ 30, the time of each decomposition step in the pressure swing adsorption cycle is greater than or equal to 9s; when the slope of the initial pressure point of the adsorption isotherm of the selected adsorbent is 30 ⁇ k 0 ⁇ 50, the pressure swing adsorption cycle The time of each decomposition step in is greater than or equal to 24s.
  • the adsorbent is suitable for fast-cycle pressure swing adsorption.
  • the sequence time is greater than or equal to 0.05s.
  • the adsorbent is suitable for the time of each decomposition step in the cycle is greater than or equal to 3s fast cycle pressure swing adsorption.
  • the adsorbent is suitable for the time of each decomposition step in the cycle is greater than or equal to 9s fast cycle pressure swing adsorption.
  • the adsorbent is suitable for the time of each decomposition step in the cycle period is greater than or equal to 24s fast cycle pressure swing adsorption.
  • the adsorbent can be selected for gradation according to the above method.
  • the cycle period applicable to the composite bed layer of multiple adsorbent gradations is determined by the one that takes the longest time for the decomposition step. Adsorbent decision.
  • k 0 can be other reasonable ranges, for example, 50 ⁇ k 0 ⁇ 200, and, for different sub-ranges, it is also possible to determine each decomposition step in the cycle of pressure swing adsorption corresponding to different sub-ranges sequence time.
  • the determination of the shortest time t (in s) of each decomposition step in the cycle period of the pressure swing adsorption of each adsorbent may include:
  • T is the preset longest step time, the unit is s; and k 0 is the slope of each adsorbent.
  • the shortest time t of the decomposition step corresponding to each adsorbent can be determined according to the above formula.
  • Step S202 selecting a specific adsorbent from the plurality of adsorbents according to the determined shortest time.
  • the shortest time corresponding to the specific adsorbent is less than or equal to the preset time.
  • the preset time can be reasonably set according to the actual situation: for example, the preset time can be set to 15.10s (the corresponding slope is 24).
  • Adsorbent Adsorbate initial point slope Minimum time (s) Molecular sieve 1 N 2 twenty one 10.76 Molecular sieve 2 N 2 7 1.38 Activated carbon 1 N 2 8 1.62
  • the shortest time in Table 1 is obtained according to the calculation formula of t.
  • the shortest times corresponding to the three adsorbents are all less than 15.10 s, thus the three adsorbents can be selected.
  • the period of pressure swing adsorption can be optimized to realize rapid adsorption.
  • Step S203 determining the product of the slope and the adsorption capacity of the specific adsorbent.
  • Step S204 selecting the adsorbent corresponding to the maximum product as the target adsorbent.
  • the product value of the slope of the adsorption isotherm of molecular sieve 1 at the initial pressure and the adsorption capacity (1 bar/25°C) is the largest, so molecular sieve 1 is determined as the target adsorbent.
  • a small amount of target adsorbent can be used to achieve effective adsorption of the target adsorbate, reducing the volume of the adsorption tower.
  • the PSA cycle can be optimized, the amount of adsorbent can be reduced, and the operation and production costs of the PSA can be reduced, thereby ensuring the product recovery rate while satisfying the productivity of the PSA device.
  • the selection method further includes: determining the shortest time corresponding to the target adsorbent as the adsorption time; and according to the amount of the target adsorbate introduced into the adsorption tower within the adsorption time and the The adsorption amount of the target adsorbent is determined, and the amount of the target adsorbent is determined.
  • the shortest time corresponding to the target adsorbent determined in step S201 is determined as the adsorption time; then, the amount of target adsorbate introduced into the adsorption tower within the adsorption time can be determined, combined with the adsorption amount of the target adsorbent, it can be determined The amount of target adsorbate.
  • the present invention is creatively based on the slope of the adsorption isotherm of each of the plurality of adsorbents for the target adsorbate at the initial pressure and the adsorption capacity of each of the adsorbents at the specific temperature and specific pressure.
  • the adsorption amount of the target adsorbate to the target adsorbate, and the target adsorbent for adsorbing the target adsorbate is selected from the plurality of adsorbents, so that the pressure swing adsorption cycle can be optimized in the pressure swing adsorption process, and the adsorption capacity of the adsorbent can be reduced.
  • the dosage thereby reducing the operating and production costs of pressure swing adsorption.
  • An embodiment of the present invention also provides a pressure swing adsorption method, which includes: selecting a target adsorbent for adsorbing one or more target adsorbates according to the adsorbent selection method; and using The target adsorbent performs pressure swing adsorption on the one or more target adsorbates at a specific temperature.
  • the pressure swing adsorption method further includes: when the slope of the adsorption isotherm of the target adsorbent at the initial pressure point is greater than the first preset slope and less than or equal to the second preset slope , using an integrated rotary valve to control the pressure swing adsorption; or when the slope of the adsorption isotherm of the target adsorbent at the initial pressure point is greater than the second preset slope and less than or equal to the third preset slope, program-controlled The valve controls the process sequence of the pressure swing adsorption.
  • the integrated rotary valve is used to realize the process sequence, so that very precise control can be achieved; when the adsorption of the selected adsorbent When the slope of the isotherm at the initial pressure satisfies 20 ⁇ k 0 ⁇ 50, the process sequence is realized by using a program-controlled valve.
  • the pressure swing adsorption method further includes: grading the multiple target adsorbents, and using the target
  • the adsorbent performing pressure swing adsorption on the one or more target adsorbates at a specific temperature includes: using the graded multiple target adsorbents to perform pressure swing adsorption on the one or more target adsorbates at the specific temperature pressure swing adsorption.
  • the pressure swing adsorption method further includes: according to the slope of the adsorbent having the largest slope of the adsorption isotherm at the initial pressure among the plurality of target adsorbents, setting each decomposition step in the cycle of the pressure swing adsorption the shortest time.
  • adsorbents are selected for the multiple target adsorbates one by one, and the selected multiple adsorbents are graded.
  • grading refers to arranging multiple beds of target adsorbents according to the molecular weight of the target adsorbate, and adsorbing them sequentially according to the molecular weight of the corresponding target adsorbate from large to small.
  • the same adsorbent is more likely to adsorb the adsorbate with large molecular weight, but the impurities with large molecular weight are not easy to desorb. Therefore, it is beneficial for the desorption of the adsorbent to make the graded adsorbent adsorb the adsorbate in sequence according to the molecular weight.
  • the shortest time for each decomposition step in the cycle of pressure swing adsorption is determined by the target adsorbent with the largest slope of the adsorption isotherm at the initial pressure among the target adsorbents forming grades.
  • the relationship between the shortest time for each decomposition step of each adsorbent in the pressure swing adsorption cycle and the slope of the initial pressure point of the adsorption isotherm refers to the above technical solution, and will not be repeated here.
  • the process sequence of the pressure swing adsorption cycle includes the steps of adsorption, pressure equalization drop, desorption and pressure equalization increase in time sequence.
