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公开(公告)号：US06518391B1
公开(公告)日：2003-02-11
申请号：US09911505
申请日：2001-07-24
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。
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12.发明授权Mixed dialkali metal salts of sulfuric acid containing at least one cesium equivalent as polymerization catalysts 有权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。
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公开(公告)号：US06228973B1
公开(公告)日：2001-05-08
申请号：US09584984
申请日：2000-06-02
申请人： Patrick Joseph McCloskey , Timothy Brydon Burnell , Paul Michael Smigelski, Jr. , Johan Pieter Anna Heuts , Hendricus Franciscus Zirkzee
发明人： Patrick Joseph McCloskey , Timothy Brydon Burnell , Paul Michael Smigelski, Jr. , Johan Pieter Anna Heuts , Hendricus Franciscus Zirkzee
IPC分类号： C08G6400
CPC分类号： C08G64/307
摘要： A method of preparing polycarbonate by the melt process comprising the steps of: a) melting a dihydric phenol and a diester of carbonic acid for a time and at a temperature sufficient to form a melt; and thereafter introducing a catalyst composition comprising a tetraorganophosphonium salt or a derivative thereof and 1) an alkali and/or alkali earth metal compound or derivative thereof or 2) a less active alkali and/or alkali earth metal derivative thereof into the melt; and b) oligomerizing the product from step a) to a number average molecular weight of from about 3000 to about 7500; and c) polymerizing the product from step b) to a number average molecular weight of from about 16,000 to about 35,000.
摘要翻译： 通过熔融法制备聚碳酸酯的方法包括以下步骤：a）在足以形成熔体的时间和温度下熔化二元酚和碳酸二酯; 然后引入含有四有机鏻盐或其衍生物的催化剂组合物，和1）碱金属和/或碱土金属化合物或其衍生物，或2）其活性较低的碱金属和/或碱土金属衍生物; 和b）使来自步骤a）的产物低聚至约3000至约7500的数均分子量; 和c）将来自步骤b）的产物聚合至数均分子量为约16,000至约35,000。
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公开(公告)号：US06891015B2
公开(公告)日：2005-05-10
申请号：US10216512
申请日：2002-08-12
摘要： High yields of ester-substituted diary carbonates such as bis-methyl salicyl carbonate were obtained by the condensation of ester-substituted phenols with phosgene in the presence of a phase transfer catalyst (PTC) and optionally a tertiary amine catalyst in a solvent free reaction system comprising an aqueous phase held at a pH of 8.3 or higher. The optimized conditions of the present invention use an excess of ester-substituted phenol relative to phosgene and high conversion of phosgene to ester-substituted diaryl carbonate is observed. The product ester-substituted diaryl carbonate may be conveniently isolated as a solid by filtration or as a liquid in which the excess ester-substituted phenols serves as solvent. The method represents an attractive route for the manufacture of bis methyl salicyl carbonate and ester-substituted diaryl carbonates generally. The ester-substituted diaryl carbonates are useful for the preparation and modification of polycarbonates.
摘要翻译： 通过在相转移催化剂（PTC）和任选的叔胺催化剂存在下，在无溶剂反应体系中，酯取代的酚与光气的缩合得到高收率的酯取代的二元碳酸酯，例如碳酸双甲基水杨酸酯 包含保持在8.3或更高的pH的水相。 本发明的优化条件相对于光气使用过量的酯取代的苯酚，观察到光气转化为酯取代的碳酸二芳基酯的高转化率。 产物酯取代的碳酸二芳基酯可以通过过滤或作为其中过量的酯取代的酚用作溶剂的液体方便地分离为固体。 该方法通常用于制造碳酸双甲基水杨酸酯和酯取代的二芳基碳酸酯的有吸引力的途径。 酯取代的碳酸二芳基酯可用于聚碳酸酯的制备和改性。
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公开(公告)号：US06469192B1
公开(公告)日：2002-10-22
申请号：US09911527
申请日：2001-07-24
IPC分类号： C07C6996
摘要： High yields of ester-substituted diary carbonates such as bis-methyl salicyl carbonate were obtained by the condensation of ester-substituted phenols with phosgene in the presence of a phase transfer catalyst (PTC) and optionally a tertiary amine catalyst in a solvent free reaction system comprising an aqueous phase held at a pH of 8.3 or higher. The optimized conditions of the present invention use an excess of ester-substituted phenol relative to phosgene and high conversion of phosgene to ester-substituted diaryl carbonate is observed. The product ester-substituted diaryl carbonate may be conveniently isolated as a solid by filtration or as a liquid in which the excess ester-substituted phenols serves as solvent. The method represents an attractive route for the manufacture of bis methyl salicyl carbonate and ester-substituted diaryl carbonates generally.
