公开(公告)号：US06323149B1

公开(公告)日：2001-11-27

申请号：US09571863

申请日：2000-05-16

申请人： Toshifumi Takemori ,  Shigeharu Yamamoto ,  Masatoshi Tsuchitani

发明人： Toshifumi Takemori ,  Shigeharu Yamamoto ,  Masatoshi Tsuchitani

IPC分类号： C08F464

CPC分类号： C08F32/00 ,  C07F17/00 ,  C08F4/65908 ,  C08F4/65912 ,  C08F4/65927 ,  C08F10/00 ,  C08F10/02 ,  C08F12/00 ,  C08F12/04 ,  C08F110/02 ,  C08F210/02 ,  C08F210/16 ,  C08F2420/04 ,  Y10S526/943 ,  C08F236/20 ,  C08F2500/25 ,  C08F210/14 ,  C08F4/65925

摘要： The present invention relates to a metallocene compound as a catalyst component for the polymerization of olefins, said compound, is stable to air and moisture so that generates no hydrogen halide by hydrolysis and easily handled, and has a high storage stability and a high catalyst activity. Specifically, the catalyst component for the polymerization of olefins comprises a transition metal composition represented by the general formula [1] and [2]: (Ra Cp)m(R′b Cp)M(—X—Ar—Yc)4−(m+n)  [1] R″(Rd Cp) (R′e Cp)M(—X—Ar—Yc)2  [2] wherein M is Ti, Zr or Hf; (Ra Cp),(R′b Cp), (Rd Cp) and (R″e Cp ) each is a radical having the cyclopentadienyl skeleton; R″ is a radical which links (Rd Cp) and (R′e Cp); (—X—Ar—Yc) is a grouping in which the aromatic ring Ar substituted by a specified radical Y bonds to M through an oxygen or sulphur atom X.

摘要翻译： 本发明涉及作为烯烃聚合的催化剂组分的茂金属化合物，所述化合物对空气和水分是稳定的，因此通过水解不易产生卤化氢并易于处理，并且具有高储存稳定性和高催化剂活性 。 具体地，用于烯烃聚合的催化剂组分包括由通式[1]和[2]表示的过渡金属组合物：其中M是Ti，Zr或Hf; （R a Cp），（R bb），（R d Cp）和（R“C”）各自为具有环戊二烯基骨架的基团; R“是连接（Rd Cp）和（R'e Cp）的基团; （-X-Ar-Yc）是其中被特定基团Y取代的芳环Ar经由氧或硫原子X与M键合的基团。

公开(公告)号：US4818449A

公开(公告)日：1989-04-04

申请号：US818499

申请日：1986-01-13

申请人： Yasuhiro Yamada ,  Takeshi Imamura ,  Hidemasa Honda ,  Masatoshi Tsuchitani ,  Ryoichi Nakajima

发明人： Yasuhiro Yamada ,  Takeshi Imamura ,  Hidemasa Honda ,  Masatoshi Tsuchitani ,  Ryoichi Nakajima

IPC分类号： D01F9/14 ,  C10C1/00 ,  D01D4/02 ,  D01D4/06 ,  D01F6/00 ,  D01F9/00 ,  D01F9/155 ,  D01F9/32 ,  D01F9/12

CPC分类号： D01F9/155 ,  C10C1/00 ,  D01D4/06 ,  D01F9/00 ,  D01F9/322

摘要： When preparing carbon fibers from mesophase pitches, we usually encounter to the formation of cracks along the fiber axis. The crack formation is the most serious and troublesome problem. A simple process which can effectively prevent the crack formation comprises preparing the carbon fibers from mesophase pitches by melt spinning sufficient only to give a rotatory motion to the molten mesophase pitches just before extrusion substantially around the axis of a spinning nozzle hole. The process employs a usual nozzle plate having a pitch introducing tube and a spinning nozzle hole further containing a plug member having an outer spiral groove such as a drill point or a worm gear which is inserted within the pitch introducing tube.

