Asphalts, Tars, Pitches And Resins Patents (Class 208/22)
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Patent number: 4655902Abstract: In a process for producing an optically anisotropic carbonaceous pitch having a low softening point for the production of carbon material starting oil to be used is a tar-like substance which is a mixture of compounds not substantially containing chloroform insolubles but containing components having a boiling point of 540.degree. C. or more as principal components and consisting principally of carbon and hydrogen. The tar-like substance has a content of n-heptane insolubles of up to 1 wt % and contains an aromatic oil fraction and a resin fraction as the principal components of n-heptane soluble components. The aromatic carbon fraction, fa, is at least 0.7, the number-average molecular weight is up to 1,000 and the maximum molecular weight is up to 2,000 for each of the aromatic oil and resin fractions.Type: GrantFiled: September 3, 1985Date of Patent: April 7, 1987Assignee: Toa Nenryo Kogyo Kabushiki KaishaInventors: Takayuki Izumi, Tsutomu Naito, Masuo Shinya, Tomio Nomura
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Patent number: 4637906Abstract: A method of producing carbon materials having high density and strength, which method includes starting from a calcined product or its classified product having particular properties obtained by calcining a residue after heat treatment, solvent extraction and filtration of coal tar pitch at 250.degree.-500.degree. C. in an inert gas atmosphere, and then molding, firing and graphitizing it.Type: GrantFiled: March 20, 1985Date of Patent: January 20, 1987Assignee: Kawasaki Steel CorporationInventors: Noriyoshi Fukuda, Ken Nagasawa
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Patent number: 4631181Abstract: A mesophase pitch suitable for carbon products, particularly for carbon fibers, which has a mesophase content of at least 40%, preferably at least 60%, and a larger mesophase domain, is produced by adding at least one part by weight of at least one of an alcohol and a phenol to 100 parts by weight of heavy bitumens, subjecting the resulting mixture to pretreatment by heating at least at 250.degree. C., and then subjecting the pretreated mixture to heat treatment until mesophases are formed.Type: GrantFiled: March 28, 1985Date of Patent: December 23, 1986Assignees: Nippon Steel Corporation, Nippon Steel Chemical Co., Ltd.Inventors: Mitsuaki Matsumoto, Masatosi Furuyama, Tadao Tomioka, Hirofumi Sunago, Masakazu Higuchi
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Patent number: 4631088Abstract: A road asphalt composition having a penetration at 25.degree. C. in the range of 85 to 100 is made by blending together: (a) a pitch having an initial boiling point of at least 520.degree. C. obtained as a residue in the visbreaking of crude oil, and (b) a distillation residue having a penetration at 25.degree. C. in the range of 150 to 500 obtained in the distillation of crude oil.Type: GrantFiled: December 11, 1985Date of Patent: December 23, 1986Assignee: Her Majesty the Queen in right of Canada, as represented by the Minister of Energy, Mines and ResourcesInventor: Marc-Andre Poirier
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Patent number: 4620919Abstract: Pitch for the production of carbon fibers which contains from 5 to 40% of the optically anisotropic region which is insoluble in organic solvents having a solubility parameter from 7.4 to 9.0 but is soluble in organic solvents having a solubility parameter from 9.2 to 11.0.Type: GrantFiled: December 23, 1985Date of Patent: November 4, 1986Assignee: Nippon Oil CompanyInventors: Seiichi Uemura, Hiroaki Takashima, Osamu Kato, Hazime Nakazima
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Patent number: 4618373Abstract: A process for air-blowing asphalt in the presence of hydrohalic acids, particularly hydrobromic acid, and an asphalt composition comprising a major amount of asphalt and a minor but effective amount of hydrohalic acid is disclosed.Type: GrantFiled: February 28, 1984Date of Patent: October 21, 1986Assignee: Chevron Research CompanyInventor: Penny K. Eidem
