CN107606874B - Device for recycling argon through full rectification purification and argon recycling method thereof - Google Patents
Device for recycling argon through full rectification purification and argon recycling method thereof Download PDFInfo
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- CN107606874B CN107606874B CN201711014301.XA CN201711014301A CN107606874B CN 107606874 B CN107606874 B CN 107606874B CN 201711014301 A CN201711014301 A CN 201711014301A CN 107606874 B CN107606874 B CN 107606874B
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Abstract
The invention relates to a device for purifying, purifying and recycling argon through full rectification, which comprises a crude argon purifying and recycling system and an argon circulating system, wherein the crude argon purifying and recycling system comprises a raw material air compressor unit, a main heat exchanger, a deoxidizing tower, a refined argon tower and a subcooler, and the argon circulating system comprises a circulating air compressor unit and an expander which are connected through corresponding pipelines; the argon circulation system provides cold for the cold box at low temperature without argon liquefaction; the invention also relates to a method for recycling argon by adopting the device, which comprises the steps of pressurizing and cooling crude argon and rectifying and purifying the crude argon, wherein the oxygen content in the prepared high liquid nitrogen is less than 1.5ppm, and the nitrogen content is less than 4ppm. According to the invention, the cooling capacity is provided by the circulating machine, and the argon is liquefied while being purified, so that the defect of air separation matched with coal chemical industry is overcome; and through reasonable configuration heat exchange flow, energy utilization is optimized, loss of cold energy is reduced, argon is recovered to the greatest extent, waste is reduced, and certain economic benefit is achieved.
Description
Technical Field
The invention relates to the technical field of gas separation, in particular to a device for recycling argon through full rectification purification and a method for recycling argon through the device.
Background
Argon is a colorless odorless inert gas with a molecular formula of Ar, a molecular weight of 39.95, a vapor pressure of 202.64kPa (-179 ℃), a melting point of-189.2 ℃ and a boiling point of-185.7 ℃. In industrial production, argon is generally used as a high-efficiency shielding gas, and is widely used.
The main source of argon is produced as a by-product from large air separation. Pure argon is generally generated in the air separation matched with the steel plant. However, in the air separation equipment used in the coal chemical process, because argon is not required in the coal chemical process, pure argon is not generally produced by the matched air separation, the air separation can be matched with a synergistic tower, crude argon from the top of the synergistic tower generally contains 85% of argon, the rest is oxygen, and the rest is nitrogen, and other impurities are not contained. This part of crude argon is directly vented, resulting in waste.
Disclosure of Invention
The invention aims at overcoming the defects in the prior art, aiming at the matched air separation characteristic of coal chemical industry, the invention develops a method for purifying crude argon by using low-temperature full rectification to obtain pure argon, namely pure liquid argon, and particularly provides a device for purifying and recycling argon by full rectification and a method for recycling argon, so as to reduce waste.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a first object of the present invention is to provide an apparatus for purifying and recovering argon by total rectification, comprising: the crude argon purification and recovery system comprises a raw gas compressor unit, a main heat exchanger, a deoxidizing tower, a refined argon tower and a subcooler which are connected through pipelines, wherein the main heat exchanger, the deoxidizing tower, the refined argon tower and the subcooler are all arranged in a cold box, the deoxidizing tower comprises a deoxidizing tower reboiler arranged at the bottom of the deoxidizing tower and a deoxidizing tower condensation evaporator arranged at the top of the deoxidizing tower, and the refined argon tower comprises a refined argon tower reboiler arranged at the bottom of the refined argon tower and a refined argon tower condensation evaporator arranged at the top of the refined argon tower; the argon gas circulation system comprises a circulating gas compressor unit and an expander which are connected through pipelines, and the circulating gas compressor unit and the expander are respectively connected with corresponding equipment in the crude argon gas purification and recovery system through corresponding pipelines.
In order to further optimize the device, the technical measures adopted by the invention further comprise:
further, the raw gas compressor unit comprises a raw gas compressor and a raw gas compressor aftercooler which are connected through pipelines in sequence, the circulating gas compressor unit comprises a circulating gas compressor and a circulating gas compressor aftercooler which are connected through pipelines in sequence, and the expander comprises an expander pressurizing end, a pressurizing aftercooler and an expander expanding end which are connected through pipelines in sequence; wherein the expansion end of the expander is arranged in the cold box.
