CN212941496U - Double-isotope low-temperature synchronous separation device - Google Patents

Double-isotope low-temperature synchronous separation device Download PDF

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CN212941496U
CN212941496U CN202020753725.9U CN202020753725U CN212941496U CN 212941496 U CN212941496 U CN 212941496U CN 202020753725 U CN202020753725 U CN 202020753725U CN 212941496 U CN212941496 U CN 212941496U
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isotope
tower
nitrogen
stage
air separation
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何晖
袁士豪
李剑锋
李冬锋
朱程浩
任美凤
康玉茹
吴秀杰
韩小磊
包汉波
孙潇
汪晗
蒋澎
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Hang Yang Group Co ltd
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Hangzhou Oxygen Plant Group Co Ltd
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Abstract

A dual-isotope low-temperature synchronous separation device at least comprises an air separation oxygen purification system and an air separation nitrogen purification system,18o isotope and15an N isotope synchronous low-temperature rectification system,18o isotope and15n isotopeThe molecular cracking recombination system consists of three parts; empty oxygen purification system and empty nitrogen gas purification system of dividing includes empty oxygen purification device and empty nitrogen gas purification device of dividing at least and assembles the combined column that becomes and the reboiler of its lower bottom of tower, empty oxygen purification device and empty nitrogen gas purification device of dividing, the utility model discloses combine regular packing and random packing characteristics separately, preceding several grades of cascaded towers and several grades of cascaded towers in back set up double-deck wire mesh ripple filler and rectangle helicoid filler respectively, and it is better to guarantee the device raw material volume throughput, and device rectification efficiency is also higher, is equipped with isotope molecule schizolysis recombination catalytic system, improves target isotope abundance and output.

Description

Double-isotope low-temperature synchronous separation device
Technical Field
The utility model relates to a double isotope synchronous separation device, in particular to a cryogenic rectification technology for synchronously separating oxygenIs/are as follows18In O isotope and nitrogen15N isotope utilization18O isotope raw material oxygen is used as heat source for evaporation15N isotope as raw material liquid nitrogen at the same time18O isotope raw material oxygen condensing and liquefying18And (4) rectifying reflux liquid by using an O isotope. The utility model discloses the output has huge economic value and scientific research utilization value18O isotope and15an N isotope.
Background
Isotopes have important applications in the fields of national defense, space exploration, medical science and the like, and extraction thereof is quite difficult. The isotope cryogenic rectification separation technology is the top technology in the cryogenic low-temperature field, and the development of the isotope low-temperature separation technology has great significance at the strategic level. At present, domestic18O isotope and15the N isotope market is basically monopolized by America, Japan and Europe. The utility model discloses developed and had originality18O isotope and15n isotope synchronous integrated rectification process and device, output18O isotope and15an N isotope. The utility model provides a18O isotope and15the N isotope low-temperature synchronous separation device can simultaneously separate18O isotope and15the N isotope has large raw material processing amount,18o isotope and15the extraction rate of the N isotope is high, and the method is particularly suitable for industrial isotope production.
Disclosure of Invention
In order to realize the technical vacancy of China in the aspect of isotope industrial production, the utility model develops18O isotope and15the N isotope synchronous rectification process and device take oxygen and nitrogen produced by air separation as raw materials to produce the N isotope synchronous rectification device with strategic significance18O isotope and15an N isotope.
The utility model aims to realize the technical proposal that the double-isotope low-temperature synchronous separation device at least comprises an air separation oxygen purification system and an air separation nitrogen purification system,18o isotope and15an N isotope synchronous low-temperature rectification system,18o isotope and15the N isotope molecule cracking recombination system comprises three parts(ii) a The air separation oxygen purification system and the air separation nitrogen purification system at least comprise a combined tower formed by respectively integrating an air separation oxygen purification device and an air separation nitrogen purification device, a reboiler arranged at the bottom of the lower tower of the air separation oxygen purification device and the air separation nitrogen purification device, condensation evaporators of the air separation oxygen purification device and the air separation nitrogen purification device, a condenser arranged at the top of the upper tower of the air separation oxygen purification device and the air separation nitrogen purification device, and a pressure reducing valve;18o isotope and15the N isotope synchronous cryogenic rectification system at least comprises18O isotope and15the system comprises an N isotope multi-stage rectifying tower, a liquid oxygen nitrogen reboiler, an oxygen and nitrogen condensation evaporator and a liquid nitrogen condenser;18o isotope and15the N isotope atom cracking recombination system at least comprises an oxygen/nitrogen molecule cracking recombination catalytic device and a catalytic electric heater, wherein the combined tower is divided into an upper tower and a lower tower, wherein the upper tower filters light component impurities, the lower tower filters heavy component impurities, the pressure of the lower tower is higher than that of the upper tower, steam rising from the top of the lower tower is used as a heat source through boiling point difference to boil the accumulated liquid at the bottom of the upper tower, the upper towers of the air separation oxygen purification device and the air separation nitrogen purification device are operated under reduced pressure to remove light component impurities such as hydrogen, the lower towers of the air separation oxygen purification device and the air separation nitrogen purification device filter heavy component impurities through low-temperature rectification, and the content of the heavy component impurities such as hydrocarbon can be reduced to below 1 ppm.
