CN214780753U - Device for preparing high-purity oxygen based on coupling separation technology - Google Patents

Device for preparing high-purity oxygen based on coupling separation technology Download PDF

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CN214780753U
CN214780753U CN202120430845.XU CN202120430845U CN214780753U CN 214780753 U CN214780753 U CN 214780753U CN 202120430845 U CN202120430845 U CN 202120430845U CN 214780753 U CN214780753 U CN 214780753U
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zeolite membrane
gas
membrane separator
oxygen
separation
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陈奕璇
罗二平
罗鹏
李新
申广浩
王晨
顾修筑
谢东红
贾吉来
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Suishan Ningbo Technology Co ltd
SHANGHAI SUISHAN INDUSTRIAL CO LTD
Air Force Medical University of PLA
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Suishan Ningbo Technology Co ltd
SHANGHAI SUISHAN INDUSTRIAL CO LTD
Air Force Medical University of PLA
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Abstract

The utility model belongs to the technical field of gas separation, specifically be a device based on high-purity oxygen is prepared to coupling separation technique. The utility model couples the pressure swing adsorption drying technology with the zeolite membrane separation technology, namely the oxygen production process comprises a preceding stage pressure swing adsorption drying process and a later stage zeolite membrane separation process. Wherein, the pressure swing adsorption drying technology adopts an adsorption tower to remove moisture in the air and compresses the air; the zeolite membrane separation technology is to adopt a zeolite membrane separator to carry out oxygen and nitrogen separation and oxygen and argon separation, remove nitrogen and argon from dry compressed air with moisture removed from an adsorption drying bed layer, and obtain high-purity oxygen with purity of 90 percent and even more than 99.5 percent; wherein a part of the waste gas generated in the zeolite membrane separation process flows back to the preceding stage pressure swing adsorption drying process to be used as the cleaning gas in the regeneration stage. The utility model discloses can obviously reduce system tolerance and consume, improve the whole rate of recovery of system.

Description

Device for preparing high-purity oxygen based on coupling separation technology
Technical Field
The utility model belongs to the technical field of gas separation, concretely relates to prepare device of high-purity oxygen from the air, adopt this device separable purity to reach the oxygen more than 90% 99.5% even.
Background
Pressure Swing Adsorption (PSA) is an important and widely used gas separation method, such as pressure swing adsorption drying, pressure swing adsorption oxygen production, nitrogen production, etc., wherein adsorption drying is usually used to remove moisture contained in compressed air to obtain dry compressed air with a low dew point.
Conventional PSA processes for producing oxygen from an air stream typically produce oxygen based on equilibrium adsorption theory using nitrogen adsorbents such as CaA, CaX, NaX, LiX types, but even if all nitrogen in the air is adsorbed, it is difficult to produce product oxygen at a concentration greater than 95%, with the product gas containing about 5% argon. Therefore, in order to obtain high-purity oxygen, based on the adsorption method, people have to adopt a more complicated multistage pressure swing adsorption system, and domestic patent CN1226142A discloses a pressure swing adsorption method for obtaining 98.4% purity by multistage pressure swing adsorption, which uses zeolite nitrogen adsorbent to remove a large amount of nitrogen, and uses carbon molecular sieve based on kinetic separation characteristic to realize the separation of oxygen and argon, although the separation process is realized by single power equipment, the purity still can not meet the requirement of more than 99.5%, and the 15% oxygen recovery rate greatly limits the application.
