公开(公告)号：US06680398B1

公开(公告)日：2004-01-20

申请号：US10219080

申请日：2002-08-16

申请人： Lisa Marie Boswell ,  William Charles Maki ,  Anil Kumar Tomar

发明人： Lisa Marie Boswell ,  William Charles Maki ,  Anil Kumar Tomar

IPC分类号： C07F708

CPC分类号： C07F7/1892

摘要： In a first embodiment of a process for making mercaptoalkylalkoxysilanes, a pH adjusting agent and a sulfide containing compound are mixed in an aqueous phase to provide a pH of 4-9, a phase transfer catalyst is added to the aqueous phase, a haloalkylalkoxysilane is then added to the aqueous phase to form a reaction mixture containing mercaptoalkylalkoxysilanes and water soluble byproducts, and the desired mercaptoalklyalkoxysilanes are separated from the water soluble byproducts. In an alternate embodiment, the haloalkylalkoxysilane, the phase transfer catalyst, and an anhydrous pH adjusting agent such as sulfur dioxide, carbon dioxide, hydrogen sulfide, phosphoric acid, boric acid, and hydrochloric acid, are mixed, then an aqueous solution of a sulfide containing compound is added to form a reaction mixture containing mercaptoalkylalkoxysilanes and water soluble byproducts, and desired mercaptoalklyalkoxysilanes are separated from water soluble byproducts.

摘要翻译： 在制备巯基烷基烷氧基硅烷的方法的第一个实施方案中，将pH调节剂和含硫化物的化合物在水相中混合以提供4-9的pH，将相转移催化剂加入到水相中，然后将卤代烷基烷氧基硅烷 加入到水相中以形成含有巯基烷基烷氧基硅烷和水溶性副产物的反应混合物，并将所需的巯基烷基烷氧基硅烷与水溶性副产物分离。 在另一个实施方案中，将卤代烷基烷氧基硅烷，相转移催化剂和无水pH调节剂如二氧化硫，二氧化碳，硫化氢，磷酸，硼酸和盐酸混合，然后加入硫化氢水溶液 加入含有巯基烷基烷氧基硅烷和水溶性副产物的反应混合物，并将所需的巯基烷氧基硅烷与水溶性副产物分离。

公开(公告)号：US06384256B1

公开(公告)日：2002-05-07

申请号：US09895720

申请日：2001-06-29

申请人： Michael Wolfgang Backer ,  Howard Marvin Bank ,  John Michael Gohndrone ,  William Charles Maki ,  Charles Edmund Skinner ,  Anil Kumar Tomar ,  Hongjun Yue

发明人： Michael Wolfgang Backer ,  Howard Marvin Bank ,  John Michael Gohndrone ,  William Charles Maki ,  Charles Edmund Skinner ,  Anil Kumar Tomar ,  Hongjun Yue

IPC分类号： C07F208

CPC分类号： C07F7/1892

摘要： A process for the production of organosilicon compounds of the formula: (RO)3−mRmSi-Alk-Sn-Alk-SiRm(OR)3−m where R is independently a monovalent hydrocarbon of 1 to 12 carbon atoms; Alk is a divalent hydrocarbon of 1 to 18 carbon atoms; m is an integer of 0 to 2, n is a number from 1 to 10; is disclosed. The process comprises: (A) reacting an alkali metal hydroxide compound, a sulfide compound having the formula M2Sn or MHS, where H is hydrogen, M is ammonium or an alkali metal, n is as defined above,  and sulfur in water to form a polysulfide mixture, (B) reacting said polysulfide mixture with a silane compound of the formula; (RO)3−mRmSi-Alk-X where X is Cl, Br or I, and m is the same as above, in the presence of a phase transfer catalyst. The process provides sulfur containing organosilicon compounds based on phase transfer catalysis techniques that result in a final product composition having greater stability, purity, and appearance. The process also minimizes or eliminates hydrogen sulfide as a side product.

