CN113280575A - Device for preparing high-purity coarse neon and helium and using method thereof - Google Patents
Device for preparing high-purity coarse neon and helium and using method thereof Download PDFInfo
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- CN113280575A CN113280575A CN202110821890.2A CN202110821890A CN113280575A CN 113280575 A CN113280575 A CN 113280575A CN 202110821890 A CN202110821890 A CN 202110821890A CN 113280575 A CN113280575 A CN 113280575A
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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
- F25J3/0228—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
- F25J3/029—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 of helium
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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
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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
- F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
- F25J3/04163—Hot end purification of the feed air
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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
- F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
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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
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/82—Processes or apparatus using other separation and/or other processing means using a reactor with combustion or catalytic reaction
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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
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/42—Nitrogen
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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
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/30—Helium
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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
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/32—Neon
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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
- F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
- F25J2230/30—Compression of the feed stream
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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
- 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
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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
- F25J2270/00—Refrigeration techniques used
- F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
- F25J2270/908—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by regenerative chillers, i.e. oscillating or dynamic systems, e.g. Stirling refrigerator, thermoelectric ("Peltier") or magnetic refrigeration
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Abstract
The device comprises a raw material film press connected with a mixer through a valve; the outlet of the mixer is connected with the catalytic reaction system; the outlet of the catalytic reaction system is connected with the drying system, the outlet at the top of the drying system is connected with the nitrogen removal system, the catalytic reaction system comprises a catalytic reactor and a water cooler, the catalytic reactor is connected with the water cooler, the drying system comprises a first gas-liquid separator and a molecular sieve adsorber, the first gas-liquid separator is connected with the molecular sieve adsorber, the molecular sieve adsorber comprises an adsorber A and an adsorber B, and the nitrogen removal system comprises a heat exchanger, a second gas-liquid separator, a GM refrigerator, a cold head heat exchanger of the GM refrigerator and a third gas-liquid separator. The invention has the characteristics of low requirement on the purity of the raw material gas, high product purity, simple equipment, energy saving, flexible operation, easy maintenance and the like.
Description
Technical Field
The invention relates to a further purification process of a high value-added byproduct rare gas by air separation, in particular to a device and a method for preparing high-purity crude neon helium.
Background
The rare gas is called as 'gold gas' because the rare gas has very low content in air and high price, and is widely applied to the fields of low temperature, electronics, aerospace, medical treatment and the like, the primary coarse neon helium gas obtained from an air separation device has the neon helium content of only about 50%, most of the rest is nitrogen and a small amount of hydrogen impurities, and in order to obtain high-purity neon and helium gas, the primary coarse neon helium gas needs to be further subjected to impurity removal and purification to obtain high-purity coarse neon-helium mixed gas (Ne + He = 100%), is used as a raw material gas for low-temperature separation of neon and helium, and is further subjected to low-temperature separation to obtain neon and helium products. At present, two manufacturers such as new and acute manufacturers have neon and helium refining technologies, related patent reports specially aiming at the extraction of high-purity coarse neon and helium (Ne + He = 100%) are not seen in China, and for the neon and helium refining technology which is not mature in China, the preparation of the high-purity coarse neon and helium makes a step toward the preparation of high-purity neon and helium.
At present, Russian deep cooling and the like adopt secondary oxygen adding and hydrogen removing, molecular sieve adsorption and water removing and condensation and nitrogen removing processes to obtain high-purity coarse neon helium, wherein a condensation and nitrogen removing module utilizes normal-pressure liquid nitrogen and negative-pressure liquid nitrogen as cold sources to carry out secondary nitrogen removal. The process is the mainstream process at present, and the process of few domestic manufacturers is similar to the mainstream process. The process adopts normal-pressure liquid nitrogen and negative-pressure liquid nitrogen as cold sources, the consumption of the liquid nitrogen is high, a vacuum pumping system is required to be configured and comprises a vacuum pumping port, a vacuum silicon tube, a corrugated tube, a screw pump and the like, the equipment is complex and is difficult to operate, the stability of the equipment is greatly reduced, and the investment cost is high. Secondly, the secondary oxygen adding dehydrogenation increases the complexity of the equipment, and the single dehydrogenation effect is poor.
