CN108106326B - Method and device for recycling nitrogen in krypton-xenon refining process - Google Patents

Method and device for recycling nitrogen in krypton-xenon refining process Download PDF

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Publication number
CN108106326B
CN108106326B CN201810050490.4A CN201810050490A CN108106326B CN 108106326 B CN108106326 B CN 108106326B CN 201810050490 A CN201810050490 A CN 201810050490A CN 108106326 B CN108106326 B CN 108106326B
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tower
xenon
nitrogen
pure
krypton
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CN108106326A (en
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郝文炳
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Hanmo Energy Technology Shanghai Co ltd
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Hanmo Energy Technology Shanghai Co ltd
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04745—Krypton and/or Xenon
    • F25J3/04751—Producing pure krypton and/or xenon recovered from a crude krypton/xenon mixture
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0204—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the feed stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/028—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0295—Start-up or control of the process; Details of the apparatus used, e.g. sieve plates, packings
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04278—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using external refrigeration units, e.g. closed mechanical or regenerative refrigeration units
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/10—Processes or apparatus using separation by rectification in a quadruple, or more, column or pressure system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/34—Krypton
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/36—Xenon
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/42—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/12—External refrigeration with liquid vaporising loop
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration cycle
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • F25J2270/904—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
    • F25J3/0426—The cryogenic component does not participate in the fractionation

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

The invention relates to a method for recycling nitrogen in a krypton-xenon refining process, which adopts liquid nitrogen as a cold source, and nitrogen discharged by each condensation evaporator is recycled, wherein the recycled nitrogen is divided into normal-temperature nitrogen and low-temperature nitrogen; the method comprises the steps of taking vaporized nitrogen discharged from a first-stage condensation evaporator as low-temperature nitrogen, summarizing nitrogen discharged from other condensation evaporators, and re-heating the nitrogen by a main heat exchanger to obtain normal-temperature nitrogen; the invention also relates to a device applied to the method, which comprises each rectifying tower, each condensing evaporator, a main heat exchanger, a circulating compressor and a connecting pipeline. Compared with the prior art, the invention adopts the mixed gas of liquid nitrogen and nitrogen as a cold source, can stably maintain the operation temperature of each condensation evaporator, and ensures the smooth proceeding of rectification; by recycling nitrogen, the consumption of liquid nitrogen or nitrogen in the krypton-xenon refining process can be greatly reduced, so that the energy consumption and the production cost are reduced.

Description

Method and device for recycling nitrogen in krypton-xenon refining process
Technical Field
The invention relates to a method for recycling gas, in particular to a method and a device for recycling nitrogen in a krypton-xenon refining process.
Background
The krypton and xenon contents in the atmosphere are about 1.138×10 -6 and 0.0857 ×10 -6, respectively, and after entering the low-temperature rectifying tower of the air separation device along with air, the high-boiling components krypton (Kr), xenon (Xe), hydrocarbon (mainly methane) and fluoride are all accumulated in the liquid oxygen of the low-pressure tower, and the liquid oxygen of the low-pressure tower is sent to an additional rectifying tower (commonly called a lean krypton tower) of krypton. A krypton-xenon-depleted concentrate having a kr+xe content of 0.2 to 0.3% can be obtained, wherein the methane content is about 0.3 to 0.4%. Too high a methane content in the oxygen (typically not exceeding 0.5% ch 4) is extremely dangerous and it is only possible to continue to increase the concentration of krypton-xenon in the liquid oxygen after the pre-removal of methane from the krypton-xenon-depleted concentrate, which is first pressurized to a critical pressure of 5.5MPa and vaporized and then depressurized to 1.0MPa before entering the methane purification unit in the known process. The methane purifying device is to remove methane after oxygen and methane are chemically reacted at 480-500 ℃ through palladium catalyst (the residual methane content can be lower than 1X 10 -6), and then to remove chemical reaction products-carbon dioxide and water through molecular sieve adsorption. And (3) feeding the raw material gas after removing methane into a first-stage rectifying tower to obtain a krypton-xenon mixture.
