Process for recovery and purification of nitrous oxide

Patent metadata

Field	Value
Publication number	US-10464813-B2
Application number	US-201414295724-A
Country	US
Kind code	B2
Filing date	Jun 4, 2014
Priority date	Jun 18, 2013
Publication date	Nov 5, 2019
Grant date	Nov 5, 2019

Abstract

This invention is aimed at recovering and purifying nitrous oxide from the gas stream containing N2O to produce different grade of nitrous oxide by combination of unit operation including, but not limited to, wet scrubbing, adsorption, liquefaction, flash distillation or continuous distillation with reflux.

First claim

The invention claimed is:

1. A system for of recovering and purifying N 2 O, the system comprising:
a gas stream comprising N 2 O and impurities comprising light and heavy impurities, water, and organic compounds, the gas stream first entering a wet scrubbing absorption unit that is selected from the group consisting of: a caustic scrubbing unit, an acid scrubbing unit, water scrubbing unit, and combinations thereof;
a compressor having at least one stage of compression that compresses the gas stream from the wet scrubber to a preset pressure greater than 1.0 MPa;
a cooling and drying unit that cools the gas stream from the compressor to less than 10.0° C. and removes condensed water;
an adsorption unit comprising at least two parallel adsorption beds, each bed having at least one adsorbent layer adapted to remove heavy impurities, water and organic compounds from the gas stream from the cooling and drying unit;
a buffer tank that stores the gas stream from the adsorption unit;
a liquefaction unit that partially liquefies the gas stream from the buffer tank to create: (1) a first recycle gas mixture containing N 2 O and at least one non-condensation gas, and (2) a liquid mixture containing N 2 O;
a releaser in fluid communication with the buffer tank and a distillation unit, wherein the releaser transmits the first recycle gas mixture from the liquefaction unit back to the adsorption unit and passes the liquid mixture from the liquefaction unit to the distillation unit, wherein the buffer tank is adapted to permit the gas to flow back to the adsorption unit via the releaser to repressurize the adsorption unit to the preset pressure, wherein
the distillation unit is selected from a group consisting of a flash drum, a distillation column with reflux, and combinations thereof, wherein the distillation unit removes light impurities and organic compounds from the liquid mixture, and directs: (1) a second recycle gas mixture containing N 2 O and at least one non-condensation gas directly back to the compressor, and (2) purified liquid mixture to a holding tank; wherein,
the gas stream exiting the wet scrubber has less than 500.0 ppm of NO 2 and CO 2 ,
the gas stream exiting the adsorption unit has less than 0.5 ppm of NO 2 and less than 1.0 ppm of CO 2 , and
the purified liquid mixture has a N 2 O concentration of greater than 99.9% by volume.

2. The system according to claim 1 , wherein
prior to entering the wet scrubbing absorption unit, the gas stream contains 5.0 to 99.9% N 2 O by volume, and wherein
the light impurities are selected from the group consisting of N 2 , O 2 , NO, CO, Ar, H 2 , methane, and C 2 compounds;
the heavy impurities are selected from the group consisting of CO 2 , NO 2 , CO, H 2 O, and C 2+ compounds;
the organic compound is selected from the group consisting of methane, C 2+ compounds, CH 4 , and C 2 compounds;

the first recycle gas mixture and the second recycle gas mixture both include molecules selected from the group consisting of Ar, N 2 , O 2 , CO, NO, and methane; and
the purified liquid mixture has a N 2 O concentration ranging from 99.9% to 99.9999% by volume.

3. The system according to claim 1 , wherein
the compressor has at least two stages of compression and the second recycle gas mixture is introduced to the compressor between the first and the second stage; and
the preset pressure of the gas mixture exiting the second stage of compression ranges from between 2.0 to 5.0 MPa.

4. The system according to claim 1 , wherein
the parallel adsorption beds are alternately used in continuous swing operation and the first recycle gas mixture is used to regenerate the adsorption unit; and
the adsorbent layer comprises molecular sieves selected from the group consisting of 13X, 3A, 4A, SA, CaX, silica gel, calcium Y zeolite, zinc X zeolite, molecular sieve with high ratio of silica to alumina, active alumina, activated carbon, and combinations thereof.

5. The system according to claim 1 , wherein
the gas stream is an off gas stream from adipic acid production process or nitric acid production process; and
prior to entering the wet scrubbing absorption unit, the gas stream contains
28.0 to 70.0% N 2 O by volume,
1.0 to 6.0% O 2 by volume,
20.0 to 60.0% N 2 by volume,
0.2 to 1.0% Ar by volume,
2 to 10.0% CO 2 by volume,
0.1 to 1.0% CO by volume,
1.0 ppm to 0.5% NO 2 by volume,
1.0 ppm to 1.0% NO by volume, and
1.0 ppm to 0.1% hydrocarbons by volume.

Assignees

• Air Prod & Chem
• Versum Mat Us Llc

Inventors

• Xiu Guohua
• Zhang Peng

Classifications

• B01D47/12

  Washers with plural different washing sections (B01D47/14 takes precedence) · CPC title

• F25J1/00

  Processes or apparatus for liquefying or solidifying gases or gaseous mixtures {(recovering volatile solvents by condensation B01D5/00; vapor recovery systems combined with filling nozzles B67D7/54; solidification of carbonic acid C01B32/55; for ammonia in general C01C1/00)} · CPC title

• B01D53/75

  Multi-step processes · CPC title

• C01B21/22 Primary

  Nitrous oxide (N2O) {(C01B21/203 takes precedence)} · CPC title

• B01D53/26

  Drying gases or vapours · CPC title