Continuous process for the production of azide salts

• US 5,098,597 A
• Filed: 06/29/1990
• Issued: 03/24/1992
• Est. Priority Date: 06/29/1990
• Status: Expired due to Fees

• Current Assignee: Arch Chemicals Incorporated (Lonza Group AG)
• Original Assignee: OLIN Corporation
• Inventors: Thomas, Kimberly A., Gavin, David F., Rothgery, Eugene F.
• Primary Examiner(s): Miller, Edward A.
• Application Number:
  US07/545,784
• Time in Patent Office: 634 Days
• Field of Search: 252/182.34, 423/410, 558/488
• US Class Current: 252/182.34
• CPC Class Codes: C01B 21/08 Hydrazoic acid; Azides; Halogen azides

Abstract

The present invention relates to a continuous process for making an alkali metal azide or an alkaline earth metal azide which comprises the steps of: (a) reacting a first reaction mixture comprising an alkali metal nitrite or alkaline earth metal nitrite, a C1--C3 alkanol, and a high boiling acid in a first reactor to form a gaseous C1-C3 alkyl nitrite, (b) controllably feeding said gaseous C1-C3 alkyl nitrite into a second reactor and reacting in a controlled manner a second reaction mixture comprising said gaseous C1-C3 alkyl nitrite, hydrazine, and an alkali metal hydroxide or alkaline earth metal hydroxide, in the presence of an organic solvent, thereby producing an alkali metal azide or alkaline earth metal azide, and (c) removing said alkali metal azide or alkaline earth metal azide from said second reactor and replenishing said reaction mixture in said second reactor to provide a continuous, controlled process for producing said alkali metal azide or alkaline earth metal azide.

Claims

1. A continuous process for making an alkali metal azide or an alkaline earth metal azide which comprises the steps of:

(a) reacting a first reaction mixture comprising an alkali metal nitrite or alkaline earth metal nitrite, a C1-C3 alkanol, and a high boiling acid in a first reactor to form a gaseous C1-C3 alkyl nitrite,

(b) controllably feeding said gaseous C1-C3 alkyl nitrite into a second reactor and reacting in a controlled manner a second reaction mixture comprising said gaseous C1-C3 alkyl nitrite, hydrazine, and an alkali metal hydroxide or alkaline earth metal hydroxide, in the presence of an organic solvent, thereby producing an alkali metal azide or alkaline earth metal azide, and

(c) removing said alkali metal azide or alkaline earth metal azide from said second reactor and replenishing said reaction mixture in said second reactor with hydrazine and alkali metal hydroxide or alkaline earth metal hydroxide to provide a continuous, controlled process for producing said alkali metal azide or alkaline earth metal azide.

2. The process of claim 1 wherein said alkali metal azide or alkaline earth metal azide is selected from the group consisting of sodium azide, potassium azide, calcium azide, and magnesium azide, and combinations thereof.

3. The process of claim 1 wherein said high boiling acid is selected from the group consisting of sulfuric, phosphoric, sulfonic, and phosphonic acids, and combinations thereof.

4. The process of claim 1 wherein said C1-C3 alkanol employed in step (a) is suitably selected from the group of lower carbon-containing alcohols consisting of methanol, ethanol, 1-propanol, 2-propanol, and combinations thereof.

5. The process of claim 1 wherein step (a) is carried out in the presence of a water solvent.

6. The process of claim 1 wherein step (a) is carried out using a ratio of molar equivalents of acid:

nitrite salt;

alkanol of between 2;

2;

1 and 1;

1;

2.

7. The process of claim 1 wherein step (a) is carried out using a ratio of molar equivalents of acid:

nitrite salt;

alkanol of between 1.2;

1.2;

1 and 0.9;

0.9;

1.

8. The process of claim 1 wherein the organic solvent employed in step (b) is a C1-C3 alkanol.

9. The process of claim 1 wherein step (b) is carried out using a ratio of molar equivalents of alkyl nitrite:

hydrazine;

metal hydroxide of between 2;

2;

1 and 1;

1;

2.