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    Method of purifying dianhydrides
    4.
    发明授权
    Method of purifying dianhydrides 有权
    二酸酐的纯化方法

    公开(公告)号：US07863463B2

    公开(公告)日：2011-01-04

    申请号：US11286190

    申请日：2005-11-22

    申请人： Eric James Pressman ,  Albert Santo Stella ,  Beatriz Peñalver Bernabe ,  Lioba Maria Kloppenburg ,  Lee Harris Bergman

    发明人： Eric James Pressman ,  Albert Santo Stella ,  Beatriz Peñalver Bernabe ,  Lioba Maria Kloppenburg ,  Lee Harris Bergman

    IPC分类号： C07D307/77

    CPC分类号： C07D307/89

    摘要： Disclosed herein is a method for purification of dianhydrides comprising a substantial amount (10000 ppm or more) of at least one metal salt. In one aspect the method is useful for the purification of dianhydrides prepared by the reaction of a halophthalic anhydride with a metal carbonate and may be optionally catalyzed by a phase transfer catalyst. The purification of the dianhydrides may be accomplished by hydrolyzing the dianhydride metal salt mixture directly to a tetraacid with an inorganic acid, followed by separating the impurities from an aqueous phase, and subsequently heating the tetraacid to effect ring closure to form a purified dianhydride having less than 50 parts per million metal halide and lower levels of other residual impurities. In one aspect the method is highly effective in removing phase transfer catalyst impurities such as hexalkylguanidinium halides initially present in the dianhydride undergoing purification.

    摘要翻译： 本文公开了包含大量（10000ppm或更多）至少一种金属盐的二酸酐的纯化方法。 在一个方面，该方法可用于纯化通过卤代邻苯二甲酸酐与金属碳酸盐的反应制备的二酐，并且可任选地通过相转移催化剂催化。 二酸酐的纯化可以通过用无机酸将二酐金属盐混合物直接水解成四元酸，然后从水相中分离出杂质，随后加热四酸以实现闭环以形成具有较少量的纯化二酐 超过50ppm的金属卤化物和较低水平的其他残留杂质。 在一个方面，该方法在除去最初存在于经过纯化的二酐中的相转移催化剂杂质如六烷基卤化镓中是非常有效的。

    Method of purifying dianhydrides, the dianhydrides formed thereby, and polyetherimides formed therefrom
    6.
    发明授权
    Method of purifying dianhydrides, the dianhydrides formed thereby, and polyetherimides formed therefrom 有权
    纯化二酸酐的方法，由此形成的二酸酐和由其形成的聚醚酰亚胺

    公开(公告)号：US08013173B2

    公开(公告)日：2011-09-06

    申请号：US12058344

    申请日：2008-03-28

    申请人： Beatriz Penalver Bernabe ,  Vijay Gopalakrishnan ,  Lioba Maria Kloppenburg ,  Matt Kuhlman ,  Roy Ray Odle ,  Eric Pressman ,  Narayan Ramesh ,  Harpreet Singh

    发明人： Beatriz Penalver Bernabe ,  Vijay Gopalakrishnan ,  Lioba Maria Kloppenburg ,  Matt Kuhlman ,  Roy Ray Odle ,  Eric Pressman ,  Narayan Ramesh ,  Harpreet Singh

    IPC分类号： C07D493/00

    CPC分类号： C07D307/89 ,  C08G73/1053

    摘要： A method for purifying an oxydiphthalic anhydride comprises diluting a first mixture comprising an oxydiphthalic anhydride, a solvent, a catalyst, and an inorganic salt with a solvent, to provide a second mixture having a solids content of 10 to 30 percent based on total weight of the second mixture; filtering and washing the solids of the second mixture at a temperature below the crystallization point temperature of the oxydiphthalic anhydride to provide a third mixture; hydrolyzing the third mixture by adding water and a water-soluble acid to form a fourth mixture; heating the fourth mixture; then cooling to provide a solid-liquid mixture, optionally decanting a portion of the liquid, rediluting the remaining solid-liquid mixture, then filtering to provide a solid component; washing the solid component with water to provide a fifth mixture of oxydiphthalic tetraacid and water; ring closing the oxydiphthalic tetraacid to provide oxydiphthalic anhydride, and filtering the oxydiphthalic anhydride.

