Chemical Modification Of Asphalt, Tar, Pitch Or Resin Patents (Class 208/44)
  • Patent number: 5405524
    Abstract: The process of the invention comprises:a) heating at least one low molecular weight aromatic hydrocarbon in the presence of a Lewis acid under conditions sufficient to produce a pitch of desired composition and properties;b) recovering a pitch of desired composition and properties.The process of the invention may be used to produce pitch which can be used in roofing and binder applications.
    Type: Grant
    Filed: October 29, 1993
    Date of Patent: April 11, 1995
    Assignee: AlliedSignal Inc.
    Inventors: Raj K. Sharma, Dusan C. Prevorsek
  • Patent number: 5387333
    Abstract: An optically isotropic pitch can be obtained by a two-stage heat-treatment which combines a heat treatment with air-blowing under normal pressure with a heat treatment with air-blowing under a reduced pressure. Such a pitch is suitable for using as a raw material for producing carbon fibers or activated fibers.
    Type: Grant
    Filed: March 25, 1992
    Date of Patent: February 7, 1995
    Assignee: Petoca Ltd.
    Inventor: Toshio Tamaki
  • Patent number: 5372702
    Abstract: The improved composition for use in the production of composite carbon materials comprises a mesophase pitch containing at least 80% of an optical anisotropic phase and having a softening point of no higher than 250.degree. C., and sulfur present in an amount of 6-35 parts by weight per 100 parts by weight of said mesophase pitch. Said composition may be heated together with an aggregate and subsequently shaped to yield a composite carbon material. The improved process for producing a composite carbon material comprises impregnating an aggregate with said composition as it is melted, shaping the mixture in a temperature range of 150.degree.-350.degree. C, and then carbonizing the shaped part.
    Type: Grant
    Filed: April 22, 1992
    Date of Patent: December 13, 1994
    Assignee: Mitsubishi Gas Chemical Company, Inc.
    Inventors: Takashi Kojima, Hitoshi Sakamoto
  • Patent number: 5330569
    Abstract: Disclosed is a method of producing an industrial asphalt from a bituminous material. One preferred embodiment comprises mixing together without air-blowing:a. a feed material comprising a bituminous material having a viscosity of at least 50 centistokes at 350.degree. F. and wherein said feed material forms a single phase when mixed with 5 percent of 85 percent phosphoric acid; andb. from about 0.1 to 20.0 percent by weight of phosphoric acid, said mixing being done at a temperature in the range of 351.degree. to 600.degree. F., whereby the softening point of the feed is substantially increased and the penetration is significantly decreased.
    Type: Grant
    Filed: December 18, 1991
    Date of Patent: July 19, 1994
    Assignee: Chevron Research and Technology Company
    Inventors: Edgar L. McGinnis, Judson E. Goodrich
  • Patent number: 5320739
    Abstract: This invention relates to a method of producing a softer asphalt product with improved low temperature properties and reduced solids buildup from an asphalt feed which comprises measuring the penetration and Penetration Index of the asphalt feed and heat soaking the asphalt feed in the presence of at least one C.sub.1 to C.sub.5 halogenated aliphatic hydrocarbon as dehydrogenation agent wherein from about 0.05 to about 10 wt. % of the dehydrogenation agent, based on weight of the asphalt, is present during heat soaking, at a temperature ranging between about 300.degree. C. and about 400.degree. C., said temperature being sufficient to increase the penetration and Penetration Index over that of the asphalt feed provided that the temperature should not exceed the temperature at which onset of coking occurs and further provided that the asphalt product has a trichloroethylene solubles content of at least about 99.5 wt. %, based on asphalt.
    Type: Grant
    Filed: May 6, 1993
    Date of Patent: June 14, 1994
    Assignee: Exxon Research and Engineering Company
    Inventors: Lyle E. Moran, William J. Murphy
  • Patent number: 5316654
    Abstract: There are provided improved processes for the manufacture of enriched pitches, carbon fiber precursors, carbon fibers, and graphite fibers. The improvement comprises employing an elevated wiped-film evaporator in a wiped-film evaporator system comprising the wiped-film evaporator and a means for recovering enriched pitch, such as a positive displacement pump, to form an enriched pitch from catalytic pitch and regulating the operating conditions of the wiped-film evaporator system to provide the desired enriched pitch. The wiped-film evaporator is located a specific distance above the means for recovering enriched pitch. The vertical distance between the outlet of the wiped-film evaporator and the inlet of the means for recovering enriched pitch is within the range of about 10 feet to about 40 feet, preferably about 20 feet to about 40 feet.
