AU2020100284A4 - Enrichment and Purification Device for Single Gas in Mixed Gas - Google Patents
Enrichment and Purification Device for Single Gas in Mixed Gas Download PDFInfo
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- 238000000746 purification Methods 0.000 title claims abstract description 95
- 239000007789 gas Substances 0.000 claims abstract description 184
- 238000007710 freezing Methods 0.000 claims abstract description 90
- 230000008014 freezing Effects 0.000 claims abstract description 90
- 238000010438 heat treatment Methods 0.000 claims abstract description 72
- 239000002808 molecular sieve Substances 0.000 claims abstract description 12
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 108
- 239000007788 liquid Substances 0.000 claims description 60
- 229910052757 nitrogen Inorganic materials 0.000 claims description 54
- 239000000523 sample Substances 0.000 claims description 17
- 229910001220 stainless steel Inorganic materials 0.000 claims description 14
- 239000010935 stainless steel Substances 0.000 claims description 14
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 3
- 230000008016 vaporization Effects 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 30
- 238000004458 analytical method Methods 0.000 description 15
- 229910002092 carbon dioxide Inorganic materials 0.000 description 15
- 238000001179 sorption measurement Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000003039 volatile agent Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D8/00—Cold traps; Cold baffles
-
- 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
- B01D53/0462—Temperature swing adsorption
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0011—Sample conditioning
- G01N33/0014—Sample conditioning by eliminating a gas
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0011—Sample conditioning
- G01N33/0019—Sample conditioning by preconcentration
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Immunology (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Abstract The invention provides a device for enriching and purifying a single gas in a mixed gas, which comprises a pre-purification cold trap capable of freezing and adsorbing part of non-target gases in the mixed gas, the pre-purification cold trap provided with a mixed gas inlet for the mixed gas to enter; enrichment cold and hot trap, having molecular sieves of different specifications detachably filled therein, the gas inlet of the enrichment cold and hot trap connected with the gas outlet of the pre-purification cold trap through a first switching valve; a freezing unit for reducing the temperature of the enrichment cold and hot trap; a vacuum acquisition system for enabling the enrichment and purification device to reach a preset vacuum degree and capable of exhausting other non-target gases in the mixed gas that are not adsorbed out of the enrichment cold and hot trap, having a suction connected with the gas outlet of the enrichment cold and hot trap; a heating unit for heating the enrichment cold and hot trap to completely release the target gas absorbed by the enrichment cold and hot trap; and a purification outlet connected to the gas outlet of the enrichment cold and hot trap through a second switching valve. It achieves the extraction and purification of a single gas in a mixed gas with different molecular weights. 100 -c -19M Fig.1
Description
Enrichment and Purification Device for Single Gas in Mixed Gas
Technical Field
The invention relates to the technical field of gas analysis instruments, and more particularly, to an enrichment and purification device for a single gas in a mixed gas.
Background Art
It is a very important analytical method and pretreatment method in the analysis of analytical chemistry, geochemistry and environmental science to extract and purify a gas in a mixed gas of different molecular weights.
In the study of earth science, the analysis of volatiles in a mineral inclusion is of important scientific significance, but with traditional means of analysis, under a vacuum condition and after the mineral is broken, the gases of different molecular weights in the volatiles typically include gaseous H2O, CO2, SO2, NH3, N2, O2, inert gases and the like, leading to difficulty in distinguishing them.
In addition, at present, for the extraction and purification of a gas of a specific molecular weight in a mixed gas, and the preparation of cold liquid for freezing are generally done manually, which is time-consuming and labor-intensive, and it is also difficult to accurately control the freezing temperature of the cold liquid, which in turn affects the accuracy of the analysis.
Summary of the Invention
In view of this, the purpose of the present invention is to provide an enrichment and purification device for a single gas in a mixed gas, so as to realize the extraction and purification of a single gas in a mixed gas with different molecular weights.
In order to achieve the above object, the present invention provides the following technical solutions.
