A kind of method for preparing sodium borohydride
A technology of sodium borohydride and preparation steps, which is applied in the field of preparation of hydrogen storage materials, can solve the problems of complex production process, high preparation cost of hydrogen storage materials, and difficulty in realizing industrialization development, and achieves simple and easily controllable reaction conditions and high yield. , to achieve the effect of industrialized production
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Embodiment 1
[0035] A. Add 7.5g of Na 2 B 4 o 7 Dissolve 3.0g of NaOH in 100mL of deionized water, evaporate the solution to dryness at 70 degrees Celsius to obtain 16.2g of precipitate, place it in a microwave oven, and heat it for 10 minutes to obtain 9.6g of NaBO 2 .
[0036] B. NaBO 2 Dissolved in 150mL of methanol solution, and then evaporated to dryness under negative pressure to obtain NaBO 2 with NaB(OCH 3 ) 4 The mixture was then repeatedly dissolved in methanol and evaporated to dryness under vacuum three times. The final precipitate was 20.4 g after drying and the yield was about 80%. The precipitate was dissolved in THF, centrifuged at a speed of 20,000 rpm, and the supernatant was removed to obtain NaB(OCH 3 ) 4 .
[0037] C. NaBH 4 Configured as a THF solution with a mass fraction of 10%. Take 5.0 g of the solution, together with 12.9 mmol of triethylsilane, and put them into a hydrothermal kettle, and the operation is performed in a glove box under an Ar atmosphe...
Embodiment 2
[0039] A, with embodiment 1;
[0040] B, with embodiment 1;
[0041] C. NaBH 4 Configured as a THF solution with a mass fraction of 10%. Take 5.0 g of this solution, together with 12.9 mmol of triethylsilane, and put them into a hydrothermal kettle, and the operation is carried out in a glove box under an Ar gas environment. Then the hydrothermal still is put into baking oven, is warming up to 150 degree with the speed of 5 degree Celsius / minute. Then the hydrothermal kettle was taken out, the precipitate was filtered out and washed three times with pentane, and dried to obtain NaBH 4 .
Embodiment 3
[0043] A, with embodiment 1;
[0044] B, with embodiment 1;
[0045] C. NaBH 4 Configured as a THF solution with a mass fraction of 10%. Take 5.0 g of this solution, together with 12.9 mmol of triethylsilane, and put them into a hydrothermal kettle, and the operation is carried out in a glove box under an Ar gas environment. Then the hydrothermal still is put into baking oven, is warming up to 200 degrees Celsius with the speed of 5 degrees Celsius / minute. Then the hydrothermal kettle was taken out, the precipitate was filtered out and washed three times with pentane, and dried to obtain NaBH 4 .
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