CN112758892A - Pressure swing adsorption hydrogen purification system and method thereof - Google Patents
Pressure swing adsorption hydrogen purification system and method thereof Download PDFInfo
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- CN112758892A CN112758892A CN202110007141.6A CN202110007141A CN112758892A CN 112758892 A CN112758892 A CN 112758892A CN 202110007141 A CN202110007141 A CN 202110007141A CN 112758892 A CN112758892 A CN 112758892A
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- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
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Abstract
The invention discloses a system and a method for purifying hydrogen by pressure swing adsorption, when the product hydrogen requires CO and CO2And CH4When the method is strict, the nitrogen is added into the raw material gas, the proportion of each impurity in the raw material gas is adjusted, so that the molar content of the product hydrogen is ensured to be more than 99.9%, the hydrogen recovery rate is increased, and the hydrogen recovery rate can be increased by 0.3-2% for every 1% of the flow of the raw material gas, compared with a conventional pressure swing adsorption hydrogen purification system, the method has the advantages of small change, obvious benefits, suitability for newly-built devices and the improvement of the existing devices.
Description
Technical Field
The invention belongs to the technical field of pressure swing adsorption gas separation, and particularly relates to a pressure swing adsorption hydrogen purification system and a pressure swing adsorption hydrogen purification method.
Background
The pressure swing adsorption technology is widely applied to the separation of various mixed gases, such as the purification of oxygen and nitrogen from air, the purification of carbon dioxide from industrial tail gas rich in carbon dioxide, the purification of carbon monoxide from mixed gas rich in carbon monoxide, and the purification of hydrogen from various mixed gases rich in hydrogen, wherein hydrogen is used as important industrial gas, the demand is large, the application range is wide, and therefore, the research and development of the technology for purifying hydrogen by pressure swing adsorption are deeper.
For example, patent CN 1984705B discloses a continuous feeding three-bed pressure swing adsorption system, which realizes a twelve-step circulation process of pressure swing adsorption with two-step pressure equalization of three adsorption towers; in order to improve the efficiency of large plants, patent US6565628B2 discloses a sixteen-tower cycle process, patent CN103534002B discloses a twelve-to sixteen-tower process cycle; in order to enhance the regeneration effect of the adsorbent, patent CN1298410C discloses a pressure swing adsorption process with two sequential discharge tanks, which realizes a two-time staggered flushing process, and patent CN100588449C discloses a multiple-time sequential discharge staggered flushing pressure swing adsorption process, which realizes a three-time staggered flushing process; patent CN106039917B discloses porous adsorbent material in order to increase the adsorption rate of the adsorbent.
The largest application of hydrogen is the hydrogenation reaction process in the field of petrochemical industry, and the purity requirement of the chemical reaction process on the hydrogen is not high, generally 99.9% (mol/mol), but the C atom content in the hydrogen, such as CO and CO2、CH4The requirements are strict, and CO are generally required2Less than 20ppmv, individual process requirements for CO less than 5ppmv or even 1ppmv, and many industrial hydrogen production such as hydrocarbon steam reforming hydrogen production, coal hydrogen production and some industrial tail gas hydrogen production all contain a certain proportion of CO and CO in raw material gas before hydrogen purification2And CH4To ensure that the hydrogen purified by pressure swing adsorption contains C atoms in an amount of 10ppmv or even lower, the purity of the hydrogen is often 99.99 to 99.999% (mol/mol), which leads to variationThe recovery rate of the pressure adsorption purified hydrogen is limited.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a system and a method for purifying hydrogen by pressure swing adsorption, which solves the problem that the existing equipment for purifying hydrogen by pressure swing adsorption is used for purifying C atoms (CO and CO) in product hydrogen2And CH4) The hydrogen recovery rate is low when the content requirement is strict.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a pressure swing adsorption hydrogen purification system comprises at least three adsorption towers, a mixed raw material gas conveying pipeline connected into the adsorption towers and provided with a raw material gas program control valve, a desorption gas pipeline provided with a desorption gas program control valve, a flushing inlet pipeline connected out of the adsorption towers and provided with a flushing inlet program control valve, a forward discharge pipeline provided with a forward discharge program control valve, a pressure equalizing pipeline provided with a pressure equalizing valve, a first pressure equalizing and final boosting pipeline provided with a first pressure equalizing and final boosting program control valve, and a product gas output pipeline provided with a product gas program control valve; the mixed raw material gas conveying pipeline is connected with a hydrogen-containing raw material gas conveying pipeline and a nitrogen conveying pipeline.
Furthermore, a first flowmeter is arranged on the hydrogen-containing raw material gas conveying pipeline, and a second flowmeter and a regulating valve are arranged on the nitrogen conveying pipeline.