An enrichment and purification device for a single gas in a mixed gas comprises:
a pre-purification cold trap capable of freezing and adsorbing part of non-target gases in the mixed
2020100284 26 Feb 2020 gas, the pre-purification cold trap provided with a mixed gas inlet for the mixed gas to enter;
an enrichment cold and hot trap capable of adsorbing the target gas in the mixed gas when frozen, and capable of releasing the adsorbed purified target gas when heated, the enrichment cold and hot trap detachably filled with molecular sieves of different specifications, the gas inlet of the enrichment cold and hot trap connected with the gas outlet of the pre-purification cold trap through a first switching valve;
a freezing unit for reducing the temperature of the enrichment cold and hot trap so that the enrichment cold and hot trap absorbs the target gas;
a vacuum acquisition system for enabling the enrichment and purification device to reach a preset vacuum degree and capable of exhausting other non-target gases in the mixed gas that are not adsorbed out of the vacuum acquisition system of the enrichment cold and hot trap, the suction of the vacuum acquisition system connected with the gas outlet of the enrichment cold and hot trap;
a heating unit for heating the enrichment cold and hot trap to completely release the target gas adsorbed by the enrichment cold and hot trap; and a purification outlet connected to a gas outlet of the enrichment cold and hot trap through a second switching valve.
Preferably, in the enrichment and purification device described above, the freezing unit comprises:
a freezing sleeve sleeved on the enrichment cold and hot trap;
a self-adapting liquid nitrogen tank storing liquid nitrogen, the self-adapting liquid nitrogen tank introducing the liquid nitrogen required for freezing the target gas into the freezing sleeve through a conduit, the conduit extending below the level of the liquid nitrogen of the self-adapting liquid nitrogen tank;
a heating module for vaporizing the liquid nitrogen in the self-adapting liquid nitrogen tank to generate pressure to introduce the liquid nitrogen into the freezing sleeve.
Preferably, in the enrichment and purification device described above, the freezing unit further
2020100284 26 Feb 2020 comprises:
a tapered guide structure provided at the end of the conduit extending into the self-adapting liquid nitrogen tank, the tapered guide structure gradually diverging from the end proximal to the freezing sleeve to the end distant from the freezing sleeve, the heating module disposed in the tapered guide structure.
Preferably, in the enrichment and purification device described above, the freezing sleeve is a polytetrafluoroethylene (Teflon) sleeve, the conduit is a polytetrafluoroethylene tube, and the tapered guide structure is a metal tapered tube.
Preferably, the enrichment and purification device described above further comprises:
a first temperature control probe for detecting the freezing temperature of the enrichment cold and hot trap;
a freezing temperature controller for controlling the amount of liquid nitrogen entering into the freezing sleeve, the freezing temperature controller connected to the first temperature control probe and the heating module.
Preferably, in the above enrichment and purification device described above, the enrichment cold and hot trap is a stainless steel cold and hot trap, and the heating unit is a heating wire provided on the stainless steel cold and hot trap.
Preferably, the enrichment and purification device described above further comprises:
a second temperature control probe for detecting the heating temperature of the enrichment cold and hot trap;
a heating temperature controller for controlling the heating temperature of the heating wire, the heating temperature controller connected to the second temperature control probe and the heating wire.
Preferably, in the enrichment and purification device described above, the vacuum acquisition system comprises:
a molecular turbo pump, a suction of the molecular turbo pump connected to the gas outlet of the enrichment cold and hot trap;
a mechanical pump, a suction of the mechanical pump connected to the exhaust of the molecular turbo pump; and a vacuum gauge for measuring the degree of vacuum of the enrichment and purification device.
Preferably, in the enrichment and purification device descried above, the enrichment cold and hot trap is a spiral tube with a spiral axis.
Preferably, in the enrichment and purification device described above, the pre-purification cold trap is a U-shaped tube with a U-shaped axis.
