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    • 5. 发明授权
    • Extrusion method for making polycarbonate
    • 制造聚碳酸酯的挤出方法
    • US06420512B1
    • 2002-07-16
    • US09911439
    • 2001-07-24
    • Patrick Joseph McCloskeyJames DayPaul Michael SmigelskiJohn Lester MaxamJohn Aibangbee Osaheni
    • Patrick Joseph McCloskeyJames DayPaul Michael SmigelskiJohn Lester MaxamJohn Aibangbee Osaheni
    • C08G6400
    • C08G64/307
    • 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.
    • 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。
    • 10. 发明授权
    • Method of polycarbonate preparation by solid state polymerization
    • 通过固态聚合制备聚碳酸酯的方法
    • US06518391B1
    • 2003-02-11
    • US09911505
    • 2001-07-24
    • Patrick Joseph McCloskeyJames DayPaul Michael Smigelski, Jr.Timothy Brydon Burnell
    • Patrick Joseph McCloskeyJames DayPaul Michael Smigelski, Jr.Timothy Brydon Burnell
    • C08G6400
    • C08G64/307C08G64/06
    • 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.
    • 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。