The common refining equipment uses the krypton-xenon mixture as a raw material, uses the mixed gas of nitrogen and liquid nitrogen as a cold source, separates the krypton gas and the xenon gas in a multi-stage rectification mode, and further purifies the krypton gas and the xenon gas. The nitrogen needed by the refining equipment is usually obtained from the vaporization of the liquid nitrogen, so that the liquid nitrogen of the refining equipment is large in use amount and high in cost, but the cold of the cold source is not fully recovered in the prior art, so that certain energy loss is caused, the energy consumption is high, and the economic benefit is reduced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to develop a krypton-xenon refining method based on the characteristic that the nitrogen usage amount in the existing krypton-xenon refining equipment is too large, and the method accurately recycles the nitrogen in the krypton-xenon refining, so that the nitrogen is recycled, the liquid nitrogen usage amount is effectively reduced, and the energy consumption is reduced.
In order to achieve the above purpose, the invention adopts the following technical scheme:
The first object of the invention is to provide a method for recycling nitrogen in a krypton-xenon refining process, wherein the krypton-xenon refining process comprises a first-stage rectifying tower, a second-stage rectifying tower, a pure krypton tower, a crude xenon tower and a pure xenon tower which are used for separation and refining, the tops of the towers are respectively provided with a first-stage condensation evaporator, a second-stage condensation evaporator, a pure krypton tower condensation evaporator, a crude xenon tower condensation evaporator and a pure xenon tower condensation evaporator, the krypton-xenon refining process adopts liquid nitrogen as a cold source, nitrogen discharged by each condensation evaporator is recycled, and the recycled nitrogen is divided into normal-temperature nitrogen and low-temperature nitrogen; the vaporized nitrogen discharged from the first-stage condensation evaporator is taken as low-temperature nitrogen, and the nitrogen discharged from the rest condensation evaporators is collected and reheated by the main heat exchanger to be taken as normal-temperature nitrogen.
In order to further optimize the method, the technical measures adopted by the invention further comprise:
Further, according to the operation temperature of each tower, the primary condensation evaporator adopts liquid nitrogen mixed in a certain proportion and normal-temperature nitrogen after partial cooling as cold sources, and the secondary condensation evaporator, the pure krypton tower condensation evaporator, the crude xenon tower condensation evaporator and the pure xenon tower condensation evaporator respectively adopt low-temperature nitrogen and normal-temperature nitrogen mixed in a corresponding proportion as cold sources.
Further, nitrogen discharged from the secondary condensation evaporator, the pure krypton tower condensation evaporator, the crude xenon tower condensation evaporator and the pure xenon tower condensation evaporator is collected and then reheated by the main heat exchanger, and then sent to the circulating compressor for pressurization to form normal-temperature nitrogen; the normal temperature nitrogen gas comes out of the circulating compressor and is divided into two paths, one path is cooled by the main heat exchanger and then enters the condensing evaporator of the first-stage rectifying tower to be mixed with liquid nitrogen to generate low-temperature nitrogen gas, and the other path directly enters the tower to be used as normal temperature nitrogen gas to participate in temperature adjustment.
Further, the primary rectifying tower, the secondary rectifying tower, the pure krypton tower, the crude xenon tower, the pure xenon tower and the main heat exchanger are all placed in the same cold box to serve as a fractionating tower.
Further, the krypton-xenon refining process comprises the following treatment steps: concentrating the krypton-xenon mixture by front-end krypton-xenon crude equipment, adding the concentrated krypton-xenon mixture into a first-stage rectifying tower in a fractionating tower through a pipeline or a container, removing low-boiling components, and then sending the low-boiling components into a second-stage rectifying tower; in the secondary rectifying tower, the materials are separated into high-boiling crude xenon and low-boiling crude krypton;
Wherein, the crude krypton discharged from the top of the secondary rectifying tower is sent to a pure krypton tower, in which high boiling components are separated and discharged from the bottom of the tower, and the pure krypton is discharged from the top of the tower and sent to the next step;
the method comprises the steps that crude xenon discharged from the bottom of a secondary rectifying tower firstly enters the crude xenon tower to remove high-boiling-point components, purer xenon is obtained from the top of the crude xenon tower, and enters the pure xenon tower; the low boiling point components are removed again in a pure xenon column, pure xenon is withdrawn from the bottom of the column and sent to the next process.
Further, the low boiling point components removed in the primary rectifying tower are mainly oxygen and nitrogen.
Further, the next step of pure krypton and the next step of pure xenon include filling or piping.