It may be seen from the above technical solution that the enrichment and purification device for a single gas in a mixed gas provided by the present invention comprises: a pre-purification cold trap capable of freezing and adsorbing part of non-target gases in the mixed gas, the pre-purification cold trap provided with a mixed gas inlet for the mixed gas to enter; an enrichment cold and hot trap capable of adsorbing the target gas in the mixed gas when frozen, and capable of releasing the adsorbed purified target gas when heated, the enrichment cold and hot trap detachably filled with molecular sieves of different specifications, the gas inlet of the enrichment cold and hot trap connected with the gas outlet of the pre-purification cold trap through a first switching valve; a freezing unit for reducing the temperature of the enrichment cold and hot trap so that the enrichment cold and hot trap absorbs the target gas; a vacuum acquisition system for enabling the enrichment and purification device to reach a preset vacuum degree and capable of exhausting out of the enrichment cold and hot trap other non-target gases in the mixed gas that are not adsorbed, the suction of the vacuum acquisition system connected with the gas outlet of the enrichment cold and hot trap; a heating unit for heating the enrichment cold and hot trap to completely release the target gas adsorbed by the enrichment cold and hot trap; a purification outlet connected to the gas outlet of the enrichment cold and hot trap through a second switching valve.
It is applied in the following means: firstly, by the vacuum acquisition system, placing the enrichment and purification device at the preset vacuum degree, and opening the first switching valve and closing the second switching valve; passing the mixed gas through the mixed gas inlet
2020100284 26 Feb 2020 of the pre-purification cold trap to freeze and absorb, by the pre-purification cold trap, part of non-target gases in the mixed gas; then passing the remaining gas into the enrichment cold and hot trap, and reducing, by the freezing unit, the temperature of the enrichment cold and hot trap; and then based on the molecular weight or freezing point of the target gas to be purified, either selecting to adsorb the target gas by the enrichment cold and hot trap itself, or absorbing the target gas through the molecular sieves of different specifications in the enrichment cold and hot trap; after the target gas is completely adsorbed, exhausting, by the vacuum acquisition system, other non-target gases in the mixed gas that are not adsorbed out of the enrichment cold and hot trap; and finally, closing the first switching valve, and opening the second switching valve, and heating, by the heating unit, the enrichment cold and hot trap to completely release the target gas adsorbed by the enrichment cold and hot trap, thereby obtaining a purified target gas at the purification outlet, which may then be sent to next analysis step.
In summary, the enrichment and purification device for a single gas in a mixed gas by the present invention realizes the extraction and purification of a single gas in a mixed gas with different molecular weights.
Brief Description of the Drawings
In order to more clearly explain the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. It may be apparent for those skilled in the art that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an enrichment and purification device for a single gas in a mixed gas according to an embodiment of the present invention.
Detailed Description of the Invention
Embodiments of the present invention provide an enrichment and purification device for a single gas in a mixed gas, so as to realize the extraction and purification of a single gas in a mixed gas with different molecular weights.
In order to make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described with reference to the accompanying drawings in the
2020100284 26 Feb 2020 embodiments of the present invention. It is apparent that the described embodiments are a part of the embodiments of the present invention, but not all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by a person of ordinary skill in the art without creative efforts are fall within the protection scope of the present invention.
Referring to FIG. 1, the enrichment and purification device for a single gas in a mixed gas provided by the embodiments of the present invention comprises: a pre-purification cold trap 10 capable of freezing and adsorbing part of non-target gases in the mixed gas, the pre-purification cold trap 10 provided with a mixed gas inlet for the mixed gas to enter; an enrichment cold and hot trap 1 capable of adsorbing the target gas in the mixed gas when frozen, and capable of releasing the adsorbed purified target gas when heated, the enrichment cold and hot trap 1 detachably filled with molecular sieves of different specifications, the gas inlet of the enrichment cold and hot trap 1 connected with the gas outlet of the pre-purification cold trap 10 through a first switching valve; a freezing unit for reducing the temperature of the enrichment cold and hot trap 1 so that the enrichment cold and hot trap 1 absorbs the target gas; a vacuum acquisition system for enabling the enrichment and purification device to reach a preset vacuum degree and capable of exhausting other non-target gases in the mixed gas that are not adsorbed out of the enrichment cold and hot trap 1, the suction of the vacuum acquisition system connected with the gas outlet of the enrichment cold and hot trap 1; a heating unit for heating the enrichment cold and hot trap 1 to completely release the target gas adsorbed by the enrichment cold and hot trap 1; a purification outlet connected to the gas outlet of the enrichment cold and hot trap 1 through a second switching valve.
