CN113983760A - Helium ultra-low temperature purification and liquefaction system - Google Patents

Helium ultra-low temperature purification and liquefaction system Download PDF

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Publication number
CN113983760A
CN113983760A CN202111269006.5A CN202111269006A CN113983760A CN 113983760 A CN113983760 A CN 113983760A CN 202111269006 A CN202111269006 A CN 202111269006A CN 113983760 A CN113983760 A CN 113983760A
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China
Prior art keywords
heat exchanger
liquefaction
purification
helium
unit
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CN202111269006.5A
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Chinese (zh)
Inventor
江蓉
赖勇杰
向润清
程香
李亮
李自飞
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Sichuan Air Separation Plant Group Co ltd
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Sichuan Air Separation Plant Group 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/0002—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the fluid to be liquefied
    • F25J1/0005—Light or noble gases
    • F25J1/0007—Helium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B01D53/0407—Constructional details of adsorbing systems
    • B01D53/0438—Cooling or heating systems
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B23/00—Noble gases; Compounds thereof
    • C01B23/001—Purification or separation processes of noble gases
    • C01B23/0036—Physical processing only
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0032—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration"
    • F25J1/0035—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration" by gas expansion with extraction of work
    • F25J1/0037—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration" by gas expansion with extraction of work of a return 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0032—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration"
    • F25J1/004—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration" by flash gas recovery
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0203—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a single-component refrigerant [SCR] fluid in a closed vapor compression cycle
    • F25J1/0204—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a single-component refrigerant [SCR] fluid in a closed vapor compression cycle as a single flow SCR 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0221—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using the cold stored in an external cryogenic component in an open refrigeration loop
    • F25J1/0224—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using the cold stored in an external cryogenic component in an open refrigeration loop in combination with an internal quasi-closed refrigeration 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0228—Coupling of the liquefaction unit to other units or processes, so-called integrated processes
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0228—Coupling of the liquefaction unit to other units or processes, so-called integrated processes
    • F25J1/0235—Heat exchange integration
    • F25J1/0237—Heat exchange integration integrating refrigeration provided for liquefaction and purification/treatment of the gas to be liquefied, e.g. heavy hydrocarbon removal from natural gas
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0243—Start-up or control of the process; Details of the apparatus used; Details of the refrigerant compression system used
    • F25J1/0279—Compression of refrigerant or internal recycle fluid, e.g. kind of compressor, accumulator, suction drum etc.
    • F25J1/0281—Compression of refrigerant or internal recycle fluid, e.g. kind of compressor, accumulator, suction drum etc. characterised by the type of prime driver, e.g. hot gas expander
    • 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
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • 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
    • F25J5/00—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • 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
    • F25J2215/04—Recovery of liquid products
    • 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
    • F25J2215/30—Helium
    • 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/02—Separating impurities in general from 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
    • F25J2260/00—Coupling of processes or apparatus to other units; Integrated schemes
    • F25J2260/20—Integration in an installation for liquefying or solidifying a fluid stream
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    • 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
    • F25J2270/04—Internal refrigeration with work-producing gas expansion loop
    • F25J2270/06—Internal refrigeration with work-producing gas expansion loop with multiple gas expansion loops

Abstract

The invention relates to the technical field of chemical gas separation and liquefaction, and provides a helium ultralow-temperature purification and liquefaction system which comprises a purification unit, a liquefaction unit, a precooling unit and a cold transfer unit, wherein the liquefaction unit is communicated with the purification unit through a gas supplementing channel, and the cold transfer unit is connected between the purification unit and the liquefaction unit; the purification unit comprises a raw material helium inlet pipe, a first flow channel of a first purification heat exchanger, a low-temperature adsorber, a first flow channel of a second purification heat exchanger, an ultralow-temperature adsorber, a second flow channel of the second purification heat exchanger, a second flow channel of the first purification heat exchanger and a high-purity helium outlet pipe which are sequentially connected through a pipeline; the working temperature interval of the low-temperature adsorber is a liquid nitrogen temperature zone, and the working temperature interval of the ultralow-temperature adsorber is 25-40K. According to the invention, different impurities in the raw material helium are respectively purified in different temperature areas through two-stage adsorption of the low-temperature adsorber and the ultralow-temperature adsorber of the purification unit, so that helium switching loss in the purification process is reduced, and helium extraction rate is improved.

