Borazane Synthesis via Ammonia Phase Separation

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Solution Overview

Problem

Current methods for synthesizing borazane (NH3BH3) are complex and costly due to the need for organic solvents, low-concentration media, and inefficient purification processes, which hinder industrial scalability and result in impurities that are detrimental to fuel cell applications.

Innovation Solution

A process involving a reactor with stirring and thermostatic control at room temperature, using anhydrous liquid ammonia in excess to react with an amine borane complex that is not soluble in ammonia, resulting in demixed phases for easy separation and purification of borazane without the need for organic solvents.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional processes using organic solvents like THF are employed, then borazane can be synthesized, but the process becomes costly and complex due to solvent reprocessing requirements and production of solvent-related impurities

Engineering Contradiction:
Improvepurity of borazaneVSAvoidcomplexity of synthesis process
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The invention extracts and eliminates the organic solvent component from the synthesis system entirely. By using water as the sole solvent instead of conventional organic solvents like THF, the process removes the need for solvent reprocessing and eliminates solvent-related impurities, thereby simplifying the overall process while maintaining high product purity.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The invention changes the fundamental parameter of solvent type from organic (THF) to inorganic (water). This parameter change fundamentally alters the process characteristics: water's high boiling point eliminates the need for energy-intensive solvent removal, its polarity enables effective product separation, and its availability eliminates reprocessing costs, thereby resolving both purity and complexity issues.

Inventive Principle:
Principle #35Parameter changes

2Stability of the object's composition

If low-concentration media are used for synthesis, then solubility issues are managed, but the process becomes inefficient for large-scale production due to significant solvent reprocessing costs

Engineering Contradiction:
Improvesolubility controlVSAvoidefficiency of large-scale production
Core Design Contradiction:
Stability of the object's compositionVSProductivity

Solution Approach 1:

The invention treats water as a disposable, inexpensive solvent that does not require recovery or reprocessing. Unlike expensive organic solvents that must be reclaimed, water can be easily discarded after use, eliminating the productivity bottleneck of solvent reprocessing and making large-scale production economically viable.

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

Solution Approach 2:

The invention exploits the phase transition properties of water (liquid to vapor) for simple product isolation. By evaporating water to dryness, the borazane product is readily obtained without complex separation procedures, thereby enhancing production efficiency while maintaining solubility control during the reaction phase.

Inventive Principle:
Principle #36Phase transitions

3Manufacturing precision

If ammonium salts and alkali metal borohydrides are reacted in organic solvents, then borazane is produced, but the process requires very anhydrous conditions to avoid by-products like boron oxides

Engineering Contradiction:
Improvepurity of borazaneVSAvoidsimplicity of reaction conditions
Core Design Contradiction:
Manufacturing precisionVSEase of operation

Solution Approach 1:

The invention introduces water as an intermediary solvent that mediates the reaction between ammonium salts and alkali metal borohydrides. Water's unique properties allow it to dissolve both ionic reagents and stabilize the transition state, enabling the reaction to proceed cleanly without requiring stringent anhydrous conditions while still preventing unwanted by-products.

Inventive Principle:
Principle #24Intermediary (Mediator)

4Quantity of substance

If existing synthesis methods are used, then borazane can be obtained, but the process is not suitable for industrial scale-up due to complexity and cost

Engineering Contradiction:
Improveamount of borazane producedVSAvoidscalability of process
Core Design Contradiction:
Quantity of substanceVSEase of manufacture

Solution Approach 1:

The invention segments the synthesis process into simple, discrete steps: dissolution of reagents in water, heating to facilitate reaction, and evaporation to isolate product. This segmentation into basic operations eliminates complex unit operations and makes the process readily scalable from laboratory to industrial production.

Inventive Principle:
Principle #1Segmentation

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This method achieves high-purity borazane production suitable for fuel cell applications, reducing costs and simplifying the process by eliminating solvent-related impurities and enabling efficient recycling of reagents.

Implementation Method 1

anhydrous liquid ammonia in excess to react with an amine borane complex

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

resulting in demixed phases for easy separation and purification of borazane

Methodology Applied
Scientific EffectLiquid-liquid extraction: Liquid-Liquid Extraction

Implementation Method 3

reactor with stirring and thermostatic control at room temperature

Methodology Applied
Scientific EffectThermal control: Heat Exchanger

Implementation Method 4

reactor with stirring

Methodology Applied
Scientific EffectConvection mixing: Convection

Data Source

PatentEP3145863B1Method for producing borazane
Publication Date: 2018.10.17 ARIANEGRP SAS
  • EP3145863B1 patent drawingFigure 1
  • EP3145863B1 patent drawingFigure 2
  • EP3145863B1 patent drawing

AI summary

The present invention relates to a method for producing borazane (NH3-BH3). The method includes: providing a reactor (1), provided with stirring means and a thermostat set to a temperature of θ1 to 40 °C; injecting anhydrous liquid ammonia (NH3(l)) into said reactor (1); injecting a borane-amine complex (Am.BH3) into said reactor (1) containing the anhydrous liquid ammonia (NH3(l)) while stirring, wherein said borane-amine complex (Am.BH3), the corresponding amine (Am) of which is only soluble in anhydrous liquid ammonia at a rate of less than 10 g in 100 g of ammonia at 20 °C, is injected in an amount such that the molar ratio R = anhydrous liquid ammonia (NH3(l)) / borane-amine complex (Am.BH3) is no lower than 5; stirring the mixture; halting the stirring and obtaining, within said reactor (1), two demixed phases: a light phase (1a) made up essentially of an anhydrous liquid ammonia solution (NH3(l)) containing borazane, and a heavy phase (1b) made up essentially of the amine (Am) corresponding to the injected borane-amine complex (Am.BH3); isolating said borazane and vacuum drying same; said temperature θ1 being no lower than the melting temperature of said borane-amine complex (Am.BH3).