    摘要翻译： 一种氧联二邻苯二甲酸酐的纯化方法包括用溶剂将包含氧联二邻苯二甲酸酐，溶剂，催化剂和无机盐的第一混合物稀释，得到固体含量为10-30重量％ 第二混合物; 在低于氧联二邻苯二甲酸酐的结晶点温度的温度下过滤和洗涤第二混合物的固体以提供第三混合物; 通过加入水和水溶性酸来水解第三混合物以形成第四混合物; 加热第四混合物; 然后冷却以提供固液混合物，任选地倾析一部分液体，重新稀释剩余的固液混合物，然后过滤以提供固体组分; 用水洗涤固体组分以提供氧联二邻苯四酸和水的第五混合物; 闭环氧二邻苯四酸以提供氧联二邻苯二甲酸酐，并过氧化邻苯二甲酸酐。

    Methods for preparing oxydiphthalic anhydrides, oxydiphthalic anhydrides prepared thereby, and polyetherimides derived therefrom
    7.
    发明授权
    Methods for preparing oxydiphthalic anhydrides, oxydiphthalic anhydrides prepared thereby, and polyetherimides derived therefrom 有权
    制备氧联二邻苯二甲酸酐的方法，由此制备的氧联二邻苯二甲酸酐和由其衍生的聚醚酰亚胺

    公开(公告)号：US07674920B2

    公开(公告)日：2010-03-09

    申请号：US12058331

    申请日：2008-03-28

    申请人： Beatriz Penalver Bernabe ,  Lioba Maria Kloppenburg ,  Matt Kuhlman ,  Roy Ray Odle ,  Eric Pressman ,  Narayan Ramesh ,  Harpreet Singh

    发明人： Beatriz Penalver Bernabe ,  Lioba Maria Kloppenburg ,  Matt Kuhlman ,  Roy Ray Odle ,  Eric Pressman ,  Narayan Ramesh ,  Harpreet Singh

    IPC分类号： C07D307/89

    CPC分类号： C07D307/88 ,  C07D307/89 ,  C08G73/1046

    摘要： A method for preparing an oxydiphthalic anhydride comprises contacting, under reactive and substantially anhydrous conditions in a reactor, at least one halophthalic anhydride containing more than 250 ppm chlorophthalide impurity with a carbonate of the formula M2CO3, wherein M is an alkali metal, in the presence of a catalytic proportion of at least one phase transfer catalyst selected from the group consisting of hexaalkylguanidinium halides and alpha,omega-bis(pentaalkylguanidinium)alkane salts, phosphonium salts, phosphazenium salts, pyridinium salts, phosphazenium salts, ammonium salts, and combinations thereof. The phase transfer catalyst is present in a sufficient amount to prepare the oxydiphthalic anhydride when the chlorophthalide is present in an amount that is more than 250 ppm, and the oxydiphthalic anhydride is produced in a yield, based on the carbonate, of at least 70%.

    摘要翻译： 一种制备氧联二邻苯二甲酸酐的方法包括在反应器和反应性基本上无水的条件下，在反应器中使至少一种含有多于250ppm氯酞酸盐杂质的卤代邻苯二甲酸酐与式M2CO3的碳酸酯（其中M为碱金属）在存在下 选自六烷基卤化镓和α，ω-双（五烷基胍）烷烃盐，鏻盐，磷氮烯基鏻盐，吡啶鎓盐，磷氮烯基鏻盐，铵盐及其组合的至少一种相转移催化剂的催化剂比例。 当氯代苯酞以250ppm以上的量存在时，相转移催化剂的存在量足以制备氧联二邻苯二甲酸酐，并且基于碳酸酯的产率以氧化邻苯二甲酸酐的产率为至少70％ 。

    Method of Purifying Dianhydrides, the Dianhydrides Formed Thereby, and Polyetherimides Formed Therefrom
    9.
    发明申请
    Method of Purifying Dianhydrides, the Dianhydrides Formed Thereby, and Polyetherimides Formed Therefrom 有权
    纯化二酸酐的方法，由此形成的二酸酐和由其形成的聚醚酰亚胺

    公开(公告)号：US20090247727A1

    公开(公告)日：2009-10-01

    申请号：US12058344

    申请日：2008-03-28

    申请人： Beatriz Penalver Bernabe ,  Vijay Gopalakrishnan ,  Lioba Maria Kloppenburg ,  Matt Kuhlman ,  Roy Ray Odle ,  Eric Pressman ,  Narayan Ramesh ,  Harpreet Singh

    发明人： Beatriz Penalver Bernabe ,  Vijay Gopalakrishnan ,  Lioba Maria Kloppenburg ,  Matt Kuhlman ,  Roy Ray Odle ,  Eric Pressman ,  Narayan Ramesh ,  Harpreet Singh