The enrichment cold and hot trap 1 is used to freeze and enrich the target gas to be analyzed.
The vacuum acquisition system is used to obtain the required vacuum degree in the system, and keep the vacuum of the pipeline and the pre-purification cold trap 10 and the enrichment cold and hot trap 1.
Specifically, the pre-purification cold trap 10 freezes and absorbs part of non-target gases in the mixed gas by a liquid nitrogen cup sleeved thereon. Certainly, depending on the non-target gases to be adsorbed, the liquid nitrogen cup may also be replaced with other freezing devices, such as a carbon dioxide cold liquid device, etc.
It is applied in the following means: firstly, by the vacuum acquisition system, placing the
2020100284 26 Feb 2020 enrichment and purification device at the preset vacuum degree, and opening the first switching valve and closing the second switching valve; passing the mixed gas through the mixed gas inlet of the pre-purification cold trap 10 to freeze and absorb, by the pre-purification cold trap 10, part of non-target gases in the mixed gas; then passing the remaining gas into the enrichment cold and hot trap 1, and reducing, by the freezing unit, the temperature of the enrichment cold and hot trap 1; and then based on the molecular weight or freezing point of the target gas to be purified, either selecting to adsorb the target gas by the enrichment cold and hot trap 1 itself, or absorbing the target gas through the molecular sieves of different specifications in the enrichment cold and hot trap 1; after the target gas is completely adsorbed, exhausting, by the vacuum acquisition system, other non-target gases in the mixed gas that are not adsorbed out of the enrichment cold and hot trap 1; and finally, closing the first switching valve, and opening the second switching valve, and heating, by the heating unit, the enrichment cold and hot trap 1 to completely release the target gas adsorbed by the enrichment cold and hot trap 1, thereby obtaining a purified target gas at the purification outlet, which may then be sent to next analysis step.
In summary, the enrichment and purification device for a single gas in a mixed gas provided in this embodiment realizes the extraction and purification of a single gas in a mixed gas of different molecular weights. The gases that may be directly frozen, enriched and purified include H2O, CO2, SO2, NH3, N2, and O2, etc. O2 and N2 may be frozen, enriched and purified by loading 10A and 5A molecular sieves into the enrichment cold and hot trap 1, respectively.
Preferably, the freezing unit comprises a freezing sleeve 2; a self-adapting liquid nitrogen tank 3 storing liquid nitrogen, the self-adapting liquid nitrogen tank 3 introducing the liquid nitrogen required for freezing the target gas into the freezing sleeve 2 through a conduit, the conduit extending below the level of the liquid nitrogen of the self-adapting liquid nitrogen tank 3; a heating module 4 for vaporizing the liquid nitrogen in the self-adapting liquid nitrogen tank 3 to generate pressure to introduce the liquid nitrogen into the freezing sleeve 2.
Specifically, the inner diameter of the freezing sleeve 2 is about 2 mm larger than the outer diameter of the enrichment cold and hot trap 1. The liquid nitrogen in the freezing sleeve 2 is used to cool the enrichment cold and hot trap 1 to a low temperature required for freezing the target gas. The self-adapting liquid nitrogen tank 3 is in a semi-sealed state, and only supplies liquid nitrogen to the freezing sleeve 2 through a conduit.
In this embodiment, the liquid nitrogen in the self-adapting liquid nitrogen tank 3 is vaporized by
2020100284 26 Feb 2020 the heating module 4 to generate pressure to introduce the liquid nitrogen automatically into the freezing sleeve 2 through the conduit, to reduce the temperature of the enrichment cold and hot trap 1 with the freezing sleeve 2, so that the enrichment cold and hot trap 1 reaches the freezing temperature of the target gas. The liquid nitrogen entering into the freezing sleeve 2 may be adjusted according to different target gas, thereby facilitating the control of the freezing temperature of the enrichment cold and hot trap 1.
