CN109173583B - Medium-temperature vacuum pressure swing adsorption system and method - Google Patents
Medium-temperature vacuum pressure swing adsorption system and method Download PDFInfo
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- CN109173583B CN109173583B CN201811160591.3A CN201811160591A CN109173583B CN 109173583 B CN109173583 B CN 109173583B CN 201811160591 A CN201811160591 A CN 201811160591A CN 109173583 B CN109173583 B CN 109173583B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/047—Pressure swing adsorption
- B01D53/0476—Vacuum pressure swing adsorption
Abstract
The invention discloses a medium-temperature vacuum pressure swing adsorption system and a medium-temperature vacuum pressure swing adsorption method. The system comprises an adsorption tower, a product gas tank, a forward flushing gas tank, a reverse discharging gas tank and the like. The system is provided with a plurality of adsorption towers or pressure equalizing tanks. The method comprises the working procedures of adsorption, constant-pressure forward flushing, reverse releasing, flushing, vacuum desorption and the like. In the operation of multiple towers or tower tanks, the adsorption tower after the constant-pressure sequential flushing process enters a pressure equalizing and reducing process, and the other adsorption tower or pressure equalizing tank connected with the adsorption tower enters a pressure equalizing and increasing process. The adsorption tower after pressure reduction enters flushing and/or vacuum desorption, so that the adsorbent is regenerated and then enters pressure equalizing and boosting, and the other adsorption tower or pressure equalizing tank connected with the adsorption tower enters pressure equalizing and pressure reducing. The constant pressure forward impact comprises high pressure forward impact and low pressure forward impact. The invention adds the steps of high pressure forward flushing, low pressure forward flushing and other constant pressure forward flushing steps, so that the effective gas in the adsorption tower can still enter the product gas tank after the adsorption is finished, the recovery rate of the pressure swing adsorption gas is obviously improved, and the purity of the product gas can still meet the requirement.
Description
Technical Field
The invention relates to a medium-temperature vacuum pressure swing adsorption system and a medium-temperature vacuum pressure swing adsorption method, and belongs to the technical field of gas purification.
Background
In the fields of chemical industry, power generation and the like, various mixed gases need to be separated and purified, for example, CO in synthesis gas needs to be separated and purified in an ammonia synthesis process2、H2S and the like are removed to prepare pure hydrogen for reaction and synthesis with nitrogen. The traditional mixed gas purification mode is low-temperature methanol washing, the method firstly needs to cool the gas, the cooled gas enters an absorption tower, and CO in the cooled gas enters an absorption tower2、H2S is absorbed by low-temperature liquid methanol, and the rest gas is cooled and returnedAnd (4) after the mixture is collected and heated again, the subsequent processes are continued. The cooling and reheating processes of the gas result in wasted energy and require complex heat exchange and refrigeration equipment.
The pressure swing adsorption purification method is an effective method which can separate and recycle various gases to obtain high-purity gas with specific components. The traditional pressure swing adsorption process is mainly used for air separation and gas purification and recovery, the working temperature is normal temperature, the purity and the yield of product gas are difficult to reach higher levels at the same time, and technical indexes need to be improved through process improvement and adsorbent performance improvement. CN102351147A discloses a method for CO2、H2S and H2Medium temperature pressure swing adsorption method for mixed gas separation, used for directly removing CO at medium temperature2、H2S and other acidic gases, thereby avoiding energy loss caused by temperature reduction in the medium-temperature gas purification process and improving the energy utilization efficiency. But in this process H2Low recovery rate of CO2The removal accuracy of the catalyst needs to be improved.
Disclosure of Invention
The invention aims to provide a medium-temperature vacuum pressure swing adsorption system and a medium-temperature vacuum pressure swing adsorption method.
The invention is realized by the following technical scheme:
a medium temperature vacuum pressure swing adsorption system comprises an adsorption tower, a product gas tank, a forward flushing gas tank, a flushing gas tank and a reverse discharging gas tank; a raw material gas inlet, a reverse-bleeding gas outlet and a forward flushing gas inlet are arranged below the adsorption towers, and a product gas port, a pressure equalizing port and a flushing gas inlet are arranged above each adsorption tower; the adsorption tower is filled with an adsorbent; the product gas tank is connected with a product gas port of the adsorption tower through a connecting pipeline, and the forward flushing gas tank and the reverse discharging gas tank are respectively connected with a forward flushing gas inlet and a reverse discharging gas outlet of the adsorption tower; the flushing gas tank is connected with a flushing gas inlet of the adsorption tower through a connecting pipeline.
In the technical scheme, the forward flushing gas tank comprises a high-pressure forward flushing gas tank and a low-pressure forward flushing gas tank; the product gas tanks include high pressure product gas tanks and low pressure product gas tanks.
In the technical scheme, the system is provided with a plurality of adsorption towers at least comprising an adsorption tower A and an adsorption tower B, and the adsorption towers are connected through pressure equalizing ports.
Or the system also comprises a pressure equalizing tank, and the pressure equalizing tank is connected with a pressure equalizing port of the adsorption tower.
