Inert gaseous components such as methane and argon are indeed should be eliminated from the system in order not to lower the partial pressure of the reactants too much. Technically there is usually a standalone gas separation plant where the extraction of argon from the recycle gas is performed basically using modified Linde process [1 , pp. 428–430].

Suitable cryoprocesses [...] are available for production of noble gases from synthesis purge gas. Initially, extensive separation of nitrogen, argon, and methane is carried out by partial condensation. Purge argon is then recovered from the condensate in a two-stage condensation process. If helium is to be recovered it can be concentrated by liquefaction of the hydrogen in the hydrogen-rich gas phase, followed by purification. The heavier noble gases, krypton and xenon, pass into the methane fraction.

 

The purge gas at pressures of up to $\pu{70 bar}$ is first introduced into the adsorber (a) where traces of water and ammonia are removed. It is then transferred to the heat exchangers (b1) and (b2) for cooling. The gas is then fed into separators (c1) and (c2) where separation of liquefied nitrogen, argon, and methane from gaseous hydrogen takes place, and dissolved hydrogen flashes off. The liquid bottom product is fed into the fractionating column (d1) where methane (bottom) is separated from the nitrogen fraction (top).

 

A methane-free nitrogen – argon mixture (liquid) is withdrawn from the middle of this column and fed as reflux into the $\ce{Ar}$ purification column (d2), where nitrogen is separated from argon. The bottom product is argon of product purity and is transferred to a vacuum-insulated storage tank.

 

Both columns (d1) and (d2) are operated within an $\ce{N2}$ cycle in which cold is produced by expanding high- or medium-pressure nitrogen.

 

The $\ce{CH4}$ bottom stream from (d1), compressed by liquid pump (g), is evaporated against feed gas and normally led to battery limits as fuel gas. The higher boiling noble gases krypton and xenon are contained in this stream and, in principle, can be isolated.

Reference

1. Häussinger, P.; Glatthaar, R.; Rhode, W.; Kick, H.; Benkmann, C.; Weber, J.; Wunschel, H.-J.; Stenke, V.; Leicht, E.; Stenger, H. In Ullmann’s Encyclopedia of Industrial Chemistry; Wiley-VCH Verlag GmbH & Co. KGaA, Ed.: Weinheim, Germany, 2001. DOI: 10.1002/14356007.a17_485.

Inert gaseous components such as methane and argon are indeed should be eliminated from the system in order not to lower the partial pressure of the reactants too much. Technically there is usually a standalone gas separation plant where the extraction of argon from the recycle gas is performed basically using modified Linde process [1 , pp. 428–430].

Suitable cryoprocesses [...] are available for production of noble gases from synthesis purge gas. Initially, extensive separation of nitrogen, argon, and methane is carried out by partial condensation. Purge argon is then recovered from the condensate in a two-stage condensation process. If helium is to be recovered it can be concentrated by liquefaction of the hydrogen in the hydrogen-rich gas phase, followed by purification. The heavier noble gases, krypton and xenon, pass into the methane fraction.

The purge gas at pressures of up to $\pu{70 bar}$ is first introduced into the adsorber (a) where traces of water and ammonia are removed. It is then transferred to the heat exchangers (b1) and (b2) for cooling. The gas is then fed into separators (c1) and (c2) where separation of liquefied nitrogen, argon, and methane from gaseous hydrogen takes place, and dissolved hydrogen flashes off. The liquid bottom product is fed into the fractionating column (d1) where methane (bottom) is separated from the nitrogen fraction (top).

A methane-free nitrogen – argon mixture (liquid) is withdrawn from the middle of this column and fed as reflux into the $\ce{Ar}$ purification column (d2), where nitrogen is separated from argon. The bottom product is argon of product purity and is transferred to a vacuum-insulated storage tank.

Both columns (d1) and (d2) are operated within an $\ce{N2}$ cycle in which cold is produced by expanding high- or medium-pressure nitrogen.

The $\ce{CH4}$ bottom stream from (d1), compressed by liquid pump (g), is evaporated against feed gas and normally led to battery limits as fuel gas. The higher boiling noble gases krypton and xenon are contained in this stream and, in principle, can be isolated.

