CN218811566U - Helium refining device capable of removing neon - Google Patents

Helium refining device capable of removing neon Download PDF

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CN218811566U
CN218811566U CN202222502905.1U CN202222502905U CN218811566U CN 218811566 U CN218811566 U CN 218811566U CN 202222502905 U CN202222502905 U CN 202222502905U CN 218811566 U CN218811566 U CN 218811566U
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helium
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邓海
文向南
曹卫华
朱磊
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Sichuan Shudao Equipment Technology Co ltd
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Sichuan Shudao Equipment Technology Co ltd
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Abstract

The utility model discloses a helium refining device capable of removing neon, which comprises units such as low-temperature rectification, catalytic dehydrogenation, adsorption dehydration, condensation separation, PSA helium extraction, low-temperature adsorption and the like, wherein a feed gas inlet of a low-temperature rectification unit is connected with a feed gas pipeline; the liquid nitrogen is connected with a liquid nitrogen inlet of the cryogenic rectification unit through a valve I and a pipeline I; the cryogenic rectification unit is provided with a nitrogen vent; the low-temperature rectification unit separates methane in the feed gas to produce methane; the first-stage crude helium outlet of the cryogenic rectification unit is connected with the inlet of the catalytic dehydrogenation unit after being converged with the return gas pipeline.

Description

Helium refining device capable of removing neon
Technical Field
The utility model relates to a helium purification technical field, concretely relates to helium refining plant of desorption neon.
Background
Helium is a rare strategic resource, high-purity helium is widely applied in the fields of military industry, medical treatment, semiconductors, superconduction, deep low-temperature refrigeration and the like, the helium resource in China is deficient, the price is high, the helium depends on import to a great extent, particularly, the helium is easily produced by people under the influence of complex international situation, so that a helium refining device with high yield, high purity and good economical efficiency, particularly capable of deeply dehydrogenating and removing neon, is urgently needed.
Chinese utility model CN 111547691A "an apparatus and process for extracting helium from BOG gas with high hydrogen content" is used for extracting helium by multi-stage membrane separation. There are the following problems: 1. a plurality of compressors are required to be additionally arranged, so that the investment is large and the energy consumption is high; 2. hydrogen molecules and helium molecules are difficult to realize through membrane separation, trace hydrogen left after catalytic dehydrogenation can be concentrated step by step, the purity of helium is influenced, and high purity of more than 99.999 percent cannot be produced; 3. has no neon removing function.
Chinese utility model patent CN 114314534A "a natural gas helium extraction process", adding oxygen to remove hydrogen until the hydrogen content is less than 1ppm, then dehydrating, and denitriding under the pressure of 19-20 MPa. There are the following problems: 1. the operation pressure is high, the investment and the operation cost are high, and the type selection of equipment and instruments is difficult; 2. after denitrification, hydrogen can be concentrated, the purity of helium is influenced, and high-purity helium with the purity of more than 99.999 percent cannot be produced; 3. catalytic dehydrogenation, high hydrogen concentration, high reaction temperature and low safety; 4. has no neon removing function.
At present, in various helium extraction devices, neon is not considered in raw material gas components, and a neon removal process method is not adopted. According to the regulations GB/T4844-2011 of pure helium, high-purity helium and ultra-pure helium, the neon content in the high-purity helium is less than 4ppm, and the neon content in the ultra-pure helium is less than 1ppm. The standard requirement therefore requires consideration of the de-neon process.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a helium refining plant of desorption neon to solve and carry helium device and technology investment, running cost height and do not have the technical problem who takes off the neon function among the prior art.
In order to achieve the above purpose, the utility model provides a following technical scheme:
the utility model provides a pair of helium refining plant that can desorption neon, carry helium unit, cryosorption unit including cryogenic rectification unit, catalytic dehydrogenation unit, absorption dehydration unit, condensation separation unit, PSA.
Further, a raw gas inlet of the low-temperature rectification unit is connected with a raw gas pipeline; the liquid nitrogen is connected with a liquid nitrogen inlet of the cryogenic rectification unit through a valve I and a pipeline I; the cryogenic rectification unit is provided with a nitrogen vent; the low-temperature rectification unit separates methane in the feed gas to produce methane; the first-stage crude helium outlet of the cryogenic rectification unit is connected with the inlet of the catalytic dehydrogenation unit after being converged with the return gas pipeline.
Further, an oxygen inlet of the catalytic dehydrogenation unit is connected with an oxygen pipeline; the secondary crude helium outlet of the catalytic dehydrogenation unit is connected with the inlet of the adsorption dehydration unit.
