IP Library Granted Patent US 11,491,435
Granted Patent B2
US 11,491,435 · App. 16/879,444 · Granted Nov 8, 2022

Methods and systems for removing ammonia from a gas mixture

Inventors: Charles H. Applegarth (San Luis Obispo, CA); Rocky D. Gipson (San Marcos, CA); Sarah Vogt (Grover Beach, CA); Joshua T. Cook (San Diego, CA); Matthew Browning (San Luis Obispo, CA); Marco Holzner (San Luis Obispo, CA)
Assignee: ENTEGRIS, INC.
B01D53/0438B01D45/12B01D50/20C01C1/02B01D53/0462B01D2253/102B01D2256/10B01D2256/16B01D2257/406B01D2257/706B01D2258/0216B01D2259/401B01D2259/40001B01D2259/402B01D2259/40088
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 11,491,435
App. No.
16/879,444
Granted
Nov 8, 2022
Kind
B2
Abstract

Described are methods, devices, and systems useful for removing gaseous ammonia from a gas mixture at a pressure in an ambient pressure range by allowing the ammonia to adsorb onto a solid adsorbent, as well as related systems and methods.

Claims (38)

1. A method of removing ammonia from a gas mixture comprising gaseous ammonia, gaseous hydrogen, and gaseous nitrogen, the method comprising:

delivering the gas mixture at an ambient flow pressure to a vessel that contains a solid adsorbent, with the gas mixture, the solid adsorbent, or both at an ammonia adsorption temperature in a range of from −40 to 0 degrees Celsius,

contacting the gas mixture at the ambient flow pressure and at the ammonia adsorption temperature with the solid adsorbent to cause an amount of ammonia to adsorb onto the solid adsorbent,

after the amount of ammonia has adsorbed onto the solid adsorbent, increasing the temperature of the solid adsorbent that contains adsorbed ammonia to a desorption temperature to desorb the adsorbed ammonia from the solid adsorbent to form liquid ammonia; and

removing the desorbed liquid ammonia from the vessel.

2. The method of claim 1 , wherein the gas mixture, the solid adsorbent, or both are cooled to the ammonia adsorption temperature at which the gaseous ammonia of the gas mixture adsorbs onto the solid adsorbent at the ambient flow pressure.

3. The method of claim 1 , wherein the ammonia adsorption temperature is in a range from −35 degrees Celsius to −5 degrees Celsius.

4. The method of claim 1 , wherein the gaseous hydrogen and the gaseous nitrogen do not adsorb onto the solid adsorbent at the ammonia adsorption temperature.

5. The method of claim 1 , wherein the gas mixture, the solid adsorbent, or both have a temperature in a range from −30 to −15 degrees Celsius.

6. The method of claim 1 , wherein the desorption temperature is below 60 degrees Celsius.

7. The method of claim 1 , wherein the solid adsorbent is selected from activated carbon and zeolite.

8. The method of claim 1 , wherein the gas mixture delivered to the vessel comprises:

from 15 to 40 volume percent gaseous ammonium;

from 0 to 60 volume percent gaseous hydrogen; and

from 0 to 70 volume percent gaseous nitrogen.

9. The method of claim 1 , wherein the gas mixture further comprises organometallic vapor and solid particles, and wherein the method further comprises:

cooling the gas mixture to the ammonia adsorption temperature by passing the gas mixture through a heat exchanger to produce a cooled gas mixture,

passing the cooled gas mixture through a particle filter to substantially remove the solid particles, and

passing the cooled gas mixture with substantially removed solid particles through a first solid adsorbent to substantially remove organometallic vapor by adsorbing the organometallic vapor onto the first solid adsorbent.

10. The method of claim 9 , wherein, the gas mixture has a temperature greater than 60 degrees Celsius prior to delivering the gas mixture to the vessel.

11. The method of claim 9 , wherein the cooled gas mixture has a temperature in a range from 0 to 60 degrees Celsius.

12. The method of claim 9 , wherein the heat exchanger is a counterflow coil heat exchanger comprising:

a heat exchanger body comprising a body inlet, a body outlet, and a body interior volume, and

a hollow coil body located within the heat exchanger body interior volume and comprising a coil inlet, a coil outlet, and multiple coil turns between the coil inlet and the coil outlet, wherein:

the gas mixture enters the heat exchanger body at the body inlet, flows through the body interior volume and over an exterior surf ace of the hollow coil body, and exits the heat exchanger body at the body outlet, and

a cooling liquid enters the hollow coil body at the coil inlet, flows through the hollow coil body in a direction opposite of a direction of flow of the gas mixture passing through the heat exchanger body, and exits the hollow coil body at the coil outlet.

13. The method of claim 9 , wherein the gas mixture comprises:

from 15 to 40 volume percent gaseous ammonia;

from 0 to 60 volume percent gaseous hydrogen;

from 0 to 70 volume percent gaseous nitrogen; and

organometallic vapor.

14. The method of claim 13 , wherein the organometallic vapor is trimethyl gallium vapor.

15. A system for processing a gas mixture comprising gaseous ammonia, non-ammonia vapor, organometallic vapor, and solid particles, the system comprising:

a heat exchanger adapted to reduce a temperature of the gas mixture;

a particle filter capable of removing solid particles from the gas mixture;

an organometallic vapor removal filter capable of removing organometallic vapor from the gas mixture; and

a vessel that contains solid adsorbent capable of removing ammonia vapor from the gas mixture by adsorbing the ammonia vapor onto the solid adsorbent at conditions that include an ambient flow pressure and an ammonia adsorption temperature and is further capable of desorbing the adsorbed ammonia vapor from the solid adsorbent at conditions that include a desorption temperature to form liquid ammonia that is removable from the vessel,

wherein the heat exchanger, the particle filter, the organometallic vapor removal filter and the vessel are in fluid communication with each other.

Assignments (3)
SECURITY INTEREST Recorded Jul 8, 2022
From: ENTEGRIS, INC.; ENTEGRIS GP, INC.; POCO GRAPHITE, INC.; CMC MATERIALS, INC.; INTERNATIONAL TEST SOLUTIONS, LLC; QED TECHNOLOGIES INTERNATIONAL, INC.
To: TRUIST BANK, AS NOTES COLLATERAL AGENT
Reel/Frame 060613/0072 →
SECURITY INTEREST Recorded Jul 8, 2022
From: ENTEGRIS, INC.; ENTEGRIS GP, INC.; POCO GRAPHITE, INC.
To: MORGAN STANLEY SENIOR FUNDING, INC., AS COLLATERAL AGENT
Reel/Frame 060614/0980 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 20, 2020
From: APPLEGARTH, CHARLES H.; GIPSON, ROCKY D.; VOGT, SARAH; COOK, JOSHUA T.; BROWNING, MATTHEW; HOLZNER, MARCO
To: ENTEGRIS, INC.
Reel/Frame 052716/0514 →
Continuity (2)
Provisional Application 62852478 · May 24, 2019
Related Publication 20200368668A1 · Nov 26, 2020