Non-solvated alpha-aluminum hydride and preparation method thereof
A non-solvated, aluminum hydride technology, applied in chemical instruments and methods, metal hydrides, inorganic chemistry, etc., can solve the problems of complex synthesis conditions, high equipment requirements, difficult preparation, etc., and achieve mild preparation conditions and product purity. High, easy-to-use effects
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Embodiment 1
[0041] Disperse 0.033g of anhydrous aluminum trichloride and 0.028g of lithium aluminum hydride in 30ml of dehydrated ethylene glycol, and stir at 60°C for 15 minutes to dissolve as much as possible to form a white suspension. The resulting suspension was transferred to a 50 mL airtight reactor, and the airtight reactor was placed in an oven at 100° C. for 8 hours, and then the airtight reactor was taken out and cooled naturally in the air. The cooled suspension was transferred to a 50 mL centrifuge tube and centrifuged at 8000 rpm for 20 min, and the supernatant was removed. Then use 20mL of anhydrous acetone to disperse the sediment at the bottom of the centrifuge tube. After the dispersion is as uniform as possible, centrifuge at 8000rpm for 5min, remove the supernatant, and repeat this operation once. The final precipitate is dried in a vacuum oven to obtain the product. attached figure 1 is the X-ray diffraction pattern of the sample prepared in this embodiment.
Embodiment 2
[0043] Disperse 0.027g of polyvinylpyrrolidone (PVP, protective agent), 0.033g of anhydrous aluminum trichloride and 0.028g of lithium aluminum hydride in 30ml of dehydrated ethylene glycol, and stir at 60°C for 15 minutes to make it fully May dissolve, forming a white suspension. The resulting suspension was transferred to a 50 mL airtight reactor, and the airtight reactor was placed in an oven at 100° C. for 10 hours, and then the airtight reactor was taken out and cooled naturally in the air. The cooled suspension was transferred to a 50 mL centrifuge tube and centrifuged at 8000 rpm for 20 min, and the supernatant was removed. Then use 20mL of anhydrous acetone to disperse the sediment at the bottom of the centrifuge tube. After the dispersion is as uniform as possible, centrifuge at 8000rpm for 5min, remove the supernatant, and repeat this operation once. The final precipitate is dried in a vacuum oven to obtain the product. attached figure 2 is the X-ray diffraction ...
Embodiment 3
[0045] Disperse 0.033g of anhydrous aluminum trichloride and 0.028g of lithium aluminum hydride in 30ml of dehydrated ethylene glycol, and stir at 60°C for 15 minutes to dissolve as much as possible to form a white suspension. The resulting suspension was transferred to a 50 mL airtight reactor, and the airtight reactor was placed in an oven at 120° C. for 4 hours, and then the airtight reactor was taken out and cooled naturally in the air. The cooled suspension was transferred to a 50 mL centrifuge tube and centrifuged at 8000 rpm for 20 min, and the supernatant was removed. Then use 20mL of anhydrous acetone to disperse the sediment at the bottom of the centrifuge tube. After the dispersion is as uniform as possible, centrifuge at 8000rpm for 5min, remove the supernatant, and repeat this operation once. The final precipitate is dried in a vacuum oven to obtain the product. attached image 3 is the X-ray diffraction pattern of the sample prepared in this embodiment.
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Abstract
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