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Patent number: 4608150Abstract: The invention provides a novel pitch material useful as a base material of carbon fibers having excellent mechanical properties and characterized by a unique combination of several property parameters including the content of the optically anisotropic phase of at least 80%, a content of the pyridine-insoluble matter in the range from 30 to 70% by weight, a number average molecular weight in the range from 1000 to 1400 and a softening point in the range from 330.degree. to 380.degree. C. Such a pitch material is obtained from a starting pitch of a petroleum-based residual oil freed from light oily matter through a two-step heat treatment, of which the first step is performed at 400.degree. to 460.degree. C. under a pressure of 5 to 50 mmHg and the second step is performed at 450.degree. to 550.degree. C. for 0.2 to 30 minutes under a pressure of 0.1 to 5 mmHg. The advantages obtained by use of a film evaporator in the above mentioned heat treatment are described.Type: GrantFiled: March 11, 1985Date of Patent: August 26, 1986Assignee: Idemitsu Kosan Company LimitedInventors: Masaaki Itoi, Masakatsu Ohta, Taizo Sugioka, Kunio Yoshihara, Hiroshi Nishitani
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Patent number: 4606808Abstract: The invention provides a method for the preparation of a pitch spinnable into pitch filaments as a precursor of carbon fibers starting from a pitch material such as coal tar and coal tar pitch. Different from the conventional procedure involving hydrogenation of the starting pitch, the starting pitch in the inventive method is first heated together with an aromatic oil, preferably, in the presence of a cracking catalyst such as silica-alumina and zeolite at 350.degree. to 500.degree. C. for 10 to 60 minutes under no pressurization with hydrogen and, after removal of insoluble materials, then heated at a temperature of 430.degree. to 600.degree. C. The thus obtained pitch for spinning has good spinnability and the carbon fibers prepared from the pitch have a unique microscopic structure and excellent physical properties exceeding by far the conventional pitch-based carbon fibers and approximating the HP-grade carbon fibers prepared from polyacrylonitrile fibers.Type: GrantFiled: April 23, 1984Date of Patent: August 19, 1986Assignee: Director-General of the Agency of Industrial Science & TechnologyInventors: Yasuhiro Yamada, Takeshi Imamura, Masao Shibata, Seiji Arita, Hidemasa Honda
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Patent number: 4604184Abstract: The present invention relates to specialty pitches having low Q.I. content, lower viscosity, lower average Q.I. particle size, lower ash content, higher toluene insoluble and beta-resin content. They may be prepared by extracting the coal-tar material with a solvent, where the solvent contains at least one n-methyl-2-pyrrolidone and the wash oil fraction of coal-tar distillate. The solvent-dissolved fraction of the coal-tar material is then distilled to obtain the specialty pitch material.Type: GrantFiled: February 4, 1985Date of Patent: August 5, 1986Assignee: Domtar Inc.Inventors: Samuel Cukier, Henry A. F. L. Kremer
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Patent number: 4601813Abstract: In a process for producing an optically anisotropic carbonaceous pitch having a low softening point for the production of carbon material a starting oil to be used is a tar-like substance which is a mixture of compounds not substantially containing chloroform insolubles but containing components having a boiling point of 540.degree. C. or more as principal components and consisting principally of carbon and hydrogen. The tar-like substance has a content of n-heptane insolubles of up to 1 wt % and contains an aromatic oil fraction and a resin fraction as the principal components of n-heptane soluble components. The aromatic carbon fraction, fa, is at least 0.7, the number-average molecular weight is up to 1,000 and the maximum molecular weight is up to 2,000 for each of the aromatic oil and resin fractions.Type: GrantFiled: August 27, 1982Date of Patent: July 22, 1986Assignee: Toa Wenryo Kogyo Kabushiki KaishaInventors: Takayuki Izumi, Tsutomu Naito, Masuo Shinya, Tomio Nomura
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Patent number: 4600496Abstract: Pitch is converted to mesophase pitch in the presence of catalytically effective amounts of oxides, diketones, carboxylates and carbonyls of metals selected from vanadium, chromium, molybdenum, iron, nickel and cobalt. The crystalloidal or mesophase pitch obtained can be used for the production of carbon fibers and other carbon and graphite products and articles of manufacture of unusually high quality.Type: GrantFiled: November 18, 1983Date of Patent: July 15, 1986Assignee: Phillips Petroleum CompanyInventors: Paul J. Cheng, Tammy M. Elkins