Preferably, the method comprises the following steps: the air separation nitrogen purification device is connected with air separation nitrogen, the top of the lower tower A of the air separation nitrogen purification device is connected with the bottom of the air separation nitrogen condensation evaporator A, the upper gas outlet of the lower tower A of the air separation nitrogen purification device is connected with the inlet of a pressure reducing valve A, the outlet of the pressure reducing valve A is connected with the upper tower A feed inlet of the air separation nitrogen purification device, and the bottom of the upper tower A of the air separation nitrogen purification device is connected with the top of the air separation nitrogen condensation evaporator A. The bottom of a lower tower A of the air separation nitrogen purification device is connected with the top of a lower tower reboiler A, the top of an upper tower A of the air separation nitrogen purification device is connected with the bottom of an upper tower A top condenser A, an outlet of the air separation nitrogen purification device is connected with an inlet of a high-purity raw material nitrogen mass flow controller, and an outlet of the high-purity raw material nitrogen mass flow controller is connected with a first-stage cascade15The raw material inlet at the middle part of the N isotope poverty removing tower. First stage of cascade15And exhausting the waste gas at the top of the N isotope depletion tower to the atmosphere. First stage of cascade15The bottom of the N isotope lean elimination tower is connected with a first-stage cascade18O isotope and first order cascade15The top of the N isotope condensation evaporator is cascaded in the first stage15The outlet of the N isotope condensation evaporator is connected with the second-stage cascade15The raw material inlet at the middle part of the N isotope poverty removing tower. Second stage of cascade15The top waste gas of the N isotope lean removal tower is connected with the first-stage cascade15And an N isotope lean removal tower return air port. Second stage of cascade15The bottom of the N isotope lean elimination tower is connected with a second-stage cascade18O isotope and second order cascade15N isotope condensation evaporation top, second stage cascade15The outlet of the N isotope condensation evaporator is connected with the next stage cascade15The raw material inlet of the N isotope lean removing tower is cascaded in the second stage15The return air port of the N isotope lean removal tower is connected with the next stage of cascade15A top gas outlet of the N isotope lean removal tower, the first stage is cascaded15The top of the N isotope lean removal tower is connected with a first-stage cascade15N isotope condenser bottom, second stage cascade15The top of the N isotope lean removal tower is connected with a second-stage cascade15The bottom of the N isotope condenser is provided with a product discharge port of the second-stage cascade tower18O isotope and15n isotope molecule cracking recombination catalytic unit.
Preferably, the method comprises the following steps: the air separation oxygen and air separation oxygen purification device is characterized in that an inlet of the air separation oxygen and air separation oxygen purification device is connected with air separation oxygen, the top of a lower tower B of the air separation oxygen purification device is connected with the bottom of an air separation oxygen condensation evaporator B, an upper gas outlet of the lower tower B of the air separation oxygen purification device is connected with an inlet of a pressure reducing valve B, an outlet of the pressure reducing valve B is connected with an upper tower B feed inlet of the air separation oxygen purification device, and the bottom of an upper tower B of. The bottom of a lower tower B of the air separation oxygen purification device is connected with the top of a lower tower reboiler B, the top of an upper tower B of the air separation oxygen purification device is connected with the bottom of an upper tower top condenser B, an outlet of the air separation oxygen purification device is connected with an inlet of a high-purity raw material oxygen mass flow controller, and an outlet of the high-purity raw material oxygen mass flow controller is connected with a first-stage cascade18The middle raw material inlet of the O isotope poverty removing tower. First stage of cascade18And exhausting the waste gas at the top of the O isotope depletion tower to the atmosphere. First stage of cascade18The bottom of the O isotope lean elimination tower is connected with a first-stage cascade18O isotope dephenolizing tower nitrogen reboiler I, the first stage is cascaded18The top of the O isotope lean-removing tower is connected with a first-stage cascade18O isotope and first order cascade15N isotope condensing evaporator bottom. First stage of cascade18The outlet of the nitrogen reboiler I of the O isotope lean removal tower is connected with the second-stage cascade18The middle raw material inlet of the O isotope poverty removing tower. Second stage of cascade18The top of the O isotope lean-removing tower is connected with a second-stage cascade18O isotope and second order cascade15N isotope condensing evaporator bottom, second stage cascade18The top of the O isotope lean removal tower is connected with a first-stage cascade18And an O isotope element de-lean tower gas return port. Second stage of cascade18The bottom of the O isotope lean elimination tower is connected with a second-stage cascade18A nitrogen reboiler II of an O isotope lean removal tower and a second-stage cascade18The outlet of a nitrogen reboiler II of the O isotope lean removal tower is connected with the next stage of cascade18And a raw material inlet of the O isotope dephenolizing tower.
Preferably, the method comprises the following steps: the second stage18O isotope and15product discharge port arrangement of N isotope multi-stage rectifying tower18O isotope and15the N isotope molecule cracking recombination catalytic device is characterized in that a nitrogen inlet of the isotope molecule cracking recombination catalytic device is connected with a second-stage cascade15N isotopes and cascades18The outlet of the O isotope condensation evaporator and the oxygen inlet of the isotope molecule cracking recombination catalytic device are connected with the second cascade18The nitrogen outlet of the isotope molecule cracking recombination catalytic device is connected with the inlet of a catalyzed nitrogen outlet valve, and the outlet of the catalyzed nitrogen outlet valve is connected with the last-stage cascade15Raw material inlet and final stage cascade of N isotope concentration tower15The top of the N isotope concentration tower is connected with an upper-stage cascade15And an N isotope lean removal tower return air port. Last stage cascade15N isotope concentration tower bottom connection last stage cascade18O isotope and15and N isotope condensing the top of the evaporator. Last stage cascade15N isotope concentration towerTop-connected last-stage cascade15The bottom of the N isotope condenser. The oxygen outlet of the isotope molecule cracking recombination catalytic device is connected with the inlet of a catalyzed oxygen outlet valve, and the outlet of the catalyzed oxygen outlet valve is connected with the last-stage cascade18Raw material inlet of O isotope concentration tower and final stage cascade18The top of the O isotope concentration tower is connected with an upper-stage cascade18And an O isotope element de-lean tower gas return port. Last stage cascade18The bottom of the O isotope concentration tower is connected with the last-stage cascade18The last stage of the nitrogen reboiler III top of the O isotope lean removal tower18O isotope concentration tower top connected last stage cascade18O isotope and15n isotope condensing evaporator bottom.
Preferably, the method comprises the following steps: the first stage of cascade18And a nitrogen outlet of the O isotope lean-removing tower nitrogen reboiler I is connected with an inlet of a stop valve B, and an outlet of the stop valve B is exhausted to the atmosphere. Second stage of cascade18The nitrogen outlet of the O isotope lean-removing tower nitrogen reboiler II is connected with the inlet of a stop valve D, the outlet of the stop valve D is exhausted, and the last stage is connected with the tail end18The nitrogen outlet of the O isotope lean-removing tower nitrogen reboiler III is connected with the inlet of a stop valve F, the outlet of the stop valve F is exhausted, and the first stage is cascaded18The nitrogen inlet of the nitrogen reboiler I of the O isotope lean removal tower is connected with the outlet of the stop valve A, and the second stage is cascaded18The nitrogen inlet of a nitrogen reboiler II of the O isotope lean removal tower is connected with the outlet of a stop valve C and is connected with the final stage18The nitrogen inlet of the O isotope lean-separating tower nitrogen reboiler III is connected with the outlet of a stop valve E, the inlet of the stop valve A, the inlet of the stop valve C and the inlet of the stop valve E are connected with the outlets of an air separation cold nitrogen buffer device, and the first stage is cascaded18O isotope dephenolization tower nitrogen reboiler I, second stage cascade18O isotope element lean removing tower nitrogen reboiler II and final stage combination18And the O isotope depletion tower nitrogen reboiler III takes air separation cold nitrogen as a heat source.
