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    • 1. 发明授权
    • METHOD FOR PREPARING A COMPOSITION COMPRISING PERFLUOROPOLYETHER HAVING A HYDROXYL GROUP AT ONE TERMINAL
    • 制备包含在一端具有羟基的全氟聚醚的组合物的方法
    • EP2930201B1
    • 2017-05-17
    • EP15162845.0
    • 2015-04-08
    • SHIN-ETSU CHEMICAL CO., LTD
    • Yamane, YujiMatsuda, TakashiKoike, Noriyuki
    • C08G65/00C08G65/30C08G65/46
    • C08L71/00B01D15/12C08G65/007C08G65/30C08G65/46Y02P20/544
    • An object of the present invention is to provide a method for efficiently and highly selectively preparing a composition comprising perfluoropolyether having a hydroxyl group at one terminal at a higher ratio. The present invention provides a method for increasing a ratio of perfluoropolyether having a hydroxyl group at one terminal, relative to a total amount of the perfluoropolyether having a hydroxyl group at one terminal and perfluoropolyether having hydroxyl groups at both terminals in a composition comprising these perfluoropolyethers, wherein the method comprises a step of subjecting the composition to chromatography in which a moving phase is supercritical or subcritical state carbon dioxide of the specific temperature and the specific pressure, and a stationary phase is silica gel to thereby collect a fraction containing the perfluoropolyether having a hydroxyl group at one terminal at a higher ratio. Further, present invention provides for increasing a ratio of perfluoropolyether having a hydroxyl group at one terminal, relative to a total amount of the perfluoropolyether having a hydroxyl group at one terminal, perfluoropolyether having hydroxyl groups at both terminals and perfluoropolyether having no hydroxyl group at any terminal perfluoropolyether, in a composition comprising these perfluoropolyethers, wherein the method comprises a step of subjecting the composition to chromatography in which a moving phase is supercritical or subcritical state carbon dioxide of the specific temperature and the specific pressure, and a stationary phase is silica gel to thereby collect a fraction containing the perfluoropolyether having a hydroxyl group at one terminal at a higher ratio.
    • 本发明的一个目的是提供一种用于有效和高度选择性地制备包含在一个末端具有较高比例的羟基的全氟聚醚的组合物的方法。 本发明提供一种提高一个末端具有羟基的全氟聚醚相对于一个末端具有羟基的全氟聚醚和两个末端具有羟基的全氟聚醚的总量的比例的方法,所述组合物包含这些全氟聚醚, 其中所述方法包括使组合物经受色谱法的步骤,其中移动相是特定温度和特定压力的超临界或亚临界状态二氧化碳,并且固定相是硅胶,从而收集含有全氟聚醚的部分,所述全氟聚醚具有 一个末端羟基的比例较高。 此外,本发明提供了增加一端具有羟基的全氟聚醚相对于一端具有羟基的全氟聚醚,两端具有羟基的全氟聚醚和任何具有羟基的全氟聚醚的总量的比例 在包含这些全氟聚醚的组合物中,其中所述方法包括使组合物经受色谱法的步骤,其中运动相是特定温度和特定压力的超临界或亚临界状态二氧化碳,并且固定相是硅胶 从而以更高的比率收集含有在一个末端具有羟基的全氟聚醚的部分。
    • 3. 发明授权
    • Perfluoropolyether-modified polysiloxane, a method for preparing the same and a defoaming agent comprising the same
    • Perfluorpolyethermodifiziertes聚硅氧烷,其制备和消泡剂方法因此
    • EP2301989B1
    • 2014-04-23
    • EP10169689.6
    • 2010-07-15
    • Shin-Etsu Chemical Co., Ltd.
    • Yamaguchi, HiromasaKoike, Noriyuki
    • C08G77/46
    • C08G77/46B01D19/0427B01D19/0431B01D19/0409B01D19/0413
    • The present invention relates to a perfluoropolyether-modified polysiloxane represented by general formula (1): wherein X is a divalent group represented by formula -CH 2 -, -CH 2 O-, -CH 2 OCH 2 - or -Y-NR-CO-, wherein Y is a divalent group represented by formula -CH 2 - or the following formula: and R is a hydrogen atom, an alkyl group having 1 to 10 carbon atoms or an aryl group; R 1 , R 2 , and R 3 are, independently of each other, an alkyl group having 1 to 10 carbon atoms or an aryl group; X' is a divalent group represented by formula -CH 2 -, -OCH 2 -, -CH 7 OCH 2 - or -CO-NR-Y'-, wherein Y'is a divalent group represented by formula -CH 2 - or the following formula: and R is as defined above; a is, independently of each other, 0 or 1; z and z' are, independently of each other, an integer of 5 to 100; and Rf is a divalent group represented by the following general formula (2) : €ƒ€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ-C t -F 2t [OCF 2 CF(CF 3 )] m OCF 2 (CF 2 ) z CF 2 O[CF(CF 3 )CF 2 O] n C t F 2t -€ƒ€ƒ€ƒ€ƒ€ƒ(2) wherein m and n are an integer of 1 to 150, provided that an average of the total of m and n is 2 to 200; r is an integer of 0 to 6; t is 2 or 3; and C t F 2t is linear or branched; or by the following general formula (3): €ƒ€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ-C t' F 2t' (OCF 2 CF 2 ) u (OCF 2 ) v OC t' F 2t' -€ƒ€ƒ€ƒ€ƒ€ƒ(3) wherein u is an integer of 1 to 200; v is an integer of 1 to 50; t' is an integer of 1 to 3; and C t ,F 2t , is linear or branched.
    • 8. 发明公开
    • Perfluoropolyether-modified polysiloxane, a method for preparing the same and a defoaming agent comprising the same
    • Perfluorpolyethermodifiziertes聚硅氧烷,其制备和消泡剂方法因此
    • EP2301989A2
    • 2011-03-30
    • EP10169689.6
    • 2010-07-15
    • Shin-Etsu Chemical Co., Ltd.
    • Yamaguchi, HiromasaKoike, Noriyuki
    • C08G77/46
    • C08G77/46B01D19/0427B01D19/0431B01D19/0409B01D19/0413
    • The present invention relates to a perfluoropolyether-modified polysiloxane represented by general formula (1):