Furthermore, the flushing inlet pipeline is communicated with the forward discharging pipeline through a flushing regulating valve, or the forward discharging pipeline is communicated with the flushing inlet pipeline through one to two forward discharging buffer tanks and the flushing regulating valve; the first pressure equalizing product gas output pipelines are communicated through a final-charging regulating valve.
A pressure swing adsorption hydrogen purification method of a pressure swing adsorption hydrogen purification system adopts at least three adsorption towers to carry out pressure swing adsorption hydrogen purification through repeated circulation steps, and each adsorption tower undergoes repeated circulation steps including an adsorption step, a forward pressure reduction step, a reverse pressure reduction step, a regeneration step and a pressure increase step in sequence. Each adsorption tower is filled with at least one adsorbent which can selectively and easily adsorb other gas components except hydrogen in the feed gas conveying pipeline, and the adsorbents filled in all the adsorption towers can selectively and easily adsorb all other gas components except hydrogen in the feed gas conveying pipeline.
Further, the adsorption step is to contain at least CO and CO2And CH4After nitrogen is added into the hydrogen-containing raw material gas of the one impurity gas component, the mixed raw material gas enters the adsorption tower from the feed end of the adsorption tower under the pressure of 1.0-7.0 MPa, the non-hydrogen impurities are adsorbed by the adsorbent, and the hydrogen product flows out from the discharge end of the adsorption tower.
Further, the forward depressurization step is that the gas in the adsorption tower flows out of the adsorption tower along the gas flow direction during adsorption, and the pressure in the adsorption tower is reduced; preferably, the forward depressurization step comprises at least two depressurization processes, and the forward depressurization step is either entirely an equalizing depressurization step or comprises both an equalizing depressurization step and a forward purge step of providing a purge regeneration gas to the regeneration adsorption column.
Further, the reverse pressure reduction step is that the gas in the adsorption tower flows out of the adsorption tower against the gas flow direction during adsorption, the pressure in the adsorption tower is reduced, and the reverse pressure reduction step comprises at least one pressure reduction process.
Further, the regeneration step is a step of flowing the impurity gas components adsorbed in the adsorption tower out of the adsorption tower against the gas flow during adsorption, and the regeneration step is a step of flushing the regeneration tower by using the forward purge gas of other adsorption towers in a counter-current manner or a step of evacuating the adsorption tower by using vacuum equipment.
Further, the pressure increasing step is an adsorption tower after regeneration is completed, and the gas and the product gas in the forward pressure reducing step are used for increasing the pressure of the adsorption tower, wherein the pressure equalizing and increasing step is carried out when the gas in the forward pressure reducing step is received, and the final pressure increasing step is carried out when the product gas is received.
Further, the mixed raw material gas in the mixed raw material gas conveying pipeline enters an adsorption tower for adsorption in the adsorption process, and the volume flow ratio of the nitrogen in the nitrogen conveying pipeline to the hydrogen-containing raw material gas in the hydrogen-containing raw material gas conveying pipeline is less than or equal to 0.1; preferably, the volume flow ratio of the nitrogen in the nitrogen conveying pipeline to the hydrogen-containing raw material gas in the hydrogen-containing raw material gas conveying pipeline is less than or equal to 0.07; preferably, the molar content of nitrogen in the nitrogen conveying line is greater than or equal to 99.9%; preferably, the adsorption tower is filled with a molecular sieve adsorbent, or the molecular sieve and one or more of activated alumina, activated carbon and silica gel form a composite adsorption bed.
Compared with the prior art, the invention has the following beneficial effects:
the invention has simple implementation, scientific and reasonable design and convenient use, and the adsorption capacity of nitrogen on various adsorbents such as molecular sieve, activated carbon and silica gel is less than CH4CO and CO2In the adsorption capacity of (2) in the presence of a catalyst selected from the group consisting of2、CO、CO2、CH4、CnHmWhen purifying hydrogen from a mixture of hydrogen and nitrogen, the nitrogen (except hydrogen) first penetrates the adsorbent bed and then is CH4、CO、CO2Thus, when the C atoms in the product hydrogen are CO, CO2、CH4When the requirements are strict, if N in the raw material gas2The low content of the hydrogen leads to high purity of the product hydrogen, for example, when the C atom of the product hydrogen is controlled at 10ppmv, the purity of the product hydrogen is up to 99.99-99.999%. By using N2The adsorption capacity on the adsorbent is small and is prior to CO and CO2、CH4Penetrate the characteristics of the adsorption bed, through adding nitrogen in the raw materials, the impurity proportion in the raw material gas has been adjusted, nitrogen content has been increased, thereby when the C atom of the same index of product gas control, have more nitrogen to get into product hydrogen, the purity of product hydrogen has been reduced, when satisfying the index of hydrogen purity 99.9%, the adsorption front edge of hydrogen compares the product gas end that is closer to the adsorption tower with not adding nitrogen, thereby the rate of recovery of hydrogen has been increased, the rate of recovery that can promote hydrogen about 0.3% -2.0% per increase 1% nitrogen in the raw material gas. The invention is not only suitable for the newly-built device, but also suitable for the reconstruction of the existing pressure swing adsorption hydrogen extraction device.