A medium-temperature vacuum pressure swing adsorption method comprises the working procedures of adsorption, constant-pressure forward flushing, reverse releasing, flushing and/or vacuum desorption and the like, and comprises the following steps:
opening a product gas port of the adsorption tower to communicate the adsorption tower with a product gas tank, and reversely boosting the pressure to the adsorption set pressure to enable the adsorption tower to enter an adsorption process;
adsorption: communicating a product gas port of the adsorption tower with a product gas tank, and enabling a feed gas inlet of the adsorption tower to be in an open state; the raw gas enters the adsorption tower from a raw gas inlet of the adsorption tower, the gas which is easy to adsorb is separated in the adsorption tower through selective adsorption of an adsorbent, and the gas which is difficult to adsorb enters a product gas tank from a product gas port of the adsorption tower;
constant-pressure forward flushing: the raw gas inlet of the adsorption tower is in a closed state, the product gas port of the adsorption tower is in an open state, and the forward aeration inlet of the adsorption tower is opened, so that the adsorption tower is respectively communicated with the product gas tank and the forward aeration tank; allowing the flush gas to enter an adsorption tower; under the propulsion of the flushing gas, the gas which is difficult to adsorb at the top of the adsorption tower enters the product gas tank from the product gas port; the pressure in the adsorption tower is constant in the forward flushing process;
reverse amplification: opening a reverse-bleeding gas outlet of the adsorption tower to communicate with the atmosphere or a reverse-bleeding gas tank, releasing gas in the adsorption tower in the reverse direction of adsorption, and reducing the pressure of the adsorption tower in the reverse direction to be the same as the ambient pressure, so that the gas easy to adsorb enters the reverse-bleeding gas tank through the reverse-bleeding gas outlet;
after the reverse decompression of the adsorption tower is finished, flushing and/or vacuum desorption are carried out to regenerate the adsorbent in the adsorption tower and release the gas components easy to adsorb out of the adsorption tower; and
washing: in the flushing procedure, a reverse-air outlet and a flushing gas inlet of the adsorption tower are opened, so that flushing gas enters from the top of the adsorption tower and flows out from the reverse-air outlet, the adsorbent is regenerated, and gas components easy to adsorb flow out of the adsorption tower along with flushing gas; and/or
Vacuum desorption: opening a reverse-release gas outlet of the adsorption tower, communicating the reverse-release gas outlet with an inlet of a vacuum pump, and releasing gas in the adsorption tower in the reverse direction of adsorption by vacuumizing so as to further reversely reduce the pressure of the adsorption tower and obtain gas easy to adsorb at an outlet of the vacuum pump so as to regenerate the adsorbent;
after the adsorption tower is flushed and/or vacuum desorbed, a product gas port of the adsorption tower is opened, the adsorption tower is communicated with a product gas tank, the pressure is reversely increased to the adsorption set pressure, and the adsorption tower enters an adsorption process.
The method further comprises the following steps:
the system is provided with a plurality of adsorption towers at least comprising an adsorption tower A and an adsorption tower B; or the system comprises a plurality of adsorption towers and a plurality of pressure equalizing tanks;
one of the adsorption towers is reversely boosted to the adsorption set pressure, and then sequentially enters the adsorption and constant-pressure sequential flushing processes; under the constant pressure state, the gas difficult to adsorb on the top of the adsorption tower is pushed to enter the product gas tank from the product gas port;
opening pressure equalizing openings of two adsorption towers or the adsorption tower and a pressure equalizing tank and enabling the adsorption towers or the adsorption tower and the pressure equalizing tank to be communicated with each other, enabling the adsorption tower which completes constant-pressure forward flushing to be in a pressure equalizing and reducing process to carry out forward pressure reduction, and enabling the other adsorption tower or one pressure equalizing tank to be in a pressure equalizing and increasing process to carry out reverse pressure increase;
the adsorption tower after pressure equalization and depressurization enters a flushing process and/or a vacuum desorption process to complete the regeneration of the adsorbent, and then enters a pressure equalization and pressurization process; opening and communicating pressure equalizing openings of the two adsorption towers or the adsorption tower and the pressure equalizing tank, so that the adsorption tower completing adsorbent regeneration carries out reverse pressure equalizing and boosting, and simultaneously, the other adsorption tower or the pressure equalizing tank carries out forward pressure equalizing and pressure reducing;
after the pressure equalizing and boosting of the adsorption tower reaches the preset pressure, a product gas port of the adsorption tower is opened, so that the adsorption tower is communicated with a product gas tank, and the adsorption tower enters the adsorption process again.
In the above technical solution, the constant-pressure forward flushing includes high-pressure forward flushing and low-pressure forward flushing, and the method further includes:
high-pressure forward flushing: entering a high-pressure forward flushing process after the adsorption process is finished, enabling a product air port of the adsorption tower to be in an open state, and opening a forward flushing air inlet of the adsorption tower to enable the adsorption tower to be respectively communicated with a high-pressure product tank and a high-pressure forward flushing air tank; leading high-pressure forward flushing gas to enter an adsorption tower, and obtaining the gas which is difficult to adsorb and has the purity meeting the requirement in a high-pressure product gas tank;
pressure equalizing and reducing: after the high-pressure forward flushing process is finished, entering a voltage-equalizing and pressure-reducing process; opening and communicating the pressure equalizing openings of two adsorption towers or one adsorption tower and one pressure equalizing tank, enabling one adsorption tower to be in a pressure equalizing and reducing process to carry out forward pressure reduction, and enabling the other adsorption tower or one pressure equalizing tank to be in a pressure equalizing and increasing process to carry out reverse pressure increase;
low-pressure forward flushing: the adsorption tower after pressure equalization and depressurization enters a low-pressure forward flushing process, a product gas port and a forward flushing gas inlet of the adsorption tower are opened and are respectively communicated with a low-pressure product tank and a low-pressure forward flushing gas tank; introducing low-pressure flushing gas into the adsorption tower, and obtaining the gas which is difficult to adsorb and has the purity meeting the requirement in a low-pressure product gas tank of the device;
reverse amplification: the adsorption tower which is subjected to low-pressure forward flushing enters a reverse-releasing process, a reverse-releasing outlet of the adsorption tower is opened to be communicated with the atmosphere or a reverse-releasing gas tank, gas in the adsorption tower is released in the reverse direction of adsorption, the pressure of the adsorption tower is reversely reduced to be the same as the ambient pressure, and gas which is easy to adsorb enters the reverse-releasing gas tank through the reverse-releasing outlet.
In the technical scheme, the medium-temperature vacuum pressure swing adsorption system used in the method is provided with a plurality of adsorption towers comprising an adsorption tower A and an adsorption tower B, and the adsorption towers in pressure equalizing and reducing and pressure equalizing and increasing are in one-to-one correspondence.
In the above technical solution, the gas easy to adsorb includes one or more of hydrogen sulfide, carbon dioxide, carbon monoxide, methane, water vapor, and oxygen.