The membrane separation technology is a high and new technology developed in the middle of 20 th century, in the industrial practice applied to the aspect of purifying oxygen, so far, a representative organic membrane separation material which can be applied to air separation has an alpha (alpha) value of 2-7 mostly for separating oxygen and nitrogen, and a selectivity of oxygen and argon separation of no more than 3.5 mostly, and is less common for separation materials having oxygen and nitrogen and oxygen and argon separation characteristics, wherein alpha is the selectivity of so-called oxygen and nitrogen or oxygen and argon, namely the ratio of permeation quantities of the membrane separation material to oxygen/nitrogen and oxygen/argon, simulation process calculation shows that the membrane separation material with the selectivity of about 7 can directly obtain oxygen with the purity of about 60% or less from air, and a system adopting a multi-stage membrane separation process can obtain oxygen with the purity of even more than 90%, for example, U.S. patent 656259 discloses a method and a system for separating a pure component gas from a gaseous mixture, pure oxygen (purity 60-90%) can be obtained efficiently from ambient air, providing a system and method that uses at least three permeators, but does not require a compressor for each stage, although the energy requirements are reduced for membrane separation systems, it is clear that the system is complex and, in particular, the separation efficiency is so low that it cannot be used industrially as compared to the pressure swing adsorption process for oxygen production.
There are also methods for producing 99% pure oxygen by using an organic membrane separation technology, such as a Continuous Membrane Column (CMC), and various methods for purifying oxygen by using 95% oxygen generated by PSA as a raw material and using a general organic membrane separation method or a Continuous Membrane Column (CMC), especially a membrane recycling separation system with 4 outlet membrane modules, which can produce oxygen with a purity of 99% or more, but the extra compression power of the separation system is very high in energy consumption, and the special membrane separator required by CMC recycling is very expensive, which restricts its industrial application. The membrane separator has been commercialized to have a separation system having a selectivity of oxygen-argon separation of not more than 3.5, and the separation efficiency thereof is difficult to be applied to, for example, purification of high purity oxygen of 99% or more. In addition, the adoption of the organic hollow fiber membrane has no industrial application value because of excessive energy consumption.
Meanwhile, along with the coupling of the process system, a larger number of control valves and storage tanks required for recovering the intermediate process gas and the like are needed, so that the complexity of the equipment is greatly increased, the volume of the equipment is also greatly increased, and the failure rate of the equipment is excellent and prominent due to the complexity of the process system.
Disclosure of Invention
In view of above circumstances, to obtaining 90% or even the high-purity oxygen that the purity is up to more than 99.5% with empty technical means of dividing of non-cryrogenic, the utility model provides a prepare high-purity oxygen's device from the air, high-purity oxygen is the oxygen that the purity reaches 90% or even reaches more than 99.5%.
The utility model provides a prepare device of high-purity oxygen from air is with pressure swing adsorption drying technique and zeolite membrane separation technique coupled mutually, and the process of making oxygen promptly includes preceding stage pressure swing adsorption drying process and secondary zeolite membrane separation process. Wherein:
the pressure swing adsorption drying technology is like the conventional technology, and adopts an adsorption drying bed layer to remove moisture in air and compress, so that the consumption of compressed air is saved by using waste gas in the primary membrane separation process as cleaning gas in order to ensure that the subsequent zeolite membrane separation material is not polluted and reduce the gas consumption of a system, and the overall recovery rate of the system is improved.
The zeolite membrane separation technology is to adopt a zeolite membrane separator to separate oxygen and nitrogen and oxygen and argon, and remove nitrogen and argon from dry compressed air with moisture removed from an adsorption drying bed layer, so as to obtain high-purity oxygen with purity of 90 percent or even more than 99.5 percent, instead of adopting multi-stage pressure swing adsorption, a known organic membrane separator or a multi-stage organic membrane separation process to obtain the high-purity oxygen.
And, in the utility model discloses in, at least partly backward flow the preceding stage pressure swing adsorption drying process with the waste gas that zeolite membrane separation process produced, as the purge gas of regeneration stage.
Also, in the present invention, if higher purity oxygen is required, at least a portion of the gas produced by the secondary membrane separation process may be vented out of the system.