Further, a regenerated gas outlet of the adsorption dehydration unit is connected with an inlet of a supercharger, and an outlet of the supercharger is connected with a primary crude helium pipeline and enters the catalytic dehydrogenation unit; and a three-stage crude helium outlet of the adsorption dehydration unit is connected with an inlet of the condensation separation unit.
Further, a four-stage crude helium outlet of the condensation separation unit is connected with an inlet of the PSA helium extraction unit; the liquid nitrogen is connected with a liquid nitrogen inlet of the condensation separation unit through a second valve and a second pipeline; the condensation separation unit is provided with a vacuum pump for emptying nitrogen, and is also provided with a first separation tank for separating crude helium to enter the next unit, the rest impurity gases enter a second separation tank through a first throttle valve, and a recovered gas outlet of the condensation separation unit is connected with an inlet of a second booster.
Furthermore, a pure helium outlet of the PSA helium extraction unit is divided into two parts, one part is connected with a valve in a three-phase mode to produce pure helium, and the other part is connected with an inlet of the low-temperature adsorption unit through a valve IV; and the desorption gas outlet of the PSA helium extraction unit is connected with the inlet of the second booster, and the outlet of the second booster is converged and connected with the primary crude helium pipeline and enters the catalytic dehydrogenation unit.
Further, the cryoadsorption unit is used to produce high purity helium; the cold source is connected with an inlet of the low-temperature adsorption unit, the heat recovery gas is generated through the heat exchanger II, the heat recovery gas is connected with an outlet of the low-temperature adsorption unit, and the pure helium enters the low-temperature adsorber through the heat exchanger II to generate the high-purity helium.
Further, the system also comprises a control system; the first valve, the second valve, the third valve and the fourth valve are all electromagnetic valves; the control system is respectively and electrically connected with the cryogenic rectification unit, the catalytic dehydrogenation unit, the adsorption dehydration unit, the condensation separation unit, the PSA helium extraction unit, the cryogenic adsorption unit, the first valve, the second valve, the third valve, the fourth valve, the first booster and the second booster.
Based on the technical scheme, the embodiment of the utility model provides a can produce following technological effect at least:
(1) The utility model discloses the low temperature adsorption unit solves degree of depth dehydrogenation and takes off the neon problem to make the high-purity helium that is more than or equal to 99.999%.
(2) The utility model discloses helium unit is carried to condensation separating element + PSA, and the solution yield is low to and high pressure operation scheduling problem, reduce equipment, instrument investment, improve device operation economy and security.
(3) The utility model discloses regeneration gas, recycle gas, analytic gas recycle improve the helium yield, reduce catalytic dehydrogenation reaction hydrogen concentration, reduce reaction temperature, need not to increase circulating compressor alone again, solve the helium yield low, catalytic dehydrogenation reaction temperature height scheduling problem.
Drawings
In order to more clearly illustrate 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 described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic process diagram of example 1 of the present invention;
FIG. 2 is a schematic process diagram of example 2 of the present invention;
FIG. 3 is a schematic diagram of the structure of the condensation separation unit of the present invention;
FIG. 4 is a schematic structural view of cryoadsorption according to embodiment 1 of the present invention;
FIG. 5 is a schematic view of the cryoadsorption structure of embodiment 2 of the present invention;
names of corresponding components represented by numerals or letters in the drawings:
1. a cryogenic rectification unit; 101. a first valve; 102. a first pipeline; 2. a catalytic dehydrogenation unit; 3. an adsorption dehydration unit; 301. a first supercharger; 4. a condensation separation unit; 401. a second valve; 402. a second pipeline; 403. a second supercharger; 404. a vacuum pump; 405. a first heat exchanger; 406. a first separating tank; 407. a first throttle valve; 408 separating tank II; 5. a PSA helium extraction unit; 501. a third valve; 502. a fourth valve; 6. a low-temperature adsorption unit; 601. a cold source; 602. heating the air; 603. a second heat exchanger; 604. a low temperature adsorber; 605. a deep cryogenic refrigerator.
Detailed Description
It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the invention.
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention. In addition, the technical solutions in the embodiments may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, it should be considered that the combination of the technical solutions does not exist, and is not within the protection scope of the present invention.
