A kind of treatment method of magnesium shavings for Grignard reaction
A treatment method, Grignard reaction technology, applied in the direction of magnesium organic compounds, etc., to achieve the effect of wide application range, reduce labor intensity and material consumption, and the method is simple and practical
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Embodiment 1
[0020] Weigh 0.5kg of magnesium chips and add it to a pulverizer with a material hopper volume of 2L, cover the upper cover, switch on the power supply of the motor, and divide it into 3 times at high speed (3000-3500 rpm) (10 seconds for the first crushing, 10 seconds for the second crushing). 20 seconds for the first crushing, 20 seconds for the third crushing) intermittent crushing, the interval between each crushing is 7 seconds, after the last crushing is completed, turn off the motor, open the upper cover, and quickly pour the processed magnesium chips into the cleaned and dried The bag was quickly transferred to the reaction kettle through the funnel. Close the valve, start the vacuum pump to evacuate the reactor to -0.1Mpa, and fill the reactor with nitrogen to make the pressure reach the normal air pressure outside. Put 3kg of tetrahydrofuran into the reaction kettle from a high position, raise the temperature of the interlayer of the reaction kettle through hot water...
Embodiment 2
[0022] Take by weighing 1.7kg of magnesium chips and add it to the pulverizer with a material hopper volume of 4L, cover the upper cover, connect the power supply of the motor, and divide it into 4 times at high speed (2700-3500 rpm) (the first pulverization takes 10 seconds, the second 15 seconds for the first crushing, 20 seconds for the third crushing, 20 seconds for the fourth crushing) intermittent crushing, the interval between each crushing is 10 seconds, after the last crushing is completed, turn off the motor, open the upper cover, and quickly dispose of the processed magnesium chips Pour it into the cleaned and dried bag at one time, and quickly transfer it to the reaction kettle through the funnel. Close the valve, start the vacuum pump to evacuate the reactor to -0.1Mpa, and fill the reactor with nitrogen to make the pressure reach the normal air pressure outside. Put 10kg of tetrahydrofuran into the reaction kettle from a high position, raise the temperature of th...
Embodiment 3
[0024] Weigh 6kg of magnesium scraps and add it to the pulverizer with a material hopper volume of 10L, cover the upper cover, connect the power supply of the motor, and divide it into 5 times at high speed (3000-3500 rpm) (10 seconds for the first time, 10 seconds for the second time) 15 seconds for crushing, 20 seconds for the third crushing, 15 seconds for the fourth crushing, 20 seconds for the fifth crushing) Intermittent crushing, the interval between each crushing is 6-8 seconds, after the last crushing is completed, turn off the motor and open the upper cover , quickly pour the processed magnesium chips into the cleaned and dried bag, and quickly transfer it to the reaction kettle through the funnel. Close the valve, start the vacuum pump to evacuate the reactor to -0.1Mpa, and fill the reactor with nitrogen to make the pressure reach the normal air pressure outside. Put 30kg of tetrahydrofuran into the reaction kettle from a high position, raise the temperature of the...
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