Description

Helium ultra-low temperature purification and liquefaction system
Technical Field
The invention relates to the technical field of chemical gas separation and liquefaction, in particular to a helium ultralow-temperature purification and liquefaction system.
Background
Helium is a rare gas, has a very small content in the earth, is not renewable, has the characteristics of stable chemical property, extremely low boiling point and the like, is widely applied to the fields of aerospace, nuclear industry high-temperature gas-cooled reactors, low-temperature superconducting research, photoelectron product production, refrigeration, semiconductors, medical treatment, leak detection, deep sea diving, high-precision welding and the like, and is an important strategic material for the development of national safety and high and new technology industries.
At present, the extraction of helium is from natural gas, air, synthesis ammonia tail gas and the like, but the content of helium in the air is only 5.24ppm, the amount of helium extracted from a large-scale air separation unit is small, and the extraction of helium is generally used as a byproduct for extracting neon in an air separation unit and has no industrial extraction value. Extraction of helium from helium-rich natural gas is currently the only method for commercial production of helium.
The helium extraction is divided into two steps of crude extraction and refined purification. The crude extraction can purify helium gas to 40-80%, and the main components are helium, nitrogen, hydrogen and trace neon. The crude helium is subjected to catalytic oxygenation dehydrogenation and drying in a refining system, and finally enters low-temperature condensation and low-temperature adsorption to remove impurities such as nitrogen, neon and the like to obtain high-purity helium. The cryogenic environment required for cryocondensation and cryoadsorption is provided by liquid nitrogen. However, neon cannot be removed by condensation in the liquid nitrogen temperature region, and neon has smaller adsorption capacity in the liquid nitrogen temperature region, so that the size of low-temperature adsorber equipment is larger, and further helium loss is more in the low-temperature adsorption switching process, especially in the high-pressure low-temperature adsorption process; in addition, the final product only contains high-purity helium, and the output product is single.
Disclosure of Invention
The invention provides a helium ultralow-temperature purification and liquefaction system aiming at overcoming the defects in the prior art, and aims to solve the problem that in the prior art, a low-temperature adsorber has a large size due to small adsorption capacity to neon in a liquid nitrogen temperature region, so that helium loss is large in a low-temperature adsorption switching process.
In order to achieve the purpose, the invention provides the following technical scheme:
a helium ultra-low temperature purification and liquefaction system comprising:
the purification unit is used for purifying helium serving as a raw material to prepare high-purity helium;
the liquefying unit is communicated with the purifying unit through a gas supplementing channel and is used for liquefying high-purity helium gas to prepare liquid helium;
the precooling unit is used for providing precooling cold energy for liquefying the high-purity helium gas; and
the cold transfer unit is connected between the purification unit and the liquefaction unit and used for transferring the cold energy of the liquefaction unit to the purification unit so as to provide the cold energy required by low-temperature adsorption;
the purification unit comprises a raw material helium gas inlet pipe, a first purification heat exchanger first flow passage, a low-temperature adsorber, a second purification heat exchanger first flow passage, an ultralow-temperature adsorber, a second purification heat exchanger second flow passage, a first purification heat exchanger second flow passage and a high-purity helium gas outlet pipe which are sequentially connected through a pipeline; the working temperature interval of the low-temperature adsorber is a liquid nitrogen temperature zone, and the working temperature interval of the ultralow-temperature adsorber is 25-40K.
In one embodiment of the disclosure, the gas supply channel comprises a gas supply pipeline and a gas supply valve installed on the gas supply pipeline, and one end of the gas supply pipeline is communicated with the high-purity helium gas outlet pipe, and the other end of the gas supply pipeline is communicated with the liquefaction unit.
In one embodiment disclosed herein, when the gas supply passage is fully closed, the entire system is operated in a purification mode to produce high purity helium gas; when the gas supplementing channel is fully opened, the whole system is operated in a liquefaction mode to prepare liquid helium.