Further, the deoxidizing tower reboiler, deoxidizing tower condensing evaporator, refined argon tower reboiler and refined argon tower condensing evaporator are immersed heat exchangers.
Further, the deoxidizing tower and the refined argon tower adopt a regular packing structure, a random packing structure or a sieve plate tower structure.
Further, the connecting pipeline of each device in the crude argon purification and recovery system comprises:
a feeding pipe for feeding the crude argon to the middle upper part of the deoxidizing tower sequentially through a raw gas compressor unit and a main heat exchanger;
a deoxidized crude argon pipe for sending deoxidized crude argon from the top of the deoxidizing tower to the middle of the refined argon tower, and a liquid argon pipe for sending high-purity liquid argon from the bottom of the refined argon tower;
a deoxidizing crude argon branch pipe for conveying part of deoxidizing crude argon from the deoxidizing crude argon pipe to a deoxidizing tower condensing evaporator and a deoxidizing crude argon condensate return pipe for conveying deoxidizing crude argon condensate back to the top of the deoxidizing tower;
the nitrogen pipe is used for sending nitrogen out of the top of the refined argon tower and recovering cold energy through the main heat exchanger for discharging, the nitrogen branch pipe is used for sending part of nitrogen from the nitrogen pipe to the refined argon tower condensation evaporator, and the nitrogen condensate return pipe is used for sending nitrogen condensate back to the top of the refined argon tower.
And the mixed gas pipe is used for sending the mixed gas of the nitrogen and the oxygen out of the lower part of the denitrification tower, recovering cold energy through the main heat exchanger and then discharging the cold energy, and the oxygen-containing liquid pipe is used for discharging the oxygen-containing liquid from the bottom of the deoxidizing tower.
Further, the connecting pipeline between each device in the argon circulation system and each device in the crude argon purification recovery system comprises:
the mixed argon circulating gas discharged from the tops of the deoxidizing tower condensing evaporator and the refined argon tower condensing evaporator is sent to a circulating gas pipe of a circulating gas compressor unit after cold energy is recovered by a subcooler and a main heat exchanger;
a recycle gas return line for delivering recycle gas from the recycle gas compressor train to the main heat exchanger;
a first recycle gas return line for delivering a portion of the recycle gas from the main heat exchanger to the deoxygenation column reboiler and a first recycle gas condensate return line for returning a portion of the recycle gas condensate to the deoxygenation column condensation evaporator;
a second recycle gas return line for delivering a portion of the recycle gas from the main heat exchanger to the refined argon column reboiler and a second recycle gas condensate return line for returning a portion of the recycle gas condensate to the refined argon column condensate evaporator.
Further, a circulating gas return branch pipe is arranged on the circulating gas return pipe, and the circulating gas return branch pipe is used for sending part of circulating gas back through a booster end of the expander, a booster aftercooler, a main heat exchanger and an expansion end of the expander in sequence and combining the circulating gas with a circulating gas pipe at an outlet of the subcooler; further, the circulating gas led out from the middle part of the main heat exchanger is communicated to the expansion end of the expander.
Further, a first circulating gas condensate return branch pipe connected to the condensing evaporator of the refined argon tower is arranged on the first circulating gas condensate return pipe.
Further, regulating valves are arranged on a feeding pipe at the outlet of the main heat exchanger, a deoxidized crude argon pipe, a first circulating gas condensate return pipe, a second circulating gas condensate return pipe and a first circulating gas condensate return branch pipe.
Further, the device also comprises a liquid nitrogen storage tank for storing high-purity liquid nitrogen.
The second object of the invention is to provide a method for purifying and recovering argon by full rectification by adopting the device, which comprises the following steps:
step 1) pressurizing and cooling crude argon: the crude argon containing oxygen and hydrogen enters a raw material air compressor unit for pressurization and preliminary cooling, and is further cooled to the liquefaction temperature through a main heat exchanger;
step 2) rectification and purification of crude argon: the crude argon at the liquefaction temperature enters the middle lower part of the deoxidizing tower for rectification separation, deoxidized crude argon is obtained at the top of the deoxidizing tower, and oxygen-containing liquid is discharged at the bottom of the deoxidizing tower; the deoxidized crude argon is discharged from the top of the deoxidizing tower and enters the middle part of the refined argon tower for rectification separation, high-purity liquid argon is obtained at the bottom of the refined argon tower, and nitrogen is discharged from the top of the refined argon tower;
the main heat exchanger, the deoxidizing tower and the refined argon tower are all arranged in the cold box, and the argon circulation system provides low temperature for the cold box and cold energy for argon liquefaction.
