Sodium tert-butoxide preparation process
A sodium tert-butoxide and preparation technology, applied in the field of compound synthesis, can solve the problems of reducing the reaction contact area, increasing the risk factor, and long time, so as to facilitate safe production, increase the contact area, and simplify the preparation process Effect
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Embodiment 1
[0027] The invention provides a kind of preparation technology of sodium tert-butoxide, comprising the following steps:
[0028] (1) Take a 1000ml reaction bottle as a reaction kettle, set a stirring device on the reaction kettle, a reflux condenser, a constant pressure dropping funnel, a thermometer and a nitrogen protection device, first add 500ml of o-xylene to the reaction kettle, o-xylene The water content of toluene is 0.04%, then open the nitrogen valve on the nitrogen protection device to regulate the flow of nitrogen;
[0029] (2) Add 23g of metal sodium block into the reaction kettle, then heat the reaction kettle, when the temperature of the reaction kettle rises to 105°C, turn on the stirring device, at this time, the sodium block melts to form sodium sand;
[0030] (3) Open the constant pressure dropping funnel and slowly add 81ml of tert-butanol to the reaction kettle dropwise, and increase the flow rate of nitrogen to fully drive away the hydrogen generated duri...
Embodiment 2
[0033] The invention provides a kind of preparation technology of sodium tert-butoxide, comprising the following steps:
[0034] (1) Take a 1000ml reaction bottle as a reaction kettle, set a stirring device on the reaction kettle, a reflux condenser, a constant pressure dropping funnel, a thermometer and a nitrogen protection device, first add 500ml of o-xylene to the reaction kettle, o-xylene The water content of toluene is 0.04%, then open the nitrogen valve on the nitrogen protection device to regulate the flow of nitrogen;
[0035] (2) Add 25.56g of metal sodium block into the reaction kettle, then heat the reaction kettle, when the temperature of the reaction kettle rises to 105°C, turn on the stirring device, at this time, the sodium block melts to form sodium sand;
[0036] (3) Open the constant pressure dropping funnel and slowly add 81ml of tert-butanol to the reaction kettle dropwise, and increase the flow rate of nitrogen to fully drive away the hydrogen generated d...
Embodiment 3
[0039] The invention provides a kind of preparation technology of sodium tert-butoxide, comprising the following steps:
[0040] (1) Take a 1000ml reaction bottle as a reaction kettle, set a stirring device on the reaction kettle, a reflux condenser, a constant pressure dropping funnel, a thermometer and a nitrogen protection device, first add 500ml of o-xylene to the reaction kettle, o-xylene The water content of toluene is 0.03%, then open the nitrogen valve on the nitrogen protection device to regulate the flow of nitrogen;
[0041] (2) Add 27.6g of metal sodium block into the reaction kettle, then heat the reaction kettle, when the temperature of the reaction kettle rises to 105°C, turn on the stirring device, at this time, the sodium block melts to form sodium sand;
[0042] (3) Open the constant pressure dropping funnel and slowly add 81ml of tert-butanol to the reaction kettle dropwise, and increase the flow rate of nitrogen to fully drive away the hydrogen generated du...
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