  • the number of adsorption towers - the number of towers in the adsorption state at the same time - the number of pressure equalization times are 10-3-4, 12-3-6, 4-1-2, 6-1-2, 8-2-3, 8-2-2 or 9-2-3 process flow.
  • This embodiment also provides the gradation method of the adsorbent, which provides a simple and feasible method for the gradation scheme of the adsorbent for the fast cycle pressure swing adsorption.
  • the fast cycle pressure swing adsorption method in each of the above embodiments can meet the requirements of various pressure swing adsorption cycle periods through the selection of the adsorbent, and does not need additional process sequences to compensate for the desorption performance of the adsorbent; increase the yield of the adsorbent bed Efficiency, reducing energy consumption in the regeneration process, such as reducing the amount of purge regeneration gas, reducing the power consumption of vacuuming, or even omitting vacuuming, so as to reduce the energy consumption of the entire process and effectively improve the overall efficiency.
  • the pressure swing adsorption cycle is the adsorption tower From the start of one adsorption to the completion of the final charge, and the time between preparing for the start of the next adsorption, the time of each pressure swing adsorption cycle is the sum of the time of all decomposition steps. Referring to Table 3, if the time of each decomposition step is 30s, then the entire pressure swing adsorption cycle is 480s (8min).
  • suction means the adsorption step sequence
  • charging means the final charging step sequence
  • drop 1/rise 1 means the first average pressure drop/rise step sequence
  • drop 2/rise 2 means the second average pressure drop/rise step sequence
  • sequence means the sequence Release step sequence
  • Reverse means reverse release step sequence
  • Blow means use forward blowing purge sequence.
  • Embodiment one (specific temperature is 25 °C)
  • the shortest time corresponding to the three adsorbents (molecular sieve 1, molecular sieve 2, and activated carbon 1) in Table 1 is less than 15.10 s, so the three adsorbents all meet the primary selection conditions. Then, the molecular sieve 1 with the largest product of slope and adsorption capacity (as shown in Table 2) was screened from the three adsorbents to determine it as the target adsorbent.
  • Embodiment two (specific temperature is 20 °C)
  • the composition (volume fraction) of the raw material gas is 1% nitrogen, 8% methane and 91% hydrogen, the pressure is 2 MPa, the temperature is 20° C., and the flow rate is 1000 Nm 3 /h.
  • the goal is to use pressure swing adsorption process to purify and produce hydrogen product (hydrogen purity: 99.999%) from this feed gas.
  • the purification process in this example is determined to be a typical 10-3-4 process, that is, 10 adsorption towers, 3 towers for simultaneous adsorption, 4 pressure equalization processes, the yield remains unchanged at 85%, and the material balance is shown in Table 4.
  • the fast cycle pressure swing adsorption method of the present invention the adsorption isotherm and desorption isotherm of the adsorbent to two kinds of adsorbates (nitrogen and methane), and the corresponding slope curves are measured.
  • the three adsorbents shown in Table 5 can realize the rapid cycle pressure swing adsorption process at room temperature.
  • one kind of adsorbent can be used to realize the purification of the above-mentioned raw material gas to produce hydrogen, and the method of adsorbent grading can also be used to realize hydrogen purification.
  • the adsorption times of the three adsorbents are all less than 15.10s (or the slopes are all less than 24), so they all meet the primary selection conditions; then select the molecular sieve 2 with the largest slope and adsorption capacity as the target adsorbent.
  • the adsorption time of molecular sieve 1 is less than 15.10s (or the slope is less than 24), so molecular sieve 1 is determined as the target adsorbent.
  • the slope of molecular sieve 2 is larger, the corresponding shortest time 8s is determined as the shortest time of each decomposition step of pressure swing adsorption, so it can be determined that the adsorption cycle is about 2.7min.
  • Adsorbent loading scheme 1 uses a graded bed composed of molecular sieve 2 and molecular sieve 1.
  • the molecular weight of methane is greater than that of nitrogen. Therefore, when the adsorbent is loaded in grades, the raw material gas first passes through molecular sieve 1 to absorb methane, and then through molecular sieve 2 to absorb nitrogen. .
  • the adsorption period is determined by the adsorbent with the largest slope of the initial point of the adsorption isotherm, the activated carbon bed can ensure that methane is completely adsorbed and is not brought into the molecular sieve bed, so that the effects of the two adsorbents can be maximized.
  • the adsorption cycle is preferably 2.7min.
  • the grading scheme takes into account the adsorption period and the adsorption capacity of the adsorbent to the adsorbate, and makes use of the characteristics of each adsorbent for different adsorbates, so that the optimal grading process and operation cycle can be realized. At the same time, the volume of the adsorption tower can be realized minimum.
  • the present invention creatively selects target adsorbents for adsorbing one or more target adsorbates according to the adsorbent selection method, and then adopts the target adsorbents for the one or more target adsorbents.
  • the adsorbate undergoes pressure swing adsorption at a specific temperature, thereby reducing the operation and production costs of pressure swing adsorption by reducing the amount of adsorbent and optimizing the pressure swing adsorption cycle.
  • An embodiment of the present invention also provides an adsorbent selection system, the selection system includes: a memory for storing the adsorption isotherm of each adsorbent on a target adsorbate in a plurality of adsorbents; It is configured to perform the following operation: obtain the slope of the adsorption isotherm of each adsorbent for the target adsorbate at the initial pressure, wherein the adsorption isotherm is a curve of adsorption amount varying with pressure at a specific temperature; Obtaining the adsorption capacity of each adsorbent on the target adsorbate at the specific temperature and specific pressure; and selecting from the plurality of adsorbents according to the slope and adsorption capacity of each adsorbent A target adsorbent for adsorbing the target adsorbate.
  • An embodiment of the present invention also provides a pressure swing adsorption system, the pressure swing adsorption system comprising: according to the adsorbent selection system, for selecting a target adsorbent for adsorbing one or more target adsorbates; And an adsorption device for performing pressure swing adsorption at a specific temperature on the one or more target adsorbates by using the target adsorbent.
  • An embodiment of the present invention also provides a computer-readable storage medium, where a computer program is stored on the computer-readable storage medium, and when the computer program is executed by a processor, the above-mentioned adsorbent selection method and/or the above-mentioned variable pressure adsorption method.
  • the aforementioned storage media include: U disk, mobile hard disk, read-only memory (ROM, Read-Only Memory), random access memory (RAM, Random Access Memory), magnetic disk or optical disc, etc., which can store program codes. .

