β‑h-containing secondary amino metal organic compound and its preparation and application
A secondary amine-based metal and organic compound technology, applied in magnesium organic compounds, calcium organic compounds, lithium organic compounds, etc., can solve problems such as high-density storage problems, and achieve the effects of easy operation and control, rich varieties, and convenient materials.
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Embodiment 1
[0092] In a glove box filled with high-purity argon, measure 1 ml of ethylenediamine liquid in a high-pressure reactor, add 30 ml of tetrahydrofuran as a solvent; remove the surface layer of lithium strips, expose the fresh surface, cut into small pieces, and weigh 0.1 gram of lithium metal, the flake metal lithium is placed on the sample holder installed in the high-pressure reactor, and the reactor is sealed after being protected by argon. Connect to the pressure recording device, use mechanical stirring to make the metal lithium flakes fall into the tetrahydrofuran solution of ethylenediamine, and react, the stirring speed is 200 rpm, the stirring temperature is room temperature, and the stirring time is 4 hours. A blue solution was obtained after the reaction was complete. The solvent was removed from this solution by distillation under reduced pressure to obtain a solid powder product. The X-ray diffraction pattern of the product is as figure 1 As shown, only the diffra...
Embodiment 2
[0094] In a glove box filled with high-purity argon, measure 1 ml of benzylamine liquid in a ball mill jar; weigh 0.07 g of lithium hydride, press it into a disc with a diameter of about 1 cm with a manual tablet press, and place the lithium hydride disc The slices were placed on the sample holder installed on the ball mill tank, protected by argon, and ball milled on a planetary ball mill with a ball-to-material ratio of 50:1, a speed of 200 rpm, and a ball milling time of 36 hours at room temperature. Under the condition of cutting off the air, take the above-mentioned ball mill product, and burn it at 100 degrees Celsius for 24 hours. The X-ray diffraction pattern of the product is obtained as Figure 4 As shown, there are only diffraction peaks of the new substance in the solid reaction product, and the existence of the raw material is not seen, indicating that the reaction is carried out completely and there is no reactant remaining. Product (C 6 h 5 )CH 2 The tempera...
Embodiment 3
[0096] In a glove box filled with high-purity argon, measure 1 ml of ethylenediamine liquid in a ball mill jar; weigh 0.24 g of lithium hydride, press it into a disc with a diameter of about 1 cm with a manual tablet press, and place the lithium hydride disc The slices were placed on the sample holder installed on the ball mill jar, protected by argon, and mixed by ball milling on a planetary ball mill. In 36 hours, the product ethylenediamine dilithium (LiNHCH 2 CH 2 NHLi), its X-ray diffraction pattern is as Figure 7 shown.
[0097] In a glove box filled with high-purity argon, weigh 0.5 g of dilithium ethylenediamine and 0.66 g of magnesium chloride in a ball mill jar, and use argon protection to ball mill and mix them on a planetary ball mill with a ball-to-material ratio of 100:1. The rotating speed is 200 rpm, the ball milling temperature is room temperature, and the ball milling time is 10 hours. After the reaction was completed, the ball mill tank was opened in th...
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