CN113582144A - Nitrogen and argon terminal purification device and purification method - Google Patents
Nitrogen and argon terminal purification device and purification method Download PDFInfo
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- CN113582144A CN113582144A CN202010360269.6A CN202010360269A CN113582144A CN 113582144 A CN113582144 A CN 113582144A CN 202010360269 A CN202010360269 A CN 202010360269A CN 113582144 A CN113582144 A CN 113582144A
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 88
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 44
- 229910052786 argon Inorganic materials 0.000 title claims abstract description 43
- 238000000746 purification Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 11
- 230000003197 catalytic effect Effects 0.000 claims abstract description 48
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000001257 hydrogen Substances 0.000 claims abstract description 39
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 39
- 239000006096 absorbing agent Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 7
- 239000006200 vaporizer Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 5
- 239000003463 adsorbent Substances 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/04—Purification or separation of nitrogen
- C01B21/0405—Purification or separation processes
- C01B21/0494—Combined chemical and physical processing
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B23/00—Noble gases; Compounds thereof
- C01B23/001—Purification or separation processes of noble gases
- C01B23/0094—Combined chemical and physical processing
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0003—Chemical processing
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0009—Physical processing
- C01B2210/0014—Physical processing by adsorption in solids
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0043—Impurity removed
- C01B2210/0045—Oxygen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0043—Impurity removed
- C01B2210/0062—Water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0043—Impurity removed
- C01B2210/0098—Other impurities
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
The invention relates to the technical field related to nitrogen or argon purification, in particular to a nitrogen and argon terminal purification device and a purification method, wherein the nitrogen and argon terminal purification device comprises an adsorber and a catalytic reactor, and the adsorber and the catalytic reactor are communicated through a main path connecting pipe; electric heaters are respectively arranged on the absorber and the catalytic reactor; the adsorber and the catalytic reactor are also communicated with a flow passage communicated with a high-purity hydrogen bottle. The invention has novel design, dehydrates high-pressure nitrogen or high-pressure argon by the arranged absorber and other impurities, and deoxidizes the high-pressure nitrogen or the high-pressure argon by the catalytic reactor to obtain high-purity nitrogen or the high-purity argon, thereby ensuring the purification effect and having strong practicability.
Description
Technical Field
The invention relates to the technical field related to nitrogen or argon purification, in particular to a nitrogen and argon terminal purification device and a purification method.
Background
Most of the high-purity nitrogen or high-purity argon sold in the market at present is obtained by pumping liquid nitrogen or liquid argon from a cryogenic pump, vaporizing the liquid nitrogen or liquid argon by a vaporizer and filling a bottle with the vaporized liquid nitrogen or liquid argon.
However, when the high-purity liquid nitrogen or the high-purity liquid argon produced by the air separation plant is transported by the cryogenic tanker and then is refilled into the cryogenic storage tank of the production plant, because air pollution may be introduced during the operation process, the oxygen, nitrogen, water and total carbon content of the high-purity nitrogen or the high-purity argon produced by the polluted cryogenic liquid can not reach the quality technical index of the high-purity nitrogen or the high-purity argon specified by the national standard.
Disclosure of Invention
The invention aims to provide a nitrogen and argon terminal purification device and a purification method, which aim to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a terminal purification device for nitrogen and argon comprises an adsorber and a catalytic reactor, wherein the adsorber and the catalytic reactor are communicated through a main path connecting pipe;
electric heaters are respectively arranged on the absorber and the catalytic reactor;
the adsorber and the catalytic reactor are also communicated with a flow passage communicated with a high-purity hydrogen bottle.
As a further scheme of the invention: and the two ends of the main path connecting pipe are respectively provided with an air inlet and a collecting tank interface.
As a still further scheme of the invention: and a second valve body is arranged on the main path connecting pipe at one side of the adsorber, which is far away from the catalytic reactor, and a third valve body is arranged on the main path connecting pipe at one end of the catalytic reactor, which is far away from the adsorber.
As a still further scheme of the invention: and a fifth valve body and a fourth valve body are respectively arranged on the flow channel connected with the high-purity hydrogen bottle and at the positions respectively positioned at the side ends of the absorber and the catalytic reactor.
As a still further scheme of the invention: the main path connecting pipe is also communicated with a bypass connecting pipe, a first valve body is installed on the bypass connecting pipe, and ports at two ends of the bypass connecting pipe are respectively located at a position between the second valve body and the air inlet and a position between the third valve body and the collecting tank interface.