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Abstract

一种吸附剂的选择方法、变压吸附方法及其系统。选择方法包括：获取多个吸附剂中的每个吸附剂对目标吸附质的吸附等温线在初始压力处的斜率，其中，吸附等温线为在特定温度下吸附量随压力变化的曲线；获取在所述特定温度与特定压力下的每个吸附剂对所述目标吸附质的吸附量；以及根据每个吸附剂的斜率与吸附量，从多个吸附剂中选择用于吸附目标吸附质的目标吸附剂。在变压吸附过程中可优化变压吸附周期，减少吸附剂的用量，进而降低变压吸附运行与生产成本。

Description

吸附剂的选择方法、变压吸附方法及其系统
相关申请的交叉引用
本申请要求2021年12月31日提交的中国专利申请202111681815.7的权益，该申请的内容通过引用被合并于本文。
技术领域
本发明实施例涉及吸附分离技术领域，特别涉及一种吸附剂的选择方法、变压吸附方法及其系统。
背景技术
变压吸附技术可用于氢气、氦气、氮气等气体的提纯，还可用于二氧化碳捕集、低碳烃类的回收等工业过程。变压吸附根据应用场景不同，选用的吸附剂可以吸附需要脱除的杂质，或吸附需要生产的产品，吸附剂吸附的杂质或产品都称为吸附质。吸附剂、控制工艺与设备是变压吸附技术应用于生产的关键。
根据不同的吸附质选择吸附剂，并匹配相应的控制工艺，进一步选用可靠的设备，是实现变压吸附最优化生产方案的一般流程。一般而言，变压吸附通过不少于两个塔的顺序切换实现连续生产，每个塔器中装填同样种类、相等重量的吸附剂，在一个吸附塔中装填一定量的吸附剂，可以通过延长吸附周期的方式提高产品回收率；如果减少吸附剂的装填量，则可以通过缩短吸附周期的方式保证产品回收率、并减小装置占地。
在现有技术中，针对不同的吸附质，主要通过经验选择相应吸附剂，由此，通常需要装填过量的吸附剂且设置较长的吸附周期，来实现充分吸附的目的。
从可持续发展的角度出发，在保证变压吸附装置整体性能的条件下，通过减少吸附剂使用量，进而减小吸附塔体积，实现减小装置占地是更优的选择。因此，针对同样原料的气体变压吸附过程，如何实现优化变压吸附周期，减少吸附剂用量，从而减小装置占地与总重是亟待解决的问题。
发明内容
本发明的目的是提供一种吸附剂的选择方法、变压吸附方法及其系统，其可基于吸附等温线在初始压力处的斜率及特定温度与特定压力下的吸附剂对目标吸附质的吸附量，选择目标吸附剂，从而在变压吸附过程中可优化变压吸附周期，减少吸附剂的用量，进而降低变压吸附运行与生产成本。
为了实现上述目的，本发明第一方面提供一种吸附剂的选择方法，所述选择方法包括：获取多个吸附剂中的每个吸附剂对目标吸附质的吸附等温线在初始压力处的斜率，其中，所述吸附等温线为在特定温度下吸附量随压力变化的曲线；获取在所述特定温度与特定压力下的所述每个吸附剂对所述目标吸附质的吸附量；以及根据所述每个吸附剂的斜率与吸附量，从所述多个吸附剂中选择用于吸附所述目标吸附质的目标吸附剂。
优选地，所述从所述多个吸附剂中选择用于吸附所述目标吸附质的目标吸附剂包括：根据所述每个吸附剂的斜率，确定在所述每个吸附剂的变压吸附的循环周期中的每个分解步序的最短时间；根据所确定的最短时间，从所述多个吸附剂中选择特定吸附剂，其中，所述特定吸附剂所对应的最短时间小于或等于预设时间；确定所述特定吸附剂的斜率与吸附量的乘积；以及将与最大乘积相对应的吸附剂选择为所述目标吸附剂。
优选地，所述确定在所述每个吸附剂的变压吸附的循环周期中的每个分解步序的最短时间包括：在一吸附剂的斜率大于第一斜率且小于或等于第二斜率的情况下，与该吸附剂所对应的最短时间大于或等于第一最短时间；在一吸附剂的斜率大于所述第二斜率且小于或等于第三斜率的情况下，与该吸附剂所对应的最短时间大于或等于第二最短时间；在一吸附剂的斜率大于所述第三斜率且小于或等于第四斜率的情况下，与该吸附剂所对应的最短时间大于或等于第三最短时间；或者在一吸附剂的斜率大于所述第四斜率且小于或等于第五斜率的情况下，与该吸附剂所对应的最短时间大于或等于第四最短时间，其中，所述第一斜率、所述第二斜率、所述第三斜率、所述第四斜率以及所述第五斜率逐渐增大；以及所述第一最短时间、所述第二最短时间、所述第三最短时间以及所述第四最短时间逐渐增大。
优选地，在所述第一斜率为1、所述第二斜率为10、所述第三斜率为20、所述第四斜率为30且所述第五斜率为50的情况下，所述第一最短时间为0.05s、所述第二最短时间为3s、所述第三最短时间为9s且所述第四最短时间为24s。
优选地，所述确定在所述每个吸附剂的变压吸附的循环周期中的每个分解步序的最短时间t包括：
Figure PCTCN2022136912-appb-000001
其中，T为预设最长步序时间，单位为s；以及k 0为所述每个吸附剂的斜率。
优选地，T小于或等于40。
优选地，所述选择方法还包括：将所确定的最短时间确定为吸附时间；以及根据在所述吸附时间内引入吸附塔的所述目标吸附质的量以及所述目标吸附剂的吸附量，确定所述目标吸附剂的量。
优选地，所述获取多个吸附剂中的每个吸附剂对目标吸附质的吸附等温线在初始压力处的斜率的步骤在满足预设前提条件下被执行，其中，所述预设前提条件包括：在各个压力处，所述每个吸附剂对所述目标吸附质的吸附等温线与解吸等温线的吸附量之差 的绝对值小于或等于吸附等温线的吸附量的预设比例，其中，所述解吸等温线为在所述特定温度下解吸量随压力变化的曲线。
优选地，所述预设前提条件还包括：在各个压力处，所述每个吸附剂对所述目标吸附质的吸附等温线的吸附量小于或等于解吸等温线的吸附量。
优选地，所述特定温度为10℃～40℃。
优选地，所述初始压力小于或等于10kPa。
优选地，所述吸附剂选自：微孔分子筛；MOFs；碳分子筛；；或者硅胶。
通过上述技术方案，本发明创造性地根据多个吸附剂中的每个吸附剂对目标吸附质的吸附等温线在初始压力处的斜率及在所述特定温度与特定压力下的所述每个吸附剂对所述目标吸附质的吸附量，从所述多个吸附剂中选择用于吸附所述目标吸附质的目标吸附剂，从而在变压吸附过程中可，优化变压吸附周期减少吸附剂的用量，进而降低变压吸附运行与生产成本。