The utility model relates to a two isotope low temperature synchronous separation device, production15N isotope and18an isotope of O. The utility model discloses will18O isotope and15the low-temperature enrichment of N isotope is integrated into a set of equipment so as to18O isotope and15low temperature of N isotopeThe rectification is carried out synchronously, and the isotope rectification efficiency is greatly improved. The utility model discloses utilize the boiling point difference of nitrogen gas and oxygen under certain pressure, will through the condensation evaporimeter18Cryogenic O-isotope rectification plant and15the N isotope low-temperature rectification device is combined and utilized18Evaporating oxygen at the top of the O isotope low-temperature rectifying tower as a heat source15N isotope low-temperature rectification tower bottom liquid nitrogen, and oxygen condensation18And (3) rectifying reflux liquid at low temperature by using the O isotope.18The reboiling heat source at the bottom of the O isotope cryogenic rectification tower is air separation cold nitrogen, and the cold energy of the air separation equipment is fully utilized. The utility model discloses18O isotope and15the N isotope cryogenic rectification device adopts a design of a plurality of cascades connected in series front and back, and each cascade is arranged in parallel by adopting a plurality of tubular towers. By combining the respective characteristics of regular packing and random packing, the two-layer wire mesh corrugated packing is arranged in the front cascade tower stages, and the rectangular spiral coil packing is arranged in the rear cascade tower stages, so that the raw material quantity processing capacity of the device is better, and the rectification efficiency of the device is higher. An isotope molecule cracking recombination catalysis system is arranged in the system, so that the abundance and the yield of the target isotope are improved.
Drawings
FIG. 1 is a schematic view of the present invention;
FIG. 2 is a schematic view of the air separation oxygen/nitrogen purification apparatus of FIG. 1;
FIG. 3 is a view of FIG. 118O isotope and15an N isotope synchronous cryogenic rectification cascade diagram;
FIG. 4 is a drawing showing18O isotope and15schematic diagram 1 of the N isotope cracking recombination catalytic device;
FIG. 5 is a drawing showing18O isotope and15the schematic diagram of the N isotope cracking recombination catalytic device is shown in a figure 2.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings, wherein a dual isotope low temperature synchronous separation device as shown in fig. 1 at least comprises an air separation oxygen purification system and an air separation nitrogen purification system,18o isotope and15an N isotope synchronous low-temperature rectification system,18o isotope and15the N isotope molecule cracking recombination system comprises three parts; the air separation oxygen purification system and the air separation nitrogen purification system at least comprise a combined tower formed by respectively integrating an air separation oxygen purification device and an air separation nitrogen purification device, a reboiler arranged at the bottom of the lower tower of the air separation oxygen purification device and the air separation nitrogen purification device, condensation evaporators of the air separation oxygen purification device and the air separation nitrogen purification device, a condenser arranged at the top of the upper tower of the air separation oxygen purification device and the air separation nitrogen purification device, and a pressure reducing valve;18o isotope and15the N isotope synchronous cryogenic rectification system at least comprises18O isotope and15the system comprises an N isotope multi-stage rectifying tower, a liquid oxygen nitrogen reboiler, an oxygen and nitrogen condensation evaporator and a liquid nitrogen condenser;18o isotope and15the N isotope atom cracking recombination system at least comprises an oxygen/nitrogen molecule cracking recombination catalytic device and a catalytic electric heater, wherein the combined tower is divided into an upper tower and a lower tower, wherein the upper tower filters light component impurities, the lower tower filters heavy component impurities, the pressure of the lower tower is higher than that of the upper tower, steam rising from the top of the lower tower is used as a heat source through boiling point difference to boil the accumulated liquid at the bottom of the upper tower, the upper towers of the air separation oxygen purification device and the air separation nitrogen purification device are operated under reduced pressure to remove light component impurities such as hydrogen, the heavy component impurities are filtered by the lower towers of the air separation oxygen purification device and the air separation nitrogen purification device through low-temperature rectification, and the content of the heavy component impurities such as hydrocarbon can be reduced to below 1ppm,
an inlet of the air separation nitrogen purification device 16 is connected with air separation nitrogen 33, the top of a lower tower A98 of the air separation nitrogen purification device 16 is connected with the bottom of an air separation nitrogen condensation evaporator A99, an upper gas outlet of a lower tower A98 of the air separation nitrogen purification device 16 is connected with an inlet of a pressure reducing valve A90, an outlet of the pressure reducing valve A90 is connected with a feed inlet of an upper tower A96 of the air separation nitrogen purification device 16, and the bottom of an upper tower A96 of the air separation nitrogen purification device 16 is connected with the top of the air separation nitrogen. The bottom of a lower tower A98 of an air separation nitrogen purification device 16 is connected with the top of a lower tower reboiler A109, the top of an upper tower A96 of the air separation nitrogen purification device 16 is connected with the bottom of an upper tower top condenser A101, the outlet of the air separation nitrogen purification device 16 is connected with the inlet of a high-purity raw material nitrogen mass flow controller 18, and the outlet of the high-purity raw material nitrogen mass flow controller 18 is connected with the bottom of a high-purity towerConnected to the first cascade15The middle raw material inlet of the N isotope lean removing tower 1. First stage of cascade15And exhausting the top waste gas of the N isotope depletion tower 1 to the atmosphere. First stage of cascade15The bottom of the N isotope lean removing tower 1 is connected with a first-stage cascade18O isotope and first order cascade15The top of the N isotope condensation evaporator 2 is cascaded in the first stage15The outlet of the N isotope condensation evaporator 2 is connected with a second-stage cascade15The middle raw material inlet of the N isotope lean removing tower 5. Second stage of cascade15The top waste gas 36 of the N isotope lean removing tower 5 is connected with the first-stage cascade15The return air port of the N isotope lean removing tower 1. Second stage of cascade15The bottom of the N isotope lean removing tower 5 is connected with a second-stage cascade18O isotope and second order cascade15N isotope condensing evaporator 6 top, second stage cascade15The outlet of the N isotope condensation evaporator 6 is connected with the next stage cascade15The raw material inlet of the N isotope lean removing tower is cascaded in the second stage15The return air port of the N isotope lean removing tower 5 is connected with the next stage of cascade15A top gas outlet of the N isotope lean removal tower, the first stage is cascaded15The top of the N isotope lean removing tower 1 is connected with a first-stage cascade15Bottom of N isotope condenser 13, second stage cascade15The top of the N isotope lean removing tower 5 is connected with a second-stage cascade15The bottom of the N isotope condenser 14, and the product discharge port of the second-stage cascade tower is arranged18O isotope and15the N isotope molecule cracking recombination catalysis device 32.