In the above technical solution, the gas difficult to adsorb comprises one or more of hydrogen, nitrogen, and rare gas.
In the above technical scheme, the forward flushing gas is gas which is easy to separate from the product gas and is not easy to be adsorbed by the adsorbent, and comprises nitrogen, water vapor or argon.
The invention has the following advantages and beneficial effects: by adding the steps of high-pressure forward flushing, low-pressure forward flushing and the like, the effective gas in the adsorption tower can still enter the product gas tank after the adsorption is finished, the recovery rate of the pressure swing adsorption gas is obviously improved, and meanwhile, the purity of the product gas can still meet the requirement.
Drawings
FIG. 1 is a schematic diagram of a medium temperature vacuum pressure swing adsorption system in accordance with the present invention.
FIG. 2 is a schematic view of a pressure swing adsorption system for ammonia synthesis shift gas purification according to an embodiment of the present invention.
FIG. 3 is a methanol steam reforming H according to an embodiment of the present invention2Schematic diagram of a 4-column pressure swing adsorption system for purification.
In the figure: 1-flushing the gas tank; 2-product gas tank; 3-raw material gas tank; 4-gas tank is put inversely; 5-flushing the air tank; 6-vacuum pump; 7-adsorption column A; 8-adsorption column B; 9-solenoid valve.
Detailed Description
The following describes the embodiments and operation of the present invention with reference to the accompanying drawings.
The terms of orientation such as up, down, left, right, front, and rear in the present specification are established based on the positional relationship shown in the drawings. The corresponding positional relationship may also vary depending on the drawings, and therefore, should not be construed as limiting the scope of protection.
As shown in fig. 1, a medium temperature vacuum pressure swing adsorption system comprises an adsorption tower, a product gas tank 2, a forward flushing gas tank 5, a flushing gas tank 1 and a reverse discharging gas tank 4. The adsorption tower below all is equipped with feed gas entry, contrary gassing export and along with the flushing gas entry, and the adsorption tower top all is equipped with product gas port, voltage-sharing mouth and flushing gas entry, controls it through solenoid valve 9 and opens.
The adsorption tower is filled with an adsorbent.
The product gas tank is connected with a product gas port of the adsorption tower through a connecting pipeline. The forward flushing gas tank 5 and the reverse discharging gas tank 4 are respectively connected with a forward flushing gas inlet and a reverse discharging gas outlet of the adsorption tower. The flushing gas tank is connected with a flushing gas inlet of the adsorption tower through a connecting pipeline.
The flushing gas tank 5 comprises a high-pressure flushing gas tank and a low-pressure flushing gas tank, and the corresponding product gas tank comprises a high-pressure product gas tank and a low-pressure product gas tank.
When the system is provided with only the adsorption tower, at least two adsorption towers are arranged, and the adsorption towers comprise an adsorption tower A7 and an adsorption tower B8. The adsorption towers are connected through pressure equalizing ports.
Or the system also comprises a pressure equalizing tank, and the pressure equalizing tank is connected with a pressure equalizing port of the adsorption tower. The pressure equalizing tank preferably has the same structure as the adsorption tower, and has a volume equal to the effective volume of the adsorption tower filled with the adsorbent without the adsorbent filled therein.
A medium-temperature vacuum pressure swing adsorption method comprises the working procedures of adsorption, constant-pressure forward flushing, reverse releasing, flushing and/or vacuum desorption and the like, and comprises the following steps:
and opening a product gas port of the adsorption tower to communicate the adsorption tower with the product gas tank, and reversely boosting the pressure to the adsorption set pressure to enable the adsorption tower to enter an adsorption process. This process is also referred to as final charging.
Adsorption: communicating a product gas port of the adsorption tower with a product gas tank, and enabling a feed gas inlet of the adsorption tower to be in an open state; the raw gas enters the adsorption tower from a raw gas inlet of the adsorption tower, the gas which is easy to adsorb is separated in the adsorption tower through selective adsorption of an adsorbent, and the gas which is difficult to adsorb enters a product gas tank from a product gas port of the adsorption tower; the duration of the adsorption process can be freely regulated.
Constant-pressure forward flushing: the raw gas inlet of the adsorption tower is in a closed state, the product gas port of the adsorption tower is in an open state, and the forward aeration inlet of the adsorption tower is opened, so that the adsorption tower is respectively communicated with the product gas tank and the forward aeration tank; allowing the flush gas to enter an adsorption tower; under the propulsion of the flushing gas, the gas which is difficult to adsorb at the top of the adsorption tower enters the product gas tank from the product gas port; the pressure in the adsorption tower is constant in the process of forward flushing.
Reverse amplification: and opening the reverse-bleeding gas outlet of the adsorption tower to communicate with the atmosphere or the reverse-bleeding gas tank, releasing gas in the adsorption tower in the reverse direction of adsorption, and reducing the pressure of the adsorption tower in the reverse direction to be the same as the ambient pressure so that the gas easy to adsorb enters the reverse-bleeding gas tank through the reverse-bleeding gas outlet.
After the reverse decompression of the adsorption tower is finished, flushing and/or vacuum desorption are carried out to regenerate the adsorbent in the adsorption tower and release the gas components easy to adsorb from the adsorption tower. Subsequent flushing and/or vacuum desorption
Washing: in the flushing procedure, a reverse-air outlet and a flushing gas inlet of the adsorption tower are opened, so that flushing gas enters from the top of the adsorption tower and flows out from the reverse-air outlet, the adsorbent is regenerated, and gas components easy to adsorb flow out of the adsorption tower along with flushing gas.
True. Air desorption: the reverse vent outlet of the adsorption tower is opened and communicated with the inlet of the vacuum pump 6, and the gas in the adsorption tower is released in the reverse direction of adsorption by vacuumizing, so that the adsorption tower further reversely reduces the pressure, and the gas easy to adsorb is obtained at the outlet of the vacuum pump, and the adsorbent is regenerated.
