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    • 1. 发明申请
    • Method for making polyetherimides
    • 制备聚醚酰亚胺的方法
    • US20070073035A1
    • 2007-03-29
    • US11603523
    • 2006-11-21
    • Albert StellaDavid Hall
    • Albert StellaDavid Hall
    • C08G69/26
    • C08G73/1007C07C51/573C08G73/1014C08G73/1028C08G73/105C07C65/24
    • A method for making polyetherimides is provided by reacting a high purity dianhydride with an aromatic diamine under condensation polymerization conditions. The dianhydrides employed are purified by a method comprising contacting a first solution containing a dianhydride compound, a solvent, and a phase transfer catalyst, with a solid inorganic adsorbent material having a total pore volume of about 0.5 milliliters/gram or greater and a cumulative pore volume distribution of about 20 percent or greater of particles having a pore diameter in a range between about 3 nanometers and about 20 nanometers. The solution containing the dianhydride compound is then separated from the solid inorganic adsorbent material to provide a purified dianhydride compound which is substantially free of the phase transfer catalyst. The purified dianhydrides are then condensed with aromatic diamines to provide polyetherimide compositions which are substantially free of residual phase transfer catalyst.
    • 通过在缩聚条件下使高纯度二酐与芳族二胺反应来提供制备聚醚酰亚胺的方法。 所用的二酸酐通过包括将含有二酐化合物,溶剂和相转移催化剂的第一溶液与总孔体积为约0.5毫升/克或更大的固体无机吸附材料和累积孔 约20%或更大的孔径在约3纳米至约20纳米之间的颗粒的体积分布。 然后将含有二酐化合物的溶液与固体无机吸附材料分离,得到基本上不含相转移催化剂的纯化二酐化合物。 然后将纯化的二酸酐与芳族二胺缩合,得到基本上不含残余相转移催化剂的聚醚酰亚胺组合物。
    • 3. 发明申请
    • Method of purifying dianhydrides
    • 二酸酐的纯化方法
    • US20060293528A1
    • 2006-12-28
    • US11167832
    • 2005-06-24
    • Albert StellaQing YeDavid WoodruffPaul Howson
    • Albert StellaQing YeDavid WoodruffPaul Howson
    • C07D405/02
    • C07D307/89
    • A method for purifying oxybisphthalic anhydrides is provided. A first mixture comprising at least one oxybisphthalic anhydride, at least one solvent, and at least one inorganic salt is diluted with a solvent such that the concentration of oxybisphthalic anhydride is less than 25 weight percent. This second mixture is then heated to dissolve the oxybisphthalic anhydride thereby providing a third mixture. The third mixture is then filtered at a temperature above the crystallization temperature of the oxybisphthalic anhydride. The oxybisphthalic anhydride present in the filtrate is then crystallized to provide a purified oxybisphthalic anhydride as a slurry. Also included within the scope of the present invention are a method for preparing oxybisphthalic anhydrides and a method for preparing polyetherimides comprising structural units derived from the oxybisphthalic anhydride purified by the method of the present invention.
    • 提供了一种纯化羟基双苯二甲酸酐的方法。 包含至少一种氧基双邻苯二甲酸酐,至少一种溶剂和至少一种无机盐的第一混合物用溶剂稀释,使得邻苯二甲酸酐的浓度小于25重量%。 然后将该第二混合物加热以溶解氧基双苯酐,从而提供第三混合物。 然后在高于氧邻苯二甲酸酐的结晶温度的温度下过滤第三混合物。 然后使存在于滤液中的氧化双苯酐酐结晶,得到纯化的氧联苯二甲酸酐作为浆料。 还包括在本发明范围内的是一种制备羟基双苯二甲酸酐的方法和一种制备聚醚酰亚胺的方法,其包括通过本发明的方法纯化的由相对于邻苯二甲酸酐取代的结构单元。
    • 4. 发明申请
    • METHODS OF PREPARING POLYMER-ORGANOCLAY COMPOSITES AND ARTICLES DERIVED THEREFROM
    • 制备聚合物 - 组织复合材料的方法及其衍生物
    • US20080004391A1
    • 2008-01-03
    • US11766456
    • 2007-06-21
    • Kwok ChanSarah GenoveseErik HagbergDavid HallJohn MaxamTara MullenRoy OdleAlbert StellaJames White
    • Kwok ChanSarah GenoveseErik HagbergDavid HallJohn MaxamTara MullenRoy OdleAlbert StellaJames White
    • C08K9/04
    • C08F2/44
    • A method for preparing a polymer-organoclay composite composition comprises combining a solvent and an unexfoliated organoclay to provide a first mixture, wherein the unexfoliated organoclay comprises alternating inorganic silicate layers and organic layers, and has an initial spacing between the silicate layers; exposing the first mixture to an energized condition of a sufficient intensity and duration to increase the initial spacing of the inorganic silicate layers, to provide a second mixture; contacting the second mixture with a polymer composition so that the polymer composition fills at least one region located between at least one pair of silicate layers, wherein the polymer composition is at least partially soluble in the solvent; and removing at least a portion of the solvent from the second mixture, wherein the inorganic silicate layers remain separated by the polymer after removal of the solvent.
