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公开(公告)号：US4131644A
公开(公告)日：1978-12-26
申请号：US780520
申请日：1977-03-23
CPC分类号： D01F9/21
摘要： Carbon fibers having excellent modulus of elasticity and tensile strength are produced in a high yield by a process wherein polybutadiene fibers are prepared by melt-spinning polybutadiene having at least 85% of vinyl structure, a melting point of at least 100.degree. C and a reduced viscosity of 0.3 to 1.2 dl/g; the fibers are then treated in a solution or suspension of a Lewis acid in an inert organic liquid, whereby the pollybutadiene is cyclized and cross-linked; the polybutadiene fibers treated as mentioned above are further treated in a melted sulphur or a sulphur-containing solution at a temperature of 170 to 300.degree. C, whereby the cyclized and cross-linked polybutadiene is dehydrogenated and aromatized; and the fibers treated as mentioned above are carbonized by raising the temperature thereof to 750.degree. C to 3000.degree. C to form carbon fibers or graphite fibers. If so desired, the ordinary carbon fibers which have been produced at 750 to 1500.degree. C, can be converted to graphite fibers by heating them to a temperature of 1500 to 3000.degree. C.
摘要翻译： 具有优异的弹性模量和拉伸强度的碳纤维通过以下方法以高产率生产，其中聚丁二烯纤维通过熔体纺丝具有至少85％的乙烯基结构，熔点至少为100℃的聚丁二烯和减少的 粘度为0.3〜1.2dl / g; 然后将纤维在路易斯酸在惰性有机液体中的溶液或悬浮液中处理，由此将聚丁二烯环化并交联; 如上所述处理的聚丁二烯纤维在熔融硫或含硫溶液中在170〜300℃下进一步处理，由此使环化和交联的聚丁二烯脱氢和芳构化; 如上所述处理的纤维通过将其温度升高至750℃至3000℃而碳化，以形成碳纤维或石墨纤维。 如果需要，在750〜1500℃下生产的普通碳纤维可以通过将其加热至1500〜3000℃的温度而转化为石墨纤维。
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公开(公告)号：US4684717A
公开(公告)日：1987-08-04
申请号：US676264
申请日：1984-11-29
申请人： Hidetomo Ashitaka , Kazuya Jinda , Yoshiyuki Miwa
发明人： Hidetomo Ashitaka , Kazuya Jinda , Yoshiyuki Miwa
IPC分类号： C07C255/65 , C08F4/04 , C07C107/02 , C08G63/68
CPC分类号： C07C255/65
摘要： A process for the preparation of a diazocyano acid, which comprises reacting a keto-acid or its sodium salt with a cyanogen compound such as sodium cyanide or hydrogen cyanide and a hydrazine in water to form a concentrated aqueous solution of a hydrazo compound, adding acetone or acetone and water to the concentrated aqueous solution to form an acetone-water solution of the hydrazo compound, adding an oxidant such as chlorine gas to the solution to oxidize the hydrazo compound and form a diazocyano acid, forming at least two transparent liquid layers by adding acetone and/or water to the obtained reaction mixture during or after oxidation if necessary, and further adding sodium chloride to the reaction mixture if necessary, and separating and recovering the upper layer of the acetone-water solution containing the diazocyano acid from the mixture.
摘要翻译： 一种制备重氮氰酸的方法，其包括使酮酸或其钠盐与氰化氰或氰化氢等氰化合物和肼在水中反应以形成浓水化合物的水溶液，加入丙酮 或丙酮和水加到浓缩的水溶液中以形成氢化合物的丙酮 - 水溶液，向溶液中加入氧化剂如氯气，以氧化氢化合物并形成重氮氰酸，通过以下方式形成至少两个透明液体层 如果需要，在氧化过程中或氧化后向所得反应混合物中加入丙酮和/或水，如果需要，向反应混合物中加入氯化钠，并从混合物中分离并回收含有重氮氰酸的丙酮 - 水溶液的上层 。
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3.发明授权Process for producing polybutadiene rubber with enhanced mechanical strength 失效具有增强机械强度的生产聚丁二烯橡胶的方法
公开(公告)号：US4472559A
公开(公告)日：1984-09-18
申请号：US451756
申请日：1982-12-21
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。
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4.发明授权Process for the preparation of diazocyano acids by reacting keto-acids with cyanogen compounds 失效通过使酮酸与氰化合物反应制备重氮氰酸的方法
公开(公告)号：US4684718A
公开(公告)日：1987-08-04
申请号：US676265
申请日：1984-11-29
申请人： Hidetomo Ashitaka , Kazuya Jinda , Yoshiyuki Miwa
发明人： Hidetomo Ashitaka , Kazuya Jinda , Yoshiyuki Miwa
IPC分类号： C07C255/65 , C08F4/04 , C07C101/26 , C07C107/02 , C08G63/68
CPC分类号： C07C255/65
摘要： A process for the preparation of a diazocyano acid, which comprises reacting a keto-acid or its sodium salt with a cyanogen compound such as sodium cyanide or hydrogen cyanide and a hydrazine in water to form a concentrated aqueous solution of a hydrazo compound, adding acetone and/water to the concentrated aqueous solution to form a solution of the hydrazo compounds, adding chlorine gas to the solution to oxidize the hydrazo compound and form a diazocyano acid, adding acetone to the obtained reaction mixture during or after the oxidation if necessary, and separating and recovering the supernatant layer of the acetone-water solution containing the diazocyano acid from the mixture.