It may be appreciated that the above-mentioned freezing unit may also be a liquid nitrogen bucket, which achieves the same effect of adjusting the freezing temperature of the enrichment cold and hot trap 1 by controlling the amount of liquid nitrogen in the liquid nitrogen bucket. Certainly, the above liquid nitrogen may also be replaced with another cold liquid, such as a mixed liquid of liquid nitrogen and anhydrous alcohol, or a carbon dioxide cold liquid and the like.
In a further technical solution, the freezing unit further comprises a tapered guide structure provided at the end of the conduit extending into the self-adapting liquid nitrogen tank 3, the tapered guide structure gradually diverging from the end proximal to the freezing sleeve 2 to the end distant from the freezing sleeve 2, the heating module 4 disposed in the tapered guide structure. The tapered guide structure is used to gather the pressure generated by the heating module 4 in heating the liquid nitrogen, and push the liquid nitrogen into the freezing sleeve 2 to facilitate the output of the liquid nitrogen. Of course, in the present application, the above-mentioned tapered guide structure may also be replaced with a structure with an opening larger than the through hole of the conduit.
In order to prolong the life, the freezing sleeve 2 is a polytetrafluoroethylene sleeve, the conduit is a polytetrafluoroethylene tube, and the tapered guide structure is a metal tapered tube 5. Of course, the above components may also be replaced with other suitable materials.
Preferably, the enrichment and purification device further comprises a first temperature control probe for detecting the freezing temperature of the enrichment cold and hot trap 1; a freezing temperature controller 7 for controlling the amount of liquid nitrogen entering into the freezing sleeve 2, the freezing temperature controller 7 connected to the first temperature control probe and the heating module 4. The first temperature control probe is placed at the enrichment cold and hot trap 1. This application automatically controls the amount of liquid nitrogen entering into the freezing sleeve 2 through the freezing temperature controller 7. When the freezing temperature of the enrichment cold and hot trap 1 detected by the first temperature control probe is higher than
2020100284 26 Feb 2020 the preset target gas freezing temperature, the freezing temperature controller 7 controls the heating unit to heat up. When the freezing temperature of the enrichment cold and hot trap 1 detected by the first temperature control probe is lower than the preset target gas freezing temperature, the freezing temperature controller 7 controls heating unit to reduce the temperature. It saves time and effort, and facilitates accurate control of the freezing temperature of the cold liquid, which improves the accuracy of the analysis. The present invention may also manually control the heating temperature of the heating module 4.
To further simplify the structure, the enrichment cold and hot trap 1 is a stainless steel cold and hot trap, and the heating unit is a heating wire provided on the stainless steel cold and hot trap. In this application, the stainless steel cold and hot trap is directly heated by the heating wire, thereby releasing the adsorbed target gas. This structure is relatively simple. Certainly, the above-mentioned enrichment cold and heat trap 1 may also use other media. The heating unit may also have other structures, such as a heater.
The enrichment and purification device further comprises a second temperature control probe for detecting the heating temperature of the enrichment cold and hot trap 1; a heating temperature controller 6 for controlling the heating temperature of the heating wire, the heating temperature controller 6 connected to the second temperature control probe and the heating wire. The second temperature control probe is placed at the enrichment cold and hot trap 1. This application automatically controls the heating temperature of the enrichment cold and hot trap 1 through the heating temperature controller 6. When the heating temperature of the enrichment cold and hot trap 1 detected by the second temperature control is lower than the preset target gas release temperature, the heating temperature controller 6 controls the heating wire to heat up. When the heating temperature of the enrichment cold and hot trap 1 detected by the second temperature control probe is higher than the preset target gas release temperature, the heating temperature controller 6 controls the heating wire to stop heating, which facilitates the accurate control of the heating temperature of the enrichment cold and hot trap 1. The present invention may also manually control the heating temperature of the heating wire.