    Type: Grant
    Filed: September 13, 1985
    Date of Patent: May 31, 1994
    Inventors: Donald C. Berkebile, deceased, Catherine Berkebile, Administratrix, Donald M. Lee, Larry D. Veneziano, Joseph J. Lauer, Roy E. Booth, William P. Hettinger, Willard Jones
  • Patent number: 5306415
    Abstract: A method is provided which includes infusing oxygen into pitch material without stabilizing the oxygen-infused pitch material. In addition, the invention includes further processing steps (including heat stabilization in either an inert atmosphere or an oxygen-containing atmosphere, deformation, pyrolysis, and/or composite formation) performed after or in conjunction with the oxygenation process. Moreover, the invention includes the composition of matter (in any of a number of different physical forms such as powder, fiber, shaped article, composites) resulting from the practice of this oxygenation process, either alone or in conjunction with the further processing steps. The composition has a homogeneous distribution of oxygen and can be heat stabilized in an inert atmosphere.
    Type: Grant
    Filed: April 16, 1993
    Date of Patent: April 26, 1994
    Assignee: Clemson University
    Inventors: Ludovic P. Cornec, Charles C. Fain
  • Patent number: 5266184
    Abstract: Described is a preferred process for obtaining an increased pitch yield from the distillation of crude coal tar material. The process includes treating a crude coal tar material by reaction with formaldehyde, followed by distillation of the coal tar to afford a yield of coal tar pitch which is significantly increased over that obtained without the formaldehyde treatment.
    Type: Grant
    Filed: February 7, 1992
    Date of Patent: November 30, 1993
    Assignee: Reilly Industries, Inc.
    Inventor: William R. Roder
  • Patent number: 5262043
    Abstract: An isotropic coal tar pitch having a low content of carcinogenic compounds is prepared by distilling a coal tar pitch in an evaporator having a specific evaporator surface of from 330 to 10,000 m.sup.2 /m.sup.3, at a temperature in the range of from 300.degree. to 380.degree. C., under a pressure not exceeding 1 mbar, whereby the average stay period is from 2 to 10 minutes. The isotropic pitch thus obtained contains less that 50 ppm of benzo[a]pyrene and is suitable, optionally after adding an oil, resin or other modifying agents having a low benzo[a]pyrene content, for use as binding and impregnating agent and also as protecting agent in construction materials or as varnish (painting agent).
    Type: Grant
    Filed: April 17, 1992
    Date of Patent: November 16, 1993
    Assignee: Rutgerswerke AG
    Inventors: Winfried Boenigk, Hans-Dieter Behrens, Hans Spengler
  • Patent number: 5259947
    Abstract: This invention relates to low melting solvated mesophase pitches which are suitable for spinning into carbon fibers. The solvated mesophase pitches have a lower melting point than conventional mesophase pitch but remain substantially anisotropic. The solvated mesophase can be produced as an intermediate during solvent fractionation or supercritical solvent fractionation of mesogen-containing isotropic pitches. The process is enhanced through the ability to recover pseudomesogens with an increased average molecular weight which, in combination with the solvent content, provides a fusible mesophase capable of being spun directly into infusible oriented anisotropic carbon fibers.
    Type: Grant
    Filed: September 19, 1991
    Date of Patent: November 9, 1993
    Assignee: Conoco Inc.
    Inventors: Walter M. Kalback, H. Ernest Romine, Xavier M. Bourrat
  • Patent number: 5248407
    Abstract: Paving binders, especially hot mix paving mixtures, having excellent storage stability, reduced binder runoff, and high temperature viscosity are formed by adding a copolymer of ethylene with an alkyl acrylate or vinyl acetate and a neutralized sulfonated polymer to the asphalt. Preferably, the alkyl acrylate is methyl acrylate and the neutralized sulfonated polymer is a terpolymer of ethylene, propylene, and a diene monomer.
