CN101301999A - Method for collecting oxygen from air - Google Patents

Method for collecting oxygen from air Download PDF

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Publication number
CN101301999A
CN101301999A CNA200810053623XA CN200810053623A CN101301999A CN 101301999 A CN101301999 A CN 101301999A CN A200810053623X A CNA200810053623X A CN A200810053623XA CN 200810053623 A CN200810053623 A CN 200810053623A CN 101301999 A CN101301999 A CN 101301999A
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oxygen
adsorption tower
molecular sieve
dehumidifying
air
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CNA200810053623XA
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张东辉
何东荣
胡智辉
吴婷婷
崔乐雨
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Tianjin University
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Tianjin University
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Abstract

The invention discloses a method for enriching oxygen in the air, comprising the following steps that: firstly, an absorption tower which is filled with dehumidifying absorbent and oxygen generation molecular sieves section by section is prepared, and the pressure is increased; secondly, raw material air is inputted into the absorption tower; oxygen is collected; an oxygen outlet valve and a raw material air input valve are closed down when the dehumidifying absorbent and the oxygen generation molecular sieves are saturated; thirdly, an atmospheric valve is opened; air absorbed by the absorption tower is released; the pressure is reduced; fourthly, heated oxygen is taken as regenerated flushing gas to enter into the absorption tower from the oxygen generation molecular sieves of the absorption tower; substances absorbed on the dehumidifying absorbent and the oxygen generation molecular sieves are flushed; the dehumidifying absorbent and the oxygen generation molecular sieves are driven to regenerate; fifthly, the pressure of the absorption tower is increased; and the steps from the second step to the fifth step are repeated. The method saves equipment investment, simultaneously uses heat which is only used for regenerating the dehumidifying absorbent for regenerating the dehumidifying absorbent and the oxygen generation molecular sieves simultaneously, and optimizes the technique under the condition that energy consumption is not increased.

Description

The method of collecting oxygen from air
Technical field
The present invention relates to a kind of from air the method for collecting oxygen.
Background technology
Along with fast development of modern industry, also be more and more to the demand and the kind of air products, so developed the air separation industries of a lot of various scales, the absorbed air isolation technique has obtained good development under this form.Because the simple energy-conservation advantage of the expansion in market and absorbed air isolation technique, this technology also can further develop.
Now general absorbed air separate adopt be mostly PSA (transformation absorption) or VPSA (Vacuum Pressure Swing Adsorption) method.With the air-separating oxygen-making is example, and the airborne nitrogen of zeolite molecular sieve preferentially adsorbed makes oxygen obtain carrying dense.PSA system oxygen principle is that air is through dehumidifying and removing CO 2After under high pressure by zeolite molecular sieve absorption nitrogen wherein, zeolite molecular sieve is desorption and regeneration under normal pressure again, concrete steps are generally: high pressure absorption, step-down (perhaps all step-downs), emptying, boost (perhaps all boosting), absorption.VPSA adsorbs under normal pressure or pressure-fired condition, vacuumizes regeneration, and step and PSA are similar.Both are general with stable the carrying out of multitower coupling cycle, continuously produce oxygen.
Owing to always contain certain moisture and other foreign gases in the air, raw air must be removed the contained H in the inside in traditional technology before entering adsorption tower 2O and CO 2Deng impurity to the toxic effect of system oxygen molecular sieve.General small air tripping device all is furnished with pretreatment units such as oil removal filter, cooling driers moisture trap; Large-scale absorbed air separation oxygen generating plant has employing two-stage air separation, and promptly the first step utilizes the dehumidifying sorbent material to remove the more intense H of air Semi-polarity earlier 2Impurity molecules such as O, and make oxygen part enrichment, oxygen is produced the product (associated description being arranged as patent CN1252322, US4190424 etc.) that needs concentration again in the second stage.
The first step pretreatment stage of two-stage air separation is because H 2O and CO 2More intense with the bonding force of sorbent material, desorb is difficulty relatively, and sorbent material must could be reused preferably through thermal regeneration.So pertinent literature have with after second section the product waste gas heating as first section stripping gas.Though improved the raw air utilization ratio like this, just seeming of whole device is comparatively complicated, and cost and energy consumption are also high.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, provide a kind of device simple, adsorbent reactivation is the method for collecting oxygen from air rapidly and thoroughly.