The vacuum acquisition system comprises: a molecular turbo pump 8, the suction of the molecular turbo pump 8 connected to the gas outlet of the enrichment cold and heat trap 1; a mechanical pump, the suction of the mechanical pump connected to the exhaust of the molecular turbo pump 8; a vacuum gauge 9 for measuring the degree of vacuum of the enrichment the purification device. As the structure of the vacuum acquisition system is relatively simple, and certainly may also be
2020100284 26 Feb 2020 replaced with other structures capable of vacuuming, it will not be exemplified in detail in the present invention.
In order to ensure the adsorption effect of the enrichment cold and hot trap 1, the enrichment cold and hot trap 1 is a spiral tube having a spiral axis. The adsorption capacity of the enrichment cold and hot trap 1 is relatively large, which ensures the purification effect. Certainly, the enrichment cold and heat trap 1 may also have other shapes, such as a serpentine tube and the like.
Preferably, the pre-purification cold trap 10 is a U-shaped tube with a U-shaped axis, and may also be other shapes, such as a serpentine tube.
There are two main cases when purifying a specific gas from a mixed gas:
In the first case, a gas with a lighter molecular weight or a relatively low freezing point is extracted from the mixed gas. For example, N2 and O2 are extracted and purified from a mixed gas containing H2O, CO2, N2, and O2. First, the vacuum acquisition system, including a mechanical pump and a molecular turbo pump 8, is used to place the pipeline of the enrichment and purification device at the required vacuum degree, and the vacuum gauge 9 is used to determine the vacuum degree.
The mixed gas is passed through the pipeline of the enrichment and purification device, where the pre-purification cold trap 10 is provided with a liquid nitrogen cup sleeved thereon. The mixed gas first passes through the pre-purification cold trap 10. As the freezing points of H2O and CO2 are 0°C and -78.5%°C respectively, and the temperature of liquid nitrogen is -195.8°C, the H2O and CO2, etc. therein will be frozen first. Completion of the freezing may be determined by vacuum gauge 9. As the freezing points of N2 and O2 are -209.8°C and- 218°C, so they cannot be adsorbed.
The purified mixed gas of N2 and O2 enters into the stainless steel cold and hot trap. At the same time, the freezing temperature controller 7 is used to set the freezing temperature as the nitrogen liquefaction temperature. For the adsorption of N2 and O2, molecular sieves must be filled in the stainless steel cold and hot trap to adsorb O2, where a 10A molecular sieve is required to be filled to absorb O2, and a 5A molecular sieve is required to be filled to absorb N2. The adsorbed N2 or O2 is purified by a molecular turbo pump 8, and the vacuum gauge 9 may be used to detect the purification process. The purified N2 or O2 then uses the heating temperature controller 6 to set the
2020100284 26 Feb 2020 heating temperature as 120°C, at which the target gas adsorbed in the molecular sieve may be completely desorbed. The degree of gas release may be detected using the vacuum gauge 9. In this way, the N2 or O2 extracted and purified from the mixed gas may proceed to the next analysis step.
In the second case, a gas with a relatively heavy molecular weight or a relatively high freezing point is extracted from the mixed gas. Taking the above mixed gas as an example, H2O or CO2 is extracted and purified therefrom. First, the vacuum acquisition system, including a mechanical pump and a molecular turbo pump 8, is used to place the pipeline of the enrichment and purification device at the required vacuum degree, and the vacuum gauge 9 is used to determine the vacuum degree.
When extracting and purifying CO2, the mixed gas passes into the pipeline of the enrichment and purification device. Since the freezing points of H2O and CO2 are 0°C and -78.5°C, respectively, H2O therein is frozen by controlling the temperature of the pre-purification cold trap 10 to set this temperature between the freezing points of H2O and CO2. The completion of freezing may be determined by the vacuum gauge 9. The remaining mixed gas is then entered into the stainless steel cold and hot trap, so that CO2 is adsorbed in the stainless steel cold and hot trap by setting the temperature of the stainless steel cold and hot trap at lower than the CO2 adsorption temperature, where the CO2 adsorption temperature is set to -90°C.
