公开(公告)号：US5182011A

公开(公告)日：1993-01-26

申请号：US616836

申请日：1990-11-21

Applicant: Masatoshi Tsuchitani ,  Makoto Tamura ,  Kiyotaka Suzuki ,  Shuji Okada ,  Ryoichi Nakajima ,  Sakae Naito

Inventor： Masatoshi Tsuchitani ,  Makoto Tamura ,  Kiyotaka Suzuki ,  Shuji Okada ,  Ryoichi Nakajima ,  Sakae Naito

IPC: C10C1/00 ,  C10C3/00

CPC classification number: C10C3/00 ,  C10C1/00

Abstract: 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 more than 60 ton/mm.sup.2. Processes with minor modifications to the above are also disclosed.

Abstract translation: 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BTX-溶剂不溶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。 事实上，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的石墨纤维和大于60吨的弹性模量 / mm2。 还公开了对上述的微小修改的处理。

公开(公告)号：US4820401A

公开(公告)日：1989-04-11

申请号：US48376

申请日：1987-05-11

Applicant: Masatoshi Tsuchitani ,  Sakae Naito ,  Ryoichi Nakajima

Inventor： Masatoshi Tsuchitani ,  Sakae Naito ,  Ryoichi Nakajima

IPC: C10C3/02 ,  C10C1/16 ,  C10C1/18 ,  C10C1/19 ,  C10C3/00 ,  C10C3/04 ,  C10C3/08 ,  C10C3/10 ,  D01F9/145 ,  D01F9/15 ,  D01F9/155

CPC classification number: D01F9/15 ,  C10C1/18 ,  C10C1/19 ,  C10C3/002 ,  C10C3/08 ,  D01F9/155

Abstract: 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.degree. 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/mm.sup.2 and a modulus of elasticity of above 60 ton/mm.sup.2 can be obtained from the mesophase pitch. Further, even carbon fibers prepared at a carbonization temperature of 1000.degree. C. have a tensile strength of about 300 Kg/mm.sup.2.

公开(公告)号：US4789456A

公开(公告)日：1988-12-06

申请号：US48415

申请日：1987-05-11

Applicant: Masatoshi Tsuchitani ,  Sakae Naito ,  Ryoichi Nakajima

Inventor： Masatoshi Tsuchitani ,  Sakae Naito ,  Ryoichi Nakajima

IPC: C10C3/02 ,  C10C1/16 ,  C10C3/00 ,  C10C3/04 ,  C10C3/06 ,  C10C3/10 ,  C10G67/02 ,  C10G69/06 ,  D01F9/145

CPC classification number: C10C3/00

Abstract: A process for an efficient preparation of a mesophase pitch is disclosed. The process is suitable for the production of high performance carbon fibers, from a coal tar or a petroleum residual oil. More particularly, the present invention relates to a process for the preparation of a homogeneous mesophase pitch which comprises a continuous thermal treatment of a heavy oil or a pitch which does not contain quinoline insoluble fractions, in the presence or absence of an aromatic oil, subsequent distillation of the thermally treated product, recovery of a pitch with extremely low quinoline insoluble contents, hydrogenation of the pitch by continuous thermal treatment in the presence of a hydrogen-donating solvent, distillation and recovery of a hydrogenation pitch, and thermal treatment of the hydrogenated pitch. The mesophase pitch prepared by the process of the present invention is suitable for the production of high performance carbon fibers.

公开(公告)号：US4705618A

公开(公告)日：1987-11-10

申请号：US849568

申请日：1986-04-08

Applicant: Masatoshi Tsuchitani ,  Ryoichi Nakajima

Inventor： Masatoshi Tsuchitani ,  Ryoichi Nakajima

IPC: C10C3/02 ,  C10C1/08 ,  C10C1/16 ,  C10C1/19 ,  C10C3/00 ,  C10C3/06 ,  C10C3/10 ,  D01F9/145 ,  D01F9/155 ,  D01F9/12

CPC classification number: C10C1/08 ,  C10C1/16 ,  C10C1/19 ,  C10C3/002 ,  C10C3/06 ,  D01F9/145

Abstract: Until now, it has not yet been succeeded to prepare high performance carbon fibers having satisfactory strength from heavy oils of coal or petroleum origin. We now succeeded to prepare an excellent intermediate pitch which allows the preparation of high performance carbon fibers having tensile strength of higher than 300 Kg/mm.sup.2 and Young's modulus of 50 ton/mm.sup.2.The intermediate pitch can be obtained by heating a heavy oil of coal or petroleum origin in a tubular heater under a specific conditions, and then flash distilling the heater effluent in a flash distillation column under a specific condition so as to remove lighter fractions and recovering heavy fraction from the column bottom as the intermediate pitch. The process for the preparation of the intermediate pitch is simple and economical and allows continuous production without fluctuation of quality of the intermediate pitch. The intermediate pitch is also suitable for the production of higher density carbon products.