Compared with the method using negative pressure liquid nitrogen as the second-stage cold source, the method provided by the invention has the advantages that the nitrogen removal temperature and the provided cold quantity are easier to control, the nitrogen removal is more efficient, and the investment cost is greatly reduced. Meanwhile, the high-efficiency one-time oxygen adding and hydrogen removing are adopted, the operation is simple, the safety is higher, and the equipment is more stable.
Disclosure of Invention
Aiming at the defects and defects in the prior art, the invention designs the device and the method for preparing the high-purity coarse neon helium with low purity requirement, high equipment efficiency and flexible operation for the raw material coarse neon helium, and the device and the method for preparing the high-purity coarse neon helium with high efficiency and low consumption by using the GM refrigerator to replace negative pressure liquid nitrogen as a cold source.
The invention is completed by the following technical scheme: the device for preparing high-purity crude neon and helium comprises a raw material film press, wherein the raw material film press is connected with a mixer through a valve; the outlet of the mixer is connected with the catalytic reaction system; the outlet of the catalytic reaction system is connected with a drying system, and the outlet at the top of the drying system is connected with a nitrogen removal system.
Preferably, the method comprises the following steps: the catalytic reaction system comprises a catalytic reactor and a water cooler, wherein the catalytic reactor is connected with the water cooler, and a palladium catalyst is filled in the catalytic reactor.
Preferably, the method comprises the following steps: the drying system comprises a first gas-liquid separator and a molecular sieve adsorber, wherein the first gas-liquid separator is connected with the molecular sieve adsorber, and the molecular sieve adsorber comprises an adsorber A and an adsorber B which can be switched to use.
Preferably, the method comprises the following steps: the nitrogen removal system comprises a heat exchanger, a second gas-liquid separator, a GM refrigerator cold head heat exchanger and a third gas-liquid separator, wherein the heat exchanger is sequentially connected with the second gas-liquid separator, the GM refrigerator cold head heat exchanger and the third gas-liquid separator.
Preferably, the method comprises the following steps: the bottom of the mixer is provided with an oxygen inlet.
Preferably, the method comprises the following steps: the bottom of the first gas-liquid separator is provided with a condensed water discharge port communicated with a drainage system, the bottoms of the second gas-liquid separator and the third gas-liquid separator are provided with liquid nitrogen discharge ports communicated with a liquid nitrogen discharge pool, and the top of the third gas-liquid separator is provided with a high-purity coarse neon-helium product outlet communicated with a filling system.
Preferably, the method comprises the following steps: the high-purity coarse neon and helium device can be integrated into a skid-mounted block, and the skid-mounted block can be fixedly mounted and can also be flexibly moved, so that the high-purity coarse neon and helium device can be used for processing coarse neon and helium at different places or can be used for centralized processing and production of dispersed coarse neon and helium.
The use method of the device for preparing high-purity crude neon and helium comprises the following steps:
(1) oxygen addition and hydrogen removal: the primary crude neon and helium gas led out from the air separation device is pressurized to 1-2MPa by a raw material membrane press, then proper excessive oxygen gas is added and fully mixed in a mixer, and then the mixture enters a catalytic reactor in a dehydrogenation module, a palladium catalyst is filled in the catalytic reactor, and hydrogen and oxygen react under the action of the catalyst palladium catalyst and at the temperature of 100 ℃;
(2) dewatering and drying: the gas is sent into a water cooler for cooling after catalytic reaction, the cooled gas is sent into a first gas-liquid separator for removing condensed water, and the gas after removing the condensed water is sent into a molecular sieve MSA or a molecular sieve MSB for switching to use for drying;
(3) nitrogen removal: and (3) precooling the dry mixed gas without hydrogen obtained in the step (2) by a heat exchanger, then feeding the dry mixed gas into a Dewar filled with liquid nitrogen, cooling the dry mixed gas by the liquid nitrogen, then feeding the cooled mixed gas into a second gas-liquid separator for gas-liquid separation, enabling the second gas-liquid separator to be soaked in normal-pressure liquid nitrogen at the temperature of 80K, liquefying most of nitrogen in the mixed gas in the second gas-liquid separator and discharging the liquefied nitrogen from the bottom of the second gas-liquid separator GS2, feeding the mixed gas led out from the top of the second gas-liquid separator into a cold-head heat exchanger of a GM refrigerator for further cooling, performing secondary nitrogen removal, feeding the cooled helium mixed gas into a third gas-liquid separator, discharging liquid nitrogen from the bottom of the third gas-liquid separator, and obtaining high-purity coarse helium neon at the top.
