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Method for obtaining borazane, suitable for obtaining highly pure and very highly pure borazane

A kind of borane ammonia, non-solvent technology, applied in the field of obtaining borane ammonia containing low level, even very low level impurities

Inactive Publication Date: 2013-04-03
ARIANEGRP SAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the prior art never mentions the application of this method in the context of obtaining borazane ammonia of high purity

Method used

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  • Method for obtaining borazane, suitable for obtaining highly pure and very highly pure borazane
  • Method for obtaining borazane, suitable for obtaining highly pure and very highly pure borazane
  • Method for obtaining borazane, suitable for obtaining highly pure and very highly pure borazane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment I

[0073] a) Synthesis and removal of solids from the reaction medium

[0074] 288 g of ammonium carbonate and 4 liters of dry tetrahydrofuran (0.0005% in water) were introduced into a 4 liter reactor equipped with a stirring device and a condenser and placed under argon.

[0075] 112 g of sodium borohydride, which had been pretreated in an oven at 140° C. for 2 h, were introduced into this mixture.

[0076] The medium was stirred at 40 °C for 12 h.

[0077] Thereafter, the medium was filtered to remove unconsumed reagent and sodium carbonate formed.

[0078] b) Solvent evaporated

[0079] The obtained ammonium borane solution in tetrahydrofuran was introduced again into the reactor. The solvent (THF) was evaporated and the borane ammonia (product B) was subsequently recovered.

[0080] The thermogram of the borane ammonia is shown in Figure 1B. It involves exothermic decomposition in the solid state at low temperature (44°C). Its characteristics are described in Table 1 ab...

Embodiment II

[0083] a) Synthesis and removal of solids from the reaction medium

[0084] Step a) of Example I above was repeated.

[0085] b) Extraction with ether

[0086] The crude ammonium borane solid recovered after distilling off the THF was introduced into the Soxhlet extractor. Extraction was carried out by refluxing diethyl ether according to the teaching of application WO2007 / 106459. Extraction was performed at 35°C for 12h.

[0087] c) Solvent evaporated

[0088] After extraction, the ether was evaporated, and the borane ammonia was recovered and dried, and finally stored under an argon atmosphere.

[0089] The thermogram of the extracted ammonia borane (product C) is shown in Figure 1C. It includes exothermic decomposition in the solid state at a higher temperature than the exothermic decomposition of products A and B. Its characteristics are described in Table 1 above.

Embodiment 1

[0091] a) Synthesis and removal of solids from the reaction medium

[0092] Step a) of Example I above was repeated.

[0093] b) Purification according to the invention

[0094] The ammonium borane solution in tetrahydrofuran was introduced again into the reactor, followed by partial evaporation until 400 ml remained at the bottom of the vessel, ie 10% of the total amount of THF introduced at the beginning of the synthesis.

[0095] Then 2.5 liters of dry dichloromethane (0.005% water) were introduced into the reactor under vigorous stirring. Ammonia borane precipitated, which was then filtered and dried in an oven at 20° C. under vacuum for 12 h.

[0096] 70 g of borazane powder was recovered. Therefore, the yield of this method is greater than 70%.

[0097] The thermogram of described powder is shown in appendix Figure 2A , which includes exothermic decomposition in the solid state at a higher temperature than the exothermic decomposition of products A and B. Its char...

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Abstract

The invention relates to a method for obtaining borazane, suitable for obtaining borazane containing a low level of impurities. The borazane (obtained by reacting at least one ammonium salt with at least one borohydride of alkaline metal and / or alkaline earth) is dissolved in THF and selectively precipitated with a non-solvent. The precipitated borazane can be further purified by means of selective dissolution. The borazane obtained after selective precipitation and dissolution contains less than 1 mass-% impurities and / or does not demonstrate solid-state exothermic decomposition, with an endothermic melting peak temperature range above 110 DEG C.

Description

technical field [0001] The present invention relates to a process for obtaining borazane. More specifically, the subject of the invention is a process suitable for obtaining borane ammonia with low, even very low, levels of impurities. According to an advantageous variant, said method of obtaining consists of carrying out in succession the two given purification techniques, producing borane ammonia which, in its solid state before melting, does not show exothermic decomposition. Background technique [0002] The generation of hydrogen from solid compounds is one of the methods currently proposed for supplying fuel cells with hydrogen. [0003] Thus, the use of borane ammonia as a solid precursor in hydrogen production is known. [0004] In fact, the borane ammonia (chemical formula is BH 3 NH 3 ) was obtained as a white crystalline powder, showing a unique potential to contain 19.6 wt% hydrogen. Thus, ammonia borazine is positioned as a particularly interesting candidat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/08C01B35/14
CPCC01B35/14C01B35/146C01B35/08
Inventor 让-菲利普·古登若埃尔·勒努阿尔
Owner ARIANEGRP SAS
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