重结晶提纯碳酸二苯酯的溶剂选择

为了寻找重结晶法提纯碳酸二苯酯(DPC)的适宜溶剂,文章对DPC重结晶溶剂的选择及影响DPC纯度的因素进行了研究。结果表明:乙醇是重结晶纯化DPC的适宜溶剂,DPC在乙醇中溶解度在5—15℃的区间内变化缓慢,重结晶中止温度在15℃左右,DPC的收率高于89.0%。乙醇和DPC比率(质量比)采用8∶5为重结晶DPC时的适宜比率。通过对重结晶溶剂的进一步研究,发现采用水-乙醇的混合溶剂作为重结晶溶剂时,可以明显提高DPC的收率。水的质量分数在25.0%—35.0%范围内时,DPC的收率大于93.0%,纯度高于99.6%。其纯度符合合成聚碳酸酯的要求。

Solvents selection of the recrystallization for purification of diphenyl carbonate

In order to look for the feasible recrystallization solvents for purification diphenyl carbonate,solvents selection and effect factors for the recrystallization of diphenyl carbonate were studied.The results show that ethanol is the optimal solvent to recrystallize diphenyl carbonate,the solubility of diphenyl carbonate(DPC) in ethanol changed slowly in the recrystallization temperature range between 5 ℃ and 15 ℃.The yield of DPC is as high as 89.0% at the recrystallization temperature of 15 ℃.The optimum ratio of ethanol to DPC is about 8 ∶5(mass ratio).The yield of DPC can be obviously improved in the case of a mixture of water and ethanol used as the recrystallization solvent.The yield of DPC is higher than 93.0% and the purity of product is 99.6 % when the mass fraction of water varies between 25.0% and 35.0%.The purity of DPC accords with the demand of polycarbonate synthesis.