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Patent number: 4597853Abstract: A pitch is disclosed which is used as a raw material for making carbon fibers. The pitch has a quinoline insoluble content of 7-18% by weight and a toluene insoluble content of 70-90% by weight. Further, the pitch preferably has a n-heptane soluble content of 1.0% by weight or less. A process for producing the pitch is also disclosed. The process comprises carrying out thermal modification of a petroleum heavy residual oil having a boiling point of 400.degree. C. or more (atmospheric pressure) and a sulfur content of 1.5% by weight or less. Insoluble substances are then separated and removed by heating at a temperature of 380.degree. C. or less. Thereafter, a low boiling point fraction is removed by vacuum distillation. The pitch can be utilized to producd carbon fibers without breaking of filaments in spinning or adhesion by fusion of the fibers in infusibilization. The carbon fibers produced have a high tensile strength and high modulus of elasticity.Type: GrantFiled: February 23, 1983Date of Patent: July 1, 1986Assignee: Mitsubishi Oil Co., Ltd.Inventors: Kunihiko Moriya, Kazuhito Tate, Goro Muroga, Kazuhiro Yanagida
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Patent number: 4596652Abstract: A process for producing a mesophase pitch by heating a carbonaceous pitch at 350.degree. to 550.degree. C. wherein the heat treatment is conducted while supplying a hydrogen donor to the pitch. The mesophase pitch thus produced has an excellent spinnability.Type: GrantFiled: February 8, 1984Date of Patent: June 24, 1986Assignee: Mitsubishi Petrochemical Co., Ltd.Inventors: Haruo Shibatani, Kunimasa Takahashi
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Patent number: 4591424Abstract: A method of preparing an carbonaceous pitch, including the steps of:subjecting a raw material oil to thermal cracking conditions while removing cracked, light hydrocarbon components to obtain a pitch product containing at least 5 weight % of mesophase and not more than 10 weight % of light hydrocarbon components with a boiling point at 60 mmHg of 300.degree. C. or less and having a softening point of between 160.degree. and 220.degree. C., the raw material oil being composed mainly of a residual oil which has a boiling point of 350.degree. C. or more and which is derived from a naphthene base petroleum crude; andremoving the mesophase from the pitch product to obtain a substantially mesophase-free carbonaceous pitch.Type: GrantFiled: May 17, 1984Date of Patent: May 27, 1986Assignee: Fuji Standard Research, Inc.Inventors: Shimpei Gomi, Tomio Arai, Fumio Mogi, Takao Nakagawa, Kunio Miura, Sugio Otani
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Patent number: 4589974Abstract: This invention describes a substantially homogeneous, optically anisotropic carbonaceous pitch characterized in that the major portion of said pitch consists of a continuous, optically anisotropic phase, said optically anisotropic phase contains spherules of an optically isotropic phase having diameters of not more than about 100 .mu.m and dispersed in said optically anisotropic phase, the content of said optically isotropic spherules is up to about 20% on the basis of said pitch as a whole, said pitch contains at least about 30 wt % (based on said pitch) of a quinoline-soluble component, and said pitch has a lower softening point.Type: GrantFiled: September 7, 1982Date of Patent: May 20, 1986Assignee: Toa Nenryo Kogyo Kabushiki KaishaInventor: Takayuki Izumi
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Patent number: 4589975Abstract: A method of producing a precursor pitch for use in the production of carbon fibers, which comprises hydrogenating a soft or middle tar pitch to obtain a hydrogenated pitch containing no free carbon and high molecular weight components and then subjecting it to a heat treatment. In this method, the hydrogenation is carried out in the presence of tetralin at a temperature of 400.degree.-450.degree. C., and the heat treatment after the removal of solvent insoluble components and solvent is carried out in an inert gas atmosphere at a temperature of 450.degree.-500.degree. C. and under a reduced pressure of 0.1-10 Torr.Type: GrantFiled: December 27, 1984Date of Patent: May 20, 1986Inventors: Kozo Yudate, Yukihiro Ohsugi, Mamoru Kamishita, Ken Nagasawa
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Patent number: 4590055Abstract: The invention provides carbon fibers having mechanical properties equival to or even better than those of the polyacrylonitrile-based carbon fibers from a bituminous material, e.g. coal tar pitch, as the starting material. The starting pitch is first partially hydrogenated in tetrahydroquinoline under specific conditions followed by a heat treatment to give a pitch composition suitable for spinning which can be characterized by several parameters including the proportions of the carbons and hydrogens having different chemical shifts in the NMR analysis. The pitch composition for spinning is then subjected to spinning under specific conditions including the temperature condition for controlling the viscosity behavior of the molten pitch composition determined by use of the Andrade's equation and the pitch filament is then infusibilized in an oxidative atmosphere and carbonized in an inert atmosphere into carbon fibers having a tensile strength of at least 200 kg/mm.sup.Type: GrantFiled: August 23, 1983Date of Patent: May 20, 1986Assignee: Director-General of the Agency of Industrial Science and TechnologyInventors: Yasuhiro Yamada, Takeshi Imamura, Hidemasa Honda, Toru Sawaki, Hideharu Sasaki