Technical scheme of the present invention is summarized as follows:
A kind of from air the method for collecting oxygen, comprise the steps:
(1) preparing segmentation, to be filled with mass ratio be 1: 1~30 the dehumidifying sorbent material and the adsorption tower of system oxygen molecular sieve, boosts to 0.03~2.0Mpa;
(2) with pressure be the dehumidifying sorbent material end of the raw air input adsorption tower of 0.03~2.0Mpa, collect oxygen from the outlet of the system oxygen molecular sieve end of adsorption tower, wait to dehumidify sorbent material and system oxygen molecular sieve when saturated substantially, close the oxygen outlet valve and the raw air transfer valve of adsorption tower;
(3) with the emptying valve open of adsorption tower, emit the gas of adsorption tower occlusion, make the pressure in the adsorption tower reduce to normal pressure;
(4) will be heated to 50~160 ℃ oxygen again and feed described adsorption tower from the system oxygen molecular sieve end of adsorption tower, the material that is adsorbed on dehumidifying sorbent material and the system oxygen molecular sieve is washed, make dehumidifying sorbent material and the regeneration of system oxygen molecular sieve as the regeneration purge gas;
(5) described adsorption tower is boosted to 0.03~2.0Mpa; Repeating said steps (2)-(5).
The ratio of the dehumidifying sorbent material of described step (1) and system oxygen molecular sieve is 1: 1~25.
Described dehumidifying sorbent material is that activated alumina, silica gel, 3A zeolite molecular sieve and gac are at least a.
Described system oxygen molecular sieve is 5A zeolite molecular sieve or 13X zeolite molecular sieve.
Oxygen described in the described step (4) is the oxygen of being collected by the system oxygen molecular sieve end of described adsorption tower, and the feeding volume of described heating oxygen is 0.2~5 times of adsorption tower volume.
The heating means of oxygen described in the described step (4) are direct electrically heated or waste heat of plant heating or steam heating.
Advantage of the present invention is:
1. simplified equipment, two equipment that traditional two-stage air separation is required: dehumidification equipment and oxygen generating plant are reduced in the adsorption tower, have reduced cost.
2. the absorbed air that the present invention is traditional relatively separates system oxygen technology, the regeneration of dehumidifying sorbent material and system oxygen molecular sieve is step-down, intensification (heating of oxygen), flushing (flushing of oxygen) the three's combined action by adsorption tower, makes the bed desorption and regeneration of adsorption tower faster more thorough.The present invention's regeneration that the heat of adsorbent reactivation is used to make oxygen molecular sieve and dehumidifying sorbent material simultaneously that will originally only be used to dehumidify, under the situation that does not increase energy consumption with process optimization.
3. traditional relatively PSA (transformation absorption) air-separating oxygen-making, under the identical adsorptive pressure and desorption pressures, because bed desorb situation is better than the latter, and the flushing tolerance that requires of desorb can lack than psa process a lot, so just directly improved the product production and the rate of recovery; Traditional relatively VPSA (Vacuum Pressure Swing Adsorption) makes oxygen, the investment and the energy consumption of having saved vacuum pump.Low waste heat can utilize if factory has good taste, and the running cost of method so of the present invention further reduces.
This method of the present invention has been saved facility investment to a great extent, especially is fit to have surplus heat can utilize and not require under the very high condition with oxygen purity use.Utilize the high-temperature product circulation of vital energy in the wrong direction to flushing in the time of regeneration, nitrogen that is adsorbed and water vapour etc. desorb successively, and the nitrogen of first desorb has washing action to the desorb of the more intense gas of the polarity of adsorption tower dehumidifying section absorption.
Description of drawings
Fig. 1 is the method process flow sheet (single tower) of collecting oxygen from air.
Fig. 2 is the method process flow sheet (three towers) of collecting oxygen from air.
Embodiment
The present invention is further illustrated below in conjunction with drawings and Examples.