    • 一种制备聚合物 - 有机粘土复合材料组合物的方法,包括将溶剂和未剥离的有机粘土组合以提供第一混合物,其中未剥离的有机粘土包含交替的无机硅酸盐层和有机层,并且在硅酸盐层之间具有初始间隔; 将第一混合物暴露于足够强度和持续时间的通电状态以增加无机硅酸盐层的初始间隔,以提供第二混合物; 使所述第二混合物与聚合物组合物接触,使得所述聚合物组合物填充位于至少一对硅酸盐层之间的至少一个区域,其中所述聚合物组合物至少部分地可溶于所述溶剂中; 以及从所述第二混合物中除去至少一部分所述溶剂,其中在去除所述溶剂之后,所述无机硅酸盐层保持被所述聚合物分离。
    • 5. 发明申请
    • Method of purifying dianhydrides
    • 二酸酐的纯化方法
    • US20070117990A1
    • 2007-05-24
    • US11286190
    • 2005-11-22
    • Eric PressmanAlbert StellaBeatriz BernabeLioba KloppenburgLee Bergman
    • Eric PressmanAlbert StellaBeatriz BernabeLioba KloppenburgLee Bergman
    • C07D405/02
    • C07D307/89
    • 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.
    • 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。
    • 6. 发明申请
    • Method for purifying dianhydrides
    • 二酸酐的纯化方法
    • US20070073066A1
    • 2007-03-29
    • US11603764
    • 2006-11-22
    • Albert StellaDavid Hall
    • Albert StellaDavid Hall
    • C07D405/02
    • C07D407/12
    • A method for purifying dianhydrides is provided. In one aspect, purified oxybisphthalic anhydrides, intermediates useful in the preparation of polyetherimides are provided. In one embodiment, a first solution containing a dianhydride compound, a solvent, and a phase transfer catalyst is contacted with a solid inorganic adsorbent material having a total pore volume of about 0.5 milliliters/gram or greater and a cumulative pore volume distribution of about 20 percent or greater of particles having a pore diameter in a range between about 3 nanometers and about 20 nanometers. The solution containing the dianhydride compound is then separated from the solid inorganic adsorbent material to provide a purified dianhydride compound which is substantially free of the phase transfer catalyst. The purification technique is especially valuable for preparing high purity oxybisphthalic anhydrides, such as 4,4′-oxybisphthalic anhydride (4,4′-ODPA), which are substantially free of residual phase transfer catalyst.
    • 提供了一种纯化二酸酐的方法。 在一个方面,提供了纯的氧化双邻苯二甲酸酐,可用于制备聚醚酰亚胺的中间体。 在一个实施方案中,将含有二酐化合物,溶剂和相转移催化剂的第一溶液与总孔体积为约0.5毫升/克或更大并且累积孔体积分布约为20的固体无机吸附材料接触 百分比或更大的具有在约3纳米和约20纳米之间的孔径的颗粒。 然后将含有二酐化合物的溶液与固体无机吸附材料分离,得到基本上不含相转移催化剂的纯化二酐化合物。 纯化技术对于制备基本上不含残余相转移催化剂的4,4'-氧双苯二甲酸酐(4,4'-ODPA)的高纯度羟基双苯酐具有特别的价值。
    • 7. 发明申请
    • Method for purifying bisimides
    • 纯化双酰亚胺的方法
    • US20070073063A1
    • 2007-03-29
    • US11603394
    • 2006-11-22
    • Albert StellaDavid Hall
    • Albert StellaDavid Hall
    • C07D403/02
    • C07D209/48
    • A method for purifying bisimides is provided. In one aspect, purified oxybisphthalimides, intermediates useful in the preparation of polyetherimides are provided. In one embodiment, a first solution containing a bisimide compound, a solvent, and a phase transfer catalyst is contacted with a solid inorganic adsorbent material having a total pore volume of about 0.5 milliliters/gram or greater and a cumulative pore volume distribution of about 20 percent or greater of particles having a pore diameter in a range between about 3 nanometers and about 20 nanometers. The solution containing the bisimide compound is then separated from the solid inorganic adsorbent material to provide a purified bisimide compound which is substantially free of the phase transfer catalyst. The purification technique is especially valuable for preparing high purity oxybisphthalimides, such as 4,4′-oxybis(N-methylphthalimide), which are substantially free of residual phase transfer catalyst.
    • 提供了一种纯化双酰亚胺的方法。 一方面,提供了纯化的氧联双苯二酰亚胺,可用于制备聚醚酰亚胺的中间体。 在一个实施方案中,将含有双酰亚胺化合物,溶剂和相转移催化剂的第一溶液与总孔体积为约0.5毫升/克或更大并且累积孔体积分布约为20的固体无机吸附材料接触 百分比或更大的具有在约3纳米和约20纳米之间的孔径的颗粒。 然后将含有双酰亚胺化合物的溶液与固体无机吸附剂材料分离,以提供基本上不含相转移催化剂的纯化双酰亚胺化合物。 纯化技术对于制备基本上不含残余相转移催化剂的4,4'-氧双(N-甲基邻苯二甲酰亚胺)的高纯度氧联双苯二酰亚胺是特别有价值的。