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1. 发明授权

US06333394B1 Copolycarbonate preparation by solid state polymerization 有权
标题翻译：通过固态聚合制备共聚碳酸酯
公开(公告)号：US06333394B1
公开(公告)日：2001-12-25
申请号：US09379234
申请日：1999-08-23
申请人： Christian Maria Emile Bailly , Bhaskar Bhairavnath Idage , Swaminathan Sivaram , Nayaku Nivarati Chavan , Rein Mollerus Faber , Shamal Karunakaran Menon , Gautam Chatterjee , Godavarthi Satyana Varadarajan , James Day , Patrick Joseph McCloskey , Joseph Anthony King, Jr. , Arun Savalaram Jadhav
发明人： Christian Maria Emile Bailly , Bhaskar Bhairavnath Idage , Swaminathan Sivaram , Nayaku Nivarati Chavan , Rein Mollerus Faber , Shamal Karunakaran Menon , Gautam Chatterjee , Godavarthi Satyana Varadarajan , James Day , Patrick Joseph McCloskey , Joseph Anthony King, Jr. , Arun Savalaram Jadhav
IPC分类号： C08G6400
CPC分类号： C08G64/20 , C08G64/06 , C08G64/14 , C08G64/183 , C08G64/307
摘要： Copolycarbonates containing such structural units as birefringence-reducing or “soft block” units are prepared by conducting a reaction, such as melt polymerization or equilibration, between a precursor polycarbonate and a monomer, polycarbonate oligomer or high molecular weight polycarbonate which is a source of other structural units. The crystallinity of the resulting precursor copolycarbonate or one of the reagents employed in its preparation is enhanced and the precursor copolycarbonate is subjected to solid state polymerization.
摘要翻译：通过在前体聚碳酸酯和单体，聚碳酸酯低聚物或高分子量聚碳酸酯之间进行诸如熔融聚合或平衡的反应来制备含有诸如双折射降低或“软嵌段”单元的结构单元的共聚碳酸酯结构单位。得到的前体共聚碳酸酯或其制备中使用的试剂之一的结晶度提高，前体共聚碳酸酯进行固态聚合。

2. 发明授权

US6143859A Copolycarbonate preparation by solid state polymerization 有权
标题翻译：通过固态聚合制备共聚碳酸酯
公开(公告)号：US6143859A
公开(公告)日：2000-11-07
申请号：US370433
申请日：1999-08-09
申请人： Gautam Chatterjee , Godavarthi Satyanarayana Varadarajan , James Day , Patrick Joseph McCloskey , Bhaskar Bhairavnath Idage , Joseph Anthony King, Jr. , Arun Savalaram Jadhav
发明人： Gautam Chatterjee , Godavarthi Satyanarayana Varadarajan , James Day , Patrick Joseph McCloskey , Bhaskar Bhairavnath Idage , Joseph Anthony King, Jr. , Arun Savalaram Jadhav
IPC分类号： C08G64/06 , C08G64/18 , C08G64/20 , C08G64/00
CPC分类号： C08G64/20 , C08G64/06 , C08G64/183
摘要： Copolycarbonates containing such structural units as birefringence-reducing or "soft block" units are prepared by conducting a reaction, such as melt polymerization or equilibration, between a precursor polycarbonate and a monomer, polycarbonate oligomer or high molecular weight polycarbonate which is a source of other structural units. The crystallinity of the resulting precursor copolycarbonate or one of the reagents employed in its preparation is enhanced and the precursor copolycarbonate is subjected to solid state polymerization.
摘要翻译：通过在前体聚碳酸酯和单体，聚碳酸酯低聚物或高分子量聚碳酸酯之间进行诸如熔融聚合或平衡的反应来制备含有诸如双折射降低或“软嵌段”单元的结构单元的共聚碳酸酯结构单位。得到的前体共聚碳酸酯或其制备中使用的试剂之一的结晶度提高，前体共聚碳酸酯进行固态聚合。

3. 发明授权

US06187895B1 Method for preparing polymers by solid state polymerization 有权
标题翻译：通过固态聚合制备聚合物的方法
公开(公告)号：US06187895B1
公开(公告)日：2001-02-13
申请号：US09370435
申请日：1999-08-09
申请人： Godavarthi Satyana Varadarajan , James Day , Bhaskar Bhairavnath Idage
发明人： Godavarthi Satyana Varadarajan , James Day , Bhaskar Bhairavnath Idage
IPC分类号： C08G6400
CPC分类号： C08G64/20 , C08G63/80
摘要： Solid state polymerization of polycarbonates and polyesters is preceded by a step of contacting particles of an amorphous precursor polymer with a particulate material, typically a crystallized polycarbonate, which prevents adherence of the precursor polymer particles to each other. It is then possible to perform the solid state polymerization step without crystallizing the precursor polymer.
摘要翻译：聚碳酸酯和聚酯的固态聚合之前是将无定形前体聚合物的颗粒与颗粒材料（通常为结晶的聚碳酸酯）接触的步骤，其阻止前体聚合物颗粒相互粘附。然后可以进行固态聚合步骤而不使前体聚合物结晶。