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Patent number: 4579645Abstract: Provided is a starting pitch for producing carbon fiber by heat-treating the starting pitch to obtain a precursor pitch, melt-spinning the precursor pitch, then rendering the resultant pitch fiber infusible, followed by carbonization, and further followed by graphitization if required, the starting pitch comprising a mixture of (a) 100 parts by weight of a pitch and (b) 5 to 500 parts by weight of a methanol-insoluble and benzene-soluble component contained in a heavy oil obtained in a fluid catalytic cracking of petroleum, the heavy oil having a boiling range not lower than 200.degree. C.Type: GrantFiled: April 12, 1983Date of Patent: April 1, 1986Assignee: Nippon Oil Company, LimitedInventors: Seiichi Uemura, Hiroaki Takashima, Osamu Kato, Michiharu Harakawa
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Patent number: 4575411Abstract: A precursor pitch for the production of carton fibers is obtained by heat-treating a carbonaceous pitch in the form of a thin film having a thickness not larger than 5 mm at a temperature in the range of 250.degree. to 390.degree. C. and under a reduced pressure not higher than 100 mmHg. By melt-spinning this precursor pitch and subjecting the resultant pitch fiber to infusiblization and carbonization and, if required, to subsequent graphitization, there is obtained a high quality carbon fiber.Type: GrantFiled: November 21, 1984Date of Patent: March 11, 1986Assignee: Nippon Oil Company, LimitedInventors: Seiichi Uemura, Shunichi Yamamoto, Takao Hirose, Hiroaki Takashima, Osamu Kato
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Patent number: 4559128Abstract: Disclosed is a one-step method of producing an industrial asphalt from a bituminous material which comprises mixing together without air-blowing:(a) a feed material comprising a bituminous material having a viscosity of at least 50 centistokes at 350 degrees Fahrenheit and wherein the feed petroleum residuum forms a single phase when mixed with 5 percent of 98 percent sulfuric acid; and(b) from about 0.1 to 20.0 percent by weight of sulfuric acid, said mixing being done at a temperature in the range of 351 to 600 degrees Fahrenheit, whereby the softening point of the feed is substantially increased and the penetration is significantly decreased.Type: GrantFiled: August 31, 1984Date of Patent: December 17, 1985Assignee: Chevron Research CompanyInventor: Judson E. Goodrich
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Patent number: 4551225Abstract: An improved process for preparing an optically anisotropic pitch which comprises heating a pitch feed material at a temperature within the range of about 350.degree. C. to 450.degree. C. while passing an inert gas therethrough at a rate of at least 2.5 SCFH/lb of pitch feed material and agitating said pitch feed material at a stirrer rate of from about 500 to 600 rpm to obtain an essentially 100% mesophase pitch product suitable for carbon production.Type: GrantFiled: May 23, 1984Date of Patent: November 5, 1985Assignee: E. I. Du Pont de Nemours and CompanyInventor: Ghazi B. Dickakian
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Patent number: 4548704Abstract: A pitch suitable for carbon fiber manufacture features a pitch having a weight content of between 80 and 100 percent toluene insolubles and greater than about 10 percent quinoline insolubles. The pitch is derived from a deasphaltenated middle fraction of a feedstock. The pitch is characterized as being relatively free of impurities and ash. The pitch can be spun directly into carbon fibers.Type: GrantFiled: September 4, 1984Date of Patent: October 22, 1985Assignee: E. I. Du Pont De Nemours and CompanyInventor: Ghazi B. Dickakian
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Patent number: 4548703Abstract: A pitch suitable for carbon fiber manufacture features a pitch having a weight content of between 80 and 100 percent toluene insolubles. The pitch is derived from a deasphaltenated middle fraction of a feedstock. The pitch is characterized as being relatively free of impurities and ash. The pitch can be spun directly into carbon fibers.Type: GrantFiled: September 4, 1984Date of Patent: October 22, 1985Assignee: E. I. Du Pont de Nemours and CompanyInventor: Ghazi B. Dickakian