Embodiment 1
A kind of from air the method for collecting oxygen, comprise the steps: (see figure 1)
(1) select adsorption tower, its internal diameter 30mm, the long 500mm of tower, adsorption tower press mass ratio filling in 1: 7 activated alumina (dehumidifying sorbent material, the B among the figure) and 5A zeolite molecular sieve (system oxygen molecular sieve, the A among the figure), operation adsorptive pressure 0.3MPa; (2) open valve VF, VP, VR1, and manual regulation product gas oxygen flow and regeneration purge gas branch road (a shunting part is used for flushing regeneration from product gas oxygen) throughput ratio are about 2.5: 1, other valves are all closed, with pressure is the dehumidifying sorbent material end of the raw air input adsorption tower of 0.3Mpa, collect oxygen from the outlet of the system oxygen molecular sieve end of adsorption tower, VR1 is controlled by hot resurgent gases surge tank pressure feedback, hot resurgent gases surge tank pressure is fluctuateed in the 0.05-0.1MPa scope, when treating that activated alumina and 5A zeolite molecular sieve are saturated substantially, close oxygen outlet valve VP and the VR1 and the raw air transfer valve VF of adsorption tower;
(3) the emptying valve VW with adsorption tower opens, and emits the gas of adsorption tower occlusion, makes the pressure in the adsorption tower reduce to normal pressure;
(4) open valve VR2, and the opened condition of maintenance VW, the oxygen that is heated to 100 ℃ is fed described adsorption tower as the system oxygen molecular sieve end of purge gas from adsorption tower of regenerating, the material that is adsorbed on dehumidifying adsorbent activity aluminum oxide and the system oxygen molecular sieve 5A zeolite molecular sieve is washed, make dehumidifying sorbent material and the regeneration of system oxygen molecular sieve;
(5) after flushing finished, an open valve VF closed other all valves, and described adsorption tower is boosted to 0.3Mpa; Repeating said steps (2)-(5), the just above oxygen product of energy production concentration enrichment to 80% intermittently.Owing to be single tower flow process, lack the pressure equalizing between tower and the tower, but oxygen recovery rate still can reach 36.4%, exceed much than the making oxygen of prior art.
The volume ratio of regeneration purge gas flushing dose and adsorption tower is 1.4: 1.
The time sequential routine table is:
Absorption 180s Emptying 20s Heat regeneration purge gas flushing 60s 30s boosts
After circulation arrived and stablizes, can obtain product gas concentration was 81.4%, oxygen recovery rate 36.4%.
Fig. 1 explanation: A representative filling is system oxygen molecular sieve such as 5A zeolite molecular sieve etc. among the figure, and the B representative is the dehumidifying sorbent material
As activated alumina etc.Valve is described as follows:
VF: the raw air transfer valve, VW: the emptying valve,
VR1: high-temperature product resurgent gases branch road sequencing valve, VR2: resurgent gases flushing sequencing valve,
VP: oxygen outlet valve, VPH: resurgent gases tolerance manual modulation valve.
Embodiment 2
A kind of from air the method for collecting oxygen, comprise the steps:
(1) preparing segmentation, to be filled with mass ratio be 1: 5 dehumidifying sorbent material (silica gel) and the adsorption tower of making oxygen molecular sieve (5A zeolite molecular sieve), boosts to 0.03Mpa;
(2) with pressure be the dehumidifying sorbent material end of the raw air input adsorption tower of 0.03Mpa, collect oxygen from the outlet of the system oxygen molecular sieve end of adsorption tower, wait to dehumidify sorbent material and system oxygen molecular sieve when saturated substantially, close the oxygen outlet valve and the raw air transfer valve of adsorption tower;
(3) the emptying valve VW with adsorption tower opens, directly with the gas emptying of adsorption tower occlusion to atmosphere, make the pressure in the adsorption tower reduce to normal pressure;
(4) will be heated to 50 ℃ oxygen again and feed described adsorption tower, the material that is adsorbed on dehumidifying sorbent material and the system oxygen molecular sieve is washed, make dehumidifying sorbent material and the regeneration of system oxygen molecular sieve from the system oxygen molecular sieve end of adsorption tower;
(5) described adsorption tower is boosted to 0.03Mpa; Repeating said steps (2)-(5).
Oxygen described in the described step (4) is the oxygen of being collected by the system oxygen molecular sieve end of described adsorption tower, and the feeding volume of described heating oxygen is 0.2 times of adsorption tower volume.The heating means of oxygen are direct electrically heated.