本发明第二方面提供一种变压吸附方法，所述变压吸附方法包括：所述的吸附剂的选择方法，选择用于吸附一个或多个目标吸附质的目标吸附剂；以及采用所述目标吸附剂对所述一个或多个目标吸附质进行变压吸附。
优选地，所述变压吸附方法还包括：在所述目标吸附剂的吸附等温线在初始压力点处的斜率大于第一预设斜率且小于或等于第二预设斜率的情况下，采用集成旋转阀控制变压吸附的工艺时序；或者在所述目标吸附剂的吸附等温线在初始压力点处的斜率大于所述第二预设斜率且小于或等于第三预设斜率时，采用程控阀控制变压吸附的工艺时序。
优选地，在所述目标吸附剂为多个目标吸附剂的情况下，所述变压吸附方法还包括：对所述多个目标吸附剂进行级配，所述采用所述目标吸附剂对所述一个或多个目标吸附质进行特定温度下的变压吸附包括：采用级配后的所述多个目标吸附剂对所述一个或多个目标吸附质进行所述特定温度下的变压吸附。
优选地，所述变压吸附方法还包括：根据所述多个目标吸附剂中的具有吸附等温线在初始压力处的最大斜率的吸附剂的斜率，设置变压吸附的循环周期中的每个分解步序的最短时间。
通过上述技术方案，根据所述的吸附剂的选择方法，选择用于吸附一个或多个目标吸附质的目标吸附剂，然后采用所述目标吸附剂对所述一个或多个目标吸附质进行特定温度下的变压吸附，由此，可通过减少吸附剂的用量与优化变压吸附周期来降低变压吸附运行与生产成本。
本发明第三方面提供一种吸附剂的选择系统，所述选择系统包括：存储器，用于存储多个吸附剂中的每个吸附剂对目标吸附质的吸附等温线；以及处理器，被配置为执行以下操作：获取所述每个吸附剂对所述目标吸附质的吸附等温线在初始压力处的斜率， 其中，所述吸附等温线为在特定温度下吸附量随压力变化的曲线；获取在所述特定温度与特定压力下的所述每个吸附剂对所述目标吸附质的吸附量；以及根据所述每个吸附剂的斜率与吸附量，从所述多个吸附剂中选择用于吸附所述目标吸附质的目标吸附剂。
有关本发明提供的吸附剂的选择系统的具体细节及益处可参阅上述针对吸附剂的选择方法的描述，于此不再赘述。
本发明第四方面提供一种变压吸附系统，所述变压吸附系统包括：所述的吸附剂的选择系统，用于选择用于吸附一个或多个目标吸附质的目标吸附剂；以及吸附装置，用于采用所述目标吸附剂对所述一个或多个目标吸附质进行特定温度下的变压吸附。
有关本发明提供的变压吸附系统的具体细节及益处可参阅上述针对变压吸附方法的描述，于此不再赘述。
本发明第五方面提供一种计算机可读存储介质，所述计算机可读存储介质上存储有计算机程序，该计算机程序被处理器执行时实现上述的吸附剂的选择方法和/或上述的变压吸附方法。
本发明的其它特征和优点将在随后的具体实施方式部分予以详细说明。
附图说明
附图是用来提供对本发明实施例的进一步理解，并且构成说明书的一部分，与下面的具体实施方式一起用于解释本发明实施例，但并不构成对本发明实施例的限制。在附图中：
图1是本发明一实施例提供的吸附剂的选择方法的流程图；
图2是本发明一实施例提供的从所述多个吸附剂中选择用于吸附所述目标吸附质的目标吸附剂的流程图；
图3为一种吸附剂对某吸附质的吸附等温线与解吸等温线；
图4为图3中吸附等温线的斜率曲线与解吸等温线的斜率曲线；
图5为一种吸附剂对某吸附质的吸附等温线与解吸等温线；
图6为图5中吸附等温线的斜率曲线与解吸等温线的斜率曲线；
图7为另一种吸附剂对某吸附质的吸附等温线与解吸等温线；
图8为图7中吸附等温线的斜率曲线与解吸等温线的斜率曲线；
图9为另一种吸附剂对某吸附质的吸附等温线与解吸等温线；
图10为图9中吸附等温线的斜率曲线与解吸等温线的斜率曲线；
图11为一种吸附剂对某吸附质的吸附等温线及该吸附等温线的斜率曲线；以及
图12为一种吸附剂对某吸附质的吸附等温线及该吸附等温线的斜率曲线。
具体实施方式
以下结合附图对本发明的具体实施方式进行详细说明。应当理解的是，此处所描述的具体实施方式仅用于说明和解释本发明，并不用于限制本发明。
图1是本发明一实施例提供的吸附剂的选择方法的流程图。如图1所示，所述选择方法可包括：步骤S101，获取多个吸附剂中的每个吸附剂对目标吸附质的吸附等温线在初始压力处的斜率，其中，所述吸附等温线为在特定温度下吸附量随压力变化的曲线；步骤S102，获取在所述特定温度与特定压力下的所述每个吸附剂对所述目标吸附质的吸附量；以及步骤S103，根据所述每个吸附剂的斜率与吸附量，从所述多个吸附剂中选择用于吸附所述目标吸附质的目标吸附剂。
本实施例通过针对目标吸附质进行吸附剂选型，能够实现快周期变压吸附循环，优化变压吸附工艺流程，实现减少吸附剂用量，有效减少同生产规模(相同杂质组成与含量的等量原料气)变压吸附装置的占地与重量，降低变压吸附运行与生产成本。
在执行步骤S101之前，可先获取每个吸附剂对目标吸附质的吸附等温线与解吸等温线的重合度，然后判断所述重合度。若重合度较好，则表明将吸附的吸附质充分地解析出来，解析能力较强，执行步骤S101；否则，，针对该吸附剂无需执行相应的后续步骤。
其中，吸附等温线与解吸等温线的重合度是指两条曲线在同一压力下的吸附量的重合度。具体地，吸附等温线指静态吸附等温线，具有重复性好、易于获得、几乎适用所有吸附剂的性能表征的特点；解吸等温线指完成静态吸附等温线测试的吸附剂，在同样的温度条件下，开始降压解吸获得的吸附量等温线。吸附等温线的测试方法为，以压力为横坐标，单位为bar，以吸附量为纵坐标，单位为ml/g；获得的吸附等温线表示单位质量的吸附剂在一定吸附质压力下的平衡吸附量。
在一实施例中，所述获取多个吸附剂中的每个吸附剂对目标吸附质的吸附等温线在初始压力处的斜率的步骤(即步骤S101)在满足预设前提条件下被执行。
其中，所述预设前提条件可包括：在各个压力处，所述每个吸附剂对所述目标吸附质的吸附等温线与解吸等温线的吸附量之差的绝对值小于或等于吸附等温线的吸附量的预设比例(例如15％)。
其中，所述解吸等温线为在所述特定温度下解吸量随压力变化的曲线。所述特定温度为常温(例如，10℃～40℃)，优选为25℃。
优选地，所述预设前提条件还可包括：在各个压力处，所述每个吸附剂对所述目标吸附质的吸附等温线的吸附量小于或等于解吸等温线的吸附量。由此，可快速将吸附的吸附质完全且快速地解析出来。