摘要翻译： 通过在相转移催化剂（PTC）和任选的叔胺催化剂存在下，在无溶剂反应体系中，酯取代的酚与光气的缩合得到高收率的酯取代的二元碳酸酯，例如碳酸双甲基水杨酸酯 包含保持在8.3或更高的pH的水相。 本发明的优化条件相对于光气使用过量的酯取代的苯酚，观察到光气转化为酯取代的碳酸二芳基酯的高转化率。 产物酯取代的碳酸二芳基酯可以通过过滤或作为其中过量的酯取代的酚用作溶剂的液体方便地分离为固体。 该方法通常用于制造碳酸双甲基水杨酸酯和酯取代的二芳基碳酸酯的有吸引力的途径。
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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.
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。
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17.发明授权Method and apparatus for nondestructive determination of polymer hydrolytic stability 失效无损检测聚合物水解稳定性的方法和装置公开(公告)号：US06576911B1
公开(公告)日：2003-06-10
申请号：US09690478
申请日：2000-10-19
IPC分类号： B05D512
CPC分类号： G01N21/64
摘要： In an embodiment, the present invention is directed a method and an apparatus comprising irradiating a polymer sample with at least one wavelength of substantially monochromatic light and monitoring radiation emitted by the polymer sample which is correlated to sample hydrolysis and a change in polymer molecular weight.
摘要翻译： 在一个实施方案中，本发明涉及一种方法和设备，包括用至少一个基本上单色光的波长照射聚合物样品并监测与样品水解相关的聚合物样品发射的辐射和聚合物分子量的变化。
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公开(公告)号：US07541420B2
公开(公告)日：2009-06-02
申请号：US11688533
申请日：2007-03-20
申请人： Sjef Berndsen , Hans Peter Brack , Bernd Jansen , Jan Henk Kamps , Edward Kung , Daniel Lowery , Patrick Joseph McCloskey , Paul Michael Smigelski, Jr. , Dennis Willemse
发明人： Sjef Berndsen , Hans Peter Brack , Bernd Jansen , Jan Henk Kamps , Edward Kung , Daniel Lowery , Patrick Joseph McCloskey , Paul Michael Smigelski, Jr. , Dennis Willemse
CPC分类号： C08G64/307 , C08G64/14
摘要： A method for preparing a molded article includes the steps of (a) obtaining a polycarbonate resin and (b) molding the polycarbonate resin. The polycarbonate resin is made by a transesterification reaction using an activated diaryl carbonate such that the polycarbonate is susceptible to the formation of internal ester linkages (IEL). The method occurs with the proviso that the polycarbonate resin, the molding conditions or both are selected to control the amount of IEL formed during the molding process to a level of less than 0.4 mol %.
摘要翻译： 制备模塑制品的方法包括以下步骤：（a）获得聚碳酸酯树脂和（b）模塑聚碳酸酯树脂。 聚碳酸酯树脂通过使用活化的碳酸二芳基酯的酯交换反应制备，使得聚碳酸酯容易形成内部酯键（IEL）。 该方法发生，条件是选择聚碳酸酯树脂，成型条件或两者以控制在模制过程中形成的IEL的量至小于0.4mol％的水平。
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公开(公告)号：US07498400B2
公开(公告)日：2009-03-03
申请号：US11427885
申请日：2006-06-30
申请人： Bernd Jansen , Jan Henk Kamps , Edward Kung , Patrick Joseph McCloskey , Paul Michael Smigelski, Jr.
发明人： Bernd Jansen , Jan Henk Kamps , Edward Kung , Patrick Joseph McCloskey , Paul Michael Smigelski, Jr.
CPC分类号： C08G64/14 , C08G64/307
摘要： Polycarbonates incorporating terminal carbonate groups derived from ester-substituted activated carbonates in a transesterification process have unfavorable properties with respect to color, hydrolytic stability and thermal stability, particularly when the polycarbonate containing such end groups is molded. The number of activated carbonate end groups formed during the melt transesterification formation of polycarbonate can be reduced by reacting a dihydroxy compound with an activated diaryl carbonate in the presence of an esterification catalyst to produce a polycarbonate, in the presence of a monohydroxy chainstopper such as para-cumyl phenol in an amount that results in 35 to 65 mol % of the end groups being derived from the monohydroxy chainstopper. Suitably, the reactants are provided such that the molar ratio of activated diaryl carbonate to the total of dihydroxy compound plus ½ the chainstopping reagent that is less than 1.
摘要翻译： 在酯交换方法中，衍生自酯取代的活性碳酸酯的末端碳酸酯基团的聚碳酸酯在颜色，水解稳定性和热稳定性方面具有不利的性质，特别是当含有这样的端基的聚碳酸酯被成型时。 在聚碳酸酯的熔融酯交换形成期间形成的活化碳酸酯端基的数量可以通过在酯化催化剂的存在下使二羟基化合物与活化的碳酸二芳基酯反应来制备聚碳酸酯，在单羟基链断裂剂例如对 - 辛基苯酚，其量导致35-65mol％端基衍生自单羟基链断裂剂。 适当地，提供反应物使得活化的碳酸二芳基酯与二羟基化合物的总和加上1/2的阻滞剂的摩尔比小于1。
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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。
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