Absorption 60s Emptying 10s Heat regeneration purge gas flushing 30s 20s boosts
Circular flow can obtain oxygen concentration 31%, the oxygen enriched product gas of oxygen recovery rate 60%.
Embodiment 3
A kind of from air the method for collecting oxygen, comprise the steps:
(1) prepares segmentation and be filled with the adsorption tower that mass ratio is 1: 1: 10 3A zeolite molecular sieve, activated alumina and 13X zeolite molecular sieve, boost to 2.0Mpa;
(2) with pressure be the dehumidifying sorbent material end of the raw air input adsorption tower of 2.0Mpa, collect oxygen from the outlet of the system oxygen molecular sieve end of adsorption tower, wait to dehumidify sorbent material and system oxygen molecular sieve when saturated substantially, close the oxygen outlet valve and the raw air transfer valve of adsorption tower;
(3) the emptying valve VW with adsorption tower opens, directly with the gas emptying of adsorption tower occlusion to atmosphere, make the pressure in the adsorption tower reduce to normal pressure;
(4) will be heated to 160 ℃ oxygen again and feed described adsorption tower, the material that is adsorbed on dehumidifying sorbent material and the system oxygen molecular sieve is washed, make dehumidifying sorbent material and the regeneration of system oxygen molecular sieve from the system oxygen molecular sieve end of adsorption tower;
(5) described adsorption tower is boosted to 2.0Mpa; Repeating said steps (2)-(5).
Oxygen is the oxygen of being collected by the system oxygen molecular sieve end of adsorption tower in the step (4), and the feeding volume of heating oxygen is 5 times of adsorption tower volume.The heating means of oxygen are the waste heat of plant heating.
Absorption 720s Emptying 60s Heat regeneration purge gas flushing 100s 60s boosts
Circular flow can obtain oxygen concentration 89%, the oxygen enriched product gas of oxygen recovery rate 40%.
Embodiment 4
A kind of from air the method for collecting oxygen, comprise the steps:
(1) prepares segmentation and be filled with the adsorption tower that mass ratio is 2: 1: 25 gac, silica gel and 5A zeolite molecular sieve, boost to 0.1Mpa;
(2) with pressure be the dehumidifying sorbent material end of the raw air input adsorption tower of 0.1Mpa, collect oxygen from the outlet of the system oxygen molecular sieve end of adsorption tower, wait to dehumidify sorbent material and system oxygen molecular sieve when saturated substantially, close the oxygen outlet valve and the raw air transfer valve of adsorption tower;
(3) the emptying valve VW with adsorption tower opens, directly with the gas emptying of adsorption tower occlusion to atmosphere, make the pressure in the adsorption tower reduce to normal pressure;
(4) will be heated to 120 ℃ oxygen again and feed described adsorption tower, the material that is adsorbed on dehumidifying sorbent material and the system oxygen molecular sieve is washed, make dehumidifying sorbent material and the regeneration of system oxygen molecular sieve from the system oxygen molecular sieve end of adsorption tower;
(5) described adsorption tower is boosted to 0.1Mpa; Repeating said steps (2)-(5).
Oxygen is the oxygen of being collected by the system oxygen molecular sieve end of adsorption tower in the step (4), and the feeding volume of heating oxygen is 0.93 times of adsorption tower volume.The heating means of oxygen are steam heating in the step (4).
Absorption 180s Emptying 20s Heat regeneration purge gas flushing 60s 30s boosts
The oxygen enriched product concentration 38.4% that finally obtains, yield 50%.
Embodiment 5
A kind of from air the method for collecting oxygen, comprise the steps:
(1) prepares segmentation and be filled with the adsorption tower that mass ratio is 1: 1: 3 activated alumina, 3A zeolite molecular sieve and 5A zeolite molecular sieve, boost to 1.0Mpa;
(2) with pressure be the dehumidifying sorbent material end of the raw air input adsorption tower of 1.0Mpa, collect oxygen from the outlet of the system oxygen molecular sieve end of adsorption tower, wait to dehumidify sorbent material and system oxygen molecular sieve when saturated substantially, close the oxygen outlet valve and the raw air transfer valve of adsorption tower;
(3) the emptying valve VW with adsorption tower opens, directly with the gas emptying of adsorption tower occlusion to atmosphere, make the pressure in the adsorption tower reduce to normal pressure;
(4) will be heated to 110 ℃ oxygen again and feed described adsorption tower, the material that is adsorbed on dehumidifying sorbent material and the system oxygen molecular sieve is washed, make dehumidifying sorbent material and the regeneration of system oxygen molecular sieve from the system oxygen molecular sieve end of adsorption tower;
(5) described adsorption tower is boosted to 1.0Mpa; Repeating said steps (2)-(5).