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Patent number: 4540480Abstract: A process for preparing a hydrogenated petroleum resin in which a petroleum resin having an aromatic ring is hydrogenated by introducing hydrogen gas and the molten petroleum resin from the upper or lower part of a vertical reactor to parallel-currently pass them through a fixed bed of a supported catalyst containing platinum and/or rhodium which may be used in combination with at most 50% by weight of a metal selected from palladium, ruthenium and rhenium.Type: GrantFiled: October 21, 1983Date of Patent: September 10, 1985Assignee: Arakawa Kagaku Kogyo Kabushiki KaishaInventors: Noriharu Azuma, Shigeru Suetomo
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Patent number: 4534850Abstract: A composition for an optically anisotropic carbonaceous pitch suitable for the production of a carbon material having a high tensile strength and a high modulus of elasticity. The composition comprises about 2 to 20 percent by weight of a first, n-heptane-soluble component, about 15 to 45 percent by weight of an n-heptane-insoluble and benzene-soluble, second component and the balance of the composition including benzene-insoluble components. The composition has a volume ratio of an optically anisotropic phase of at least about 90% and a softening point of up to about 320.degree. C.Type: GrantFiled: April 22, 1983Date of Patent: August 13, 1985Assignee: Toa Nenryo Kogyo Kabushiki KaishaInventors: Takayuki Izumi, Tsutomu Naito, Tomoo Nakamura
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Patent number: 4533535Abstract: A starting pitch for carbon fibers is obtained by mixing (1) 100 parts by volume of a heavy fraction oil boiling at not lower than 200.degree. C. and obtained at the time of fluidized catalytic cracking of petroleum with (2) 10 to 200 parts by volume of a fraction boiling in the range of 250.degree. to 550.degree. C. obtained by distilling under reduced pressure an oil produced at the time of heat treating a starting pitch and then heat treating the resulting mixture at a temperature of from 370.degree. C. to 480.degree. C. under a pressure of from 2 to 50 Kg/cm.sup.2.G thereby to obtain the starting pitch for carbon fibers. The thus obtained starting pitch is heat treated to obtain a precursor pitch which is melt spun, infusibilized, carbonized or graphitized to obtain the carbon fibers.Type: GrantFiled: February 10, 1984Date of Patent: August 6, 1985Assignee: Nippon Oil Co., Ltd.Inventors: Seiichi Uemura, Shunichi Yamamoto, Takao Hirose, Hiroaki Takashima, Osamu Katoh
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Patent number: 4529498Abstract: A method for producing a 100% mesophase pitch composed only of Q.I. and Q.S. components is provided. This method comprises subjecting petroleum-origin pitch to heat treatment with stirring under a stream of a hydrocarbon gas of small carbon atom numbers at atmospheric or superatmospheric pressure, holding said heat-treated pitch in quiescent state to melt and coalesce only the mesophase therein and dividing and separating non-mesophase and mesophase layers. Resulting 100% mesophase enables us to produce high strength, high modulus carbon fibers.Type: GrantFiled: June 24, 1983Date of Patent: July 16, 1985Assignee: Kashima Oil Company LimitedInventor: Masami Watanabe
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Patent number: 4529499Abstract: A method for producing a 100% mesophase composed only of Q.I. component and Q.S. component is provided. This method comprises forming mesophase by the heat treatment of petroleum-origin pitch, subjecting the heat-formed pitch to a condition of heating under quiescent state to cause only the mesophase in the heat-formed pitch to grow and coalesce, separating only the non-mesophase of the upper layer and repeating the operation of the heat treatment and maintenance of heating under a quiescent state by the separated non-mesophase, as a raw material.Type: GrantFiled: June 24, 1983Date of Patent: July 16, 1985Assignee: Kashima Oil Company LimitedInventor: Masami Watanabe
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Patent number: 4528087Abstract: Mesophase pitch containing quinoline soluble mesophase is produced from a pitch having a specific aromatic hydrogen content with a short heat treatment time without conducting any special treatment such as extraction.Type: GrantFiled: March 8, 1983Date of Patent: July 9, 1985Assignee: Mitsubishi Petrochemical Co., Ltd.Inventors: Haruo Shibatani, Kunimasa Takahashi, Takashi Kameda
