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1. 发明授权

US07132498B2 Process to make polycarbonate from bismethylsalicylcarbonate (BMSC) 有权
公开(公告)号：US07132498B2
公开(公告)日：2006-11-07
申请号：US10951574
申请日：2004-09-27
申请人： Patrick Joseph McCloskey , Norberto Silvi , Alberto Nisoli , Mark Giammattei
发明人： Patrick Joseph McCloskey , Norberto Silvi , Alberto Nisoli , Mark Giammattei
IPC分类号： C08G63/00
CPC分类号： B29C47/76 , B29C47/0009 , C08G64/307
摘要： The present invention relates to a method of preparing polycarbonate comprising the steps of: (i) introducing to an extruder through a feed port a plurality of reaction components comprising a polycarbonate oligomer, an activated carbonate residue, and a transesterification catalyst, wherein the extruder comprises the feed port, a first back vent port, and a polycarbonate exit port, wherein the feed port is located between the first back vent port and the polycarbonate exit port, and wherein the resistance to flow of the reaction components from the feed port to the first back vent port is less than or equal to the resistance to flow of the reaction components from the feed port to the polycarbonate exit port; and (ii) extruding the reaction components at one or more temperatures in a range between 100° C. and 400° C., wherein during the extrusion of the reaction components, activated carbonate residue is removed through the first back vent port, thereby preparing a polycarbonate.

2. 发明授权

US06790929B2 Method for making an aromatic polycarbonate 有权
标题翻译：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。

3. 再颁专利

USRE40697E1 Method for making an aromatic polycarbonate 有权
标题翻译：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。

4. 发明授权

US08218291B2 Monomers for preparing polycarbonate resins, methods of preparing the monomers, polycarbonate resins prepared with the monomers, and capacitors comprising the polycarbonate resins 失效
标题翻译：用于制备聚碳酸酯树脂的单体，制备单体的方法，用单体制备的聚碳酸酯树脂，以及包含聚碳酸酯树脂的电容器
公开(公告)号：US08218291B2
公开(公告)日：2012-07-10
申请号：US12751649
申请日：2010-03-31
申请人： Norberto Silvi , Gary Charles Davis , Patrick Joseph McCloskey , Sheldon Jay Shafer , Julia Lam Lee , Yang Cao , Patricia Chapman Irwin
发明人： Norberto Silvi , Gary Charles Davis , Patrick Joseph McCloskey , Sheldon Jay Shafer , Julia Lam Lee , Yang Cao , Patricia Chapman Irwin
IPC分类号： H01G9/00
CPC分类号： C08G64/12 , C07C255/53 , H01G4/18 , Y10T29/41 , Y10T29/417
摘要： A monomer and polycarbonate resin are provided, as are methods of making the monomer. The resin may be used to provide a thin film that has a higher dielectric constant and higher glass transition temperature, and similar breakdown strength and similar dissipation factor to films prepared from polycarbonate resins not so modified. The thin films, in turn, may advantageously be used to form, wholly or in part, articles such as capacitors, sensors, batteries, flexible printed circuit boards, keyboard membranes, motor/transformer insulations, cable wrappings, industrial tapes, interior coverage materials, and the like. In particular, a capacitor comprising the polycarbonate resin is also provided.
摘要翻译：提供单体和聚碳酸酯树脂，以及制备单体的方法。该树脂可用于提供具有较高介电常数和较高玻璃化转变温度的薄膜，以及与未进行改性的聚碳酸酯树脂制备的薄膜相似的击穿强度和相似的耗散因数。薄膜又可有利地用于整体或部分地形成诸如电容器，传感器，电池，柔性印刷电路板，键盘膜，电动机/变压器绝缘体，电缆包装，工业胶带，内部覆盖材料，等等。特别地，还提供了包含聚碳酸酯树脂的电容器。

