CN109179335A - A kind of device and method that pressure-variable adsorption prepares high-purity oxygen - Google Patents
A kind of device and method that pressure-variable adsorption prepares high-purity oxygen Download PDFInfo
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- CN109179335A CN109179335A CN201811310605.5A CN201811310605A CN109179335A CN 109179335 A CN109179335 A CN 109179335A CN 201811310605 A CN201811310605 A CN 201811310605A CN 109179335 A CN109179335 A CN 109179335A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/02—Preparation of oxygen
- C01B13/0229—Purification or separation processes
- C01B13/0248—Physical processing only
- C01B13/0259—Physical processing only by adsorption on solids
- C01B13/0262—Physical processing only by adsorption on solids characterised by the adsorbent
- C01B13/027—Zeolites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/047—Pressure swing adsorption
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- C01B13/02—Preparation of oxygen
- C01B13/0229—Purification or separation processes
- C01B13/0248—Physical processing only
- C01B13/0259—Physical processing only by adsorption on solids
- C01B13/0262—Physical processing only by adsorption on solids characterised by the adsorbent
- C01B13/0266—Carbon based materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
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- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0009—Physical processing
- C01B2210/0014—Physical processing by adsorption in solids
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Abstract
The present invention relates to the device and method that a kind of pressure-variable adsorption prepares high-purity oxygen.The present invention improves existing two-stage omnibus control system technology, the rich argon tail gas that second level pressure swing adsorption system is discharged is as the level-one purgative gas of first order pressure swing adsorption system adsorption tower, simultaneously using the oxygen-containing relatively low product gas of the initial stage institute's output obtained after the pressure swing adsorption system separating-purifying of the second level as the three-level purgative gas of the last wash phase of first order pressure swing adsorption system adsorption tower, the primary oxygen product gas concentration for improving the generation of first order pressure swing adsorption system improves the rate of recovery of whole system oxygen product and reduces energy consumption.And initial stage, mid-term and later stage parsing separation are carried out to the product gas of second level pressure swing adsorption system, using mid-term product gas as final products gas, the purity of oxygen is further improved, ensure that the oxygen purity of final products gas 99.0% or even 99.7% or more.
Description
Technical field
The invention belongs to gas separation technique field, relate to the use of pressure swing adsorption to air carry out separation prepare it is high-purity
The technology of oxygen, and in particular to a kind of transformation based on equilibrium selective absorption and kinetic selectivity adsorbing separation mechanism is inhaled
The attached device and method for preparing high-purity oxygen.
Background technique
As a kind of industrial gasses using increasingly extensive, demand is also continuously increased oxygen, is widely used in metallurgy and is changed
The fields such as work are also widely used in energy conservation and environmental protection, such as waste incineration, industrial combustion, sewage treatment.Tradition oxygen
Method is Deep Cooling Method, but cost is high, space occupied is big, process is complicated, energy consumption is high, suitable for oxygen processed on a large scale.Pressure-variable adsorption
Isolation technics is one for gas purification and isolated technology, prepares oxygen, process letter from air separation using pressure-variable adsorption
It is single, it is easy to operate, it can run at normal temperature, maintenance rate is low, and low energy consumption, and occupied area is small, can be quick with oxygen scene
Cheap oxygen is easily continuously produced, and may be implemented to be fully automated.Due to these advantages, separating oxygen from air by means of pressure swing adsorption
Technology is widely used to the fields such as metallurgy, oxygen-enriched combusting, chemical industry gas making and medical treatment.
Omnibus control system technology is by separation air using the principle of physical absorption come oxygen producing, pressure-variable adsorption
The mechanism of oxygen processed is broadly divided into two kinds, one is according to adsorbent to the adsorption capacity of nitrogen be greater than to the adsorption capacity of oxygen come
Oxygen producing；Another kind is diffusion rate of the diffusion rate according to oxygen in adsorbent micropore greater than nitrogen, and remote
Carry out oxygen producing when from adsorption equilibrium.The adsorbent that the former uses is equilibrium selective adsorbent, such as zeolite molecular sieve；The latter makes
Adsorbent is kinetic selectivity adsorbent, such as carbon molecular sieve.Since oxygen and argon gas are in adsorbents such as zeolite molecular sieves
On equilibrium adsorption curve it is essentially the same, equilibrium adsorption agent can not achieve the separation of oxygen argon；And in dynamics such as carbon molecular sieves
On selective absorbent, quickly, but nitrogen argon rate of adsorption difference is little for the diffusion rate of Oxygen Adsorption, is difficult to realize point of nitrogen argon
From；Therefore the adsorption process of Balancing selection or selection of kinetics no matter is used, only level-one pressure-variable adsorption is difficult to produce purity
Oxygen higher than 95%, this just greatly limits cutting, medical treatment etc. and needs the higher oxygen application of purity.In order to from air
The middle oxygen for obtaining higher purity, is just come into being using two-stage or stage variable pressure pressure swing adsorption come oxygen processed.