The inlet of the air separation oxygen 41 air separation oxygen purification device 17 is connected with the air separation oxygen 41 the top of a lower tower B58 of the air separation oxygen purification device 17 is connected with the bottom of an air separation oxygen condensation evaporator B79, the upper air outlet of a lower tower B58 of the air separation oxygen purification device 17 is connected with the inlet of a pressure reducing valve B60, the outlet of the pressure reducing valve B60 is connected with the feed inlet of an upper tower B56 of the air separation oxygen purification device 17, and the bottom of an upper tower B56 of the air separation oxygen purification device 17 is connected with the top of an. The bottom of a lower tower B58 of the air separation oxygen purification device 17 is connected with the top of a lower tower reboiler B59, the top of an upper tower B56 of the air separation oxygen purification device 17 is connected with the bottom of an upper tower top condenser B100, the outlet of the air separation oxygen purification device 17 is connected with the inlet of a high-purity raw material oxygen mass flow controller 19, and the high-purity raw material oxygen mass flow controllerThe outlet of the raw material oxygen mass flow controller 19 is connected with the first-stage cascade18The middle raw material inlet of the O isotope lean removing tower 3. First stage of cascade18And exhausting the waste gas at the top of the O isotope depreciation tower 3. First stage of cascade18The bottom of the O isotope lean removing tower 3 is connected with a first-stage cascade18O isotope dephenolization tower nitrogen reboiler I4, first stage cascade18The top of the O isotope lean removing tower 3 is connected with a first-stage cascade18O isotope and first order cascade15The N isotope condenses the bottom of the evaporator 2. First stage of cascade18The outlet of an O isotope lean removal tower nitrogen reboiler I4 is connected with a second-stage cascade18The middle raw material inlet of the O isotope lean removing tower 7. Second stage of cascade18The top of the O isotope lean removing tower 7 is connected with a second-stage cascade18O isotope and15the bottom of the N isotope condensation evaporator 6 is cascaded in the second stage18The top of the O isotope lean removal tower 7 is connected with a first-stage cascade18The return air port of the O isotope lean removing tower 3. Second stage of cascade18The bottom of the O isotope lean removing tower 7 is connected with a second-stage cascade18O isotope element de-lean tower nitrogen reboiler II 8, second stage cascade18The outlet of a nitrogen reboiler II 8 of the O isotope lean removal tower is connected with the next stage of cascade18And a raw material inlet of the O isotope dephenolizing tower.
The second stage18O isotope and15product discharge port arrangement of N isotope multi-stage rectifying tower18O isotope and15an N isotope molecule cracking recombination catalytic device 32, wherein a nitrogen inlet of the isotope molecule cracking recombination catalytic device 32 is connected with a second-stage cascade15N isotopes and cascades18The outlet of the O isotope condensation evaporator and the oxygen inlet of the isotope molecule cracking recombination catalytic device 32 are connected with the second cascade18An outlet of a nitrogen reboiler II of the O isotope lean removal tower, a nitrogen outlet of the isotope molecule cracking recombination catalytic device 32 is connected with an inlet of a catalyzed nitrogen outlet valve 20, and an outlet of the catalyzed nitrogen outlet valve 20 is connected with a final-stage cascade15N isotope concentration tower 9 raw material inlet, last stage cascade15The top of the N isotope concentration tower 9 is connected with an upper-stage cascade15And an N isotope lean removal tower return air port. Last stage cascade15N isotope enrichmentTower 9 bottom connected last stage cascade18O isotope and15the N isotope condenses the top of the evaporator 10. Last stage cascade15The top of the N isotope concentration tower 9 is connected with the last stage cascade15The bottom of the N isotope condenser 15. The oxygen outlet of the isotope molecule cracking recombination catalytic device 32 is connected with the inlet of the catalyzed oxygen outlet valve 21, the outlet of the catalyzed oxygen outlet valve 21 is connected with the final-stage cascade18Raw material inlet and final stage cascade of O isotope concentration tower 1118The top of the O isotope concentration tower is connected with an upper-stage cascade18And an O isotope element de-lean tower gas return port. Last stage cascade18The bottom of the O isotope concentration tower 11 is connected with the last stage cascade18The top of a nitrogen reboiler III 12 of an O isotope lean removal tower is cascaded at the last stage18The top of the O isotope concentration tower 11 is connected with the last stage cascade18O isotope and15the N isotope condenses the bottom of the evaporator 10.
The first stage of cascade18And a nitrogen outlet of the O isotope lean removal column nitrogen reboiler I4 is connected with an inlet of a stop valve B24, and an outlet of the stop valve B24 is exhausted to the atmosphere. Second stage of cascade18The nitrogen outlet of the O isotope lean-removing tower nitrogen reboiler II 8 is connected with the inlet of a stop valve D26, the outlet of the stop valve D26 is exhausted, and the last stage is connected with the tail stage18The nitrogen outlet of the O isotope lean removal tower nitrogen reboiler III 12 is connected with the inlet of a stop valve F28, the outlet of the stop valve F28 is exhausted to the atmosphere, and the first stage cascade is18The nitrogen inlet of an O isotope lean-removing tower nitrogen reboiler I4 is connected with the outlet of a stop valve A23, and the second stage is cascaded18The nitrogen inlet of a nitrogen reboiler II 8 of the O isotope lean removal tower is connected with the outlet of a stop valve C25 and is connected with the final stage18The nitrogen inlet of the O isotope lean removal tower nitrogen reboiler III 12 is connected with the outlet of a stop valve F27, the inlet of a stop valve A23, the inlet of a stop valve C25 and the inlet of a stop valve E27 are connected with the outlets of air-separation cold-nitrogen-blocking buffer devices 22, and the first-stage cascade is connected with the inlet of a first-stage cascade lean removal tower nitrogen reboiler III 1218O isotope dephenolization tower nitrogen reboiler I4, second stage cascade18O isotope element lean removing tower nitrogen reboiler II 8, final stage connection18And the O isotope depletion tower nitrogen reboiler III 12 takes air separation cold nitrogen as a heat source.