The second object of the invention is to provide a device for recycling nitrogen in a krypton-xenon refining process, which comprises a first-stage rectifying tower, a second-stage rectifying tower, a pure krypton tower, a crude xenon tower and a pure xenon tower which are used for separation and refining, wherein the tops of the towers are respectively provided with a first-stage condensation evaporator, a second-stage condensation evaporator, a pure krypton tower condensation evaporator, a crude xenon tower condensation evaporator and a pure xenon tower condensation evaporator correspondingly; the device also comprises a main heat exchanger, a circulating compressor and pipelines which are connected with the main heat exchanger and the circulating compressor in sequence and used for providing cold energy, wherein the main heat exchanger and the circulating compressor are respectively connected with the first-stage condensation evaporator, the second-stage condensation evaporator, the pure krypton tower condensation evaporator, the crude xenon tower condensation evaporator and the pure xenon tower condensation evaporation.
In order to further optimize the device, the technical measures of the invention also comprise:
Further, the pipe includes:
a liquid nitrogen inlet pipe for delivering liquid nitrogen to the primary condensing evaporator;
The low-temperature nitrogen pipe is used for respectively conveying the vaporized nitrogen discharged from the first-stage condensation evaporator to the second-stage condensation evaporator, the pure krypton tower condensation evaporator, the crude xenon tower condensation evaporator and the pure xenon tower condensation evaporator as low-temperature nitrogen;
The nitrogen outlet pipe is used for collecting nitrogen discharged by the secondary condensation evaporator, the pure krypton tower condensation evaporator, the crude xenon tower condensation evaporator and the pure xenon tower condensation evaporator and then conveying the nitrogen to the main heat exchanger for reheating;
the normal-temperature nitrogen pipe is used for conveying the nitrogen reheated by the main heat exchanger to the circulating compressor as normal-temperature nitrogen;
The first normal-temperature nitrogen branch pipe is used for conveying part of normal-temperature nitrogen at the outlet of the circulating compressor to the second-stage condensation evaporator, the pure krypton tower condensation evaporator, the crude xenon tower condensation evaporator and the pure xenon tower condensation evaporator respectively;
and the second normal-temperature nitrogen branch pipe is used for conveying part of normal-temperature nitrogen at the outlet of the circulating compressor to the main heat exchanger for cooling and conveying the part of normal-temperature nitrogen to the first-stage condensation evaporator.
Further, the normal temperature nitrogen pipes which are conveyed to the secondary condensation evaporator, the pure krypton tower condensation evaporator, the crude xenon tower condensation evaporator and the pure xenon tower condensation evaporator are respectively communicated with the low temperature nitrogen pipes which are conveyed to the secondary condensation evaporator, the pure krypton tower condensation evaporator, the crude xenon tower condensation evaporator and the pure xenon tower condensation evaporator.
Further, the middle part of the primary rectifying tower is connected with a feeding pipe, the top outlet pipe of the primary rectifying tower is connected to the main heat exchanger to recover cold energy, and the bottom outlet pipe of the primary rectifying tower is communicated to the middle part of the secondary rectifying tower; the crude krypton pipe at the top of the secondary rectifying tower is communicated to the middle part of the pure krypton tower, the pure krypton pipe is arranged at the top of the pure krypton tower, and a high-boiling-point component discharge pipe is arranged at the bottom of the pure krypton tower; the crude xenon pipe at the bottom of the secondary rectifying tower is communicated to the middle part of the crude xenon tower, the top of the crude xenon tower is provided with a purer xenon pipe, and the bottom of the crude xenon tower is provided with a high-boiling-point component discharge pipe; the purer xenon tube is communicated to the middle part of the pure xenon tower, the top of the pure xenon tower is provided with a low boiling point component discharge tube, and the bottom of the pure xenon tower is provided with the purer xenon tube.
Further, the nitrogen outlet pipe is communicated to the middle part of the main heat exchanger.
Further, the recycle compressor comprises a compressor and a compressor aftercooler which are connected in sequence.
Further, electric heaters are respectively arranged at the bottoms of the first-stage rectifying tower, the second-stage rectifying tower, the pure krypton tower, the crude xenon tower and the pure xenon tower.
Further, the main heat exchanger, the primary rectifying tower, the secondary rectifying tower, the pure krypton tower, the crude xenon tower, the pure xenon tower and connecting pipelines thereof are all placed in the same cold box and used as a fractionating tower.
Further, the heat insulating material is paved in the cold box, and the heat insulating material comprises superfine glass wool or expanded perlite, and other suitable insulating materials can also be adopted.
Further, the first-stage rectifying tower, the second-stage rectifying tower, the pure krypton tower, the crude xenon tower and the pure xenon tower are plate towers or packed towers.