      wherein X is a divalent group represented by formula -CH 2 -, -CH 2 O-,
      -CH 2 OCH 2 - or -Y-NR-CO-,
      wherein Y is a divalent group represented by formula -CH 2 - or the following formula:

      and R is a hydrogen atom, an alkyl group having 1 to 10 carbon atoms or an aryl group;
      R 1 , R 2 , and R 3 are, independently of each other, an alkyl group having 1 to 10 carbon atoms or an aryl group;
      X' is a divalent group represented by formula -CH 2 -, -OCH 2 -,
      -CH 7 OCH 2 - or -CO-NR-Y'-,
      wherein Y'is a divalent group represented by formula -CH 2 - or the following formula:

      and R is as defined above;
      a is, independently of each other, 0 or 1;
      z and z' are, independently of each other, an integer of 5 to 100; and
      Rf is a divalent group represented by the following general formula (2) :

              -C t -F 2t [OCF 2 CF(CF 3 )] m OCF 2 (CF 2 ) z CF 2 O[CF(CF 3 )CF 2 O] n C t F 2t -     (2)

      wherein m and n are an integer of 1 to 150, provided that an average of the total of m and n is 2 to 200;
      r is an integer of 0 to 6;
      t is 2 or 3; and
      C t F 2t is linear or branched;
      or by the following general formula (3):

              -C t' F 2t' (OCF 2 CF 2 ) u (OCF 2 ) v OC t' F 2t' -     (3)

      wherein u is an integer of 1 to 200;
      v is an integer of 1 to 50;
      t' is an integer of 1 to 3; and
      C t ,F 2t , is linear or branched.
    • 本发明涉及由通式的全氟聚醚改性的聚硅氧烷(1):其中X是由下式表示的二价基团-CH 2 - , - CH 2 O-,-CH 2 OCH 2 - 或-Y-NR CO-,worin Y是由式-CH 2 - 表示的二价基团 - 或下式:且R为氢原子,在具有1〜10碳原子上或在芳基烷基; R 1,R 2,和R 3,彼此独立地,在具有1〜10碳原子上或在芳基烷基; X“是由下式表示的二价基团-CH 2 - , - OCH 2 - ,-CH 7 OCH 2 - 或-CO-NR-Y'-,worin Y'是由式-CH 2 - 表示的二价基团 - 或 以下公式:和R如上所定义; 一个是,海誓山盟,0或1的unabhängig; Z和Z“是,上为5至100的整海誓山盟unabhängig; 并且Rf为下述通式(2)表示的二价基团:€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ-C五六2吨[OCF 2 CF(CF 3)]米OCF 2 (CF 2)z的CF 2 O [CF(CF 3)CF 2 O] N c个五六2吨 - €ƒ€ƒ€ƒ€ƒ€ƒ(2)worin m和n是从1到150的整数,条件 做了平均总的米和n为2至200; r为0〜6的整数; t为2或3; 和C五六2T为直链或支链的; 或下述通式(3):€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ-C吨 'F2吨'(OCF 2 CF 2)u(OCF 2)V OC吨“F2吨 “ - €ƒ€ƒ€ƒ€ƒ€ƒ(3)worin u是1〜200的整数; v是1至50的整数; T“是1〜3的整数; 和C五六2T,为直链或支链的。