    Type: Grant
    Filed: July 16, 1992
    Date of Patent: September 28, 1993
    Assignee: Exxon Research and Engineering Company
    Inventors: Jacques G. Bardet, Martin L. Gorbaty, Nicholas C. Nahas
  • Patent number: 5238672
    Abstract: Producing carbon fiber precursors and carbonized fibers comprise by treating a thin film of catalytic pitch at elevated temperature conditions, treating the resulting heavy isotropic pitch by agitating with an inert gas under elevated temperature conditions to form a mesophase pitch, forming green fibers from said mesophase pitch, stabilizing and optionally carbonizing said green fibers to obtain the desired product.
    Type: Grant
    Filed: June 20, 1989
    Date of Patent: August 24, 1993
    Assignee: Ashland Oil, Inc.
    Inventors: Michael B. Sumner, William P. Hettinger
  • Patent number: 5228977
    Abstract: This invention relates to a method for producing asphalt that has improved low temperature properties. More specifically, the penetration and Penetration Index of an asphalt can be increased if the asphalt is heat soaked in the presence of a dehydrogenation agent at a temperature above the temperature at which oxidation of the asphalt occurs and below the temperature at which coking is initiated. Polyvinyl chloride and a chlorinated wax are preferred dehydrogenation agents.
    Type: Grant
    Filed: November 18, 1991
    Date of Patent: July 20, 1993
    Assignee: Exxon Research & Engineering Company
    Inventors: Lyle E. Moran, William J. Murphy
  • Patent number: 5225070
    Abstract: A method is provided which includes infusing oxygen into pitch material without stabilizing the oxygen-infused pitch material. In addition, the invention includes further processing steps (including heat stabilization in either an inert atmosphere or an oxygen-containing atmosphere, deformation, pyrolysis, and/or composite formation) performed after or in conjunction with the oxygenation process. Moreover, the invention includes the composition of matter (in any of a number of different physical forms such as powder, fiber, shaped article, composites) resulting from the practice of this oxygenation process, either alone or in conjunction with the further processing steps. The composition has a homogeneous distribution of oxygen and can be heat stabilized in an inert atmosphere.
    Type: Grant
    Filed: July 29, 1991
    Date of Patent: July 6, 1993
    Assignee: Clemson University
    Inventors: Ludovic P. Cornec, Charles C. Fain
  • Patent number: 5213677
    Abstract: Spinning pitch for carbon fibers, which (1) has a glass transition temperature width of at most 60.degree. C. as measured by a differential scanning calorimeter, (2) contains at least 80% by volume an optically anisotropic phase, and (3) shows a shear viscosity of 200 poise at a temperature of from 270.degree. to 370.degree. C.
    Type: Grant
    Filed: October 22, 1991
    Date of Patent: May 25, 1993
    Assignee: Mitsubishi Kasei Corporation
    Inventors: Iwao Yamamoto, Ryuichi Hara, Toshiyuki Tajiri, Kazuo Shirosaki, Akihiko Yoshiya
  • Patent number: 5214224
    Abstract: Dispersing asphaltenes in liquid hydrocarbons, particularly formed during the refining of crude petroleum, is disclosed. The dispersant comprises a free radically polymerized copolymer of an .alpha.-olefin of from about 10 to about 36 carbon atoms and maleic anhydride wherein the anhydride moieties along the copolymer backbone are substantially unhydrolyzed or otherwise not derivatized. The copolymer has a ratio of .alpha.-olefin to maleic anhydride of from about 1:1 to about 1:5 and a molecular weight of from 5000 to about 100,000. Alternatively the dispersant comprises a mixture of the .alpha.-olefin/maleic anhydride copolymer and an alkyl substituted phenol/formaldehyde liquid polymer, such as nonyl phenol/formaldehyde polymer, or a lipophilic/hydrophilic vinylic polymer, such as hydroxyethyl methacrylate/lauryl acrylate copolymer. Also disclosed is a liquid hydrocarbon dispersion containing asphaltenes and 1-100 ppm of the .alpha.-olefin/maleic anhydride copolymer.