In the present application, unless expressly stated or limited otherwise, the first feature may be directly on or directly under the second feature or indirectly via intermediate members. Also, a first feature "on," "above," and "over" a second feature may be directly on or obliquely above the second feature, or simply mean that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
The purpose of the utility model is realized through the following technical scheme:
a helium refining device capable of removing neon comprises a cryogenic rectification unit 1, a catalytic dehydrogenation unit 2, an adsorption dehydration unit 3, a condensation separation unit 4, a PSA helium extraction unit 5 and a cryogenic adsorption unit 6.
Example 1: as shown in fig. 1, 3 and 4;
specifically, a raw material gas inlet of the low-temperature rectification unit 1 is connected with a raw material gas pipeline; liquid nitrogen is connected with a liquid nitrogen inlet of the cryogenic rectification unit 1 through a valve I101 and a pipeline I102; the cryogenic rectification unit 1 is provided with a nitrogen vent; the low-temperature rectification unit 1 separates methane in the feed gas to produce methane; the first-stage crude helium outlet of the cryogenic rectification unit 1 is connected with the inlet of the catalytic dehydrogenation unit 2 after being converged with the return gas pipeline.
Specifically, an oxygen inlet of the catalytic dehydrogenation unit 2 is connected with an oxygen pipeline; the secondary crude helium outlet of the catalytic dehydrogenation unit 2 is connected with the inlet of the adsorption dehydration unit 3. The outlet of the regenerated gas of the adsorption dehydration unit 3 is connected with the inlet of a first booster 301, and the outlet of the first booster 301 is connected with a primary crude helium pipeline and enters a catalytic dehydrogenation unit 2; and a three-level crude helium outlet of the adsorption dehydration unit 3 is connected with an inlet of the condensation separation unit 4.
Specifically, a four-stage crude helium outlet of the condensation separation unit 4 is connected with an inlet of the PSA helium extraction unit 5; the liquid nitrogen is connected with a liquid nitrogen inlet of the condensation separation unit 4 through a second valve 401 and a second pipeline 402; the condensation separation unit 4 is provided with a vacuum pump 404 for emptying nitrogen, a first separation tank 406 for separating crude helium and entering the next unit, the rest impurity gas enters a second separation tank 408 through a first throttling valve 407, the second separation tank 408 separates the recovered gas from the nitrogen, and the recovered gas outlet of the condensation separation unit 4 is connected with the inlet of a second booster 403.
Specifically, a pure helium outlet of the PSA helium extraction unit 5 is divided into two parts, one part is connected with a valve III 501 to produce pure helium, and the other part is connected with an inlet of the low-temperature adsorption unit 6 through a valve IV 502; the outlet of the desorption gas of the PSA helium extraction unit 5 is connected with the inlet of a second booster 403, and the outlet of the second booster 403 is connected with a primary crude helium pipeline in a converging way and enters the catalytic dehydrogenation unit 2.
Specifically, the low-temperature adsorption unit 6 is provided with a high-purity helium outlet to produce high-purity helium; the cold source 601 is connected with an inlet of the low-temperature adsorption unit 6, the hot gas 602 is generated through a second heat exchanger 603, the hot gas 602 is connected with an outlet of the low-temperature adsorption unit 6, and the pure helium enters the low-temperature adsorber 604 through the second heat exchanger 603 to generate the high-purity helium.
The specific implementation steps are as follows:
s1: introducing a raw material gas with the pressure of 1.0-5.0 MPa into a low-temperature rectification unit, and then introducing liquid nitrogen to generate primary crude helium, wherein the raw material gas comprises methane, nitrogen, argon, hydrogen and a small amount of neon, and the low-temperature rectification unit comprises one tower and low-temperature condensation or one or two of two tower processes;
s2: the first-stage crude helium outlet of the cryogenic rectification unit is converged with the return gas pipeline and then enters the catalytic dehydrogenation unit for catalytic reaction to generate second-stage crude helium;
s3: the second-stage crude helium gas generated by the catalytic dehydrogenation unit enters an adsorption dehydration unit, and is dehydrated to less than 1ppm by using a molecular sieve comprising one or more of 3A, 4A, 5A and 13X to generate third-stage crude helium gas;
s4: the third-level crude helium gas generated by the adsorption dehydration unit enters a condensation separation unit, the temperature of the condensation separation unit is controlled to be-170 ℃ to-210 ℃, and condensation separation is carried out to generate fourth-level crude helium gas; the regenerated gas of the adsorption dehydration unit, the recovered gas of the condensation separation unit and the desorbed gas of the PSA helium extraction unit are sent to the catalytic dehydrogenation unit through a first booster and a second booster;
s5: and the four-stage crude helium gas generated by the condensation separation unit enters a PSA helium extraction unit with an adsorbent for adsorption and purification, the adsorbent comprises one or a combination of 5A, 13X and lithium molecular sieves, one part of the adsorbent passes through a valve III to produce pure helium after the adsorption and purification is finished, and the other part of the adsorbent passes through a valve IV to enter a low-temperature adsorption unit to produce high-purity helium.