In order to further optimize the above method, the technical measures of the invention include:
further, the composition (volume content) of the crude argon gas is Ar: 82-87%; o (O) 2 ：12～18％；N 2 :0.01 to 0.03%, and further, the composition (volume content) of the crude argon is Ar:85%; o (O) 2 ：14.98％；N 2 ：0.02％。
Further, the pressure of the crude argon at the outlet of the raw material gas compressor unit is 0.6MPaA, and the temperature is 40 ℃.
Further, in said step 2), in the rectification separation of the deoxidizing column, a deoxidizing column reboiler at the bottom of the deoxidizing column supplies a gas required for the rectification of the deoxidizing column, and a deoxidizing column condensation evaporator at the top of the deoxidizing column supplies a liquid required for the rectification of the deoxidizing column; in the rectification separation of the refined argon tower, a refined argon tower reboiler at the bottom of the refined argon tower provides gas required by the rectification of the refined argon tower, and a refined argon tower condensation evaporator at the top of the refined argon tower provides liquid required by the rectification of the refined argon tower;
the heat sources of the deoxidization tower reboiler and the refined argon tower reboiler are circulating argon from an argon circulating system, the cold sources are respectively liquid at the bottom of the deoxidization tower and liquid at the bottom of the refined argon tower, and in the heat exchange process, the circulating argon is liquefied into liquid, and the liquid at the bottom of the tower is vaporized to generate gas;
the heat sources of the deoxidization tower condensation evaporator and the refined argon tower condensation evaporator are deoxidization crude argon and nitrogen respectively, the cold sources are liquid argon, the deoxidization crude argon and the nitrogen are respectively condensed into liquid in the heat exchange process, the liquid argon is vaporized to generate gas, and the vaporized gas from the deoxidization tower condensation evaporator and the refined argon tower condensation evaporator is mixed and sent into an argon circulation system.
Further, the operation steps of the nitrogen circulation system include:
after the circulating gas from the cold box is compressed and cooled by the circulating compressor unit, the circulating gas is divided into two parts:
part of the refrigerant enters the booster end of the expander to be boosted, is cooled by the cooler after being boosted, enters the main heat exchanger, is pumped out from the middle part of the main heat exchanger, enters the expansion end of the expander to be expanded, is cooled and depressurized, and enters the main heat exchanger to be reheated and returned to the circulating compressor;
the other part enters the main heat exchanger and is divided into two parts after being cooled by the circulating gas flowing back: part of the liquid enters a deoxidizing tower reboiler to be used as a heat source, releases heat through phase change, and vaporizes the liquid at the bottom of the deoxidizing tower to be liquefied into liquid; the other part of the liquid enters a reboiler of the refined argon tower to be used as a heat source, the heat is released through phase change, the liquid at the bottom of the vaporized refined argon tower is liquefied into liquid; liquid discharged from the reboiler of the deoxidizing tower and the reboiler of the refined argon tower are throttled and then respectively enter the condensing evaporator of the deoxidizing tower and the condensing evaporator of the refined argon tower, and then the deoxidized crude argon and nitrogen are respectively cooled to respectively provide rectification liquid for the deoxidizing tower and the refined argon tower;
the liquid argon in the deoxidization tower condensation evaporator and the refined argon tower condensation evaporator are respectively vaporized to generate gas, the gas is mixed and then exchanges heat with the non-throttled liquefied liquid respectively discharged by the deoxidization tower reboiler and the refined argon tower reboiler in the subcooler, the gas from the subcooler and the gas expanded by the expansion end of the expander are mixed into circulating gas, the circulating gas is reheated by the main heat exchanger and discharged out of the cold box, and the circulating gas enters the circulating compressor unit for pressurization and circulation.
Further, the pressure of the circulating gas at the outlet of the circulating compressor unit is 1MPaA, and the temperature is 40 ℃.
Further, the temperature of part of the circulating gas at the outlet of the post-pressurizing cooler is 40 ℃, part of the circulating gas at the outlet of the post-pressurizing cooler enters the main heat exchanger and is pumped out from the middle part of the main heat exchanger at about-90 ℃ to the expansion end of the expander to be expanded to 0.12MPaA.