Drawings
FIG. 1 is a diagram of a pressure swing adsorption hydrogen purification system of the present invention.
FIG. 2 is a diagram of a pressure swing adsorption hydrogen purification system with a surge tank in accordance with the present invention.
FIG. 3 is the adsorption isotherms of four gases on a molecular sieve of certain type at 25 ℃ according to the invention.
FIG. 4 is a graph showing the distribution of hydrogen in the adsorbent bed at the end of adsorption in accordance with the present invention.
FIG. 5 shows the distribution of hydrogen in the top zone of the adsorption bed at the end of the adsorption according to the present invention.
Wherein, the names corresponding to the reference numbers are:
1-mixed raw material gas conveying pipeline, 2-flushing pipeline, 3-reverse gas discharging pipeline, 4-flushing pipeline, 5-forward discharging pipeline, 6-fourth pressure equalizing/fifth pressure equalizing pipeline, 7-second pressure equalizing/third pressure equalizing pipeline, 8-first pressure equalizing and final boosting pipeline, 9-product gas outward conveying pipeline, 10-final charging regulating valve, 11-flushing regulating valve, 12-hydrogen-containing raw material gas conveying pipeline, 13-nitrogen conveying pipeline, 14-first flowmeter, 15-second flowmeter, 16-regulating valve, 17-hydrogen product, 18-adsorption tower, 19-forward discharging buffer tank, 1-raw material gas program control valve, 2 XX-flushing outlet program control valve, 3 XX-reverse gas discharging program control valve, 4 XX-flushing inlet program control valve, 5 XX-forward-release program control valve, 6 XX-fourth pressure equalizing/fifth pressure equalizing program control valve, 7 XX-second pressure equalizing/third pressure equalizing program control valve, 8 XX-first pressure equalizing and final boosting program control valve and 9 XX-product gas program control valve.
Wherein XX in 1XX, 2XX, 3XX, 4XX, 5XX, 6XX, 7XX, 8XX and 9XX is the last two digits of the adsorption tower number, as shown in fig. 1, 1XX, 2XX, 3XX, 4XX, 5XX, 6XX, 7XX, 8XX and 9XX corresponding to the adsorption tower number 003 are 103, 203, 303, 403, 503, 603, 703, 803 and 903 respectively, and so on.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation or be constructed and operated in a particular orientation, and thus, it should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; of course, mechanical connection and electrical connection are also possible; alternatively, they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The invention provides a pressure swing adsorption hydrogen purification system which comprises at least three adsorption towers, a mixed raw material gas conveying pipeline connected into the adsorption towers and provided with a raw material gas program control valve, a desorption gas pipeline provided with a desorption gas program control valve, a flushing inlet pipeline connected out of the adsorption towers and provided with a flushing inlet program control valve, a forward discharge pipeline provided with a forward discharge program control valve, a pressure pipeline provided with a pressure equalizing program control valve, a first pressure equalizing and final boosting pipeline provided with a first pressure equalizing and final boosting program control valve and a product gas outer conveying pipeline provided with a product gas program control valve; the mixed raw material gas conveying line is connected with a hydrogen-containing raw material gas conveying line and a nitrogen conveying line, the hydrogen-containing raw material gas conveying line is provided with a first flowmeter, and the nitrogen conveying line is provided with a second flowmeter and an adjusting valve. The flushing inlet pipeline is communicated with the forward discharging pipeline through a flushing regulating valve, or the forward discharging pipeline is communicated with the flushing inlet pipeline through one to two forward discharging buffer tanks 19 and the flushing regulating valve; the first pressure equalizing product gas output pipelines are communicated through a final-charging regulating valve.