Based on the above principle, the utility model provides a device based on high-purity oxygen is prepared to coupling separation technique, include:
(1) at least one compression device providing the necessary pressurized feed air, including the equipment required for air pre-treatment (not shown in the drawings);
(2) at least one set of pressure swing adsorption drying device in the known technology comprises at least one adsorption tower, wherein one or more combinations of molecular sieves for adsorbing water, such as activated alumina, 13X, silica gel and the like, as well as an air inlet valve and necessary connecting pipelines thereof, an air exhaust valve and necessary connecting pipelines thereof, and an air production valve and necessary connecting pipelines thereof are arranged in the adsorption tower;
(3) at least one zeolite membrane separator, wherein the zeolite membrane separator is filled with a zeolite membrane separation material and is coupled in the adsorption drying separation system; each zeolite membrane separator has three ports: the device comprises a raw gas interface, a permeate gas outlet and a retentate gas outlet, wherein the raw gas interface is connected in series with a product end of a pressure swing adsorption drying device, the permeate gas outlet is connected in series with a control valve at a product end of an adsorption separator, and the retentate gas outlet is communicated with a product end of another group of adsorption drying towers and is used as a regeneration cleaning gas of the towers;
(4) at least one secondary zeolite membrane separator is connected in series after the product end control valve of the coupling separator, and the permeation gas outlet of the secondary zeolite membrane separator is connected to a product gas buffer tank through a control valve with adjustable flow;
(5) at least one product gas buffer tank in communication with the permeate gas outlet end of the secondary zeolite membrane separator for receiving the permeate fraction enriched from the zeolite membrane separator;
(6) a complete set of control components for the necessary operational control of the valves on the circuit and the necessary control of the compression equipment.
Typically, a device for producing high purity oxygen based on coupled separation technology is shown in FIG. 2; in fig. 2, 01A, 02A, 03A, 01B, 02B, 03B represent automatic control valves which can be opened or closed according to a preset logic, and of course, can be automatic control valves with flow control regulation performance, and the valves can be pneumatic control valves, electric control valves and hydraulic control valves; drying A and drying B which are serial numbers of the adsorption towers and are filled with adsorbents; PV102 represents a surge tank; m01 represents a zeolite membrane separator, M01A, M01B, M01C represent different zeolite membrane separators.
In fig. 2, there are two adsorption columns: dry a, dry B, the corresponding zeolite membrane separator also has two: M01A, M01B; automatic control valves are respectively arranged between the raw gas pipeline and the air inlets of the drying A and the drying B: 01A, 01B; the air inlet pipeline of drying A and drying B is provided with a bypass after being positioned on the automatic control valves 01A and 01B and is connected to the silencer, and the automatic control valves are correspondingly arranged on the two bypasses: 02A, 02B; the air outlets of the drying A and the drying B are respectively connected with the raw material gas side ports of M01A and M01B to form two parallel drying and separating systems; the stagnant gas side connectors of the two zeolite membrane separators M01A and M01B are connected through a pipeline, and a trap valve V0 is arranged on the connecting pipeline; the permeation gas side ports of the two zeolite membrane separators M01A and M01B are respectively connected with a secondary zeolite membrane separator M01C through a pipeline; the back of the secondary zeolite membrane separator M01C is connected with a buffer tank PV 102; automatic control valves 03A and 03B are correspondingly arranged on connecting pipelines of permeation gas side ports of the two zeolite membrane separators M01A and M01B and the secondary zeolite membrane separator M01C; and a control valve 4A is arranged on a connecting pipeline of the secondary zeolite membrane separator M01C and the buffer tank PV 102.
The above is only an example: two parallel dry separation systems. Furthermore, the adsorption tower and the zeolite membrane separator can be coupled in parallel by more paths; in each path, a plurality of zeolite membrane separators can be connected in series; and a plurality of subsequent zeolite membrane separators of the stage can be connected in series.
In the above apparatus for producing high-purity oxygen based on the coupling separation technique, a standard operation sequence is as follows:
1. opening 01A and 03A, drying A for work, and adsorbing; at the moment, 02B is opened, the drying B is emptied and regenerated, meanwhile, 4A of the separation part of the later stage zeolite membrane is opened, the yield is adjusted, and oxygen can be produced, and when the adsorption of the adsorption drying A is saturated, the next step is carried out;
2. opening 01B and 03B, drying B for work, and adsorbing; at the moment, 02A is opened, the dried A is emptied and regenerated, at the same time, 4A of the separation part of the later stage zeolite membrane is opened, the yield is adjusted to produce oxygen, and when the adsorption of the adsorption dried B is saturated, the previous step is carried out.