Further, valves are arranged on the pipelines, and the valves are selected from stop valves, ball valves, gate valves, angle valves and butterfly valves.
It is well known that the operation of a rectifying column, the gas rising at the bottom of the column and the liquid descending at the top of the column are conditions necessary for the proper operation of the rectifying column. The flow rate of the krypton-xenon refining equipment is generally small, and the ascending gas is usually obtained by heating liquid by an electric heater at the bottom of the tower. The descending liquid is obtained by condensing the gas at the top of each rectifying tower through a respective condensing evaporator. The invention adopts liquid nitrogen to provide a cold source for the whole system, and can supplement nitrogen with circulation loss. If the liquid nitrogen amount is larger than the nitrogen leakage amount, the redundant nitrogen in the system is required to be exhausted.
Compared with the prior art, the invention has the following beneficial effects:
According to the invention, the cold source of the condensation evaporator is mixed with nitrogen into low-temperature gas through liquid nitrogen, the direct mixed gas is used as the cold source of the first-stage rectification tower according to different operation temperatures of each rectification tower, and the vaporized low-temperature nitrogen is mixed with normal-temperature nitrogen outside the separation tower after exiting the first-stage condensation evaporator. According to the different operating temperatures of each rectifying tower, the low-temperature nitrogen and the normal-temperature nitrogen are mixed in different proportions. The temperature difference of each condensing evaporator is ensured to be within the design range, so that the rectifying tower is ensured to smoothly separate various substances. According to the invention, through recycling nitrogen, the consumption of liquid nitrogen or nitrogen in the krypton-xenon refining process can be greatly reduced, so that the energy consumption and the production cost are reduced.
Drawings
FIG. 1 is a schematic flow diagram of an apparatus for recycling nitrogen in refining krypton and xenon according to an embodiment of the present invention;
Reference numerals in the drawings are as follows:
1. A recycle compressor; 101. a compressor; 102. a compressor aftercooler; 2. a fractionating tower; 3. a main heat exchanger; 4. a first-stage rectifying tower; 5. a second-stage rectifying tower; 6. a pure krypton column; 7. a crude xenon column; 8. a pure xenon column; 9. a first stage condensing evaporator; 10. a secondary condensing evaporator; 11. a pure krypton column condensation evaporator; 12. a crude xenon column condensing evaporator; 13. condensing evaporator of pure xenon tower; 21. a liquid nitrogen inlet pipe; 22. a low temperature nitrogen pipe; 23. a nitrogen outlet pipe; 24. a normal temperature nitrogen pipe; 25. a first normal temperature nitrogen manifold; 26. and a second normal temperature nitrogen branch pipe.
Detailed Description
The invention provides a method for recycling nitrogen in a krypton-xenon refining process, which comprises a first-stage rectifying tower, a second-stage rectifying tower, a pure krypton tower, a crude xenon tower and a pure xenon tower which are used for separation and refining, wherein the tops of the towers are respectively provided with a first-stage condensation evaporator, a second-stage condensation evaporator, a pure krypton tower condensation evaporator, a crude xenon tower condensation evaporator and a pure xenon tower condensation evaporator correspondingly, the krypton-xenon refining process adopts liquid nitrogen as a cold source, nitrogen discharged by each condensation evaporator is recycled, and the recycled nitrogen is divided into normal-temperature nitrogen and low-temperature nitrogen; the vaporized nitrogen discharged from the first-stage condensation evaporator is used as low-temperature nitrogen, and the nitrogen discharged from the rest condensation evaporators is mixed and reheated by the main heat exchanger to be used as normal-temperature nitrogen. The invention also provides a device for recycling nitrogen in the krypton-xenon refining process applied to the method.
The following describes the embodiments of the present invention further with reference to the drawings and examples. The following examples are only for more clearly illustrating the technical aspects of the present invention, and are not intended to limit the scope of the present invention.
Example 1
This embodiment is a preferred form of apparatus for recycling nitrogen in the purification of krypton-xenon.