    IPC分类号： C07D407/12 ,  C08G65/26

    CPC分类号： C07D307/89 ,  C08G73/1053

    摘要： A method for purifying an oxydiphthalic anhydride comprises diluting a first mixture comprising an oxydiphthalic anhydride, a solvent, a catalyst, and an inorganic salt with a solvent, to provide a second mixture having a solids content of 10 to 30 percent based on total weight of the second mixture; filtering and washing the solids of the second mixture at a temperature below the crystallization point temperature of the oxydiphthalic anhydride to provide a third mixture; hydrolyzing the third mixture by adding water and a water-soluble acid to form a fourth mixture; heating the fourth mixture; then cooling to provide a solid-liquid mixture, optionally decanting a portion of the liquid, rediluting the remaining solid-liquid mixture, then filtering to provide a solid component; washing the solid component with water to provide a fifth mixture of oxydiphthalic tetraacid and water; ring closing the oxydiphthalic tetraacid to provide oxydiphthalic anhydride, and filtering the oxydiphthalic anhydride.

    摘要翻译： 一种氧联二邻苯二甲酸酐的纯化方法包括用溶剂将包含氧联二邻苯二甲酸酐，溶剂，催化剂和无机盐的第一混合物稀释，得到固体含量为10-30重量％ 第二混合物; 在低于氧联二邻苯二甲酸酐的结晶点温度的温度下过滤和洗涤第二混合物的固体以提供第三混合物; 通过加入水和水溶性酸来水解第三混合物以形成第四混合物; 加热第四混合物; 然后冷却以提供固液混合物，任选地倾析一部分液体，重新稀释剩余的固液混合物，然后过滤以提供固体组分; 用水洗涤固体组分以提供氧联二邻苯四酸和水的第五混合物; 闭环氧二邻苯四酸以提供氧联二邻苯二甲酸酐，并过氧化邻苯二甲酸酐。

    Methods for Preparing Oxydiphthalic Anhydrides, Oxydiphthalic Anhydrides Prepared Thereby, and Polyetherimides Derived Therefrom
    10.
    发明申请
    Methods for Preparing Oxydiphthalic Anhydrides, Oxydiphthalic Anhydrides Prepared Thereby, and Polyetherimides Derived Therefrom 有权
    制备氧联二邻苯二甲酸酐，由此制备的氧联二邻苯二甲酸酐的方法及其衍生的聚醚酰亚胺

    公开(公告)号：US20090247725A1

    公开(公告)日：2009-10-01

    申请号：US12058331

    申请日：2008-03-28

    申请人： Beatriz Penalver Bernabe ,  Lioba Maria Kloppenburg ,  Matt Kuhlman ,  Roy Ray Odle ,  Eric Pressman ,  Narayan Ramesh ,  Harpreet Singh

    发明人： Beatriz Penalver Bernabe ,  Lioba Maria Kloppenburg ,  Matt Kuhlman ,  Roy Ray Odle ,  Eric Pressman ,  Narayan Ramesh ,  Harpreet Singh

    IPC分类号： C07D307/89 ,  C08G73/10

    CPC分类号： C07D307/88 ,  C07D307/89 ,  C08G73/1046

    摘要： a method for preparing an oxydiphthalic anhydride comprises contacting, under reactive and substantially anhydrous conditions in a reactor, at least one halophthalic anhydride containing more than 250 ppm chlorophthalide impurity with a carbonate of the formula M2CO3, wherein M is an alkali metal, in the presence of a catalytic proportion of at least one phase transfer catalyst selected from the group consisting of hexaalkylguanidinium halides and alpha,omega-bis(pentaalkylguanidinium)alkane salts, phosphonium salts, phosphazenium salts, pyridinium salts, phosphazenium salts, ammonium salts, and combinations thereof. The phase transfer catalyst is present in a sufficient amount to prepare the oxydiphthalic anhydride when the chlorophthalide is present in an amount that is more than 250 ppm, and the oxydiphthalic anhydride is produced in a yield, based on the carbonate, of at least 70%.

    摘要翻译： 一种制备氧联二邻苯二甲酸酐的方法包括在反应器和反应性基本上无水的条件下，在反应器中使至少一种含有多于250ppm氯酞酸盐杂质的卤代邻苯二甲酸酐与式M2CO3的碳酸盐接触，其中M为碱金属， 选自六烷基卤化镓和α，ω-双（五烷基胍）烷烃盐，鏻盐，磷氮烯基鏻盐，吡啶鎓盐，磷氮烯基鏻盐，铵盐及其组合的至少一种相转移催化剂的催化剂比例。 当氯代苯酞以250ppm以上的量存在时，相转移催化剂的存在量足以制备氧联二邻苯二甲酸酐，并且基于碳酸酯的产率以氧化邻苯二甲酸酐的产率为至少70％ 。