Oxygen is the oxygen of being collected by the system oxygen molecular sieve end of adsorption tower in the step (4), and the feeding volume of heating oxygen is 0.75 times of adsorption tower volume.The heating means of oxygen are steam heating in the step (4).
Absorption 600s Emptying 60s Heat regeneration purge gas flushing 60s 60s boosts
The oxygen enriched product concentration 44.4% that finally obtains, yield 62%.
Embodiment 6
Described the flow process of single tower system oxygen among Fig. 1, in actually operating, can also select multitower coupled mode for use, seen Fig. 2)
Following table is the explanation (is example with three towers) of figure number among Fig. 2:
F1, F2, F3: unstripped gas intake valve P1, P2, P3: product gas air outlet valve
R1, R2, R3: hot resurgent gases flushing intake valve E1, E2, E3: equalizing valve
BD1, BD2, BD3: blow-off valve RV: product gas divides the road valve of diffluence heating
This three towers omnibus control system works time-scale
Figure A20081005362300071
Because zeolite molecular sieve belongs to equilibrium adsorption to the absorption of nitrogen, so the change of a depended on pressure can make the regeneration level of adsorption tower limited in the traditional technology.In order to obtain better separation factor as much as possible, absorption and regeneration between the two a more significant pressure reduction just must be arranged.And through we experimental studies have found that, elevated temperature makes the ability drop of zeolite molecular sieve absorption nitrogen very fast, and for example 85 ℃ of following loading capacities have only under 27 ℃ about 0.2 times.Fully prove by theoretical and experiment: step-down intensification combined action, must improve the adsorbent reactivation degree greatly.
The used adsorption tower of the present invention has loaded dehumidifying sorbent material and system oxygen molecular sieve in proportion, and the filling ratio is according to airborne H 2O, CO 2Content and sorbent material calculate its absorption property.And the saturation time that requires the dehumidifying section is not less than the saturation time of system oxygen molecular sieve section.
The oxygen enrichment flow process is: enter the adsorption tower under the high pressure after the raw air pressurization, impurity and nitrogen are adsorbed the agent occlusion in adsorption tower, oxygen flows out from the product end as product gas, after treating that adsorbents adsorb is saturated substantially, reduce bed layer pressure to normal pressure, reverse feeding adsorption tower after a spot of product oxygen is heated to 50~160 ℃, heating be the flushing reproducing adsorbent also, and it can be recycled.

Claims (6)

1. the method for a collecting oxygen from air is characterized in that comprising the steps:
(1) preparing segmentation, to be filled with mass ratio be 1: 1~30 the dehumidifying sorbent material and the adsorption tower of system oxygen molecular sieve, boosts to 0.03~2.0Mpa;
(2) with pressure be the dehumidifying sorbent material end of the raw air input adsorption tower of 0.03~2.0Mpa, collect oxygen from the outlet of the system oxygen molecular sieve end of adsorption tower, wait to dehumidify sorbent material and system oxygen molecular sieve when saturated substantially, close the oxygen outlet valve and the raw air transfer valve of adsorption tower;
(3) with the emptying valve open of adsorption tower, emit the gas of adsorption tower occlusion, make the pressure in the adsorption tower reduce to normal pressure;
(4) will be heated to 50~160 ℃ oxygen again and feed described adsorption tower from the system oxygen molecular sieve end of adsorption tower, the material that is adsorbed on dehumidifying sorbent material and the system oxygen molecular sieve is washed, make dehumidifying sorbent material and the regeneration of system oxygen molecular sieve as the regeneration purge gas;
(5) described adsorption tower is boosted to 0.03~2.0Mpa; Repeating said steps (2)-(5).