The embodiment of the utility model provides a
The utility model relates to a two isotope synchronous separation device uses empty oxygen of dividing and empty nitrogen gas of dividing as raw materials source, as rectification system feed gas after the edulcoration. The utility model discloses before the device starts, all valves are all closed. Before the system is started, the tightness of the system needs to be tested, and the leakage point of a system pipeline is ensured to be avoided. And then an electric control system of the detector is detected to ensure that electrical equipment such as the instrument and the like works normally.
Before the system is started, the oxygen and nitrogen pipelines of the system need to be correspondingly purged. Referring to fig. 1 and 2, the valve 90 and the mass flow controller 18 are opened, the air in the corresponding nitrogen line is replaced by normal pressure nitrogen (108 kpa (a)), when the dew point of the purge gas outlet is as low as-170 ℃, the purge is stopped, and the valve 90 and the mass flow controller 18 are closed. Opening the valve 60 and the mass flow controller 19, replacing air in the corresponding oxygen pipeline with normal pressure oxygen (108 Kpa (A)), stopping purging when the dew point of a purge gas outlet is as low as-170 ℃, and closing the valve 60 and the mass flow controller 19.
The system is started, firstly, the air separation nitrogen 33 enters the lower tower A98 of the air separation nitrogen purification device 16, the pressure reducing valve A90 is opened, the air separation nitrogen enters the upper tower A96 of the air separation nitrogen purification device 16, the upper tower 98 of the air separation nitrogen purification device 16 is started, the air separation nitrogen is liquefied, and liquid is accumulated at the bottom of the upper tower A96. When the liquid accumulation at the bottom of the upper tower A96 reaches the specified liquid level, the lower tower A98 reboiler A109 is opened, the ascending steam of the lower tower A98 is used as the reboiling heat source at the bottom of the upper tower A96, and the air separation nitrogen purification rectification balance is established.
Further, when the air-separated nitrogen impurities are detected to be qualified, the high-purity raw material nitrogen mass flow controller 18 is slowly opened, and the high-purity nitrogen 34 enters the first-stage cascade connection15An N isotope depreciation tower 1. Enabling first level cascading15N isotope condenser 13, high purity nitrogen liquefaction, first stage cascade15The bottom of the N isotope depreciation tower 1 is accumulated liquid.
And starting an air separation oxygen pipeline, enabling the air separation oxygen 41 to enter a lower tower B58 of the air separation oxygen purification device 17, opening a pressure reducing valve B60, enabling the air separation oxygen to enter an upper tower B56 of the air separation oxygen purification device 17, starting an upper tower B58 of the air separation oxygen purification device 17, liquefying the air separation oxygen, and adding liquid at the bottom of the upper tower B56. When the liquid accumulation at the bottom of the upper tower B56 reaches the specified liquid level, the lower tower B58 reboiler B59 is opened, the ascending steam of the lower tower B58 is used as the reboiling heat source at the bottom of the upper tower B56, and the air separation oxygen purification rectification balance is established.
Further, when the air-separated oxygen impurities are detected to be qualified, the high-purity raw material oxygen mass flow controller 19 is slowly opened, and the high-purity oxygen 42 enters the first-stage cascade connection18The O isotope lean removing tower 3, high-purity oxygen 42 are cascaded in the first stage18The top of the O isotope lean removing tower 3 is cascaded through a first stage18O isotope and first order cascade15N isotope condensing evaporator 2 evaporating first-stage cascade15The bottom of the N isotope lean removing tower 1 is accumulated liquid, high-purity oxygen 42 is condensed at the same time, and the first stage is cascaded18The bottom liquid of the O isotope depreciation tower 3. The stop valve A23 is slowly opened, and the air-separated cold nitrogen 50 enters the first stage cascade18O isotope element de-lean tower nitrogen reboiler I4 used as heat source to evaporate first-stage cascade18The accumulated liquid at the bottom of the O isotope lean removal tower 3 establishes a first-stage cascade18O isotope depletion tower 3 and first stage cascade15The rectification of the N isotope dephenolizing tower 1 is balanced. First stage of cascade18The waste gas at the top of the O isotope lean removing tower 3 is emptied and cascaded in a first stage15And exhausting the waste gas at the top of the N isotope dephenolizing tower 1. The valve 24 is opened, and the cold air 50 is cooled and then 51 exhausted to the atmosphere.
To pair18O isotope and15the synchronous rectification separation of N isotope is further explained. When the first stage is cascaded18O isotope depletion tower 3 and first stage cascade15The rectification balance of the N isotope lean removing tower 1 is established, and after products at the bottom of each tower are analyzed to be qualified, the first-stage cascade is firstly carried out15Qualified products 35 at the bottom of the N isotope lean removing tower 1 are cascaded through a first stage18O isotope and first order cascade15The gas outlet of the N isotope condensation evaporator 2 enters the second-stage cascade15And an N isotope depreciation tower 5. Enabling second stage cascading15N isotope condenser 14, first stage cascade15Qualified products 35 at the bottom of the N isotope lean removing tower 1 are liquefied and accumulated in a second-stage cascade15The bottom of the N isotope depreciation tower 5.