Chinese patent CN201930684U discloses a kind of production oxygen-enriched containing argon obtained in first order pressure swing adsorption system
The high-purity oxygen pressure-variable adsorption separator of 99.5% or more purity is produced on the basis of product gas, which selects a kind of special dilute
The oxygen selective sorbent of native X-type zeolite, it is equilibrium adsorption type molecular sieve.Another Chinese patent CN103768891B is disclosed
A kind of to use two-stage two-stage series connection swing adsorption oxygen generating system and its operating method, the first order of the patent is equipped with Conventional zeolites
The oxygen nitrogen based on equilibrium selective adsorption mechanism of equal nitrogen absorbers separates pressure-variable adsorption separation system, and the second level is to select equipped with oxygen
The oxygen argon based on equilibrium adsorption mechanism of selecting property adsorbent separates pressure-variable adsorption separation system, and improves traditional two-stage and become
Adsorption system is pressed, an oxygen-containing rich argon tail gas recycling loop is set between the first order and second level pressure swing adsorption system.Above-mentioned two
A patent common feature is the oxygen rich gas containing argon that obtains from first order pressure swing adsorption system again through second level pressure swing adsorption system
Separation prepares high purity oxygen gas, and second level pressure swing adsorption system is all based on equilibrium selective and adsorbs rare earth loaded molecular sieve absorption
Agent.Due to low to the adsorptive selectivity of oxygen argon based on equilibrium adsorption, so that the two-stage pressure-variable adsorption system of this kind of high pure oxygen preparation
System the disadvantages of there are low separation efficiency and high energy consumptions, using being restricted, there are no relevant industry so far for disclosed technology
Using.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of transformation suctions that product oxygen purity and the rate of recovery can be improved
The attached device and method for preparing high-purity oxygen obtain the purity of oxygen product 99% or more by two-stage pressure swing adsorption system.
First order pressure swing adsorption system is that the primary oxygen enriched product containing argon is obtained based on equilibrium adsorption, and second level pressure swing adsorption system is
Based on the aerodynamic types adsorbent such as carbon molecular sieve, primary oxygen enriched product is further purified and obtains high pure oxygen product, and will obtained
Product oxygen carry out interim parsing, extract mid-term product gas as final products, purity is up to 99% or more.The second level becomes simultaneously
Product gas early period of adsorption system is pressed to utilize respectively as three-level and level-one purgative gas with rich argon tail gas recycle to first order transformation
Adsorption system is cleaned, the primary product gas of first order pressure swing adsorption system be also used as second level purgative gas to the first order adsorb into
Row cleaning, effectively increases the primary oxygen product gas concentration of first order pressure swing adsorption system generation, improves the oxygen of whole system
Gas recovery rate and reduction energy consumption.
The technical solution adopted in the present invention is as follows:
A kind of method that pressure-variable adsorption prepares high-purity oxygen, including two-stage pressure swing adsorption system, first order pressure-variable adsorption
Adsorbent of the system based on equilibrium adsorption mechanism separates nitrogen from pretreated compressed air, obtains primary oxygen and produces
Product gas, unstripped gas of the primary oxygen product gas as second level pressure swing adsorption system, by the power of second level pressure swing adsorption system
It learns selective absorbent and is separated off argon gas, obtain the high pure oxygen of product gas, wherein the rich argon of second level pressure swing adsorption system discharge
Level-one purgative gas of the tail gas recycle as first order pressure swing adsorption system, collection part first order pressure swing adsorption system obtain first
Second level purgative gas of the grade oxygen product gas as first order pressure swing adsorption system, effective nitrogen purge and reduction first order pressure-variable adsorption
Cleaning systems oxygen-containing gas dosage, collection part second level pressure swing adsorption system output early period product gas as first order transformation
The three-level purgative gas of adsorption system, three-level purgative gas sequentially clean first order pressure swing adsorption system, and three-level cleaning is effective
The primary oxygen product gas concentration for improving the generation of first order pressure swing adsorption system, improves the oxygen recovery rate and drop of whole system
Low energy consumption.
Further, the product gas that the second level pressure swing adsorption system obtains is divided into product gas early period, mid-term product
Gas and later product gas collect the high mid-term product gas of product purity as the high pure oxygen of final products gas, effectively improve final production
Product gas purity.And product gas early period is collected and is cleaned as three-level purgative gas to first order pressure swing adsorption system, is effectively improved
The concentration distribution of oxygen and reduction argon concentration in first order pressure swing adsorption system.
Further, product gas early period is 5%~25% production of second level pressure swing adsorption system initial stage output
Product gas, mid-term product gas are 75%~90% product gas of second level pressure swing adsorption system mid-term output, and later product gas is
5%~10% product gas of second level pressure swing adsorption system later period output.
Further, the adsorbent of the first order pressure swing adsorption system based on equilibrium adsorption mechanism includes but is not limited to
Two or more combination in 5A, 10X, 13X and LiLSX zeolite adsorbent；The second level pressure-variable adsorption
Adsorbent of the system based on kinetic selectivity includes but is not limited to carbon molecular sieve adsorbent.The absorption of the aerodynamic types such as carbon molecular sieve
Agent is significantly larger than silver or rare earth loaded zeolite adsorbent to the separation selectivity of oxygen argon, to the separating property of oxygen argon
Good, therefore, system effectiveness is high, and low energy consumption, can obtain very high oxygen recovery rate and oxygen purity.
Further, the operation of the first order pressure swing adsorption system and second level pressure swing adsorption system can relatively solely
It is former that second level pressure swing adsorption system has not yet been reached in the primary product gas oxygen content of first order pressure swing adsorption system output in vertical operation
When expecting gas purity requirement, second level pressure swing adsorption system can wouldn't be opened, effectively saving energy consumption.And reach primary for only requiring
The oxygen product that product gas oxygen content requires, the operation of first order pressure swing adsorption system can be completed, and do not need the operation second level and become
Press adsorption system.Implement the Discrete control of two-stage pressure swing adsorption system, flexible operation can be effectively compared with low energy consumption.