In the above steps, except for the appointed opening of the valve, all the other valves are in a closed state, the oxygen flow can be controlled by adjusting 4A, and the flow of quantitative cleaning can be controlled by adjusting the shutoff valve.
According to the steps, after the adsorption of the drying A is saturated, the fluid is controlled to enter the adsorption tower B for continuously producing oxygen by switching the symmetrical fluid control valve, the drying A is regenerated, and the steps are repeated in such a circulating way, so that the oxygen with the purity of 90 percent and even more than 99.5 percent can be produced.
The above device of the utility model does not exclude the use of a plurality of zeolite membrane separators to separate, and the technical personnel of this specialty can know, can adopt more multistage membrane separator to separate the more high-purity infiltration gas component even. Even if the pressure of the feed gas is insufficient, an additional feed gas compression device (not shown) may be used to feed the feed gas to the zeolite membrane separator, and the compressor described in the drawing may be used to feed the gas to the zeolite membrane separator in further stages simply by providing the necessary additional piping and switching valves.
The product gas buffer vessel, such as described in the known art, may be filled with the necessary packing to achieve a more economical buffer volume.
The zeolite membrane separators are coupled in the adsorption drying system, the systems in which the plurality of zeolite membrane separators operate can be not communicated with each other, namely, the systems can be in parallel and in multiple groups, namely, gas transfer among the zeolite membrane separators is not generated when the plurality of zeolite membrane separators operate according to the steps. Because there are no more process intermediate gas surge tanks associated with it, multiple zeolite membrane separator systems can achieve higher recovery without the use of membrane separator interactions. This can obviously reduce the size of the equipment and reduce the occupied area of the equipment.
Necessary gas detection equipment can be arranged at the inlet and outlet ends of the zeolite membrane separator, and necessary pressure detection equipment, dew point detection equipment and purity detection equipment are arranged on the zeolite membrane separator and the buffer tank, so that a system which runs according to the required pressure and purity completely is formed, and an intelligent control program is used for controlling the system. The method is not difficult to realize in the technical field, and experienced technicians know that the debugging process of the equipment is almost the process from system self-adaptation to stability, and in the fault judgment, a control program gives more sufficient information to maintenance and repair personnel and even directly specifies a fault point.
In the device described above, various changes may be made without departing from the scope of the invention. Thus, although it is preferred that 1 or more zeolite membrane separators, either of fixed volume or fixed pressure, be used in conjunction with a preceding adsorption drying system and the subsequent 1 or more stages form a complete coupled separation system with the product gas surge tank and necessary power equipment.
Furthermore, the gas flow pattern through the zeolite membrane separator of the present invention may be axial flow, radial flow, lateral flow or other patterns.
For a single zeolite membrane separator, multiple primary membrane separation layers are included, or one or more pretreatment layers may be absent or provided, to remove other components (non-oxygen moieties, such as water vapor). In addition, each membrane separation layer may comprise a single species of membrane separation material or a mixture of two or more membrane separation materials.
The utility model discloses can be used for separating out the gas that is adsorbed easily from the gas of difficult absorption/seeing through with an adsorbent, easily adsorb/see through the component, perhaps difficult absorption/see through the component, all can regard as required product gas alone or simultaneously. The utility model discloses the priority is applied to the PSA process based on balanced adsorption theory rather than dynamics separation theory, nevertheless does not get rid of the PSA process based on dynamics separation theory and can adopt the utility model discloses in order to realize the utility model discloses the purpose. The basic principles disclosed can be applied to many other separation applications. Through the utility model discloses, can realize that the typical example of separation includes:
by selective penetration of N2To recover N from air2
By selective permeation of O2To recover O from air2
Enriching CO from the gasified coal with a CO-permselective zeolite membrane material;
by selective permeation of CO2The zeolite membrane material is used for removing CO from gasified coal2
Realization of CO2/CH4Separation of, CO2/N2Separation of (A) from (B), H2/N2Separation of olefins/alkanes, etc.
