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    • 10. 发明授权
    • Two-stage solution polymerization of high molecular weight
poly(phosphoesters)
    • 高分子量聚(磷酸酯)的两阶段溶液聚合
    • US6008318A
    • 1999-12-28
    • US98620
    • 1998-06-17
    • Zhong ZhaoHai-quan MaoKam W. Leong
    • Zhong ZhaoHai-quan MaoKam W. Leong
    • C08G79/04C08G79/02
    • C08G79/04
    • A process for making a phosphoester polymer comprising the recurring monomeric units of formula I: ##STR1## wherein: X is --O-- or --NR"--, where R" is H or alkyl;L is a divalent organic moiety;R' is H, alkyl, alkoxy, aryl, aryloxy, heterocyclic, or heterocycloxy; andn is between about 25 to 2,000,is described. The process comprises the steps of:(a) polymerizing in the presence of a solvent p moles of a di-XH compound having formula II:H--X--L--X--H II wherein X and L are as defined above, with q moles, where p.apprxeq.q, of a phosphorodihalo compound to form a polymer of formula I, wherein n is about 12 to 1000, having a first molecular weight Mw.sub.1, wherein the solvent is present in an amount greater than about 5 ml of solvent per gram of compound of formula II;(b) removing at least about 25% of the solvent to form a more concentrated reaction mixture; and(c) further polymerizing the concentrated reaction mixture for an additional time sufficient to produce a polymer of formula I wherein n is between about 25 and 2,000, the polymer having a second molecular weight Mw.sub.2, which is significantly higher than Mw.sub.1.
    • 制备含有式I的重复单体单元的磷酸酯聚合物的方法:其中:X是-O-或-NR“ - ,其中R”是H或烷基; L是二价有机部分; R'是H,烷基,烷氧基,芳基,芳氧基,杂环或杂环氧基; 并且n在约25至2,000之间。 该方法包括以下步骤:(a)在溶剂的存在下聚合,其中p摩尔的q摩尔具有式II的二-XH化合物:其中X和L如上所定义,其中X和L如上所定义,其中p APPROX q, 的二卤代化合物以形成式I的聚合物,其中n为约12至1000,具有第一分子量Mw1,其中溶剂的存在量为每克式II化合物大于约5ml溶剂; (b)除去至少约25%的溶剂以形成更浓缩的反应混合物; 并且(c)将浓缩的反应混合物进一步聚合另外的时间足以产生其中n在约25和2,000之间的式I的聚合物,该聚合物具有明显高于Mw1的第二分子量Mw2。