CN114950071A - Pressure swing adsorption device and process for efficiently recovering adsorbed components - Google Patents

Pressure swing adsorption device and process for efficiently recovering adsorbed components Download PDF

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CN114950071A
CN114950071A CN202210677655.7A CN202210677655A CN114950071A CN 114950071 A CN114950071 A CN 114950071A CN 202210677655 A CN202210677655 A CN 202210677655A CN 114950071 A CN114950071 A CN 114950071A
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adsorption
gas
pressure
tower
pressure swing
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刘大欢
王颢
穆龙飞
许信龙
邓海锋
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Beijing Fufeng Purification Technology Co ltd
Beijing University of Chemical Technology
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Beijing Fufeng Purification Technology Co ltd
Beijing University of Chemical Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/02Separation 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
    • B01D53/04Separation 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
    • B01D53/047Pressure swing adsorption
    • YGENERAL 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
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    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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    • Y02P20/151Reduction of greenhouse gas [GHG] emissions, e.g. CO2

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  • Separation Of Gases By Adsorption (AREA)

Abstract

The invention discloses a pressure swing adsorption device and a process for efficiently recovering adsorbed components, wherein the adsorbed components are purified by the pressure swing adsorption device to be used as product gas; the pressure swing adsorption device comprises at least four adsorption towers and a plurality of control valves for controlling gas flow; each adsorption tower is filled with an adsorbent with better adsorption effect on the preferential adsorption component; gas passes through adsorption towers, each adsorption tower is subjected to the steps of adsorption, emptying, uniform pressure drop, forward purging, evacuation, pre-adsorption, uniform pressure rise, final filling and the like, pre-adsorption tail gas components separated in the pre-adsorption process are conveyed into raw gas for cyclic separation, and adsorption components separated in the evacuation process are output as final product gas; the sequential steps of the multi-tower process are set by controlling the opening and closing of the valve, different process flows are designed, and the continuous separation of the gas is realized by the alternate use of the multiple towers. The method can improve the purity and the yield of the preferential adsorption component, reduce the investment and the operation cost, and has simple process and strong universality.