From containing O2Separation of O from a gas mixture of Ar (e.g. obtained by separation of air by pressure swing adsorption coupled membrane separation)2Or Ar;
any combination of one or more suitable adsorbent-zeolite membrane materials may also be used for separation, for example, CaA zeolite, LiX zeolite, or any other specific separation material to recover oxygen or nitrogen; gases that are difficult to adsorb/permeate are enriched from the non-feed end while components that are more readily selectively adsorbed/permeate are enriched from the other end.
The utility model discloses in, the product gas of saying indicates the difficult gas that is adsorbed by the adsorbent, if to the nitrogen adsorbent, nitrogen gas is adsorbed more easily, and oxygen, argon gas then are difficult to adsorb.
In the present invention, the waste gas refers to gas that is relatively easily adsorbed by the adsorbent, such as nitrogen, moisture, etc., which is relatively easily adsorbed by the nitrogen adsorbent.
The present invention relates to an oxygen generation system, and more particularly to an oxygen generation system, wherein the oxygen generation system is composed of 13X molecular sieves, activated alumina, silica gel, etc. the nitrogen adsorbents such as CaA, CaX, NaX, LiX, etc. are used for pressure swing adsorption of dry molecular sieves such as 13X, activated alumina, silica gel, etc. and are usually used in the conventional PSA method for producing oxygen by air flow.
The adsorption tower, also called as adsorber, adsorption bed, separator, of the utility model refers to a container filled with at least one adsorbent, which has stronger adsorption capacity to the components that are easy to be adsorbed in the mixed gas.
In the present invention, the terms of Pressure Swing Adsorption, Adsorption separation, PSA, etc. are known to those skilled in the art, and these methods refer to not only PSA methods, but also methods similar thereto, such as Vacuum Swing Adsorption (VSA) or Mixed Pressure Swing Adsorption (MPSA), etc., which are understood in a broader sense, that is, for the Adsorption Pressure of the periodic cycle, a higher Pressure is a higher Pressure relative to the desorption step, which may include a Pressure greater than or equal to atmospheric Pressure, and for the desorption Pressure of the periodic cycle, a lower Pressure is a lower Pressure relative to the Adsorption step, which includes a Pressure less than or equal to atmospheric Pressure.
The utility model discloses in, to the membrane separation process, zeolite membrane separator has the separation function of oxygen and nitrogen gas, argon gas, and oxygen sees through more easily and nitrogen gas, argon gas are difficult to pass through more.
As is well known, zeolitic materials are generally referred to as aluminosilicate molecular sieves, but zeolites are sometimes also referred to as crystalline molecular sieves, and the present invention is generally directed to molecular sieves, including, for example, aluminosilicates, aluminophosphates, gallium phosphates and variants of these materials substituted with metals, and generally zeolitic materials are often referred to as molecular sieve materials, but in practice, by controlling their composition and manufacture, they may be structured to contain a plurality of pores or cavities of a specific size, so that atoms or molecules having the desired maximum size are effectively filtered and/or adsorbed, and in addition, zeolitic materials may be made to have the desired electrical polarization characteristics, and polar molecules or atoms or molecules susceptible to polarization may be selectively attracted to the zeolitic material. Thus, combining the size selectivity (which is due to the similarity of the pore and channel sizes of the zeolite material to the molecular size) with the control of the electrical properties of the zeolite material, the control of the gas species adsorbed and adsorbed on the zeolite membrane is possible. Thus, the zeolite material can be used as a membrane separation material having selectivity for a specific component, so that the crystal structure thereof enables the atoms or molecules of the gas desired to be separated to be adsorbed therein and to diffuse through the material, typically, a membrane is made of a readily polarizable zeolite material, such as chabazite, since one of the components to be separated in the mixed gas is attracted toward the polarized zeolite material. In this way the rate at which the relative component is initially adsorbed onto the zeolite membrane material can be increased and once the component to be separated is absorbed into the membrane, the pore channel dimensions of the zeolite material are only such that, for example, molecular oxygen passes through but nitrogen and argon do not diffuse through, whereby the separation efficiency can be significantly increased by this method of control in which the rate at which oxygen is adsorbed onto the membrane is greater than the rate at which other gases (e.g. nitrogen, argon) in the gas mixture are adsorbed.