摘要翻译： 一种制备重氮氰酸的方法，其包括使酮酸或其钠盐与氰化氰或氰化氢等氰化合物和肼在水中反应以形成浓水化合物的水溶液，加入丙酮 和/水加入到浓水溶液中以形成氢化合物的溶液，向溶液中加入氯气以氧化氢化合物并形成重氮氰酸，如果需要，在氧化期间或之后向所得反应混合物中加入丙酮，以及 从混合物中分离和回收含有重氮氰酸的丙酮 - 水溶液的上清液层。
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5.发明授权Process for producing polybutadiene rubber with enhanced mechanical strength 失效具有增强机械强度的生产聚丁二烯橡胶的方法
公开(公告)号：US4476287A
公开(公告)日：1984-10-09
申请号：US448232
申请日：1982-12-09
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。
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公开(公告)号：US5173235A
公开(公告)日：1992-12-22
申请号：US620805
申请日：1990-12-03
申请人： Eiichi Kamei , Hidetomo Ashitaka , Toru Takahashi
发明人： Eiichi Kamei , Hidetomo Ashitaka , Toru Takahashi
CPC分类号： B01D67/0027 , B01D69/02 , B01D71/26 , B29C55/005 , C08J5/18 , H01M10/05 , H01M2/14 , H01M2/1653 , B01D2323/08 , B01D2325/26 , B29K2023/00 , B29K2105/04 , C08J2323/12 , H01M2300/0017
摘要： This microporous film has an approximately uniform configuration in which the intervals between slender fibrils extend approximately two-dimensionally which are connected to each other between adjacent unstretched planar flat portions to define fine through-pores, and the distribution of pore size is sharp and the porosity is high. Accordingly, the microporous film excels in water filtration rate and selective separating capability and is suitable for use as filter membrane, separator membrane, gas exchange membrane, and a battery separator.
摘要翻译： 该微孔膜具有大致均匀的构造，其中细长纤维之间的间隔大致二维地延伸，它们在相邻的未拉伸的平坦平坦部分之间彼此连接以限定细小的通孔，并且孔径的分布是尖锐的，并且孔隙度 高。 因此，微孔膜在水过滤率和选择性分离能力方面优异，适用于过滤膜，隔膜，气体交换膜和电池隔膜。
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公开(公告)号：US4908283A
公开(公告)日：1990-03-13
申请号：US342122
申请日：1989-04-24
IPC分类号： H01M6/18
CPC分类号： H01M6/181
摘要： An improved ion conductive solid electrolyte favorably emplolyable for an solid electrolyte cell comprises a cured product of an acryloyl-denatured polyalkylene oxide having a molecular weight of 200-3,000 and an inorganic ion salt. Another improved ion conductive solid electrolyte comprises a cured product of an acryloyl-denatured polyalkylene oxide having a molecular weight of 200-3,000, an inorganic ion salt and a polyalkylene glycol.