摘要翻译： 一种制备下式的有机硅化合物的方法：其中R独立地是1至12个碳原子的一价烃; Alk为1〜18个碳原子的二价烃，m为0〜2的整数，n为1〜10的数。 该方法包括：（A）使碱金属氢氧化物化合物，具有式M2Sn或MHS的硫化物，其中H是氢，M是铵或碱金属，n如上定义，和硫在水中形成 （B）使所述多硫化物混合物与下式的硅烷化合物反应;其中X是Cl，Br或I，m与上述相同，在相转移催化剂的存在下。 该方法基于相转移催化技术提供含硫有机硅化合物，其导致最终产物组合物具有更高的稳定性，纯度和外观。 该方法还使作为副产物的硫化氢最小化或消除。

公开(公告)号：US06534668B2

公开(公告)日：2003-03-18

申请号：US09895719

申请日：2001-06-29

申请人： Michael Wolfgang Backer ,  Howard Marvin Bank ,  John Michael Gohndrone ,  William Charles Maki ,  Charles Edmund Skinner ,  Anil Kumar Tomar ,  Hongjun Yue

发明人： Michael Wolfgang Backer ,  Howard Marvin Bank ,  John Michael Gohndrone ,  William Charles Maki ,  Charles Edmund Skinner ,  Anil Kumar Tomar ,  Hongjun Yue

IPC分类号： C07F708

CPC分类号： C07F7/1892

摘要： A process for the production of sulfur containing organosilicon compounds of the formula: (RO)3−mRmSi—Alk—Sn—Alk—SiRm(OR)3−m where R is independently a monovalent hydrocarbon of 1 to 12 carbon atoms; Alk is a divalent hydrocarbon of 1 to 18 carbon atoms; m is an integer of 0 to 2, n is a number from 1 to 8; based on phase transfer catalysis techniques is disclosed. The process comprises reacting: (A) a sulfide compound having the formula M2Sn or MHS, where H is hydrogen, M is ammonium or an alkali metal, n is as defined above, with (B) a silane compound of the formula; (RO)3−mRmSi—Alk—X where X is Cl, Br or I, and m is the same as above, and optionally, (C) sulfur in the presence of a phase transfer catalyst and an aqueous phase containing a buffer. The improvement of the present invention is characterized by adding a buffer to the aqueous phase, which minimizes or prevents gelling of the sulfur containing organosilicon compounds. The present invention also teaches a process for the production of sulfur containing organosilicon compounds by controlling the pH of the aqueous phase.

摘要翻译： 一种生产下式的含硫有机硅化合物的方法：其中R独立地为1至12个碳原子的一价烃; Alk是1至18个碳原子的二价烃; m是0至2的整数，n是1至8的数;基于相转移催化技术被公开。 该方法包括：（A）具有式M2Sn或MHS的硫化物，其中H是氢，M是铵或碱金属，n如上定义，与（B）下式的硅烷化合物反应：其中X 是Cl，Br或I，m与上述相同，任选地，（C）硫在存在相转移催化剂和含有缓冲液的水相的存在下。本发明的改进的特征在于将缓冲剂加入 水相，其最小化或防止含硫有机硅化合物的胶凝。 本发明还教导了通过控制含水相的pH来生产含硫有机硅化合物的方法。

公开(公告)号：US06448426B1

公开(公告)日：2002-09-10

申请号：US09895721

申请日：2001-06-29

申请人： Michael Wolfgang Backer ,  Howard Marvin Bank ,  John Michael Gohndrone ,  William Charles Maki ,  Charles Edmund Skinner ,  Anil Kumar Tomar ,  Hongjun Yue

发明人： Michael Wolfgang Backer ,  Howard Marvin Bank ,  John Michael Gohndrone ,  William Charles Maki ,  Charles Edmund Skinner ,  Anil Kumar Tomar ,  Hongjun Yue