When the purified H2O is extracted and purified, the mixed gas is passed into the pipeline of the enrichment and purification device, while the pre-purification cold trap 10 is kept at a normal temperature. The extraction and purification processes are both performed in a stainless steel cold and hot trap. The freezing temperature controller 7 is used to set the H2O adsorption temperature lower than the freezing point of H2O. The H2O adsorption temperature is set to -15 °C to ensure that only H2O is adsorbed.
After the purification of the above two gases, the vacuum gauge 9 is used to determine the completion of the adsorption. After the adsorption is completed, the molecular turbine pump 8 is first used to pump away other gases in the pipeline to achieve the purpose of purifying the target gas. The purification process is detected using a vacuum gauge 9. When the gas purification is completed, the heating temperature is set to 120 °C by using the heating temperature controller 6, which may be able to completely desorb the target gas adsorbed in the stainless steel cold and hot trap. The degree of gas release is detected by the vacuum gauge 9. In this way, the H2O or CO2 extracted and purified from the mixed gas may proceed to the next analysis step.
The enrichment and purification device for a single gas in a mixed gas provided by the present invention has the following advantages.
1. Broad scope of application. No matter it is a simple mixed gas or a complex mixed gas mixed with different molecular weights, the present invention may effectively enrich and purify a gas of a certain molecular weight.
2. High accuracy of analysis. Because the high-vacuum pipeline design of the molecular turbo pump 8 is adopted, and the internal volume of the system pipeline is small, the analysis accuracy may be improved by an order of magnitude compared with the traditional methods.
3. Efficient and simple analysis process. As the integrated module design is adopted, and the freezing and desorption of the system are controlled automatically, the analysis efficiency is greatly improved compared with the traditional methods.
The invention will provide an efficient and feasible instrument analysis platform for the research of earth science and environmental science.
The embodiments in this specification are described in a progressive manner. Each embodiment focuses on the differences from other embodiments. Simply refer to each other for the same and similar parts between the embodiments.
The above description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the present invention will not be limited to the embodiments shown herein, but should conform to the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
- Claims1. An enrichment and purification device for a single gas in a mixed gas, characterized by comprising:a pre-purification cold trap (10) capable of freezing and adsorbing part of non-target gases in the mixed gas, the pre-purification cold trap (10) provided with a mixed gas inlet for the mixed gas to enter;an enrichment cold and hot trap (1) capable of adsorbing the target gas in the mixed gas when frozen, and capable of releasing the adsorbed purified target gas when heated, the enrichment cold and hot trap (1) detachably filled with molecular sieves of different specifications, the gas inlet of the enrichment cold and hot trap (1) connected with the gas outlet of the pre-purification cold trap (10) through a first switching valve;a freezing unit for reducing the temperature of the enrichment cold and hot trap (1) so that the enrichment cold and hot trap (1) absorbs the target gas;a vacuum acquisition system for enabling the enrichment and purification device to reach a preset vacuum degree and capable of exhausting other non-target gases in the mixed gas that are not adsorbed out of the vacuum acquisition system of the enrichment cold and hot trap (1), the suction of the vacuum acquisition system connected with the gas outlet of the enrichment cold and hot trap (1);a heating unit for heating the enrichment cold and hot trap (1) to completely release the target gas adsorbed by the enrichment cold and hot trap (1); and a purification outlet connected to a gas outlet of the enrichment cold and hot trap (1) through a second switching valve.
- 2. The enrichment and purification device according to claim 1, characterized in that the freezing unit comprises: a freezing sleeve (2) sleeved on the enrichment cold and heat trap (1);a self-adapting liquid nitrogen tank (3) storing liquid nitrogen, the self-adapting liquid nitrogen2020100284 26 Feb 2020 tank (3) introducing the liquid nitrogen required for freezing the target gas into the freezing sleeve (2) through a conduit, the conduit extending below the level of the liquid nitrogen of the self-adapting liquid nitrogen tank (3);a heating module (4) for vaporizing the liquid nitrogen in the self-adapting liquid nitrogen tank (3) to generate pressure to introduce the liquid nitrogen into the freezing sleeve (2).
