Nanometer nitrogen hydride and in-situ preparation method and application thereof
An in-situ preparation and hydride technology, which is applied in the field of hydrogen storage materials and nanomaterials, can solve the problems of nitrogen hydride insolubility, less research on nitrogen hydride nanotechnology, and inapplicability, so as to prevent agglomeration and mild reaction conditions , the effect of controlling the particle size
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Embodiment 1
[0091] Preparation of nano-lithium amide: Add 2ml of butyllithium solution (2M) dropwise into a flask containing 70ml of n-hexane in an argon atmosphere glove box, inject ammonia gas into the flask under ultrasonication, and continue ultrasonication for 0.5h. During this process In, butyllithium (Li-C 4 h 9 ) absorb ammonia to form lithium amide (LiNH 2 ). Subsequently, the white powdery solid product was obtained by suction filtration, and the product was kept under dynamic vacuum for 30 minutes to remove residual organic molecules to obtain dry nano-lithium amide, and the product was stored in an argon atmosphere glove box.
[0092] Adopt XRD to carry out crystal structure analysis to the product of embodiment 1, test result is as follows figure 1 As shown, the diffraction peak of the sample synthesized in Example 1 is consistent with the standard PDF card of lithium amide, which shows that the sample synthesized in Example 1 is lithium amide. Adopt scanning electron mic...
Embodiment 2
[0094] Preparation of nano-lithium amide: Add 2ml of butyllithium solution (2M) dropwise into a flask containing 70ml of cyclohexane in an argon atmosphere glove box, feed ammonia gas into the flask while magnetically stirring, and continue stirring for 2h. During this process, butyllithium (Li-C4H9) slowly absorbs ammonia and gradually forms lithium amide (LiNH2), and the mixture in the flask gradually changes from a clear liquid to a white suspension. Subsequently, the white powdery solid product was separated by centrifugation, and the product was kept under dynamic vacuum for 30 minutes to remove residual organic molecules to obtain dry nano-lithium amide, and the product was stored in an argon atmosphere glove box.
Embodiment 3
[0096] Preparation of nano-lithium amide-lithium hydride (1:1) composite material: Add 2ml of butyllithium solution (2M) dropwise into a flask containing 70ml of n-hexane in an argon atmosphere glove box, pass ammonia gas into the flask and open Ultrasonic vibration, continuous ultrasonic 0.5h, during this process, butyllithium (Li-C 4 h 9 ) absorb ammonia gas and gradually form lithium amide (LiNH 2 ), the mixture in the flask gradually changed from a clear liquid to a white suspension. Subsequently, the mixture in the flask was put into a high-pressure reactor, 2ml of butyllithium solution (2M) was added to the mixture, after stirring evenly, 50bar high-purity hydrogen gas was introduced into the reactor, and the reactor was heated to 100°C. And keep warm for 24h. Subsequently, the powdery solid product was separated by suction filtration, and the product was kept under dynamic vacuum for 30 minutes to remove residual organic molecules to obtain a dry nanometer lithium am...
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