A terminal purification method of nitrogen and argon comprises the following steps:
s1, closing the first valve body, the second valve body and the third valve body, simultaneously opening the fourth valve body and the fifth valve body, then opening the high-purity hydrogen bottle, adjusting a hydrogen pressure reducer at the outlet of the high-purity hydrogen bottle, introducing high-purity hydrogen from the fourth valve body at a flow rate of 1.4-1.5 Nm3/h, and heating and activating a catalyst in the catalytic reactor and an adsorbent in the adsorber;
s2, turning on an electric heater to heat the adsorber and the catalytic reactor;
s3, closing the high-purity hydrogen bottle, the fourth valve body and the fifth valve body, closing the second valve body and the third valve body at the same time, opening the first valve body, and blowing off hydrogen in the bypass connecting pipe by using nitrogen or argon vaporized by the vaporizer;
s4, closing the first valve body, opening the second valve body and the third valve body, keeping the fourth valve body and the fifth valve body in a closed state, purifying the gas, and then filling high-purity nitrogen or high-purity argon into the collection tank;
and S5, after the filling is finished, closing the second valve body and the third valve body, and realizing constant pressure in the adsorber and the catalytic reactor.
As a still further scheme of the invention: in the step S1, after the temperature of the adsorber is raised to 350 ℃, the temperature raising rate of the catalytic reactor is adjusted, the temperature is maintained at 100 ℃, 200 ℃ and 300 ℃ for one hour, the temperature is maintained at 400 ℃ for 5 hours, until the average introduced hydrogen amount per gram of catalyst reaches 1.5-2.OL, the heating is stopped, hydrogen is continuously introduced to the temperature close to the room temperature, and then the fourth valve body and the fifth valve body are closed for standby.
Compared with the prior art, the invention has the beneficial effects that: the invention has novel design, dehydrates high-pressure nitrogen or high-pressure argon by the arranged absorber and other impurities, and deoxidizes the high-pressure nitrogen or the high-pressure argon by the catalytic reactor to obtain high-purity nitrogen or the high-purity argon, thereby ensuring the purification effect and having strong practicability.
Drawings
FIG. 1 is a schematic structural diagram of a nitrogen and argon terminal purification device.
In the figure: 1-air inlet, 2-first valve body, 3-second valve body, 4-third valve body, 5-fourth valve body, 6-fifth valve body, 7-adsorber, 8-catalytic reactor, 9-electric heater, 10-collection tank interface, 11-bypass connecting pipe and 12-main pipe connecting pipe.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, an element of the present invention may be said to be "fixed" or "disposed" to another element, either directly on the other element or with intervening elements present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only and do not represent the only embodiments.
Referring to fig. 1, in an embodiment of the present invention, a nitrogen and argon terminal purification device includes an adsorber 7 and a catalytic reactor 8, where the adsorber 7 and the catalytic reactor 8 are communicated through a main path connection pipe 12;
the adsorber 7 and the catalytic reactor 8 are both provided with electric heaters 9;
the absorber 7 and the catalytic reactor 8 are also communicated with a flow passage communicated with a high-purity hydrogen bottle.
In the embodiment of the invention, the high-pressure nitrogen or high-pressure argon is dehydrated and other impurities are removed through the arranged absorber 7, and then the high-pressure nitrogen or high-pressure argon is deoxidized through the catalytic reactor 8 to obtain high-purity nitrogen or high-purity argon, so that the purification effect is ensured, and the practicability is high.
In the embodiment of the present invention, the high-purity hydrogen bottle is disposed at one side of the catalytic reactor 8, and the flow passage is a conduit communicated with the main path connecting pipe 12.
In an embodiment of the present invention, the main pipe connecting pipe 12 is provided with an air inlet 1 and a collection tank interface 10 at both ends thereof.
In the embodiment of the invention, the purification device is communicated with the collecting tank and the vaporizer.
In one embodiment of the present invention, the second valve body 3 is provided on the main pipe 12 located on the side of the adsorber 7 remote from the catalytic reactor 8, and the third valve body 4 is provided on the main pipe 12 located on the end of the catalytic reactor 8 remote from the adsorber 7.
In the embodiment of the invention, the second valve body 3 and the third valve body 4 are arranged to realize the conduction or the closing of the main connecting pipe 12, thereby being convenient to control.
