CN115869740A - Device and method for purifying gas impurities in Xe based on graphene film - Google Patents

Device and method for purifying gas impurities in Xe based on graphene film Download PDF

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Publication number
CN115869740A
CN115869740A CN202211691503.9A CN202211691503A CN115869740A CN 115869740 A CN115869740 A CN 115869740A CN 202211691503 A CN202211691503 A CN 202211691503A CN 115869740 A CN115869740 A CN 115869740A
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flange
box body
graphene oxide
gas
purifying
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陈俊哲
顾志勇
陈熙
吴重钧
吴文娟
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Research Institute of Physical and Chemical Engineering of Nuclear Industry
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Research Institute of Physical and Chemical Engineering of Nuclear Industry
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Priority to CN202211691503.9A priority Critical patent/CN115869740A/en
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Abstract

The invention discloses a device and a method for purifying gas impurities in Xe (Xe) based on a graphene oxide film, wherein the device comprises a box body, the side surface of the box body is provided with a flange structure, the flange structure is provided with an impurity gas extraction opening, and the flange structure comprises a concave flange fixed with the side surface of the box body and a convex flange connected with the concave flange; the purification method comprises introducing Xe gas containing impurity gas into the box via gas inlet, pumping out impurity gas via impurity gas pumping port, and maintaining the internal pressure of the box at 20hPa and temperature at 20 deg.C during purification. The invention utilizes the graphene oxide membrane to filter impurities mixed in the Xe production process, so that the obtained Xe product meets delivery requirements, provides a new technical route for gas purification, and provides possibility for applying the graphene oxide membrane to the purification of other gases in the future.