Further, step 2) is followed by step 3) of recovering crude argon: high-purity liquid argon is conveyed to a liquid argon storage tank for storage and recovery; still further, the step 3) is followed by pumping the high purity liquid nitrogen from the liquid argon storage tank to a deoxidizing column condensing evaporator and a refined argon column condensing evaporator, respectively.
Further, the oxygen content in the deoxidized crude argon is less than 1.5ppm; the oxygen content in the high-purity liquid argon is less than 1.5ppm, and the nitrogen content is less than 4ppm.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the cooling capacity is provided by the circulating machine, and the argon is liquefied while being purified, so that the defect of air separation matched with coal chemical industry is overcome; according to the invention, through reasonable configuration of the heat exchange flow, the energy utilization is optimized, the loss of cold energy is reduced, argon is recovered to the greatest extent, the waste is reduced, and the method has certain economic benefit.
Drawings
FIG. 1 is a schematic flow diagram of an apparatus for purifying and recovering argon by total rectification in accordance with one embodiment of the present invention;
reference numerals in the drawings are as follows:
the raw gas compressor unit 11, the raw gas compressor 111, the raw gas compressor aftercooler 112, the main heat exchanger 12, the deoxidizing column 13, the deoxidizing column reboiler 131, the deoxidizing column condensing evaporator 132, the refined argon column 14, the refined argon column reboiler 141, the refined argon column condensing evaporator 142, the subcooler 15, the circulating gas compressor unit 21, the circulating gas compressor 211, the circulating gas compressor aftercooler 212, the expander 22, the expander booster end 221, the booster aftercooler 222, and the expander expansion end 223;
the device comprises a feed pipe L1, a deoxidizing crude argon pipe L2, a deoxidizing crude argon branch pipe L21, a deoxidizing crude argon condensate return pipe L22, a liquid argon pipe L3, a nitrogen pipe L4, a nitrogen branch pipe L41, a nitrogen condensate return pipe L42, a mixed gas pipe L5, an oxygen-containing liquid pipe L6, a circulating gas pipe L7, a circulating gas return pipe L8, a first circulating gas return pipe L81, a first circulating gas condensate return pipe L82, a second circulating gas return pipe L83, a second circulating gas condensate return pipe L84, a circulating gas return branch pipe L85, a first circulating gas condensate return branch pipe L86 and regulating valves V1-V5.
Detailed Description
The invention provides a device for recycling argon through full rectification purification, which comprises: the crude argon purification and recovery system comprises a raw gas compressor unit, a main heat exchanger, a deoxidizing tower, a refined argon tower and a subcooler which are connected through pipelines; the argon circulation system comprises a circulating gas compressor unit and an expander which are connected through pipelines, wherein the circulating gas compressor unit and the expander are respectively connected with corresponding equipment in the crude argon purification and recovery system through corresponding pipelines; the invention also relates to a method for recycling argon by the device.
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
As shown in figure 1, the top of the synergistic tower comes out from the matched air separation of the coal chemical industry processCrude argon (containing Ar:85 mol%, O) 2 ：～14.98％；N 2 : 0.02%) is compressed to 0.6MPaA by a feed gas compressor 111 through a feed pipe L1, cooled to 40 ℃ by a feed gas compressor cooler 112, enters a main heat exchanger 12 in a cold box 1, cooled to liquefaction temperature therein, throttled by a regulating valve V1 and enters the middle lower part of a deoxidizing tower 13. In the deoxidizing tower 13, a deoxidizing tower reboiler 131 at the bottom thereof supplies a gas required for rectification of the deoxidizing tower 13, and a deoxidizing tower condensation evaporator 132 at the top thereof supplies a liquid required for rectification of the deoxidizing tower 13. The crude argon gas is mixed with the gas supplied from the deoxidizer reboiler 131 as an ascending gas, and the liquid supplied from the deoxidizer condenser evaporator 132 as a descending liquid, both of which are rectified in the deoxidizer. The oxygen component is separated into the liquid at the bottom of the column and discharged through an oxygen-containing liquid pipe L6. Obtaining oxygen content from the top of the deoxidizing tower 13<1.5ppm of deoxidized crude argon passes through a deoxidized crude argon pipe L2 and enters the middle part of the refined argon tower 14 after being controlled by a regulating valve V2. In order to maintain the separation efficiency in the deoxidizing column 13, the mixed gas of oxygen and argon at the bottom of the deoxidizing column is discharged after cold is recovered by the main heat exchanger 12 through the gas mixing pipe L5.