Description

Pressure swing adsorption device and process for efficiently recovering adsorbed components
Technical Field
The invention relates to a pressure swing adsorption device and a pressure swing adsorption process for efficiently recovering adsorbed components, and belongs to the technical field of gas separation.
Background
The pressure swing adsorption technology is that by utilizing the difference of adsorption performance of a solid adsorbent to different adsorbed components, part of gas mainly comprising the preferential adsorption component of the adsorbent is adsorbed by adsorption under certain pressure, and the unadsorbed components flow out through an adsorption tower; the adsorbed components are desorbed through the steps of pressure reduction, vacuum pumping and the like, and the adsorbent is regenerated, thereby realizing the separation or purification of the gas.
The product of pressure swing adsorption separation can be composed of main products of components which are difficult to be adsorbed by an adsorbent, and the product is extracted from gas flowing out of an adsorption tower through an adsorption step; or the adsorbent can be used for preferentially adsorbing components to form a main product, and the product is extracted by vacuumizing the adsorption tower in the desorption step.
The pressure swing adsorption separation device and the process which take product gas as the preferential adsorption component of the adsorbent have wide application. The main applications at present are: separating and recovering carbon monoxide from the coal gasification gas after the carbon dioxide is removed; separating and recovering carbon monoxide from calcium carbide tail gas, converter gas in a steel mill and other gases rich in carbon monoxide; separating and recovering carbon dioxide from the shift gas; separating and recovering methane from low-concentration coal bed gas, methane and the like; separating and recovering mixed gas mainly containing C2 and C2 hydrocarbon components from catalytic cracking dry gas in oil refinery.
A pressure swing adsorption separation device and a pressure swing adsorption separation process for preferentially adsorbing components by using an adsorbent are generally designed with a forward purging operation step, wherein part of product gas is pressurized by a compressor and then enters an adsorption tower through a feed gas inlet, and the unadsorbed gas in the gaps of a bed layer in the adsorption tower and the impurity gas adsorbed in the adsorbent are purged in a forward direction by using the product gas with higher content of the components of the product gas, so that the purity of the easily adsorbed components in the adsorption tower is improved. The recovery treatment of the purge effluent gas will increase the product gas recovery rate due to the higher concentration of the preferentially adsorbed component in the purge effluent gas.
The pressure swing adsorption separation device and process for preferentially adsorbing components by using adsorbent also generally design a venting operation step, and realize the recycling of the components which are not adsorbed in the adsorption tower by sequentially discharging the gas which is under high pressure and not adsorbed in the adsorption tower after the adsorption step is finished and re-feeding the gas back to the raw material gas, thereby improving the recovery rate of the device.
However, before the product gas of the strongly adsorbed component is extracted, the non-adsorption of the adsorption bed layer needs to be subjected to forward purging by using the product gas so as to improve the product yield. As shown in patents CN102343196A and CN104740972A, the prior art uses positive pressure for forward purge, which requires a large amount of forward purge gas and has a slow gas flow rate under positive pressure, resulting in an unclean forward purge. The pressure swing adsorption process of US5,354,356 mentions that for weakly adsorbed components as product, there is a negative pressure purge at the end of regeneration, with the purge gas being discharged directly. Aiming at the problems, the invention provides a negative pressure forward purging process for strongly adsorbed components, which can reduce the forward purging gas amount and improve the product yield and the product purity.
Disclosure of Invention
The technical scheme provided by the invention is as follows:
a pressure swing adsorption device and process for high-efficiently recovering adsorbed components, wherein the pressure swing adsorption device comprises at least four adsorption towers; the gas passes through the adsorption towers at a certain pressure, each adsorption tower sequentially undergoes a plurality of steps of adsorption, emptying, pressure equalizing, forward purging, evacuation, pre-adsorption, pressure equalizing, final filling and the like, the purged effluent gas separated in the forward purging process is conveyed to an inlet of the adsorption tower to be used as a pre-adsorption raw material for cyclic separation, part of product gas (5-50% of the product gas) obtained in the evacuation step is used for forward purging, the optimized operation range is 10-30%, and the rest part of the product gas is output to be used as the final product gas.
Further, a pressure swing adsorption device and a process for efficiently recovering adsorbed components, wherein a product gas of the components preferentially adsorbed by an adsorbent is obtained by the pressure swing adsorption device, and the pressure swing adsorption device comprises at least four adsorption towers and a plurality of control valves for controlling the circulation disconnection of air flow; the raw material gas passes through adsorption towers at a certain pressure at normal temperature, and each adsorption tower is filled with a certain amount of adsorbent; each adsorption tower sequentially goes through the basic steps of adsorption, emptying, pressure equalizing and reducing, forward purging, evacuating, pre-adsorption, pressure equalizing and increasing, final charging and the like. In the basic steps, different process flows can be designed by selecting the time of the steps; the sequential steps of the four-tower or multi-tower process steps are set through the switch of the control valve, and the purity and the yield of the preferential adsorption component of the adsorbent are improved through the alternative use of the four-tower or multi-tower.
The specific process of the pressure swing adsorption cycle of the present invention is controlled as follows:
