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    Method for making an aromatic polycarbonate
    1.
    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

    申请人： Norberto Silvi ,  Mark Howard Giammattei ,  Patrick Joseph McCloskey ,  Alberto Nisoli ,  James Day ,  Narayan Ramesh ,  Paul Michael Smigelski, Jr. ,  Paul Russell Wilson

    发明人： Norberto Silvi ,  Mark Howard Giammattei ,  Patrick Joseph McCloskey ,  Alberto Nisoli ,  James Day ,  Narayan Ramesh ,  Paul Michael Smigelski, Jr. ,  Paul Russell Wilson

    IPC分类号： C08G6400

    CPC分类号： B29C47/0004 ,  B29C47/0009 ,  B29C47/60 ,  B29C47/76 ,  B29C47/767 ,  B29C67/246 ,  B29K2069/00 ,  C08G64/081 ,  C08G64/14 ,  C08G64/205 ,  C08G64/307

    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。

    Method for making an aromatic polycarbonate
    2.
    再颁专利
    Method for making an aromatic polycarbonate 有权
    制备芳族聚碳酸酯的方法

    公开(公告)号：USRE40697E1

    公开(公告)日：2009-04-07

    申请号：US11345691

    申请日：2006-01-31

    申请人： Norberto Silvi ,  Mark Howard Giammattei ,  Patrick Joseph McCloskey ,  Alberto Nisoli ,  James Day ,  Narayan Ramesh ,  Paul Michael Smigelski, Jr. ,  Paul Russell Wilson

    发明人： Norberto Silvi ,  Mark Howard Giammattei ,  Patrick Joseph McCloskey ,  Alberto Nisoli ,  James Day ,  Narayan Ramesh ,  Paul Michael Smigelski, Jr. ,  Paul Russell Wilson

    IPC分类号： C08G64/00

    CPC分类号： B29C47/0004 ,  B29C47/0009 ,  B29C47/60 ,  B29C47/76 ,  B29C47/767 ,  B29C67/246 ,  B29K2069/00 ,  C08G64/081 ,  C08G64/14 ,  C08G64/205 ,  C08G64/307

    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。

    Extrusion method for making polycarbonate
    3.
    发明授权
    Extrusion method for making polycarbonate 有权
    制造聚碳酸酯的挤出方法

    公开(公告)号：US06506871B1

    公开(公告)日：2003-01-14

    申请号：US10167903

    申请日：2002-06-12

    申请人： Norberto Silvi ,  Patrick Joseph McCloskey ,  James Day ,  Mark Howard Giammattei

    发明人： Norberto Silvi ,  Patrick Joseph McCloskey ,  James Day ,  Mark Howard Giammattei

    IPC分类号： C08G6400

    CPC分类号： C08G64/307

    摘要： Extrusion of a mixture of an ester-substituted diaryl carbonate, such as bis(methyl salicyl) carbonate, a dihydroxy aromatic compound such as bisphenol A and a transesterification catalyst such as tetrabutylphosphonium acetate (TBPA) affords polycarbonate having a weight average molecular weight of greater than 20,000 daltons. The extruder is equipped with one or more vacuum vents to remove by-product ester-substituted phenol. Similarly, a precursor polycarbonate having ester-substituted phenoxy endgroups, for example methyl salicyl endgroups, when subjected to extrusion affords a polycarbonate having a significantly increased molecular weight relative to the precursor polycarbonate. The reaction to form a higher molecular weight polycarbonate may be catalyzed by residual transesterification catalyst present in the precursor polycarbonate, or by a combination of any residual catalyst and an additional catalyst such as TBPA introduced in the extrusion step. Fries rearrangement products are not observed in the product polycarbonates.

    摘要翻译： 碳酸二（甲基水杨基）酯，二羟基芳族化合物如双酚A和酯交换催化剂如四丁基鏻乙酸酯（TBPA）的酯取代的二芳基碳酸酯的混合物的挤出得到重均分子量更大的聚碳酸酯 超过20,000道尔顿。 挤出机配备有一个或多个真空通风口以除去副产物酯取代的苯酚。 类似地，具有酯取代的苯氧基端基的前体聚碳酸酯，例如甲基水杨基端基，当进行挤出时，得到相对于前体聚碳酸酯具有显着增加的分子量的聚碳酸酯。 形成较高分子量聚碳酸酯的反应可以通过存在于前体聚碳酸酯中的残留酯交换催化剂，或者通过任何残余催化剂和另外的催化剂如在挤出步骤中引入的TBPA的组合来催化。 在产品聚碳酸酯中没有观察到薯条重排产物。

    Method of making block copolymers by solid state polymerization
    4.
    发明授权
    Method of making block copolymers by solid state polymerization 有权
    通过固态聚合制备嵌段共聚物的方法

    公开(公告)号：US06960641B2

    公开(公告)日：2005-11-01

    申请号：US10743241

    申请日：2003-12-22

    申请人： Gregory Allen O'Neil ,  James Day ,  Daniel Joseph Brunelle ,  Joseph Anthony Suriano ,  Patrick Joseph McCloskey ,  Paul Michael Smigelski, Jr.

