Method and apparatus for cryogenic separation of a mixture containing at least carbon monoxide, hydrogen and nitrogen

Patent metadata

Field	Value
Publication number	US-10539365-B2
Application number	US-201415024124-A
Country	US
Kind code	B2
Filing date	Sep 23, 2014
Priority date	Sep 24, 2013
Publication date	Jan 21, 2020
Grant date	Jan 21, 2020

Abstract

The invention relates to an apparatus for cryogenic separation of a mixture of carbon monoxide, hydrogen and nitrogen, including a stripping column and a denitrogenation column, a pipe for sending the mixture in liquid form to the head of the stripping column, a pipe for removing a liquid depleted of hydrogen connected to the stripping column, a pipe for removing a gas enriched with hydrogen from the stripping column, means for sending the liquid depleted of hydrogen or a fluid derived from said liquid to the denitrogenation column, a pipe for drawing a liquid enriched with carbon monoxide from the denitrogenation column, a pipe for drawing a gas enriched with nitrogen from the head of the denitrogenation column and means for sending at least one portion of the gas enriched with hydrogen to the denitrogenation column.

First claim

The invention claimed is:

1. A method for the cryogenic separation of a mixture containing at least carbon monoxide, hydrogen, nitrogen, and methane, the method comprising the steps of:
introducing the mixture, in liquid form, to the top of a stripping column under conditions effective for separation therein to form a hydrogen-lean liquid and a hydrogen-enriched gas;
introducing the hydrogen-lean liquid to a separation column under conditions effective for separation therein to form a methane-enriched liquid at a bottom portion and a carbon monoxide-enriched gas at a top portion, the separation column having a top condenser;
introducing the carbon monoxide-enriched gas from the top of the separation column to a nitrogen-removal column under conditions effective for separation therein to form a carbon monoxide-enriched liquid and a nitrogen-enriched gas containing the majority of the nitrogen present in the mixture;
determining if the nitrogen content of an identified stream(s) selected from the group consisting of the mixture, the nitrogen-enriched gas, the carbon monoxide-enriched gas removed from the top of a separation column, and combinations thereof is/are below a respective threshold(s);
selectively introducing at least part of the hydrogen-enriched gas from the stripping column to an intermediate point of the separation column based on the determined nitrogen content of the identified stream, and selectively introducing an uncondensed gas from the top condenser of the separation column to the nitrogen-removal column based on the nitrogen content of the identified stream.

2. The method as claimed in claim 1 , wherein the step of determining if the nitrogen content of the identified streams(s) is/are below the respective threshold(s) is based on a signal received from a detector configured to measure the flow rate of the nitrogen-enriched gas.

3. The method as claimed in claim 1 , wherein a pressure detector (PIC) is configured to control a flow rate of the carbon monoxide-enriched gas coming from the top portion of the separation column.

4. The method as claimed in claim 1 , wherein the uncondensed gas from the top condenser is mixed with the carbon monoxide-enriched gas prior to introduction to the nitrogen-removal column.

5. The method as claimed in claim 1 , wherein, if, and only if, the nitrogen content of the identified stream(s) is below the respective threshold(s) is at least part of the hydrogen-enriched gas sent to the separation column at an intermediate point of the separation column and is the uncondensed gas from the top condenser sent to the nitrogen-removal column.

6. The method as claimed in claim 1 , wherein the mixture is a bottom liquid from a methane scrubbing column, wherein a scrubbing liquid used in the methane scrubbing column is comprised of the methane-enriched liquid received from the bottom portion of the separation column.

7. A method for the cryogenic separation of a mixture containing at least carbon monoxide, hydrogen and nitrogen, the method comprising the steps of:
introducing the mixture, in liquid form, to the top of a stripping column under conditions effective for separation therein to form a hydrogen-lean liquid and a hydrogen-enriched gas;
introducing the hydrogen-lean liquid or a fluid derived from the hydrogen-lean liquid to a nitrogen-removal column under conditions effective for separation therein to form a carbon monoxide-enriched liquid and a nitrogen-enriched gas containing the majority of the nitrogen present in the mixture; and
determining if the nitrogen content of an identified stream(s) selected from the group consisting of the mixture, the nitrogen-enriched gas, and combinations thereof is/are below a respective threshold(s),
selectively introducing at least part of the hydrogen-enriched gas coming from the stripping column to an intermediate point of the nitrogen-removal column based on the nitrogen content of the identified stream.

8. The method as claimed in claim 7 , wherein the fluid derived from the hydrogen-lean liquid is produced by expanding the hydrogen-lean liquid through a valve.

9. A method for the cryogenic separation of a mixture comprising carbon monoxide, hydrogen and nitrogen, the method comprising the steps of:
introducing the mixture, in liquid form, to the top of a stripping column under conditions effective for separation therein to form a hydrogen-lean liquid and a hydrogen-enriched gas; and
introducing the hydrogen-lean liquid or a fluid derived from the hydrogen-lean liquid to a nitrogen-removal column under conditions effective for separation therein to form a carbon monoxide-enriched liquid and a nitrogen;
selectively increasing a flow rate of incondensables introduced to the nitrogen-removal column based on the nitrogen content within the nitrogen removal column, wherein the incondensables comprise hydrogen from the hydrogen-enriched gas.

Assignees

• Air Liquide

Inventors

• Fernandez Angela
• Marty Pascal
• Prasad Bhadri
• Victor Marie-Pascal

Classifications

• F25J2205/30

  using a washing, e.g. "scrubbing" or bubble column for purification purposes · CPC title

• F25J3/0252

  separation of hydrogen (production of hydrogen containing gas in general C01B3/00, e.g. separation of hydrogen or hydrogen containing gases form gaseous mixtures at low temperatures C01B3/506) · CPC title

• F25J3/0223 Primary

  H2/CO mixtures, i.e. synthesis gas; Water gas or shifted synthesis gas (production of carbon monoxide containing gas in general C01B32/40, C10J, C10K; production of hydrogen containing gas C01B3/00) · CPC title

• F25J2205/04

  in the feed line, i.e. upstream of the fractionation step · CPC title

• F25J3/0655 Primary

  separation of hydrogen (production of hydrogen containing gas in general C01B3/00, e.g. separation of hydrogen or hydrogen containing gases form gaseous mixtures at low temperatures C01B3/506) · CPC title