Pacific Scientific Energetic Materials Company

US Government As Represented by the Secretary of the Army

Sri International

Jon G Bragg

John William Fronabarger

Michael D Williams

Neha Mehta

Jason B Pattison

Jerry S Salan

Matthew L Jorgensen

Andrew G Pearsall

Jeffrey C Bottaro

Mark A Petrie

Lily F W Walsh

Daniel W Ward

R Hunter Muir

John W Fronabarger

The present invention is directed to a process for continuous production of copper (I) nitrotetrazolate (DBX-1) by reacting aqueous copper salt with aqueous 5-nitrotetrazolate salt in the presence of a reducing agent. All the reactants are introduced into a continuous flow reactor system, which is composed of a temperature controlled tubular reactor and a mixer that allows for radial mixing. An optional stirred tank reactor may also be incorporated into the process to complete the reaction and allow for crystal growth.

Continuous manufacture of DBX-1

The present invention is directed to a method for preparing 5-nitrotetrazolate using a strongly acidic ionic cation exchange resin that has improve yields over prior art methods. The methods disclosed herein can be used either in a batch process or continuous flow reactor. In one exemplary process, starting material sodium 5-aminotetrazolate in solution is added into a reaction vessel containing a strongly acidic ionic cation exchange resin to facilitate production of 5-nitrotetrazolate. Multiple reactors containing resins may be connected in series to improve 5-nitrotetrazolate yields and purity levels.

Method for preparing sodium nitrotetrazolate using cation exchange resin

Described are methods of preparing silver azide comprising reacting a silver salt, an azide salt, ammonium hydroxide, and a hydrolysable ester at an elevated temperature.

Method for preparation of silver azide

Described are methods for preparing salts of 5-nitrotetrazolate that include reacting aqueous solutions of 5-aminotetrazole, an acid, and sodium nitrite in a continuous flow system at an ambient temperature.

Facile method for preparation of sodium 5-nitrotetrazolate using a flow system

Described are methods for preparing salts of 5-nitrotetrazolate that include reacting aqueous solutions of 5-aminotetrazole, an acid, and sodium nitrite in a continuous flow system at an elevated temperature.

Facile method for preparation of 5-nitrotetrazolates using a flow system

Described are methods for preparing salts of 5-nitrotetrazolate by reacting 5-aminotetrazole, an acid, and sodium nitrite in water in a batch reaction at an elevated temperature. As examples, the acid is nitric acid, sulfuric acid, perchloric acid, or hydrochloric acid, and the elevated temperature is at or above 65&#xb0; C.

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Phoenix, AZ, United States of America

Jon G Bragg