Method and apparatus for adsorptive distillation for cryogenic argon/oxygen separation
US-11885562-B2 · Jan 30, 2024 · US
US9759482B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9759482-B2 |
| Application number | US-201715468234-A |
| Country | US |
| Kind code | B2 |
| Filing date | Mar 24, 2017 |
| Priority date | Mar 1, 2013 |
| Publication date | Sep 12, 2017 |
| Grant date | Sep 12, 2017 |
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A method and apparatus for producing a purified liquid argon product in which liquid argon having oxygen impurities is produced in a cryogenic air separation plant by separating argon from oxygen within an argon column. An impure liquid argon stream, composed of part of the liquid argon, is purified in an adsorbent bed by adsorbing the oxygen impurities in an adsorbent to produce a purified liquid argon stream that constitutes the purified liquid argon product. During adsorption, the adsorbent bed is maintained at a reduced temperature with a coolant to prevent vaporization of the liquid argon. The bed is then regenerated by draining residual liquid argon from the adsorbent bed, introducing the residual liquid argon back into the air separation plant and then desorbing the oxygen impurities with a regeneration gas. After regeneration, the adsorbent bed is refilled with purified liquid argon prior to being brought back on-line.
Opening claim text (preview).
What is claimed is: 1. An apparatus for producing a purified liquid argon product comprising: a cryogenic air separation plant configured to separate argon from air and having an argon column to separate the argon from oxygen and produce an impure liquid argon stream having oxygen impurities; an argon purification system integrated within the cryogenic air separation plant and having a flow network connected to the impure liquid argon stream and an adsorbent bed configured to receive the impure liquid argon stream and having an adsorbent to adsorb the oxygen impurities and thereby produce a purified liquid argon stream constituting the purified liquid argon product and the argon purification system further configured for indirectly exchanging heat from the adsorbent bed to a coolant stream, thereby preventing vaporization of the impure liquid argon stream; the flow network configured to subject the adsorbent bed to an alternating cycle having an on-line phase where the impure liquid argon stream is purified within the adsorbent bed and an off-line phase where the adsorbent contained in the adsorbent bed is regenerated; the flow network having a piping system and a system of valves within the piping system configured to selectively introduce the coolant stream into the adsorbent bed and for introducing the impure liquid argon stream into the adsorbent bed during the on-line phase to prevent vaporization of the impure liquid argon stream and the purified liquid argon product during the on-line phase and to conduct a regeneration sequence during the off-line phase; the regeneration sequence comprising: terminating introduction of the impure liquid argon stream into the adsorbent bed; draining the adsorbent bed of residual liquid argon contained in the adsorbent bed to produce a residual liquid argon stream; passing a regeneration gas through the adsorbent bed to at least in part regenerate the adsorbent by removing the oxygen impurities from the adsorbent; and, prior to the on-line phase of the alternating cycle, introducing purified liquid argon composed of the purified liquid argon product into the adsorbent bed and thereby refilling the adsorbent bed; and the piping system of the flow network connected to the cryogenic air separation plant so that during the off-line phase, the residual liquid argon stream passes into the argon column or a low pressure column of the cryogenic air separation plant as a liquid or a vapor or a mixture of liquid and vapor. 2. The apparatus of claim 1 , wherein: the adsorbent is a molecular sieve and the alternating cycle is a temperature swing adsorption process; the regeneration gas is a heated regeneration gas stream to warm the adsorbent bed and thereby desorb adsorbed oxygen; the regeneration sequence also comprises terminating introduction of the coolant stream into the adsorbent bed and the indirect heat exchange between the adsorbent bed and the coolant stream after the adsorbent bed is drained of residual argon; and resuming introduction of the coolant stream into the adsorbent bed and the indirect heat exchange between the adsorbent bed and the coolant stream prior to refilling the adsorbent bed with the purified argon liquid. 3. The apparatus of claim 2 , wherein: the cryogenic air separation plant has a main heat exchanger to cool a compressed and purified air stream composed of the air to be separated and the main heat exchanger is in flow communication with the low pressure column and a high pressure column of the cryogenic air separation plant so that a nitrogen-rich vapor column overhead stream, composed of nitrogen-rich vapor produced in either the high pressure column or the low pressure column, at least partially warms within the main heat exchanger; and the piping system is connected to the main heat exchanger so that the regeneration gas is formed from part of the nitrogen-rich vapor column overhead stream after having been at least partially warmed in the main heat exchanger. 4. The apparatus of claim 3 , wherein: the argon purification system further comprises a storage tank and a vaporizer positioned between the storage tank and the adsorbent bed and the piping system is connected to the storage tank; and the flow network is configured such that during the on-line phase of the alternating cycle, a subsidiary liquid argon stream is produced that contains a further part of the impure liquid argon stream and the subsidiary liquid argon stream is introduced into the storage tank and during the off-line phase of the alternating cycle, a liquid argon stream flows from the storage tank to the vaporizer, thereby vaporizing the liquid argon stream to form a displacement gas stream and the displacement gas stream is introduced into the adsorbent bed to assist in motivating the residual liquid argon stream from the adsorbent bed to the cryogenic air separation plant. 5. The apparatus of claim 3 , wherein: the cryogenic air separation plant is configured to produce shelf liquid in the high pressure column or the low pressure column; and the piping system of the flow network is in flow communication with the high pressure column or the low pressure column so that coolant stream is formed from the shelf liquid of the cryogenic air separation plant.
in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column · CPC title
Zeolites · CPC title
Lachmann expansion, i.e. expanded into oxygen producing or low pressure column · CPC title
of oxygen · CPC title
using simple phase separation in a vessel or drum · CPC title
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