A kind of pressure-variable adsorption prepares the device of high-purity oxygen, which is characterized in that including two-stage pressure swing adsorption system, first
Grade pressure swing adsorption system loads the adsorbent based on equilibrium adsorption mechanism, and second level pressure swing adsorption system loads kinetic selectivity
Adsorbent, first order pressure swing adsorption system primary product gas outlet connection primary product gas storage tank, the connection of primary product gas storage tank
Second level pressure swing adsorption system unstripped gas entrance, while primary product gas storage tank is connected to first order pressure swing adsorption system and constitutes two
Grade detergent line；Second level pressure swing adsorption system product gas outlet is separately connected product gas storage tank early period, mid-term product gas storage tank
With later product gas discharge pipe, the second pressure swing adsorption system tail gas outlet connects tail gas storage tank, and tail gas storage tank is connected to the
Level-one pressure swing adsorption system constitutes level-one detergent line, and the product early period gas storage tank is connected to first order pressure swing adsorption system structure
At three-level detergent line；Autocontrol valve, autocontrol valve are both provided on two-stage pressure swing adsorption system, storage tank and pipeline
Connect PLC control system.
Further, the first order pressure swing adsorption system includes at least two adsorption towers, the second level transformation
Adsorption system includes at least two adsorption towers.
Further, the product early period gas storage tank collects the 5% of second level pressure swing adsorption system initial stage output
~25% product gas, mid-term product gas storage tank collect 75%~90% product of second level pressure swing adsorption system mid-term output
Gas, 5%~10% product gas of second level pressure swing adsorption system later period output are discharged as later product gas from discharge pipe
To outside device, tail gas storage tank receives the rich argon tail gas that pressure swing adsorption system adsorbing separation in the second level comes out.
Further, PLC control system independently connects the first order pressure swing adsorption system and second level transformation
Adsorption system enables two-stage pressure swing adsorption system is relatively independent to run.It is produced in the primary of first order pressure swing adsorption system output
When second level pressure swing adsorption system unstripped gas purity requirement has not yet been reached in product gas oxygen content, second level pressure-variable adsorption can wouldn't be opened
System, flexible operation can effectively save energy consumption.And reach the oxygen product of primary product gas oxygen content requirement for only requiring,
The operation of first order pressure swing adsorption system can be completed, and not need operation second level pressure swing adsorption system.Implement two-stage pressure-variable adsorption
The Discrete control of system, effectively compared with low energy consumption.
Compared with the prior art, the beneficial effects of the present invention are:
The present invention improves existing two-stage omnibus control system technology, by arranging second level pressure swing adsorption system
Level-one purgative gas of the rich argon tail gas as first order pressure swing adsorption system adsorption tower out reduces first order pressure swing adsorption system and obtains
The primary oxygen product gas obtained is used for the dosage of itself second level purgative gas, improves the oxygen recovery of first order pressure swing adsorption system
Rate, while the oxygen-containing relatively low product gas of the initial stage institute's output obtained after the pressure swing adsorption system separating-purifying of the second level being made
For the three-level purgative gas of the last wash phase of first order pressure swing adsorption system adsorption tower, improves first order pressure swing adsorption system and inhale
Oxygen concentration is distributed in attached tower, improves oxygen purity and the rate of recovery in first order pressure swing adsorption system adsorption tower.In addition, by
The high mid-term of the oxygen purity of second level pressure swing adsorption system produces gas stage resulting mid-term product gas as final products gas, further
The purity for improving oxygen ensure that the oxygen purity of final products gas 99.0% or even 99.7% or more.
The present invention extracts mid-term product gas and makees by carrying out initial stage, mid-term and later stage parsing separation to product gas
For final products gas, the oxygen purity of final products gas is effectively increased, and using product gas early period and rich argon tail gas as level-one
The three-level and level-one purgative gas of absorption improve the rate of recovery of oxygen product and reduce energy consumption.
Detailed description of the invention
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The some embodiments recorded in application, for those of ordinary skill in the art, without creative efforts,
It is also possible to obtain other drawings based on these drawings.
Fig. 1 is the flow chart for the method that pressure-variable adsorption of the present invention prepares high-purity oxygen；
Fig. 2 is the structural schematic diagram for the device that pressure-variable adsorption of the present invention prepares high-purity oxygen；
Fig. 3 is that the air separation by PSA of existing two-stage series connection prepares the structural schematic diagram of high purity oxygen gas device.
In figure: refer to that adsorption tower, the adsorption tower of first order pressure swing adsorption system are T1A and T1B with the symbol that T takes the lead, the
The adsorption tower of second level pressure swing adsorption system is T2A and T2B；Refer to that air accumulator or surge tank, G1 are primary produce with the symbol that G takes the lead
Product gas storage tank, G2 are product early period gas storage tank, and G3 is tail gas storage tank, and G4 is oxygen surge tank, and G5 is mid-term product gas storage tank；With
The symbol that V takes the lead refers to autocontrol valve, and it is all pre- that these valves can be pneumatically or electrically equal autocontrol valves, these valves
It first sets and opens or closes logic, control the flow direction of gas in pressure swing adsorption system, including V01-V24, in valve number
Number might not be continuous；Refer to that have a flow control regulatory function is automatically or manually controlled valve with the symbol that NV takes the lead,
It can carry out the aperture of manually or automatically control valve as the case may be, aperture can reach control gas flow from 0-100%
Purpose, including NV01-NV08；C01 is the oxygen compressor of second level pressure swing adsorption system.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only
It is only a part of the embodiment of the present invention, instead of all the embodiments.It is real to the description of at least one exemplary embodiment below
It is merely illustrative on border, never as to the present invention and its application or any restrictions used.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to exemplary embodiments of the present invention.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
Unless specifically stated otherwise, positioned opposite, the digital table of the component and step that otherwise illustrate in these embodiments
It is not limited the scope of the invention up to formula and numerical value.Simultaneously, it should be clear that for ease of description, each portion shown in attached drawing
The size divided not is to draw according to actual proportionate relationship.Technology known for person of ordinary skill in the relevant, side
Method and equipment may be not discussed in detail, but in the appropriate case, and the technology, method and apparatus should be considered as authorizing explanation
A part of book.In shown here and discussion all examples, appointing should be construed as merely illustratively to occurrence, and
Not by way of limitation.Therefore, the other examples of exemplary embodiment can have different values.It should also be noted that similar label
Similar terms are indicated in following attached drawing with letter, therefore, once it is defined in a certain Xiang Yi attached drawing, then subsequent attached
It does not need that it is further discussed in figure.
