Sodium tert-butoxide and preparation method thereof
A technology of sodium tert-butoxide and tert-butanol, which is applied in the field of compound synthesis, can solve the problems of not reaching the melting temperature of metal sodium, increasing the stirring load of the reactor, and increasing the danger of the production process, etc., and achieves the improvement of reaction speed, Improve production efficiency and be conducive to the effect of safe production
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Embodiment 1
[0027] The invention provides a kind of preparation method of sodium tert-butoxide, specifically:
[0028] (1) Add 240 mL of heptane with a water content of 0.03% to the reactor, and then add sodium amide and tert-butanol with a molar mass ratio of 1:1.015, wherein the amount of sodium amide added is 9.8 g, and the amount of tert-butanol The amount of addition is 19g, stir well to make it dissolve completely, and obtain a mixed solution;
[0029] (2) The temperature of the mixed solution was raised to 70°C, and the reaction was carried out, and the ammonia gas released during the reaction was absorbed with water, and the heating was stopped after 2 hours of reaction to obtain the crude sodium tert-butoxide;
[0030] (3) Cool the crude sodium tert-butoxide product to normal temperature, distill off most of the reaction medium and the slightly excessive tert-butanol in the reaction under normal pressure, and then distill off the remaining small amount of reaction medium under re...
Embodiment 2
[0032] The invention provides a kind of preparation method of sodium tert-butoxide, specifically:
[0033] (1) Add 240 mL of heptane with a water content of 0.02% to the reactor, and then add sodium amide and tert-butanol with a molar mass ratio of 1:1.015, wherein the amount of sodium amide added is 0.25 mol, and the amount of tert-butanol The addition amount is 0.254mol, stir well to make it dissolve completely, and obtain a mixed solution;
[0034] (2) The temperature of the mixed solution was raised to 80°C, and the reaction was carried out. The ammonia gas released during the reaction was absorbed by lye, and the heating was stopped after 1.8 hours of reaction to obtain the crude sodium tert-butoxide;
[0035] (3) Cool the crude sodium tert-butoxide product to normal temperature, distill off most of the reaction medium and the slightly excessive tert-butanol in the reaction under normal pressure, and then distill off the remaining small amount of reaction medium under red...
Embodiment 3
[0037] The invention provides a kind of preparation method of sodium tert-butoxide, specifically:
[0038] (1) Add 240 mL of heptane with a water content of 0.01% to the reaction kettle, then add sodium amide and tert-butanol with a molar mass ratio of 1.015:1, stir thoroughly to dissolve completely, and obtain a mixed solution;
[0039] (2) The temperature of the mixed solution was raised to 100°C, and the reaction was carried out, and the ammonia gas released during the reaction was absorbed with water, and the heating was stopped after 1 hour of reaction to obtain the crude sodium tert-butoxide;
[0040] (3) Cool the crude sodium tert-butoxide product to normal temperature, distill off most of the reaction medium and the slightly excessive tert-butanol in the reaction under normal pressure, and then distill off the remaining small amount of reaction medium under reduced pressure to obtain 23.8 g of white solid Powder, the product content is 99.2% through acid-base titration...
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