1. adsorption (a): mixing the pre-adsorption tail gas, the emptying tail gas and the raw material gas, and feeding the mixture into an adsorption tower through a raw material gas inlet of the adsorption tower. Under the adsorption pressure and temperature, preferentially adsorbing components in the feed gas are adsorbed by the adsorbent in the adsorption tower, and unadsorbed components are discharged from the outlet of the adsorption tower as impurity gas, so that the separation of easily adsorbed components and difficultly adsorbed components is realized;
2. emptying (D): after the adsorption step is finished, discharging the unadsorbed gas at high pressure in the adsorption tower in a sequential manner, and sending the unadsorbed gas back to the raw material gas again, so that the recycling of unadsorbed components in the tower is realized, and the recovery rate of the device is improved;
3. mean pressure drop (ED): and connecting the adsorption tower after emptying with a pressure equalizing buffer tank or the adsorption tower in the pressure equalizing step, reducing the pressure in the adsorption tower, and recovering the components of the product preferentially adsorbed in the bed space of the adsorption tower. The pressure equalizing step can be designed into multiple stages, and is represented as pressure equalizing 1(E1D), pressure equalizing 2 (E2D);
4. forward purge (RP): part of product gas (5-50%) obtained in the evacuation step is used for forward purging, enters the adsorption tower through a feed gas inlet, optimizes the operation range by 10-30%, purges unadsorbed gas in the gaps of the bed layer in the adsorption tower and impurity gas adsorbed in the adsorbent, and improves the purity of the easily adsorbed components in the adsorption tower; in the invention, the purge gas is purged by adopting normal pressure or negative pressure gas, so that the adsorption balance operation interval is moved forward, and the concentration of the product gas is improved;
5. evacuation (V): after the forward purging step, vacuumizing the adsorption tower by a vacuum pump to reduce the pressure in the tower, gradually desorbing the adsorbent phase component in the adsorbent, and storing part of product gas (5-50%) obtained in the vacuumizing step in a purge gas buffer tank for use in the forward purging stage; the rest gas obtained by pumping out is directly used as product gas to be output;
6. pre-adsorption (BA): the purging effluent gas discharged from the adsorption tower in the forward purging step enters the adsorption tower after evacuation from the gas inlet section, the preferential adsorption component in the tail gas is adsorbed by the adsorbent in the tower, the pre-adsorbed tail gas mixed with the adsorption component and the non-adsorption component is discharged from the upper layer of the adsorption tower, and the pre-adsorbed tail gas is pressurized by the booster pump and mixed with the feed gas;
7. mean pressure rise (ER): and connecting the adsorption tower after the pre-adsorption step is finished with a pressure equalizing buffer tank or the adsorption tower in the pressure equalizing step, so that the pressure in the tower is gradually increased, and recovering the preferentially adsorbed product components in part of the pressure equalizing operation gas. The pressure equalizing step can be designed into a plurality of sections, such as pressure equalizing lift 2(E2R), pressure equalizing lift 1 (E1R);
8. final charge (FR): raw gas is used for feeding gas from an inlet end to pressurize the adsorption tower, so that the pressure in the adsorption tower gradually reaches the adsorption working pressure.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a pressure swing adsorption device and a process for improving preferential adsorption components of an adsorbent, wherein a product which is mainly composed of the preferential adsorption components of the adsorbent is obtained through the pressure swing adsorption device, the purity and the yield of the product gas are improved, the investment and the operating cost are reduced, and the process is simple and strong in universality. Specifically, the invention has the advantages that:
1. in the forward purging step, the product gas obtained by evacuation is purged from the inlet of the adsorption tower under the condition of normal pressure or negative pressure, so that the compressor required for boosting the pressure of the purge gas can be reduced, the use amount of the purge gas is reduced, and the energy consumption is saved; meanwhile, the adsorption balance operation range can be moved forward by forward purging under normal pressure or negative pressure, so that the concentration of the product gas is improved.
2. And blowing effluent gas flow generated in the forward blowing step enters the adsorption tower after evacuation is finished for pre-adsorption, so that the preferential adsorption component in the tail gas is adsorbed by the adsorbent in the tower and the adsorbed component is difficult to enter the upper layer of the adsorption tower, and the pre-adsorbed tail gas generated in the pre-adsorption step is pressurized by a booster pump for 5-30KPa and then is returned to the feed gas again, so that the product gas yield is improved.
3. And in the emptying step, the high-pressure unadsorbed gas in the adsorption tower is discharged in a forward discharge manner, and the unadsorbed gas is fed back to the raw material gas again, so that the unadsorbed components in the tower are recycled, and the recovery rate of the device is improved.
Drawings
FIG. 1 is a flow diagram of a pressure swing adsorption process for increasing preferential adsorption of components by an adsorbent
FIG. 2 is a block diagram of a pressure swing adsorption process for increasing preferential adsorption of components by an adsorbent
Detailed description of the preferred embodiment
The invention is further described below with reference to examples, but without limiting the scope of the invention in any way.