In the description of the present invention, it is to be understood that, the noun of locality such as " front, rear, top, and bottom, left and right ", " it is laterally, vertical,
Vertically, orientation or positional relationship indicated by level " and " top, bottom " etc. is normally based on orientation or position shown in the drawings and closes
System, is merely for convenience of description of the present invention and simplification of the description, in the absence of explanation to the contrary, these nouns of locality do not indicate that
It must have a particular orientation or be constructed and operated in a specific orientation with the device or element for implying signified, therefore cannot manage
Solution is limiting the scope of the invention: the noun of locality " inside and outside " refers to inside and outside the profile relative to each component itself.
For ease of description, spatially relative term can be used herein, as " ... on ", " ... top ",
" ... upper surface ", " above " etc., for describing such as a device shown in the figure or feature and other devices or spy
The spatial relation of sign.It should be understood that spatially relative term is intended to comprising the orientation in addition to device described in figure
Except different direction in use or operation.For example, being described as if the device in attached drawing is squeezed " in other devices
It will be positioned as " under other devices or construction after part or construction top " or the device of " on other devices or construction "
Side " or " under its device or construction ".Thus, exemplary term " ... top " may include " ... top " and
" in ... lower section " two kinds of orientation.The device can also be positioned with other different modes and (is rotated by 90 ° or in other orientation), and
And respective explanations are made to the opposite description in space used herein above.
In addition, it should be noted that, limiting components using the words such as " first ", " second ", it is only for be convenient for
Corresponding components are distinguished, do not have Stated otherwise such as, there is no particular meanings for above-mentioned word, therefore should not be understood as to this
The limitation of invention protection scope.
Embodiment 1
In order to improve the overall recovery of oxygen and improve product oxygen purity, the present invention is to existing two-stage series connection pressure-variable adsorption
Oxygenerating technology is improved, and a kind of device and method that pressure-variable adsorption prepares high-purity oxygen are proposed.
As shown in Figure 1, a kind of method that pressure-variable adsorption prepares high-purity oxygen includes two-stage pressure swing adsorption system, the first order
Adsorbent of the pressure swing adsorption system based on equilibrium adsorption mechanism separates nitrogen from pretreated compressed air, and first
The adsorbent based on equilibrium adsorption mechanism of grade pressure swing adsorption system includes but is not limited to 5A, 10X, 13X and LiLSX zeolite molecules
Two or more combination in sieve adsorbant.Nitrogen in air is adsorbed agent bed selective absorption, generates oxygen-containing argon
Primary product gas, mainly contain oxygen 90-95%, argon gas 4-5%, remaining be a small amount of nitrogen, first order pressure swing adsorption system
Oxygen recovery rate it is related with the oxygen purity of primary product gas with operating condition, generally between 40-60%；
Unstripped gas of the primary oxygen product gas as second level pressure swing adsorption system, by the dynamic of second level pressure swing adsorption system
Mechanics selective absorbent is separated off argon gas, and the adsorbent based on kinetic selectivity of second level pressure swing adsorption system includes
But it is not limited to carbon molecular sieve adsorbent, adsorption of oxygen rate is fast, so as to which the oxygen in primary product gas is separated with argon gas,
Oxygen purity in product gas is further increased, high pure oxygen product gas is obtained.The rich argon tail gas of second level pressure swing adsorption system discharge
Recycling, since wherein for oxygen content generally 80% or more, the level-one purgative gas as first order pressure swing adsorption system is first to reduce
Grade product gas is used for the dosage of second level purgative gas, while oxygen overall recovery is greatly improved, and oxygen always recycles
Rate can reach 25-35%, and the purity of oxygen can reach 99-99.8% in product.Collection part first order pressure swing adsorption system obtains
Second level purgative gas of the primary oxygen product gas obtained as first order pressure swing adsorption system, effective nitrogen purge, collection part second
Three-level purgative gas of the product gas as first order pressure swing adsorption system early period of grade pressure swing adsorption system output, three-level purgative gas are suitable
Secondary to clean to first order pressure-variable adsorption, the primary oxygen that three-level cleaning effectively increases the generation of first order pressure swing adsorption system produces
Product gas concentration improves the oxygen recovery rate of whole system and reduces energy consumption.
