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CN101717406A 一种非水电解液用阻燃剂三（氟氧乙基）磷酸酯的精制方法 无效 - 撤回

一种非水电解液用阻燃剂三（氟氧乙基）磷酸酯的精制方法
摘要：
一种非水电解液用阻燃剂三(氟氧乙基)磷酸酯的精制方法，其特征在于：具有工艺步骤：1、加热水洗：搅拌的情况下，将纯度60％粗品三(氟氧乙基)磷酸酯缓缓倒入热蒸馏水中，搅拌一段时间，分离出油相三(氟氧乙基)磷酸酯；热蒸馏水温度70～85℃，水洗时间为20～40min，反复操作以上步骤，直到分离出的水相呈中性。2、减压蒸馏：加入精制添加剂选自无水氯化钙、无水硫酸镁、氧化钙其中一种，三(氟氧乙基)磷酸酯与精制添加剂的重量比为1∶0.005～1∶0.03，真空度为0.095MPa，取158～162℃段馏份，即为高纯低水份含量的三(氟氧乙基)磷酸酯产品。
摘要（英）：

The invention discloses a method for refining a tris(fluoroethoxy) phosphate flame retardant for a non-water electrolyte. The method is characterized by comprising the following steps: 1, heating and rinsing: slowly pouring a coarse tris(fluoroethoxy) phosphate product with a purity of 60 percent into hot distilled water under a condition of stirring, stirring the mixture for a certain period of time to separate the oil-phase tris(fluoroethoxy) phosphate, and under the conditions a temperature of the hot distilled water of 70 to 85 DEG C and a rinsing time of 20 to 40 minutes, repeatedly operating the previous steps till a water phase separated out is neutral; and 2, reduced pressure distillation: adding a refined additive which may be one of anhydrous calcium chloride, anhydrous magnesium sulfate or calcium oxide under the conditions of a weight ratio of tris(fluoroethoxy) phosphate to the refined additive of 1:0.005 to 1:0.03, a vacuum degree of 0.095MPa, and collecting a distillate at 158 to 162 DEG C to obtain the high-purity low-water-content tris(fluoroethoxy) phosphate product.

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