Synthesis method of fine-grained alpha-AlH3
A synthesis method and fine-grained technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve the problems of wide grain distribution, limited effect of reducing grain size, grain reduction, etc., and improve crystal quality. , the use of flexible equipment, the effect of reducing particle size
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Embodiment 1
[0048] Put the mixed solution of 800 ml ether and 800 ml toluene into a 5L four-neck flask, turn on the refrigerator and stir, lower the temperature of the mixed solution in the reaction bottle to about -10°C, and weigh 88g of AlCl 3 Add to the reaction flask in portions, making sure that the temperature does not rise sharply. Add a mixed solution of 2400ml ether and 600ml toluene to a 5L beaker, weigh 91g LiAlH 4 Add to the beaker in batches and stir.
[0049] will be dissolved with LiAlH 4 The mixed solution was added to a 1000 ml dropping funnel in batches, and added dropwise to the reaction flask. The rate of addition ensured that the temperature of the solution in the reaction flask was always kept at about -10°C-0°C. After ensuring the dropwise addition, continue to stir the reaction for 20 min. Stop stirring and let stand.
[0050] In a 10L four-necked crystallization flask, mechanical stirring, a penetrating ultrasonic generator, and a condensation collector were re...
Embodiment 2
[0054] Put the mixed solution of 800 ml ether and 800 ml toluene into a 5L four-neck flask, turn on the refrigerator and stir, lower the temperature of the mixed solution in the reaction bottle to about -10°C, and weigh 88g AlCl 3Add to the reaction flask in portions, making sure that the temperature does not rise sharply. Add 2400ml ether into a 5L beaker, weigh 91g LiAlH 4 Add to the beaker in batches and stir.
[0055] will be dissolved with LiAlH 4 The mixed solution was added to a 1000 ml dropping funnel in batches, and added dropwise to the reaction flask. The rate of addition ensured that the temperature of the solution in the reaction flask was always maintained at about -10°C-0°C. Make sure that after the dropwise addition, continue to stir the reaction for 20min. Stop stirring and let stand.
[0056] In a 10L four-necked crystallization flask, mechanical stirring, a penetrating ultrasonic generator, and a condensation collector were respectively installed, 6L of t...
Embodiment 3
[0060] Put the mixed solution of 900 ml ether and 800 ml toluene into a 5L four-neck flask, turn on the refrigerator and stir, lower the temperature of the mixed solution in the reaction bottle to about -10°C, and weigh 96g of AlCl 3 Add to the reaction flask in portions, making sure that the temperature does not rise sharply. Add a mixed solution of 2600ml ether and 600ml toluene into a 5L beaker, weigh 100g LiAlH 4 Add to the beaker in batches and stir.
[0061] will be dissolved with LiAlH 4 The mixed solution was added to a 1000 ml dropping funnel in batches, and added dropwise to the reaction flask. The rate of addition ensured that the temperature of the solution in the reaction flask was always maintained at about -10°C-0°C. After ensuring the dropwise addition, continue to stir the reaction for 20min. Stop stirring and let stand.
[0062] In a 10L four-necked crystallization flask, mechanical stirring, a penetrating ultrasonic generator, and a condensation collector...
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