The product gas that second level pressure swing adsorption system obtains is divided into product gas early period, mid-term product gas and later product gas,
Product gas early period is 5%~25% product gas of second level pressure swing adsorption system initial stage output, and mid-term product gas is the second level
75%~90% product gas of pressure swing adsorption system mid-term output, later product gas are the production of second level pressure swing adsorption system later period
5%~10% product gas out.The high mid-term product gas of product purity is collected as final high pure oxygen product gas, early period product
Gas, which is collected, cleans first order pressure swing adsorption system as three-level purgative gas.The present invention is only second level pressure swing adsorption system
It produces the higher product gas of gas mid-term stage oxygen purity to collect as final products gas, this guarantees final products gas
Oxygen possesses very high-purity, and the present invention has also recycled second level pressure swing adsorption system and produced gas initial stage oxygen purity
Relatively low product gas early period finally cleans the first order absorption after the cleaning of primary product gas second level as three-level purgative gas
Tower bed although product gas oxygen purity early period is lower than final products gas, but still significant is higher than first order pressure swing adsorption system
The primary product gas of generation, therefore the oxygen argon concentration distribution in first order pressure swing adsorption system adsorption tower bed can be improved, it is bright
The primary product oxygen purity of first order pressure swing adsorption system is improved aobviously, and greatly shortens the available machine time, this will greatly be saved
Can, while correspondingly also improving the final products gas oxygen purity of second level pressure-variable adsorption.
The operation of first order pressure swing adsorption system and second level pressure swing adsorption system of the present invention relatively independent can be run,
It, can when second level adsorption system unstripped gas purity requirement has not yet been reached in the primary product gas oxygen content of first order adsorption system output
Second level pressure swing adsorption system wouldn't be opened, flexible operation can effectively save energy consumption.And reach primary product gas for only requiring
The oxygen product that oxygen content requires, the operation of first order pressure swing adsorption system can be completed, and not need operation second level pressure-variable adsorption
System.The Discrete control for implementing second level pressure swing adsorption system, effectively compared with low energy consumption.
As shown in Fig. 2, a kind of pressure-variable adsorption prepares the device of high-purity oxygen, including two-stage pressure swing adsorption system, this reality
Applying first order pressure swing adsorption system in example includes two adsorption towers T1A and T1B, and second level pressure swing adsorption system includes two absorption
Tower T2A and T2B.The process and structure of two-stage series connection pressure swing adsorption system shown in the drawings only designate two-stage transformation in figure
Two-stage adsorption tower, air accumulator and all valve locations and type of adsorption system, do not mark PLC control system and air pressure
The routine pressure-variable adsorption such as contracting machine, compressed air pretreatment system, muffler, pressure gauge, temperature measurer, oxygen analyser, counterbalance valve
The equipment or component of VS .NET Prerequisites, but this does not indicate that two-stage pressure swing adsorption system of the invention does not include these equipment or portion
Part.Label symbol in attached drawing is described as follows: referring to adsorption tower, the absorption of first order pressure swing adsorption system with the symbol that T takes the lead
Tower is T1A and T1B, and the adsorption tower of second level pressure swing adsorption system is T2A and T2B；Refer to air accumulator with the symbol that G takes the lead or delays
Tank is rushed, G1 is the storage tank of the primary product gas of first order pressure swing adsorption system output, and G2 is second level pressure swing adsorption system output
Relatively low product gas storage tank early period of oxygen content, G3 is the rich argon tail gas storage tank of second level pressure swing adsorption system discharge,
G4 is the oxygen surge tank of second level pressure swing adsorption system, and G5 is that the final products gas of second level pressure swing adsorption system output stores up
Tank；Refer to autocontrol valve with the symbol that V takes the lead, these valves can be pneumatically or electrically equal autocontrol valves, these valves
Door, which has all been preset, opens or closes logic, the flow direction of gas in control pressure-swing absorption apparatus system, including V01~V24, valve
Number in number might not be continuous；Refer to have the automatic or manual control of flow control regulatory function with the symbol that NV takes the lead
Valve processed, can carry out the aperture of manually or automatically control valve as the case may be, and aperture can reach control from 0-100%
The purpose of gas flow, these valves include NV01~NV08, and C01 is the oxygen compressor of second level pressure swing adsorption system.
The first order pressure-swing absorber T1A and T1B load the adsorbent based on equilibrium adsorption mechanism, are based on equilibrium adsorption mechanism
Adsorbent include but is not limited in 5A, 10X, 13X and LiLSX zeolite adsorbent two or more combination,
The adsorption tower T2A and T2B of second level pressure swing adsorption system load kinetic selectivity adsorbent, the suction based on kinetic selectivity
Attached dose includes but is not limited to carbon molecular sieve adsorbent.First order pressure swing adsorption system primary product gas outlet connection primary product gas
Storage tank G1, primary product gas storage tank G1 connection second level pressure swing adsorption system unstripped gas entrance, while primary product gas storage tank G1
It is connected to first order pressure swing adsorption system and constitutes second level detergent line；Second level pressure swing adsorption system product gas outlet is separately connected
Early period product gas storage tank G2, mid-term product gas storage tank G5 and later product gas discharge pipe, second level pressure swing adsorption system tail gas
Outlet connects tail gas storage tank G3, and tail gas storage tank G3 collects the rich argon tail gas that pressure swing adsorption system adsorbing separation in the second level comes out,
Tail gas storage tank G3 is connected to first order pressure swing adsorption system and constitutes level-one detergent line, and the product early period gas storage tank G2 collects the
5%~25% product gas of second level pressure swing adsorption system initial stage output is connected to first order pressure swing adsorption system and constitutes three-level
Detergent line；Mid-term product gas storage tank G5 is collected in the pressure swing adsorption system of the second level by oxygen compressor C01 and oxygen surge tank G4
75%~90% product gas of phase output as final products gas, second level pressure swing adsorption system later product gas 5%~
10% is emitted into outside device from discharge pipe.Be both provided on two-stage adsorption system, storage tank and pipeline autocontrol valve V01~
V24 and NV01~NV08, autocontrol valve connect PLC control system.