Reference

1. Häussinger, P.; Glatthaar, R.; Rhode, W.; Kick, H.; Benkmann, C.; Weber, J.; Wunschel, H.-J.; Stenke, V.; Leicht, E.; Stenger, H. In Ullmann’s Encyclopedia of Industrial Chemistry; Wiley-VCH Verlag GmbH & Co. KGaA, Ed.: Weinheim, Germany, 2001. DOI: 10.1002/14356007.a17_485.

Inert gaseous components such as methane and argon are indeed should be eliminated from the system in order not to lower the partial pressure of the reactants too much. Technically there is usually a separate gas separation plant where the extraction of argon from the recycle gas is performed using Linde process [1 , p. 428].

Suitable cryoprocesses [...] are available for production of noble gases from synthesis purge gas. Initially, extensive separation of nitrogen, argon, and methane is carried out by partial condensation. Purge argon is then recovered from the condensate in a two-stage condensation process. If helium is to be recovered it can be concentrated by liquefaction of the hydrogen in the hydrogen-rich gas phase, followed by purification. The heavier noble gases, krypton and xenon, pass into the methane fraction.

Reference

1. Häussinger, P.; Glatthaar, R.; Rhode, W.; Kick, H.; Benkmann, C.; Weber, J.; Wunschel, H.-J.; Stenke, V.; Leicht, E.; Stenger, H. In Ullmann’s Encyclopedia of Industrial Chemistry; Wiley-VCH Verlag GmbH & Co. KGaA, Ed.; Wiley-VCH Verlag GmbH & Co. KGaA: Weinheim, Germany, 2001. DOI: 10.1002/14356007.a17_485.

Inert gaseous components such as methane and argon are indeed should be eliminated from the system in order not to lower the partial pressure of the reactants too much. Technically there is usually a standalone gas separation plant where the extraction of argon from the recycle gas is performed basically using modified Linde process [1 , pp. 428–430].

Suitable cryoprocesses [...] are available for production of noble gases from synthesis purge gas. Initially, extensive separation of nitrogen, argon, and methane is carried out by partial condensation. Purge argon is then recovered from the condensate in a two-stage condensation process. If helium is to be recovered it can be concentrated by liquefaction of the hydrogen in the hydrogen-rich gas phase, followed by purification. The heavier noble gases, krypton and xenon, pass into the methane fraction.

The purge gas at pressures of up to $\pu{70 bar}$ is first introduced into the adsorber (a) where traces of water and ammonia are removed. It is then transferred to the heat exchangers (b1) and (b2) for cooling. The gas is then fed into separators (c1) and (c2) where separation of liquefied nitrogen, argon, and methane from gaseous hydrogen takes place, and dissolved hydrogen flashes off. The liquid bottom product is fed into the fractionating column (d1) where methane (bottom) is separated from the nitrogen fraction (top).

A methane-free nitrogen – argon mixture (liquid) is withdrawn from the middle of this column and fed as reflux into the $\ce{Ar}$ purification column (d2), where nitrogen is separated from argon. The bottom product is argon of product purity and is transferred to a vacuum-insulated storage tank.

Both columns (d1) and (d2) are operated within an $\ce{N2}$ cycle in which cold is produced by expanding high- or medium-pressure nitrogen.

The $\ce{CH4}$ bottom stream from (d1), compressed by liquid pump (g), is evaporated against feed gas and normally led to battery limits as fuel gas. The higher boiling noble gases krypton and xenon are contained in this stream and, in principle, can be isolated.

Reference

1. Häussinger, P.; Glatthaar, R.; Rhode, W.; Kick, H.; Benkmann, C.; Weber, J.; Wunschel, H.-J.; Stenke, V.; Leicht, E.; Stenger, H. In Ullmann’s Encyclopedia of Industrial Chemistry; Wiley-VCH Verlag GmbH & Co. KGaA, Ed.: Weinheim, Germany, 2001. DOI: 10.1002/14356007.a17_485.