IPC分类号： C07F708

CPC分类号： C07F7/1892 ,  B60C1/00 ,  C08K5/548 ,  C08L21/00

摘要： An improved process for the production of organosilicon compounds of the formula (RO)3−mRmSi—Alk—Sn—Alk—SiRm(OR)3−m where R is independently a monovalent hydrocarbon of 1 to 12 carbon atoms, Alk is a divalent hydrocarbon of 1 to 18 carbon atoms; m is an integer of 0 to 2, n is a number from 1 to 8 is disclosed. The process comprises: (A) reacting sulfur, a phase transfer catalyst, a sulfide compound having the formula M2Sn or MHS, where H is hydrogen, M is ammonium or an alkali metal, n is the same as above, and water to form an intermediate reaction product; (B) reacting said intermediate reaction product with a silane compound of the formula; (RO)3−mRmSi—Alk—X where X is Cl, Br or I, and m is the same as above (C) separating the organosilicon compound from the product mixture by adding water or a dilute acidic solution to the product mixture, and phase separating the product mixture into an organic phase containing the organosilicon compound and an aqueous phase.

摘要翻译： 制备式R的有机硅化合物的改进方法独立地是1至12个碳原子的单价烃，Alk是1至18个碳原子的二价烃; m是0-2的整数，n是数 从1到8被公开。 该方法包括：（A）使硫，相转移催化剂，具有式M2Sn或MHS的硫化物反应，其中H是氢，M是铵或碱金属，n与上述相同，和水形成 中间反应产物;（B）使所述中间体反应产物与下式的硅烷化合物反应;其中X为Cl，Br或I，m与上述相同（C）通过加入水分将有机硅化合物与产物混合物分离 或稀酸性溶液，并将产物混合物相分离成含有有机硅化合物和水相的有机相。

公开(公告)号：US06384255B1

公开(公告)日：2002-05-07

申请号：US09895700

申请日：2001-06-29

申请人： Michael Wolfgang Backer ,  Howard Marvin Bank ,  John Michael Gohndrone ,  William Charles Maki ,  Charles Edmund Skinner ,  Anil Kumar Tomar ,  Hongjun Yue

发明人： Michael Wolfgang Backer ,  Howard Marvin Bank ,  John Michael Gohndrone ,  William Charles Maki ,  Charles Edmund Skinner ,  Anil Kumar Tomar ,  Hongjun Yue

IPC分类号： C07F708

CPC分类号： C07F7/1804

摘要： A process for the production of organosilicon compounds of the formula (RO)3−mRmSi—Alk—Sn—Alk—SiRm(OR)3−m where R is independently a monovalent hydrocarbon of 1 to 12 carbon atoms, Alk is a divalent hydrocarbon of 1 to 18 carbon atoms; m is an integer of 0 to 2, n is a number from 1 to 8 is disclosed. The process comprises: (A) reacting sulfur, a phase transfer catalyst, a sulfide compound having the formula M2Sn or MHS, where H is hydrogen, M is ammonium or an alkali metal, n is the same as above,  and water to form an intermediate reaction product; (B) reacting said intermediate reaction product with  a silane compound of the formula; (RO)3−mRmSi—Alk—X  where X is Cl, Br or I, and m is the same as above. The invention provides an improvement process characterized by adding the phase transfer catalyst to the aqueous phase prior to mixing the aqueous phase with the silane compound for the reaction.

摘要翻译： 制备式R的有机硅化合物的方法独立地是1至12个碳原子的一价烃，Alk是1至18个碳原子的二价烃; m是0-2的整数，n是 公开了图1至图8。 该方法包括：（A）使硫，相转移催化剂，具有式M2Sn或MHS的硫化物反应，其中H是氢，M是铵或碱金属，n与上述相同，和水形成 中间反应产物;（B）使所述中间体反应产物与下式的硅烷化合物反应; 其中X是Cl，Br或I，m与上述相同。本发明提供了一种改进方法，其特征在于在将水相与用于反应的硅烷化合物混合之前将相转移催化剂加入到水相中。