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    • 1. 发明授权
    • Gel-free process for making hydrogenated functionalized anionically polymerized polymers
    • 制备氢化官能化阴离子聚合聚合物的无凝胶工艺
    • US06242537B1
    • 2001-06-05
    • US09260239
    • 1999-03-02
    • Robert Charles BeningCarl Lesley WillisCharles Roy DonahoDaniel Earl GoodwinZaida DiazJohn David Wilkey
    • Robert Charles BeningCarl Lesley WillisCharles Roy DonahoDaniel Earl GoodwinZaida DiazJohn David Wilkey
    • C08F804
    • C08C19/44C08C19/42C08F8/00C08F12/00
    • This invention relates to a gel-free process for making hydrogenated functionalized polymers that mitigates the problem of ionic gel. When multi-alkali metal initiators are used to make these polymers anionically, the process comprises anionically polymerizing at least one monomer with a multi-alkali metal initiator, usually a lithium alkyl, in a hydrocarbon solvent, capping the polymer by adding to the polymer a capping agent that reacts with the ends of the polymer chains such that strongly associating chain ends are formed wherein a strongly associating polymer gel is formed, adding a trialkyl aluminum compound to the polymer gel, whereby the gel dissipates, optionally terminating the polymerization by addition of an alcohol, washing the polymer with aqueous acid, preferably aqueous mineral acid, most preferably phosphoric acid, wherein there is at least one mole of phosphoric acid per mole of alkali metal and at least three moles of phosphoric acid per mole of aluminum, and hydrogenating the polymer with a hydrogenation catalyst. In a second embodiment, the present invention relates to a process for making such polymers which comprises anionically polymerizing them as described and adding a trialkyl aluminum compound prior to the addition of the functionalizing agent and washing the product prior to hydrogenation as described above. In the first embodiment, a gel is formed and then removed. In the second embodiment, the gel never is formed because of the presence of the trialkyl aluminum compound.
    • 本发明涉及一种用于制备氢化官能化聚合物的无凝胶方法,其减轻了离子凝胶的问题。 当使用多碱金属引发剂阴离子制造这些聚合物时,该方法包括在烃溶剂中将至少一种单体与多碱金属引发剂(通常为烷基锂)进行阴离子聚合,通过向聚合物加入聚合物 形成与聚合物链的端部反应的封端剂,从而形成强缔合的链端,其中形成强缔合的聚合物凝胶,将三烷基铝化合物加入到聚合物凝胶中,由此凝胶消散,任选地通过加入聚合物终止聚合 醇,用酸水溶液洗涤聚合物,优选无机酸水溶液,最优选磷酸,其中每摩尔铝存在至少1摩尔磷酸/摩尔碱金属和至少3摩尔磷酸/摩尔氢化 该聚合物与氢化催化剂。 在第二个实施方案中,本发明涉及一种制备这种聚合物的方法,其包括如上所述阴离子聚合它们,并且在加入官能化试剂之前加入三烷基铝化合物并在如上所述的氢化之前洗涤产物。 在第一实施方案中,形成凝胶然后除去。 在第二实施方案中,由于存在三烷基铝化合物,所以不会形成凝胶。
    • 2. 发明授权
    • Process for making hydrogenated gel-free functionalized anionically polymerized polymers
    • 制备无凝胶的官能化阴离子聚合聚合物的方法
    • US06242538B1
    • 2001-06-05
    • US09304915
    • 1999-05-04
    • Robert Charles BeningCarl Lesley WillisJohn David WilkeyZaida Diaz
    • Robert Charles BeningCarl Lesley WillisJohn David WilkeyZaida Diaz
    • C08F804
    • C08F8/04
    • This invention relates to a process for making gel-free functionalized polymers. When multi-lithium initiators are used to make these polymers anionically, the process comprises anionically polymerizing at least one monomer with a multi-lithium initiator in a hydrocarbon solvent, functionalizing the polymer by adding to the polymer a capping agent that reacts with the ends of the polymer chains such that strongly-associating chain ends are formed wherein a polymer gel is formed, adding a trialkyl aluminum compound to the polymer gel, whereby the gel dissipates, adding a sufficient amount of a proton source to provide at least 1 mole of protons per mole of lithium ions and at least 2 moles of protons per mole of aluminum wherein the proton source is an organic acid with a pKa of 11 or less or a mixture of the organic acid and an alkanol, provided that sufficient organic acid is added to provide at least 0.4 moles of protons per mole of lithium ions, hydrogenating the polymer with a hydrogenation catalyst, and optionally washing the polymer with aqueous mineral acid in sufficient.
    • 本发明涉及一种制备不含凝胶的官能化聚合物的方法。 当使用多锂引发剂阴离子制造这些聚合物时,该方法包括在烃溶剂中使多个锂引发剂的至少一种单体阴离子聚合,通过向聚合物中添加与端基反应的封端剂官能化聚合物 聚合物链使得形成强缔合的链端,其中形成聚合物凝胶,将三烷基铝化合物加入到聚合物凝胶中,由此凝胶消散,加入足够量的质子源以提供至少1摩尔的质子 每摩尔锂离子和至少2摩尔质子/摩尔铝,其中质子源是pKa为11或更低的有机酸或有机酸和链烷醇的混合物,条件是将足够的有机酸加入到 每摩尔锂离子提供至少0.4摩尔质子,用氢化催化剂氢化聚合物,并任选地用无机酸水溶液洗涤聚合物 足够了