The present invention provides a method for preparing relatively insoluble bisimides under conditions which afford high imidization reaction rates and which permit the monitoring and adjustment of reactant stoichiometry at any stage of the reaction. The bisimides provided by the present invention are prepared either by reaction of a diamine such as 4,4′-diaminodiphenylsulfone (DDS) with an anhydride, for example 3-chlorophthalic anhydride (3-ClPA) in the presence of a solvent at a pressure greater than one atmosphere and at a temperature above the normal boiling point of the solvent, or by reaction of a monoamine with a dianhydride under the same conditions. In one embodiment, the relatively insoluble product bisimides provided by the present invention have a solubility in ortho-dichlorobenzene of less than about 10 percent by weight at a temperature of about 180° C.
本发明提供了一种制备相对不溶性双亚
酰亚胺的方法,该方法在条件下提供高
咪唑化反应速率,并允许在反应的任何阶段监测和调整反应物的
化学计量。本发明提供的双亚
酰亚胺可以通过在溶剂存在下、压力大于一大气压且温度高于溶剂的正常沸点的条件下,例如将二胺(如4,4′-二
氨基二苯基砜(
DDS))与酸酐(例如3-
氯邻苯二酐(3-ClPA))反应,或者将一胺与二酐在相同条件下反应来制备。在一个实施例中,本发明提供的相对不溶性产物双亚
酰亚胺在约180°C时在
邻二氯苯中的溶解度重量百分比小于约10%。