Description

Device and method for purifying gas impurities in Xe based on graphene film
Technical Field
The invention belongs to the field of gas filtration and purification, and particularly relates to a device and a method for purifying gas impurities in Xe based on a graphene oxide membrane.
Background
Xe isotopes have a high application value and therefore create certain use requirements, which are currently met by means of industrial production. In the production process of Xe, due to the problems of equipment sealing, gas transportation and the like, other gas impurities are inevitably doped in Xe, so that the obtained product cannot meet delivery requirements, and the Xe must be purified. In view of the high value of Xe, it is desirable to minimize the loss of Xe during the purification process; in view of the difficulty of meeting the above requirements with the currently known gas purification techniques, new gas purification techniques need to be explored.
At present, there are many examples of purifying and separating liquid-solid mixtures by using a filtering membrane, such as crude salt purification and seawater desalination; compared with other methods, the filtering membrane has many advantages, taking seawater desalination as an example, if fresh water is extracted from the sea by distillation, a large amount of energy is wasted, which is contrary to the current trend of "energy conservation and emission reduction", and the existing commercial cellulose triacetate desalination membrane completely avoids the disadvantage.
The molecular size of gases tends to be smaller than liquids, so separation of gas mixtures with membranes is more difficult than separation of liquid mixtures; therefore, the technology of the filtering membrane is only applied to a certain extent in the liquid field at present, and there are few cases of applying the related technology in the gas field, and particularly, no reference is made to the purification method of Xe.
Disclosure of Invention
The invention provides a method for solving the problem that the existing gas purification technology is determined when applied to Xe purification, and aims to provide a method for purifying gas impurities in Xe based on a graphene oxide film.
In order to achieve the purpose, the invention adopts the following technical scheme:
a device for purifying gas impurities in Xe based on a graphene oxide membrane comprises a box body, wherein a flange structure is arranged on the side surface of the box body, the flange structure is provided with an impurity gas pumping hole communicated with the interior of the box body, the flange structure comprises a concave flange fixed with the side surface of the box body and a convex flange connected with the concave flange, and a filtering membrane is arranged between the concave flange and the convex flange; the case is provided with a gas inlet and a Xe outlet.
In the above technical solution, the gas inlet is arranged at the bottom of the box body, and the Xe outlet is arranged at the top of the box body.
In the technical scheme, a container pressure measuring point interface is arranged on the side face of the box body and connected with a barometer.
In the technical scheme, the container pressure measuring point interface and the flange structure are arranged on different side surfaces of the box body.
In the technical scheme, the through hole is formed in the middle of the concave flange, the end face of the concave flange, which deviates from the box body, forms an inner groove and an outer groove which are concentric, the end face of the concave flange, which is connected with the box body, forms an inner pumping hole, and the inner pumping hole extends into the box body and is coaxial with the through hole in the middle of the concave flange.
In the technical scheme, the through hole is formed in the middle of the convex flange, the end face, close to the concave flange, of the convex flange forms the inner convex ring and the outer convex ring which are concentric, the inner convex ring and the inner groove are arranged in a one-to-one correspondence mode, and the sealing gaskets are arranged between the inner convex ring and the inner groove and between the outer convex ring and the outer groove.
In the technical scheme, an impurity gas pumping hole and an outlet pressure measuring point interface are formed on the end face, back to the concave flange, of the convex flange, the impurity gas pumping hole is communicated with a through hole of the convex flange and is coaxial, and the outlet pressure measuring point interface is communicated with a region between the inner convex ring and the outer convex ring.
In the above technical solution, the outlet pressure measurement point interface is arranged on the impurity gas extraction opening.
In the technical scheme, the filtering membrane assembly consists of a membrane and a base material arranged on the outer circumference of the membrane; the membrane is made of graphene oxide, the thickness of the membrane is not more than 3 mm, and the interlayer spacing of the graphene oxide membrane is 0.37-0.52 nm; the base material is made of polytetrafluoroethylene or ceramic.