The rectification condition of the refined argon column 14 is also established by providing liquid through a refined argon column condensing evaporator 142 at the top of the column and providing gas through a refined argon column reboiler 141 at the bottom of the column. The deoxidized crude argon gas is mixed with the gas supplied from the reboiler 141 of the refined argon column as an ascending gas, and the liquid supplied from the condensing evaporator 142 of the refined argon column as a descending liquid, and both are rectified in the refined argon column. Mainly removed in the refined argon column 14 is a component with nitrogen component and the like having a boiling point lower than that of argon, high-purity liquid argon (containing 1.5ppm of oxygen and 4ppm of nitrogen) meeting the requirements is obtained at the bottom of the refined argon column 14, is pumped out through a high-purity liquid nitrogen pipe L3 and sent out of a cold box to be stored in a liquid argon storage tank, and the liquid argon in the liquid argon storage tank can be pumped to a deoxidizing column condensing evaporator 132 and a refined argon column condensing evaporator 142 to be used as cold sources.
The cold energy required for low temperature and argon liquefaction in the cold box 1 is mainly provided by an argon circulation system. The argon gas from the cold box 1 is compressed to 1MPaA by a circulating compressor 211, cooled to 40 ℃ by a circulating compressor cooler 212, then divided into two parts, one part enters an expander pressurizing end 221 of an expander 22 through a circulating gas return branch pipe L85, is pressurized and then cooled to 40 ℃ by a post-pressurizing cooler 222, enters a main heat exchanger 12 in the cold box 1, is pumped out from the middle part (about-90 ℃) of the main heat exchanger 12 to an expander expansion end 223 of the expander 21 to be expanded to 0.12MPaA, and enters the main heat exchanger 12 for reheating and recycling to the circulating compressor unit 21 after being cooled and depressurized.
The other part enters the main heat exchanger 12 of the cold box 1 through the circulating gas return pipe L8, the temperature of the returned gas is reduced to a liquefaction point, the gas is divided into two parts, one part enters the high temperature side of the deoxidizing tower reboiler 131 through the first circulating gas return pipe L81, heat is released through phase change, the liquid at the low temperature side is vaporized, the gas is provided for rectification of the deoxidizing tower 13, and the gas is liquefied into liquid. The other part enters the high temperature side of the refined argon tower reboiler 141 through the second circulating gas return pipe L82, releases heat through phase change, vaporizes the liquid at the low temperature side, provides gas for the rectification of the refined argon tower 14, and is liquefied into liquid. Liquefied liquid from the two reboilers 131 and 141 enters a deoxidizing tower condensing evaporator 132 and a refined argon tower condensing evaporator 142 after being throttled by a regulating valve V3 and a regulating valve V4 respectively through a first circulating gas condensate return pipe L82 and a second circulating gas condensate return pipe L84, and cools gas at the tops of the deoxidizing tower 13 and the refined argon tower 14 to provide rectification liquid for the two towers; wherein part of the deoxidized crude argon at the top of the deoxidizing tower 13 enters the deoxidizing tower condensation evaporator 132 through a branch of the deoxidized crude argon pipe L2-a deoxidized crude argon branch pipe L21, and condensate thereof returns to the deoxidizing tower 13 through a deoxidized crude argon condensate return pipe L22; part of nitrogen at the top of the refined argon tower 14 enters a refined argon tower condensation evaporator 142 through a branch-nitrogen branch pipe L41 of a nitrogen pipe L4, condensate of the nitrogen enters the refined argon tower 14 through a nitrogen condensate return pipe L42, and the rest of nitrogen is discharged after cold energy is recovered through the main heat exchanger 12 through the nitrogen pipe L4. After the liquid in the deoxidizing tower condensing evaporator 132 and the refined argon tower condensing evaporator 142 are vaporized, the un-throttled liquefied liquid respectively discharged from the deoxidizing tower reboiler and the refined argon tower reboiler is subjected to heat exchange in the subcooler 17, the gas discharged from the subcooler 17 is mixed with the gas at the outlet of the expansion end 223 of the expander through the circulating gas pipe L7, and the gas is reheated by the main heat exchanger 12 to be discharged from the cold box 1 and enters the circulating compressor unit 21 for pressurized circulation.