As shown in fig. 1, the device described in this embodiment includes a first-stage rectifying column 4, a second-stage rectifying column 5, a pure krypton column 6, a crude xenon column 7, and a pure xenon column 8 for separation and refining, the tops of the respective columns are respectively provided with a first-stage condensing evaporator 9, a second-stage condensing evaporator 10, a pure krypton column condensing evaporator 11, a crude xenon column condensing evaporator 12, and a pure xenon column condensing evaporator 13, and the bottoms of the respective columns are respectively provided with electric heaters; the middle part of the primary rectifying tower 4 is connected with a feeding pipe, the top outlet pipe of the primary rectifying tower 4 is used for recovering cold energy through the main heat exchanger 3, and the bottom outlet pipe of the primary rectifying tower 4 is communicated with the middle part of the secondary rectifying tower 5; the crude krypton pipe at the top of the second-stage rectifying tower 5 is communicated to the middle part of the pure krypton tower 6, the pure krypton pipe is arranged at the top of the pure krypton tower 6, the high-boiling-point component discharge pipe is arranged at the bottom of the pure krypton tower 6, the crude xenon pipe at the bottom of the second-stage rectifying tower 5 is communicated to the middle part of the crude xenon tower 7, the purer xenon pipe is arranged at the top of the crude xenon tower 7, the high-boiling-point component discharge pipe is arranged at the bottom of the crude xenon tower 7, the purer xenon pipe is communicated to the middle part of the pure xenon tower 8, the low-boiling-point component discharge pipe is arranged at the top of the pure xenon tower 8, and the pure xenon pipe is arranged at the bottom of the pure xenon tower 8.
As shown in fig. 1, the device further comprises a main heat exchanger 3, a circulating compressor 1 and pipelines connected with the condensation evaporators 9/10/11/12/13 for providing cold energy, wherein the main heat exchanger 3, the circulating compressor 1 and the pipelines are connected in sequence; wherein the recycle compressor 1 comprises a compressor 101 and a compressor after cooler 102 connected in sequence. The above-mentioned piping for supplying cold includes a liquid nitrogen inlet pipe 21 for feeding liquid nitrogen to the primary condensing evaporator 9; a low-temperature nitrogen pipe 22 for conveying the vaporized nitrogen discharged from the first-stage condensation evaporator 9 as low-temperature nitrogen to the second-stage condensation evaporator 10, the pure krypton column condensation evaporator 11, the crude xenon column condensation evaporator 12 and the pure xenon column condensation evaporator 13, respectively; the nitrogen outlet pipe 23 is used for collecting nitrogen discharged by the secondary condensation evaporator 10, the pure krypton tower condensation evaporator 11, the crude xenon tower condensation evaporator 12 and the pure xenon tower condensation evaporator 13 and then conveying the nitrogen to the main heat exchanger 3 for reheating; the normal-temperature nitrogen pipe 24 is used for conveying the nitrogen reheated by the main heat exchanger 3 to the circulating compressor 1 as normal-temperature nitrogen; a first normal temperature nitrogen branch pipe 25 for conveying part of normal temperature nitrogen at the outlet of the recycle compressor 1 to the second-stage condensation evaporator 10, the pure krypton column condensation evaporator 11, the crude xenon column condensation evaporator 12 and the pure xenon column condensation evaporator 13, respectively; and a second normal temperature nitrogen branch pipe 26 for conveying part of normal temperature nitrogen at the outlet of the circulating compressor 1 to the main heat exchanger 3 for cooling and to the first condensation evaporator 9.
In the embodiment, a main heat exchanger 3, a primary rectifying tower 4, a secondary rectifying tower 5, a pure krypton tower 6, a crude xenon tower 7, a pure xenon tower 8 and connecting pipelines thereof are all placed in the same cold box to serve as a fractionating tower 2, and heat insulation materials are paved in the cold box and are ultrafine glass wool; the first-stage rectifying tower 4, the second-stage rectifying tower 5, the pure krypton tower 6, the crude xenon tower 7 and the pure xenon tower 8 are all packed towers; and valves are arranged on various pipelines, and the valves are selected from stop valves, ball valves, gate valves, angle valves and butterfly valves.
Example 2
The embodiment is a method for recycling nitrogen by using the device described in embodiment 1, and the process flow comprises the following steps:
The krypton-xenon mixture is concentrated by front-end krypton-xenon crude equipment (Kr: 92.2%, xe: 7.2%, and the rest is oxygen, nitrogen, hydrocarbon, fluoride, etc.), and then is added into a first-stage rectifying tower 4 (operating pressure 0.3 MPa-0.6 MPaG, temperature is affected by pressure and component variation, typically minus 125-minus 170 ℃) in a separating tower 2 through a pipeline or a container, after removing low-boiling components (typically mixed oxygen, nitrogen, etc.), the low-boiling components are sent into a second-stage rectifying tower 5, the operating pressure of the second-stage rectifying tower 5 is slightly lower than that of the first-stage rectifying tower 1, typically 0.25-0.5 MPaG, impurity content is reduced, and operating temperature is relatively stable, typically minus 130 ℃. The high-boiling crude xenon and the low-boiling crude krypton are separated in the second-stage rectifying column 5, wherein the crude krypton is fed into a pure krypton column 6 (operating pressure is 0.22-0.5 MPaG, operating temperature is-135 ℃), and high-boiling components (mainly fluoride) are separated in the pure krypton column 6 and discharged from the bottom of the column. Pure krypton (purity of more than 99.999% in national standard) is discharged from the top of the tower and sent to the next (filling or pipeline transportation) process.