In one embodiment of the disclosure, the liquefaction unit comprises a recycle compressor process gas flow passage, a first liquefaction heat exchanger second flow passage, a second liquefaction heat exchanger second flow passage, a third liquefaction heat exchanger second flow passage, a fourth liquefaction heat exchanger second flow passage, a fifth liquefaction heat exchanger second flow passage, a sixth liquefaction heat exchanger second flow passage, a throttle valve, a liquid helium storage tank, a pressure regulating valve, a sixth liquefaction heat exchanger first flow passage, a fifth liquefaction heat exchanger first flow passage, a fourth liquefaction heat exchanger first flow passage, a third liquefaction heat exchanger first flow passage, a second liquefaction heat exchanger first flow passage, a first liquefaction heat exchanger first flow passage, and a recycle compressor inlet which are sequentially connected through a pipeline;
and the process gas flow passage outlet of the circulating compressor is converged with the gas supplementing pipeline.
In an embodiment disclosed in the present application, the pre-cooling unit mainly consists of a third flow channel of the first liquefied heat exchanger, and a medium flowing in the flow channel is liquid nitrogen.
In one embodiment of the disclosure, the cold transfer unit includes a connecting pipeline branch port of a fifth liquefaction heat exchanger second flow channel and a sixth liquefaction heat exchanger second flow channel which are sequentially connected by a pipeline, a first regulating valve, a second purification heat exchanger third flow channel, a first purification heat exchanger third flow channel, and a connecting pipeline junction port of a first liquefaction heat exchanger first flow channel and a circulating compressor inlet.
In one embodiment disclosed herein, the system further comprises a refrigeration unit for providing refrigeration to the purification unit and/or liquefaction unit.
In one embodiment disclosed herein, the refrigeration unit includes a connection pipeline branch port of a second flow channel of the second liquefaction heat exchanger and a second flow channel of the third liquefaction heat exchanger sequentially connected by a pipeline, a second regulating valve, a first expander process gas flow channel, a third flow channel of the fourth liquefaction heat exchanger, a second expander process gas flow channel, and a connection pipeline junction port of a first flow channel of the sixth liquefaction heat exchanger and a first flow channel of the fifth liquefaction heat exchanger;
and a bypass pipeline is connected between the process gas flow passage outlet of the first expander and the process gas flow passage outlet of the second expander, and a bypass valve is installed on the bypass pipeline.
In one embodiment disclosed in the present application, the ultra-low temperature adsorber mainly comprises two parallel adsorbers, and the inlet and outlet of each adsorber are respectively provided with a switching valve;
through the mutual opening and closing of the switching valves, the two adsorbers can be switched to be used on line, and one adsorber is used for adsorption while the other adsorber is used for regeneration.
In one embodiment of the present disclosure, the first purifying heat exchanger and the second purifying heat exchanger are both stainless steel sleeve wound heat exchangers.
Compared with the prior art, the invention has the beneficial effects that:
1. different impurities in the raw material helium are respectively purified in different temperature areas through two-stage adsorption of a low-temperature adsorber and an ultra-low-temperature adsorber of a purification unit, so that helium switching loss in the purification process is reduced, and helium extraction rate is improved;
2. through the adjustment of the gas supplementing channel, the arbitrary switching of three operation modes of helium purification, helium liquefaction, helium purification and liquefaction mixing can be realized, and the problem of single product is solved;
3. through two parallelly connected adsorbers that switch over to use, can guarantee the continuity of helium purification production, improve production efficiency.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic process flow diagram of the present invention.
The reference numerals are explained below:
a11, low-temperature adsorber, A12A/A12B, adsorber;
c01, circulating compressor;
e01, a first liquefaction heat exchanger, E02, a second liquefaction heat exchanger, E03, a third liquefaction heat exchanger, E04, a fourth liquefaction heat exchanger, E05, a fifth liquefaction heat exchanger, E06, a sixth liquefaction heat exchanger, E11, a first purification heat exchanger, E12 and a second purification heat exchanger;
ET01, first expander, ET02, second expander;
SV01, liquid helium tank;
v01, an air compensating valve, V02, a throttle valve, V03, a pressure regulating valve, V04, a first regulating valve, V05, a second regulating valve, V06, a bypass valve, V11/V13/V12/V14 and a switching valve.
Detailed Description
In the following, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature, and not as restrictive.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing and simplifying the description, and are not intended to indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be considered as limiting the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, "above" or "below" a first feature means that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact with each other via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
The following disclosure provides many different embodiments or examples for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention.