5. 发明申请

US20110242729A1 Monomers for preparing polycarbonate resins, methods of preparing the monomers, polycarbonate resins prepared with the monomers, and capacitors comprising the polycarbonate resins 失效
标题翻译：用于制备聚碳酸酯树脂的单体，制备单体的方法，用单体制备的聚碳酸酯树脂，以及包含聚碳酸酯树脂的电容器
公开(公告)号：US20110242729A1
公开(公告)日：2011-10-06
申请号：US12751649
申请日：2010-03-31
申请人： Norberto Silvi , Gary Charles Davis , Patrick Joseph McCloskey , Sheldon Jay Shafer , Julia Lam Lee , Yang Cao , Patricia Chapman Irwin
发明人： Norberto Silvi , Gary Charles Davis , Patrick Joseph McCloskey , Sheldon Jay Shafer , Julia Lam Lee , Yang Cao , Patricia Chapman Irwin
IPC分类号： H01G4/08 , C08G64/04 , C07C255/50
CPC分类号： C08G64/12 , C07C255/53 , H01G4/18 , Y10T29/41 , Y10T29/417
摘要： A monomer and polycarbonate resin are provided, as are methods of making the monomer. The resin may be used to provide a thin film that has a higher dielectric constant and higher glass transition temperature, and similar breakdown strength and similar dissipation factor to films prepared from polycarbonate resins not so modified. The thin films, in turn, may advantageously be used to form, wholly or in part, articles such as capacitors, sensors, batteries, flexible printed circuit boards, keyboard membranes, motor/transformer insulations, cable wrappings, industrial tapes, interior coverage materials, and the like. In particular, a capacitor comprising the polycarbonate resin is also provided.
摘要翻译：提供单体和聚碳酸酯树脂，以及制备单体的方法。该树脂可用于提供具有较高介电常数和较高玻璃化转变温度的薄膜，以及与未进行改性的聚碳酸酯树脂制备的薄膜相似的击穿强度和相似的耗散因数。薄膜又可有利地用于整体或部分地形成诸如电容器，传感器，电池，柔性印刷电路板，键盘膜，电动机/变压器绝缘体，电缆包装，工业胶带，内部覆盖材料，等等。特别地，还提供了包含聚碳酸酯树脂的电容器。

6. 发明授权

US06506871B1 Extrusion method for making polycarbonate 有权
标题翻译：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。

7. 发明授权

US07041775B2 Method for preparing a polycarbonate oligomer mixture at low temperature for manufacturing polycarbonate 失效
标题翻译：低温制备聚碳酸酯低聚物混合物制造聚碳酸酯的方法
公开(公告)号：US07041775B2
公开(公告)日：2006-05-09
申请号：US10830163
申请日：2004-04-21
申请人： Maria Tomas Martinez , Alberto Nisoli , Alfredo Lopez Carretero , Ganesh Kailasam , David Domingo , Patrick Joseph McCloskey
发明人： Maria Tomas Martinez , Alberto Nisoli , Alfredo Lopez Carretero , Ganesh Kailasam , David Domingo , Patrick Joseph McCloskey
IPC分类号： C08G64/00
CPC分类号： C08G64/307 , B01J19/18 , B01J19/1806 , B01J19/1887 , B01J19/20 , B01J2219/00031 , B01J2219/0004 , B01J2219/00083 , B01J2219/00094 , B01J2219/00166 , B01J2219/00184 , B01J2219/00186 , C08G64/205
摘要： The present invention provides a method of making polycarbonate oligomers, polycarbonate, molded articles formed from polycarbonate, and an apparatus for making polycarbonate. An oligomer mixture is first prepared by the steps of providing an equilibration system comprising a vessel, a reaction mixture contained within the vessel, and means for mixing the reaction mixture contained within the vessel wherein the reaction mixture comprises a melted activated diaryl carbonate composition, and a catalyst present in sufficient amount to initiate an oligomerization reaction between a dihydroxy composition and the activated diaryl carbonate to form polycarbonate oligomers. The method further includes the steps of introducing a melted dihydroxy composition to the reaction mixture contained within the equilibration system, maintaining the reaction mixture contained within the vessel at an oligomerization temperature, said oligomerization temperature being below the melting point the dihydroxy composition, and sufficiently high to allow formation of a homogeneous melt within the vessel, and continuously drawing off a product stream from the equilibration system, wherein the product stream comprises a polycarbonate oligomer mixture. This polycarbonate oligomer mixture is suitably used as a feed stock for producing polycarbonate in a polycondensation system. The polycarbonate is suitably used for the preparation of molded articles.
摘要翻译：本发明提供一种制备聚碳酸酯低聚物，聚碳酸酯，由聚碳酸酯形成的模制品的方法和用于制备聚碳酸酯的装置。首先通过以下步骤制备低聚物混合物，所述步骤包括提供包含容器，容器内的反应混合物的平衡系统和用于混合包含在容器内的反应混合物的装置，其中反应混合物包含熔融的活化碳酸二芳基酯组合物和存在足够量的催化剂以引发二羟基组合物和活化的碳酸二芳基酯之间的低聚反应以形成聚碳酸酯低聚物。该方法还包括以下步骤：将熔融的二羟基组合物引入平衡系统中包含的反应混合物中，将容器内的反应混合物保持在低聚温度，所述低聚温度低于二羟基组合物的熔点，并且足够高以允许在容器内形成均匀的熔体，并且从平衡系统连续地抽出产物流，其中产物流包含聚碳酸酯低聚物混合物。该聚碳酸酯低聚物混合物适合用作在缩聚体系中制造聚碳酸酯的原料。聚碳酸酯适合用于制备模塑制品。