The invention provides a pressure swing adsorption hydrogen purification system, which comprises at least three adsorption towers 18, a mixed raw material gas conveying pipeline 1 connected into the adsorption towers 18 and provided with a raw material gas program control valve 1XX, a desorption gas pipeline provided with a desorption gas program control valve, a flushing inlet pipeline 4 connected out of the adsorption towers 18 and provided with a flushing inlet program control valve 4XX, a forward discharge pipeline 5 provided with a forward discharge program control valve 5XX, a pressure equalizing pipeline provided with a pressure equalizing program control valve, a first pressure equalizing and final boosting pipeline 8 provided with a first pressure equalizing and final boosting program control valve 8XX and a product gas output pipeline 9 provided with a product gas program control valve 9XX, wherein the adsorption towers are connected with the adsorption towers 18; the mixed raw material gas conveying pipeline 1 is connected with a raw material gas conveying pipeline 12 containing hydrogen and a nitrogen conveying pipeline 13, the desorption gas pipeline comprises a flushing pipeline 2 and a reverse gas discharging pipeline 3, and the desorption gas programmable valve comprises a flushing programmable valve 2XX arranged on the flushing pipeline 2 and a reverse gas discharging programmable valve 3XX arranged on the reverse gas discharging pipeline 3. The pressure equalizing pipeline comprises a second pressure equalizing/third pressure equalizing pipeline 7 and a fourth pressure equalizing/fifth pressure equalizing pipeline 6, and the pressure equalizing programmable valve comprises a second pressure equalizing/third pressure equalizing programmable valve 7XX arranged on the second pressure equalizing/third pressure equalizing pipeline 7 and a fourth pressure equalizing/fifth pressure equalizing programmable valve 6XX arranged on the fourth pressure equalizing/fifth pressure equalizing pipeline 6. The hydrogen-containing raw material gas conveying pipeline 12 is provided with a first flowmeter 14, and the nitrogen conveying pipeline 13 is provided with a second flowmeter 15 and a regulating valve 16. The flushing inlet pipeline 4 is communicated with the forward discharging pipeline 5 through a flushing regulating valve 11, and the first pressure equalizing and final boosting pipeline 8 is communicated with the product gas output pipeline 9 through a final filling regulating valve 10.
The invention provides a pressure swing adsorption hydrogen purification method of a pressure swing adsorption hydrogen purification system, which adopts at least three adsorption towers to respectively carry out pressure swing adsorption hydrogen purification through repeated circulation steps, and each adsorption tower sequentially comprises an adsorption step, a forward pressure reduction step, a reverse pressure reduction step, a regeneration step and a pressure increase step through the repeated circulation steps. Each adsorption tower is filled with at least one adsorbent which can selectively and easily adsorb other gas components except hydrogen in the feed gas conveying pipeline, and the adsorbents filled in all the adsorption towers can selectively and easily adsorb all other gas components except hydrogen in the feed gas conveying pipeline. The mixed raw material gas in the mixed raw material gas conveying pipeline enters an adsorption tower for adsorption in the adsorption process, and the volume flow ratio of the nitrogen in the nitrogen conveying pipeline to the hydrogen-containing raw material gas in the hydrogen-containing raw material gas conveying pipeline is less than or equal to 0.1; preferably, the volume flow ratio of the nitrogen in the nitrogen conveying pipeline to the hydrogen-containing raw material gas in the hydrogen-containing raw material gas conveying pipeline is less than or equal to 0.07; preferably, the molar content of nitrogen in the nitrogen conveying line is greater than or equal to 99.9%; preferably, the adsorption tower is filled with a molecular sieve adsorbent, or a composite adsorption bed consisting of one or more of molecular sieve, activated alumina, activated carbon and silica gel
The pressure swing adsorption method for purifying hydrogen comprises the adsorption step of at least containing CO and CO2And CH4After nitrogen is added into the hydrogen-containing raw material gas of the one impurity gas component, the mixed raw material gas enters the adsorption tower from the feed end of the adsorption tower under the pressure of 1.0-7.0 MPa, the non-hydrogen impurities are adsorbed by the adsorbent, and the hydrogen product flows out from the discharge end of the adsorption tower.
The forward pressure reduction step in the pressure swing adsorption hydrogen purification method comprises the steps that gas in the adsorption tower flows out of the adsorption tower along the gas flow direction during adsorption, and the pressure in the adsorption tower is reduced; preferably, the forward depressurization step comprises at least two depressurization processes, and the forward depressurization step is either entirely an equalizing depressurization step or comprises both an equalizing depressurization step and a forward purge step of providing a purge regeneration gas to the regeneration adsorption column.
The reverse pressure reduction step in the pressure swing adsorption hydrogen purification method comprises the steps that gas in the adsorption tower flows out of the adsorption tower in the opposite direction of the gas flow during adsorption, the pressure in the adsorption tower is reduced, and the reverse pressure reduction step comprises at least one pressure reduction process.
The regeneration step in the pressure swing adsorption hydrogen purification method of the invention is that the impurity gas components adsorbed in the adsorption tower flow out of the adsorption tower against the gas flow direction during adsorption, and the regeneration step is a forward-discharge gas countercurrent flushing regeneration step of other adsorption towers or an evacuation regeneration step of vacuumizing the adsorption tower by using vacuum equipment.