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Referring to fig. 1, the present invention provides a helium ultra-low temperature purification and liquefaction system comprising:
the purification unit is used for purifying helium serving as a raw material to prepare high-purity helium;
the liquefying unit is communicated with the purifying unit through the gas supplementing channel and is used for liquefying high-purity helium gas to prepare liquid helium;
the precooling unit is used for providing precooling cold energy for liquefying the high-purity helium gas; and
the cold transfer unit is connected between the purification unit and the liquefaction unit and used for transferring the cold energy of the liquefaction unit to the purification unit so as to provide the cold energy required by low-temperature adsorption;
the purification unit comprises a raw material helium inlet pipe, a first flow channel of a first purification heat exchanger E11, a low-temperature adsorber A11, a first flow channel of a second purification heat exchanger E12, an ultralow-temperature adsorber, a second flow channel of a second purification heat exchanger E12, a second flow channel of a first purification heat exchanger E11 and a high-purity helium outlet pipe which are sequentially connected through a pipeline; the working temperature interval of the low-temperature adsorber A11 is a liquid nitrogen temperature zone, and the working temperature interval of the ultralow-temperature adsorber is 25-40K.
The air supply channel comprises an air supply pipeline and an air supply valve V01 arranged on the air supply pipeline, one end of the air supply pipeline is communicated with the high-purity helium outlet pipe, and the other end of the air supply pipeline is communicated with the liquefaction unit. When the gas supplementing channel is completely closed, the whole system operates in a purification mode to prepare high-purity helium; when the gas supplementing channel is fully opened, the whole system is operated in a liquefying mode to prepare liquid helium. Namely, the helium gas to be liquefied can be supplemented by adjusting the opening of the aeration valve V01, so that the demand proportion of the high-purity helium gas and the liquid helium gas of the product is adjusted, and different production demands are met.
The liquefaction unit comprises a circulating compressor C01 process gas flow passage, a first liquefaction heat exchanger E01 second flow passage, a second liquefaction heat exchanger E02 second flow passage, a third liquefaction heat exchanger E03 second flow passage, a fourth liquefaction heat exchanger E04 second flow passage, a fifth liquefaction heat exchanger E05 second flow passage, a sixth liquefaction heat exchanger E06 second flow passage, a throttle valve V02, a liquid helium storage tank SV01, a pressure regulating valve V03, a sixth liquefaction heat exchanger E06 first flow passage, a fifth liquefaction heat exchanger E05 first flow passage, a fourth liquefaction heat exchanger E04 first flow passage, a third liquefaction heat exchanger E03 first flow passage, a second liquefaction heat exchanger E02 first flow passage, a first liquefaction heat exchanger E01 first flow passage and a circulating compressor C01 inlet which are sequentially connected through pipelines (namely, all the devices are connected end to form a circulating passage); the outlet of the process gas flow passage of the circulating compressor C01 is merged with the gas supplementing pipeline.
The pre-cooling unit mainly comprises a third flow channel of the first liquefaction heat exchanger E01, wherein a medium flowing in the flow channel is liquid nitrogen, namely the liquid nitrogen is adopted to provide pre-cooling cold for liquefaction of high-purity helium gas.
The cold transfer unit comprises a connecting pipeline branch port of a second flow channel of the fifth liquefaction heat exchanger E05 and a second flow channel of the sixth liquefaction heat exchanger E06, a first regulating valve V04, a third flow channel of the second purification heat exchanger E12, a third flow channel of the first purification heat exchanger E11, a first flow channel of the first liquefaction heat exchanger E01 and a connecting pipeline junction port of an inlet of the circulating compressor C01, which are connected in sequence through pipelines.
