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    • 6. 发明授权
    • Polycarbonate-polyorganosiloxane copolymer and method for continuously producing same
    • 聚碳酸酯 - 聚有机硅氧烷共聚物及其连续制造方法
    • US09371419B2
    • 2016-06-21
    • US14411275
    • 2013-06-26
    • IDEMITSU KOSAN CO., LTD.
    • Yukiko NagaoYasuhiro IshikawaHiroaki Motegi
    • C08G64/18C08G64/22C08L83/10C08G64/24C08G64/40C08G77/38C08G77/34C08G77/448
    • C08G77/448C08G64/186C08G64/22C08G64/24C08G64/406C08G77/16C08G77/34C08G77/38C08K5/07C08K5/13C08L83/06C08L83/10
    • Provided are a polycarbonate-polyorganosiloxane copolymer having a carbon tetrachloride concentration of less than 4 ppm by mass, and the following production method for producing the polycarbonate-polyorganosiloxane copolymer. More specifically, provided is a method of continuously producing a polycarbonate-polyorganosiloxane copolymer, the method comprising the steps of: (A) continuously or intermittently taking a polymerization reaction liquid, which is obtained by polymerizing a dihydric phenol compound, a carbonate precursor, and a specific polyorganosiloxane in the presence of an alkaline compound aqueous solution and a water-insoluble organic solvent, out of a reactor; (B) separating the polymerization reaction liquid taken out in the step (A) into an aqueous phase and a water-insoluble organic solvent phase; (C) washing the water-insoluble organic solvent phase separated in the step (B), followed by separation thereof into an aqueous phase and a water-insoluble organic solvent phase; (D) concentrating the water-insoluble organic solvent phase separated in the step (C); and (E) recovering part or all of the water-insoluble organic solvent removed by evaporation in the step (D), followed by distillation purification thereof in a distillation column, the water-insoluble organic solvent obtained in the step (E) being reused as at least part of the water-insoluble organic solvent in the step (A) or as an extraction solvent for the aqueous phase separated in the step (B), or as both thereof, in the step (E), the distillation purification being performed while a concentration of the polycarbonate-polyorganosiloxane copolymer in a column bottom liquid of the distillation column is controlled to 6% by mass or less.
    • 本发明提供四氯化碳浓度小于4质量ppm的聚碳酸酯 - 聚有机硅氧烷共聚物,以及以下制造聚碳酸酯 - 聚有机硅氧烷共聚物的制造方法。 更具体地说,提供连续制造聚碳酸酯 - 聚有机硅氧烷共聚物的方法,该方法包括以下步骤:(A)连续地或间歇地取出聚合反应液,该聚合反应液是通过使二元酚化合物,碳酸酯前体和 在碱性化合物水溶液和水不溶性有机溶剂的存在下,从反应器中除去特定的聚有机硅氧烷; (B)将步骤(A)中取出的聚合反应液分离成水相和水不溶性有机溶剂相; (C)洗涤步骤(B)中分离的水不溶性有机溶剂相,然后分离成水相和水不溶性有机溶剂相; (D)浓缩步骤(C)中分离的水不溶性有机溶剂相; 和(E)回收在步骤(D)中通过蒸发除去的部分或全部水不溶性有机溶剂,然后在蒸馏塔中蒸馏纯化,将步骤(E)中得到的水不溶性有机溶剂重新使用 作为步骤(A)中的至少一部分水不溶性有机溶剂或作为在步骤(B)中分离的水相的提取溶剂,或两者在步骤(E)中,蒸馏纯化为 在将蒸馏塔的塔底液中的聚碳酸酯 - 聚有机硅氧烷共聚物的浓度控制在6质量%以下的同时进行。
    • 7. 发明授权
    • Method for continuous production of polycarbonate-polyorganosiloxane copolymer
    • US09359473B2
    • 2016-06-07
    • US14434486
    • 2013-10-10
    • IDEMITSU KOSAN CO., LTD.