Example 2: as shown in fig. 2, 3 and 5;
specifically, a feed gas inlet of the cryogenic rectification unit 1 is connected with a feed gas pipeline; the liquid nitrogen is connected with a liquid nitrogen inlet of the cryogenic rectification unit 1 through a valve I101 and a pipeline I102; the cryogenic rectification unit 1 is provided with a nitrogen vent; the low-temperature rectification unit 1 separates methane in the feed gas to produce methane; the first-stage crude helium outlet of the cryogenic rectification unit 1 is converged with a gas pipeline passing through the first booster 301 and then connected with the inlet of the catalytic dehydrogenation unit 2.
Specifically, an oxygen inlet of the catalytic dehydrogenation unit 2 is connected with an oxygen pipeline; the secondary crude helium outlet of the catalytic dehydrogenation unit 2 is connected with the inlet of the adsorption dehydration unit 3. The outlet of the regenerated gas of the adsorption dehydration unit 3 is connected with the inlet of a first booster 301, and the outlet of the first booster 301 is connected with a primary crude helium pipeline and enters a catalytic dehydrogenation unit 2; and a three-level crude helium outlet of the adsorption dehydration unit 3 is connected with an inlet of the condensation separation unit 4.
Specifically, a four-stage crude helium outlet of the condensation separation unit 4 is connected with an inlet of the PSA helium extraction unit 5; the liquid nitrogen is connected with a liquid nitrogen inlet of the condensation separation unit 4 through a second valve 401 and a second pipeline 402; the condensation separation unit 4 is provided with a vacuum pump 404 for emptying nitrogen, a first separation tank 406 for separating crude helium and entering the next unit, the rest impurity gas enters a second separation tank 408 through a first throttling valve 407, the second separation tank 408 separates the recovered gas from the nitrogen, and the recovered gas outlet of the condensation separation unit 4 is connected with the inlet of a second booster 403.
Specifically, a pure helium outlet of the PSA helium extraction unit 5 is divided into two parts, one part is connected with a valve III 501 to produce pure helium, and the other part is connected with an inlet of the low-temperature adsorption unit 6 through a valve IV 502; the outlet of the recovered gas of the condensation separation unit 4 is converged with the outlet of the desorption gas of the PSA helium extraction unit 5 and then is connected with the inlet of the second booster 403, the outlet of the second booster 403 is converged with the outlet of the regenerated gas of the adsorption dehydration unit 3 and then is connected with the inlet of the first booster 301, and the outlet of the first booster 301 is converged with the primary crude helium pipeline and then is connected with the primary crude helium pipeline to enter the catalytic dehydrogenation unit 2.
Specifically, the low-temperature adsorption unit 6 is provided with a high-purity helium outlet to produce high-purity helium; and the deep cryogenic refrigerator 605 is connected with the second heat exchanger 603, and the pure helium enters the cryogenic absorber 604 through the second heat exchanger 603 to generate high-purity helium.
The specific implementation steps are as follows:
s1: introducing a raw material gas with the pressure of 1.0-5.0 MPa into a low-temperature rectification unit, and introducing liquid nitrogen to generate primary crude helium, wherein the raw material gas comprises methane, nitrogen, argon, hydrogen and a small amount of neon, and the low-temperature rectification unit comprises one tower and low-temperature condensation or one or two combinations of two tower processes;
s2: the first-stage crude helium outlet of the cryogenic rectification unit is converged with the return gas pipeline and then enters the catalytic dehydrogenation unit for catalytic reaction to generate second-stage crude helium;
s3: the second-stage crude helium gas generated by the catalytic dehydrogenation unit enters an adsorption dehydration unit, and is dehydrated to less than 1ppm by using a molecular sieve comprising one or more of 3A, 4A, 5A and 13X to generate third-stage crude helium gas;
s4: the third-level crude helium gas generated by the adsorption dehydration unit enters a condensation separation unit, the temperature of the condensation separation unit is controlled to be-170 ℃ to-210 ℃, and condensation separation is carried out to generate fourth-level crude helium gas; the regenerated gas of the adsorption dehydration unit, the recovered gas of the condensation separation unit and the desorbed gas of the PSA helium extraction unit are sent to the catalytic dehydrogenation unit through a first booster and a second booster;
s5: and the four-stage crude helium gas generated by the condensation separation unit enters a PSA helium extraction unit with an adsorbent for adsorption and purification, the adsorbent comprises one or more of 5A, 13X and lithium molecular sieves, one of the four components passes through a valve III to produce pure helium after adsorption and purification is finished, and the other component passes through a valve IV to enter a low-temperature adsorption unit to produce high-purity helium.
