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11. 发明公开

EP0393724A1 Process for preparing mesophase pitches 失效
标题翻译：一种中间相过程节距生产。
公开(公告)号：EP0393724A1
公开(公告)日：1990-10-24
申请号：EP90109689.1
申请日：1988-06-16
申请人： MARUZEN PETROCHEMICAL CO., LTD.
发明人： Tsuchitani, Masatoshi , Tamura, Makoto , Suzuki, Kiyotaka, E-5404, Maruzen Sekiyu Kagaku , Okada, Shuji, B-2402, Maruzen Sekiyu Kagaku , Nakajima, Ryoichi , Naito, Sakae
IPC分类号： C10C1/00 , C10C3/00
CPC分类号： C10C1/00 , C10C3/00
摘要： A process for the preparation of an excellent mesophase pitch suitable for use as a spinning pitch for the production of high-performance carbon fibers is disclosed. The mesophase pitch can satisfy the four remarkable characteristics at the same time, i.e., a Mettler method softening point of below 310°C, a mesophase content of above 90% as examined on a polarized microscope, a quinoline insoluble content of less than 10 wt%, and a xylene soluble content of less than 10 wt%. The mesophase pitch is particularly homogeneous and is easily spinnable. The process can be characterized 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 hydrogenation treatment and succeeding final heat treatment for converting into a mesophase pitch. 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. The process of the present invention can provide a carbon fiber having a tensile strength of more than 2942 MPa (300 kg/mm²) and a graphite fiber having a tensile strength of more than 3923 MPa (400 kg/mm²) and a modulus of elasticity of more than 588 GPa (60 ton/mm²).

12. 发明公开

EP0246591A1 Process for the preparation of mesophase pitches 失效转让
标题翻译： Verfahren zur Herstellung mesophaser Peche。
公开(公告)号：EP0246591A1
公开(公告)日：1987-11-25
申请号：EP87107189.0
申请日：1987-05-18
申请人： Director-General of Agency of Industrial Science and Technology , MARUZEN PETROCHEMICAL CO., LTD.
发明人： Tsuchitani, Masatoshi , Naito, Sakae , Nakajima, Ryoichi
IPC分类号： C10C3/00 , C10C3/08
CPC分类号： D01F9/15 , C10C1/18 , C10C1/19 , C10C3/002 , C10C3/08 , D01F9/155
摘要： A process for the preparation of an excellent mesophase pitch suitable for use as a spinning pitch for the production of high performance carbon fibers is disclosed. The mesophase pitch can satisfy the four remarkable characteristics at the same time, i.e., a softening point of below 320°C as determined by Mettler method, a mesophase content of above 90% as examined on a polarized microscope, a quinoline insoluble content of less than 20%, and a xylene soluble content of less than 20%. The mesophase pitch is particularly homogeneous and is easily spinnable. The process can be characterized by a preliminary extraction step, a continuous heat treatment step, and an extraction step. In some cases, the preliminary extraction step can be omitted. Graphite fibers having a tensile strength of about 400 Kg/mm² and a modulus of elasticity of above 60 ton/mm² can be obtained from the mesophase pitch. Further, even carbon fibers prepared at a carbonization temperature of 1000°C have a tensile strength of about 300 Kg/mm² .
摘要翻译：公开了一种制备适合用作生产高性能碳纤维的纺丝沥青的优良中间相沥青的方法。中间相沥青可以同时满足四个显着特征，即通过Mettler方法测定的软化点低于320℃，在偏光显微镜下检测的中间相含量高于90％，喹啉不溶物含量少 20％以上，二甲苯可溶物含量小于20％。中间相沥青是特别均匀的并且易于纺丝。该方法可以通过预萃取步骤，连续热处理步骤和萃取步骤来表征。在一些情况下，可以省略初步提取步骤。可以从中间相沥青得到拉伸强度为约400Kg / mm 2，弹性模量高于60吨/ mm 2的石墨纤维。此外，即使在碳化温度为1000℃下制备的碳纤维的拉伸强度也为约300Kg / mm 2。