The pressure increasing step in the pressure swing adsorption hydrogen purification method is an adsorption tower after regeneration is completed, and the pressure of the adsorption tower is increased by utilizing gas in the forward pressure reducing step and product gas, wherein the pressure equalizing and increasing step is performed when the gas in the forward pressure reducing step is received, and the final pressure increasing step is performed when the product gas is received.
The invention has simple implementation, scientific and reasonable design and convenient use, and the adsorption capacity of nitrogen on various adsorbents such as molecular sieve, activated carbon and silica gel is less than CH4CO and CO2In the adsorption capacity of (2) in the presence of a catalyst selected from the group consisting of2、CO、CO2、CH4、CnHmWhen purifying hydrogen from a mixture of hydrogen and nitrogen, the nitrogen (except hydrogen) first penetrates the adsorbent bed and then is CH4、CO、CO2Thus, when the C atoms in the product hydrogen are CO, CO2、CH4When the requirements are strict, if N in the raw material gas is2The low content of the hydrogen leads to high purity of the product hydrogen, for example, when the C atom of the product hydrogen is controlled at 10ppmv, the purity of the product hydrogen is up to 99.99-99.999%. By using N2The adsorption capacity on the adsorbent is small and is prior to CO and CO2、CH4Pierce through the characteristics of adsorption bed, through wherein add nitrogen gas at the raw materials, the impurity proportion in the feed gas has been adjusted, nitrogen content has been increased, thereby when the C atom of the same index of product gas control, have more nitrogen gas to get into product hydrogen, the purity of product hydrogen has been reduced, when satisfying hydrogen purity 99.9%'s index, the adsorption front edge of hydrogen compares the product gas end that is close to the adsorption tower more with not adding nitrogen gas, thereby the rate of recovery of hydrogen has been increased, the rate of recovery that can promote hydrogen every increase 1% nitrogen gas in the feed gas is about 0.3 ~ 2.0%. The invention is not only suitable for the newly-built device, but also suitable for the reconstruction of the existing pressure swing adsorption hydrogen extraction device.
The concentration percentages used in the present invention are mole percentages, pressure gauge, unless specifically indicated as absolute pressure.
The invention discloses a pressure swing adsorption hydrogen purification system, which meets the requirements of CO and CO on product hydrogen2And CH4Strictly, the nitrogen is added into the feed gas to adjust the proportion of each impurity in the feed gas, so that the molar content of the product hydrogen is ensured to be more than 99.9%, the hydrogen recovery rate is increased, and the hydrogen recovery rate is increased when the volume flow of the feed gas is increased by 1% of the nitrogenThe rate can be increased by 0.3-2.0%, compared with the conventional pressure swing adsorption hydrogen purification system, the invention has small change and obvious benefits, and is not only suitable for newly-built devices, but also suitable for the reconstruction of the existing devices.
A pressure swing adsorption gas separation system for purifying hydrogen from a hydrogen-rich gas mixture, the system comprising more than three adsorption towers respectively subjected to repeated circulation steps, each adsorption tower is filled with only one adsorbent which is selective to adsorb and can be easily adsorbed, and the repeated circulation steps experienced by each adsorption tower are an adsorption step (a), a forward depressurization step (b), a reverse depressurization step (c), a regeneration step (d) and a pressurization step (e) in sequence, wherein:
an adsorption step (a): at least CO and CO2And CH4After nitrogen is added into the hydrogen-containing raw material gas of the first impurity, the mixed raw material gas enters the adsorption tower from the feed end of the adsorption tower under the pressure of 1.0-7.0 MPa, the non-hydrogen impurities are adsorbed by the adsorbent, and the hydrogen product flows out from the discharge end of the adsorption tower.
Forward depressurization step (b): the gas in the adsorption tower flows out of the adsorption tower along the gas flow direction during adsorption, the pressure in the adsorption tower is reduced, the forward pressure reduction step comprises at least two pressure reduction processes, and the forward pressure reduction step is a pressure-equalizing pressure reduction step or comprises a pressure-equalizing pressure reduction step and two steps of a forward release step for providing flushing regeneration gas for the regeneration adsorption tower.
And (c) reverse pressure reduction: the gas in the adsorption tower flows out of the adsorption tower against the gas flow during adsorption, the pressure in the adsorption tower is reduced, and the reverse pressure reduction step comprises at least one pressure reduction process.
A regeneration step (d): impurities adsorbed in the adsorption tower flow out of the adsorption tower against the gas flow during adsorption, and the regeneration step is a forward-exhaust gas countercurrent flushing regeneration step of other adsorption towers or an evacuation regeneration step of vacuumizing the adsorption tower by using vacuum equipment.
A pressure increasing step (e): and (3) the regenerated adsorption tower reversely boosts the pressure of the adsorption tower by utilizing the gas and the product gas in the forward pressure reduction step, wherein the pressure equalizing and boosting step is carried out when the gas in the forward pressure reduction step is received, and the final pressure boosting step is carried out when the product gas is received.
