Method for preparing carbonic acid glyceride by catalytic reaction-azeotropic reification coupling
A technology of glycerol carbonate and azeotropic distillation, which is applied in the preparation of organic carbonates and organic chemistry, can solve the problems of complicated treatment process, large amount of dimethyl carbonate, and poisonous carbon monoxide, so as to achieve simple purification process and save use quantity, beneficial to the effect of recycling
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Embodiment 1
[0027] Example 1: Take 0.1 mole of glycerin, 0.1 mole of dimethyl carbonate, 10.65 g of ethyl acetate and 0.224 g of calcium oxide and add them to the reaction kettle at the bottom of the tower, heat the bottom of the tower while stirring, and open the condenser at the top of the tower. When the temperature of the tower bottom is 67°C and the top of the tower is 58°C, start to extract the overhead distillate under the condition of the reflux ratio of 4, react for 1 hour, the temperature of the bottom of the tower reaches 91°C, and the temperature of the top of the tower reaches 61°C. React, stop heating, turn off condensed water. Take out the reaction product in the reaction kettle at the bottom of the tower, filter to remove the solid alkali catalyst, evaporate and remove the constant boiling agent in a vacuum, and obtain the glycerol carbonate product, the yield of glycerol carbonate is 86.5%, and the concentration of glycerol carbonate in the product is 85.0%.
Embodiment 2
[0028] Example 2: Take 0.1 mole of glycerin, 0.1 mole of dimethyl carbonate, 17.58 g of n-hexane and 0.224 g of calcium hydroxide and add them to the reaction kettle at the bottom of the tower, heat the tower kettle while stirring, and open the condenser at the top of the tower. When the temperature of the tower bottom is 63°C and the top of the tower is 54°C, start to extract the overhead distillate under the condition of reflux ratio of 4, react for 0.8h, the temperature of the bottom of the tower reaches 90°C, and the temperature of the top of the tower reaches 56°C, at this time End the reaction, stop heating, turn off the condensed water. Take out the reaction product in the reaction kettle at the bottom of the tower, filter to remove the solid alkali catalyst, and evaporate the constant boiling agent in a vacuum to obtain a glycerol carbonate product with a glycerol carbonate yield of 92.5% and a glycerol carbonate concentration of 90.0% in the product.
Embodiment 3
[0029]Embodiment 3: Get 0.1 mole of glycerin, 0.1 mole of dimethyl carbonate, 10.02g of dichloroethane and 0.112g of calcium oxide and join in the reaction kettle at the bottom of the tower, heat the tower kettle, stir simultaneously, open the condenser at the top of the tower, when the tower When the temperature of the still was 65°C and the top of the tower was 60°C, the overhead distillate was extracted under the condition of a reflux ratio of 4. After 0.5h of reaction, the temperature of the bottom of the tower reached 100°C and the temperature of the top of the tower reached 66°C. At this point, the reaction was terminated, the heating was stopped, and the condensed water was turned off. Take out the reaction product in the reaction kettle at the bottom of the tower, filter to remove the solid alkali catalyst, evaporate and remove the constant boiling agent in vacuo, and obtain the glycerol carbonate product, the yield of glycerol carbonate is 97.2%, and the concentration ...
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