公开(公告)号：US4476287A

公开(公告)日：1984-10-09

申请号：US448232

申请日：1982-12-09

申请人： Nobunori Maehara ,  Norihumi Utada ,  Taiji Oda ,  Hidetomo Ashitaka ,  Hideo Ishikawa

发明人： Nobunori Maehara ,  Norihumi Utada ,  Taiji Oda ,  Hidetomo Ashitaka ,  Hideo Ishikawa

IPC分类号： C08F4/00 ,  C08F4/60 ,  C08F6/00 ,  C08F6/06 ,  C08F6/10 ,  C08F36/00 ,  C08F136/06 ,  C08F236/00 ,  C08F295/00 ,  C08F4/26

CPC分类号： C08F295/00 ,  C08F136/06

摘要： A polybutadiene rubber having an enhanced mechanical strength is produced in such a manner that the content of water in a solution of 1,3-butadiene in an inert organic solvent is controlled to 0.2 to 5 millemoles per liter of 1,3-butadiene; a first polymerization mixture is prepared from the controlled 1,3-butadiene solution, an organic aluminum compound of the formula Al R.sub.n X.sub.3-n, wherein R=C.sub.1-6 alkyl, phenyl, or cycloalkyl, X=halogen, and n=1.5-2.0, and a cobalt compound, for example, by aging a mixture of the controlled 1,3-butadiene solution with the aluminum compound for at least one minute and then by admixing the aged mixture with the cobalt compound; the first polymerization mixture is subjected to a cis-1,4-polymerization; a second polymerization comprising the resultant cis-1,4-polybutadiene, non-reacted 1,3-butadiene, the inert organic solvent, and a catalyst comprising an organic aluminum compound of the formula AlR.sub.3, a cobalt compound, and carbon disulfide is subjected to a 1,2-polymerization to produce a polybutadiene rubber consisting essentially of 5% to 30% by weight of a boiling n-hexane-insoluble fraction and 70% to 95% by weight of a boiling n-hexane-soluble fraction thereof and having an excellent mechanical strength; and after the 1,2-polymerization is shortstopped, the resultant polybutadiene rubber is isolated from the 1,2-polymerization mixture.

摘要翻译： 制造具有增强的机械强度的聚丁二烯橡胶，使得1,3-丁二烯在惰性有机溶剂中的溶液中的水含量控制在每升1,3-丁二烯0.2至5毫摩尔; 由对照的1,3-丁二烯溶液制备第一聚合混合物，式为Al RnX 3-n的有机铝化合物，其中R = C 1-6烷基，苯基或环烷基，X =卤素，n = 1.5- 2.0和钴化合物，例如通过将受控1,3-丁二烯溶液与铝化合物的混合物老化至少1分钟，然后将老化的混合物与钴化合物混合; 将第一聚合混合物进行顺式-1,4-聚合; 包含所得顺式-1,4-聚丁二烯，未反应的1,3-丁二烯，惰性有机溶剂和包含式AlR 3的有机铝化合物，钴化合物和二硫化碳的催化剂的第二聚合物被 进行1,2-聚合以制备基本上由沸腾正己烷不溶部分的5重量％至30重量％的沸石正己烷不溶部分和70重量％至95重量％的沸腾的正己烷可溶部分组成的聚丁二烯橡胶， 具有优良的机械强度; 并且在1,2-聚合反应快速之后，从1,2-聚合混合物中分离得到的聚丁二烯橡胶。

公开(公告)号：US4472559A

公开(公告)日：1984-09-18

申请号：US451756

申请日：1982-12-21

申请人： Nobunori Maehara ,  Norihumi Utada ,  Taiji Oda ,  Hidetomo Ashitaka ,  Hideo Ishikawa

发明人： Nobunori Maehara ,  Norihumi Utada ,  Taiji Oda ,  Hidetomo Ashitaka ,  Hideo Ishikawa

IPC分类号： C08F136/06 ,  C08F295/00 ,  C08F4/26

CPC分类号： C08F295/00 ,  C08F136/06

摘要： A polybutadiene rubber having an enhanced mechanical strength is produced in such a manner that the contents of water and carbon disulfide in a solution of 1,3-butadiene and carbon disulfide in an inert organic solvent is controlled to 0.2 to 5 m moles and 20 m moles or less, respectively, per liter of the 1,3-butadiene-carbon disulfide solution; a first polymerization mixture is prepared from the controlled 1,3-butadiene-carbon disulfide solution, an organic aluminum compound of the formula Al R.sub.n X.sub.3-n, wherein R=C.sub.1-6 alkyl, phenyl, or cycloalkyl, X=halogen, and n=1.5-2.0, and a cobalt compound, for example, by aging a mixture of the controlled 1,3-butadiene-carbon disulfide solution with the aluminum compound for at least one minute and then by admixing the aged mixture with the cobalt compound; the first polymerization mixture is subjected to a cis-1,4-polymerization; a second polymerization comprising the resultant cis-1,4-polybutadiene, non-reacted 1,3-butadiene, the inert organic solvent, an organic aluminum compound of the formula AIR.sub.3, a cobalt compound, and the carbon disulfide is subjected to a 1,2-polymerization to produce a polybutadiene rubber consisting essentially of 5% to 30% by weight of a boiling n-hexane-insoluble fraction and 70% to 95% by weight of a boiling n-hexane-soluble fraction thereof; and after the 1,2-polymerization is shortstopped, the resultant polybutadiene rubber is isolated from the 1,2-polymerization mixture.

摘要翻译： 制造具有增强的机械强度的聚丁二烯橡胶，使得将1,3-丁二烯和二硫化碳在惰性有机溶剂中的溶液中的水和二硫化碳的含量控制在0.2至5微摩尔和20微米 摩尔或更少，分别为每升1,3-丁二烯 - 二硫化碳溶液; 由对照的1,3-丁二烯 - 二硫化碳溶液制备第一聚合混合物，式为Al RnX 3-n的有机铝化合物，其中R = C 1-6烷基，苯基或环烷基，X =卤素和n = 1.5-2.0，和钴化合物，例如通过将受控1,3-丁二烯 - 二硫化碳溶液与铝化合物的混合物老化至少1分钟，然后将老化的混合物与钴化合物混合; 将第一聚合混合物进行顺式-1,4-聚合; 包含所得顺式-1,4-聚丁二烯，未反应的1,3-丁二烯，惰性有机溶剂，式AIR3的有机铝化合物，钴化合物和二硫化碳的第二聚合物经受1 2-聚合，以制备基本上由沸腾的正己烷不溶部分的5％至30％重量的沸点正己烷可溶级分的70％至95％的聚丁二烯橡胶; 并且在1,2-聚合反应快速之后，从1,2-聚合混合物中分离得到的聚丁二烯橡胶。