Specifically, high-pressure raw material helium (with the pressure of 10-20 MPa) from a raw material helium inlet pipe is cooled to a liquid nitrogen temperature zone (about 80K) through heat exchange between a first purification heat exchanger E11 and a cold transfer unit, enters a low-temperature adsorber A11 to remove impurities such as oxygen, nitrogen, argon and the like through low-temperature adsorption, the raw material helium after impurity removal enters a second purification heat exchanger E12 and the cold transfer unit to be cooled to about 25-40K through heat exchange again, then enters an ultralow-temperature adsorber, impurities such as hydrogen and the like in the raw material helium are removed in the ultralow-temperature adsorber to obtain ultralow-temperature high-pressure high-purity helium, and the ultralow-temperature high-pressure neon high-purity helium sequentially returns to the second purification heat exchanger E12 and the first purification heat exchanger E11 to obtain high-pressure normal-temperature high-purity helium. The high-pressure normal-temperature high-purity helium is divided into two strands, one strand is used as a high-purity helium product, the other strand enters a process gas flow channel outlet of a circulating compressor C01 of a liquefaction unit through an air supplementing pipeline of an air supplementing channel and an air supplementing valve V01, heat exchange is carried out between the two strands and liquid nitrogen flowing in a pre-cooling unit in a first liquefaction heat exchanger E01, and then the two strands are cooled through a second flow channel of a second liquefaction heat exchanger E02, a second flow channel of a third liquefaction heat exchanger E03, a second flow channel of a fourth liquefaction heat exchanger E04 and a second flow channel of a fifth liquefaction heat exchanger E05 in sequence, and the two strands are divided again: a strand of low-temperature helium enters a second flow channel of a sixth liquefied heat exchanger E06, is cooled again through a throttle valve V02 and then is changed into a gas-liquid two-phase gas, and then enters a liquid helium storage tank SV01, wherein the liquid-phase low-temperature liquid helium is deposited in the liquid helium storage tank SV01, and the low-temperature low-pressure helium (flash gas) is subjected to pressure regulation through a pressure regulating valve V03 and then sequentially returns to a first flow channel of the sixth liquefied heat exchanger E06, a first flow channel of a fifth liquefied heat exchanger E05, a first flow channel of a fourth liquefied heat exchanger E04, a first flow channel of a third liquefied heat exchanger E03, a first flow channel of a second liquefied heat exchanger E02 and a first flow channel of a first liquefied heat exchanger E01 to recover cold and reheat and then enters an inlet C01 of a circulating compressor to complete circulation; and the other low-temperature helium enters a cold transfer unit, passes through a second purification heat exchanger E12 and a first purification heat exchanger E11 in sequence to provide cold energy for the purification unit, is reheated, returns to the inlet of a circulating compressor C01, and enters a liquefaction unit to realize circulation.
Research shows that at the ultralow temperature of 35K, the neon adsorption capacity of the same adsorbent is about 200-500 times that of the liquid nitrogen temperature region. Therefore, in this embodiment, the operating temperature of the ultra-low temperature adsorber is about 30K, that is, the temperature of the high-pressure raw material helium flowing out of the second purification heat exchanger E12 and entering the ultra-low temperature adsorber, thereby increasing the adsorption capacity to neon, reducing the size of the adsorber device, and simultaneously reducing the helium switching loss in the purification process, and effectively increasing the helium extraction rate.
As shown in the figure, the ultralow temperature adsorber mainly comprises two adsorbers A12A and A12B which are connected in parallel, and the inlet and the outlet of each adsorber are respectively provided with a switching valve V11/V13 and a switching valve V12/V14; through the mutual opening and closing of the switching valves, the two adsorbers can be switched to be used on line, and one adsorber is used for adsorption while the other adsorber is used for regeneration. The switching valves V11 and V12 are opened, V13 and V14 are closed, the high-pressure raw material helium of 30K is subjected to impurity removal in the ultralow-temperature adsorber A12A to obtain ultralow-temperature high-pressure high-purity helium, and the ultralow-temperature high-pressure high-purity helium returns to the second purification heat exchanger E12 and the first purification heat exchanger E11 in sequence to be reheated to obtain high-pressure normal-temperature high-purity helium; the ultra-low temperature adsorber a12B is regenerated for the next adsorption use and vice versa. Namely, the two adsorbers which are connected in parallel and switched to use can ensure the continuity of helium purification production and improve the production efficiency.
In this embodiment, the first purifying heat exchanger E11 and the second purifying heat exchanger E12 are both stainless steel sleeve wound heat exchangers. The stainless steel sleeve winding type heat exchanger has the characteristics of wide applicable temperature range, high pressure resistance and the like, and can simultaneously conduct multi-flow heat transfer.