4. 发明授权

US06248858B1 Method for conducting solid state polymerization of polycarbonates 失效
标题翻译：聚碳酸酯的固态聚合方法
公开(公告)号：US06248858B1
公开(公告)日：2001-06-19
申请号：US09192350
申请日：1998-11-16
申请人： James Day , Godavarthi Satyana Varadarajan
发明人： James Day , Godavarthi Satyana Varadarajan
IPC分类号： C08G6400
CPC分类号： C08G64/20 , C08G63/64 , C08G64/40
摘要： Polymerization of polycarbonates is performed by first enhancing the crystallinity of a precursor polycarbonate, such as an oligomer, by contact in pellet form with an alkanol in the liquid or vapor state as non-solvent, and then conducting solid state polymerization in a stream of inert gas such as nitrogen. The solid state polymerization operation includes a stage of heating at a constant temperature in the range of about 215-225° C., optionally combined with a first heating stage at a constant temperature in the range of about 180-190° C. The method is adaptable to continuous operation and produces a polycarbonate having a number average molecular weight, as determined by gel permeation chromatography relative to polystyrene, of at least 15,000.
摘要翻译：聚碳酸酯的聚合通过首先通过以颗粒形式与液体或蒸气状态的链烷醇作为非溶剂接触来提高前体聚碳酸酯如低聚物的结晶度，然后在惰性气流中进行固态聚合气体如氮气。固态聚合操作包括在约215-225℃的恒定温度下加热的阶段，任选地在约180-190℃的恒定温度下与第一加热阶段组合。方法适用于连续操作，并且通过凝胶渗透色谱法相对于聚苯乙烯产生数均分子量为至少15,000的聚碳酸酯。

5. 发明授权

US6140461A Method for preparing solid state polycarbonates in a unitary series of operations 有权
标题翻译：在一系列操作中制备固态聚碳酸酯的方法
公开(公告)号：US6140461A
公开(公告)日：2000-10-31
申请号：US371449
申请日：1999-08-10
申请人： James Day , Bhaskar Bhairavnath Idage
发明人： James Day , Bhaskar Bhairavnath Idage
IPC分类号： C08G64/20 , C08G59/00
CPC分类号： C08G64/20
摘要： Amorphous precursor polycarbonates, such as oligomers, are converted to high molecular weight polycarbonates in a unitary series of operations that includes contact with an alkanol having a boiling point up to about 180.degree. C. and heating the resulting wetted particles so as to effect solid state polymerization. Heating is at progressively increasing temperatures from below the boiling point of the alkanol to a final level between the Tg and the melting temperature of said enhanced crystallinity polycarbonate.
摘要翻译：无定形前体聚碳酸酯，例如低聚物，以一系列操作转化为高分子量聚碳酸酯，其包括与沸点高达约180℃的链烷醇接触，并加热得到的润湿颗粒以实现固态聚合。加热处于逐渐升高的温度，从低于烷醇的沸点到所述增强的结晶度聚碳酸酯的Tg和熔融温度之间的最终水平。

6. 发明授权

US6031063A Method for enhancing crystallinity of polycarbonates 失效
标题翻译：提高聚碳酸酯结晶度的方法
公开(公告)号：US6031063A
公开(公告)日：2000-02-29
申请号：US370434
申请日：1999-08-09
申请人： James Day , Bhaskar Bhairavnath Idage , Andrew James Caruso
发明人： James Day , Bhaskar Bhairavnath Idage , Andrew James Caruso
IPC分类号： C08G64/20 , C08G64/00
CPC分类号： C08G64/20
摘要： The crystallinity of an amorphous precursor polycarbonate is enhanced by contact in the liquid or vapor state with a non-solvent which may be water, an alkanol or a mixture thereof and which is dialkyl carbonate-free. Contact temperatures are at least about 75.degree. C. and are further defined by the relationshipT.sub.c .gtoreq.T.sub.b -z,wherein T.sub.c is the contact temperature, T.sub.b is the boiling point of the non-solvent at the contact pressure employed (both in degrees C.) and z is a constant whose value is 60.
摘要翻译：无定形前体聚碳酸酯的结晶度通过在液体或蒸汽状态下与非溶剂（其可以是水，链烷醇或其混合物）接触而提高，并且是无碳酸二烷基酯。接触温度至少约为75℃，并且进一步由关系式T> = Tb-z定义，其中Tc是接触温度，Tb是所用接触压力下非溶剂的沸点（均以度数计） C），z是值为60的常数。

7. 发明授权

US06420512B1 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：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。

8. 发明授权

US06809817B2 Method and apparatus for in situ determination of molten polycarbonate composition using electronic absorption spectroscopy 失效
标题翻译：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。

9. 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。

10. 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。

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