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CN103113344A 一种高纯度氟代碳酸乙烯酯的提纯方法 无效 - 驳回

一种高纯度氟代碳酸乙烯酯的提纯方法
摘要：
本发明为一种高纯度氟代碳酸乙烯酯的提纯方法，其特征在于：粗制氟代碳酸乙烯酯在蒸馏釜（3）内减压蒸馏，釜内压力为5~100 mmHg，导热油温度为60～180 oC，塔顶冷凝水（7）温度为30～70 oC，釜内蒸汽在冷凝器（5）内部分冷凝，轻组分作为不凝汽（8）从粗制产物内脱除，使得蒸馏釜（3）内氟代碳酸乙烯酯纯度达到99%以上；将蒸馏釜（3）内脱除轻组分的产物溶解在低沸点结晶溶剂中，所述结晶溶剂选自为甲苯、乙苯、正己烷、碳酸二甲酯、环己烷；在搅拌条件下降温至-20~15 oC，析出晶体，纯度高于99%；结晶产品通过真空干燥，脱除其中的结晶溶剂，得到纯度99.95%以上的精制氟代碳酸乙烯酯。
摘要（英）：

The invention relates to a purification method of high-purity fluoroethylene carbonate, which is characterized by comprising the following steps: carrying out vacuum distillation on rough fluoroethylene carbonate in a distillation kettle (3), wherein the kettle internal pressure is 5-100 mmHg, the temperature of the heat-conducting oil is 60-180 DEG C, the temperature of tower top condensation water (7) is 30-70 DEG C, steam in the kettle is partially condensed in a condenser (5), and light components are removed from the rough product as noncondensing steam (8), so that the purity of the fluoroethylene carbonate in the distillation kettle (3) is higher than 99%; dissolving the product without the light components in the distillation kettle (3) in a low-boiling-point crystallizing solvent, wherein the crystallizing solvent is selected from toluene, ethylbenzene, n-hexane, dimethyl carbonate and cyclohexane; under stirring conditions, cooling to -20-15 DEG C to precipitate crystals of which the purity is higher than 99%; and carrying out vacuum drying on the crystallizing product to remove the crystallizing solvent, thereby obtaining the refined fluoroethylene carbonate of which the purity is higher than 99.95%.

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