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Synthesis method of boron hydride [NH3BH2NH3]B3H8

A technology of borohydride compounds and synthesis methods, which is applied in the field of synthesis of borohydride compounds, can solve problems such as cumbersome synthesis steps, and achieve the effect of simple operation

Inactive Publication Date: 2017-12-01
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reported synthesis of [NH 3 BH 2 NH 3 ]B 3 h 8 The method mainly utilizes metathesis reaction, [NH 3 BH 2 NH 3 ]Cl and NaB 3 h 8 prepared by the reaction, where [NH 3 BH 2 NH 3 ]Cl and NaB 3 h 8 To be prepared separately in the laboratory, and the synthesis steps are cumbersome

Method used

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  • Synthesis method of boron hydride [NH3BH2NH3]B3H8

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Experimental program
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Effect test

Embodiment 1

[0016] All manipulations were performed under nitrogen atmosphere. In the glove box, add 0.31 g of ammonia borane to the 100 mL schlenk reaction bottle equipped with a magnet, seal the schlenk reaction bottle with a stopper, and then remove the schlenk reaction bottle from the glove box, and then add 50 mL of B with a molar concentration of 0.1 mol / L 3 h 7 Tetrahydrofuran solution in THF·B 3 h 7 , stirred at room temperature for 8 hours, filtered to remove insoluble matter, concentrated the filtrate to remove the solvent to obtain a white sticky solid, then washed the solid with toluene 3 times, 20 mL each time, then concentrated in vacuo to remove the solvent to obtain a white solid product, which is borohydride [ NH 3 BH 2 NH 3 ]B 3 h 8 , the resulting [NH 3 BH 2 NH 3 ]B 3 h 8 Weighing 0.36g, the calculated yield is 82%, and its purity is close to 100% in nuclear magnetic detection.

Embodiment 2

[0018] All manipulations were performed under nitrogen atmosphere. In the glove box, add 0.31 g of ammonia borane to a 100 mL schlenk reaction bottle equipped with a magnet, seal the schlenk reaction bottle with a stopper, then remove the schlenk reaction bottle from the glove box, and then add 5 mL of B with a molar concentration of 1 mol / L 3 h 7 Tetrahydrofuran solution in THF·B 3 h 7, stirred at 0°C for 12 hours, filtered to remove insoluble matter, concentrated the filtrate to remove the solvent to obtain a white sticky solid, then washed the solid with toluene 3 times, 20 mL each time, then concentrated in vacuo to remove the solvent to obtain a white solid product, which is borohydride [NH 3 BH 2 NH 3 ]B 3 h 8 , the resulting [NH 3 BH 2 NH 3 ]B 3 h 8 Weighing is 0.35g, the calculated yield is 80%, and its purity is close to 100% in nuclear magnetic detection.

Embodiment 3

[0020] All manipulations were performed under nitrogen atmosphere. In the glove box, add 0.15 g of ammonia borane to a 100 mL schlenk reaction bottle equipped with a magnet, seal the schlenk reaction bottle with a stopper, and then remove the schlenk reaction bottle from the glove box, and then add 10 mL of B with a molar concentration of 0.5 mol / L 3 h 7 Tetrahydrofuran solution in THF·B 3 h 7 , stirred at room temperature for 6 h, filtered to remove insoluble matter, concentrated the filtrate to remove the solvent to obtain a white sticky solid, then washed the solid with toluene 3 times, 20 mL each time, then concentrated in vacuo to remove the solvent to obtain a white solid product, which is borohydride [ NH 3 BH 2 NH 3 ]B 3 h 8 , the resulting [NH 3 BH 2 NH 3 ]B 3 h 8 Weighing 0.36g, the calculated yield is 82%, and its purity is close to 100% in nuclear magnetic detection.

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Abstract

The invention discloses a synthesis method of boron hydride [NH3BH2NH3]B3H8 and belongs to the technical field of synthesis of boron hydride. The technical scheme is characterized in that ammonia borane is added to a reaction container under waterless and oxygen-free conditions, a tetrahydrofuran solution THF.B3H7 of B3H7 is added and stirred at the temperature of 0-50 DEG C for a reaction, and the target product boron hydride [NH3BH2NH3]B3H8 is prepared. The method is simple to operate, low-toxicity, harmless, safe, reliable and suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of synthesis of borohydride compounds, in particular to a borohydride compound [NH 3 BH 2 NH 3 ]B 3 h 8 synthetic method. Background technique [0002] Negative ion B 3 h 8 - It has a wide range of uses. Due to its high hydrogen content, it has great application prospects in the field of hydrogen storage, such as the synthesized hydrogen storage material NH 4 [B 3 h 8 ] (Inorg. Chem. 2011, 50, 3738-3742), [NH 3 BH 2 NH 3 ]B 3 h 8 (RSC Adv. 2013, 3, 7460-7465), contains a large amount of negative hydrogen; and has good solubility in common organic solvents, so it can be used as a reducing agent; and can be used as a precursor for the synthesis of other boron-containing compounds substances, such as the synthetic semiconductor material MgB 2 The precursor of Mg(B 3 h 8 ) 2 (Inorg. Chem. 2007, 46, 9060-9066). [0003] Due to the limitations of the synthesis method, the B of metal cations and...

Claims

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Application Information

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IPC IPC(8): C01B35/02
Inventor 陈学年冯笑阁陈西孟刘新冉李书军张絜
Owner HENAN NORMAL UNIV
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