Thiokol Corporation

Morton Thiokol Inc.

Michael L Levinthal

Rodney L Willer

Dennis J Park

Ronnelle Bridges

Larry W Poulter

Gale F Allred

Charles L Denton

David W Endicott, Jr

The present invention concerns a method for making energetic oxidizer salts and solutions thereof, and in particular relates to processes for making aqueous solutions of hydroxylammonium nitrate in high purity suitable for use in making liquid gun propellants. The present alcohol-free process yields high purity alcohol-free hydroxylammonium nitrate by neutralizing an aqueous nitric acid solution (20-70% wt./wt.) with an alcohol-free aqueous hydroxylamine solution at temperatures ranging from above -50.degree. C. to substantially less than ambient (20.degree. C.) to produce the desired alcohol-free aqueous hydroxylammonium nitrate solution in a usable concentration and in high purity. The process is economical, environmentally acceptable, and facile.

Method of making hydroxyamine and products therefrom

The present invention pertains to a method for making energetic oxidizer salts and solutions thereof, and in particular relates to processes for making aqueous solutions of hydroxylammonium nitrate in high purity suitable for use in making liquid gun propellants. The present alcohol-free process yields high purity alcohol-free hydroxylammonium nitrate in a simple chemical neutralization reaction by combining an aqueous nitric acid solution 120 to 70 wt. %) with an alcohol-free aqueous hydroxylamine solution at temperatures ranging from about -50.degree. C. to above ambient to produce the desired alcohol-free aqueous hydroxylammonium nitrate solution in a usable concentration and in high purity. The process is economical, environmentally acceptable, and facile.

Process for making high purity hydroxylammonium nitrate

Recovery of sulfuric and nitric acids from spent acid streams in a process for producing beta HMX in which hexamine, ammonia and acetic anhydride are reacted to produce DAPT, the DAPT is treated with a mixture of sulfuric and nitric acids to produce DADN which is then nitrolyzed with N.sub.2 O.sub.5 and anhydrous nitric acid to produce a HMX solution which is added to a dispersion of beta HMX seed crystals in water to selectively precipitate beta HMX from the HMX solution is accomplished by maintaining the DAPT/DADN spent acid stream separate from the HMX spent acid stream and treating the DAPT/DADN spent acid stream in a sulfuric acid recovery unit and treating the HMX spent acid stream in a magnesium nitrate nitric acid recovery unit.

Recovery of nitric acid and sulfuric acids in production of beta HMX

Method of directly precipitating substantially pure beta HMX from a substantially anhydrous nitric acid solution without forming and recrystallizing polymorphic HMX. HMX dissolved in a solvent consisting essentially of anhydrous nitric acid is added to water which is seeded with crystals of beta HMX to substantially completely precipitate all the HMX from solution as beta HMX without forming crystals of the other polymorphic forms of HMX. A preferred reaction and apparatus for preparing HMX in anhydrous nitric acid is also disclosed.

Crystallization of beta HMX

Improved process for manufacturing an explosive eutectic composition comprising about 46% by weight ammonium nitrate, about 46% by weight ethylene diamine dinatrate, and about 8% by weight potassium nitrate. First, potassium hydroxide, ammonia, water, nitric acid, and ethylene diamine are reacted in aqueous solution to produce the indicated components of the eutectic mixture. Then the solution is cooled to supersaturate each solute thereof and passed through a continuous crystallizer to crystallize the components of the product in eutectic proportions. The product is then separated from the mother liquor, which is recycled. The process can be operated continuously and safely without producing by-products or employing solvents which must be evaporated from the composition or disposed of.

Process for simultaneously crystallizing components of EAK explosive

A process for the separation of nitroglycerin from mixtures of nitroglycerin and diethylene glycol diluent which avoids the presence of undiluted nitroglycerin is disclosed. The process avoids the hazards inherent in handling undiluted nitroglycerin.

Process for separation of nitroglycerin from mixtures with diethylene

Crystals of cyclotetramethylenetetranitramine (HMX) are dissolved in a suitable solvent, as are crystals of ammonium perchlorate. The two solutions are then mixed thoroughly and desiccated. This produces cocrystals of HMX and ammonium perchlorate that may be used as an oxidizer in rocket propellant, pyrotechnic materials, or in gas generators. Stoichiometric proportions are 50 parts of HMX to 30 parts of ammonium perchlorate.

Propellant made with cocrystals of cyclotetramethylenetetranitramine and

A method of making finely particulate ammonium perchlorate which comprises establishing a two-phase liquid system in which the upper phase is a concentrated solution of ammonium perchlorate and the lower phase is a liquid which is immiscible with the upper phase solvent and a non-solvent for ammonium perchlorate. Precipitation of ammonium perchlorate from the solution into the non-solvent is effected by either cooling the solution or evaporating the solvent thereof while subjecting the system to ultra-sonic vibrations. Fine ammonium perchlorate particles collect in the non-solvent phase and are recovered therefrom.

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Marshall, TX, United States of America

Michael L Levinthal