A method for purifying gaseous impurities in Xe based on a graphene oxide membrane comprises the steps of introducing Xe gas containing impurity gas into a box body from a gas inlet, extracting the impurity gas through an impurity gas extraction opening, and keeping the internal pressure of the box body at 20hPa and the temperature at 20 ℃ in the purification process.
The invention has the beneficial effects that:
the invention provides a method for purifying gas impurities in Xe based on a graphene oxide film, which can effectively remove impurity gases (such as N) contained in Xe 2 ) Impurities mixed in the Xe during the production process of the Xe are filtered by using the graphene oxide film, so that the obtained Xe product meets the delivery requirement. The invention not only expands the application range of the graphene oxide membrane, but also provides a new technical route for the purification of gases, and provides possibility for applying the graphene oxide membrane to the purification of other gases in the future.
Drawings
FIG. 1 is a schematic structural view of an apparatus for purifying gaseous impurities in Xe based on a graphene oxide film according to the present invention;
FIG. 2 is a front view of a concave flange in the apparatus for purifying gaseous impurities in Xe based on graphene oxide film according to the present invention;
FIG. 3 is a rear view of a concave flange in the apparatus for purifying gaseous impurities in Xe based on graphene oxide films according to the present invention;
FIG. 4 is a front view of a convex flange in the apparatus for purifying gaseous impurities in Xe based on graphene oxide film according to the present invention;
FIG. 5 is a rear view of a convex flange in the apparatus for purifying gaseous impurities in Xe based on graphene oxide film according to the present invention;
FIG. 6 is a schematic view of an assembly structure of a concave flange and a convex flange in the apparatus for purifying gaseous impurities in Xe based on a graphene oxide film according to the present invention;
fig. 7 is a schematic structural view of a graphene film in the apparatus for purifying gaseous impurities in Xe based on a graphene oxide film according to the present invention.
Wherein:
1 case 2 concave flange
3 convex flange 4 gas inlet
5Xe export 6 container pressure measurement point interface
7 impurity gas extraction opening 8 outlet pressure measuring point interface
9 outer groove 10 inner groove
11 inner flange hole 12 inner pumping hole
13 outer convex ring and 14 inner convex ring
15 outer flange hole 16 filter membrane
17 a membrane 18 substrate.
For a person skilled in the art, without inventive effort, other relevant figures can be derived from the above figures.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the technical solutions of the present invention based on the method for purifying gaseous impurities in Xe by using graphene oxide film will be further described below by means of specific embodiments in conjunction with the drawings of the specification.
Example 1
As shown in fig. 1 and 6, an apparatus for purifying gas impurities in Xe based on a graphene oxide membrane comprises a box 1, wherein a flange structure is arranged on the side surface of the box 1, the flange structure is provided with an impurity gas extraction opening 7, the flange structure comprises a concave flange 2 fixed on the side surface of the box 1 and a convex flange 3 connected with the concave flange 2, and a filter membrane 16 is arranged between the concave flange 2 and the convex flange 3.
The bottom of the box body 1 is provided with a gas inlet 4, the top of the box body is provided with an Xe outlet 5, the side surface of the box body is provided with a container pressure measuring point interface 6, the container pressure measuring point interface 6 is used for connecting a barometer, and the pressure condition in the box body 1 is known through the barometer. The gas inlet 4, the Xe outlet 5 and the impurity gas pumping port 7 of the flange structure on the box body 1 form a gas flow passage of 'one inlet and two outlets'.
In this embodiment, the box body 1 is a rectangular parallelepiped structure, and the vessel pressure measurement point interface 6 and the flange structure are disposed on different sides of the box body 1.
As shown in fig. 2 and 3, a through hole is formed in the middle of the concave flange 2, an inner groove 10 and an outer groove 9 which are concentric with each other are formed on the end surface of the concave flange 2 away from the box body 1, an inner pumping hole 12 is formed on the end surface of the concave flange 2 connected with the box body 1, and the inner pumping hole 12 extends into the box body 1 and is coaxial with the through hole in the middle of the concave flange 2. The concave flange 2 is evenly distributed with a plurality of inner flange holes 11 along the circumference.
As shown in fig. 4 and 5, a through hole is formed in the middle of the convex flange 3, a plurality of outer flange holes 15 are uniformly distributed along the circumference, the outer flange holes 15 and the inner flange holes 11 are arranged in a one-to-one correspondence manner, and the fixed connection between the concave flange 2 and the convex flange 3 is realized; the through hole of the convex flange 3 is coaxial with the through hole of the concave flange 2;