步骤S101，获取多个吸附剂中的每个吸附剂对目标吸附质的吸附等温线在初始压 力处的斜率。
其中，所述吸附等温线为在特定温度下吸附量随压力变化的曲线。所述特定温度为常温(例如，10℃～40℃)，优选为25℃。在本文中，若无特别指出特定温度的数值，均默认为25℃。
其中，所述初始压力小于或等于10kPa。对于不同的吸附剂该压力值设置可以是相同的。
其中，所述吸附剂选自：微孔分子筛；MOFs；碳分子筛；在微孔分子筛、MOFs或碳分子筛中填充特定材料(例如，填充Cu/Zn等金属材料)的专用吸附剂；硅胶。
例如，对于成型的吸附剂，粒径范围在0.4mm至2.5mm之间，成型的吸附剂可以是球状、条状、柱状或核壳等型式。对于结构化吸附剂，吸附剂涂层的厚度在50μm至400μm之间。结构化的吸附剂一般指将吸附剂粉涂敷在多孔载体上，多孔载体可以为金属烧结多孔材料、氧化铝烧结多孔材料、有机玻璃纤维多孔材料等。
具体地，首先，测定吸附剂的特定温度下的静态吸附等温线与解吸等温线(如图3、图5、图7、图9、图11-12所示)，进一步对吸附等温线与解吸等温线的拟合曲线求取导数(切线斜率)，获得每个点的切线斜率并得到等温线斜率曲线(如图4、图6、图8、图10-12所示)，从而可得到各个吸附等温线在初始压力处的斜率。当然，也可仅获取在初始压力处的斜率即可。
步骤S102，获取在所述特定温度与特定压力下的所述每个吸附剂对所述目标吸附质的吸附量。
从每个吸附剂对目标吸附质的吸附等温线上，可获取所述特定温度与特定压力(例如，1bar)下的所述每个吸附剂对所述目标吸附质的吸附量。在本文中，若无特别指出特定压力的数值，可均默认为1bar。当然，所述特定压力是指用于测量吸附量的一个合理的压力，其可根据实际情况进行合理设置，而不限于1bar。
步骤S103，根据所述每个吸附剂的斜率与吸附量，从所述多个吸附剂中选择用于吸附所述目标吸附质的目标吸附剂。
对于步骤S103，如图2所示，所述从所述多个吸附剂中选择用于吸附所述目标吸附质的目标吸附剂可包括以下步骤S201-S204。
步骤S201，根据所述每个吸附剂的斜率，确定在所述每个吸附剂的变压吸附的循环周期中的每个分解步序的最短时间。
根据所确定的每个分解步序的最短时间，可确定整个循环周期(吸附周期)。
在一实施例中，对于步骤S201，所述确定在所述每个吸附剂的变压吸附的循环周期中的每个分解步序的最短时间包括：在一吸附剂的斜率大于第一斜率且小于或等于第二斜率的情况下，与该吸附剂所对应的最短时间大于或等于第一最短时间；在一吸附剂 的斜率大于所述第二斜率且小于或等于第三斜率的情况下，与该吸附剂所对应的最短时间大于或等于第二最短时间；在一吸附剂的斜率大于所述第三斜率且小于或等于第四斜率的情况下，与该吸附剂所对应的最短时间大于或等于第三最短时间；或者在一吸附剂的斜率大于所述第四斜率且小于或等于第五斜率的情况下，与该吸附剂所对应的最短时间大于或等于第四最短时间。
其中，所述第一斜率、所述第二斜率、所述第三斜率、所述第四斜率以及所述第五斜率逐渐增大；以及所述第一最短时间、所述第二最短时间、所述第三最短时间以及所述第四最短时间逐渐增大。
在所述第一斜率为1、所述第二斜率为10、所述第三斜率为20、所述第四斜率为30且所述第五斜率为50的情况下，所述第一最短时间为0.05s、所述第二最短时间为3s、所述第三最短时间为9s且所述第四最短时间为24s。
具体地，若对于目标吸附质，吸附剂的吸附等温线初始压力点的斜率大于50时，可判断该吸附剂不适用于常温的变压吸附连续生产过程。对于目标吸附质，吸附剂的吸附等温线初始压力点的斜率小于或等于50时，该吸附剂适用于常温变压吸附过程，在适宜的变压吸附周期时间内可以实现吸附剂的周期循环吸附与再生(即降压再生工艺)。
例如，当所选择的吸附剂的吸附等温线初始压力点的斜率1＜k 0≤10，变压吸附的循环周期中每个分解步序的时间大于或等于0.05s；当所选择的吸附剂的吸附等温线初始压力点的斜率10＜k 0≤20，变压吸附的循环周期中每个分解步序的时间大于或等于3s；当所选择的吸附剂的吸附等温线初始压力点的斜率20＜k 0≤30，变压吸附的循环周期中每个分解步序的时间大于或等于9s；当所选择的吸附剂的吸附等温线初始压力点的斜率30＜k 0≤50，变压吸附的循环周期中每个分解步序的时间大于或等于24s。
当测定的吸附剂对某一吸附质的吸附等温线和解吸等温线以及相应的斜率曲线如图1和图2所示，该吸附剂适用于快周期变压吸附，循环周期中每个分解步序的时间大于或等于0.05s即可。
当测定的吸附剂对某一吸附质的吸附等温线和解吸等温线以及相应的斜率曲线如图3和图4所示，该吸附剂适用于循环周期中每个分解步序的时间大于或等于3s的快周期变压吸附。
当测定的吸附剂对某一吸附质的吸附等温线和解吸等温线以及相应的斜率曲线如图5和图6所示，该吸附剂适用于循环周期中每个分解步序的时间大于或等于9s的快周期变压吸附。
当测定的吸附剂对某一吸附质的吸附等温线和解吸等温线以及相应的斜率曲线如图7和图8所示，该吸附剂适用于循环周期中每个分解步序的时间大于或等于24s的快周期变压吸附。
当气源中含有多种需要吸附质组分时，可按照上述方法选择吸附剂进行级配，多种吸附剂级配的复合床层适用的循环周期，由分解步序所需时间最长的吸附剂决定。
当测定的吸附剂对某一吸附质的吸附等温线与吸附等温线切线斜率曲线如图9或图10所示，由于该吸附剂在测定温度下，不能实现解吸，故不能得到同温度的解吸等温线；同时，该吸附剂吸附等温线初始压力点的斜率大于50，该吸附剂不能用于实现常温变压吸附过程。
因此，上述实施例可适用于降压再生工艺。对于其他工艺，k 0可为其他合理范围，例如，50＜k 0≤200，并且，也可针对不同的子范围，确定与不同的子范围对应的变压吸附的循环周期中每个分解步序的时间。
在另一实施例中，对于步骤S201，所述确定在所述每个吸附剂的变压吸附的循环周期中的每个分解步序的最短时间t(单位为s)可包括：
Figure PCTCN2022136912-appb-000002
其中，T为预设最长步序时间，单位为s；以及k 0为所述每个吸附剂的斜率。
