Process for manufacture of ultra-high purity ammonium hydroxide

• US 5,746,993 A
• Filed: 10/17/1996
• Issued: 05/05/1998
• Est. Priority Date: 10/17/1996
• Status: Expired due to Fees

• Current Assignee: Advanced Micro Devices, Inc.
• Original Assignee: Advanced Micro Devices, Inc.
• Inventors: Mullee, William H.
• Primary Examiner(s): LANGEL, WAYNE A
• Application Number:
  US08/733,277
• Time in Patent Office: 565 Days
• Field of Search: 423/352
• US Class Current: 423/352
• CPC Class Codes: C01C 1/022 Preparation of aqueous ammonia solutions, i.e. ammonia water

Abstract

A process for obtaining an ultra-high purity aqueous ammonium hydroxide solution according to the invention includes the steps of reacting highly pure, typically electronics grade, ammonia (NH₃) with ultrapure water (upw) under conditions effective to produce an ultra-high purity stream of aqueous ammonium hydroxide (NH₄ OH) which is available for immediate use in a wide variety of applications especially those requiring high purity aqueous solutions of ammonium hydroxide.

Claims

1. A process for the production of an ammonium hydroxide solution, comprising the steps of:

(a) injecting gaseous ammonia into a closed first reactor vessel through a sparger tube that releases the ammonia within the first reactor vessel;

(b) adding ultra-pure water to the first reactor vessel so that the ammonia comes in contact with the ultra-pure water and forms the ammonium hydroxide solution;

(c) cooling the first reactor vessel as the ammonium hydroxide solution is formed to maintain a reaction temperature effective to promote the reaction between the ammonia and the ultra-pure water;

(d) maintaining a quantity of the ammonium hydroxide solution in the first reactor vessel;

(e) withdrawing the ammonium hydroxide solution from the first reactor vessel; and

(f) cooling the ammonium hydroxide solution after it is withdrawn from the first reactor vessel;

wherein steps (a) to (f) are conducted substantially concurrently so that the ultra-pure water and the ammonia are added and the ammonium hydroxide solution is withdrawn, without recirculation back to the first reactor vessel, in a manner effective to provide a substantially steady state of reaction within the first reactor vessel;

(g) providing the ammonium hydroxide solution from the closed first reactor vessel into a closed second reactor vessel;

(h) injecting gaseous ammonia into the second reactor vessel through a sparger tube that releases the ammonia within the second reactor vessel so that the ammonia comes in contact with the ammonium hydroxide solution and forms a higher concentration ammonium hydroxide solution;

(i) cooling the second reactor vessel as the higher concentration ammonium hydroxide solution is formed to maintain a reaction temperature effective to promote the reaction between the ammonia and the ammonium hydroxide solution;

(j) maintaining a quantity of the higher concentration ammonium hydroxide solution in the second reactor vessel;

(k) withdrawing the higher concentration ammonium hydroxide solution from the second reactor vessel; and

(l) cooling the higher concentration ammonium hydroxide solution after it is withdrawn from the second reactor vessel;

wherein steps (g) to (l) are conducted substantially concurrently so that the ammonium hydroxide solution is added and the higher concentration ammonium hydroxide solution is withdrawn, without recirculation back to the second reactor vessel, in a manner effective to provide a substantially steady state of reaction within the second reactor vessel.

2. The process of claim 1, wherein step (c) further comprises maintaining the temperature in the first reactor vessel in the range of about 0°

C. to 50°

C., and step (f) further comprises cooling the ammonium hydroxide solution to about 10°

C. or less.

3. The process of claim 1, wherein the ammonia gas is admitted to the first reactor vessel at a rate in the range of about 1.5 to 2.2 lbs NH₃ per gallon of the ultra-pure water solution, and the ammonium hydroxide solution is admitted at a rate in the range of about 0.1 to 60 gallons per minute.

4. The process of claim 1, wherein the amount of the ammonia gas occupies from about 10% to 40% by volume of the first reactor vessel.

5. The process of claim 1, further comprising a step (m) of storing the higher concentration ammonium hydroxide solution in a holding tank for no more than about 24 hours.

6. The process of claim 5, wherein step (m) further comprises storing the higher concentration ammonium hydroxide solution in the holding tank for no more than about 6 hours.

7. The process of claim 5, further comprising a step (n) of controlling production of the higher concentration ammonium hydroxide solution in the second reactor vessel and withdrawal of the higher concentration ammonium hydroxide solution from the holding tank so that the holding tank remains at least about 75% full during operation, and purging the holding tank with an inert gas in a manner effective to reduce loss of concentration of the higher concentration ammonium hydroxide solution during storage.

8. The process of claim 5, wherein the holding tank is a flexible-walled plastic container having an HDPE interior surface.