After the adsorption tower is flushed and/or vacuum desorbed, a product gas port of the adsorption tower is opened, the adsorption tower is communicated with a product gas tank, the pressure is reversely increased to the adsorption set pressure, and the adsorption tower enters the adsorption process again.
When the system is provided with a plurality of adsorption towers including at least an adsorption tower A and an adsorption tower B, or a plurality of adsorption towers and a plurality of pressure equalizing tanks, the method further comprises the following steps:
one of the adsorption towers is reversely boosted to the adsorption set pressure, and then sequentially enters the adsorption and constant-pressure sequential flushing processes; under the constant pressure state, the gas difficult to adsorb on the top of the adsorption tower is pushed to enter the product gas tank from the product gas port;
opening pressure equalizing openings of the two adsorption towers or the adsorption tower and the pressure equalizing tank and enabling the two adsorption towers or the adsorption tower and the pressure equalizing tank to be communicated with each other, enabling the adsorption tower which finishes constant-pressure forward flushing to be in a pressure equalizing and reducing process to carry out forward pressure reduction, and enabling the other adsorption tower or the pressure equalizing tank to be in a pressure equalizing and increasing process to carry out reverse pressure increase;
the adsorption tower after pressure equalization and depressurization enters a flushing process and/or a vacuum desorption process to complete the regeneration of the adsorbent, and then enters a pressure equalization and pressurization process; opening and communicating pressure equalizing openings of the two adsorption towers or the adsorption tower and the pressure equalizing tank, so that the adsorption tower completing adsorbent regeneration carries out reverse pressure equalizing and boosting, and the other adsorption tower or the pressure equalizing tank carries out forward pressure equalizing and pressure reducing;
after the pressure equalizing and boosting of the adsorption tower reaches the preset pressure, a product gas port of the adsorption tower is opened, so that the adsorption tower is communicated with a product gas tank, and the adsorption tower enters the adsorption process again.
The constant-pressure forward punching comprises high-pressure forward punching and low-pressure forward punching, and the method further comprises the following steps:
high-pressure forward flushing: entering a high-pressure forward flushing process after the adsorption process is finished, enabling a product air port of the adsorption tower to be in an open state, and opening a forward flushing air inlet of the adsorption tower to enable the adsorption tower to be respectively communicated with a high-pressure product tank and a high-pressure forward flushing air tank; leading high-pressure forward flushing gas to enter an adsorption tower, and obtaining the gas which is difficult to adsorb and has the purity meeting the requirement in a high-pressure product gas tank;
pressure equalizing and reducing: after the high-pressure forward flushing process is finished, entering a voltage-equalizing and pressure-reducing process; opening pressure equalizing ports of an adsorption tower A7 and an adsorption tower B8 and communicating the pressure equalizing ports, enabling one adsorption tower to be in a pressure equalizing and reducing process to carry out forward pressure reduction, and enabling the other adsorption tower or a pressure equalizing tank to be in a pressure equalizing and increasing process to carry out reverse pressure increase;
low-pressure forward flushing: after the pressure equalizing and reducing process is finished, entering a low-pressure forward flushing process, so that a product gas port and a forward flushing gas inlet of the adsorption tower are opened and are respectively communicated with a low-pressure product tank and a low-pressure forward flushing gas tank; introducing low-pressure flushing gas into the adsorption tower, and obtaining the gas which is difficult to adsorb and has the purity meeting the requirement in a low-pressure product gas tank;
reverse amplification: and (3) entering a reverse releasing process after the low-pressure forward flushing is finished, opening a reverse releasing outlet of the adsorption tower to communicate with the atmosphere or a reverse releasing gas tank, releasing the gas in the adsorption tower in the reverse direction of adsorption, reversely depressurizing the adsorption tower to the same pressure as the ambient pressure, and enabling the gas easy to adsorb to enter the reverse releasing gas tank through the reverse releasing outlet.
And the adsorption tower after the pressure reduction is reversely released continues to enter the subsequent working procedures.
When the adsorption tower sets up more than two, be in the adsorption tower that the pressure-equalizing is stepped down and the pressure-equalizing is stepped up for the one-to-one, have an adsorption tower to be in the pressure-equalizing and step down promptly, have an adsorption tower to be in the pressure-equalizing simultaneously and step up.
The easy adsorption gas comprises one or more of hydrogen sulfide, carbon dioxide, carbon monoxide, methane, water vapor and oxygen.
The difficult-to-adsorb gas comprises one or more of hydrogen, nitrogen and rare gas.
The flushing gas is gas which is easy to separate from the product gas and is not easy to be adsorbed by the adsorbent, and comprises nitrogen, water vapor or argon.
Example 1: the synthetic ammonia conversion gas is subjected to medium-temperature sulfur and carbon co-removal.
The method comprises the following steps of (1) carrying out pressure swing adsorption separation on synthetic ammonia conversion gas serving as a raw material, wherein the water-gas ratio in the conversion gas is 1.2-1.4, the pressure is 3.4MPa, and the pressure of dry-base raw material gas is about 1.5MPa, and the components are shown in Table 1:
TABLE 1 shift gas composition
| Components | CO2(％) | CO(％) | H2(％) | CH4(％) | N2(％) | Total sulfur (ppm) |
| Concentration of | 28-36 | 0.3-0.5 | 51-65 | 4.0-7.8 | 2.0-4.0 | 1000 |
The pressure swing adsorption system for purifying the shift gas is shown in figure 2 and comprises 4 adsorption towers A1-A4, 4 pressure equalizing tanks T1-T4, a product gas storage tank, a reverse-release gas storage tank, a high-pressure forward-filling buffer tank, a low-pressure forward-filling buffer tank and a vacuum pump V. The pressure equalizing tank and the adsorption tower are connected in parallel. The design and arrangement of the pressure swing adsorption tower use the method, and the inside of the pressure swing adsorption tower is filled with the molecular sieve and the activated carbon. The pressure equalizing tank is not filled, and a pressure equalizing opening is only arranged at the top, and the volume of the pressure equalizing tank is similar to that of the adsorption tower filled with the molecular sieve. Steam is selected as the air.