由于本实施例适用于快周期变压吸附过程，故T小于或等于40(在本文中，如无特殊说明，均默认T＝40)。在根据步骤S101获取k 0的情况下，可根据上式确定每个吸附剂对应的分解步序的最短时间t。
因此，上述实施例的适用范围非常广，不仅可适用于降压再生工艺(无需抽真空)，还可适用于采用抽真空与包含吹扫工艺的吸附剂选择与级配，并且据此确定的最短时间的结果也非常精确。
步骤S202，根据所确定的最短时间，从所述多个吸附剂中选择特定吸附剂。
其中，所述特定吸附剂所对应的最短时间小于或等于预设时间。该预设时间可根据实际情况进行合理设定：例如，可设置预设时间为15.10s(其对应的斜率为24)。
表1三种吸附剂吸附吸附质N 2的具体参数
吸附剂 吸附质 初始点斜率 最短时间(s)
分子筛1 N 2 21 10.76
分子筛2 N 2 7 1.38
活性炭1 N 2 8 1.62
表1中的最短时间根据t的计算公式求得。对于表1来说，三种吸附剂所对应的最短时间均小于15.10s，由此可选出所述三种吸附剂。通过本步骤可优化变压吸附的周期，以实现快速吸附。
步骤S203，确定所述特定吸附剂的斜率与吸附量的乘积。
例如，根据下述每个吸附剂的斜率与吸附量，确定相应的乘积，如表2所示。
表2三种吸附剂吸附吸附质N 2的具体参数
吸附剂 吸附质 初始点斜率 吸附量 乘积
分子筛1 N 2 21 18 378
分子筛2 N 2 7 7.5 52.5
活性炭1 N 2 8 9.2 73.6
步骤S204，将与最大乘积相对应的吸附剂选择为所述目标吸附剂。
例如，分子筛1的吸附等温线在初始压力处的斜率与吸附量(1bar/25℃)乘积值最大，所以将分子筛1确定为目标吸附剂。通过本步骤可采用少量的目标吸附剂实现对目标吸附质的有效吸附，减小吸附塔体积。
因此，通过上述各个实施例可优化变压吸附周期，减少吸附剂用量，降低变压吸附运行与生产成本，从而在满足变压吸附装置生产率的同时，保证产品回收率。
在一实施例中，所述选择方法还包括：将所述目标吸附剂所对应的最短时间确定为吸附时间；以及根据在所述吸附时间内引入吸附塔的所述目标吸附质的量以及所述目标吸附剂的吸附量，确定所述目标吸附剂的量。
例如，通过步骤S201确定的目标吸附剂所对应的最短时间确定为吸附时间；然后，可确定所述吸附时间内引入吸附塔的目标吸附质的量，再结合目标吸附剂的吸附量，可确定目标吸附质的量。
上述各个实施例可以针对各种目标吸附质进行吸附剂的选型，同时对备选的吸附剂无特别限定，因此，适用范围广泛。
综上所述，本发明创造性地根据多个吸附剂中的每个吸附剂对目标吸附质的吸附等温线在初始压力处的斜率及在所述特定温度与特定压力下的所述每个吸附剂对所述目标吸附质的吸附量，从所述多个吸附剂中选择用于吸附所述目标吸附质的目标吸附剂，从而在变压吸附过程中可优化变压吸附周期，减少吸附剂的用量，进而降低变压吸附运行与生产成本。
本发明一实施例还提供一种变压吸附方法，所述变压吸附方法包括：根据所述的吸附剂的选择方法，选择用于吸附一个或多个目标吸附质的目标吸附剂；以及采用所述目标吸附剂对所述一个或多个目标吸附质进行特定温度下的变压吸附。
在一实施例中，所述变压吸附方法还包括：在所述目标吸附剂的吸附等温线在初始压力点处的斜率大于第一预设斜率且小于或等于第二预设斜率的情况下，采用集成旋转阀控制变压吸附的；或者在所述目标吸附剂的吸附等温线在初始压力点处的斜率大于所述第二预设斜率且小于或等于第三预设斜率时，采用程控阀控制变压吸附的工艺时序。
例如，当所选择的吸附剂的吸附等温线在初始压力处的斜率满足1＜k 0≤20时，采 用集成旋转阀实现工艺时序，由此可实现非常精准的控制；当所选择的吸附剂的吸附等温线在初始压力处的斜率满足20＜k 0≤50时，采用程控阀实现工艺时序。
在另一实施例中，在所述目标吸附剂为多个目标吸附剂的情况下，所述变压吸附方法还包括：对所述多个目标吸附剂进行级配，所述采用所述目标吸附剂对所述一个或多个目标吸附质进行特定温度下的变压吸附包括：采用级配后的所述多个目标吸附剂对所述一个或多个目标吸附质进行所述特定温度下的变压吸附。
所述变压吸附方法还包括：根据所述多个目标吸附剂中的具有吸附等温线在初始压力处的最大斜率的吸附剂的斜率，设置变压吸附的循环周期中的每个分解步序的最短时间。
具体地，当目标吸附质为多个时，例如，原料气包含多种组分，逐一对多个目标吸附质选择吸附剂，将所选择的多个吸附剂形成级配。在一实施例中，级配是指按照目标吸附质的分子量的大小设置多个目标吸附剂所在的床层，按照对应目标吸附质的分子量由大到小依次吸附。同一吸附剂一般更易于吸附大分子量的吸附质，但是，大分子量的杂质不容易解吸，因此，使级配的吸附剂按分子量大小依次吸附吸附质，有利于吸附剂的解吸。
进一步地，变压吸附的循环周期中每个分解步序的最短时间由形成级配的目标吸附剂中的吸附等温线在初始压力处的斜率最大的目标吸附剂决定。每种吸附剂对变压吸附的循环周期的每个分解步序的最短时间与吸附等温线初始压力点的斜率的关系参照上述技术方案中所述，在此不再赘述。
进一步地，变压吸附的循环周期的工艺时序包括按时间顺序的吸附、均压降、解吸和均压升步骤。
进一步地，采用吸附塔数-同时处于吸附状态的塔数-均压次数为10-3-4、12-3-6、4-1-2、6-1-2、8-2-3、8-2-2或9-2-3的工艺流程。
本实施例还提供了吸附剂的级配方式，为快周期变压吸附的吸附剂的级配方案提供了简单易行的实现方法。
上述各个实施例中的快周期变压吸附方法能够通过吸附剂的选型，满足各种时长的变压吸附循环周期要求，无需额外工艺时序弥补吸附剂的解吸性能；增加吸附剂床层的产率、减小再生过程的能耗，如，减少吹扫再生气的用量、减少抽真空的功耗，甚至省略抽真空，从而降低整个过程能耗，有效提高综合效率。
以典型的8-2-2(即八个吸附塔、两个吸附塔同时处于吸附步序，每个周期经过两次均压降与均压升)工艺为例，变压吸附周期为吸附塔从一次吸附开始至终充完成，准备好下次吸附开始之间的时间，每个变压吸附周期的时间为所有分解步序的时间之和。参考表3所示，若每个分解步序的时间为30s，那么整个变压吸附周期为480s(8min)。 表3中吸表示吸附步序；充表示终充步序；降1/升1表示一次均压降/升步序，降2/升2表示二次均压降/升步序，顺表示顺放步序；逆表示逆放步序；吹表示利用顺放气吹扫步序。