The invention provides a pressure swing adsorption device and a process for efficiently recovering adsorbed components, wherein a product gas of a component preferentially adsorbed by an adsorbent is obtained by the pressure swing adsorption device, and the pressure swing adsorption device comprises at least four adsorption towers and a plurality of control valves for controlling the circulation disconnection of gas flow; the raw material gas passes through adsorption towers at a certain pressure at normal temperature, and each adsorption tower is filled with a certain amount of adsorbent; each adsorption tower sequentially goes through the basic steps of adsorption, emptying, pressure equalizing and reducing, forward purging, evacuating, pre-adsorption, pressure equalizing and increasing, final charging and the like. In the basic steps, different process flows can be designed by selecting the time of the steps; the sequential steps of four or more towers are set by controlling the switch of the valve, and the purity and the yield of the preferential adsorption component of the adsorbent are improved by alternately using the four or more towers.
Example one of the embodiments used a pressure swing adsorption unit that was a system consisting of four adsorption columns, with a cycle timing sequence as shown in table 1.
TABLE 1 cycle timing for four column PSA process for efficient recovery of adsorbed components
Figure BDA0003695384860000031
As shown in table 1, during each period of the pressure swing adsorption process, the columns are in different operating states, e.g., during the period shown in the bold box in table 1, the operating states of the columns are:
the tower A is in the adsorption step, raw material gas enters the tower from the bottom of the tower for adsorption, product gas is adsorbed in a bed layer by an adsorbent, and impurity gas is discharged from the top of the tower as adsorption tail gas; the tower B is in a pressure equalizing and rising step and is connected with the tower D for equalizing pressure, so that the pressure in the tower is gradually raised, and the preferentially adsorbed product component in part of the pressure equalizing and falling operation gas of the tower D is recovered; c, the tower is in the step of evacuating, the vacuum pump is used for evacuating the adsorption tower, so that the pressure in the tower is reduced, the adsorbent phase components in the adsorbent are gradually desorbed, part (5-50%) of the product gas obtained in the step of evacuating is stored in a purge gas buffer tank for use in a forward purge stage, and the rest gas obtained in the step of evacuating is directly output as the product gas; the tower D is in an equal pressure drop stage and is connected with the tower B to gradually reduce the pressure in the tower.
In one embodiment, the forward purge gas pressure is 0.1MPa (absolute), and the composition of the gas treated with the above process flow and process parameters is: 80.2 percent of nitrogen and 19.8 percent of methane, the concentration of the obtained product gas methane reaches more than 90 percent, and the yield reaches more than 85 percent.
Example two the pressure swing adsorption unit used was a system consisting of eight adsorption columns, and the timing sequence of one cycle of the system is shown in table 2.
TABLE 2 cycle sequence for eight column PSA process for efficient recovery of adsorbed components
Figure BDA0003695384860000041
As shown in table 2, during each period of the pressure swing adsorption process, the columns are in different operating states, e.g., during the period shown in the bold box in table 2, the operating states of the columns are:
the tower A and the tower H are in an adsorption step, raw material gas enters the tower from the bottom of the tower for adsorption, product gas is adsorbed in a bed layer by an adsorbent, and impurity gas is discharged from the top of the tower as adsorption tail gas; the first half section of the tower B is in a pressure equalizing and rising step and is connected with the tower G for equalizing pressure, so that the pressure in the tower B is gradually raised, and the preferential adsorption product component in the pressure equalizing and falling operation gas of part of the tower G is recovered, and the second half section is in a final filling step, wherein the raw gas is fed from the product end to pressurize the adsorption tower, so that the interior of the adsorption tower gradually reaches the adsorption working pressure; the first half section of the tower C is in a pre-adsorption step, purge effluent gas discharged from the adsorption tower in the tower E forward purge step enters the tower C from the gas inlet end, so that preferential adsorption components in tail gas are adsorbed by an adsorbent in the tower, the pre-adsorbed tail gas is pressurized by a booster pump and mixed with feed gas, and the second half section of the tower C is in a pressure equalizing step and is connected with the tower G for equalizing pressure; the front half section of the tower D is in the step of evacuation, the adsorption tower is subjected to vacuum-pumping desorption through a vacuum pump, a part of the obtained product gas is stored in a purge gas buffer tank for use in a forward purge stage, the rest gas is directly produced as the product gas, the rear half section of the tower D is in the pre-adsorption step, and purge effluent gas discharged from the adsorption tower in the forward purge step of the tower F enters the tower D from the gas inlet end; the front half section of the tower E is in a forward purging step, the gas which is not adsorbed in the gaps of the inner bed layers of the adsorption tower is purged in a forward direction through the product gas in the product gas buffer tank, the purged effluent gas is used for pre-adsorption of the tower C, the rear half section of the tower E is in an evacuating step, the adsorption tower is subjected to vacuum-pumping desorption through a vacuum pump, a part of the obtained product gas is stored in the purge gas buffer tank for use in the forward purging step, and the rest gas is directly output as the product gas; the first half section of the tower F is in an emptying step, gas which is at high pressure and is not adsorbed in the adsorption tower is discharged in a forward discharging manner and is sent back to the raw material gas, the second half section of the tower F is in a forward purging step, and the purged effluent gas is used for pre-adsorption of the tower D; and the tower G is in an equal pressure drop step and is respectively connected with the tower B and the tower C so as to gradually reduce the pressure in the towers.
In example two, the forward purge gas pressure was 0.09MPa (absolute), and the composition of the gas treated with the above process flow and process parameters was: 80.2 percent of nitrogen and 19.8 percent of methane, the concentration of the obtained product gas methane reaches over 96 percent, and the yield reaches 90 percent.