In one embodiment of the present invention, a fifth valve element 6 and a fourth valve element 5 are respectively installed on the flow passage connecting the high purity hydrogen bottle and at positions at the side ends of the adsorber 7 and the catalytic reactor 8.
In the embodiment of the invention, the communication control of the high-purity hydrogen bottle, the adsorber 7 and the catalytic reactor 8 is realized through the fourth valve body 5 and the fifth valve body 6.
In an embodiment of the present invention, the main pipe connecting pipe 12 is further connected to a bypass connecting pipe 11, the bypass connecting pipe 11 is provided with the first valve element 2, and ports at both ends of the bypass connecting pipe 11 are respectively located at a position between the second valve element 3 and the intake port 1 and a position between the third valve element 4 and the collection tank port 10.
In the embodiment of the invention, the vaporizer is directly communicated with the collecting tank through the bypass connecting pipe 11, the nitrogen or argon vaporized by the vaporizer is used for blowing the hydrogen in the bypass pipe (discharged by the bottle filling busbar), when the cryopump is started in normal production, because the device which is not continuously used can have air infiltration, the first valve body 2 is started first, so that impure gas in the device is blown from the bypass connecting pipe without passing through the adsorber 7 and the catalytic reactor 8, and the purification effect is improved.
The invention further provides a nitrogen and argon terminal purification method as an embodiment, which comprises the following steps:
s1, closing the first valve body 2, the second valve body 3 and the third valve body 4, simultaneously opening the fourth valve body 5 and the fifth valve body 6, then opening a high-purity hydrogen bottle, adjusting a hydrogen pressure reducer at the outlet of the high-purity hydrogen bottle, introducing high-purity hydrogen from the fourth valve body 5 at a flow rate of 1.4-1.5 Nm3/h, and heating and activating a catalyst in the catalytic reactor 8 and an adsorbent in the adsorber 7;
s2, turning on the electric heater 9 to heat the adsorber 7 and the catalytic reactor 8;
s3, closing the high-purity hydrogen bottle and the fourth valve body 5 and the fifth valve body 6, closing the second valve body 3 and the third valve body 4, opening the first valve body 2, and blowing off hydrogen in the bypass connecting pipe 11 by using nitrogen or argon vaporized by the vaporizer;
s4, closing the first valve body 2, opening the second valve body 3 and the third valve body 4, keeping the fourth valve body 5 and the fifth valve body 6 in a closed state, purifying the gas again, and then filling high-purity nitrogen or high-purity argon into the collection tank;
and S5, after the filling is finished, closing the second valve body 3 and the third valve body 4, and realizing the constant pressure in the adsorber 7 and the catalytic reactor 8.
In the present example, regeneration after catalytic reactor and adsorber failure was performed according to the following procedure:
firstly, closing a first valve body 2, a second valve body 3, a third valve body 4 and a fifth valve body 6, releasing the pressure in a terminal purification device to normal pressure, connecting a bottle of high-purity hydrogen bottle with the purity of 99.999% in front of the fourth valve body 5, electrifying and heating a catalytic reactor 8 and an adsorber 7, opening the high-purity hydrogen bottle valve and the fourth valve body 5, adjusting a hydrogen pressure reducer at the outlet of the hydrogen bottle, introducing high-purity hydrogen from the fourth valve body 5 at the flow rate of 1.4-1.5 Nm3/h, heating the adsorber 7 to 350 ℃, then heating the catalytic reactor 8 at the heating rate of 8 ℃ per minute, keeping the temperature at 100 ℃, 200 ℃ and 300 ℃ for 1 hour respectively, then heating to 400 ℃, keeping the temperature for 4 hours (replacing the hydrogen bottle during the period), stopping heating, continuously introducing hydrogen to the room temperature, closing the fourth valve body 5 and the fifth valve body 6, and reusing.
In the present example, it should be noted that the temperature of the adsorber 7 or the catalytic reactor 8 must not exceed 450 ℃ during the activation regeneration.
In the embodiment of the invention, in the filling process, the constant-pressure operation of the absorber 7 and the catalytic reactor 8 under 8-IOMPa must be ensured, the pressure is slowly increased and reduced, and the phenomenon that the adsorbent and the catalyst are pulverized and the product quality is influenced due to differential pressure impact is avoided.