In the above embodiment, the first circulating gas condensate return pipe L82 is provided with the first circulating gas condensate return branch pipe L86 that leads to the refined argon column condensation evaporator 142, and the first circulating gas condensate return branch pipe L86 is provided with the regulating valve V5; the deoxidizing tower reboiler 131, deoxidizing tower condensing evaporator 132, refined argon tower reboiler 133 and refined argon tower condensing evaporator 134 are immersed heat exchangers; the deoxidizing tower 13 and the refined argon tower 14 adopt a structured packing structure, and two sections of packing are arranged (the two sections of packing can be adjusted according to actual conditions).
According to the embodiment, the cold energy is provided by the circulating machine, and the argon is liquefied while being purified, so that the defect of subject air separation is overcome; meanwhile, the heat exchange flow is reasonably configured, so that energy utilization is optimized, loss of cold energy is reduced, argon is recovered to the greatest extent, waste is reduced, and the method has certain economic benefit.
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 (6)
1. A device for purifying and recycling argon through full rectification, which is characterized by comprising:
the crude argon purification and recovery system comprises a raw gas compressor unit (11), a main heat exchanger (12), a deoxidizing tower (13), a refined argon tower (14) and a subcooler (15) which are connected through pipelines; the main heat exchanger (12), the deoxidizing tower (13), the refined argon tower (14) and the subcooler (15) are all arranged in the cold box (1), the deoxidizing tower (13) comprises a deoxidizing tower reboiler (131) arranged at the bottom of the deoxidizing tower (13) and a deoxidizing tower condensation evaporator (132) arranged at the top of the deoxidizing tower (13), and the refined argon tower (14) comprises a refined argon tower reboiler (141) arranged at the bottom of the refined argon tower (14) and a refined argon tower condensation evaporator (142) arranged at the top of the refined argon tower (14);
the argon gas circulation system comprises a circulating gas compressor unit (21) and an expander (22) which are connected through pipelines, wherein the circulating gas compressor unit (21) and the expander (22) are respectively connected with corresponding equipment in the crude argon gas purification and recovery system through corresponding pipelines;
the method for purifying and recycling argon through full rectification by adopting the device comprises the following steps:
step 1) pressurizing and cooling crude argon: the crude argon containing oxygen and hydrogen enters a raw material air compressor unit for pressurization and preliminary cooling, and is further cooled to the liquefaction temperature through a main heat exchanger;
step 2) rectification and purification of crude argon: the crude argon at the liquefaction temperature enters the middle lower part of the deoxidizing tower for rectification separation, deoxidized crude argon is obtained at the top of the deoxidizing tower, and oxygen-containing liquid is discharged at the bottom of the deoxidizing tower; the deoxidized crude argon is discharged from the top of the deoxidizing tower and enters the middle part of the refined argon tower for rectification separation, high-purity liquid argon is obtained at the bottom of the refined argon tower, and nitrogen is discharged from the top of the refined argon tower;
the main heat exchanger, the deoxidizing tower and the refined argon tower are all arranged in a cold box, and an argon circulation system provides low temperature for the cold box and cold energy for argon liquefaction;
in the step 2), in the rectification separation of the deoxidizing tower, a deoxidizing tower reboiler at the bottom of the deoxidizing tower provides gas required by the rectification of the deoxidizing tower, and a deoxidizing tower condensation evaporator at the top of the deoxidizing tower provides liquid required by the rectification of the deoxidizing tower; in the rectification separation of the refined argon tower, a refined argon tower reboiler at the bottom of the refined argon tower provides gas required by the rectification of the refined argon tower, and a refined argon tower condensation evaporator at the top of the refined argon tower provides liquid required by the rectification of the refined argon tower;
the heat sources of the deoxidization tower reboiler and the refined argon tower reboiler are circulating argon from an argon circulating system, the cold sources are respectively liquid at the bottom of the deoxidization tower and liquid at the bottom of the refined argon tower, and in the heat exchange process, the circulating argon is liquefied into liquid, and the liquid at the bottom of the tower is vaporized to generate gas;
the heat sources of the deoxidization tower condensation evaporator and the refined argon tower condensation evaporator are deoxidization crude argon and nitrogen respectively, the cold sources are liquid argon, the deoxidization crude argon and the nitrogen are respectively condensed into liquid in the heat exchange process, the liquid argon is vaporized to generate gas, and the vaporized gas from the deoxidization tower condensation evaporator and the refined argon tower condensation evaporator is mixed and sent into an argon circulation system;