摘要翻译： 当从中间相沥青制备碳纤维时，我们通常会遇到沿着纤维轴形成裂纹。 裂缝形成是最严重和最麻烦的问题。 可以有效地防止裂纹形成的简单方法包括通过熔融纺丝从中间相沥青制备碳纤维，其仅足以在基本上围绕纺丝喷嘴孔的轴线挤出之前对熔融的中间相沥青进行旋转运动。 该方法采用具有沥青引入管和纺丝喷嘴孔的通常喷嘴板，该喷嘴孔还包含插入在沥青引入管中的具有诸如钻头或蜗轮的外螺旋槽的塞构件。

公开(公告)号：US06194344B1

公开(公告)日：2001-02-27

申请号：US09414288

申请日：1999-10-07

申请人： Masatoshi Tsuchitani ,  Ryoichi Nakajima ,  Kiyotaka Suzuki ,  Hitoshi Shigematsu ,  Katsutoshi Nishitani

发明人： Masatoshi Tsuchitani ,  Ryoichi Nakajima ,  Kiyotaka Suzuki ,  Hitoshi Shigematsu ,  Katsutoshi Nishitani

IPC分类号： B01J2118

CPC分类号： B01J21/18 ,  B01J35/002 ,  B01J35/023 ,  B01J35/1019 ,  B01J35/1038 ,  B01J37/084 ,  C04B38/0022 ,  C04B2111/0081 ,  C10C3/06 ,  C04B35/52 ,  C04B35/56

摘要： A process for the preparation of a high-softening-point pitch rich in mesopores having a softening point measured by temperature gradient method of 150° C. or higher, a weight loss by heating up to 300° C. of 5 wt. % or less and mesopores of 100 mm3/g or greater, in terms of minute pore volume calculated by the Dollimore-Heal method, and a process for making carbonaceous materials carrying metal thereon are disclosed. The high-softening-point pitch rich in mesopores can easily provide carbonaceous material carrying metal thereon by using no oxidizing agent such as nitric acid, and, therefore, the high-softening-point pitch rich in mesopores is especially suitable for the production of carbonaceous materials carrying metal thereon or highly crystalline graphitized carbonaceous materials in a short heating time. The process for the production of a high-softening-point pitch rich in mesopores comprises forming micro-shaped carbonaceous materials having a size of 100 &mgr;m or less, and contacting the micro-shaped carbonaceous materials with an extracting organic solvent so as to remove 20-90 wt. % of light components from the micro-shaped carbonaceous materials. A carbonaceous material carrying metal thereon can easily be prepared by contacting the high-softening point pitch rich in mesopores with an aqueous solution of an anionic surface active agent, and then contacting the material treated with the surface active agent with an aqueous solution of metal salts.

摘要翻译： 制备富含中温孔的高软化点沥青的方法，其具有通过温度梯度法测定的软化点为150℃以上，通过加热至300℃的重量减少为5重量％ ％以下，中孔为100mm 3 / g以上，以通过Dollimore-Heal法计算的微细孔容积，以及在其上载持金属的碳质材料的制造方法。 富含中孔的高软化点沥青可以容易地通过不使用硝酸等氧化剂提供携带金属的碳质材料，因此，富孔介质的高软化点沥青特别适用于生产碳质 在短时间内在其上携带金属的材料或高度结晶的石墨化碳质材料。 用于生产富中孔的高软化点沥青的方法包括形成尺寸为100μm或更小的微型碳质材料，并使微型碳质材料与萃取有机溶剂接触以除去20 -90重量％ 来自微型碳质材料的轻组分的％。 通过使富含中孔的高软化点沥青与阴离子表面活性剂的水溶液接触，然后使用表面活性剂处理的材料与金属盐水溶液接触，可容易地制备载有金属的碳质材料 。

公开(公告)号：US5240613A

公开(公告)日：1993-08-31

申请号：US926816

申请日：1992-08-07

申请人： Masatoshi Tsuchitani ,  Sakae Naito ,  Ryoichi Nakajima ,  Kensuke Iuchi ,  Shintaro Hasebe

发明人： Masatoshi Tsuchitani ,  Sakae Naito ,  Ryoichi Nakajima ,  Kensuke Iuchi ,  Shintaro Hasebe

IPC分类号： B01D41/04

CPC分类号： B01D41/04 ,  B01D2201/085

摘要： When preparing carbon artefacts from heavy oils of petroleum or coal origin, removal of undesirable components or recovery of desirable components from raw materials or intermediates is usually required so as to improve the quality of the final products. Such removal or recovery operation is conventionally done by filtration. In the past, regeneration of filters clogged with solid carbonaceous materials inevitably formed by the filtration operations is difficult and troublesome procedures. Herein disclosed is a simple and effective process for regenerating filters clogged with solid carboneceous materials, characterized by treating the filter medium in an aqueous solution of hydrogen peroxide with heating and then optionally conducting ultrasonic washing in water or a solvent. By this simple process, clogged filters can be regenerated completely to show the same filtration performance as new filters.