Compared with the known methods, the method of the invention has the following advantages:
(1) the purity requirement of raw material gas is low: the purity of raw material coarse neon, helium, neon and helium only needs to be higher than 30 percent to meet the requirement of high-purity coarse neon and helium (Ne + He is more than or equal to 99 percent);
(2) the product purity is high: the normal pressure liquid nitrogen and the GM cryocooler are adopted for secondary nitrogen removal, the nitrogen removal efficiency is high, and the purity of the high-purity coarse neon and helium product is as high as more than 99 percent;
(3) simple equipment and energy saving: firstly, a high-efficiency catalyst is used, and a first-stage oxygenation dehydrogenation process is adopted to achieve a high-efficiency dehydrogenation effect, so that the process reduces equipment investment and saves cost compared with a second-stage oxygenation dehydrogenation process adopted in Russian deep cooling and the like; secondly, a vacuum pumping system is not needed, so that the process flow is simplified, the operation is simple, the equipment stability is improved, and the investment cost is greatly reduced. Negative pressure liquid nitrogen is not needed, so that the consumption of liquid nitrogen is greatly reduced, and the energy consumption is reduced; and fourthly, secondary nitrogen removal adopts a GM refrigerator as a cold source. The small GM low-temperature refrigerator is used for providing a cold source, the refrigerating temperature is 65K, nitrogen is condensed at low temperature, the process and the equipment are simple, and the operation is safe and reliable. Compared with the use of negative pressure liquid nitrogen, the refrigeration temperature of the GM refrigerator and the provided cold quantity are easier to control, the nitrogen removal is more efficient, and the investment cost is greatly reduced. The GM refrigerator has the advantages of low temperature, long service life, small volume, small vibration and the like, is a low-temperature refrigerator widely applied in the world at present, and is a novel method with high efficiency and energy saving by adopting the GM refrigerator, and is also a great innovation point;
(4) the operation is flexible: different from the prior art, the crude neon helium gas cooled by the normal-pressure liquid nitrogen does not need negative-pressure liquid nitrogen but is cooled by a cold head heat exchanger of the GM refrigerator, the cooling temperature can be properly adjusted according to the nitrogen content in the crude neon helium gas, and the flexibility of system operation is improved.
(5) Easy maintenance: all parts of the system working in a low-temperature environment, such as a low-temperature valve, a heat exchanger, a low-temperature pipeline connection, a temperature and pressure measuring device, a GM refrigerator and the like, are integrated in the Dewar, and meanwhile, all the unit equipment are hung on a large flange of a top cover of the Dewar, so that the integration level is very high. For example, when a GM refrigerator or a low-temperature valve has a fault such as leakage, the refrigerator can be independently drawn out from the Dewar top cover without opening the Dewar top cover, and the production can be recovered in a short time after the maintenance of the equipment.