Further, the first stage is cascaded18The qualified product 43 at the bottom of the O isotope lean removing tower 3 passes through the first stepOne-stage cascade18An outlet of an O isotope lean removal tower nitrogen reboiler I4 enters a second-stage cascade18And an O isotope depreciation tower 7. First stage of cascade18Qualified products 43 at the bottom of the O isotope lean removing tower 3 are cascaded in the second stage18The top of the O isotope lean removing tower 7 passes through a second-stage cascade18O isotope and15n isotope condensing evaporator 6 evaporating second-stage cascade15The liquid nitrogen at the bottom of the N isotope lean removing tower 5 is cascaded in the first stage18Qualified products 43 at the bottom of the O isotope lean removing tower 3 are liquefied and accumulated in the second-stage cascade18The bottom of the O isotope depreciation tower 7. Slowly opening stop valve C25, and allowing the cold nitrogen 52 to enter the second cascade stage18O isotope element de-lean tower nitrogen reboiler II 8 as heat source evaporation second-stage cascade18The accumulated liquid at the bottom of the O isotope lean removal tower 7 establishes a second-stage cascade18O isotope depolitisation column 7 and second stage cascade15The rectification of the N isotope lean removing tower 5 is balanced. Second stage of cascade18The waste gas 44 at the top of the O isotope lean removing tower 7 returns to the first-stage cascade18O isotope lean-removing tower 3, second-stage cascade15The top waste gas 36 of the N isotope lean removing tower 5 returns to the first-stage cascade15An N isotope depreciation tower 1. Valve 26 is opened and the cooled air 53 is vented to atmosphere after air separation of cold nitrogen 52.
When the second stage is cascaded18O isotope depolitisation column 7 and second stage cascade15The rectification balance of the N isotope lean removing tower 5 is established, and the next stage is started after the products at the bottom of each tower are analyzed to be qualified18O isotope and15an N isotope cascade tower. Wherein the product oxygen 45 enters the next stage of cascade connection18The product nitrogen 37 enters the next stage of cascade connection15An N isotope depolitising tower; cascade of the next stage18The waste gas 46 at the top of the O isotope lean removing tower returns to the second-stage cascade18O isotope lean-removing tower 7, the next stage is cascaded15The top waste gas 38 of the N isotope lean removing tower returns to the second-stage cascade15And (4) an N isotope depoliferation tower.
Referring to fig. 3, the present invention provides n cascade towers connected in series, wherein the first m stages adopt structured packing, and the primary product can be produced in large quantity by utilizing the characteristic of large flux in the structured packing tower; the later (n-m) stage cascade tower adopts random packing, and utilizes the characteristic of high rectification efficiency of the random packing to quickly enrich the high-abundance product isotopes.
Further, for each stage of cascade tower, a plurality of tube tower is arranged in parallel, wherein the first stage of cascade tower is provided with m1The tube-row towers are connected in parallel, and the second-stage cascade tower is provided with m2The column-tube towers are connected in parallel, and the m-th cascade tower is provided with mmThe tube-array towers are connected in parallel, and the final-stage concentration tower is a single tube-array tower.
Referring to FIGS. 4-5, in order to save the raw material consumption and improve the rectification efficiency, the raw material inlet of the last-stage cascade tower is provided18O isotope and15the N isotope molecule cracking recombination catalysis device 32. The catalytic device 32 (the outer layer is wrapped with the heat preservation cotton 74) heats the nitrogen/oxygen to a certain temperature zone through the electric heater 73, and the oxygen molecules/nitrogen molecules are cracked and recombined under the action of the catalyst 75, so that the abundance of target isotope molecules can be improved.
Further, the electric heater 73 is turned on, from the second stage15The N isotope product enters a catalyst 75 pipeline and is subjected to the target reaction under the high-temperature catalysis action15The abundance of N isotope molecules is improved. After the catalysis is completed, the valve 20 is opened, and the final-stage cascade after the catalysis is completed15The raw material gas 39 of the N isotope rectifying tower enters the final stage cascade15N isotope rectification column, starting the last stage cascade15N isotope condenser 15, last stage cascade15N isotope rectifying tower raw material gas 39 is cascaded at last stage15N isotope rectifying tower 9 top is condensed and accumulated in the last stage cascade15The bottom of the N isotope rectifying tower 9. The valve 20 is closed and the remaining nitrogen in the catalytic device 32 for isotopic molecule cleavage recombination is evacuated.
Further, from the second stage18The O isotope product enters a catalyst 75 pipeline and is subjected to high-temperature catalysis to obtain a target18The abundance of O isotope molecules is improved. After the catalysis is completed, the valve 21 is opened, and the final-stage cascade after the catalysis is completed18The raw material gas 47 of the O isotope rectifying tower enters the final stage cascade18O isotope rectifying tower 11, cascaded at last stage18The top of the O isotope rectifying tower 11 is cascaded through the last stage18O isotope and15n isotope condensing evaporator 10 evaporation final stage cascade15Liquid nitrogen at the bottom of N isotope rectifying tower 9, and the last stage is cascaded18The raw material gas 47 of the O isotope rectifying tower is liquefied and accumulated in the final stage cascade18And the bottom of the O isotope rectifying tower 11. The valve 27 is slowly opened, and the cold nitrogen 54 enters the final cascade18O isotope dephenolization tower nitrogen reboiler 12 as heat source evaporation last stage cascade18Liquid oxygen at the bottom of the O isotope rectifying tower 11 establishes the final stage cascade15N isotope rectifying tower and final stage cascade18And (4) balancing the rectification of the O isotope rectifying tower. After the rectification is balanced, the mixture is distilled,1540 portions of N isotope product,18O-isotope product 49 goes to the product filling system. The valve 28 is opened and the cooled air 54 is vented 55 to atmosphere.
The following steps are required: air separation oxygen (200 Kpa, 97K, V/V ≧ 99.6%) and nitrogen (300 Kpa, 88K, V/V ≧ 99.9%) are purified by a purification device to remove light/heavy component impurities. The lower tower 58 (oxygen: 200KPa, 97K; nitrogen: 300KPa, 88K) of the purification tower is used for removing heavy component impurities, and the upper tower 56 (oxygen: 135KPa, 92.8K; nitrogen: 230KPa, 84.6K) of the purification tower is used for removing light component impurities, so that high-purity oxygen with the purity of more than 5n and nitrogen are obtained to be used as isotope rectification feed gases.
The following steps are required: the first stage cascade tower adopts a regular packed tower with the length-diameter ratio less than or equal to 0.04, and the subsequent stages adopt a regular packed tower with the length-diameter ratio less than or equal to 0.02. The last stages adopt a rectangular spiral random packing tower with the length-diameter ratio less than or equal to 0.02.
The following steps are required: and standing the isotope raw material gas in a temperature zone of 680-730K for 36-48 h in the catalyst. The total length of the catalyst is 50-70 m.
The following steps are required:15n isotope and18the O isotope rectification cascade tower is operated by total reflux, a cold source at the top is 80K normal pressure liquid nitrogen, and nitrogen gas 674KPa and 98K are boiled at the bottom.