公开(公告)号：US5091072A

公开(公告)日：1992-02-25

申请号：US504723

申请日：1990-04-03

申请人： Masatoshi Tsuchitani ,  Makoto Tamura ,  Kiyotaka Suzuki ,  Sjuji Okada ,  Ryoichi Nakajima ,  Sakae Naito

发明人： Masatoshi Tsuchitani ,  Makoto Tamura ,  Kiyotaka Suzuki ,  Sjuji Okada ,  Ryoichi Nakajima ,  Sakae Naito

IPC分类号： C10C1/00 ,  C10C3/00

CPC分类号： C10C1/00 ,  C10C3/00

摘要： Commercially attractive continuous processes for the preparation of mesophase pitches for manufacturing high-performance carbon fibers are disclosed. One feature resides in that conversion of a pitch into a mesophase pitch is conducted continuously by using a unique continuous dispersion-heat-treating apparatus. The other feature resides in that the raw material for hydrogenation treatment which is a pretreatment preceeding to the final heat treatment for the production of a mesophase pitch, is prepared by using a heavy oil or pitch having substantially no BTX-insoluble material as the starting raw material, subjecting the raw material to a simple four-step treatment of (1) a continuous heat treatment in a tubular heater, (2) a distillation operation, (3) a BTX-solvent extraction and (4) a distillation operation; while recycling a soluble component obtained in the step (4) to the heat treatment of step (1) and recovering a BTX-solvent insoluble component formed in step (3) as the material for the hydrogenation treatment. This feature can provide a significant increase in the yield of a mesophase pitch. Furthermore, unexpectedly, the recycle of the soluble component into the heat treatment of step (1) is helpful to improve the characteristics of the ultimate products, i.e., carbon fibers or graphite fibers. Combination of the first and the second features, of course, can provide a better commercial success. In fact, the process of the present invention can provide a carbon fiber having a tensile strength of more than 300 kg/mm.sup.2 and a graphite fiber having a tensile strength of more than 400 kg/mm.sup.2 and a modulus of elasticity of no more than 60 ton/mm.sup.2. Processes with minor modifications to the above are also disclosed.

公开(公告)号：US4925547A

公开(公告)日：1990-05-15

申请号：US397135

申请日：1989-08-21

申请人： Masatoshi Tsuchitani ,  Sakae Naito ,  Hiroshi Morijiri ,  Kiyotaka Suzuki

发明人： Masatoshi Tsuchitani ,  Sakae Naito ,  Hiroshi Morijiri ,  Kiyotaka Suzuki

IPC分类号： C10C3/02 ,  C10C1/00 ,  C10C1/16 ,  C10C3/00 ,  C10C3/04 ,  C10C3/08 ,  C10C3/10 ,  D01F9/145 ,  D01F9/15 ,  D01F9/155 ,  D01F9/32

CPC分类号： D01F9/145 ,  C10C1/00 ,  C10C1/16 ,  C10C3/00 ,  D01F9/322

摘要： A process for co-production of a pitch for the manufacture of HP carbon fibers and a pitch for the manufacture of GP carbon fibers is proposed. The pitch for the manufacture of GP carbon fibers is prepared from the spent fraction not used in the production of an optically anisotropic pitch suitable for the manufacture of HP carbon fibers. The spent fraction has hitherto been discarded as a valueless material. According to the present process, a pitch for the manufacture of so-called ultra HP carbon fibers with tensile strength of over 400 Kg/mm.sup.2 and modulus of elasticity of over 60 ton/mm.sup.2 and a pitch for the manufacture of GP carbon fibers can be produced simultaneously. Both pitches have very excellent spinnability and when they are spun, they cause no fiber cut-off even at a high spinning rate of, for example, 500 m/min or 700 m/min. One important merit of the process is that the production ratio of ultra HP carbon fibers and GP carbon fibers can easily be changed to accommodate to market's demand. Accordingly, the process has wide flexibility in operation. Of course, the effective utilization of valueless spent fraction can reduce the production costs of not only ultra HP carbon fibers but also GP carbon fibers.