PLC control system independently connects first order pressure swing adsorption system and second level pressure swing adsorption system, makes two-stage
Pressure swing adsorption system relatively independent can be run.It is not yet reached in the primary product gas oxygen content of first order pressure swing adsorption system output
To when the pressure swing adsorption system unstripped gas purity requirement of the second level, second level pressure swing adsorption system can wouldn't be opened, flexible operation has
Effect saves energy consumption.And reach the oxygen product of primary product gas oxygen content requirement, first order pressure swing adsorption system for only requiring
Operation can be completed, and not need operation second level pressure swing adsorption system.Implement the Discrete control of two-stage pressure swing adsorption system, effectively
Compared with low energy consumption.
Existing two-stage series connection swing adsorption oxygen generating system, flow chart and system structure diagram are as shown in figure 3, first
Grade pressure swing adsorption system includes two duplicate adsorption towers, and the bed of each adsorption tower is mainly equipped with based on equilibrium adsorption machine
Reason carrys out the adsorbent of separating oxygen and nitrogen, and adsorbent is conventional zeolite molecular sieve, and Preferential adsorption nitrogen, Nitrogen adsorption capacity is big, oxygen argon
Adsorption capacity it is relatively small, the discharge of first order pressure swing adsorption system tower bottom is rich nitrogen exhaust gas, and main oxygen-containing argon is discharged in tower top
Primary oxygen product.Two adsorption towers of first order pressure swing adsorption system are successively all by absorption, production gas, pressure, pressure release, blowback
Etc. different circulation steps, the resulting primary oxygen product gas of the first order is transported to second level pressure swing adsorption system further to separate
Oxygen argon obtains the oxygen product of higher purity.Second level pressure swing adsorption system also includes two identical adsorption towers, each
Based on selection of kinetics adsorption mechanism come the adsorbent of separation of oxygen and argon, adsorbent is modified carbon molecules for the bed filling of adsorption tower
The adsorbents such as sieve, oxygen is fast in the adsorbent bed rate of adsorption, and argon absorption rate is slow, from first order pressure swing adsorption system stream
Primary oxygen out enters adsorption bed by the absorption tower bottom in the pressure swing adsorption system of the second level, and oxygen is quickly inhaled by bed
Attached, the exhaust gas rich in argon gas is discharged from the tower top of adsorption tower, and the final oxygen product gas of high-purity is discharged from tower bottom.Second level transformation
The circulation step of absorption includes pressurization, absorption, pressure, pressure release, purging etc..
In contrast to the prior art, apparatus of the present invention increase tail gas storage tank G3 and early period in the pressure swing adsorption system of the second level
Product gas storage tank G2, and using two storage tanks as the detergent line of gas source two first order pressure swing adsorption systems of increase, constitute first
The three-level cleaning of grade pressure swing adsorption system, is divided into different oxygen purgative gas and sequentially carries out clearly to first order pressure swing adsorption system
It washes.Tail gas storage tank G3 collects the rich argon tail gas of second level pressure swing adsorption system absorption column overhead, since wherein oxygen content generally exists
80% or more, it can be used as the prerinse gas of first order tower, oxygen can be improved in the dosage as purgative gas to reduce primary product gas
The overall recovery of gas；Oxygen when product gas storage tank G2 early period collects the production gas initial stage of second level pressure swing adsorption system adsorption tower tower bottom
Product gas early period when purity is relatively low retains and produces gas stage hyperoxic mid-term product gas as final products, improves
The purity of final oxygen product, while the early period product gas oxygen purity that product gas storage tank G2 early period is collected is higher than first order transformation
Adsorb the primary product gas of output, early period last purgative gas of the product gas as first order pressure swing adsorption system adsorption tower, due to
Oxygen purity is high, can improve the concentration distribution of oxygen in first order pressure swing adsorption system adsorption tower bed and reduce bed argon
Gas concentration can correspondingly improve the oxygen purity of the primary oxygen product of first order pressure swing adsorption system, and first order pressure-variable adsorption again
The oxygen recovery rate of system is related with the oxygen purity of primary product gas with operating condition, so that total oxygen of whole system
The rate of recovery is greatly improved, and reaches 25-35%, the purity of oxygen can reach 99-99.8% in final products gas.
After above-mentioned improvement, two-stage series connection High Purity Oxygen Production System by PSA disclosed by the invention, first order transformation is inhaled
The adsorption tower of attached system loads the adsorbents based on equilibrium adsorption mechanism such as zeolite molecular sieve, and the nitrogen in air is selected by bed
Property absorption, generate the primary product gas of oxygen-containing argon, mainly contain oxygen 90-95%, argon gas 4-5%, remaining is a small amount of nitrogen, the
The oxygen recovery rate of level-one pressure swing adsorption system is related with the oxygen purity of primary product gas with operating condition, generally in 40-
Between 60%；The kinetic selectivities adsorbents such as the modified carbon molecular sieve of the adsorption tower filling of second level pressure swing adsorption system,
Adsorption of oxygen rate is fast, so as to which the oxygen in primary product is separated with argon gas, further increases oxygen purity in product, by
In the suction for exhaust gas in the adsorption tower of second level pressure swing adsorption system and the lower product gas of some oxygen content being recovered to the first order
In attached tower, so that oxygen overall recovery is greatly improved, oxygen overall recovery can reach 25-35%, oxygen in product
Purity can reach 99-99.8%.
The present invention is that the two-stage series connection pressure-variable adsorption system based on equilibrium selective absorption and kinetic selectivity absorption is high-purity
Oxygen system, the first order and second level pressure swing adsorption system are respectively according to respective program circular flow, in whole system stable operation
Afterwards, two-stage pressure swing adsorption system operating procedure is run according to following loop cycle.