The utility model relates to a two isotope low temperature synchronous separation device uses empty nitrogen gas and oxygen that divides as the raw materials, produces15N isotope and18an isotope of O. The utility model discloses a device18O isotope and15the low-temperature enrichment process of the N isotope is synchronously carried out, so that the isotope production is greatly improvedThe production efficiency is high. The utility model discloses utilize the boiling point difference of nitrogen gas and oxygen under certain pressure, will through the condensation evaporimeter18Cryogenic O-isotope rectification plant and15the N isotope low-temperature rectification device is combined and utilized18Evaporating oxygen at the top of the O isotope low-temperature rectifying tower as a heat source15N isotope low-temperature rectification tower bottom liquid nitrogen, and oxygen condensation18And (3) rectifying reflux liquid at low temperature by using the O isotope.18The reboiling heat source at the bottom of the O isotope cryogenic rectification tower is air separation cold nitrogen, and the cold energy of the air separation equipment is fully utilized.

Claims (5)

1. A dual-isotope low-temperature synchronous separation device at least comprises an air separation oxygen purification system and an air separation nitrogen purification system,18o isotope and15an N isotope synchronous low-temperature rectification system,18o isotope and15the N isotope molecule cracking recombination system comprises three parts; the system is characterized in that the air separation oxygen purification system and the air separation nitrogen purification system at least comprise a combined tower formed by respectively integrating an air separation oxygen purification device and an air separation nitrogen purification device, a reboiler arranged at the bottom of the lower tower of the air separation oxygen purification device and the air separation nitrogen purification device, condensation evaporators of the air separation oxygen purification device and the air separation nitrogen purification device, a condenser arranged at the top of the upper tower of the air separation oxygen purification device and the air separation nitrogen purification device, and a pressure reducing valve;18o isotope and15the N isotope synchronous cryogenic rectification system at least comprises18O isotope and15the system comprises an N isotope multi-stage rectifying tower, a liquid oxygen nitrogen reboiler, an oxygen and nitrogen condensation evaporator and a liquid nitrogen condenser;18o isotope and15the N isotope atom cracking recombination system at least comprises an oxygen/nitrogen molecule cracking recombination catalytic device and a catalytic electric heater, the combined tower of the air separation oxygen purification device and the air separation nitrogen purification device comprises an upper tower and a lower tower, wherein the upper tower filters out light component impurities, the lower tower filters out heavy component impurities, the pressure of the lower tower is higher than that of the upper tower, the steam rising from the top of the lower tower is used as a heat source to reboil the upper tower bottom accumulated liquid through the difference of boiling points, the upper tower pressure reduction operation of the air separation oxygen purification device and the air separation nitrogen purification device excludes the light component impurities such as hydrogen, and the likeHeavy component impurities are removed through low-temperature rectification filtration in the lower tower of the air separation oxygen purification device and the air separation nitrogen purification device, and the content of the heavy component impurities such as hydrocarbon can be reduced to below 1 ppm.
2. The dual-isotope low-temperature synchronous separation device according to claim 1, characterized in that the inlet of the air separation nitrogen purification device (16) is connected with air separation nitrogen (33), the top of the lower tower A (98) of the air separation nitrogen purification device (16) is connected with the bottom of an air separation nitrogen condensation evaporator A (99), the upper air outlet of the lower tower A (98) of the air separation nitrogen purification device (16) is connected with the inlet of a pressure reducing valve A (90), the outlet of the pressure reducing valve A (90) is connected with the feed inlet of an upper tower A (96) of the air separation nitrogen purification device (16), the bottom of the upper tower A (96) of the air separation nitrogen purification device (16) is connected with the top of the air separation nitrogen condensation evaporator A (99), the bottom of the lower tower A (98) of the nitrogen purification device (16) is connected with the top of a reboiler A (109), the top of the upper tower A (96) of the nitrogen purification device (16, the outlet of the air separation nitrogen purification device (16) is connected with the inlet of a high-purity raw material nitrogen mass flow controller (18), and the outlet of the high-purity raw material nitrogen mass flow controller (18) is connected with a first-stage cascade15The middle raw material inlet of the N isotope lean removing tower (1) is cascaded in the first stage15The waste gas at the top of the N isotope lean removing tower (1) is exhausted to the atmosphere, and the first stage is cascaded15The bottom of the N isotope lean removing tower (1) is connected with a first-stage cascade18O isotope and first order cascade15The top of the N isotope condensation evaporator (2) is cascaded in the first stage15The outlet of the N isotope condensation evaporator (2) is connected with the second-stage cascade15The middle raw material inlet of the N isotope lean removing tower (5) is cascaded in the second stage15The top waste gas (36) of the N isotope lean removing tower (5) is connected with the first-stage cascade15The return air port of the N isotope lean removing tower (1) is cascaded in the second stage15The bottom of the N isotope lean removing tower (5) is connected with a second-stage cascade18Isotope of O and second order15The top of the N isotope condensation evaporator (6) is the second stage15The outlet of the N isotope condensation evaporator (6) is connected with the next stage of cascade15The raw material inlet of the N isotope lean removing tower is cascaded in the second stage15The return air port of the N isotope lean removing tower (5) is connected with the next stage of cascade15A top gas outlet of the N isotope lean removal tower, the first stage is cascaded15The top of the N isotope lean removing tower (1) is connected with a first-stage cascade15The bottom of the N isotope condenser (13) is cascaded in the second stage15The top of the N isotope lean removing tower (5) is connected with a second-stage cascade15The bottom of the N isotope condenser (14) is provided with a product discharge hole of the second-stage cascade tower18O isotope and15a recombination catalytic device (32) for cracking N isotope molecules.