For zeolite membrane separators, the zeolite separation membrane may comprise a porous substrate such as sintered metal or ceramic and a zeolite membrane formed thereon, the important feature being that the zeolite membrane is substantially defect free, having no "pinholes" or small cavities throughout the entire thickness of the membrane similar or larger in size to the pores of the zeolite material itself, as described in international patent WO 94/01209.
For a feed gas of a mixture of oxygen, nitrogen and argon, the retentate gas of the zeolite membrane separator is rich in nitrogen and argon, also known as waste gas, while the permeate gas of the zeolite membrane separator is rich in oxygen, also known as product gas.
Drawings
FIG. 1 is a flow diagram of a conventional pressure swing adsorption oxygen plant.
FIG. 2 is a schematic diagram of the apparatus for producing high-purity oxygen based on the coupling separation technique of the present invention.
Detailed Description
Referring to fig. 1, a schematic diagram of a basic process and apparatus for oxygen production based on equilibrium adsorption mechanism with nitrogen adsorbent is shown, generally, the system receives compressed and pretreated relatively clean compressed air as feed gas from line 1, typically compressed by a compressor to the separation pressure required for subsequent separation, such as: after passing through a filter with the pressure of 0.3-2.0 MPa, removing moisture, solid particle impurities and oil content in compressed air by a pretreatment system consisting of an active carbon oil remover or a filter, a freeze dryer or an adsorption dryer and the like alone or in various combinations, and then entering an air buffer tank, as known technology, the method is very necessary for a gas separation system, wherein the filter can be a multi-stage combined type, the adsorption dryer and the freeze dryer can be combined or independently adopted, preferably a method for recovering compressed air compression heat energy to regenerate the moisture of a selected adsorption dryer is adopted, preferably the adsorption dryer selects an adsorbent capable of selectively removing carbon dioxide in air to remove carbon dioxide, wherein the filtering precision, the air treatment amount of the filter, the outlet dew point of the freeze dryer or the dew point in the air after being treated by the adsorption dryer and the treatment requirement on trace carbon dioxide should be met for the use of a subsequent separation system The carbon dioxide or oil content required by the gas component outlet is required as a reference, and a buffer tank is not necessary and can be realized by adopting a variable-frequency compression process of the prior art or by bypass emptying, so that the aim is to avoid frequent starting of the compressor and possible process overpressure, and the components and design requirements contained in the pretreatment system can be flexibly mastered by a person skilled in the art according to the common design requirements.
As mentioned above, the processed raw air enters the pressure swing adsorption separation system of the prior art depicted in FIG. 1, and then nitrogen, moisture, carbon dioxide and other components are removed from XYQ102, and oxygen with a purity of about 93% is output from the gas production loop consisting of V3A, V3B, D03 and the pipelines, the pressure swing adsorption oxygen generation system is a typical double-tower adsorption system, 101B is regenerated when 101A adsorbs and generates oxygen, when 101A adsorbs and is saturated, a pressure equalizing process is firstly performed (at this time, only V4A is opened to introduce the oxygen with higher purity at the product end of 101A into the feed end of 101B), then 101A starts to evacuate the atmosphere, waste gases such as nitrogen, moisture, carbon dioxide and the like are removed from XYQ102, and at the same time, 101B opens the air inlet valve V1B to generate oxygen, the pressure swing adsorption process double-tower device based on the equilibrium adsorption mechanism operates in the order of 101A and 101B out of phase, typical basic steps are shown in the following table:
Figure BDA0002955462770000071
all the valves except the appointed opening valve in the steps are in a closed state, the oxygen output can be controlled by adjusting 3C or 3D, and the oxygen flow rate of quantitative cleaning can be controlled by adjusting 5C.
According to the steps, after the 101A is saturated in adsorption, the fluid is controlled to enter the 101B to generate oxygen by switching the symmetrical fluid control valves, the 101A is regenerated, and the steps are repeated in a circulating way to generate oxygen with the purity of about 93 percent, and the balance of nitrogen and argon.