In the adsorption system, the temperature of the adsorption tower, the pressure equalizing tank and the hydrogen buffer tank is 160 ℃, the temperature of the steam buffer tank is 180 ℃, and the pressure is 1.55 MPa; adsorption pressure of 1.5MPa, CO2The pressure in the storage tank was 0.15 MPa.
After the conversion gas enters the adsorption tower from the mixed gas inlet, moisture, carbon dioxide, carbon monoxide, sulfur-containing components, methane and nitrogen in the gas are removed by the adsorbent, and hydrogen which is not easy to be adsorbed enters the hydrogen buffer tank from the product gas outlet. Each adsorption tower is subjected to adsorption, high-pressure flushing, tower-tank pressure equalizing drop 1, tower-tower pressure equalizing drop 1, tower-tank pressure equalizing drop 2, tower-tank pressure equalizing drop 3, tower-tower pressure equalizing drop 2, tower-tank pressure equalizing drop 4, vacuum desorption, tower-tank pressure equalizing rise 4, tower-tower pressure equalizing rise 2, tower-tank pressure equalizing rise 3, tower-tank pressure equalizing rise 2, tower-tower pressure equalizing rise 1 and tower-tank pressure equalizing rise 1 in sequence. Pressurizing; each pressure equalizing tank only carries out pressure equalizing rise and pressure equalizing drop steps. The process flow of each adsorption column and pressure equalizing tank is shown in Table 2. The time lengths 1-24 in Table 2 are the same.
TABLE 2 shift gas purification 8-column Process
Remarking: AD: adsorption; HR: high-pressure direct punching; EdA: the pressure drop of the tower and the tank is 1; ed 1: the pressure drop of the tower is 1; e dB: 2, tower tank pressure drop; EdC: 3, the pressure of the tower and the tank is reduced uniformly; ed 2: the pressure drop of the tower is 2; EdD: 4, tower tank pressure equalizing drop; BD: reverse discharge; VD: carrying out vacuum desorption; EpD: 4, uniformly increasing the pressure of the tower tank; ep 2: the pressure of the tower is increased by 2; EpC: 3, uniformly increasing the pressure of the tower tank; EpB: the pressure of the tower is increased by 2; ep 1: the pressure of the tower is increased by 1; EpA: the pressure of the tower tank is increased by 1; PP: and (6) pressurizing.
The operation of each adsorption column in one cycle will be described in detail by taking the adsorption column a1 as an example.
(1) Adsorption
At this point the adsorption column a1 has completed the pressurization step and the column pressure reaches the adsorption pressure. Opening the program control valves 1A and 4A, allowing the change gas to enter from the lower end of the adsorption tower, removing moisture, carbon dioxide, carbon monoxide, sulfur-containing components, methane and nitrogen by the adsorbent in the upward flow process, adsorbing a small amount of hydrogen, and allowing the residual pure hydrogen to enter the product gas storage tank from the upper end of the adsorption tower. Along with the proceeding of the adsorption process, the adsorbent at the lower part of the adsorption tower is saturated, and the impurity gas in the product gas outlet is gradually increased. When the purity of the hydrogen in the product gas drops to a certain threshold, the adsorption process is ended.
(2) High pressure down stroke
After the adsorption step of adsorption column a1 was completed, the programmable valve 4A was closed and 5A was opened. High-pressure steam enters the adsorption tower from the lower end. The original residual gas in the tower is driven by water vapor to replace the residual gas, and the residual gas flows out from the upper end of the adsorption tower and enters a product gas storage tank. When the purity of the outlet hydrogen gas is reduced to a certain threshold value, the high-pressure flushing process is finished.
(3) Column pressure drop 1
After the high-pressure downstream step is finished, the program control valves 1A and 5A are closed, and the program control valves 2A and 2E are opened. At this time, the pressure in the pressure equalizing tank T1 was lower than that in the adsorption column A1. The gas in A1 flows into T1 in forward direction, T1 is charged in reverse direction, A1 releases pressure in forward direction until the pressure in A1 is the same as that in T1.
(4) Column pressure drop 1
And after the process of the uniform pressure drop 1 of the tower tank is finished, the program control valve 2E is closed, and the program control valve 2C is opened. At this time, the pressure of the adsorption column A3 was lower than A1. The gas in A1 flows into A3 in the forward direction, A3 is charged in the reverse direction, A1 releases the pressure in the forward direction until the pressure in A1 is the same as that in A3.
(5) Pressure drop of column
And after the tower pressure equalizing drop 1 is finished, the program control valve 2C is closed, and the program control valve 2F is opened. The pressure equalizing tank T2 is lower than that of the adsorption tower A1. The pressure of A1 is released in the forward direction, and the pressure of T2 is charged in the reverse direction until the pressure of A1 is the same as that of T2.
(6) Pressure drop in column 3
And after the pressure equalizing of the tower tank is reduced by 2, the program control valves 2F and 2A are closed, and the program control valves 3A and 3G are opened. The pressure equalizing tank T3 is lower than that of the adsorption tower A1. The pressure of A1 is released in the forward direction, and the pressure of T3 is charged in the reverse direction until the pressure of A1 is the same as that of T3.
(7) Column pressure drop 2
And after the pressure equalizing of the tower tank is reduced by 3, the program control valves 3A and 3G are closed, and the program control valves 2A and 2D are opened. The pressure of adsorption column a4 was lower than that of adsorption column a 1. The pressure of A1 is released in the forward direction, and the pressure of A4 is charged in the reverse direction until the pressure of A1 is the same as that of A4.
(8) Pressure drop in the column 4
And after the tower pressure equalizing drop 2 is finished, the program control valves 2A and 2D are closed, and the program control valves 3A and 3H are opened. The pressure equalizing tank T4 is lower than that of the adsorption tower A1. The pressure of A1 is released in the forward direction, and the pressure of T4 is charged in the reverse direction until the pressure of A1 is the same as that of T4.