表3典型8-2-2工艺的分解步序
Figure PCTCN2022136912-appb-000003
下面以具体实施例的方式更详细地说明本发明的快周期变压吸附方法，应了解的是，实施例仅为示例性的，本发明并不以此为限。
实施例一(特定温度为25℃)
对于吸附质N 2来说，表1中的三种吸附剂(分子筛1、分子筛2、活性炭1)对应的最短时间小于15.10s，故三种吸附剂均符合初选条件。再从三种吸附剂中筛选斜率与吸附量的乘积最大的分子筛1(如表2所示)，将其确定为目标吸附剂。
实施例二(特定温度为20℃)
本实施例中，原料气的组成(体积分数)为氮气1％，甲烷8％和氢气91％，压力为2MPa，温度为20℃，流量为1000Nm 3/h。目标是采用变压吸附工艺从该原料气中提纯制取氢气产品(氢气纯度：99.999％)。
本实施例中提纯工艺确定为典型10-3-4流程，即10个吸附塔，3塔同时吸附，4次均压流程，收率保持85％不变，物料平衡如表4所示。根据本发明的快周期变压吸附方法，测定吸附剂对两种吸附质(氮气和甲烷)的吸附等温线与解吸等温线，及其对应的斜率曲线。表5所示的三种吸附剂可实现常温快周期变压吸附过程。
表4物料平衡
Figure PCTCN2022136912-appb-000004
表5三种吸附剂的测定结果
Figure PCTCN2022136912-appb-000005
根据上述吸附剂测定结果，可以采用一种吸附剂实现对上述原料气的提纯制取氢气，也可以采用吸附剂级配的方法实现氢气提纯。对于氮气，三种吸附剂的吸附时间均小于15.10s(或者斜率均小于24)，故均满足初选条件；再选择斜率与吸附量最大的分子筛2确定为目标吸附剂。对于甲烷，分子筛1的吸附时间小于15.10s(或者斜率小于24)，故将分子筛1确定为目标吸附剂。并且，由于分子筛2的斜率更大，故将其所对应的最短时间8s确定为变压吸附的每个分解步序的最短时间，由此可确定吸附周期约为2.7min。选择不同的吸附剂，吸附周期与吸附塔体积之间的关系，如表6所示。
表6目标吸附剂装填方案的适用吸附周期及吸附塔体积
Figure PCTCN2022136912-appb-000006
吸附剂装填方案1采用分子筛2和分子筛1组成的级配床层，甲烷的分子量大于氮气的分子量，因此吸附剂级配装填时，满足原料气先经分子筛1吸附甲烷，再经分子筛2吸附氮气。虽然吸附周期由吸附等温线初始点斜率最大的吸附剂决定，但是，活性炭床层可以保证将甲烷吸附完全，并不带入分子筛床层中，从而使两种吸附剂的作用均发挥到最大，吸附周期优选2.7min。该级配方案兼顾了吸附周期、吸附剂对吸附质的吸附 量，发挥了每种吸附剂针对不同吸附质的特性，可以实现最优的级配工艺与操作周期，同时，实现了吸附塔体积最小。
综上所述，本发明创造性地根据所述的吸附剂的选择方法，选择用于吸附一个或多个目标吸附质的目标吸附剂，然后采用所述目标吸附剂对所述一个或多个目标吸附质进行特定温度下的变压吸附，由此，可通过减少吸附剂的用量与优化变压吸附周期来降低变压吸附运行与生产成本。
本发明一实施例还提供一种吸附剂的选择系统，所述选择系统包括：存储器，用于存储多个吸附剂中的每个吸附剂对目标吸附质的吸附等温线；以及处理器，被配置为执行以下操作：获取所述每个吸附剂对所述目标吸附质的吸附等温线在初始压力处的斜率，其中，所述吸附等温线为在特定温度下吸附量随压力变化的曲线；获取在所述特定温度与特定压力下的所述每个吸附剂对所述目标吸附质的吸附量；以及根据所述每个吸附剂的斜率与吸附量，从所述多个吸附剂中选择用于吸附所述目标吸附质的目标吸附剂。
有关本发明提供的吸附剂的选择系统的具体细节及益处可参阅上述针对吸附剂的选择方法的描述，于此不再赘述。
本发明一实施例还提供一种变压吸附系统，所述变压吸附系统包括：根据所述的吸附剂的选择系统，用于选择用于吸附一个或多个目标吸附质的目标吸附剂；以及吸附装置，用于采用所述目标吸附剂对所述一个或多个目标吸附质进行特定温度下的变压吸附。
有关本发明提供的变压吸附系统的具体细节及益处可参阅上述针对变压吸附方法的描述，于此不再赘述。
本发明一实施例还提供一种计算机可读存储介质，所述计算机可读存储介质上存储有计算机程序，该计算机程序被处理器执行时实现上述的吸附剂的选择方法和/或上述的变压吸附方法。
以上结合附图详细描述了本发明实施例的可选实施方式，但是，本发明实施例并不限于上述实施方式中的具体细节，在本发明实施例的技术构思范围内，可以对本发明实施例的技术方案进行多种简单变型，这些简单变型均属于本发明实施例的保护范围。
另外需要说明的是，在上述具体实施方式中所描述的各个具体技术特征，在不矛盾的情况下，可以通过任何合适的方式进行组合。为了避免不必要的重复，本发明实施例对各种可能的组合方式不再另行说明。
本领域技术人员可以理解实现上述实施例方法中的全部或部分步骤是可以通过程序来指令相关的硬件来完成，该程序存储在一个存储介质中，包括若干指令用以使得单片机、芯片或处理器(processor)执行本申请各个实施例所述方法的全部或部分步骤。而前述的存储介质包括：U盘、移动硬盘、只读存储器(ROM，Read-Only Memory)、随机存取存储器(RAM，Random Access Memory)、磁碟或者光盘等各种可以存储程序 代码的介质。
此外，本发明实施例的各种不同的实施方式之间也可以进行任意组合，只要其不违背本发明实施例的思想，其同样应当视为本发明实施例所公开的内容。

Claims (19)

  1. 一种吸附剂的选择方法，其特征在于，所述选择方法包括：
    获取多个吸附剂中的每个吸附剂对目标吸附质的吸附等温线在初始压力处的斜率，其中，所述吸附等温线为在特定温度下吸附量随压力变化的曲线；
    获取在所述特定温度与特定压力下的所述每个吸附剂对所述目标吸附质的吸附量；以及
    根据所述每个吸附剂的斜率与吸附量，从所述多个吸附剂中选择用于吸附所述目标吸附质的目标吸附剂。
  2. 根据权利要求1所述的选择方法，其特征在于，所述从所述多个吸附剂中选择用于吸附所述目标吸附质的目标吸附剂包括：