Drawings
FIG. 1 is a flow chart of the process for producing high purity crude neon helium in accordance with the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings in which: as shown in fig. 1, an apparatus for producing high-purity crude neon helium comprises a raw material film press connected to a mixer through a valve; the outlet of the mixer is connected with the catalytic reaction system; the outlet of the catalytic reaction system is connected with a drying system, the outlet at the top of the drying system is connected with a nitrogen removal system, the catalytic reaction system comprises a catalytic reactor and a water cooler, the catalytic reactor is connected with the water cooler, a palladium catalyst is filled in the catalytic reactor, the drying system comprises a first gas-liquid separator GS1 and a molecular sieve adsorber MS, the first gas-liquid separator GS1 is connected with the molecular sieve adsorber, the molecular sieve adsorber MS comprises an adsorber A and an adsorber B which can be switched for use, the nitrogen removal system comprises a heat exchanger E1, a second gas-liquid separator GS2, a GM refrigerator cold head heat exchanger E2 and a third gas-liquid separator GS3, wherein the heat exchanger E1 is sequentially connected with the second gas-liquid separator GS2, the GM refrigerator cold head heat exchanger E2 and the third gas-liquid separator GS3, the bottom of the mixer M1 is provided with an oxygen inlet, the bottom of the first gas-liquid separator GS1 is provided with a condensed water discharge port which is communicated with a drainage system, the bottoms of the second gas-liquid separator GS2 and the third gas-liquid separator GS3 are provided with liquid nitrogen discharge ports which are communicated with a liquid nitrogen discharge pool, the top of the third gas-liquid separator GS3 is provided with a high-purity crude neon helium product outlet which is communicated with a filling system, the high-purity crude neon helium device can be integrated into a skid-mounted block, and the skid-mounted block can be fixedly mounted and can also be flexibly moved so as to process crude neon at different places or intensively process and produce dispersed crude neon helium.
The use method of the device for preparing high-purity crude neon and helium comprises the following steps:
(1) oxygen addition and hydrogen removal: the primary crude neon and helium gas led out from the air separation device is pressurized to 1-2MPa by a raw material membrane press C1, then added with proper excess oxygen gas and fully mixed in a mixer M1, and then enters a catalytic reactor DF1 in a dehydrogenation module, wherein a palladium catalyst is filled in the catalytic reactor DF1, and hydrogen and oxygen react under the action of the catalyst palladium catalyst and at the temperature of 100 ℃;
(2) dewatering and drying: the gas is sent into a water cooler WE1 for cooling after catalytic reaction, the cooled gas is sent into a first gas-liquid separator GS1 for removing condensed water, and the gas after removing the condensed water is sent into a molecular sieve MSA or MSB for drying by switching;
(3) nitrogen removal: and (3) precooling the dry mixed gas without hydrogen obtained in the step (2) by a heat exchanger E1, then feeding the dry mixed gas into a Dewar filled with liquid nitrogen, cooling the dry mixed gas by the liquid nitrogen, then feeding the cooled dry mixed gas into a second gas-liquid separator GS2 for gas-liquid separation, soaking the second gas-liquid separators GS2 and GS3 in normal-pressure liquid nitrogen at the temperature of 80K, liquefying most of nitrogen in the mixed gas in the second gas-liquid separator GS2, discharging the liquefied gas from the bottom of the second gas-liquid separator GS2, further cooling the mixed gas led out from the top of the second gas-liquid separator GS2 by a cold-head heat exchanger E2 of a GM refrigerator, performing secondary nitrogen removal, feeding the cooled neon mixed helium gas into a third gas-liquid separator GS3, discharging liquid nitrogen from the bottom of the third gas-liquid separator GS3, and obtaining high-purity crude helium neon at the top.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
At 10Nm3The production of/h primary crude neon helium is exemplified. 10Nm3The raw material of crude neon helium contains Ne35%, helium 13%, hydrogen 4% and nitrogen about 48%. Pressurizing to 1-2MPa by a raw material membrane press C1, feeding into a mixer M1, fully mixing oxygen from a pipe network with raw material crude neon and helium in a mixer M1, feeding into a catalytic reactor DF1 in a dehydrogenation module, wherein a palladium catalyst is filled in the catalytic reactor DF1Under the action of a catalyst palladium catalyst, the catalytic temperature is about 100 ℃, hydrogen and oxygen react and are sent to a water cooler WE1 to be cooled to the normal temperature, then the hydrogen and oxygen are sent to a first gas-liquid separator GS1 to remove condensed water, the gas after the condensed water is removed is sent to a molecular sieve MSA or a molecular sieve MSB which is used by switching to be dried, and at the moment, impurity hydrogen is removed.
