IP Library Granted Patent US 10,464,813
Granted Patent B2
US 10,464,813 · App. 14/295,724 · Granted Nov 5, 2019

Process for recovery and purification of nitrous oxide

Inventors: Guohua Xiu (Shanghai, CN); Peng Zhang (Shanghai, CN)
Assignee: VERSUM MATERIALS US, LLC
C01B21/22Y02C20/10
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 10,464,813
App. No.
14/295,724
Granted
Nov 5, 2019
Kind
B2
Abstract

This invention is aimed at recovering and purifying nitrous oxide from the gas stream containing N 2 O 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.

Claims (37)

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.

Assignments (4)
RELEASE OF SECURITY INTEREST Recorded Oct 7, 2019
From: CITIBANK, N.A., AS AGENT
To: VERSUM MATERIALS US, LLC
Reel/Frame 050647/0001 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 20, 2017
From: AIR PRODUCTS AND CHEMICALS, INC.
To: VERSUM MATERIALS US, LLC
Reel/Frame 041772/0733 →
PATENT SECURITY AGREEMENT Recorded Oct 27, 2016
From: VERSUM MATERIALS US, LLC
To: CITIBANK, N.A., AS COLLATERAL AGENT
Reel/Frame 040503/0442 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 19, 2014
From: XIU, GUOHUA; ZHANG, PENG
To: AIR PRODUCTS AND CHEMICALS, INC.
Reel/Frame 033138/0687 →
Priority Claims (2)
CN 2013 1 0262637 · Jun 18, 2013 · national
CN 2013 2 0375675 U · Jun 18, 2013 · national
Continuity (1)
Related Publication 20140366576A1 · Dec 18, 2014