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Patent number: 4522701Abstract: A process is described for preparing a highly anisotropic aromatic pitch characterized by a high content of toluene insolubles, a low melting point, a low viscosity, and low content of quinoline insolubles by heat soaking a petroleum pitch derived from catalytic cracking residue at high temperatures for a short time followed by stripping the distillable oils. The pitch made in accordance with this process will yield a highly anisotropic carbon on carbonization at elevated temperatures.Type: GrantFiled: February 11, 1982Date of Patent: June 11, 1985Assignee: E. I. Du Pont de Nemours and CompanyInventor: Ghazi B. Dickakian
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Patent number: 4518482Abstract: A pitch suitable for carbon fiber manufacture features a pitch having a weight content of between 80 and 100 percent toluene insolubles. The pitch is derived from a deasphaltenated fraction of a feedstock. The pitch is characterized as being relatively free of impurities and ash. The pitch can be spun directly into carbon fibers.Type: GrantFiled: July 19, 1982Date of Patent: May 21, 1985Assignee: E. I. Du Pont de Nemours and CompanyInventor: Ghazi Dickakian
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Patent number: 4518483Abstract: A pitch suitable for carbon artifact manufacture, such as the manufacture of carbon fibers, is obtained by heat-soaking an asphaltene fraction of a heavy aromatic feedstock at a temperature of about 380.degree.-440.degree. C. for about 1-500 minutes.Type: GrantFiled: June 27, 1983Date of Patent: May 21, 1985Assignee: E. I. Du Pont de Nemours and CompanyInventor: Ghazi Dickakian
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Patent number: 4517072Abstract: The present invention relates to a process for decreasing and modifying the quinoline-insoluble content (Q.I.) of coal-tar materials; and comprises extracting the coal-tar material with a solvent, where the solvent contains at least one of n-methyl-2-pyrrolidone and the wash oil fraction of coal-tar distillate. Pitches with a diminished Q.I. content, lower viscosity and lower average Q.I. particle size, may be prepared from coal-tar materials which have been so treated.Type: GrantFiled: November 16, 1983Date of Patent: May 14, 1985Assignee: Domtar Inc.Inventors: Samuel Cukier, Henry A. F. L. Kremer
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Patent number: 4512874Abstract: A method for producing continuously 100% mesophase composed only of Q.I. component and Q.S. component in which a raw material of petroleum origin pitch is subjected continuously to a heat-treatment step in an amount necessary to produce a 100% mesophase taken out from a mesophase-growing and coalescing step, transferring the heat-formed pitch formed in the heat treatment step to a mesophase growing and coalescing step, taking out a definite amount of a non-mesophase pitch from the mesophase growing and coalescing step after stirring and heating treatment to return it to the heat-treatment step to repeat the stirring and heating treatment, and at the same time to take out 100% mesophase having constant properties from the mesophase growing and coalescing step.Type: GrantFiled: June 24, 1983Date of Patent: April 23, 1985Assignee: Kashima Oil Company LimitedInventor: Masami Watanabe
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Patent number: 4511625Abstract: A process of spinning a pitch having less than 40% by weight mesophase into a pitch fiber having at least 70% by weight mesophase is described.Type: GrantFiled: September 30, 1982Date of Patent: April 16, 1985Assignee: Union Carbide CorporationInventors: Faramarz Nazem, Rostislav Didchenko, David Fink
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Patent number: 4504455Abstract: A novel reformed mesophase pitch having a mesophase content MC of between 40 and 100%, a quinoline-insoluble content QI of between 5 and 70 weight % and anisotropic domains forming a continuous phase. The reformed mesophase pitch is obtained by heat-treating a dormant mesophase pitch which comprises dormant anisotropic components which are partially hydrogenated, polycyclic polycondensed ring aromatic hydrocarbons derived from the mesophase of a mesophase pitch by hydrogenation of the mesophase and which are soluble in quinoline. The dormant mesophase pitch is optically isotropic in nature but, upon being subjected to shear forces in one direction, capable of being oriented in said direction. Preferably, the reformed mesophase pitch has a softening point SP in .degree.C. satisfying the following conditions:when 40 .ltoreq.MC<100, ##EQU1## and when MC=100, ##EQU2## The reformed mesophase pitch is useful as precursor materials for carbon fibers.Type: GrantFiled: February 7, 1984Date of Patent: March 12, 1985Assignee: Fuji Standard Research Inc.Inventors: Sugio Otani, Shimpei Gomi, Fumio Mogi