the end face, close to the concave flange 2, of the convex flange 3 forms an inner convex ring 14 and an outer convex ring 13 which are concentric, the inner convex ring 14 and the inner groove 10, the outer convex ring 13 and the outer groove 9 are arranged in a one-to-one correspondence mode and are tightly matched, and sealing gaskets are arranged between the inner convex ring 14 and the inner groove 10 and between the outer convex ring 13 and the outer groove 9;
an impurity gas pumping hole 7 and an outlet pressure measuring point interface 8 are formed in the end face, back to the concave flange 2, of the convex flange 3, the impurity gas pumping hole 7 is communicated with a through hole of the convex flange 3 and is coaxial, and the outlet pressure measuring point interface 8 is communicated with a region between the inner convex ring 14 and the outer convex ring 13.
The inner convex ring 14 and the inner groove 10, the outer convex ring 13 and the outer groove 9 and the corresponding sealing gaskets form an inner and outer double-ring sealing structure, the inner ring sealing structure can be used for fixing and sealing the graphene film 16, and the outer ring sealing structure is used for preventing external air from entering the box body of the experimental system due to failure damage or air leakage of the graphene film.
As shown in FIG. 7, the filtering membrane 16 is coaxially arranged with the inner convex ring 14 and the outer convex ring 13, and the filtering membrane 16 assembly is composed of a membrane 17 and a base material 18 arranged on the outer circumference of the membrane.
The thickness of the diaphragm 17 is not more than 3 mm, the specific thickness is determined by a used base material, the diaphragm 17 is made of graphene oxide, the interlayer distance of the graphene oxide film is 0.37-0.52 nm, and different interlayer distances are generated after the graphene oxide film is reacted with different ionic solutions.
The substrate 18 is made of teflon or ceramic.
Example 2
Based on embodiment 1, in this embodiment, the outlet pressure measuring point interface 8 is disposed on the impurity gas pumping port 7.
Example 3
Based on example 1, a method for purifying gaseous impurities in Xe based on a graphene film, wherein Xe gas containing impurity gas is introduced into a chamber through a gas inlet 4, and impurity gas (N) is extracted through an impurity gas extraction opening 7 2 ) Pumping out, and maintaining the internal pressure of the box at 20hPa and the temperature at 20 ℃ in the purification process.
The air extraction process can adopt two air flow paths of one inlet and one outlet (incapable of continuous purification) and one inlet and two outlets (continuous purification). "one-in one-out" (incapable of continuous purging), i.e., the impurity gas pumping port 7 and the Xe outlet 5 do not discharge gas at the same time, "one-in two-out" (continuous purging), i.e., the impurity gas pumping port 7 and the Xe outlet 5 discharge gas at the same time. The purification of the gas can be realized by one inlet and one outlet and one inlet and two outlets, and the purification of the Xe gas can be realized by only adjusting the inlet flow rate and the exhaust flow rate to keep the internal pressure of the box body at 20 hPa.
The working principle of the invention is as follows:
the present invention uses a graphene oxide membrane to accomplish the purification of Xe, and its principle is that there is a certain distance (about 0.5 nm) between the sheets of the graphene membrane, and since different molecules have different sizes (diameters), when the size of a molecule is smaller than the interlayer spacing of the graphene oxide membrane, the molecule can pass through the graphene oxide membrane, and the smaller the molecule is, the faster its passing rate is, and if the size of the molecule is larger than the interlayer spacing of the graphene oxide membrane, the molecule cannot pass (is trapped); experiments show that different hydrated ions have different sizes, and the graphene oxide film can generate different interlayer distances after being acted with different ion solutions, so that the interlayer distance of the graphene oxide film is adjusted by changing the hydrated ions according to the known interlayer distance of the graphene oxide film suitable for purifying Xe, the graphene oxide film capable of generating a purifying effect on the Xe is finally prepared, and the purification of the Xe is completed by using the graphene oxide film. By investigation and analysis of relevant theoretical and experimental data, xe and its impurity gases (in N) can be determined 2 Example) molecular characterization (kinetic diameter of Xe 0.396nm, N 2 Has a kinetic diameter of 0.364 nm), and thus a suitable range of the interlayer spacing of the graphene oxide film (about 0.37nm to 0.52 n) was determinedm) as a basis for preparing the graphene oxide film.
The purification of Xe is a process in which gas continuously flows, and in the flowing process, impurity gas is pumped away by an air pump through a graphene oxide membrane to complete the purification of Xe.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.