3. The dual-isotope low-temperature synchronous separation device according to claim 1, characterized in that the inlet of the air separation oxygen purification device (17) is connected with the air separation oxygen (41), the top of the lower tower B (58) of the air separation oxygen purification device (17) is connected with the bottom of an air separation oxygen condensation evaporator B (79), the upper air outlet of the lower tower B (58) of the air separation oxygen purification device (17) is connected with the inlet of a pressure reducing valve B (60), the outlet of the pressure reducing valve B (60) is connected with the feed inlet of an upper tower B (56) of the air separation oxygen purification device (17), the bottom of the upper tower B (56) of the air separation oxygen purification device (17) is connected with the top of the air separation oxygen condensation evaporator B (79), the bottom of the lower tower B (58) of the air separation oxygen purification device (17) is connected with the top of a lower tower B (59), the top of the upper tower B (56) of the, the outlet of the air separation oxygen purification device (17) is connected with the inlet of a high-purity raw material oxygen mass flow controller (19), and the outlet of the high-purity raw material oxygen mass flow controller (19) is connected with a first-stage cascade18The middle raw material inlet of the O isotope lean removing tower (3) is cascaded in the first stage18The waste gas at the top of the O isotope lean removing tower (3) is exhausted to the atmosphere, and the first stage is cascaded18The bottom of the O isotope lean removing tower (3) is connected with a first-stage cascade18O isotope dephenolization tower nitrogen reboiler I (4) and the first stage is cascaded18The top of the O isotope lean removing tower (3) is connected with a first-stage cascade18O isotope and first order cascade15The bottom of the N isotope condensation evaporator (2)One-stage cascade18The outlet of the nitrogen reboiler I (4) of the O isotope lean removal tower is connected with the second-stage cascade18The middle raw material inlet of the O isotope lean removing tower (7) is cascaded in the second stage18The top of the O isotope lean removing tower (7) is connected with a second-stage cascade18Isotope of O and second order15The bottom of the N isotope condensation evaporator (6) is cascaded in the second stage18The top of the O isotope lean removal tower (7) is exhausted and connected with a first-stage cascade18The return air port of the O isotope lean removing tower (3) is cascaded in the second stage18The bottom of the O isotope lean removing tower (7) is connected with a second-stage cascade18O isotope element de-lean tower nitrogen reboiler II (8) and the second stage is cascaded18The outlet of a nitrogen reboiler II of the O isotope lean removal tower is connected with the next stage of cascade18And a raw material inlet of the O isotope dephenolizing tower.
4. The dual-isotope cryo-synchronous separation device of claim 1, wherein the dual isotopes are separated in parallel18O isotope and15product discharge port arrangement of N isotope multi-stage rectifying tower18O isotope and15the N isotope molecule cracking recombination catalytic device (32), the nitrogen inlet of the isotope molecule cracking recombination catalytic device (32) is connected with the second-stage cascade15N isotopes and cascades18The outlet of the O isotope condensation evaporator and the oxygen inlet of the isotope molecule cracking recombination catalytic device (32) are connected with the second cascade18An outlet of a nitrogen reboiler II of the O isotope lean removal tower, a nitrogen outlet of the isotope molecule cracking recombination catalytic device (32) is connected with an inlet of a catalyzed nitrogen outlet valve (20), and an outlet of the catalyzed nitrogen outlet valve (20) is connected with an outlet of a final-stage cascade connection15The raw material inlet of the N isotope concentration tower (9) is cascaded at the last stage15The top of the N isotope concentration tower (9) is connected with an upper-stage cascade15N isotope lean-removing tower gas return port, last stage cascade15The bottom of the N isotope concentration tower (9) is connected with the last stage cascade18O isotope and15top of N isotope condensing evaporator (10) and final stage cascade15The top of the N isotope concentration tower (9) is connected with the last stage cascade15The isotope molecules are cracked at the bottom of an N isotope condenser (15)The oxygen outlet of the recombination decomposition catalytic device (32) is connected with the inlet of the catalyzed oxygen outlet valve (21), and the outlet of the catalyzed oxygen outlet valve (21) is connected with the final-stage cascade18The raw material inlet of an O isotope concentration tower (11) is cascaded at the last stage18The top of the O isotope concentration tower is connected with an upper-stage cascade18The return air port of the O isotope lean removing tower is cascaded at the last stage18The bottom of the O isotope concentration tower (11) is connected with the last stage cascade18The top of a nitrogen reboiler III (12) of an O isotope depreciation tower is cascaded at the last stage18The top of the O isotope concentration tower (11) is connected with the last stage cascade18O isotope and15n isotope condensing evaporator (10).
5. The dual isotope cryogenic synchronous separation plant of claim 3, wherein the first stage cascade is characterized by18The nitrogen outlet of the O isotope lean-removing tower nitrogen reboiler I (4) is connected with the inlet of a stop valve B (24), the outlet of the stop valve B (24) is exhausted to the atmosphere, and the second stage is cascaded18The nitrogen outlet of the O isotope lean-removing tower nitrogen reboiler II (8) is connected with the inlet of a stop valve D (26), the outlet of the stop valve D (26) is exhausted to atmosphere, and the last stage is connected with the reboiler18The nitrogen outlet of the O isotope lean-removing tower nitrogen reboiler III (12) is connected with the inlet of a stop valve F (28), the outlet of the stop valve F (28) is exhausted to the atmosphere, and the first stage is cascaded18The nitrogen inlet of the O isotope lean-removing tower nitrogen reboiler I (4) is connected with the outlet of a stop valve A (23), and the second stage is cascaded18The nitrogen inlet of a nitrogen reboiler II (8) of the O isotope lean removal tower is connected with the outlet of a stop valve C (25) and is connected with the final stage18The nitrogen inlet of the O isotope lean-rejection column nitrogen reboiler III (12) is connected with the outlet of a stop valve E (27), the inlet of a stop valve A (23), the inlet of a stop valve C (25) and the inlet of the stop valve E (27) are connected with the outlets of air-cooled nitrogen buffer devices (22), and the first-stage cascade is connected with the outlets of the air-cooled nitrogen buffer devices18O isotope dephenolization tower nitrogen reboiler I (4) and second-stage cascade18O isotope element de-lean tower nitrogen reboiler II (8) and final stage connection18And the O isotope depletion tower nitrogen reboiler III (12) takes air separation cold nitrogen as a heat source.
CN202020753725.9U 2020-05-09 2020-05-09 Double-isotope low-temperature synchronous separation device Active CN212941496U (en)

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Address after: 799 Xiangfu Road, Qingshanhu street, Lin'an District, Hangzhou City, Zhejiang Province

Patentee after: Hang Yang Group Co.,Ltd.

Address before: 310006 Hongyuan building, 592 Zhongshan North Road, Xiacheng District, Hangzhou City, Zhejiang Province

Patentee before: Hangzhou oxygen generator group Co.,Ltd.