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Patent number: 4502943Abstract: A spinnable precursor from petroleum pitch is obtained by subjecting a distillable oil removed carbonaceous residue of petroleum origin to solvent extraction and thereafter heat treating the extracted solvent insoluble fraction under reduced pressure.Type: GrantFiled: March 28, 1983Date of Patent: March 5, 1985Assignee: E. I. Du Pont de Nemours and CompanyInventor: Ghazi Dickakian
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Patent number: 4503026Abstract: A spinnable precursor from petroleum pitch is obtained by isolating a particular fraction of a molten carbonaceous pitch, which has had at least a portion of the polycondensed aromatic oils normally present in the pitch removed. The deoiled pitch is then subjected to a two-stage extraction in an organic solvent in which it has a reversed solubility curve, followed by thermal treatment. The thus obtained precursor can be directly spun into fiber.Type: GrantFiled: March 14, 1983Date of Patent: March 5, 1985Assignee: E. I. Du Pont de Nemours and CompanyInventor: Ghazi Dickakian
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Patent number: 4497789Abstract: Disclosed herein is an improved pitch for making readily stabilizable, substantially nonmesophasic carbon fibers. The pitch has a softening point of about 250.degree. C. (480.degree. F.) or above and is produced from an unoxidized thermal petroleum pitch by selectively reducing or eliminating a portion of the low molecular weight materials in a very short period of time so that the tendency to produce mesophase pitch is eliminated or reduced and so that the chemical integrity of the components of the higher molecular weight fractions is preserved as much as possible. Also disclosed is a method of producing carbon fibers therefrom and rovings or mats from such fibers.Type: GrantFiled: December 3, 1982Date of Patent: February 5, 1985Assignee: Ashland Oil, Inc.Inventors: William R. Sawran, Frank H. Turrill, John W. Newman, Norman W. Hall
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Patent number: 4490239Abstract: A pitch which affords a carbon fiber having a high strength and a high elastic modulus is obtained by treating a pitch containing 5 to 35 weight percent of an optically anisotropic region with sulfur.Type: GrantFiled: March 22, 1983Date of Patent: December 25, 1984Assignee: Nippon Oil Company, LimitedInventors: Seiichi Uemura, Shunichi Yamamoto, Takao Hirose, Hiroaki Takashima, Osamu Kato
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Patent number: 4488957Abstract: A heavy oil such as an atmospheric pressure residue, a reduced pressure residue of petroleum, etc. is heated to 400.degree. to 500.degree. C. to carry out polycondensation and provide a pitch containing mesophase microspheres. This pitch is once cooled to 200.degree. to 400.degree. C. and a turbulent flow is imparted thereto to cause agglomeration of the mesophase microspheres. The resulting agglomerates are separated to obtain a crystallizable material enriched with quinoline insolubles. Production of the crystallizable material is preferably conducted in a separation tank accommodating the lower part of a heating polycondensation reactor (6) and having a stirring device (12).Type: GrantFiled: May 26, 1982Date of Patent: December 18, 1984Assignee: Koa Oil Company, Ltd.Inventors: Kosaku Noguchi, Honami Tanaka, Yukimasa Kumura, Eiji Kitajima, Toshifumi Ishitobi, Hirokazu Teraoka
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Patent number: 4487685Abstract: A method for producing a mesophase-containing pitch from petroleum pitch or coal tar pitch is disclosed. According to this method volatile distillate fractions, which are harmful to mesophase formation and present originally in the raw material pitch or formed as by-product during heat treatment time are driven off by using a carrier gas at a temperature of 360.degree. to 450.degree. C. in order to shorten the overall heat treatment time and advance the mesophase formation smoothly by the increase of stirring effect.Type: GrantFiled: June 24, 1983Date of Patent: December 11, 1984Assignee: Kashima Oil Company LimitedInventor: Masami Watanabe
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Patent number: 4474617Abstract: A pitch which affords a carbon fiber having a high strength and a high elastic modulus is obtained by treating a pitch containing 5 to 35 wt. % of an optically anisotropic region with an oxidizing gas, followed by hydrogenation treatment if required.Type: GrantFiled: February 9, 1983Date of Patent: October 2, 1984Assignee: Nippon Oil Company, LimitedInventors: Seiichi Uemura, Shunichi Yamamoto, Takao Hirose, Hiroaki Takashima, Osamu Kato