2. according to claim 1 a kind of from air the method for collecting oxygen, it is characterized in that the dehumidifying sorbent material of described step (1) and the ratio of system oxygen molecular sieve are 1: 1~25.
3. according to claim 1 and 2 a kind of from air the method for collecting oxygen, it is characterized in that described dehumidifying sorbent material is that activated alumina, silica gel, 3A zeolite molecular sieve and gac are at least a.
4. according to claim 1 and 2 a kind of from air the method for collecting oxygen, it is characterized in that described system oxygen molecular sieve is 5A zeolite molecular sieve or 13X zeolite molecular sieve.
5. according to claim 1 a kind of from air the method for collecting oxygen, it is characterized in that oxygen described in the described step (4) is the oxygen of being collected by the system oxygen molecular sieve end of described adsorption tower, the feeding volume of described heating oxygen is 0.2~5 times of adsorption tower volume.
6. according to claim 1 a kind of from air the method for collecting oxygen, the heating means that it is characterized in that oxygen described in the described step (4) are direct electrically heated or waste heat of plant heating or steam heating.
CNA200810053623XA 2008-06-25 2008-06-25 Method for collecting oxygen from air Pending CN101301999A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103130187A (en) * 2012-09-06 2013-06-05 青岛道一氧吧设备有限公司 Nitrogen back washing technique
CN103432858A (en) * 2013-08-15 2013-12-11 青岛道一空优科技有限公司 Novel nitrogen-oxygen separation device
CN105858615A (en) * 2016-05-05 2016-08-17 珠海辉钰医疗科技有限公司 Bridge type low-pressure fan oxygen generation system
CN106268723A (en) * 2016-08-15 2017-01-04 山东洪达化工有限公司 A kind of convenient, oxygen molecular sieve situ activation method processed of safety and environmental protection
CN107399719A (en) * 2016-05-18 2017-11-28 乔治洛德方法研究和开发液化空气有限公司 The VSA type oxygen generation methods of periodic regeneration
CN113998673A (en) * 2021-10-27 2022-02-01 北京科技大学 Portable oxygen generator
CN114906814A (en) * 2022-05-07 2022-08-16 西南化工研究设计院有限公司 Oxygen-making molecular sieve and pressure swing adsorption oxygen-making method
CN115463512A (en) * 2022-09-19 2022-12-13 杨坤 Oxygen generation system
WO2023240777A1 (en) * 2022-06-16 2023-12-21 北京北大先锋科技股份有限公司 Composite adsorbent bed and use thereof

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103130187A (en) * 2012-09-06 2013-06-05 青岛道一氧吧设备有限公司 Nitrogen back washing technique
CN103130187B (en) * 2012-09-06 2015-08-12 青岛道一空优科技有限公司 Nitrogen backwashing technology
CN103432858A (en) * 2013-08-15 2013-12-11 青岛道一空优科技有限公司 Novel nitrogen-oxygen separation device
CN103432858B (en) * 2013-08-15 2015-12-02 青岛道一空优科技有限公司 A kind of Novel nitrogen-oxygen separation device
CN105858615A (en) * 2016-05-05 2016-08-17 珠海辉钰医疗科技有限公司 Bridge type low-pressure fan oxygen generation system
CN107399719A (en) * 2016-05-18 2017-11-28 乔治洛德方法研究和开发液化空气有限公司 The VSA type oxygen generation methods of periodic regeneration
CN106268723A (en) * 2016-08-15 2017-01-04 山东洪达化工有限公司 A kind of convenient, oxygen molecular sieve situ activation method processed of safety and environmental protection
CN113998673A (en) * 2021-10-27 2022-02-01 北京科技大学 Portable oxygen generator
CN113998673B (en) * 2021-10-27 2023-03-07 北京科技大学 Portable oxygen generator
CN114906814A (en) * 2022-05-07 2022-08-16 西南化工研究设计院有限公司 Oxygen-making molecular sieve and pressure swing adsorption oxygen-making method
WO2023240777A1 (en) * 2022-06-16 2023-12-21 北京北大先锋科技股份有限公司 Composite adsorbent bed and use thereof
CN115463512A (en) * 2022-09-19 2022-12-13 杨坤 Oxygen generation system
CN115463512B (en) * 2022-09-19 2024-02-13 杨坤 Oxygen generation system

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Open date: 20081112