The crude xenon gas from the bottom of the second-stage rectifying tower 5 is first introduced into a crude xenon tower 7 (operating pressure is 0.03-0.2 MPaG, operating temperature is about-100 ℃) to remove high boiling components (hydrocarbon, partial fluoride, etc.), relatively pure xenon gas is obtained from the top of the crude xenon tower 7 (operating pressure is 0.02-0.2 MPaG, operating temperature is about-100 ℃) and introduced into a pure xenon tower 8 (operating pressure is 0.02-0.2 MPaG, operating temperature is about-100 ℃). The low boiling point components are removed again in a pure xenon column 8, pure xenon (purity above 99.999% in national standard) is withdrawn from the bottom of the column and sent to the next (filling or piping) process.
The type of the rectifying tower and the internal components of the rectifying tower in the embodiment are determined by actual working conditions, and the change of the form of the rectifying tower does not influence the protection scope of the invention.
The rectification column is operated, and the gas rising from the bottom of the column and the liquid falling from the top of the column are the conditions necessary for the normal operation of the rectification column. The flow rate of the krypton-xenon refining equipment is generally small, and the ascending gas is usually obtained by heating liquid by an electric heater at the bottom of the tower. The descending liquid is obtained by condensing the gas at the top of each rectifying tower through a respective condensing evaporator.
According to the invention, the cold source of the condensation evaporator is mixed with nitrogen into low-temperature gas through liquid nitrogen, the direct mixed gas is used as the cold source of the first-stage rectifying tower 4 according to different operation temperatures of each rectifying tower, the proportion of the direct mixed gas is proportioned by the temperature and the cold required by the whole system, for example 420Nm 3/h, and the low-temperature nitrogen 630Nm 3/h at the temperature of minus 180 ℃ is obtained after the nitrogen at the temperature of minus 118 ℃ is proportioned with the liquid nitrogen at the temperature of 210Nm 3/h. The vaporized low-temperature nitrogen gas is mixed with the normal-temperature nitrogen gas from outside the fractionating tower 2 after exiting the first-stage condensing evaporator 9. According to the different operating temperatures of each rectifying tower, the low-temperature nitrogen and the normal-temperature nitrogen are mixed in different proportions, so that the temperature difference of each condensing evaporator 10, 11, 12 and 13 is ensured to be within the design range. The nitrogen coming out of the condensation evaporators 10, 11, 12 and 13 is concentrated and then is reheated to 0-20 ℃ by the main heat exchanger 3, and then is sent to the circulating compressor 1 to be pressurized to 0.4-0.8 MPa and then is sent back to the cold box for use.
The nitrogen comes out of the circulating compressor 1 and is divided into two paths, wherein one path accounts for about 60% -70%, and the nitrogen enters the condensation evaporator 9 of the primary rectifying tower 4 to be mixed with liquid nitrogen after being cooled by the main heat exchanger 3 so as to generate low-temperature nitrogen. The other path of the nitrogen enters the tower directly through the main heat exchanger 3 and is used as normal-temperature nitrogen to participate in temperature adjustment. The liquid nitrogen provides a cold source for the whole system, and meanwhile, the nitrogen with circulation loss can be supplemented. If the liquid nitrogen amount is larger than the nitrogen leakage amount, the redundant nitrogen in the system is required to be exhausted.
According to the embodiment, the mixed gas of the liquid nitrogen and the nitrogen is used as a cold source, so that the operation temperature of each condensation evaporator can be stably maintained, and the smooth proceeding of rectification is ensured; by recycling nitrogen, the consumption of liquid nitrogen or nitrogen in the krypton-xenon refining process can be greatly reduced, so that the energy consumption and the production cost are reduced. In the invention, the circulating nitrogen accounts for at least 70% of the system, and the liquid nitrogen is saved by at least 70%.