(9) Put in the contrary
And after the process of tower pressure equalization 4 is finished, the program control valves 3A and 3H are closed, and the program control valve 7A is opened. The pressure of the reverse degassing storage tank is lower than that of the adsorption tower A1, and the gas in the A1 flows out from the lower end into the reverse degassing storage tank until the pressure of the A1 is the same as that of the storage tank.
(10) Vacuum desorption
After the reverse discharging process is finished, the program control valve 7A is closed, the program control valve 8A is opened, and the vacuum pump pumps the gas in the adsorption tower A1 into the reverse discharging gas storage tank.
(11) Pressure equalization lift of tower tank 4
After the vacuum desorption is finished, the program control valve 8A is closed, and the program control valves 3A and 3H are opened. The pressure of the pressure equalizing tank T4 is higher than that of the adsorption tower A1, the A1 is charged reversely, and the T4 is discharged forwardly until the pressure of the A1 is the same as that of the T4.
(12) Column pressure equalization 2
And after the pressure equalization of the tower tank is finished and 4 is finished, the program control valves 3A and 3H are closed, and the program control valves 2A and 2B are opened. The pressure of the adsorption tower A2 is higher than that of the adsorption tower A1, the A1 is reversely pressurized, and the A2 is forwardly depressurized until the pressure of the A1 is the same as that of the A2.
(13) Pressure equalization lift of tower 3
And after the pressure equalization of the tower 2 is finished, the program control valves 2A and 2B are closed, and the program control valves 3A and 3G are opened. The pressure of the pressure equalizing tank T3 is higher than that of the adsorption tower A1, the A1 is charged reversely, and the T3 is discharged forwardly until the pressure of the A1 is the same as that of the T3.
(14) Pressure equalization lift 2 of tower
And after the pressure equalization of the tower tank is increased by 3, the program control valves 3A and 3G are closed, and the program control valves 2A and 2F are opened. The pressure of the pressure equalizing tank T2 is higher than that of the adsorption tower A1, the A1 is charged reversely, and the T2 is discharged forwardly until the pressure of the A1 is the same as that of the T2.
(15) Column pressure equalization 1
And after the pressure equalization of the tower tank 2 is finished, the program control valve 2F is closed, and the program control valve 2C is opened. The pressure of the adsorption tower A3 is higher than that of the adsorption tower A1, the A1 is reversely pressurized, and the A3 is forwardly depressurized until the pressure of the A1 is the same as that of the A3.
(16) Pressure equalization lift of tower 1
And after the pressure equalization of the tower 1 is finished, the program control valve 2C is closed, and the program control valve 2E is opened. The pressure of the pressure equalizing tank T1 is higher than that of the adsorption tower A1, the A1 is charged reversely, and the T1 is discharged forwardly until the pressure of the A1 is the same as that of the T1.
(17) Pressurizing
After the pressure equalization of the tower tank is finished and the pressure is raised by 1, the program control valves 2A and 2E are closed, the valve 1A is opened, the product gas storage tank reversely pressurizes the adsorption tower A1 until the pressure in the A1 reaches the adsorption pressure, and the pressurizing process is finished.
At this point a1 resumes the state before the adsorption step and one cycle ends and the next cycle begins. The cycle of the other adsorption columns A2-A4 and the pressure equalizing tanks T1-T4 is similar to that of A1, and the corresponding program control valves are switched on and off according to the time sequence shown in Table 2 and are staggered with each other in time.
Because the separation is carried out under the condition of medium temperature, a water vapor flushing step can be added in the pressure swing adsorption process, thereby reducing the content of hydrogen in the reverse-release gas and improving the yield of the hydrogen. The technical index pair ratio of the process and other purification processes is shown in table 3.
TABLE 3 comparison of the Process of the invention with the purification of conversion gas from other processes
Example 2: h for hydrogen production by methanol steam reforming2/CO2Separation of
The methane and the water vapor are subjected to catalytic cracking and water vapor shift reaction at a certain temperature and under a certain pressure to form a mixed gas containing carbon dioxide, hydrogen and a small amount of carbon monoxide. The reaction temperature is usually 250 ℃ to 300 ℃ and the pressure is 1-5 MPa.
For steam reforming of methanol with H2The purified 4-tower pressure swing adsorption system is shown in FIG. 3, and comprises 4 adsorption towers A1-A4, a hydrogen storage tank, a reverse-release gas storage tank, a low-pressure forward-flush gas buffer tank and a vacuum pump V, wherein the adsorbent filled with activated carbon is easy to adsorb CO2And CO, not easy to adsorb H2(ii) a The direct flushing gas is water vapor. The process flow of the adsorption column is shown in Table 4, and the opening and closing of the programmable valve is similar to that of example 1.
TABLE 4 methanol reforming H2/CO2Four-tower separation process
Remarking: AD: adsorption; ed 1: the pressure drop of the tower is 1; ed 2: the pressure drop of the tower is 2; LR: low-pressure forward flushing; BD: reverse discharge; VD: carrying out vacuum desorption; ep 2: the pressure of the tower is increased by 2; ep 1: the pressure of the tower is increased by 1; PP: pressurizing; ID: and (4) idling.
Taking the adsorption column a1 as an example:
(1) adsorption: at this time, the adsorption tower has completed the pressurizing process, and the adsorption pressure in the tower is reached. Opening the program control valves 1A and 3A to start an adsorption process;
(2) column pressure drop 1: after the adsorption process is finished, closing the program control valves 1A and 3A, and opening the program control valves 2A and 2C to start the tower pressure equalizing drop 1;
(3) idle: after the pressure equalizing and reducing of the tower 1 is finished, the program control valves 2A and 2C are closed, and A1 is in an idle state;
(4) column pressure drop 2: after the idle state is finished, opening the program control valve 2A, and starting the tower pressure equalizing drop 2 at 2D;
(5) low-pressure forward flushing: after the tower pressure equalizing drop 2 is finished, closing 2A and 2D, and opening 1A and 4A;
(6) reverse amplification: after the low-pressure forward flushing is finished, closing the program control valves 1A and 4A, and opening 5A to start the reverse discharging process;
(7) vacuum desorption: after the reverse discharging is finished, closing the valve 5A, opening the program control valve 6A, and starting to vacuumize the adsorption tower A1 by using a vacuum pump;
(8) column pressure equalization lift 2: after the vacuum desorption is finished, closing the program control valve 6A, opening the 2A and the 2B, and equalizing the pressure of the adsorption tower A1 and the pressure of the adsorption tower A2;
(9) idle: after the tower pressure equalization rise 2 is finished, closing 2A and 2B and starting an idle state;
(10) column pressure equalization 1: after the idle state is finished, opening the program control valves 2A and 2C, and equalizing the pressure of the adsorption towers A1 and A3;
(11) pressurizing: after the pressure equalization of the tower is increased by 1, the program control valves 2A and 2C are closed, the valve 1A is opened, and the product gas reversely pressurizes the adsorption tower A1.
