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81. 发明授权

US07115700B2 Method of polycarbonate preparation 有权
公开(公告)号：US07115700B2
公开(公告)日：2006-10-03
申请号：US11133827
申请日：2005-05-19
申请人： James Anthony Cella , Jan Henk Kamps , Jan Pleun Lens , Kathryn Lynn Longley , Patrick Joseph McCloskey , Narayan Ramesh , Warren William Reilly , Paul Michael Smigelski, Jr. , Marc Brian Wisnudel
发明人： James Anthony Cella , Jan Henk Kamps , Jan Pleun Lens , Kathryn Lynn Longley , Patrick Joseph McCloskey , Narayan Ramesh , Warren William Reilly , Paul Michael Smigelski, Jr. , Marc Brian Wisnudel
IPC分类号： C08G63/00
CPC分类号： C08G63/64 , C08G64/04 , C08G64/14 , C08G64/307 , C08L23/00 , C08L67/00 , C08L69/00 , C08L69/005 , C08L2666/18 , C08L2666/06
摘要： Polycarbonates containing low or undetectable levels of Fries rearrangement products and comprising repeat units derived from one or more of resorcinol, hydroquinone, methylhydroquinone, bisphenol A, and 4,4′-biphenol have been prepared by the melt reaction of one or more of the aforementioned dihydroxy aromatic compounds with an ester-substituted diaryl carbonate such as bis-methyl salicyl carbonate. Low, or in many instances undetectable, levels of Fries rearrangement products are found in the product polycarbonates obtained as the combined result of a highly effective catalyst system which suppresses the Fries reaction and the use of lower melt polymerization temperatures relative to temperatures required for the analogous polymerization reactions using diphenyl carbonate.

82. 发明授权

US06960641B2 Method of making block copolymers by solid state polymerization 有权
标题翻译：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。

83. 发明授权

US06900283B2 Method for making stable, homogeneous melt solutions 有权
标题翻译：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
申请人： Narayan Ramesh , Patrick Joseph McCloskey , Kathryn Lynn Longley
发明人： Narayan Ramesh , Patrick Joseph McCloskey , Kathryn Lynn Longley
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。

84. 发明授权

US06797802B2 Method of polycarbonate preparation 有权
标题翻译：聚碳酸酯制备方法
公开(公告)号：US06797802B2
公开(公告)日：2004-09-28
申请号：US10265419
申请日：2002-10-07
申请人： Patrick Joseph McCloskey , Warren William Reilly
发明人： Patrick Joseph McCloskey , Warren William Reilly
IPC分类号： C08G6400
CPC分类号： C08G64/307
摘要： The present invention provides a method of preparing polycarbonate, said method comprising (A) oligomerising in the presence of a catalyst at least one dihydroxyaromatic compound at a temperature in a range between about 220-280° C. and a pressure in a range between 180 mbar and 20 mbar, said catalyst comprising a tetraarylphosphonium compound and optionally a co-catalyst, to provide an oligomeric polycarbonate having a number average molecular weight, Mn, in a range between about 1000 and about 6000 daltons; and (B) in a second step heating the oligomeric polycarbonate formed in step (A) at a temperature range between about 280 and about 310° C. and a pressure in a range between about 15 mbar and about 0.1 mbar, to provide a polycarbonate having a weight average molecular weight, in a range between about 15,000 and about 50,000 daltons, said product polycarbonate comprising less than 1000 parts per million Fries product.
摘要翻译：本发明提供一种制备聚碳酸酯的方法，所述方法包括（A）在催化剂存在下，在至少一种二羟基芳族化合物的存在下，在约220-280℃之间的温度和180℃ 所述催化剂包含四芳基鏻化合物和任选的助催化剂，以提供数均分子量Mn在约1000至约6000道尔顿范围内的低聚聚碳酸酯; 和（B）在步骤（A）中形成的低聚聚碳酸酯在约280℃至约310℃之间的温度范围和约15毫巴至约0.1毫巴范围内的压力下进行加热，以提供聚碳酸酯重均分子量在约15,000至约50,000道尔顿之间的范围内，所述产品聚碳酸酯包含小于1000份百万份薯条产品。