Claims (10)

1. An apparatus for purifying gaseous impurities in Xe based on graphene oxide film, characterized in that: the device comprises a box body (1), wherein a flange structure is arranged on the side surface of the box body (1), the flange structure is provided with an impurity gas pumping hole (7) communicated with the interior of the box body (1), the flange structure comprises a concave flange (2) fixed with the side surface of the box body (1) and a convex flange (3) connected with the concave flange (2), and a filtering membrane (16) is arranged between the concave flange (2) and the convex flange (3); the box (1) is provided with a gas inlet (4) and an Xe outlet (5).
2. The apparatus for purifying Xe gas impurities based on graphene oxide films according to claim 1, characterized in that: the gas inlet (4) is arranged at the bottom of the box body (1), and the Xe outlet (5) is arranged at the top of the box body (1).
3. The apparatus for purifying gaseous impurities in Xe based on graphene oxide films according to claim 1, characterized in that: the side surface of the box body (1) is provided with a container pressure measuring point interface (6), and the container pressure measuring point interface (6) is connected with a barometer.
4. The apparatus for purifying Xe gas impurities based on graphene oxide films according to claim 3, characterized in that: the container pressure measuring point interface (6) and the flange structure are arranged on different side surfaces of the box body (1).
5. The apparatus for purifying Xe gas impurities based on graphene oxide films according to claim 1, characterized in that: the middle of the concave flange (2) is provided with a through hole, the end face of the concave flange (2) deviating from the box body (1) forms an inner groove (10) and an outer groove (9) which are concentric, the end face of the concave flange (2) connected with the box body (1) forms an inner pumping hole (12), and the inner pumping hole (12) extends into the box body (1) and is coaxial with the through hole in the middle of the concave flange (2).
6. The apparatus for purifying gaseous impurities in Xe based on graphene oxide films according to claim 1, characterized in that: a through hole is formed in the middle of the convex flange (3), an inner convex ring (14) and an outer convex ring (13) which are concentric are formed on the end face, close to the concave flange (2), of the convex flange (3), the inner convex ring (14) and the inner groove (10) are arranged, the outer convex ring (13) and the outer groove (9) are arranged in a one-to-one correspondence mode, and sealing gaskets are arranged between the inner convex ring (14) and the inner groove (10) and between the outer convex ring (13) and the outer groove (9).
7. The apparatus for purifying Xe gas impurities based on graphene oxide films according to claim 6, characterized in that: an impurity gas pumping hole (7) and an outlet pressure measuring point interface (8) are formed in the end face, back to the concave flange (2), of the convex flange (3), the impurity gas pumping hole (7) is communicated with a through hole of the convex flange (3) and is coaxial, and the outlet pressure measuring point interface (8) is communicated with a region between the inner convex ring (14) and the outer convex ring (13).
8. The apparatus for purifying Xe gas impurities based on graphene oxide films according to claim 6, characterized in that: the outlet pressure measuring point interface (8) is arranged on the impurity gas pumping hole (7).
9. The apparatus for purifying gaseous impurities in Xe based on graphene oxide films according to claim 1, characterized in that: the filtering membrane (16) assembly consists of a membrane (17) and a base material (18) arranged on the outer circumference of the membrane; the membrane (17) is made of graphene oxide, the thickness of the membrane is not more than 3 mm, and the interlayer spacing of the graphene oxide membrane is 0.37-0.52 nm; the base material (18) is made of polytetrafluoroethylene or ceramic materials.
10. A method for purifying gaseous impurities in Xe based on graphene oxide film, characterized in that: xe gas containing impurity gas is introduced into the box body through a gas inlet (4), the impurity gas is pumped out through an impurity gas pumping hole (7), and the internal pressure of the box body is kept at 20hPa and the temperature is kept at 20 ℃ in the purification process.
CN202211691503.9A 2022-12-28 2022-12-28 Device and method for purifying gas impurities in Xe based on graphene film Pending CN115869740A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2070428C1 (en) * 1994-02-16 1996-12-20 Научно-технический кооператив "Контур" Membrane apparatus
US20090126733A1 (en) * 2007-05-23 2009-05-21 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Xenon recovery from ambient pressure ventilator loop
CN102437005A (en) * 2011-09-28 2012-05-02 上海大学 Membrane feeding device on gas analysis mass spectrometer
JP2020041956A (en) * 2018-09-13 2020-03-19 日立Geニュークリア・エナジー株式会社 Ventilation air conditioning system of nuclear power plant
CN113484399A (en) * 2021-05-20 2021-10-08 南京工业大学 Graphene film-based gas production testing method for metal ion battery, film assembly and preparation method
CN216677494U (en) * 2021-10-25 2022-06-07 华挺纳米科技(上海)有限公司 Silicon-based filter material for filtering gas
CN216856313U (en) * 2021-06-18 2022-07-01 南京高谦功能材料科技有限公司 Membrane module

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2070428C1 (en) * 1994-02-16 1996-12-20 Научно-технический кооператив "Контур" Membrane apparatus
US20090126733A1 (en) * 2007-05-23 2009-05-21 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Xenon recovery from ambient pressure ventilator loop
CN102437005A (en) * 2011-09-28 2012-05-02 上海大学 Membrane feeding device on gas analysis mass spectrometer
JP2020041956A (en) * 2018-09-13 2020-03-19 日立Geニュークリア・エナジー株式会社 Ventilation air conditioning system of nuclear power plant
CN113484399A (en) * 2021-05-20 2021-10-08 南京工业大学 Graphene film-based gas production testing method for metal ion battery, film assembly and preparation method
CN216856313U (en) * 2021-06-18 2022-07-01 南京高谦功能材料科技有限公司 Membrane module
CN216677494U (en) * 2021-10-25 2022-06-07 华挺纳米科技(上海)有限公司 Silicon-based filter material for filtering gas

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