The helium ultra-low temperature purification and liquefaction system further comprises a refrigeration unit for providing refrigeration to the purification unit and/or the liquefaction unit. Specifically, the refrigeration unit comprises a connecting pipeline branch port of a second flow channel of the second liquefaction heat exchanger E02 and a second flow channel of the third liquefaction heat exchanger E03, a second regulating valve V05, a first expander ET01 process gas flow channel, a third flow channel of the fourth liquefaction heat exchanger E04, a second expander ET02 process gas flow channel, and a connecting pipeline junction port of a first flow channel of the sixth liquefaction heat exchanger E06 and a first flow channel of the fifth liquefaction heat exchanger E05, which are connected in sequence through pipelines; and a bypass pipeline is connected between the process gas runner outlet of the first expander ET01 and the process gas runner outlet of the second expander ET02, and a bypass valve V06 is installed on the bypass pipeline. The refrigeration unit is used as a branch channel of the liquefaction unit, and when a throttle valve V02 and a pressure regulating valve V03 are closed, the refrigeration unit can form a circulating channel with a first flow channel of a fifth liquefaction heat exchanger E05, a first flow channel of a fourth liquefaction heat exchanger E04, a first flow channel of a third liquefaction heat exchanger E03, a first flow channel of a second liquefaction heat exchanger E02, a first flow channel of a first liquefaction heat exchanger E01, a process gas flow channel of a circulating compressor C01, a second flow channel of the first liquefaction heat exchanger E01 and a second flow channel of a second liquefaction heat exchanger E02, so that cold energy continuously provided is transmitted to the purification unit through the cold transfer unit for low-temperature adsorption.
According to different production requirements, the system can be switched to work in three operation modes of purification, liquefaction, purification and liquefaction at will by mutual opening and closing of the air supplementing valve V01, the throttle valve V02, the pressure regulating valve V03 and the bypass valve V06. The method comprises the following specific steps:
(1) and (3) purification mode: closing an air supplementing valve V01, a throttle valve V02 and a pressure regulating valve V03, stopping the second expansion machine ET02, opening a bypass valve V06, enabling high-pressure raw material helium to pass through a purification unit to obtain all high-pressure high-purity helium products, closing a liquefaction unit, and enabling a refrigeration unit to expand and refrigerate through a first expansion machine ET01 and transmit the expansion and refrigeration to the purification unit through a cold transmission unit to provide cold energy of low-temperature adsorption.
(2) A liquefaction mode: opening a throttle valve V02 and a pressure regulating valve V03, fully opening an air compensating valve V01, cutting off a flow path of a high-pressure high-purity helium product, operating a second expansion machine ET02, closing a bypass valve V06, enabling high-pressure raw material helium to pass through a purification unit and then enter a liquefaction unit through an air compensating valve V01, and finally completely converting the high-pressure raw material helium into product liquid helium.
(3) Purification and liquefaction mixing mode: opening a throttle valve V02 and a pressure regulating valve V03, partially opening an air compensating valve V01, operating a second expansion machine ET02, closing a bypass valve V06, and supplementing helium gas needing to be re-liquefied through an air compensating valve V01 after high-pressure raw material helium gas passes through a purification unit according to the proportion of product requirements, wherein the products are high-pressure high-purity helium gas and liquid helium gas.
In summary, compared with the purification of neon impurities in a liquid nitrogen temperature zone, the invention improves the neon adsorption capacity, reduces the size of the adsorber equipment, reduces the helium switching loss in the purification process and improves the helium extraction rate by two-stage adsorption of the low-temperature adsorber and the ultralow-temperature adsorber of the purification unit; meanwhile, through the adjustment of the gas supplementing channel, the random switching of three operation modes of helium purification, helium liquefaction, helium purification and liquefaction mixing can be realized, and the problem of single product is solved.
The above embodiments are only preferred embodiments of the present invention, and are not intended to limit the technical solutions of the present invention, so long as the technical solutions can be realized on the basis of the above embodiments without creative efforts, which should be considered to fall within the protection scope of the patent of the present invention.

Claims (10)

1. Helium ultra-low temperature purification and liquefaction system, its characterized in that includes:
the purification unit is used for purifying helium serving as a raw material to prepare high-purity helium;
the liquefying unit is communicated with the purifying unit through a gas supplementing channel and is used for liquefying high-purity helium gas to prepare liquid helium;
the precooling unit is used for providing precooling cold energy for liquefying the high-purity helium gas; and
the cold transfer unit is connected between the purification unit and the liquefaction unit and used for transferring the cold energy of the liquefaction unit to the purification unit so as to provide the cold energy required by low-temperature adsorption;
the purification unit comprises a raw material helium gas inlet pipe, a first purification heat exchanger first flow passage, a low-temperature adsorber, a second purification heat exchanger first flow passage, an ultralow-temperature adsorber, a second purification heat exchanger second flow passage, a first purification heat exchanger second flow passage and a high-purity helium gas outlet pipe which are sequentially connected through a pipeline; the working temperature interval of the low-temperature adsorber is a liquid nitrogen temperature zone, and the working temperature interval of the ultralow-temperature adsorber is 25-40K.