    发明人： Gregory Allen O'Neil ,  James Day ,  Daniel Joseph Brunelle ,  Joseph Anthony Suriano ,  Patrick Joseph McCloskey ,  Paul Michael Smigelski, Jr.

    IPC分类号： C08G81/00 ,  C08G63/64 ,  C08G63/80 ,  C08G64/00

    CPC分类号： C08G63/64 ,  C08G63/80

    摘要： A method of preparing block copolymers by solid state polymerization is described. A mixture of a partially crystalline polycarbonate having activated terminal aryloxy groups, for example terminal methyl salicyl groups, when heated together with an oligomeric polyester having reactive terminal hydroxy groups under solid state polymerization conditions affords block copolymers. The activated terminal aryloxy groups play a key role in preserving the block lengths of the starting materials. A control sample in which the partially crystalline polycarbonate lacks activated terminal aryloxy groups, for example polycarbonates substituted by phenol, affords a much lower molecular weight, more highly randomized copolymer product. The product block copolymers are useful as “weatherable” plastic materials.

    摘要翻译： 描述了通过固态聚合制备嵌段共聚物的方法。 当在固态聚合条件下与具有反应性末端羟基的低聚聚酯一起加热时，具有活化的末端芳氧基的部分结晶的聚碳酸酯，例如末端甲基水杨酸酯的混合物得到嵌段共聚物。 活化的末端芳氧基在保留原料的块长度方面起关键作用。 其中部分结晶聚碳酸酯缺乏活化的末端芳氧基的对照样品，例如被苯酚取代的聚碳酸酯，得到低得多的分子量，更高度随机的共聚物产物。 产品嵌段共聚物可用作“耐候性”塑料材料。

    Method of polycarbonate preparation by solid state polymerization
    5.
    发明授权
    Method of polycarbonate preparation by solid state polymerization 失效
    通过固态聚合制备聚碳酸酯的方法

    公开(公告)号：US06518391B1

    公开(公告)日：2003-02-11

    申请号：US09911505

    申请日：2001-07-24

    申请人： Patrick Joseph McCloskey ,  James Day ,  Paul Michael Smigelski, Jr. ,  Timothy Brydon Burnell

    发明人： Patrick Joseph McCloskey ,  James Day ,  Paul Michael Smigelski, Jr. ,  Timothy Brydon Burnell

    IPC分类号： C08G6400

    CPC分类号： C08G64/307 ,  C08G64/06

    摘要： Solid state polymerization of partially crystalline polycarbonate oligomers bearing ester-substituted terminal groups occurs at useful reaction rates despite their high level of endcapping. Partially crystalline polycarbonate oligomers having ester substituted terminal groups may be obtained in a single step by reaction of an ester substituted diaryl carbonate such as bis-methyl salicyl carbonate with a dihydroxy aromatic compound such as bisphenol A in the presence of a transesterification catalyst such as sodium hydroxide. Alternatively, amorphous oligomeric polycarbonates incorporating ester substituted endgroups may be obtained through careful control of the melt reaction conditions. The amorphous oligomeric polycarbonates are crystallized upon exposure to solvent vapor and subsequently undergo solid state polymerization at synthetically useful reaction rates.