Although the preferred embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the scope of knowledge possessed by those skilled in the art.
The basic principles and the main features of the invention and the advantages of the invention have been shown and described above. It will be understood by those skilled in the art that the present invention is not limited to the above embodiments, and that the foregoing embodiments and descriptions are provided only to illustrate the principles of the present invention without departing from the spirit and scope of the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (7)

1. A helium refining device capable of removing neon is characterized in that: comprises a cryogenic rectification unit (1), a catalytic dehydrogenation unit (2), an adsorption dehydration unit (3), a condensation separation unit (4), a PSA helium extraction unit (5) and a cryogenic adsorption unit (6);
wherein, the first-stage crude helium outlet of the cryogenic rectification unit (1) is connected with the inlet of the catalytic dehydrogenation unit (2) after being converged with a return gas pipeline; a secondary crude helium outlet of the catalytic dehydrogenation unit (2) is connected with an inlet of the adsorption dehydration unit (3); a three-stage crude helium outlet of the adsorption dehydration unit (3) is connected with an inlet of the condensation separation unit (4); a four-stage crude helium outlet of the condensation separation unit (4) is connected with an inlet of the PSA helium extraction unit (5); the pure helium outlet of the PSA helium extraction unit (5) is connected with the inlet of the low-temperature adsorption unit (6).
2. A helium purification apparatus with neon removal as claimed in claim 1, wherein: the feed gas inlet of the low-temperature rectification unit (1) is connected with a feed gas pipeline; the liquid nitrogen is connected with a liquid nitrogen inlet of the cryogenic rectification unit (1) through a first valve (101) and a first pipeline (102); the cryogenic rectification unit (1) is provided with a nitrogen vent; the low-temperature rectification unit (1) separates methane in the feed gas to produce methane.
3. A helium purification apparatus with neon removal as claimed in claim 1, wherein: and an oxygen inlet of the catalytic dehydrogenation unit (2) is connected with an oxygen pipeline.
4. A helium purification apparatus with neon removal as claimed in claim 1, wherein: and a regenerated gas outlet of the adsorption dehydration unit (3) is connected with an inlet of a first booster (301), and an outlet of the first booster (301) is connected with a first-level crude helium pipeline and enters the catalytic dehydrogenation unit (2).
5. A helium purification apparatus with neon removal as claimed in claim 1, wherein: the liquid nitrogen is connected with a liquid nitrogen inlet of the condensation separation unit (4) through a second valve (401) and a second pipeline (402); the condensation separation unit (4) is provided with a vacuum pump (404) for emptying nitrogen, a first separation tank (406) for separating crude helium and entering the next unit, the rest impurity gases enter a second separation tank (408) through a first throttling valve (407), and a recycled gas outlet of the condensation separation unit (4) is connected with an inlet of a second booster (403).
6. A helium purification apparatus with neon removal as claimed in claim 1, wherein: the pure helium outlet of the PSA helium extraction unit (5) is divided into two parts, one part is connected with a valve III (501) to produce pure helium, and the other part is connected with the inlet of the low-temperature adsorption unit (6) through a valve IV (502); the outlet of the desorption gas of the PSA helium extraction unit (5) is connected with the inlet of a second booster (403), and the outlet of the second booster (403) is converged and connected with a primary crude helium pipeline and enters a catalytic dehydrogenation unit (2).
7. A helium purification apparatus with neon removal as claimed in claim 1, wherein: the low-temperature adsorption unit (6) is used for producing high-purity helium; the cold source (601) is connected with an inlet of the low-temperature adsorption unit (6), the reheat gas (602) is generated through a second heat exchanger (603), the reheat gas (602) is connected with an outlet of the low-temperature adsorption unit (6), and the pure helium enters the low-temperature adsorber (604) through the second heat exchanger (603) to generate the high-purity helium.
CN202222502905.1U 2022-09-21 2022-09-21 Helium refining device capable of removing neon Active CN218811566U (en)

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