公开(公告)号：US4874502A

公开(公告)日：1989-10-17

申请号：US220908

申请日：1988-07-19

申请人： Masatoshi Tsuchitani ,  Sakae Naito

发明人： Masatoshi Tsuchitani ,  Sakae Naito

IPC分类号： D01F9/15 ,  C10C1/08 ,  C10C1/16 ,  C10C1/18 ,  C10C3/08 ,  D01F9/155

CPC分类号： C10C1/08 ,  C10C1/18

摘要： The unwanted components from coal tars should be removed at a certain stage of the process for producing homogeneous spinning pitches which are suitable for use in the production of high-performance carbon fibers from coal tars. The unwanted components can be eliminated from coal tars in a very efficient manner by the following procedures: subjecting the coal tars to distillation or flash distillation so as to separate a heavy component having a boiling point higher than a predetermined temperature, dissolving the heavy component in a monocyclic aromatic hydrocarbon solvent, and subjecting the solution to filtration or centrifugation.

摘要翻译： 在制造均匀的纺丝沥青的过程的某一阶段，应从煤焦油中去除不需要的组分，这些沥青适用于生产来自煤焦油的高性能碳纤维。 可以通过以下步骤以非常有效的方式从煤焦中除去不需要的组分：将煤焦油蒸馏或快速蒸馏，以分离沸点高于预定温度的重组分，将重组分溶解在 单环芳族烃溶剂，并对溶液进行过滤或离心。

公开(公告)号：US06350831B1

公开(公告)日：2002-02-26

申请号：US09220589

申请日：1998-12-28

申请人： Toshifumi Takemori ,  Shigeharu Yamamoto ,  Masatoshi Tsuchitani

发明人： Toshifumi Takemori ,  Shigeharu Yamamoto ,  Masatoshi Tsuchitani

IPC分类号： C08F464

CPC分类号： C08F32/00 ,  C07F17/00 ,  C08F4/65908 ,  C08F4/65912 ,  C08F4/65927 ,  C08F10/00 ,  C08F10/02 ,  C08F12/00 ,  C08F12/04 ,  C08F110/02 ,  C08F210/02 ,  C08F210/16 ,  C08F2420/04 ,  Y10S526/943 ,  C08F236/20 ,  C08F2500/25 ,  C08F210/14 ,  C08F4/65925

摘要： A metallocene compound may be used as a catalyst component for the polymerization of olefins. The compound is stable to air and moisture so that it generates no hydrogen halide by hydrolysis and is easily handled, and it has high storage stability and high catalyst activity. Specifically, the catalyst component for the polymerization of olefins comprises a transition metal composition represented by the general formula [1] and [2]: (Ra Cp)m(R′b Cp)M(—X—Ar—Yc)4−(m+n)  [1] R″(Rd Cp)(R′e Cp)M(—X—Ar—Yc)2  [2] wherein M is Ti, Zr or Hf; each of (Ra Cp), (R′b Cp), (Rd Cp) and (R″e Cp) is a radical having the cyclopentadienyl skeleton; R″ is a radical that links (Rd Cp) and (R′e Cp); (—X—Ar—Yc) is a grouping in which the aromatic ring Ar substituted by a specified radical Y bonds to M through an oxygen or sulphur atom X.

摘要翻译： 茂金属化合物可用作烯烃聚合的催化剂组分。 该化合物对空气和水分是稳定的，因此通过水解不产生卤化氢，易于处理，具有高储存稳定性和高催化剂活性。 具体地，用于烯烃聚合的催化剂组分包括由通式[1]和[2]表示的过渡金属组合物：其中M是Ti，Zr或Hf; （Ra Cp），（R'b Cp），（Rd Cp）和（R''e Cp）中的每一个是具有环戊二烯基骨架的基团; R“是连接（Rd Cp）和（R'e Cp）的基团; （-X-Ar-Yc）是其中被特定基团Y取代的芳环Ar经由氧或硫原子X与M键合的基团。

公开(公告)号：US5736030A

公开(公告)日：1998-04-07

申请号：US565116

申请日：1995-11-30

申请人： Masatoshi Tsuchitani ,  Kiyotaka Suzuki ,  Ryoichi Nakajima ,  Tomohiko Sato

发明人： Masatoshi Tsuchitani ,  Kiyotaka Suzuki ,  Ryoichi Nakajima ,  Tomohiko Sato

