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Purification procedure dianhydrides and polyetherimides dianhydrides formed and formed from the same

机译:纯化方法形成的二酐和由其形成的聚醚酰亚胺二酐

摘要

Process for purifying a oxydiphthalic anhydride having the structure I, the process comprising the steps (a) to (f): ** ** Formula (a) providing a first mixture comprising at least one oxydiphthalic anhydride, at least one solvent, at least one catalyst and at least one inorganic salt selected from the group consisting of halide salts of alkali metal salts, alkaline earth metal halides and mixtures thereof, the oxydiphthalic anhydride being present in the first mixture in an amount of 10 to 30 weight percent based on the total weight of the first mixture; (B) diluting the first mixture with at least one solvent to provide a second mixture having a solids content of 10 to 30 percent based on the total weight of the second mixture; (C) filtering the second mixture at a temperature below the crystallization point of oxydiphthalic anhydride temperature and wash the solid with solvent to provide a mother liquor, a wash liquor and a third mixture of oxydiphthalic anhydride and salts; (D) hydrolyzing by adding (1) a water-soluble acid having a pKa less than or equal to the pKa of oxydiphthalic tetraacid and (2) water to the third mixture, forming a fourth mixture and heating the fourth mixture; wherein the fourth mixture is cooled to provide a solid-liquid mixture; filtering the solid-liquid mixture to provide a mother liquor and a solid component; and washing the solid component with water to provide wash liquor and a fifth mixture of oxydiphthalic tetraacid and water; and (e) closing the oxydiphthalic tetraacid ring heating the fifth mixture at a temperature and pressure sufficient to convert the oxydiphthalic tetraacid in the oxydiphthalic anhydride, forming a sixth mixture; and (f) filtering the sixth mixture to obtain substantially pure oxydiphthalic anhydride wherein said at least one solvent of step (b) is the mother liquor or wash liquor or mixtures thereof recycled from step (c) and obtained from a previous batch of first mixture.
机译:提纯具有结构I的氧二邻苯二甲酸酐的方法,该方法包括步骤(a)至(f):** **(a)提供包含至少一种氧二邻苯二甲酸酐,至少一种溶剂,至少一种溶剂的第一混合物。一种催化剂和至少一种选自碱金属盐的卤化物盐,碱土金属卤化物及其混合物的无机盐,第一混合物中的氧二邻苯二甲酸酐的含量为10至30重量%第一混合物的总重量; (B)用至少一种溶剂稀释第一混合物以提供第二混合物,其固体含量为第二混合物总重量的10%至30%; (C)在低于氧化二邻苯二甲酸酐温度的结晶点的温度下过滤第二混合物,并用溶剂洗涤固体,以提供母液,洗涤液以及氧化二邻苯二甲酸酐和盐的第三混合物; (D)通过向第三混合物中加入(1)pKa小于或等于对苯二甲酸二酸的pKa的水溶性酸和(2)水进行水解,形成第四混合物并加热第四混合物;其中将第四混合物冷却以提供固液混合物;过滤固液混合物以提供母液和固体成分;用水洗涤固体组分,以提供洗涤液和氧二邻苯二甲酸四酸与水的第五混合物; (e)在足以将所述氧二邻苯二甲酸四酸转化为氧二邻苯二甲酸酐的温度和压力下,将所述第五混合物加热的氧二邻苯二甲酸四酸环闭合,形成第六混合物; (f)过滤第六混合物以获得基本上纯的氧化二邻苯二甲酸酐,其中步骤(b)的所述至少一种溶剂是从步骤(c)回收的母液或洗涤液或它们的混合物,并且是从第一批第一混合物中获得的。 。

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