The dried mixed gas after dehydrogenation is pre-cooled to-130 ℃ by cold nitrogen gas through a heat exchanger E1, enters Dewar DW filled with liquid nitrogen, is cooled to-192 ℃ through a liquid nitrogen bath, enters a second gas-liquid separator GS2 for gas-liquid separation, and is soaked in normal-pressure liquid nitrogen at the temperature of-193 ℃. Most of nitrogen in the mixed gas is liquefied in a second gas-liquid separator GS2 and is discharged from the bottom of the second gas-liquid separator GS2, the mixed gas led out from the top of the second gas-liquid separator GS2 enters a cold head heat exchanger E2 of a GM refrigerator to be further cooled, secondary nitrogen removal is carried out, the refrigeration temperature of GM is 65K, the cooled neon-helium mixed gas enters a gas-liquid separator GS3, liquid nitrogen at the bottom of the gas-liquid separator GS3 is discharged, and 4.8Nm is obtained at the top3The purity of the crude neon helium gas is more than or equal to 99 percent.
The high-purity coarse neon and helium device can be integrated into a skid-mounted block, and the skid-mounted block can be fixedly mounted and can also be flexibly moved, so that the device can be used for processing coarse neon and helium at different places or can be used for centralized processing and production of scattered coarse neon and helium.
Claims (8)
1. The device for preparing high-purity crude neon and helium is characterized by comprising a raw material film press, wherein the raw material film press is connected with a mixer through a valve; the outlet of the mixer is connected with the catalytic reaction system; the outlet of the catalytic reaction system is connected with a drying system, and the outlet at the top of the drying system is connected with a nitrogen removal system.
2. The apparatus for producing high purity crude neon and helium as claimed in claim 1, wherein said catalytic reaction system comprises a catalytic reactor and a water cooler, wherein said catalytic reactor is connected to said water cooler and is filled with a palladium catalyst.
3. The apparatus of claim 1, wherein said drying system comprises a first gas-liquid separator and a molecular sieve adsorber, said first gas-liquid separator being connected to said molecular sieve adsorber, said molecular sieve adsorber comprising adsorber a and adsorber B, two of which are switchable.
4. The apparatus for producing high purity crude neon helium according to claim 1, wherein said nitrogen removal system comprises a heat exchanger, a second gas-liquid separator, a GM refrigerator, a cold head heat exchanger of the GM refrigerator, and a third gas-liquid separator, wherein said heat exchanger is connected to said second gas-liquid separator, said cold head heat exchanger of the GM refrigerator, and said third gas-liquid separator in this order.
5. The apparatus for producing high purity crude neon helium as claimed in claim 1, wherein said mixer is provided with an oxygen inlet at the bottom thereof.
6. The apparatus for producing high purity crude neon helium as claimed in claim 3, wherein said first gas-liquid separator is provided at the bottom thereof with a condensed water discharge port in communication with a water discharge system, said second gas-liquid separator and said third gas-liquid separator are provided at the bottom thereof with a liquid nitrogen discharge port in communication with a liquid nitrogen discharge tank, and said third gas-liquid separator is provided at the top thereof with a high purity crude neon helium product outlet in communication with a charging system.
7. An apparatus for producing high purity crude neon helium as claimed in claim 1 wherein said high purity crude neon helium means is integrated into a skid which is either fixedly mounted or flexibly movable to handle crude neon helium at different locations or to concentrate the production of dispersed crude neon helium.