    • Yukiko NagaoYasuhiro IshikawaHiroaki Motegi
    • C08G64/18C08G77/448C08G64/24C08G77/04C08G64/20
    • C08G64/186C08G64/205C08G64/24C08G77/04C08G77/448
    • Provided is a method for economically and stably producing a high-quality polycarbonate-polyorganosiloxane copolymer excellent in, for example, transparency and impact resistance in a continuous manner. Specifically, provided is a method of continuously producing a polycarbonate-polyorganosiloxane copolymer, the method including a step (A) of continuously or intermittently taking a polymerization reaction liquid, which is obtained by polymerizing a dihydric phenol-based compound, a carbonate precursor, and a polyorganosiloxane in the presence of an alkaline compound aqueous solution and a water-insoluble organic solvent, out of a reactor, the step (A) including the following step (a-1) and the following step (a-2), the method using a dissolution tank for dissolving the dihydric phenol-based compound in the alkaline compound aqueous solution to prepare an alkaline compound aqueous solution of the dihydric phenol-based compound to be used in each of both the step (a-1) and the step (a-2), the step (a-2) including, before mixing a polycarbonate oligomer and the dihydric phenol-based compound, mixing the alkaline compound aqueous solution and the alkaline compound aqueous solution of the dihydric phenol-based compound prepared in the dissolution tank: step (a-1): a step of mixing the alkaline compound aqueous solution of the dihydric phenol-based compound prepared in the dissolution tank and the polycarbonate precursor, followed by a reaction of the mixture in the presence of the water-insoluble organic solvent to produce the polycarbonate oligomer; and step (a-2): a step of continuously or intermittently taking the polymerization reaction liquid, which is obtained by mixing the alkaline compound aqueous solution of the dihydric phenol-based compound prepared in the dissolution tank, the polycarbonate oligomer obtained in the step (a-1), and the polyorganosiloxane, and polymerizing the mixture in the presence of the water-insoluble organic solvent, out of the reactor.
    • 8. 发明申请
    • CONTINUOUS PRODUCTION METHOD FOR POLYCARBONATE-POLYORGANOSILOXANE COPOLYMER
    • 聚碳酸酯 - 聚硅氧烷共聚物的连续生产方法
    • US20140296469A1
    • 2014-10-02
    • US14362375
    • 2012-11-16
    • IDEMITSU KOSAN CO., LTD.
    • Yasuhiro IshikawaHiroaki MotegiYukiko Nagao
    • C08G64/06
    • C08G64/06C08G64/186C08G64/24C08G64/28C08G77/448
    • The present invention provides a method for producing a polycarbonate-polyorganosiloxane copolymer economically and stably, in particular, the present invention is concerned with a method for continuous production of a polycarbonate-polyorganosiloxane copolymer including (A) a step of withdrawing a polymerization reaction solution obtained by polymerizing a dihydric phenol compound, a carbonate precursor, and a polyorganosiloxane in the presence of an alkaline compound aqueous solution and a water-insoluble organic solvent continuously or intermittently from a reactor; (B) a step of separating the polymerization reaction solution withdrawn in the step (A) into an aqueous phase and a water-insoluble organic solvent phase; and (C) a step of after washing the water-insoluble organic solvent phase separated in the step (B) with an acidic aqueous solution, separating the resultant into an aqueous phase and a water-insoluble organic solvent phase, wherein the aqueous phase separated in the step (C) is extracted with a water-insoluble organic solvent, the content of the polycarbonate-polyorganosiloxane copolymer in the obtained extract is controlled to not more than 2% by mass, and a part or the whole of the extract is reused for the step (A).
    • 本发明提供了一种经济,稳定地制备聚碳酸酯 - 聚有机硅氧烷共聚物的方法,特别是本发明涉及连续制备聚碳酸酯 - 聚有机硅氧烷共聚物的方法,其包括(A)取出获得的聚合反应溶液的步骤 通过在反应器中连续或间歇地在碱性化合物水溶液和水不溶性有机溶剂的存在下聚合二元酚化合物,碳酸酯前体和聚有机硅氧烷; (B)将步骤(A)中取出的聚合反应溶液分离成水相和水不溶性有机溶剂相的步骤; 和(C)用酸性水溶液洗涤步骤(B)中分离出的水不溶性有机溶剂相的步骤,将所得物分离成水相和水不溶性有机溶剂相,其中水相分离 在步骤(C)中用水不溶性有机溶剂萃取,将得到的提取物中的聚碳酸酯 - 聚有机硅氧烷共聚物的含量控制在2质量%以下,将部分或全部提取物再利用 步骤(A)。