8. 发明授权

US06399739B1 Preparation of polycarbonate having a predetermined molecular weight and level of endcapping 有权
标题翻译：具有预定分子量和封端水平的聚碳酸酯的制备
公开(公告)号：US06399739B1
公开(公告)日：2002-06-04
申请号：US09934929
申请日：2001-08-22
申请人： Patrick Joseph McCloskey , Alberto Nisoli , Warren William Reilly
发明人： Patrick Joseph McCloskey , Alberto Nisoli , Warren William Reilly
IPC分类号： C08G6400
CPC分类号： C08G64/307
摘要： A melt method of preparing polycarbonate having a predetermined number average molecular weight and percent endcapping is described. A computerized process model is used to determine the reaction parameters to be employed in order to furnish the product polycarbonate possessing the desired Mn and %EC. Reaction parameters of importance include a suitable starting molar ratio of diaryl carbonate to dihydroxy aromatic compound, the most appropriate reaction time, reaction temperature and pressure ranges. The target polycarbonate is then prepared using reaction parameters indicated by the process model in a reactor which forms an element of the process model. Characteristics of the reactor which may be included in the process model include agitation rate and reflux ratio during the distillative removal of hydroxy aromatic compound formed as a by-product during the polymerization.
摘要翻译：描述了制备具有预定数均分子量和百分比封端的聚碳酸酯的熔融方法。使用计算机化过程模型来确定要使用的反应参数，以便提供具有期望的Mn和％EC的产物聚碳酸酯。重要的反应参数包括碳酸二芳基酯与二羟基芳族化合物的合适起始摩尔比，最合适的反应时间，反应温度和压力范围。然后使用形成过程模型元素的反应器中由过程模型指示的反应参数制备目标聚碳酸酯。可以包括在过程模型中的反应器的特征包括在蒸馏除去在聚合期间作为副产物形成的羟基芳族化合物的搅拌速率和回流比。

9. 发明授权

US06300460B1 Mixed dialkali metal salts of sulfuric acid containing at least one cesium equivalent as polymerization catalysts 有权
标题翻译：含有至少一种铯当量的硫酸的混合二碱金属盐作为聚合催化剂
公开(公告)号：US06300460B1
公开(公告)日：2001-10-09
申请号：US09612652
申请日：2000-07-06
申请人： Patrick Joseph McCloskey , Timothy Brydon Burnell , Paul Michael Smigelski, Jr. , Alberto Nisoli
发明人： Patrick Joseph McCloskey , Timothy Brydon Burnell , Paul Michael Smigelski, Jr. , Alberto Nisoli
IPC分类号： C08G6400
CPC分类号： C08G64/307
摘要： This invention relates to mixed dialkali metal salts of sulfuric acid containing at least one cesium equivalent useful in catalyst systems in melt polymerizations. The catalysts provide product with low branching side reaction products and good properties.
摘要翻译：本发明涉及在熔融聚合中含有可用于催化剂体系的至少一种铯当量的硫酸混合二碱金属盐。催化剂提供具有低支化反应产物和良好性能的产物。

10. 发明授权

US06569985B2 Method for making polycarbonate 有权
标题翻译：制作聚碳酸酯的方法
公开(公告)号：US06569985B2
公开(公告)日：2003-05-27
申请号：US09924137
申请日：2001-08-08
申请人： Patrick Joseph McCloskey , Alberto Nisoli , Warren William Reilly
发明人： Patrick Joseph McCloskey , Alberto Nisoli , Warren William Reilly
IPC分类号： C08G6400
CPC分类号： C08G64/307
摘要： Polycarbonates having a high level of endcapping and containing a low level of Fries rearrangement product are prepared from dihydroxy aromatic compounds, such as bisphenol A, and diaryl carbonates such as diphenyl carbonate in a two stage process involving a tetraalkyl phosphonium carboxylate catalyzed oligomerization of the reactants in a first reaction stage followed by the addition of an alkali metal hydroxide co-catalyst in the second stage of the polymerization reaction. The late addition of the co-catalyst provides improved polymerization reaction rates as judged by higher polycarbonate molecular weights. The amount of alkali metal hydroxide co-catalyst is small thus avoiding the formation of excessive amounts of Fries product. The method has been used to provide Fries product levels between 200 and 800 parts per million in polycarbonates having Mn values between 7,500 and 8,500 Daltons.
摘要翻译：具有高水平的封端并含有低含量的Fries重排产物的聚碳酸酯由二羟基芳族化合物如双酚A和碳酸二芳基酯如碳酸二苯酯在涉及四烷基鏻羧酸酯催化的反应物低聚的两步法中制备在第一反应阶段，然后在聚合反应的第二阶段加入碱金属氢氧化物助催化剂。通过较高的聚碳酸酯分子量判断，辅助催化剂的晚期添加提供了改进的聚合反应速率。碱金属氢氧化物助催化剂的量很小，从而避免形成过量的油炸产品。该方法已经被用于在Mn值在7,500和8,500道尔顿之间的聚碳酸酯中提供200至800ppm之间的Fries产品水平。

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