IPC分类号： B01F3/08 ,  C10C3/00 ,  C10C3/16 ,  C10C1/00

CPC分类号： C10C3/00

摘要： A process for manufacturing fine particles or powder of pitch with a high softening point from a heavy oil raw material which is liquid at an ambient temperature or pitch having a relatively low softening point is disclosed. Fine particles of pitch with a high softening point are useful materials and can be used as carbon materials for various applications. A characteristic feature of the process resides in the utilization of emulsion of the heavy oil raw material. That is, it is disclosed a process for manufacturing fine particles of pitch with a high softening point comprising, a first step of stirring a raw material heavy oil in the presence of a surface-active agent and water by a stirring method which can provide a shearing force to produce an emulsion of fine spherical pitch particles dispersed in water, wherein the raw material heavy oil is a liquid having a viscosity of 1,000 poise or less at the stirring condition; a second step comprising causing the emulsion obtained in the first step to come in contact with an extracting organic solvent to extract and remove light components from the fine spherical particles in the emulsion, thereby obtaining fine particles of pitch with an increased softening point; and a third step comprising separating and recovering fine particles of pitch with an increased softening point.

摘要翻译： 公开了一种制造具有高软化点的细小颗粒或具有软化点的沥青粉末的方法，该重油原料是环境温度下的液体或具有较低软化点的沥青。 具有高软化点的沥青微粒是有用的材料，可用作各种应用的碳材料。 该方法的特征在于重油原料的乳液的利用。 也就是说，公开了一种制造具有高软化点的沥青的微细颗粒的方法，包括在表面活性剂和水的存在下搅拌原料重油的第一步骤，通过搅拌方法可以提供 剪切力产生分散在水中的细球形沥青颗粒的乳液，其中原料重油是在搅拌条件下具有1,000泊或更低粘度的液体; 第二步骤包括使第一步骤中获得的乳液与萃取有机溶剂接触以从乳液中的细球形颗粒提取和去除轻组分，从而获得具有增加的软化点的细沥青颗粒; 并且第三步骤包括以增加的软化点分离和回收细小的沥青颗粒。

公开(公告)号：US06569800B2

公开(公告)日：2003-05-27

申请号：US09964432

申请日：2001-09-28

申请人： Toshifumi Takemori ,  Shigeharu Yamamoto ,  Masatoshi Tsuchitani

发明人： Toshifumi Takemori ,  Shigeharu Yamamoto ,  Masatoshi Tsuchitani

IPC分类号： C08F464

CPC分类号： C08F32/00 ,  C07F17/00 ,  C08F4/65908 ,  C08F4/65912 ,  C08F4/65927 ,  C08F10/00 ,  C08F10/02 ,  C08F12/00 ,  C08F12/04 ,  C08F110/02 ,  C08F210/02 ,  C08F210/16 ,  C08F2420/04 ,  Y10S526/943 ,  C08F236/20 ,  C08F2500/25 ,  C08F210/14 ,  C08F4/65925

摘要： A metallocene compound may be used as a catalyst component for the polymerization of olefins. The compound is stable to air and moisture so that it generates no hydrogen halide by hydrolysis and is easily handled, and it has high storage stability and high catalyst activity. Specifically, the catalyst component for the polymerization of olefins comprises a transition metal composition represented by the general formula [1] and [2]: (RaCp)m(R′bCp)M(—X—Ar—Yc)4−(m+n)  [1] R″(RdCp)(R′eCp)M(—X—Ar—Yc)2  [2] wherein M is Ti, Zr or Hf; each of (RaCp), (R′b Cp), (Rd Cp) and (R″e Cp) is a radical having the cyclopentadienyl skeleton; R″ is a radical that links (Rd Cp) and (R′e Cp); (—X—Ar—Yc) is a grouping in which the aromatic ring Ar substituted by a specified radical Y bonds to M through an oxygen or sulphur atom X.

摘要翻译： 茂金属化合物可以用作烯烃聚合的催化剂组分。 该化合物对空气和水分是稳定的，因此通过水解不产生卤化氢，易于处理，具有高储存稳定性和高催化剂活性。 具体地，用于烯烃聚合的催化剂组分包括由通式[1]和[2]表示的过渡金属组合物：其中M是Ti，Zr或Hf; （RaCp），（R'b Cp），（Rd Cp）和（R''cpc）中的每一个是具有环戊二烯基骨架的基团; R“是连接（Rd Cp）和（R'e Cp）的基团; （-X-Ar-Yc）是其中被特定基团Y取代的芳环Ar经由氧或硫原子X与M键合的基团。