The pressure of the nitrogen added into the hydrogen-rich raw material gas is greater than or equal to that of the hydrogen-rich raw material gas, the molar content of the nitrogen is more than 99.9 percent, and the temperature of the nitrogen is 0-40 ℃ at normal temperature; the ratio of the volume flow rate of the nitrogen gas added into the raw gas rich in hydrogen to the volume flow rate of the raw gas rich in hydrogen is less than or equal to 0.1, and preferably less than or equal to 0.07. The volume flow of nitrogen gas added into the hydrogen-rich feed gas is changed along with the change of the flow of the feed gas.
In order to make the technical scheme of the present invention better understood by those skilled in the art, twelve adsorption towers are used as examples for illustration.
As shown in fig. 1, the system for purifying hydrogen through pressure swing adsorption of the present embodiment includes twelve adsorption towers 18(001 to 012), a mixed raw material gas delivery pipeline 1, a product gas delivery pipeline 9, a reverse gas release pipeline 3, a flushing outlet pipeline 2, a first pressure equalizing and final pressure boosting pipeline 8, a second pressure equalizing/third pressure equalizing pipeline 7, a fourth pressure equalizing/fifth pressure equalizing pipeline 6, a forward discharge pipeline 5, a flushing inlet pipeline 4, a hydrogen-containing raw material gas delivery pipeline 12, a nitrogen gas delivery pipeline 13, and program control valves 101 to 912, wherein a first flow meter 14 is disposed on the hydrogen-containing raw material gas delivery pipeline 12, a second flow meter 15 and a regulating valve 16 are disposed on the nitrogen gas delivery pipeline 13, the flushing regulating valve 11 is communicated with the forward discharge pipeline 5 and the flushing pipeline 6, and the final filling regulating valve 10 is connected with the product gas delivery pipeline 9 and the first pressure equalizing and final pressure boosting pipeline 8. A surge tank 19 may also be added in this example, as shown in FIG. 2.
In the example (figure 1), a 12-3-5/P flow path is adopted, and the process sequence is shown in table 1, namely 12 adsorption towers, 3 adsorption towers are used for adsorption at the same time, and 5 steps of pressure equalization and flushing regeneration are carried out. The pressure of the raw material gas is 3.0MPa, and the regeneration pressure is 0.02 MPa; the volume ratio of each component of the mixed raw material gas in the mixed raw material gas conveying pipeline is as follows: h2:N277: 0.5: 22.5, the purity of the product hydrogen is more than or equal to 99.9 percent; the adsorbent is molecular sieve.
Table 1 example 1 timing sequence chart
Note: a: adsorption step, 1D: a first pressure equalizing and reducing step, 2D: a second pressure equalizing and reducing step, 3D: a third pressure equalizing and reducing step, 4D: a fourth pressure equalizing and reducing step, 5D: a fifth pressure equalizing and reducing step, PP: step D: reverse amplification step, P: washing step, 5R: a fifth voltage equalizing and boosting step, 4R: a fourth voltage equalizing and boosting step, 3R: a third voltage-equalizing and boosting step, 2R: a second voltage equalizing and boosting step, 1R: a first voltage equalizing and boosting step, FR: and finally, a pressure rising step.
After the hydrogen-containing raw material gas in the hydrogen-containing raw material gas conveying pipeline 12 and the nitrogen in the nitrogen conveying pipeline 13 are mixed in the mixed raw material gas conveying pipeline 1, the mixture enters 3 adsorption towers at normal temperature and 3.0MPa for adsorption, impurities (nitrogen and carbon monoxide) are adsorbed by the adsorbent, and a hydrogen product 17 is output through a product gas output pipeline 9; the adsorption tower which finishes adsorption sequentially carries out a first pressure equalizing and reducing step, a second pressure equalizing and reducing step, a third pressure equalizing and reducing step, a fourth pressure equalizing and reducing step, a fifth pressure equalizing and reducing step and a forward releasing step so as to finish forward pressure reduction; after the forward depressurization step, depressurizing the adsorption tower against the direction of the adsorption bed, namely a reverse depressurization step, wherein reverse blowdown gas is sent out of the system through a reverse blowdown valve 3XX and a reverse blowdown pipeline 3; after reverse pressure reduction, forward pressure reduction gas of the adsorption tower in the forward discharging step is used for flushing and regenerating the adsorption tower against the direction of the adsorption bed through a forward discharging valve 5XX, a forward discharging pipeline 5, a flushing regulating valve 11, a flushing inlet pipeline 4 and a flushing inlet valve 4XX, and flushing waste gas is discharged out of the system through a flushing outlet valve 2XX and a flushing outlet pipeline 2; and the adsorption tower after being washed sequentially goes through a fifth voltage-equalizing and boosting step, a fourth voltage-equalizing and boosting step, a third voltage-equalizing and boosting step, a second voltage-equalizing and boosting step, a first voltage-equalizing and boosting step and a final voltage-boosting step. The first pressure equalizing and reducing step corresponds to the first pressure equalizing and increasing step, and the two corresponding adsorption towers are communicated with a first pressure equalizing and final pressure increasing pipeline 8 through a valve 8XX to realize pressure balance; the second/third pressure equalizing and reducing step corresponds to the second/third pressure equalizing and increasing step, and the corresponding two adsorption towers are communicated with a second pressure equalizing/third pressure equalizing pipeline 7 through a valve 7XX to realize pressure balance; the fourth/fifth pressure equalizing and reducing step corresponds to the fourth/fifth pressure equalizing and increasing step, and the corresponding two adsorption towers are communicated with a fourth pressure equalizing/fifth pressure equalizing pipeline 6 through a valve 6XX to realize pressure balance; in the final pressure increasing step, the product gas 17 passes through the final charge regulating valve 10 and then enters the adsorption tower for final pressure increase through the first pressure equalizing and final pressure increasing pipeline 8 and the final pressure increasing valve 8XX until the pressure of the adsorption tower reaches the adsorption pressure.