8. The use method of the device for preparing high-purity crude neon and helium is characterized by comprising the following steps:
oxygen addition and hydrogen removal: the primary crude neon and helium gas led out from the air separation device is pressurized to 1-2MPa by a raw material membrane press, then proper excessive oxygen gas is added and fully mixed in a mixer, and then the mixture enters a catalytic reactor in a dehydrogenation module, a palladium catalyst is filled in the catalytic reactor, and hydrogen and oxygen react under the action of the catalyst palladium catalyst and at the temperature of 100 ℃;
dewatering and drying: the gas is sent into a water cooler WE1 for cooling after catalytic reaction, the cooled gas is sent into a first gas-liquid separator for removing condensed water, and the gas after the condensed water removal is sent into a molecular sieve MSA or a molecular sieve MSB for switching use for drying;
nitrogen removal: and (3) precooling the dry mixed gas without hydrogen obtained in the step (2) by a heat exchanger, then feeding the dry mixed gas into a Dewar filled with liquid nitrogen, cooling the dry mixed gas by the liquid nitrogen, then feeding the cooled mixed gas into a second gas-liquid separator for gas-liquid separation, soaking the second gas-liquid separator and a third gas-liquid separator in normal-pressure liquid nitrogen at the temperature of 80K, liquefying most of nitrogen in the mixed gas in the second gas-liquid separator and discharging the liquefied nitrogen from the bottom of the second gas-liquid separator, feeding the mixed gas led out from the top of the second gas-liquid separator into a cold head heat exchanger of a GM refrigerator for further cooling, performing secondary nitrogen removal, feeding the cooled neon-helium mixed gas into a third gas-liquid separator, discharging liquid nitrogen from the bottom of the third gas-liquid separator, and obtaining high-purity crude helium-neon at the top.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09217982A (en) * | 1996-02-09 | 1997-08-19 | Nippon Sanso Kk | Method for liquefying and separating air and apparatus therefor |
| JPH10325674A (en) * | 1997-05-28 | 1998-12-08 | Nippon Air Rikiide Kk | Air liquefying and separating device |
| CN205575646U (en) * | 2016-05-10 | 2016-09-14 | 河北钢铁股份有限公司邯郸分公司 | System for guarantee gaseous purification in succession of helium -neon |
| CN105987580A (en) * | 2016-02-03 | 2016-10-05 | 安徽万瑞冷电科技有限公司 | Neon and helium rare gas separating and refining process method with refrigerator as cold source |
| CN107024075A (en) * | 2016-02-01 | 2017-08-08 | 浙江新锐空分设备有限公司 | The cryogenic separation extraction system and method for a kind of pure neon |
| US20180335255A1 (en) * | 2017-05-22 | 2018-11-22 | L'air Liquide, Societe Anonyme Pour I'etude Et I'exploitation Des Procedes Georges Claude | Device and method for purifying a gas mixture |
| CN113086956A (en) * | 2021-04-15 | 2021-07-09 | 衢州杭氧特种气体有限公司 | Neon purification process and purification equipment thereof |
-
2021
- 2021-07-21 CN CN202110821890.2A patent/CN113280575A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09217982A (en) * | 1996-02-09 | 1997-08-19 | Nippon Sanso Kk | Method for liquefying and separating air and apparatus therefor |
| JPH10325674A (en) * | 1997-05-28 | 1998-12-08 | Nippon Air Rikiide Kk | Air liquefying and separating device |
| CN107024075A (en) * | 2016-02-01 | 2017-08-08 | 浙江新锐空分设备有限公司 | The cryogenic separation extraction system and method for a kind of pure neon |
| CN105987580A (en) * | 2016-02-03 | 2016-10-05 | 安徽万瑞冷电科技有限公司 | Neon and helium rare gas separating and refining process method with refrigerator as cold source |
| CN205575646U (en) * | 2016-05-10 | 2016-09-14 | 河北钢铁股份有限公司邯郸分公司 | System for guarantee gaseous purification in succession of helium -neon |
| US20180335255A1 (en) * | 2017-05-22 | 2018-11-22 | L'air Liquide, Societe Anonyme Pour I'etude Et I'exploitation Des Procedes Georges Claude | Device and method for purifying a gas mixture |
| CN113086956A (en) * | 2021-04-15 | 2021-07-09 | 衢州杭氧特种气体有限公司 | Neon purification process and purification equipment thereof |
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Application publication date: 20210820 |