Method of Purifying Dianhydrides, the Dianhydrides Formed Thereby, and Polyetherimides Formed Therefrom
    25.
    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

    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
    26.
    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

    IPC分类号: C07D307/89 C08G73/10

    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% 。

    Method for making stable, homogeneous melt solutions
    29.
    发明授权
    Method for making stable, homogeneous melt solutions 有权
    制备稳定,均匀熔体溶液的方法

    公开(公告)号:US06900283B2

    公开(公告)日:2005-05-31

    申请号:US10286165

    申请日:2002-11-04

    IPC分类号: C08G64/30 C08G64/00

    CPC分类号: C08G64/307

    摘要: Stable, homogeneous melt solutions are prepared at temperatures of 200° C. or less from solid mixtures comprising at least one diaryl carbonate, at least one high melting dihydroxy aromatic compound (mp>200° C.), a transesterification catalyst, and optionally a lower melting dihydroxy aromatic compound. Thus, a stable, homogeneous melt solution is obtained from a solid mixture comprising 4,4′-biphenol (mp 282-284° C.) at a temperature of about 200° C. using either diphenyl carbonate or bis(methyl salicyl) carbonate as the diaryl carbonate component. It is shown that formation of the stable, homogeneous melt solutions requires the presence of the transesterification catalyst when substantial amounts of the high melting dihydroxy aromatic compound are present in the initial solid mixture. Solid mixtures comprising a variety of high melting bisphenols; 4,4′-biphenol; 3,3,3,3′-tetramethylspirobiindanbisphenol, and 4,4′-sulfonyidiphenol are converted to stable, homogeneous melt solutions at 200° C., a temperature substantially below the melting points of the high melting bisphenols in their pure states.

    摘要翻译: 稳定的均相熔体溶液在200℃或更低的温度下从包含至少一种碳酸二芳基酯,至少一种高熔点二羟基芳族化合物(mp> 200℃),酯交换催化剂和任选的 较低熔点的二羟基芳族化合物。 因此,使用碳酸二苯酯或碳酸二(甲基水杨酰基)酯在约200℃的温度下由包含4,4'-联苯酚(mp 282-284℃)的固体混合物获得稳定的均匀熔融溶液 作为碳酸二芳基酯组分。 显示当在初始固体混合物中存在大量的高熔点二羟基芳族化合物时,形成稳定的均相熔体溶液需要酯交换催化剂的存在。 包含各种高熔点双酚的固体混合物; 4,4'-联苯酚 3,3,3,3'-四甲基螺二茚二苯酚和4,4'-磺基二苯基酚在200℃下转化为稳定的均匀熔体溶液,其温度基本上低于其纯态中高熔点双酚的熔点。

    Method for making an aromatic polycarbonate
    30.
    发明授权
    Method for making an aromatic polycarbonate 有权
    制备芳族聚碳酸酯的方法

    公开(公告)号:US06790929B2

    公开(公告)日:2004-09-14

    申请号:US10389009

    申请日:2003-03-17

    IPC分类号: C08G6400

    摘要: This invention relates to an extrusion method preparing polycarbonates from a solution of an oligomeric polycarbonate. A mixture of bis(methyl salicyl)carbonate (BMSC), BPA and a transesterification catalyst are first equilibrated at moderate temperatures to provide a solution of polycarbonate oligomer in methyl salicylate. The solution is then fed to a devolatilizing extruder, where the polymerization reaction is completed and the methyl salicylate solvent is removed. The solution comprising the oligomeric polycarbonate can also be pre-heated under pressure to a temperature above the boiling point of methyl salicylate and subsequently fed to a devolatilizing extruder equipped for rapid flashing off the solvent. The method provides polycarbonate with greater efficiency than the corresponding process in which unreacted monomers are fed to the extruder. Additionally, the method of the invention does not require the isolation of a precursor polycarbonate comprising ester-substituted phenoxy terminal groups.

    摘要翻译: 本发明涉及从低聚聚碳酸酯溶液制备聚碳酸酯的挤压方法。 首先在中等温度下平衡双(甲基水杨酸)碳酸酯(BMSC),BPA和酯交换催化剂的混合物,以提供聚碳酸酯低聚物在水杨酸甲酯中的溶液。 然后将溶液进料到脱挥发分挤出机中,其中聚合反应完成并除去水杨酸甲酯溶剂。 包含低聚物聚碳酸酯的溶液也可以在压力下预加热到高于水杨酸甲酯沸点的温度,随后进料到脱挥发分的挤出机中,以便迅速地从溶剂中闪蒸。 该方法提供聚碳酸酯比未反应的单体进料到挤出机的相应方法具有更高的效率。 另外,本发明的方法不需要分离包含酯取代的苯氧基末端基团的前体聚碳酸酯。