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Title: Procedures for the synthesis of ethylenediamine bisborane and ammonia borane

Abstract

A method for synthesizing ammonia borane includes (a) preparing a reaction mixture in one or more solvents, the reaction mixture containing sodium borohydride, at least one ammonium salt, and ammonia; and (b) incubating the reaction mixture at temperatures between about 0.degree. C. to about room temperature in an ambient air environment under conditions sufficient to form ammonia borane. Methods for synthesizing ethylenediamine bisborane, and methods for dehydrogenation of ethylenediamine bisborane are also described.

Inventors:
; ; ;
Publication Date:
Research Org.:
PURDUE RESEARCH FOUNDATION, West Lafayette, IN (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1338064
Patent Number(s):
9,534,002
Application Number:
13/809,316
Assignee:
PURDUE RESEARCH FOUNDATION (West Lafayette, IN) GFO
DOE Contract Number:
FG36-06GO86050
Resource Type:
Patent
Resource Relation:
Patent File Date: 2011 Jul 06
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; 54 ENVIRONMENTAL SCIENCES

Citation Formats

Ramachandran, Padi Veeraraghavan, Gagare, Pravin D., Mistry, Hitesh, and Biswas, Bidyut. Procedures for the synthesis of ethylenediamine bisborane and ammonia borane. United States: N. p., 2017. Web.
Ramachandran, Padi Veeraraghavan, Gagare, Pravin D., Mistry, Hitesh, & Biswas, Bidyut. Procedures for the synthesis of ethylenediamine bisborane and ammonia borane. United States.
Ramachandran, Padi Veeraraghavan, Gagare, Pravin D., Mistry, Hitesh, and Biswas, Bidyut. Tue . "Procedures for the synthesis of ethylenediamine bisborane and ammonia borane". United States. doi:. https://www.osti.gov/servlets/purl/1338064.
@article{osti_1338064,
title = {Procedures for the synthesis of ethylenediamine bisborane and ammonia borane},
author = {Ramachandran, Padi Veeraraghavan and Gagare, Pravin D. and Mistry, Hitesh and Biswas, Bidyut},
abstractNote = {A method for synthesizing ammonia borane includes (a) preparing a reaction mixture in one or more solvents, the reaction mixture containing sodium borohydride, at least one ammonium salt, and ammonia; and (b) incubating the reaction mixture at temperatures between about 0.degree. C. to about room temperature in an ambient air environment under conditions sufficient to form ammonia borane. Methods for synthesizing ethylenediamine bisborane, and methods for dehydrogenation of ethylenediamine bisborane are also described.},
doi = {},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Tue Jan 03 00:00:00 EST 2017},
month = {Tue Jan 03 00:00:00 EST 2017}
}

Patent:

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  • The present invention discloses new methods for synthesizing ammonia borane (NH.sub.3BH.sub.3, or AB). Ammonium borohydride (NH.sub.4BH.sub.4) is formed from the reaction of borohydride salts and ammonium salts in liquid ammonia. Ammonium borohydride is decomposed in an ether-based solvent that yields AB at a near quantitative yield. The AB product shows promise as a chemical hydrogen storage material for fuel cell powered applications.
  • A method of releasing hydrogen from ammonia borane is disclosed. The method comprises heating an aqueous ammonia borane solution to between about 80-135.degree. C. at between about 14.7 and 200 pounds per square inch absolute (psia) to release hydrogen by hydrothermolysis.
  • Method of producing ammonia borane, comprising providing a reagent comprising a dehydrogenated material in a suitable solvent; and combining the reagent with a reducing agent comprising hydrazine, a hydrazine derivative, or combinations thereof, in a reaction which produces a mixture comprising ammonia borane.
  • Hydrogen ("H.sub.2") is produced when ammonia borane reacts with a catalyst complex of the formula L.sub.nM-X wherein M is a base metal such as iron, X is an anionic nitrogen- or phosphorus-based ligand or hydride, and L is a neutral ancillary ligand that is a neutral monodentate or polydentate ligand.
  • Liquid compositions of ammonia borane and a suitably chosen amine borane material were prepared and subjected to conditions suitable for their thermal decomposition in a closed system that resulted in hydrogen and a liquid reaction product.