    根据所述每个吸附剂的斜率，确定在所述每个吸附剂的变压吸附的循环周期中的每个分解步序的最短时间；
    根据所确定的最短时间，从所述多个吸附剂中选择特定吸附剂，其中，所述特定吸附剂所对应的最短时间小于或等于预设时间；
    确定所述特定吸附剂的斜率与吸附量的乘积；以及
    将与最大乘积相对应的吸附剂选择为所述目标吸附剂。
  3. 根据权利要求2所述的选择方法，其特征在于，所述确定在所述每个吸附剂的变压吸附的循环周期中的每个分解步序的最短时间包括：
    在一吸附剂的斜率大于第一斜率且小于或等于第二斜率的情况下，与该吸附剂所对应的最短时间大于或等于第一最短时间；
    在一吸附剂的斜率大于所述第二斜率且小于或等于第三斜率的情况下，与该吸附剂所对应的最短时间大于或等于第二最短时间；
    在一吸附剂的斜率大于所述第三斜率且小于或等于第四斜率的情况下，与该吸附剂所对应的最短时间大于或等于第三最短时间；或者
    在一吸附剂的斜率大于所述第四斜率且小于或等于第五斜率的情况下，与该吸附剂所对应的最短时间大于或等于第四最短时间，
    其中，所述第一斜率、所述第二斜率、所述第三斜率、所述第四斜率以及所述第五斜率逐渐增大；以及所述第一最短时间、所述第二最短时间、所述第三最短时间以及所 述第四最短时间逐渐增大。
  4. 根据权利要求3所述的选择方法，其特征在于，在所述第一斜率为1、所述第二斜率为10、所述第三斜率为20、所述第四斜率为30且所述第五斜率为50的情况下，所述第一最短时间为0.05s、所述第二最短时间为3s、所述第三最短时间为9s且所述第四最短时间为24s。
  5. 根据权利要求2所述的选择方法，其特征在于，所述确定在所述每个吸附剂的变压吸附的循环周期中的每个分解步序的最短时间t包括：
    Figure PCTCN2022136912-appb-100001
    其中，T为预设最长步序时间，单位为s；以及k 0为所述每个吸附剂的斜率。
  6. 根据权利要求5所述的选择方法，其特征在于，T小于或等于40。
  7. 根据权利要求2-6中任一项所述的选择方法，其特征在于，所述变压吸附方法还包括：
    将所述目标吸附剂所对应的最短时间确定为吸附时间；以及
    根据在所述吸附时间内引入吸附塔的所述目标吸附质的量以及所述目标吸附剂的吸附量，确定所述目标吸附剂的量。
  8. 根据权利要求1-6中任一项所述的选择方法，其特征在于，所述获取多个吸附剂中的每个吸附剂对目标吸附质的吸附等温线在初始压力处的斜率的步骤在满足预设前提条件下被执行，
    其中，所述预设前提条件包括：在各个压力处，所述每个吸附剂对所述目标吸附质的吸附等温线与解吸等温线的吸附量之差的绝对值小于或等于吸附等温线的吸附量的预设比例。
  9. 根据权利要求8所述的选择方法，其特征在于，所述预设前提条件还包括：在各个压力处，所述每个吸附剂对所述目标吸附质的吸附等温线的吸附量小于或等于解吸等温线的吸附量，
    其中，所述解吸等温线为在所述特定温度下解吸量随压力变化的曲线。
  10. 根据权利要求1-6中任一项所述的选择方法，其特征在于，所述特定温度为10℃～40℃。
  11. 根据权利要求1-6中任一项所述的选择方法，其特征在于，所述初始压力小于或等于10kPa。
  12. 根据权利要求1-6中任一项所述的选择方法，其特征在于，所述吸附剂选自：微孔分子筛；MOFs；碳分子筛；；硅胶。
  13. 一种变压吸附方法，其特征在于，所述变压吸附方法包括：
    根据权利要求1-12中任一项所述的吸附剂的选择方法，选择用于吸附一个或多个目标吸附质的目标吸附剂；以及
    采用所述目标吸附剂对所述一个或多个目标吸附质进行特定温度下的变压吸附。
  14. 根据权利要求13所述的变压吸附方法，其特征在于，所述变压吸附方法还包括：
    在所述目标吸附剂的吸附等温线在初始压力点处的斜率大于第一预设斜率且小于或等于第二预设斜率的情况下，采用集成旋转阀控制变压吸附的工艺时序；或者
    在所述目标吸附剂的吸附等温线在初始压力点处的斜率大于所述第二预设斜率且小于或等于第三预设斜率时，采用程控阀控制变压吸附的工艺时序。
  15. 根据权利要求13或14所述的变压吸附方法，其特征在于，在所述目标吸附剂为多个目标吸附剂的情况下，所述变压吸附方法还包括：对所述多个目标吸附剂进行级配，
    所述采用所述目标吸附剂对所述一个或多个目标吸附质进行特定温度下的变压吸附包括：采用级配后的所述多个目标吸附剂对所述一个或多个目标吸附质进行所述特定温度下的变压吸附。
  16. 根据权利要求15所述的变压吸附方法，其特征在于，所述变压吸附方法还包 括：
    根据所述多个目标吸附剂中的具有吸附等温线在初始压力处的最大斜率的吸附剂的斜率，设置变压吸附的循环周期中的每个分解步序的最短时间。
  17. 一种吸附剂的选择系统，其特征在于，所述选择系统包括：
    存储器，用于存储多个吸附剂中的每个吸附剂对目标吸附质的吸附等温线；以及
    处理器，被配置为执行以下操作：
    获取所述每个吸附剂对所述目标吸附质的吸附等温线在初始压力处的斜率，其中，所述吸附等温线为在特定温度下吸附量随压力变化的曲线；
    获取在所述特定温度与特定压力下的所述每个吸附剂对所述目标吸附质的吸附量；以及
    根据所述每个吸附剂的斜率与吸附量，从所述多个吸附剂中选择用于吸附所述目标吸附质的目标吸附剂。
  18. 一种变压吸附系统，其特征在于，所述变压吸附系统包括：
    根据权利要求17所述的吸附剂的选择系统，用于选择用于吸附一个或多个目标吸附质的目标吸附剂；以及
    吸附装置，用于采用所述目标吸附剂对所述一个或多个目标吸附质进行特定温度下的变压吸附。
  19. 一种计算机可读存储介质，其特征在于，所述计算机可读存储介质上存储有计算机程序，该计算机程序被处理器执行时实现上述权利要求1-12中任一项所述的吸附剂的选择方法和/或上述权利要求13-16中任一项所述的变压吸附方法。
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