公开(公告)号：US5240613A

公开(公告)日：1993-08-31

申请号：US926816

申请日：1992-08-07

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

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

IPC: B01D41/04

CPC classification number: B01D41/04 ,  B01D2201/085

Abstract: 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

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

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

IPC: C10C1/00 ,  C10C3/00

CPC classification number: C10C1/00 ,  C10C3/00

Abstract: 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：US5052116A

公开(公告)日：1991-10-01

申请号：US486627

申请日：1990-02-28

Applicant: Sakuji Oide ,  Ryoichi Nakajima

Inventor： Sakuji Oide ,  Ryoichi Nakajima

IPC: G01C17/28 ,  G01C17/30

CPC classification number: G01C17/30

Abstract: A method of measuring an azimuth by detecting the earth's magnetism by using two perpendicular coils to detect the azimuth according to the outputs of the coils, including the steps of converting the outputs of the coils by multiplying them by a constant so as to vary in a range determined by a reference value, dividing the converted signal by the reference value, and measuring the azimuth at each coil output according to an inverse trigonometric function, with the divided result as a variable. An azimuth measuring apparatus for executing the method is also provided. Thus, the method and apparatus can accurately detect the azimuth and can further detect an error due to a disorder of the earth's magnetism or the inclination of the apparatus.

Abstract translation: 一种通过使用两根垂直线圈检测地磁的方法来测量方位角的方法，以便根据线圈的输出来检测方位角，包括通过将线圈的输出乘以常数来变化的步骤，以便在 由参考值确定的范围，将转换的信号除以参考值，并根据反三角函数测量每个线圈输出处的方位角，将分割结果作为变量。 还提供了一种用于执行该方法的方位测量装置。 因此，该方法和装置可以精确地检测方位并且可以进一步检测由于地球磁性的紊乱或装置的倾斜引起的误差。

公开(公告)号：US4818449A

公开(公告)日：1989-04-04

申请号：US818499

申请日：1986-01-13

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

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

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

CPC classification number: D01F9/155 ,  C10C1/00 ,  D01D4/06 ,  D01F9/00 ,  D01F9/322

Abstract: 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.

Abstract translation: 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：US06551829B1

公开(公告)日：2003-04-22

申请号：US09256078

申请日：1999-02-24

Applicant: Hiroyuki Takano ,  Jyun Shima ,  Katumi Mori ,  Yasuo Suzuki ,  Ryoichi Nakajima ,  Hajime Watanabe

Inventor： Hiroyuki Takano ,  Jyun Shima ,  Katumi Mori ,  Yasuo Suzuki ,  Ryoichi Nakajima ,  Hajime Watanabe

IPC: C12N1564

CPC classification number: C12R1/865 ,  A21D8/047

Abstract: Disclosed is a dry baker's yeast of a diploid, practical baker's yeast, which is obtained by mating an ATH1 and/or NTH1 gene-disrupted, haploid yeast as produced through gene manipulation of disrupting the ATH1 and/or NTH1 gene in an a-type haploid yeast of which the diploid is practical baker's yeast, with an ATH1 and/or NTH1 gene-disrupted, haploid yeast as produced through gene manipulation of disrupting the ATH1 and/or NTH1 gene in an &agr;-type haploid yeast of which the diploid is practical baker's yeast. The dry yeast does not require sugared water for its re-activation but can be rapidly re-activated only with water. Using the yeast, therefore, breads having good taste can be produced within a short period of time.

Abstract translation: 公开了一种二倍体干实验面包酵母的干面包酵母，其通过将通过基因操作产生的ATH1和/或NTH1基因破坏的单倍体酵母进行交配而获得，所述酵母通过基因操作来破坏a型中的ATH1和/或NTH1基因 二倍体是实用的面包酵母的单倍体酵母，具有ATH1和/或NTH1基因破坏的单倍体酵母，其通过在二倍体为α型单倍体酵母中破坏ATH1和/或NTH1基因的基因操作产生 实木面包酵母 干酵母不需要加糖的水来重新激活，但只能用水快速重新激活。 因此，使用酵母，可以在短时间内产生具有良好味道的面包。

公开(公告)号：US06194344B1

公开(公告)日：2001-02-27

申请号：US09414288

申请日：1999-10-07

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

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

IPC: B01J2118

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

Abstract: 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.

Abstract translation: 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 。