the raw gas compressor unit (11) comprises a raw gas compressor (111) and a raw gas compressor aftercooler (112) which are connected through pipelines in sequence, the circulating gas compressor unit (21) comprises a circulating gas compressor (211) and a circulating gas compressor aftercooler (212) which are connected through pipelines in sequence, and the expander (22) comprises an expander pressurizing end (221), a pressurizing aftercooler (222) and an expander expanding end (223) which are connected through pipelines in sequence; wherein the expander expansion end (223) is disposed in the cold box (1);
the operation steps of the nitrogen circulation system comprise:
after the circulating gas from the cold box is compressed and cooled by the circulating compressor unit, the circulating gas is divided into two parts:
part of the refrigerant enters the booster end of the expander to be boosted, is cooled by the cooler after being boosted, enters the main heat exchanger, is pumped out from the middle part of the main heat exchanger, enters the expansion end of the expander to be expanded, is cooled and depressurized, and enters the main heat exchanger to be reheated and returned to the circulating compressor;
the other part enters the main heat exchanger and is divided into two parts after being cooled by the circulating gas flowing back: part of the liquid enters a deoxidizing tower reboiler to be used as a heat source, releases heat through phase change, and vaporizes the liquid at the bottom of the deoxidizing tower to be liquefied into liquid; the other part of the liquid enters a reboiler of the refined argon tower to be used as a heat source, the heat is released through phase change, the liquid at the bottom of the vaporized refined argon tower is liquefied into liquid; liquid discharged from the reboiler of the deoxidizing tower and the reboiler of the refined argon tower are throttled and then respectively enter the condensing evaporator of the deoxidizing tower and the condensing evaporator of the refined argon tower, and then the deoxidized crude argon and nitrogen are respectively cooled to respectively provide rectification liquid for the deoxidizing tower and the refined argon tower;
the liquid argon in the deoxidization tower condensation evaporator and the refined argon tower condensation evaporator are respectively vaporized to generate gas, the gas is mixed and then exchanges heat with the non-throttled liquefied liquid respectively discharged by the deoxidization tower reboiler and the refined argon tower reboiler in the subcooler, the gas from the subcooler and the gas expanded by the expansion end of the expander are mixed into circulating gas, the circulating gas is reheated by the main heat exchanger and discharged out of the cold box, and the circulating gas enters the circulating compressor unit for pressurization and circulation.
2. The apparatus for purifying and recovering argon according to claim 1, wherein the deoxidizing tower reboiler (131), deoxidizing tower condensing evaporator (132), refined argon tower reboiler (133), refined argon tower condensing evaporator (134) are immersed heat exchangers.
3. The device for purifying and recycling argon through full rectification according to claim 1, characterized in that the deoxidizing tower (13) and the refined argon tower (14) adopt a structured packing structure, a random packing structure or a sieve plate tower structure.
4. The apparatus for purifying and recovering argon by full rectification as claimed in claim 1, further comprising a liquid nitrogen storage tank for storing high purity liquid nitrogen.
5. The apparatus for purifying and recovering argon through full rectification as claimed in claim 1, wherein the method further comprises the steps of 3) recovering crude argon after the step 2): and conveying the high-purity liquid argon to a liquid argon storage tank for storage and recovery.
6. The apparatus for purifying and recovering argon through full rectification as claimed in claim 1, wherein the oxygen content in the deoxidized crude argon is less than 1.5ppm; the oxygen content in the high-purity liquid argon is less than 1.5ppm, and the nitrogen content is less than 4ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711014301.XA CN107606874B (en) | 2017-10-26 | 2017-10-26 | Device for recycling argon through full rectification purification and argon recycling method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711014301.XA CN107606874B (en) | 2017-10-26 | 2017-10-26 | Device for recycling argon through full rectification purification and argon recycling method thereof |
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| CN109506419A (en) * | 2017-09-15 | 2019-03-22 | 修国华 | For producing the method and system of liquid argon and/or argon gas product |
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| CN108507276B (en) * | 2018-06-05 | 2024-08-09 | 上海联风气体有限公司 | System and method for recycling argon through full rectification purification without expander |
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| CN111928573A (en) * | 2020-07-14 | 2020-11-13 | 国家能源集团宁夏煤业有限责任公司 | Argon preparation method |
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| CN114791204A (en) * | 2022-05-05 | 2022-07-26 | 杭州制氧机集团股份有限公司 | Nitrogen circulating low-temperature rectification crude argon purification and liquefaction device and use method thereof |
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