(1) operating procedure of first order pressure swing adsorption system
After air is compressed to certain pressure by air compressor machine, enter after the pre-treatment steps such as cold dry, multistage filtering and oil removing
Pressure-swing absorber T1A and T1B of the first order equipped with zeolite molecular sieve, two adsorption towers T1A and T1B are passed through according to out-phase sequence respectively
It crosses by pressurising, absorption, reverse emptying, reverse cleaning and after cycle period that the multi-steps such as pressure are constituted, the nitrogen in air is just
It is basically separated away and obtains primary product gas, oxygen-containing 90-95%, containing argon 4~5% and a small amount of nitrogen.Primary product gas will
The oxygen of higher purity is prepared through the further adsorbing separation of second level pressure swing adsorption system.The operating condition of two adsorption towers,
The operating procedures such as the open and close sequence of each valve are described in detail in table 1 below, unless stated otherwise, are taken the lead with V word each
The default conditions of automatic control switch valve are in off state, the control valve regulation with flow regulating function taken the lead with NV
In preferred aperture.
Main operational steps and operating condition in 1 first order pressure swing adsorption system cycle period of table
Above-mentioned 10 circulation steps are a cycle of operation, and step can be achieved with air oxygen nitrogen in the above-mentioned period of reruning
It separates and obtains primary oxygen product gas.First order pressure swing adsorption system as shown in Figure 2, the oxygen content of primary product gas is in 90-
95%.
(2) operating procedure of second level pressure swing adsorption system
The primary product gas that first order pressure swing adsorption system generates is collected in air accumulator G1, will enter the as unstripped gas
Second level pressure swing adsorption system, second level pressure swing adsorption system are based on selection of kinetics absorption principle to first order pressure swing adsorption system
Primary product in oxygen argon further separated, the final oxygen product of 99-99.8% high-purity can be obtained, collection is being stored up
In gas tank G5, oxygen compressor C01 remains operational state, and as needed, reusable oxygen compressor C01 is forced into required pressure.It removes
Non-specifically illustrate, the default conditions for each automatic control switch valve taken the lead with V word are in off state, and have stream with what NV took the lead
The control valve of adjustment regulates and controls in preferred aperture.The operating procedure of second level pressure swing adsorption system is as shown in table 2
Main operational steps and operating condition in 2 second level pressure swing adsorption system cycle period of table
10 steps constitute the period of second level pressure swing adsorption system in table 2, as shown in Fig. 2, following according to the above-mentioned period
Ring operation achieves that oxygen argon separate, the primary product gas of first order pressure swing adsorption system can be further purified to 99% with
On, when the purity is high of oxygen, oxygen recovery rate is lower, and turns down oxygen purity, can increase the overall recovery of oxygen.
3 specific embodiments are concrete operations experiments of the invention below.
Embodiment 1
As shown in Fig. 2, two adsorption towers T1A and T1B of first order pressure swing adsorption system are loaded respectively, same certain is domestic
Each 300kg of the zeolite adsorbent of brand, two adsorption towers T2A and T2B of second level pressure swing adsorption system are loaded respectively
Each 40kg of carbon molecular sieve adsorbent of certain same domestic brand.Air compressor machine compresses air to gauge pressure 0.5MPa, two-stage transformation
Adsorption system presses the operation of cycle step described in Tables 1 and 2 respectively.Only in the second level pressure swing adsorption system operation cycle
1 and 6 steps (being shown in Table 2) skip over or the time is set as 0 second.The rich argon tail of 3rd and 8 steps (being shown in Table 2) in the second level pressure-variable adsorption period
Gas acquisition time is all 8 seconds.In this way, first order pressure-variable adsorption purge gas does not just include the gas from G2.First order transformation
The yield of the primary product gas of adsorption system output is 16.4m3/h, oxygen purity 94.1%, first order pressure swing adsorption system
Oxygen recovery rate is 41.4%, and the yield of the final products gas of second level pressure swing adsorption system output is 9.6m3/h, oxygen purity
It is 99.1%, second level pressure swing adsorption system oxygen recovery rate is 59.6%, and total oxygen recovery rate is 24.7%.
Embodiment 2
As shown in Fig. 2, two adsorption towers T1A and T1B of first order pressure swing adsorption system are loaded respectively, same certain is domestic
Each 300kg of the zeolite adsorbent of brand, two adsorption towers T2A and T2B of second level pressure swing adsorption system are loaded respectively
Each 40kg of carbon molecular sieve adsorbent of certain same domestic brand.Air compressor machine compresses air to gauge pressure 0.5MPa, two-stage transformation
Adsorption system presses the operation of cycle step described in Tables 1 and 2 respectively, in the pressure-variable adsorption period of second level pressure swing adsorption system
It is all 2 seconds that the initial production gas stage of 1st and 6 steps (being shown in Table 2), which flows into air accumulator G2 acquisition time, second level pressure swing adsorption system
The rich argon exhaust collection time of the 3rd and 8 steps (being shown in Table 2) is all 8 seconds in the pressure-variable adsorption period.First order pressure swing adsorption system output
The yield of primary product gas be 17.8m3/h, oxygen purity 94.7%, first order pressure swing adsorption system oxygen recovery rate is
43.7%, the yield of second level pressure swing adsorption system final products gas is 10.2m3/h, and oxygen purity 99.5%, the second level becomes
Pressing adsorption system oxygen recovery rate is 60.2%, and total oxygen recovery rate is 26.3%.