The flow rate of nitrogen gas in the hydrogen-containing raw gas conveying pipeline 12 and the nitrogen gas conveying pipeline 13 is controlled by the regulating valve 16, so that the flow rate of the nitrogen gas and the flow rate of the hydrogen-containing raw gas are maintained at a certain proportion, and when the flow rate of the hydrogen-containing raw gas is changed, the flow rate of the nitrogen gas is regulated by the regulating valve 16.
The CO content of the product hydrogen was controlled at 10ppmv, and the recovery rate of the product hydrogen and the molar content of the product hydrogen were varied with the amount of nitrogen added as shown in Table 2. With the increase of the addition of the nitrogen, the recovery rate of the hydrogen is gradually increased, and the hydrogen tax rate is increased by 1 percentage point after 2 percent of the nitrogen is added.
The adsorption capacity of nitrogen on various adsorbents such as molecular sieve, activated carbon and silica gel is less than CH4CO and CO2Adsorption capacity of (2), as shown in FIG. 3, H2、N2、CH4The adsorption isotherm of CO on a molecular sieve of a certain type, and the adsorption isotherm of nitrogen is positioned in hydrogen and CH4And CO.
In the presence of N2、CO、CO2、CH4、CnHmAnd H2Purifying H from the gas mixture2When N is present2First through the adsorbent bed (except for hydrogen) and then CH4、CO、CO2Thus, when the C atoms in the product hydrogen are CO, CO2、CH4When the requirements are strict, if the content of nitrogen in the raw material gas is low, the purity of the product hydrogen is very high, and when the CO atom of the product hydrogen is controlled to be 10ppmv, the purity of the product hydrogen in the example is 99.996%, and the addition is addedThe hydrogen content was 99.978% after 2% nitrogen addition and 99.921% after 5% nitrogen addition.
The nitrogen gas has small adsorption capacity on the adsorbent and is prior to CO and CO2、CH4The characteristics of the penetrating adsorption bed are that N is added into the raw gas containing hydrogen2The impurity proportion in the feed gas is adjusted, the nitrogen content is increased, so that when the product gas controls C atoms with the same index, more nitrogen enters the product hydrogen, the purity of the product hydrogen is reduced, and when the index of 99.9 percent of the hydrogen purity is met, the adsorption front edge of the hydrogen and the adsorption front edge of the hydrogen are not added with N2Compare the product gas end that is closer to the adsorption tower to increased the rate of recovery of hydrogen, figure 4 is the distribution curve of hydrogen in the adsorption bed when the adsorption finishes before and after utilizing pressure swing adsorption's mathematical model simulation to add nitrogen, figure 5 is the hydrogen distribution curve in adsorption bed top region, obviously sees that the adsorption front edge of hydrogen is closer to the top of adsorption bed after adding nitrogen.
TABLE 2 influence of nitrogen addition on hydrogen recovery at a CO content of 10ppmv in the product gas
Note: k is the ratio of the volume flow rates of the nitrogen gas 13 and the feed gas 12.
Finally, it should be noted that: the above embodiments are only preferred embodiments of the present invention to illustrate the technical solutions of the present invention, but not to limit the technical solutions, and certainly not to limit the patent scope of the present invention; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention; that is, the technical problems to be solved by the present invention, which are not substantially changed or supplemented by the spirit and the concept of the main body of the present invention, are still consistent with the present invention and shall be included in the scope of the present invention; in addition, the technical scheme of the invention is directly or indirectly applied to other related technical fields, and the technical scheme is included in the patent protection scope of the invention.
