Device and method for purifying a gas mixture

Patent metadata

Field	Value
Publication number	US-10767923-B2
Application number	US-201815981378-A
Country	US
Kind code	B2
Filing date	May 16, 2018
Priority date	May 22, 2017
Publication date	Sep 8, 2020
Grant date	Sep 8, 2020

Abstract

Device and method for purifying a gas mixture to produce a concentrated gas, notably neon, starting from a mixture comprising neon, said device including, in a cold box housing a cryogenic purification circuit comprising, in series, at least one unit for purifying the mixture by cryogenic adsorption at a temperature between 65K and 100K and notably 65K, then a unit for cooling the mixture to a temperature between 25 and 65 K and then a unit for cryogenic distillation of the mixture to produce the concentrated liquid at the outlet of the cryogenic distillation unit, characterized in that the unit for cooling the mixture to a temperature between 25 and 65 K comprises at least one cryocooler that extracts thermal power from the mixture via a heat exchanger.

First claim

What is claimed is:

1. A device for purifying a gaseous fluid mixture to produce a concentrated neon gas, starting from a mixture comprising neon, said device comprising, in a cold box housing a cryogenic purification circuit comprising, in series, at least one unit for purifying the mixture by cryogenic adsorption at a temperature between 65K and 100K, then a unit for cooling the fluid mixture to a temperature between 25 and 65 K and then a unit for cryogenic distillation of the fluid mixture to produce a concentrated liquid at the outlet of the cryogenic distillation unit, characterized in that the unit for cooling the fluid mixture to a temperature between 25 and 65 K comprises at least one cryocooler that extracts thermal power from the mixture via a heat exchanger, the at least one cryocooler comprising at least one cryocooler of the Gifford McMahon type or a pulsed gas tube or a cryocooler of the Stirling type.

2. The device of claim 1 , wherein the cooling unit comprises several cryocoolers in series and at least one heat exchanger receiving the fluid mixture, in heat exchange with the cold surfaces of said cryocoolers in series.

3. The device of claim 1 , further comprising, in the cold box upstream of the unit for purification by cryogenic adsorption: i) a first cryogenic exchanger for cooling the mixture configured to cool the mixture to a temperature between 65K and 110K, and/or ii) at least one bath of liquid nitrogen in heat exchange with a pipeline that conveys the fluid mixture.

4. The device of claim 1 , wherein the unit for purification by cryogenic adsorption comprises at least two adsorbers arranged in parallel immersed in baths of liquid nitrogen at 65K and operating alternately between adsorption and regeneration phases.

5. The device of claim 1 , wherein the unit for cryogenic distillation is a column for separating neon and helium.

6. The device of claim 1 , further comprising a pipeline for recovery of the concentrated liquid at the outlet of the unit for cryogenic distillation and in that the recovery pipeline is put in heat exchange with at least one unit for cooling the mixture located in the cold box.

7. The device of claim 6 , wherein the pipeline for recovery of the concentrated liquid is in heat exchange with a: i) bath of liquid nitrogen in heat exchange with a pipeline that conveys the mixture upstream of the unit ( 12 ) for purification by cryogenic adsorption, and/or ii) an exchanger for cooling the mixture located upstream of the cryogenic cooler.

8. The device of claim 1 , further comprising, upstream of the cold box: i) a unit for withdrawing at least part of the hydrogen contained in the mixture, and/or ii) a desiccator for withdrawing at least part of the water and/or CO 2 contained in the mixture.

9. The device of claim 8 , wherein the unit for withdrawing at least part of the hydrogen contained in the mixture comprises a catalytic reactor configured for converting the hydrogen in the mixture to water by reaction with oxygen.

10. The device of claim 8 , wherein the desiccator comprises at least one adsorbent for trapping water and carbon dioxide operating alternately.

11. The method for purifying a gas mixture comprising neon to produce a neon-enriched gas using the purification device of claim 1 , said method comprising the steps of:
purifying the gas mixture by cryogenic adsorption via unit for purification by cryogenic adsorption at a temperature between 63.5K and 80K to remove at least part of the nitrogen, oxygen, carbon monoxide and argon from the mixture;
cooling the gas mixture to a temperature between 25 and 65 K via the cryocooler and close to the triple point of neon in order to condense the neon;
cryogenically distilling the mixture in the unit for cryogenic distillation to produce neon-enriched liquid at the outlet of the unit for cryogenic distillation; and
warming the neon-enriched liquid to produce the neon-enriched gas.

12. The method of claim 11 , wherein:
the gas mixture to be purified comprises 15 and 65 vol % neon, 3-20 vol % helium, 0.2-4 vol % hydrogen, and 20-60 vol % nitrogen; and
said neon-enriched gas contains 85-100 vol % neon.

13. The method of claim 11 , wherein a ratio of a volume flow rate of neon at an outlet of the device to a volume flow rate of neon at an inlet of the device is greater than 0.85.

14. The method of claim 13 , wherein the ratio of the volume flow rate of neon at the outlet of the device to the volume flow rate of neon at the inlet of the device is between 0.85-0.98.

Assignees

• Air Liquide

Inventors

• Barjhoux Pierre
• Bouvier Camille
• Durand Fabien
• Staempflin Martin
• Zick Golo

Classifications

• F25J3/08

  Separating gaseous impurities from gases or gaseous mixtures {or from liquefied gases or liquefied gaseous mixtures}(cold traps B01D8/00) · CPC title

• F25J2270/908

  by regenerative chillers, i.e. oscillating or dynamic systems, e.g. Stirling refrigerator, thermoelectric ("Peltier") or magnetic refrigeration · CPC title

• F25J2220/02

  Separating impurities in general from the feed stream · CPC title

• F25J2270/02

  Internal refrigeration with liquid vaporising loop · CPC title

• F25J3/028 Primary

  separation of noble gases (from air F25J3/04642; in general C01B23/00) · CPC title