摘要翻译： 有利地可用于固体电解质电池的改进的离子导电固体电解质包括分子量为200-3,000的丙烯酰基变性聚环氧烷的固化产物和无机离子盐。 另一种改进的离子导电固体电解质包括分子量为200-3,000的丙烯酰基变性聚环氧烷的固化产物，无机离子盐和聚亚烷基二醇。
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8.发明授权Process for producing polybutadine rubber with enhanced mechanical strength 失效生产具有增强的机械强度的聚丁二烯橡胶的方法
公开(公告)号：US4379889A
公开(公告)日：1983-04-12
申请号：US216869
申请日：1980-12-16
IPC分类号： C08F4/00 , C08F4/60 , C08F4/70 , C08F36/00 , C08F136/06 , C08F295/00 , C08F4/12
CPC分类号： C08F295/00 , C08F136/06
摘要： A polybutadiene rubber having an enhanced mechanical strength is produced by a process comprising two successive steps of:(A) cis-1,4-polymerizing 1,3-butadiene in a polymerization medium in the presence of a catalyst comprising a cobalt compound and a dialkyl aluminium halide of the formula (I): AlR.sub.2 X, wherein R=C.sub.2 -8 alkyl and X=halogen, and;(B) subjecting a mixture of the resultant cis-1,4-polybutadiene and the non-reacted 1,3-butadiene in the polymerization medium to a 1,2-polymerization in the presence of a catalyst comprising a cobalt compound, a dialkyl aluminium halide of the formula (I), carbon disulfide and an electron donative organic compound.
摘要翻译： 具有增强的机械强度的聚丁二烯橡胶通过包括以下两个连续步骤的方法制备：（A）在聚合介质中，在包含钴化合物的催化剂存在下，顺式-1,4-聚合1,3-丁二烯， 式（I）的二烷基卤化铝：AlR2X，其中R = C2-8烷基，X =卤素，和 （B）将所得到的顺式-1,4-聚丁二烯与未反应的1,3-丁二烯的混合物在聚合介质中进行1,2-聚合，所述催化剂包含钴化合物，二烷基 式（I）的卤化铝，二硫化碳和给电子有机化合物。
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公开(公告)号：US4504639A
公开(公告)日：1985-03-12
申请号：US409607
申请日：1982-08-19
申请人： Haruo Ueno , Hidetomo Ashitaka , Kazuya Jinda , Kouichi Nakajima
发明人： Haruo Ueno , Hidetomo Ashitaka , Kazuya Jinda , Kouichi Nakajima
IPC分类号： C08F4/00 , C08F4/60 , C08F36/00 , C08F136/06 , C08F4/72
CPC分类号： C08F136/06
摘要： A process for polymerizing 1,3-butadiene, comprising bring into contact a 1,2-polymerization catalyst consisting essentially of a soluble cobalt compound, an organic aluminum halide, an organic lithium compound, and carbon disulfide or phenyl isothiocyanate with 1,3-butadiene in a polymerization medium. The process can be applied particularly advantageously in the preparation of 1,2-polybutadiene, and the resultant 1,2-polybutadiene has a content of syndiotactic 1,2-structural units of not less than 90%, a melting point of 200.degree. C. to 220.degree. C., and an intrinsic viscosity [.eta.] of 1.2 to 7.
摘要翻译： 使1,3-丁二烯聚合的方法包括使基本上由可溶性钴化合物，有机铝卤化物，有机锂化合物和二硫化碳组成的1,2-聚合催化剂或异硫氰酸苯酯与1,3- 丁二烯在聚合介质中。 该方法可以特别有利地用于1,2-聚丁二烯的制备，所得1,2-聚丁二烯的间同立构1,2-结构单元的含量不小于90％，熔点为200℃ 至220℃，特性粘度η为1.2〜7。
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公开(公告)号：US4501867A
公开(公告)日：1985-02-26
申请号：US539999
申请日：1983-10-07
申请人： Haruo Ueno , Hidetomo Ashitaka , Koichi Nakajima
发明人： Haruo Ueno , Hidetomo Ashitaka , Koichi Nakajima
IPC分类号： C08F4/00 , C08F4/60 , C08F36/00 , C08F136/06 , C08F236/00 , C08F236/10 , C08L61/00
CPC分类号： C08F136/06
摘要： A 1,2-polymerization of 1,3-butadiene is carried out in a polymerization solvent in the presence of a 1,2-polymerization catalyst consisting essentially of a cobalt compound soluble in the polymerization solvent, an organic aluminum halide, an organic magnesium compound, and carbon disulfide and/or phenyl isothiocyanate and in the presence or absence of a cis-1,4-polymerization product of 1,3-butadiene.
摘要翻译： 1,3-丁二烯的1,2-聚合在聚合溶剂中在基本上由可溶于聚合溶剂的钴化合物，有机铝卤化物，有机镁 化合物和二硫化碳和/或异硫氰酸苯酯，并存在或不存在1,3-丁二烯的顺式-1,4-聚合产物。
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