By using the pressure swing adsorption process, H can be directly treated at the intermediate temperature2With CO2Separation is carried out to obtain H2The purity is higher than 99.99 percent, and the CO concentration is lower than 0.4ppm, almost meeting the requirements of all application fields on H2Can directly supply gas to the proton exchange membrane fuel cell, and has wide development prospect.
Example 3: intermediate temperature desulfurization of IGFC system
In integrated gasification fuel cell power systems (IGFC), the syngas needs to undergo deep desulfurization to supply the Solid Oxide Fuel Cell (SOFC). Typical compositions of the synthesis gas to be purified are shown in Table 1, the temperature is 200 ℃ and 300 ℃, and the pressure is generally 3-6 MPa. The SOFC is generally operated at 800 ℃, and the high-temperature tail gas of the fuel cell utilizes energy through a steam turbine. The power generation efficiency of the system is mainly related to the recovery rate of the synthesis gas and the energy consumption of gas heating. The process flow provided by the invention can be used for directly desulfurizing and purifying the synthesis gas, trapping part of carbon dioxide, and ensuring the yield of the synthesis gas without sensible heat loss, and can obviously improve the power generation efficiency of the system compared with a low-temperature purification method.
The specific implementation method comprises the following steps: the purification system consists of 4 adsorption towers and 4 pressure equalizing tanks; the adsorbent is selected from activated carbon with sulfur-carbon co-removal function, which is used for H2S、CO2Has higher adsorption capacity, H2The adsorption capacity is very small; the down-flushing and flushing gas is high pressure nitrogen and is from an air separation system of the IGFC. The PSA unit was operated according to the process flow shown in table 5. The product gas mainly comprises H2、CH4、N2、H2O、CO2、CO；H2The concentration of S can reach below 1ppm, and the SOFC requirement is met.
TABLE 5 Process flow of IGFC System syngas clean-up 8 column
Remarking: AD: adsorption; HR: high-pressure direct punching; EdA: the pressure drop of the tower and the tank is 1; ed 1: the pressure drop of the tower is 1; e dB: 2, tower tank pressure drop; EdC: 3, the pressure of the tower and the tank is reduced uniformly; ed 2: the pressure drop of the tower is 2; EdD: 4, tower tank pressure equalizing drop; BD: reverse discharge; p: flushing with nitrogen; EpD: 4, uniformly increasing the pressure of the tower tank; ep 2: the pressure of the tower is increased by 2; EpC: 3, uniformly increasing the pressure of the tower tank; EpB: the pressure of the tower is increased by 2; ep 1: the pressure of the tower is increased by 1; EpA: the pressure of the tower tank is increased by 1; PP: and (6) pressurizing.
Example 4: PEMFC fuel CO deep purification
Proton Exchange Membrane Fuel Cells (PEMFCs) have high requirements on the hydrogen purity of the fuel, wherein the CO concentration should be below 0.4 ppm. By using the process flow provided by the invention, the liquid fuel reforming synthesis gas or the detoxified gasification synthesis gas can be subjected to CO deep purification at the temperature of 100-200 ℃, and the purified gas can directly supply gas to the small-sized PEMFC without being heated.
The purification system consists of 2 adsorption towers; the adsorbent is a CO molecular sieve; the flushing gas is nitrogen or water vapor, and a vacuum desorption method is adopted. The process flow is shown in table 6.
TABLE 6 deep purification Process of CO
Remarking: adsorption of AD; HR: high-pressure direct punching; VD: and (4) vacuum desorption.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A medium temperature vacuum pressure swing adsorption method uses a medium temperature vacuum pressure swing adsorption system, which comprises an adsorption tower, a product gas tank (2), a forward flushing gas tank (5), a flushing gas tank (1) and a reverse discharging gas tank (4); a raw material gas inlet, a reverse-bleeding gas outlet and a forward flushing gas inlet are arranged below the adsorption tower, and a product gas port, a pressure equalizing port and a flushing gas inlet are arranged above the adsorption tower; the adsorption tower is filled with an adsorbent; the product gas tank (2) is connected with a product gas port of the adsorption tower through a connecting pipeline, and the forward flushing gas tank (5) and the reverse discharging gas tank (4) are respectively connected with a forward flushing gas inlet and a reverse discharging gas outlet of the adsorption tower; the flushing gas tank (1) is connected with a flushing gas inlet of the adsorption tower through a connecting pipeline; the forward flushing gas tank (5) comprises a high-pressure forward flushing gas tank and a low-pressure forward flushing gas tank; the product gas tanks include a high pressure product gas tank and a low pressure product gas tank; the method is characterized by comprising the working procedures of adsorption, constant-pressure forward flushing, reverse releasing, flushing and/or vacuum desorption, wherein the constant-pressure forward flushing comprises high-pressure forward flushing and low-pressure forward flushing, and the method comprises the following steps of:
opening a product gas port of the adsorption tower to communicate the adsorption tower with a product gas tank, and reversely boosting the pressure to the adsorption set pressure to enable the adsorption tower to enter an adsorption process;
adsorption: communicating a product gas port of the adsorption tower with a product gas tank, and enabling a feed gas inlet of the adsorption tower to be in an open state; the raw gas enters the adsorption tower from a raw gas inlet of the adsorption tower, the gas which is easy to adsorb is separated in the adsorption tower through selective adsorption of an adsorbent, and the gas which is difficult to adsorb enters a product gas tank from a product gas port of the adsorption tower;
high-pressure forward flushing: entering a high-pressure forward flushing process after the adsorption process is finished, enabling a product air port of the adsorption tower to be in an open state, and opening a forward flushing air inlet of the adsorption tower to enable the adsorption tower to be respectively communicated with a high-pressure product tank and a high-pressure forward flushing air tank; leading high-pressure forward flushing gas to enter an adsorption tower, and obtaining the gas which is difficult to adsorb and has the purity meeting the requirement in a high-pressure product gas tank;
