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机构地区:[1]黑龙江省石油化学研究院,黑龙江哈尔滨150040
出 处:《化学与粘合》2007年第2期111-112,共2页Chemistry and Adhesion
摘 要:对采用丙酸或丁酸水溶液作溶剂处理粗3,3,’4,4’-二苯醚四甲酸二酐(简称ODPA),生成3,3,’4,4’-二苯醚四甲酸(简称ODTA),然后脱水成酐和在不同有机溶剂中利用活性炭脱色,以及升华后再进行重结晶等三种方法进行对比,考查了这三种方法提纯3,3,’4,4’-二苯醚四甲酸二酐(简称ODPA)的效果。着重介绍了ODPA在较高真空下进行升华,然后升华产物与过量的乙酸酐混合回流1h以上,冷却、静置结晶、分离、干燥后得到高纯度的ODPA。该方法得到的最终产品为白色粉末晶体,纯度≥99.0%,熔点227-230℃。The comparison of three methods for purifying ODPA is carried out. The three methods are as follows: (A) ODTA is prepared after the treatment of crude ODPA with propionic acid and butyric acid aqueous solution, and then the ODTA is dehydrated to obtain ODPA. (B) Crude ODPA is discolored by active carbon in different organic solution. (C) Recrystal after sublimation of crude ODPA. The effect of these three methods is investigated. The third method is detailed. ODPA is sublimated under the condition of vacuum, and then the product is mixed with acetic anhydride and refluxed for over 1 h. After the processes of cool down ; crystallization, separation and desiccation, the ODPA with high purity is obtained. With this technique, the final product is white powder crystal, its purity is higher than 99.0% and its melting point is between 227 to 230℃.
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