85. 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。

86. 发明授权

US06723823B2 Method of polycarbonate preparation 有权
标题翻译：聚碳酸酯制备方法
公开(公告)号：US06723823B2
公开(公告)日：2004-04-20
申请号：US10167965
申请日：2002-06-12
申请人： Patrick Joseph McCloskey , Warren William Reilly , Brian James Grimmond
发明人： Patrick Joseph McCloskey , Warren William Reilly , Brian James Grimmond
IPC分类号： C08G600
CPC分类号： C08G64/307
摘要： Mixed alkali metal salts of phosphoric acid in combination with a co-catalyst such as tetramethylammonium hydroxide (TMAH) are excellent transesterification catalysts for use in the preparation of polycarbonate from bisphenol A and diphenyl carbonate. The mixed alkali metal phosphate salts were shown by kinetic measurements made on a model system composed of p-tert-octylphenol and bis(p-cumylphenyl) carbonate to be inherently more potent catalysts than salts of phosphoric acid comprising a single alkali metal ion. In addition to providing higher rates of polymerization, the new catalysts were shown to provide polycarbonates containing reduced levels of Fries rearrangement product relative to polymerization reactions catalyzed by conventional catalyst systems such as sodium hydroxide together with TMAH co-catalyst.
摘要翻译：磷酸的混合碱金属盐与诸如四甲基氢氧化铵（TMAH）的助催化剂组合是用于从双酚A和碳酸二苯酯制备聚碳酸酯的优异的酯交换催化剂。混合的碱金属磷酸盐通过在由对叔辛基苯酚和双（对枯基苯基）碳酸酯组成的模型系统上进行的动力学测量显示为比含有单一碱金属离子的磷酸盐更具有效力的催化剂。除了提供更高的聚合速率之外，新催化剂显示出提供聚碳酸酯，其含有相对于常规催化剂体系如氢氧化钠与TMAH助催化剂催化的聚合反应的降低水平的Fries重排产物。

87. 发明授权

US06576801B2 Process for the neutralization of residual acid species in crude dihydric phenols 有权
公开(公告)号：US06576801B2
公开(公告)日：2003-06-10
申请号：US09683866
申请日：2002-02-25
申请人： Paul Michael Smigelski, Jr. , Timothy Brydon Burnell , Patrick Joseph McCloskey
发明人： Paul Michael Smigelski, Jr. , Timothy Brydon Burnell , Patrick Joseph McCloskey
IPC分类号： C07C3768
CPC分类号： C07C37/86 , C07C39/16
摘要： The present invention relates to a method of neutralizing residual acid species in crude dihydric phenol comprising the step of introducing a thermally stable organic base selected from the group consisting of tetraalkyl phosphonium hydroxides, tetraorganophosphonium carboxylic acid salts, or a mixture thereof into the crude dihydric phenol.

88. 发明授权

US06518391B1 Method of polycarbonate preparation by solid state polymerization 失效
标题翻译：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。

89. 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。

90. 发明授权

US06492485B1 Redistributed polycarbonate resin 有权
标题翻译：再分散聚碳酸酯树脂
公开(公告)号：US06492485B1
公开(公告)日：2002-12-10
申请号：US09547372
申请日：2000-04-11
申请人： Eric Thomas Gohr , Chad David Mistele , Michael F. Shannon , Vijaykumar Hanagandi , Devesh Mathur , Patrick Joseph McCloskey
发明人： Eric Thomas Gohr , Chad David Mistele , Michael F. Shannon , Vijaykumar Hanagandi , Devesh Mathur , Patrick Joseph McCloskey
IPC分类号： C08G6400
CPC分类号： B29C47/92 , B29C47/0021 , B29C2947/9218 , B29C2947/922 , B29C2947/92209 , B29C2947/92314 , B29C2947/92542 , B29C2947/9259 , B29C2947/92695 , B29C2947/92704 , B29C2947/92885 , B29C2947/92952 , C08G64/42
摘要： The application relates to methods for producing a polycarbonate resin having a narrowed molecular weight distribution, specifically, the application relates to the use of a redistribution catalyst and a feedback loop control mechanism to prepare narrow molecular weight distribution resin.
摘要翻译：本申请涉及具有窄分子量分布的聚碳酸酯树脂的制造方法，具体地说，涉及使用再分布催化剂和反馈回路控制机构来制备窄分子量分布树脂。

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