Embodiment 3
Compared with Example 2, the step and operating method in the present embodiment, in addition to the transformation of second level pressure swing adsorption system
The initial production gas stage of the 1st and 6 steps (being shown in Table 2) flows into air accumulator G2 acquisition time and shorten to 1 second, and second in adsorption cycle
The rich argon exhaust collection time of the 3rd and 8 steps (being shown in Table 2) is all 6 seconds outer in the pressure-variable adsorption period of grade pressure swing adsorption system, remaining
Step is same as Example 2.The yield of the primary product gas of first order pressure swing adsorption system output is 16.4m3/h, oxygen purity
It is 94.3%, the oxygen recovery rate of first order pressure swing adsorption system is 40.1%, second level pressure swing adsorption system final products gas
Yield be 11.3m3/h, oxygen purity 99.0%, the oxygen recovery rate of second level pressure swing adsorption system is 72.3%, total oxygen
Gas recovery rate is 29.0%.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of method that pressure-variable adsorption prepares high-purity oxygen, which is characterized in that including two-stage pressure swing adsorption system, the first order
Adsorbent of the pressure swing adsorption system based on equilibrium adsorption mechanism separates nitrogen from pretreated compressed air, obtains
Primary oxygen product gas, unstripped gas of the primary oxygen product gas as second level pressure swing adsorption system, by second level pressure-variable adsorption system
The separating-purifying of the kinetic selectivity adsorbent of system obtains the high pure oxygen of product gas, wherein the discharge of second level pressure swing adsorption system
Level-one purgative gas of the rich argon tail gas recycle as first order pressure swing adsorption system, collection part first order pressure swing adsorption system obtains
Second level purgative gas of the primary oxygen product gas obtained as first order pressure swing adsorption system, collection part second level pressure swing adsorption system
Three-level purgative gas of the product gas as first order pressure swing adsorption system early period of output, three-level purgative gas is sequentially to first order transformation
Adsorption system is cleaned.
2. the method that a kind of pressure-variable adsorption according to claim 1 prepares high-purity oxygen, which is characterized in that described
The product gas that second level pressure swing adsorption system obtains is divided into product gas early period, mid-term product gas and later product gas, collects mid-term and produces
Product gas is as final high pure oxygen product gas.
3. the method that a kind of pressure-variable adsorption according to claim 2 prepares high-purity oxygen, which is characterized in that the early period
Product gas is 5%~25% product gas of second level pressure swing adsorption system initial stage output, and mid-term product gas is second level transformation
75%~90% product gas of adsorption system mid-term output, later product gas are second level pressure swing adsorption system later period output
5%~10% product gas.
4. the method that a kind of pressure-variable adsorption according to claim 1 prepares high-purity oxygen, which is characterized in that described
Adsorbent of the level-one pressure swing adsorption system based on equilibrium adsorption mechanism includes but is not limited to 5A, 10X, 13X and LiLSX zeolite molecules
Two or more combination in sieve adsorbant.
5. the method that a kind of pressure-variable adsorption according to claim 1 prepares high-purity oxygen, which is characterized in that described
Adsorbent of the second level pressure swing adsorption system based on kinetic selectivity includes but is not limited to carbon molecular sieve adsorbent.
6. a kind of method that pressure-variable adsorption prepares high-purity oxygen, feature described in -5 any one exist according to claim 1
In the operation of the first order pressure swing adsorption system and second level pressure swing adsorption system relatively independent can be run.
7. the device that a kind of pressure-variable adsorption prepares high-purity oxygen, which is characterized in that including two-stage pressure swing adsorption system, the first order
Pressure swing adsorption system loads the adsorbent based on equilibrium adsorption mechanism, and second level pressure swing adsorption system loads kinetic selectivity and inhales
Attached dose, first order pressure swing adsorption system primary product gas outlet connection primary product gas storage tank, primary product gas storage tank connection the
Second level pressure swing adsorption system unstripped gas entrance, while primary product gas storage tank is connected to first order pressure swing adsorption system and constitutes second level
Detergent line；Second level pressure swing adsorption system product gas outlet be separately connected product gas storage tank early period, mid-term product gas storage tank and
Later product gas discharge pipe, the second pressure swing adsorption system tail gas outlet connect tail gas storage tank, and tail gas storage tank is connected to first
Grade pressure swing adsorption system constitutes level-one detergent line, and the product early period gas storage tank is connected to first order pressure swing adsorption system composition
Three-level detergent line；Program-controlled valve is both provided on two-stage pressure swing adsorption system, storage tank and pipeline.
8. the device that a kind of pressure-variable adsorption according to claim 7 prepares high-purity oxygen, which is characterized in that described
Level-one pressure swing adsorption system includes at least two adsorption towers, and the second level pressure swing adsorption system includes at least two absorption
Tower.
9. the device that a kind of pressure-variable adsorption according to claim 7 prepares high-purity oxygen, which is characterized in that before described
Phase product gas storage tank collects 5%~25% product gas of second level pressure swing adsorption system initial stage output, mid-term product gas storage tank
Collect 75%~90% product gas of second level pressure swing adsorption system mid-term output, second level pressure swing adsorption system later period output
5%~10% product gas be emitted into outside device as later product gas from discharge pipe, tail gas storage tank receive the second level become
The rich argon tail gas for pressing adsorption system adsorbing separation to come out.
10. a kind of space division according to any one of claim 7-9 prepares the device of high-purity oxygen, feature exists
In PLC control system independently connects the first order pressure swing adsorption system and second level pressure swing adsorption system, makes two-stage
Pressure swing adsorption system relatively independent can be run.
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Inventor after: Shi Junxiong Inventor after: Pan Guangtong Inventor after: Liu Jinzhong Inventor after: Li Anwu Inventor after: Li Pan Inventor before: Shi Junxiong Inventor before: Pan Guangtong Inventor before: Li Anwu Inventor before: Li Pan |
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