Obviously, the pressure swing adsorption oxygen production using the above technology, not including the adsorption drying not shown in the figure, requires a large number of control valves, and can produce only oxygen-enriched air with a purity of about 93%.
As attached figure 2, the utility model discloses use adsorption drying as the basis to divide two sets of couplings respectively of zeolite membrane separator to be filling like active alumina, 13X or the necessary supporting valve of this adsorption system in adsorption drying separation bed export series connection, in M01A/B's separation process, concentrated oxygen is enriched and is discharged the back stage separation ware via 03A/B in the infiltration gas export, and waste gas then is enriched at the side export of being detained, is introduced adsorption separation system's regeneration process, thereby has practiced thrift raw materials air's consumption, has improved the system recovery rate.
Referring to FIG. 2, further, the higher purity enriched oxygen generated by the preceding stage zeolite membrane separator M01A/B is further concentrated to higher purity oxygen by passing through the zeolite membrane separator M01C via valve 03A/03B, in M01C, the concentrated oxygen is concentrated at the permeate gas outlet and discharged to the product gas buffer tank via valve 4A, the 4A is an on-off valve set to a controllable flow rate, typically a valve adjustable from 0-100% open, to control the overall yield, the oxygen separated by the preceding stage, if it is necessary to further increase the purity of oxygen, can be appropriately controlled and at least a portion of the gas is removed from the secondary separator, the removed waste gas can be introduced into the preceding stage as regeneration gas (not shown) via piping and valves, thus, following a pressure swing adsorption drying cycle as known in the art, a coupled separation process is formed, the system is simple, the number of valves is small, especially, adsorption drying is integrated, the purification requirement of front-end compressed air can be greatly reduced, and typically, the operation steps of the coupling separation system shown in the attached fig. 2 are as follows:
(1) opening 01A and 03A, drying A for work, and adsorbing; at the moment, 02B is opened, the drying B is emptied and regenerated, meanwhile, 4A of the separation part of the later stage zeolite membrane is opened, the yield is adjusted, and oxygen can be produced, and when the adsorption of the adsorption drying A is saturated, the next step is carried out;
(2) opening 01B and 03B, drying B for work, and adsorbing; at the moment, 02A is opened, the dried A is emptied and regenerated, at the same time, 4A of the separation part of the later stage zeolite membrane is opened, the yield is adjusted to produce oxygen, and when the adsorption of the adsorption dried B is saturated, the previous step is carried out.
In the above steps, except for the appointed opening of the valve, all the other valves are in a closed state, the oxygen flow can be controlled by adjusting 4A, and the flow of quantitative cleaning can be controlled by adjusting the shutoff valve.
According to the steps, after the adsorption of the drying A is saturated, the fluid is controlled to enter the adsorption tower B for continuously producing oxygen by switching the symmetrical fluid control valve, the drying A is regenerated, and the steps are repeated in such a circulating way, so that the oxygen with the purity of 90 percent and even more than 99.5 percent can be produced.
By adopting the method of the utility model, the pre-stage pressure swing adsorption drying can be replaced by the system of oxygen with the purity of about 93 percent generated by the pressure swing adsorption oxygen generating device, and the oxygen with the high purity of more than 99.5 percent can be purified by the zeolite membrane separator through the same coupling.
The above described embodiments illustrate only some of the essential features of the invention, and it will be appreciated by those skilled in the art that although the invention has been described in part in connection with the accompanying drawings, this is merely an example of its application or a method, and that all other variations which do not violate the essence of the invention as set forth in this patent also fall within the scope of the patent, which is limited only by the scope of the appended claims.
The above-mentioned contents of the present invention are further described in some detail through the specific embodiments, but it should not be understood that the scope of the above-mentioned subject matter of the present invention is limited to the above coupling examples, and all the technologies realized based on the above contents of the present invention all belong to the scope of the invention.