- 3. The enrichment and purification device according to claim 2, characterized in that the freezing unit further comprises:a tapered guide structure provided at the end of the conduit extending into the self-adapting liquid nitrogen tank (3), the tapered guide structure gradually diverging from the end proximal to the freezing sleeve (2) to the end distant from the freezing sleeve (2), the heating module (4) disposed in the tapered guide structure.
- 4. The enrichment and purification device according to claim 3, characterized in that the freezing sleeve (2) is a polytetrafluoroethylene sleeve, the conduit is a polytetrafluoroethylene tube, and the tapered guide structure is a metal tapered tube (5).
- 5. The enrichment and purification device according to any one of claims 2-4, characterized in that it further comprises a first temperature control probe for detecting the freezing temperature of the enrichment cold and hot trap (1);a freezing temperature controller (7) for controlling the amount of liquid nitrogen entering into the freezing sleeve (2), the freezing temperature controller (7) connected to the first temperature control probe and the heating module (4).
- 6. The enrichment and purification device according to claim 1, characterized in that, the enrichment cold and hot trap (1) is a stainless steel cold and hot trap, and the heating unit is a heating wire provided on the stainless steel cold and hot trap.
- 7. The enrichment and purification device according to claim 6, characterized in that it further comprises a second temperature control probe for detecting the heating temperature of the enrichment cold and hot trap (1);2020100284 26 Feb 2020 a heating temperature controller (6) for controlling the heating temperature of the heating wire, the heating temperature controller (6) connected to the second temperature control probe and the heating wire.
- 8. The enrichment and purification device according to claim 1, characterized in that, the vacuum acquisition system further comprises:a molecular turbo pump (8), a suction of the molecular turbo pump (8) connected to the gas outlet of the enrichment cold and hot trap (1);a mechanical pump, a suction of the mechanical pump connected to the exhaust of the molecular turbo pump (8); and a vacuum gauge (9) for measuring the degree of vacuum of the enrichment and purification device.
- 9. The enrichment and purification device according to claim 1, characterized in that the enrichment cold and hot trap (1) is a spiral tube having a spiral axis.
- 10. The enrichment and purification device according to claim 1, characterized in that the pre-purification cold trap (10) is a U-shaped tube with a U-shaped axis.
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| Application Number | Priority Date | Filing Date | Title |
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| AU2020100284A AU2020100284A4 (en) | 2020-02-26 | 2020-02-26 | Enrichment and Purification Device for Single Gas in Mixed Gas |
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| AU2020100284A AU2020100284A4 (en) | 2020-02-26 | 2020-02-26 | Enrichment and Purification Device for Single Gas in Mixed Gas |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114441282A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Concentration and enrichment device and method for rare gas in soil gas and application |
| CN114910593A (en) * | 2022-03-14 | 2022-08-16 | 中海油能源发展股份有限公司 | High-temperature molten carbonate enriched carbon dioxide gas purification system and use method thereof |
| CN115108879A (en) * | 2021-03-23 | 2022-09-27 | 中国石油化工股份有限公司 | Light hydrocarbon component separation, collection and online quantification device and method |
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2020
- 2020-02-26 AU AU2020100284A patent/AU2020100284A4/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114441282A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Concentration and enrichment device and method for rare gas in soil gas and application |
| CN114441282B (en) * | 2020-11-02 | 2024-05-07 | 中国石油化工股份有限公司 | Concentration and enrichment device for rare gas in soil gas, concentration and enrichment method and application |
| CN115108879A (en) * | 2021-03-23 | 2022-09-27 | 中国石油化工股份有限公司 | Light hydrocarbon component separation, collection and online quantification device and method |
| CN114910593A (en) * | 2022-03-14 | 2022-08-16 | 中海油能源发展股份有限公司 | High-temperature molten carbonate enriched carbon dioxide gas purification system and use method thereof |
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