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Patent number: 4472265Abstract: A novel carbonaceous pitch which is optically isotropic in nature and which turns into optically anisotropic when shear forces are applied thereto. The carbonaceous pitch may be obtained by hydrogenating the mesophase of a mesophase pitch to the extent that the mesophase is rendered soluble in quinoline. The carbonaceous pitch is useful as a binder and an impregnator and as a precursor material for a highly oriented, high-strength and high-modulus carbon fiber, needle coke or the like carbonaceous materials.Type: GrantFiled: December 10, 1981Date of Patent: September 18, 1984Assignee: Fuji Standard Research Inc.Inventor: Sugio Otani
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Patent number: 4470960Abstract: A process for the production of carbon fibers which comprises using a specific optically isotropic pitch having a reflectivity of 9.0-11.0% as the material for the carbon fibers.Type: GrantFiled: October 27, 1982Date of Patent: September 11, 1984Assignee: Nippon Oil Co., Ltd.Inventors: Seiichi Uemura, Shunichi Yamamoto, Takao Hirose, Hiroaki Takashima, Osamu Kato
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Patent number: 4469585Abstract: A new oxidation-resistant pitch composition is obtained by treating in the molten state a coal tar or petroleum pitch with at least one pitch-soluble and compatible alkyl-aryl sulfonic acid or some salts thereof in an amount of less than 1% of said pitch, with a pitch suitable for making an electrode treated that way, upon subsequent carbonization in conjunction with petroleum coke, an electrode can be formed, with great resistance to oxidation, and with very little dusting. Due to increased coking value of the pitch, the fuming is decreased both during the art of making electrodes and during the use of same in the actual electrolysis thus providing environmental benefits. Such a pitch may also be used as a refractory material.Type: GrantFiled: May 9, 1983Date of Patent: September 4, 1984Inventors: Samuel Cukier, Henry A. F. L. Kremer
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Patent number: 4469667Abstract: A process for the production of high performance carbon fibers which comprises using as the starting material a specific pitch having the lowest reflectivity in the range of 8.5-9.3% and the highest reflectivity in the range of 11.8-12.5%.Type: GrantFiled: December 21, 1982Date of Patent: September 4, 1984Assignee: Nippon Oil Co., Ltd.Inventors: Seiichi Uemura, Shunichi Yamamoto, Takao Hirose, Hiroaki Takashima, Osamu Kato
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Patent number: 4465585Abstract: A cholesteric mesophase pitch is disclosed along with methods for producing the same.Type: GrantFiled: March 30, 1982Date of Patent: August 14, 1984Assignee: Union Carbide CorporationInventor: Irwin C. Lewis
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Patent number: 4462893Abstract: A process for producing a pitch which can be utilized as a raw material for producing carbon fibers is disclosed. The process involves distilling a petroleum heavy residual oil under reduced pressure to produce a reduced pressure distillation residual oil or a reduced pressure distillate oil. The distillation residual oil is subjected to a solvent deasphaltening treatment to produce a solvent deasphaltened oil. The solvent deasphaltened oil or the reduced pressure distillate oil is subjected to solvent extraction to obtain a solvent extraction component. The solvent extraction component is thermally modified to produce the pitch. The pitch can be utilized in a melt-spinning process in order to produce carbon fibers having desirable characteristics.Type: GrantFiled: September 24, 1982Date of Patent: July 31, 1984Assignee: Mitsubishi Oil Company, Ltd.Inventors: Kunihiko Moriya, Kazuhito Tate, Goro Muroga, Kazuhiro Yanagida
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Patent number: 4460557Abstract: A process for the production of carbon fibers comprising heat treating a starting material, melt spinning the resulting precursor pitch, infusibilizing the pitch fibers and carbonizing or graphitizing the infusibilized pitch fibers, characterized in that the starting pitch is obtained by heat treating coal tar and/or coal liquefaction pitch at a specific temperature and a specific hydrogen pressure or by mixing coal tar and/or coal liquefaction tar with at least one nucleus-hydrogenated hydrocarbon of 2-3 rings in a specific mixing ratio and then heat treating the resulting mixture at a specific temperature and a specific pressure. In one embodiment, this invention relates to the starting pitch and carbon fibers obtained by said process.Type: GrantFiled: November 15, 1982Date of Patent: July 17, 1984Assignee: Nippon Oil Co., Ltd.Inventors: Hiroaki Takashima, Osamu Kato, Seiichi Uemura, Shunichi Yamamoto, Takao Hirose