Claims (4)

1. An apparatus for producing high purity oxygen based on a coupled separation technique, comprising:
(1) at least one compression device for supplying pressurized feed air, comprising means for air pre-treatment;
(2) at least one set of pressure swing adsorption drying device comprises an adsorption tower, wherein a molecular sieve adsorbent for adsorbing water, an air inlet valve and a connecting pipeline thereof, an air outlet valve and a connecting pipeline thereof, and a gas production valve and a connecting pipeline thereof are arranged in the adsorption tower;
(3) at least one zeolite membrane separator, wherein the zeolite membrane separator is filled with a zeolite membrane separation material and is coupled in the adsorption drying device; each zeolite membrane separator has three ports: the device comprises a raw gas interface, a permeate gas outlet and a retentate gas outlet, wherein the raw gas interface is arranged at a product end of the pressure swing adsorption drying device, the permeate gas outlet is arranged at a control valve at a product end of a zeolite membrane separator, and the retentate gas outlet is communicated to a product end of the other group of adsorption drying towers and used as regeneration cleaning gas of the towers; in addition, the device also comprises a cleaning gas connecting pipeline and a regulating valve;
(4) at least one secondary zeolite membrane separator is connected in series after the product end control valve of the zeolite membrane separator, and the permeation gas outlet of the secondary zeolite membrane separator is connected to a product gas buffer tank through a control valve with adjustable flow rate, and at least a part of waste gas is discharged;
(5) at least one product gas buffer tank in communication with the permeate gas outlet end of the secondary zeolite membrane separator for receiving the permeate fraction enriched from the zeolite membrane separator;
(6) and a complete set of control components for operating the valves on the circuit and for controlling the operation of the compression apparatus.
2. The apparatus for producing high purity oxygen based on coupled separation technology as claimed in claim 1, wherein the gas flow through the zeolite membrane separator is in the form of axial flow, radial flow or lateral flow.
3. The apparatus for producing high purity oxygen based on the coupled separation technique as claimed in claim 1, wherein a pretreatment layer for removing a non-oxygen portion is provided for the single zeolite membrane separator.
4. The apparatus for producing high-purity oxygen based on the coupled separation technology according to one of claims 1 to 3, characterized by a system comprising two parallel pressure swing adsorption drying devices coupled with a zeolite membrane separator; wherein:
there are two adsorption columns, namely: dry a, dry B, there are also two corresponding zeolite membrane separators, namely: M01A, M01B; automatic control valves 01A and 01B are respectively arranged between the raw gas pipeline and the air inlets of the drying A and the drying B; bypasses are arranged on the air inlet pipelines of the drying A and the drying B and behind the automatic control valves 01A and 01B and are connected to the silencer, and automatic control valves 02A and 02B are correspondingly arranged on the two bypasses; the air outlets of the drying A and the drying B are respectively connected with the raw material gas side interfaces of M01A and M01B to form two parallel drying and separating systems; the stagnant gas side interfaces of the two zeolite membrane separators M01A and M01B are connected through a pipeline, and a stop valve capable of controlling flow is arranged on the connecting pipeline; the permeation gas side ports of the two zeolite membrane separators M01A and M01B are respectively connected with a secondary zeolite membrane separator M01C through a pipeline; the back of the secondary zeolite membrane separator M01C is connected with a buffer tank PV 102; automatic control valves 03A and 03B are correspondingly arranged on connecting pipelines of permeation gas side ports of the two zeolite membrane separators M01A and M01B and the secondary zeolite membrane separator M01C; and a control valve 4A is arranged on a connecting pipeline of the secondary zeolite membrane separator M01C and the buffer tank PV 102.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112960650A (en) * 2021-03-01 2021-06-15 上海穗杉实业股份有限公司 Method and device for preparing high-purity oxygen based on coupling separation technology

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112960650A (en) * 2021-03-01 2021-06-15 上海穗杉实业股份有限公司 Method and device for preparing high-purity oxygen based on coupling separation technology
CN112960650B (en) * 2021-03-01 2023-09-22 上海穗杉实业股份有限公司 Method and device for preparing high-purity oxygen based on coupling separation technology

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