2. The helium ultra-low temperature purification and liquefaction system of claim 1, wherein said make-up gas channel comprises a make-up gas line and a make-up gas valve mounted on said make-up gas line, said make-up gas line having one end in communication with said high purity helium gas outlet conduit and the other end in communication with said liquefaction unit.
3. The helium ultra-low temperature purification and liquefaction system of claim 1 or 2, wherein when said gas make-up passage is fully closed, the entire system is operated in a purification mode to produce high purity helium; when the gas supplementing channel is fully opened, the whole system is operated in a liquefaction mode to prepare liquid helium.
4. The helium ultra-low temperature purification and liquefaction system of claim 2, wherein:
the liquefaction unit comprises a circulating compressor process gas flow passage, a first liquefaction heat exchanger second flow passage, a second liquefaction heat exchanger second flow passage, a third liquefaction heat exchanger second flow passage, a fourth liquefaction heat exchanger second flow passage, a fifth liquefaction heat exchanger second flow passage, a sixth liquefaction heat exchanger second flow passage, a throttle valve, a liquid helium storage tank, a pressure regulating valve, a sixth liquefaction heat exchanger first flow passage, a fifth liquefaction heat exchanger first flow passage, a fourth liquefaction heat exchanger first flow passage, a third liquefaction heat exchanger first flow passage, a second liquefaction heat exchanger first flow passage, a first liquefaction heat exchanger first flow passage and a circulating compressor inlet which are sequentially connected through pipelines;
and the process gas flow passage outlet of the circulating compressor is converged with the gas supplementing pipeline.
5. The helium ultra-low temperature purification and liquefaction system of claim 1, wherein said pre-cooling unit includes a third flow path of said first liquefaction heat exchanger, and a medium flowing in said third flow path is liquid nitrogen.
6. The helium ultra-low temperature purification and liquefaction system of claim 4 or 5, wherein said cold transfer unit comprises a connecting pipeline branch port of the fifth liquefaction heat exchanger second flow channel and the sixth liquefaction heat exchanger second flow channel connected in sequence by a pipeline, a first regulating valve, a second purification heat exchanger third flow channel, a first purification heat exchanger third flow channel, and a connecting pipeline junction port of the first liquefaction heat exchanger first flow channel and the recycle compressor inlet.
7. The helium ultra-low temperature purification and liquefaction system of claim 4, further comprising a refrigeration unit for providing refrigeration to said purification unit and/or liquefaction unit.
8. The helium ultra-low temperature purification and liquefaction system of claim 7, wherein:
the refrigeration unit comprises a connecting pipeline branch port of a second flow channel of the second liquefaction heat exchanger and a second flow channel of the third liquefaction heat exchanger which are sequentially connected through a pipeline, a second regulating valve, a first expander process gas flow channel, a third flow channel of the fourth liquefaction heat exchanger, a second expander process gas flow channel and a connecting pipeline junction port of a first flow channel of the sixth liquefaction heat exchanger and a first flow channel of the fifth liquefaction heat exchanger;
and a bypass pipeline is connected between the process gas flow passage outlet of the first expander and the process gas flow passage outlet of the second expander, and a bypass valve is installed on the bypass pipeline.
9. The helium ultra-low temperature purification and liquefaction system of claim 1, wherein:
the ultra-low temperature adsorber mainly comprises two adsorbers connected in parallel, and the inlet and the outlet of each adsorber are respectively provided with a switching valve;
through the mutual opening and closing of the switching valves, the two adsorbers can be switched to be used on line, and one adsorber is used for adsorption while the other adsorber is used for regeneration.
10. The helium ultra-low temperature purification and liquefaction system of claim 1, wherein said first purification heat exchanger and said second purification heat exchanger are both stainless steel sleeve wound heat exchangers.
CN202111269006.5A 2021-10-29 2021-10-29 Helium ultra-low temperature purification and liquefaction system Pending CN113983760A (en)

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CN116558229A (en) * 2023-04-11 2023-08-08 中国科学院理化技术研究所 Helium purifier capable of continuously working and purifying method
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