Treatment of ammonia synthesis purge gas

• US 4,058,589 A
• Filed: 01/30/1976
• Issued: 11/15/1977
• Est. Priority Date: 02/06/1975
• Status: Expired due to Term

• Current Assignee: Costain Petrocarbon Limited
• Original Assignee: Petrocarbon Developments Ltd.
• Inventors: Haslam, Alan Alfred
• Primary Examiner(s): Vertiz, O. R.
• Assistant Examiner(s): Wheelock, Eugene T.
• Application Number:
  US05/653,830
• Time in Patent Office: 655 Days
• Field of Search: 423/359, 423/360, 423/361, 423/362, 423/262
• US Class Current: 423/359
• CPC Class Codes: C01C 1/0476 Purge gas treatment, e.g. for removal of inert gases or recovery of H2
• CPC Class Codes: F25J 2210/20 H2/N2 mixture, i.e. synthesis gas for or purge gas from ammonia synthesis
• CPC Class Codes: F25J 2245/02 Recycle of a stream in general, e.g. a by-pass stream
• CPC Class Codes: F25J 3/062 Refinery gas, cracking gas, coke oven gas, gaseous mixtures containing aliphatic unsaturated CnHm or gaseous mixtures of undefined nature
• CPC Class Codes: F25J 3/068 separation of H2/N2 mixtures, i.e. of ammonia synthesis gas in general C01B3/00
• CPC Class Codes: Y02P 20/52 using catalysts, e.g. selective catalysts

Abstract

In the synthesis of ammonia with recycle of unreacted nitrogen and hydrogen to the reactor, a purge gas stream is removed from the recycle stream and partially condensed using refrigeration provided by the expansion and subsequent vaporization of the condensate. After partial condensation the condensate is rich in methane and argon while the gaseous phase is hydrogen enriched. The gaseous stream from the partial condensation is returned to the reactor and a bleed stream is removed from this gaseous stream at a temperature not exceeding 30° C above the subambient temperature of the condensation. At least a part of the bleed stream is then expanded and injected into the expanded condensate prior to vaporization in the refrigeration step. Accumulation of helium, argon and methane impurities in the reactor can thus be prevented and expanded vaporized combined condensate and bleed can be recovered at a suitable pressure for use as a fuel gas stream.

Claims

1. A method of synthesizing ammonia, comprising the steps of:

i. reacting a synthesis gas comprising nitrogen and hydrogen, and also including methane, argon and helium as contaminants, at superatmospheric pressure in an ammonia synthesis reaction zone and recycling unreacted gas to the reaction zone;

ii. withdrawing a purge gas stream at superatmospheric pressure from the gas being recycled;

iii. removing methane and argon from the purge gas stream by cooling the purge gas stream to a sub-ambient temperature to partially condense it and form a condensate phase containing methane and argon and a hydrogen-enriched gaseous phase containing helium and separating the phases into a gaseous hydrogen-enriched stream containing helium and at least one condensate stream containing methane and argon, and recycling said gaseous hydrogen-enriched stream to said reaction zone;

iv. providing refrigeration for said cooling and partial condensation of the purge gas stream by expanding at least a part of said at least one condensate stream and evaporating the expanded condensate in indirect heat exchange with the purge gas stream, and then withdrawing the evaporated expanded condensate as tail gas;

v. withdrawing a single bleed stream from the recycling hydrogen enriched stream;

vi. maintaining the concentration of methane, argon and helium in the ammonia synthesis reaction zone substantially constant by withdrawing helium, argon and methane in said bleed stream and said at least one condensate stream at substantially the same rate as they are introduced into the ammonia synthesis reaction zone with fresh synthesis gas; and

vii. recovering the tail gas at a pressure above 18 psig by withdrawing said bleed stream from said hydrogen enriched stream at a temperature not exceeding 30°

C above said subambient temperature, expanding at least a part of said bleed stream and injecting said expanded part into said expanded condensate prior to evaporating the latter.

2. A method as claimed in claim 1 in which the cooling and partial condensation of the purge gas stream are effected by a plurality of heat exchange steps with separation of the condensate formed in each heat exchange step before the gas stream is subjected to the next heat exchange step, and the bleed stream is withdrawn from the gaseous hydrogen-enriched stream resulting from the final separation step.

3. A method as claimed in claim 1 in which the bleed stream is removed from the hydrogen-enriched stream at substantially the temperature at which said hydrogen-enriched stream is separated from the condensate.