    摘要翻译： 带有酯取代的端基的部分结晶的聚碳酸酯低聚物的固态聚合以有效的反应速率发生，尽管它们具有高水平的封端。 具有酯取代的末端基的部分结晶的聚碳酸酯低聚物可以通过酯交换催化剂如钠的存在下，酯取代的碳酸二碳酸酯如碳酸双甲基酯与二羟基芳族化合物如双酚A的反应在一个步骤中获得 氢氧化物。 或者，可以通过仔细控制熔融反应条件来获得引入酯取代的端基的无定形低聚聚碳酸酯。 无定形低聚聚碳酸酯在暴露于溶剂蒸气下结晶，随后在合成有用的反应速率下进行固态聚合。

    Extrusion method for making polycarbonate
    6.
    发明授权
    Extrusion method for making polycarbonate 有权
    制造聚碳酸酯的挤出方法

    公开(公告)号：US06420512B1

    公开(公告)日：2002-07-16

    申请号：US09911439

    申请日：2001-07-24

    申请人： Patrick Joseph McCloskey ,  James Day ,  Paul Michael Smigelski ,  John Lester Maxam ,  John Aibangbee Osaheni

    发明人： Patrick Joseph McCloskey ,  James Day ,  Paul Michael Smigelski ,  John Lester Maxam ,  John Aibangbee Osaheni

    IPC分类号： C08G6400

    CPC分类号： C08G64/307

    摘要： Extrusion of a mixture of an ester-substituted diaryl carbonate, such as bis-methyl salicyl carbonate, a dihydroxy aromatic compound such as bisphenol A and a transesterification catalyst such as tetrabutyl phosphonium acetate (TBPA) affords polycarbonate having a weight average molecular weight of greater than 20,000 Daltons. The extruder is equipped with one or more vacuum vents to remove by-product ester-substituted phenol. Similarly, a precursor polycarbonate having ester-substituted phenoxy endgroups, for example methyl salicyl endgroups, when subjected to extrusion affords a polycarbonate having a significantly increased molecular weight relative to the precursor polycarbonate. The reaction to form a higher molecular weight polycarbonate may be catalyzed by residual transesterification catalyst present in the precursor polycarbonate, or by a combination of any residual catalyst and an additional catalyst such as TBPA introduced in the extrusion step. Fries rearrangement products are not observed in the product polycarbonates.

    摘要翻译： 酯取代的碳酸二芳基酯如碳酸双甲酯，双酚A等二羟基芳族化合物和乙酸四丁基鏻（TBPA）等酯交换催化剂的混合物的挤出，得到重均分子量大的聚碳酸酯 超过20,000道尔顿。 挤出机配备有一个或多个真空通风口以除去副产物酯取代的苯酚。 类似地，具有酯取代的苯氧基端基的前体聚碳酸酯，例如甲基水杨基端基，当进行挤出时，得到相对于前体聚碳酸酯具有显着增加的分子量的聚碳酸酯。 形成较高分子量聚碳酸酯的反应可以通过存在于前体聚碳酸酯中的残留酯交换催化剂，或者通过任何残余催化剂和另外的催化剂如在挤出步骤中引入的TBPA的组合来催化。 在产品聚碳酸酯中没有观察到薯条重排产物。

    Method and apparatus for in situ determination of molten polycarbonate composition using electronic absorption spectroscopy
    7.
    发明授权
    Method and apparatus for in situ determination of molten polycarbonate composition using electronic absorption spectroscopy 失效
    使用电子吸收光谱法原位测定熔融聚碳酸酯组合物的方法和装置

    公开(公告)号：US06809817B2

    公开(公告)日：2004-10-26

    申请号：US09682365

    申请日：2001-08-24

    申请人： Radislav Alexandrovich Potyrailo ,  Patrick Joseph McCloskey ,  James Day

    发明人： Radislav Alexandrovich Potyrailo ,  Patrick Joseph McCloskey ,  James Day

    IPC分类号： G01J328

    CPC分类号： G01J3/42 ,  G01J3/28

    摘要： The present invention relates to methods and devices for in-situ measurement of reaction components of interest during manufacturing of polycarbonate by melt polymerization. The present invention describes irradiating a molten polymer sample with UV/visible light, and generating an absorbance profile correlated to Fries products as well as uncapped phenolic groups in the sample. The methods and apparatus of the invention are suitable for monitoring of Fries products in reactions ranging in size from small scale combinatorial formats to production scale reactors. Also included in methods of the invention are univariate and multivariate analysis for prediction of linear Fries, branched Fries and uncapped phenolic end-groups in unknowns.

    摘要翻译： 本发明涉及通过熔融聚合在聚碳酸酯制造过程中原位测量感兴趣的反应组分的方法和装置。 本发明描述了用UV /可见光照射熔融聚合物样品，并产生与Fries产品相关的吸光度分布以及样品中未封端的酚基。 本发明的方法和装置适用于在尺寸从小规模组合形式到生产规模反应器的反应中监测薯条产品。 本发明方法中还包括单变量和多变量分析，用于预测未知物中的线性薯条，分枝油炸饼和未封端的酚类末端基团。