pressure equalizing and reducing: after the high-pressure forward flushing process is finished, entering a voltage-equalizing and pressure-reducing process; opening and communicating two adsorption towers or one adsorption tower with a pressure equalizing port of a pressure equalizing tank, so that one adsorption tower is in a pressure equalizing and reducing process to carry out forward pressure reduction, and the other adsorption tower or the pressure equalizing tank is in a pressure equalizing and increasing process to carry out reverse pressure increase;
low-pressure forward flushing: the adsorption tower after pressure equalization and depressurization enters a low-pressure forward flushing process, a product gas port and a forward flushing gas inlet of the adsorption tower are opened and are respectively communicated with a low-pressure product tank and a low-pressure forward flushing gas tank; introducing low-pressure flushing gas into the adsorption tower, and obtaining the gas which is difficult to adsorb and has the purity meeting the requirement in a low-pressure product gas tank;
reverse amplification: enabling the adsorption tower subjected to low-pressure forward flushing to enter a reverse-releasing process, opening a reverse-releasing outlet of the adsorption tower to enable the adsorption tower to be communicated with the atmosphere or a reverse-releasing gas tank, releasing gas in the adsorption tower in the reverse direction of adsorption, enabling the adsorption tower to be reversely depressurized to be the same as the ambient pressure, and enabling the gas easy to adsorb to enter the reverse-releasing gas tank through the reverse-releasing outlet;
after the reverse decompression of the adsorption tower is finished, flushing and/or vacuum desorption are carried out to regenerate the adsorbent in the adsorption tower and release the gas components easy to adsorb out of the adsorption tower; and
washing: opening a reverse-release gas outlet and a flushing gas inlet of the adsorption tower, enabling flushing gas to enter from the top of the adsorption tower and flow out from the reverse-release gas outlet, enabling the adsorbent to be regenerated, and enabling gas components easy to adsorb to flow out of the adsorption tower along with flushing gas; and/or
Vacuum desorption: the reverse-release gas outlet of the adsorption tower is opened and communicated with the inlet of a vacuum pump (6), and the gas in the adsorption tower is released in the reverse direction of adsorption by vacuumizing, so that the adsorption tower is further depressurized in the reverse direction, and the gas easy to adsorb is obtained at the outlet of the vacuum pump, and the adsorbent is regenerated;
after the adsorption tower is flushed and/or vacuum desorbed, a product gas port of the adsorption tower is opened, the adsorption tower is communicated with a product gas tank, the pressure is reversely increased to the adsorption set pressure, and the adsorption tower enters an adsorption process.
2. A medium temperature vacuum pressure swing adsorption process according to claim 1, comprising:
the system is provided with a plurality of adsorption towers at least comprising an adsorption tower A (7) and an adsorption tower B (8); or the system comprises a plurality of adsorption towers and a plurality of pressure equalizing tanks, and the pressure equalizing tanks are connected with pressure equalizing ports of the adsorption towers;
one of the adsorption towers is reversely boosted to the adsorption set pressure, and then sequentially enters the adsorption and constant-pressure sequential flushing processes; under the constant pressure state, the gas difficult to adsorb on the top of the adsorption tower is pushed to enter the product gas tank from the product gas port;
opening pressure equalizing openings of two adsorption towers or the adsorption tower and a pressure equalizing tank and enabling the adsorption towers or the adsorption tower and the pressure equalizing tank to be communicated with each other, enabling the adsorption tower which completes constant-pressure forward flushing to be in a pressure equalizing and reducing process to carry out forward pressure reduction, and enabling the other adsorption tower or one pressure equalizing tank to be in a pressure equalizing and increasing process to carry out reverse pressure increase;
the adsorption tower after pressure equalization and depressurization enters a flushing process and/or a vacuum desorption process to complete the regeneration of the adsorbent, and then enters a pressure equalization and pressurization process; opening and communicating pressure equalizing openings of the two adsorption towers or the adsorption tower and the pressure equalizing tank, so that the adsorption tower completing adsorbent regeneration carries out reverse pressure equalizing and boosting, and simultaneously, the other adsorption tower or the pressure equalizing tank carries out forward pressure equalizing and pressure reducing;
after the pressure equalizing and boosting of the adsorption tower reaches the preset pressure, a product gas port of the adsorption tower is opened, so that the adsorption tower is communicated with a product gas tank, and the adsorption tower enters the adsorption process again.
3. A medium temperature vacuum pressure swing adsorption process as claimed in claim 1, wherein the medium temperature vacuum pressure swing adsorption system used in the process is provided with a plurality of adsorption columns including adsorption column A (7) and adsorption column B (8), and wherein there is a one-to-one correspondence between the adsorption columns in pressure equalization and pressure equalization.
4. A medium temperature vacuum pressure swing adsorption process as claimed in claim 1, wherein said readily adsorbable gas comprises one or more mixtures of hydrogen sulfide, carbon dioxide, carbon monoxide, methane, water vapor, oxygen; the difficult-to-adsorb gas comprises one or more of hydrogen, nitrogen and rare gas.
5. A medium temperature vacuum pressure swing adsorption process as claimed in claim 1, wherein the purge gas is selected from gases that are easily separated from the product gas and are not easily adsorbed by the adsorbent, including nitrogen, water vapor or argon.
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