The above description of the specific embodiments of the present invention has been given by way of example only, and the present invention is not limited to the above described specific embodiments. Any equivalent modifications and substitutions for the present invention will occur to those skilled in the art, and are also within the scope of the present invention. Accordingly, equivalent changes and modifications are intended to be included within the scope of the present invention without departing from the spirit and scope thereof.

Claims (5)

1. The method for recycling nitrogen in the krypton-xenon refining process comprises a first-stage rectifying tower (4), a second-stage rectifying tower (5), a pure krypton tower (6), a crude xenon tower (7) and a pure xenon tower (8), wherein a first-stage condensation evaporator (9), a second-stage condensation evaporator (10), a pure krypton tower condensation evaporator (11), a crude xenon tower condensation evaporator (12) and a pure xenon tower condensation evaporator (13) are respectively arranged at the top of each tower, and the krypton-xenon refining process is characterized in that liquid nitrogen is adopted as a cold source, nitrogen discharged by each condensation evaporator is recycled, and the recycled nitrogen is divided into normal-temperature nitrogen and low-temperature nitrogen; wherein, the vaporized nitrogen discharged from the first-stage condensing evaporator (9) is taken as low-temperature nitrogen, and the nitrogen discharged from the second-stage condensing evaporator (10), the pure krypton tower condensing evaporator (11), the crude xenon tower condensing evaporator (12) and the pure xenon tower condensing evaporator (13) is summarized and is taken as normal-temperature nitrogen after being reheated by the main heat exchanger (3);
According to the operation temperature of each tower, the primary condensation evaporator (9) adopts liquid nitrogen mixed in a certain proportion and partial cooled normal-temperature nitrogen as cold sources, and the secondary condensation evaporator (10), the pure krypton tower condensation evaporator (11), the crude xenon tower condensation evaporator (12) and the pure xenon tower condensation evaporator (13) respectively adopt low-temperature nitrogen and normal-temperature nitrogen mixed in a corresponding proportion as cold sources;
Nitrogen discharged from the secondary condensation evaporator (10), the pure krypton tower condensation evaporator (11), the crude xenon tower condensation evaporator (12) and the pure xenon tower condensation evaporator (13) is collected and reheated by the main heat exchanger (3), and then is sent to the circulating compressor (1) for pressurization to form normal-temperature nitrogen; the normal-temperature nitrogen is separated into two paths from the circulating compressor (1), one path is cooled by the main heat exchanger (3) and then enters the first-stage condensation evaporator (9) to be mixed with liquid nitrogen to generate low-temperature nitrogen, and the other path directly enters each tower to be used as normal-temperature nitrogen to participate in temperature adjustment;
the primary rectifying tower (4), the secondary rectifying tower (5), the pure krypton tower (6), the crude xenon tower (7), the pure xenon tower (8) and the main heat exchanger (3) are all placed in the same cold box and serve as the fractionating tower (2).
2. The method for recycling nitrogen in a krypton-xenon refining process according to claim 1, wherein the krypton-xenon refining process comprises the following steps: the krypton-xenon mixture is concentrated by front-end krypton-xenon crude equipment and then is added into a first-stage rectifying tower (4) in a fractionating tower (2) through a pipeline or a container, and after removing low-boiling components, the krypton-xenon mixture is sent into a second-stage rectifying tower (5); in the secondary rectifying tower (5), the materials are separated into high-boiling crude xenon and low-boiling crude krypton;
Wherein, the crude krypton discharged from the top of the secondary rectifying tower (5) is sent to a pure krypton tower (6), in the pure krypton tower (6), high boiling components are separated and discharged from the bottom of the tower, and the pure krypton is discharged from the top of the tower to the next process;
Wherein, the crude xenon discharged from the bottom of the secondary rectifying tower (5) firstly enters the crude xenon tower (7) to remove high boiling point components, purer xenon is obtained from the top of the crude xenon tower (7) and enters the pure xenon tower (8); the low-boiling components are removed again in a pure xenon column (8), and pure xenon is drawn off from the bottom of the column and sent to the next process.
3. The method for recycling nitrogen in a krypton-xenon refining process according to claim 2, wherein the low boiling components removed in the primary rectifying column (4) are mainly oxygen and nitrogen.
4. The method of recycling nitrogen in a krypton-xenon refining process according to claim 2, wherein the next step of pure krypton and the next step of pure xenon include filling or piping.