In step S1, after the temperature of the adsorber 7 is raised to 350 ℃, the temperature raising rate of the catalytic reactor 8 is adjusted, and the temperature is maintained at 100 ℃, 200 ℃ and 300 ℃ for one hour, and at 400 ℃ for 5 hours, until the average amount of hydrogen introduced per gram of catalyst reaches 1.5-2.OL, the heating is stopped, hydrogen is introduced to the temperature close to room temperature, and then the fourth valve body 5 and the fifth valve body 6 are closed for standby.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. The nitrogen and argon terminal purification device is characterized by comprising an adsorber (7) and a catalytic reactor (8), wherein the adsorber (7) and the catalytic reactor (8) are communicated through a main path connecting pipe (12);
electric heaters (9) are respectively arranged on the absorber (7) and the catalytic reactor (8);
the absorber (7) and the catalytic reactor (8) are also communicated with a flow passage communicated with a high-purity hydrogen bottle.
2. A terminal purification device for nitrogen and argon according to claim 1, characterized in that both ends of said main path connection pipe (12) are respectively provided with an air inlet (1) and a collection tank interface (10).
3. A terminal purification device for nitrogen and argon according to claim 2, characterized in that a second valve body (3) is arranged on the main connection pipe (12) at the side of said adsorber (7) far from said catalytic reactor (8), and a third valve body (4) is arranged on the main connection pipe (12) at the end of said catalytic reactor (8) far from said adsorber (7).
4. A terminal purification device for nitrogen and argon according to claim 1, characterized in that the fifth valve body (6) and the fourth valve body (5) are respectively installed on the flow channel connected to the high purity hydrogen bottle and located at the side ends of the adsorber (7) and the catalytic reactor (8).
5. A terminal purification device for nitrogen and argon according to claim 3, characterized in that said main connecting pipe (12) is further connected with a bypass connecting pipe (11), said bypass connecting pipe (11) is installed with a first valve body (2), and the two end ports of said bypass connecting pipe (11) are respectively located at the position between said second valve body (3) and said gas inlet (1) and the position between said third valve body (4) and said collection tank interface (10).
6. A terminal purification method of nitrogen and argon is characterized by comprising the following steps:
s1, closing the first valve body (2), the second valve body (3) and the third valve body (4), simultaneously opening the fourth valve body (5) and the fifth valve body (6), then opening a high-purity hydrogen bottle, adjusting a hydrogen pressure reducer at the outlet of the high-purity hydrogen bottle, introducing high-purity hydrogen from the fourth valve body (5) at a flow rate of 1.4-1.5 Nm3/h, and heating and activating a catalyst in the catalytic reactor (8) and an adsorbent in the adsorber (7);
s2, turning on the electric heater (9) to heat the adsorber (7) and the catalytic reactor (8);
s3, closing the high-purity hydrogen bottle, the fourth valve body (5) and the fifth valve body (6), closing the second valve body (3) and the third valve body (4), opening the first valve body (2), and blowing off hydrogen in the bypass connecting pipe (11) by using nitrogen or argon vaporized by the vaporizer;
s4, closing the first valve body (2), opening the second valve body (3) and the third valve body (4), keeping the fourth valve body (5) and the fifth valve body (6) in a closed state, purifying the gas, and filling high-purity nitrogen or high-purity argon into the collecting tank;
and S5, after filling, closing the second valve body (3) and the third valve body (4) to realize constant pressure in the absorber (7) and the catalytic reactor (8).
7. A terminal purification method of nitrogen and argon according to claim 6, characterized in that in step S1, after the temperature of adsorber (7) is raised to 350 ℃, the temperature raising rate of catalytic reactor (8) is adjusted, and the temperature is maintained at 100 ℃, 200 ℃ and 300 ℃ for one hour each, and at 400 ℃ for 5 hours, until the average hydrogen gas flow per gram of catalyst reaches 1.5-2.OL, the heating is stopped, the hydrogen gas flow is continued to approach the room temperature, and then the fourth valve body (5) and the fifth valve body (6) are closed for standby.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010360269.6A CN113582144A (en) | 2020-04-30 | 2020-04-30 | Nitrogen and argon terminal purification device and purification method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010360269.6A CN113582144A (en) | 2020-04-30 | 2020-04-30 | Nitrogen and argon terminal purification device and purification method |
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-
2020
- 2020-04-30 CN CN202010360269.6A patent/CN113582144A/en active Pending
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| US5106399A (en) * | 1991-02-25 | 1992-04-21 | Union Carbide Industrial Gases Technology Corporation | Argon purification system |
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