Claims (10)
1. A pressure swing adsorption hydrogen purification system is characterized by comprising at least three adsorption towers, a mixed raw material gas conveying pipeline connected into the adsorption towers and provided with a raw material gas program control valve, a desorption gas pipeline provided with a desorption gas program control valve, a flushing inlet pipeline connected out of the adsorption towers and provided with a flushing inlet program control valve, a forward discharge pipeline provided with a forward discharge program control valve, a pressure equalizing pipeline provided with a pressure equalizing program control valve, a first pressure equalizing and final boosting pipeline provided with a first pressure equalizing and final boosting program control valve and a product gas outer conveying pipeline provided with a product gas program control valve; the mixed raw material gas conveying pipeline is connected with a hydrogen-containing raw material gas conveying pipeline and a nitrogen conveying pipeline.
2. The pressure swing adsorption hydrogen purification system of claim 1, wherein the hydrogen-containing feed gas delivery line is provided with a first flow meter, and the nitrogen delivery line is provided with a second flow meter and a regulating valve.
3. The pressure swing adsorption hydrogen purification system of claim 1, wherein the flush inlet line is in communication with the in-line flush line through a flush regulating valve, or in communication between the in-line flush line and the flush inlet line through one or two in-line buffer tanks and a flush regulating valve; the first pressure equalizing product gas output pipelines are communicated through a final-charging regulating valve.
4. The pressure swing adsorption hydrogen purification method of the pressure swing adsorption hydrogen purification system of any one of claims 1-3, characterized in that at least three adsorption towers are respectively used for pressure swing adsorption hydrogen purification through repeated circulation steps, and each adsorption tower is subjected to repeated circulation steps of adsorption step, forward pressure reduction step, reverse pressure reduction step, regeneration step and pressure increase step in turn.
5. The pressure swing adsorption hydrogen purification method of claim 4, wherein the adsorption step is to remove CO and CO2And CH4After nitrogen is added into the hydrogen-containing raw material gas of the one impurity gas component, the mixed raw material gas enters the adsorption tower from the feed end of the adsorption tower under the pressure of 1.0-7.0 MPa, the non-hydrogen impurities are adsorbed by the adsorbent, and the hydrogen product flows out from the discharge end of the adsorption tower.
6. The pressure swing adsorption hydrogen purification method of claim 4, wherein the forward depressurization step is that the gas in the adsorption tower flows out of the adsorption tower along the gas flow direction during adsorption, and the pressure in the adsorption tower is reduced; preferably, the forward depressurization step comprises at least two depressurization processes, and the forward depressurization step is either entirely an equalizing depressurization step or comprises both an equalizing depressurization step and a forward purge step of providing a purge regeneration gas to the regeneration adsorption column.
7. The pressure swing adsorption hydrogen purification method of claim 4, wherein the reverse pressure reduction step is a step in which the gas in the adsorption column flows out of the adsorption column against the gas flow during adsorption, the pressure in the adsorption column is reduced, and the reverse pressure reduction step comprises at least one pressure reduction process.
8. The pressure swing adsorption hydrogen purification method as claimed in claim 4, wherein the regeneration step is a step of flowing the impurity gas components adsorbed in the adsorption column out of the adsorption column against the flow of the gas during adsorption, and the regeneration step is a step of flushing the regeneration column with a forward purge gas of the other adsorption column in a counter current manner or a step of evacuating the regeneration column by using a vacuum apparatus.
9. The pressure swing adsorption hydrogen purification process of claim 4, wherein the pressure increasing step is an adsorption tower after completion of regeneration, and the pressure of the adsorption tower is increased by using the gas from the forward pressure decreasing step and the product gas, wherein the pressure equalizing and increasing step is performed when the gas from the forward pressure decreasing step is received, and the final pressure increasing step is performed when the product gas is received.
10. The pressure swing adsorption hydrogen purification method of claim 4, wherein the mixed raw material gas in the mixed raw material gas conveying pipeline enters an adsorption tower for adsorption in the adsorption process, and the volume flow ratio of the nitrogen in the nitrogen conveying pipeline to the hydrogen-containing raw material gas in the hydrogen-containing raw material gas conveying pipeline is less than or equal to 0.1; preferably, the volume flow ratio of the nitrogen in the nitrogen conveying pipeline to the hydrogen-containing raw material gas in the hydrogen-containing raw material gas conveying pipeline is less than or equal to 0.07; preferably, the molar content of nitrogen in the nitrogen conveying line is greater than or equal to 99.9%; preferably, the adsorption tower is filled with a molecular sieve adsorbent, or the molecular sieve and one or more of activated alumina, activated carbon and silica gel form a composite adsorption bed.
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