13. 发明授权

EP0246591B1 Process for the preparation of mesophase pitches 失效转让
标题翻译：制备麻醉剂的方法
公开(公告)号：EP0246591B1
公开(公告)日：1990-10-31
申请号：EP87107189.0
申请日：1987-05-18
申请人： Director-General of Agency of Industrial Science and Technology , MARUZEN PETROCHEMICAL CO., LTD.
发明人： Tsuchitani, Masatoshi , Naito, Sakae , Nakajima, Ryoichi
IPC分类号： C10C3/00 , C10C3/08
CPC分类号： D01F9/15 , C10C1/18 , C10C1/19 , C10C3/002 , C10C3/08 , D01F9/155

14. 发明公开

EP0358048A1 Process for producing pitch for the manufacture of high-performance carbon fibers together with pitch for the manufacture of general-purpose carbon fibers 失效
标题翻译：一种用于与生产沥青的用于任何目的的碳纤维一起制备Spitzenleistungspechkohlenstoffasern过程。
公开(公告)号：EP0358048A1
公开(公告)日：1990-03-14
申请号：EP89115563.2
申请日：1989-08-23
申请人： MARUZEN PETROCHEMICAL CO., LTD.
发明人： Tsuchitani Masatoshi , Naito, Sakae , Moriziri, Hiroshi , Suzuki, Kiyotaka E-5404, Maruzen Sekiyu Kagaku
IPC分类号： C10C1/00 , C10C3/00 , D01F9/145
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 fibrs with tensile strength of over 400 Kg/mm² and modulus of elasticity of over 60 ton/mm′ and a pitch for the manufacture of GP carbon fibers can be produced simulteneously. 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.
摘要翻译：一种用于联合生产用于碳纤维和HP GP碳纤维的制造中的节距的制造沥青的过程被提议。 GP碳纤维的制造中节距从在生产适用于碳纤维HP的制造中的光学各向异性沥青的未使用的废馏分制备。废馏分迄今丢弃作为毫无价值材料。。根据本发明的方法中，为了制造的间距所谓具有400千克/毫米<2>和超过60吨/平方毫米分钟弹性模量和对GP的制造间距抗拉强度超HP碳fibrs 碳纤维可以simulteneously来制造。两个节距具有非常优异的自旋能力，并且当它们被纺丝，它们不会引起纤维切断，即使在高纺丝速度，例如为500米/分钟或700米/分钟。该过程的一个重要优点是没有超高性能碳纤维和碳纤维GP的生产比例可以很容易地改变，以适应市场的需求。因此，该方法具有在操作中有很大的灵活性。当然，没有价值的有效利用废分数可以降低不仅超高性能碳纤维，但这样GP碳纤维的生产成本。

15. 发明公开

EP0299222A1 Process for preparing pitches 失效
标题翻译： Verfahren zur Herstellung von Pech。
公开(公告)号：EP0299222A1
公开(公告)日：1989-01-18
申请号：EP88109645.7
申请日：1988-06-16
申请人： MARUZEN PETROCHEMICAL CO., LTD.
发明人： Tsuchitani, Masatoshi , Tamura, Makoto , Suzuki, Kiyotaka / E-5404, Maruzen Sekiyu, , Okada, Shuji , Nakajima,, Ryoichi , Naito, Sakae
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/mm² and a graphite fiber having a tensile strength of more than 400 kg/mm² and a modulus of elasticity or more than 60 ton/mm². Processes with minor modifications to the above are also disclosed.
摘要翻译：公开了用于制备用于制造高性能碳纤维的中间相沥青的商业上有吸引力的连续方法。一个特征在于通过使用独特的连续分散热处理装置连续地进行沥青转化为中间相沥青。另一个特征在于，通过使用基本上不含BTX不溶性材料的重油或沥青作为起始原料，制备作为用于生产中间相沥青的最终热处理之前的预处理的氢化处理原料材料，对原料进行简单的四步处理（1）在管式加热器中的连续热处理，（2）蒸馏操作，（3）BTX-溶剂萃取和（4）蒸馏操作; 同时将步骤（4）中获得的可溶组分再循环到步骤（1）的热处理中，并回收步骤（3）中形成的不溶于BTX的溶剂组分作为氢化处理材料。该特征可以显着提高中间相沥青的产率。此外，意想不到的是，将可溶组分再循环到步骤（1）的热处理中有助于改善最终产物，即碳纤维或石墨纤维的特性。结合第一和第二功能，当然可以提供更好的商业成功。实际上，本发明的方法可以提供拉伸强度大于300kg / mm 2的碳纤维和拉伸强度大于400kg / mm 2的石墨纤维，弹性或超过60吨/ mm 2。还公开了对上述的微小修改的处理。

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