5. The utility model provides a device of cyclic utilization nitrogen gas in krypton xenon refining process, including being used for separating and refined first order rectifying column (4), second grade rectifying column (5), pure krypton tower (6), crude xenon tower (7) and pure xenon tower (8), the top of each tower corresponds respectively sets up first order condensation evaporator (9), second grade condensation evaporator (10), pure krypton tower condensation evaporator (11), crude xenon tower condensation evaporator (12) and pure xenon tower condensation evaporator (13), characterized in that, the device still includes main heat exchanger (3), cyclic compressor (1) and main heat exchanger (3) and cyclic compressor (1) that connect gradually are connected with first order condensation evaporator (9), second grade condensation evaporator (10), pure krypton tower condensation evaporator (11), crude xenon tower condensation evaporator (12) and pure xenon tower condensation evaporator (13) are used for providing the pipeline of cold volume respectively;
the pipe includes:
A liquid nitrogen inlet pipe (21) for delivering liquid nitrogen to the primary condensing evaporator (9);
A low-temperature nitrogen pipe (22) for respectively conveying the vaporized nitrogen discharged from the first-stage condensation evaporator (9) as low-temperature nitrogen to the second-stage condensation evaporator (10), the pure krypton column condensation evaporator (11), the crude xenon column condensation evaporator (12) and the pure xenon column condensation evaporator (13);
The nitrogen outlet pipe (23) is used for collecting nitrogen discharged by the secondary condensation evaporator (10), the pure krypton tower condensation evaporator (11), the crude xenon tower condensation evaporator (12) and the pure xenon tower condensation evaporator (13) and then conveying the nitrogen to the main heat exchanger (3) for reheating;
A normal temperature nitrogen pipe (24) for conveying the nitrogen reheated by the main heat exchanger (3) to the circulating compressor (1) as normal temperature nitrogen;
A first normal-temperature nitrogen branch pipe (25) for conveying part of normal-temperature nitrogen at the outlet of the circulating compressor (1) to the secondary condensation evaporator (10), the pure krypton tower condensation evaporator (11), the crude xenon tower condensation evaporator (12) and the pure xenon tower condensation evaporator (13) respectively;
the second normal-temperature nitrogen branch pipe (26) is used for conveying part of normal-temperature nitrogen at the outlet of the circulating compressor (1) to the main heat exchanger (3) for cooling and conveying to the first-stage condensation evaporator (9);
the middle part of the first-stage rectifying tower (4) is connected with a feeding pipe, the top outlet pipe of the first-stage rectifying tower (4) is connected to the main heat exchanger (3) to recover cold energy, and the bottom outlet pipe of the first-stage rectifying tower (4) is communicated with the middle part of the second-stage rectifying tower (5); the crude krypton pipe at the top of the secondary rectifying tower (5) is communicated to the middle part of the pure krypton tower (6), the pure krypton pipe is arranged at the top of the pure krypton tower (6), and a high-boiling-point component discharge pipe is arranged at the bottom of the pure krypton tower (6); the crude xenon pipe at the bottom of the secondary rectifying tower (5) is communicated to the middle part of the crude xenon tower (7), the top of the crude xenon tower (7) is provided with a purer xenon pipe, and the bottom of the crude xenon tower (7) is provided with a high boiling point component discharge pipe; the purer xenon tube is communicated to the middle part of the pure xenon tower (8), the top of the pure xenon tower (8) is provided with a low boiling point component discharge tube, and the bottom of the pure xenon tower (8) is provided with the purer xenon tube.
CN201810050490.4A 2018-01-18 2018-01-18 Method and device for recycling nitrogen in krypton-xenon refining process Active CN108106326B (en)

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CN111023697A (en) * 2019-11-20 2020-04-17 郝文炳 Method and device for reducing liquid nitrogen usage amount in refining of krypton and xenon
CN111998610A (en) * 2020-09-17 2020-11-27 上海迎飞能源科技有限公司 Krypton-xenon refining system and method capable of reducing liquid nitrogen usage amount and simultaneously producing high-purity oxygen
CN111998611A (en) * 2020-09-17 2020-11-27 上海迎飞能源科技有限公司 Krypton-xenon refining method and system capable of producing high-purity oxygen simultaneously

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CN101723339A (en) * 2009-12-10 2010-06-09 上海启元科技发展有限公司 Rectification method for extracting krypton-xenon from liquid oxygen

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GB759853A (en) * 1952-12-19 1956-10-24 Air Reduction Improvements in the low temperature separation of air
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