Claims (5)

1. A pressure swing adsorption device and process for high-efficiently recovering adsorbed components is characterized in that the pressure swing adsorption device comprises at least four adsorption towers; raw material gas enters an adsorption tower according to a certain composition and pressure; each adsorption tower is sequentially subjected to a plurality of steps of adsorption, emptying, pressure equalization, forward purging, evacuation, pre-adsorption, pressure equalization, final filling and the like to obtain the adsorbent which preferentially adsorbs component product gas.
The forward purging step comprises: purging the product gas obtained by evacuation from the inlet of the adsorption tower under the normal pressure or negative pressure condition, simultaneously, enabling all or part of the purge effluent gas flowing out in the forward purging step to flow into the evacuated adsorption tower for pre-adsorption, pumping the tail gas at the top of the pre-adsorption tower by a circulating booster pump, boosting the tail gas by the booster pump for 5-30KPa, and returning the tail gas to be mixed with the raw material gas for adsorption;
all or part of the vented tail gas flowing out in the sequential release step returns to be mixed with the raw gas to be used as the raw gas in the pressure swing adsorption separation process;
the pre-adsorption step is generally arranged before the pressure equalization rising step, so that more purging effluent gas can be absorbed for the pre-adsorption step, the pressure of the adsorption beds in the forward purging step and the pre-adsorption step can be reduced, the consumption of forward purging gas can be reduced, and when multiple pressure equalization rising steps exist in the process, 1-2 pressure equalization rising steps can be arranged before the pre-adsorption step.
2. The method of claim 1, wherein the pressure swing adsorption unit comprises a plurality of control valves for controlling the gas flow, the timing steps of the multi-column pressure swing adsorption process are set by switching the control valves, and the continuous operation of the pressure swing adsorption process and the improvement of the product gas purity and yield are achieved by the multi-column alternate operation.
3. The method according to claim 1 or 2, wherein the operating pressure of the adsorption column is 0.3MPa to 6MPa in absolute pressure; when the forward purging operation step is implemented, the purging gas pressure is 0.07MPa-0.1MPa of absolute pressure; the lowest operation pressure of the adsorption tower when the evacuation operation is carried out is 0.002MPa-0.05MPa of absolute pressure.
4. A process according to claims 1-3, characterized in that the molar fraction of the preferentially adsorbed component of the adsorbent in the feed gas is between 3% and 98%.
5. The method of claim 1, wherein the solid adsorbent filled in the adsorption tower is at least one or more selected from activated carbon, molecular sieve, silica gel, metal organic framework material, etc., and the separation coefficient of the adsorbent to the separated system is more than 10.
CN202210677655.7A 2022-06-15 2022-06-15 Pressure swing adsorption device and process for efficiently recovering adsorbed components Pending CN114950071A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4915711A (en) * 1989-05-18 1990-04-10 Air Products And Chemicals, Inc. Adsorptive process for producing two gas streams from a gas mixture
CN1235863A (en) * 1999-05-18 1999-11-24 天津大学 High efficiency flexible variable-pressure adsorption technology
CN104740972A (en) * 2015-03-09 2015-07-01 四川天一科技股份有限公司 Pressure swing adsorption gas separation method for recycling displacement waste gas and directly-discharged gas
CN106693608A (en) * 2016-12-13 2017-05-24 中国石油化工股份有限公司 Refinery dry gas separating and recycling process
CN109012030A (en) * 2018-04-19 2018-12-18 郑州富龙新材料科技有限公司 It is a kind of based on product gas methane displacement coal bed gas deoxidation denitrogenate method for concentration and device

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4915711A (en) * 1989-05-18 1990-04-10 Air Products And Chemicals, Inc. Adsorptive process for producing two gas streams from a gas mixture
CN1235863A (en) * 1999-05-18 1999-11-24 天津大学 High efficiency flexible variable-pressure adsorption technology
CN104740972A (en) * 2015-03-09 2015-07-01 四川天一科技股份有限公司 Pressure swing adsorption gas separation method for recycling displacement waste gas and directly-discharged gas
CN106693608A (en) * 2016-12-13 2017-05-24 中国石油化工股份有限公司 Refinery dry gas separating and recycling process
CN109012030A (en) * 2018-04-19 2018-12-18 郑州富龙新材料科技有限公司 It is a kind of based on product gas methane displacement coal bed gas deoxidation denitrogenate method for concentration and device

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