    Type: Grant
    Filed: July 9, 1992
    Date of Patent: May 25, 1993
    Inventors: David G. Comer, W. Kirk Stephenson
  • Patent number: 5207891
    Abstract: A composition of matter useful as an asphaltene dispersant, comprising a mixture of:(a) poly[P,P'-(propylene oxide-400)phosphite) poly[di(propylene oxide--400)diol)]]-P,P diasphalenate;(b) poly[P,P'-(propylene oxide-400)phosphite -poly[di(propylene oxide--1000) diol)]]-P,P'-diasphalenate;(c) Poly[P,P'-(propylene oxide-400)phosphite) -poly(propylene oxide-400-poly(propylene oxide-1000)diol)]]-P-P'-diasphalenate(d) Poly[P,P'-(propylene oxide-1000)phosphite -poly[di(propylene oxide-400) diol)]]-P,P'-diasphalenate;(e) poly[P,P'-(propylene oxide-1000)phosphite) poly[di(propylene oxide-1000)diol)]]-P,P'-diasphalenate;(f) poly[P,P'(propylene oxide-1000)phosphite) poly[di([propylene oxide-400-poly (propylene oxide-1000)diol)]]-P,P'-diasphaltenate;(g) cyclo[P,P'-di(polypropylene oxide -400)phosphite]-P,P'-diasphaltenate;(h) cyclo[P,P'-di-(polypropylene oxide-1000) phosphite]-P,P'-diasphaltenate;(i) cyclo[P,P'-(polypropyleneoxide-400) -(polypropyleneoxide-1000)-phosphite]-P,P'diasphaltenate;(j) poly[(dipropyleneoxide-4
    Type: Grant
    Filed: December 30, 1991
    Date of Patent: May 4, 1993
    Assignee: Texaco Inc.
    Inventors: Rodney L. Sung, Thomas F. DeRosa, David A. Storm, Benjamin J. Kaufman
  • Patent number: 5198101
    Abstract: An improved process for producing an anisotropic pitch product suitable for carbon fiber manufacture. A metal alkylaryl sulfonate is combined with a carbonaceous feedstock substantially free of mesophase pitch, and the combination is heated for a period of time at an elevated temperature while passing a non-oxidative sparging gas such as nitrogen through the feedstock. The process is carried out for a sufficient period of time to produce an anisotropic pitch having from 50 to 100 percent by volume mesophase which is suitable for producing good quality carbon fibers.In one aspect of the invention, an oxidatively reactive gas is used as the sparging gas.
    Type: Grant
    Filed: December 13, 1991
    Date of Patent: March 30, 1993
    Assignee: Conoco Inc.
    Inventor: Walter M. Kalback
  • Patent number: 5182011
    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.
    Type: Grant
    Filed: November 21, 1990
    Date of Patent: January 26, 1993
    Assignee: Maruzen Petrochemical Co., Ltd.
    Inventors: Masatoshi Tsuchitani, Makoto Tamura, Kiyotaka Suzuki, Shuji Okada, Ryoichi Nakajima, Sakae Naito
  • Patent number: 5182010
    Abstract: Pitch that is obtained from naphthalene derivatives having at least one methyl group and the content of an optically anisotropic phase in which is substantially 100% is disclosed. This mesophase pitch has a H/C atomic ratio of about 0.5-1.0 and an aromatic carbon ratio (fa) of at least about 0.7, contains methylic carbon in an amount of at least about 4% of the total carbon atoms, and has a softening point of 200.degree.-250.degree. C. The pitch contains about 12-20 mole % of molecules having an average molecular weight of less than about 600, about 55-70 mole % of molecules having an average molecular weight of from about 600-1,500 and about 20-30 mole % of molecules having an average molecular weight of higher than about 1,500. Fibers melt spun from this mesophase pitch can be converted to carbon or graphite fibers having high strength and modulus of elasticity by a heat treatment which consists of heating to a temperature of 200.degree.-350.degree. C. in an air atmosphere, then heating to about 1,000.
    Type: Grant
    Filed: July 26, 1991
    Date of Patent: January 26, 1993
    Assignee: Mitsubishi Gas Chemical Company, Inc.
    Inventors: Isao Mochida, Yukio Sakai, Hiroyuki Ohtsuka
  • Patent number: 5173172
    Abstract: Hard asphalts exhibiting acceptable penetration and low temperature properties can be produced from vacuum residua from which such hard asphalts are not normally obtainable via typical vacuum distillate such as that derived from Arab Light crude and/or feeds substantially comprising Arab Light-type crudes by ultrafiltering the residua through a membrane.
    Type: Grant
    Filed: August 19, 1991
    Date of Patent: December 22, 1992
    Assignee: Exxon Research and Engineering Company
    Inventors: Brian B. Adams, John A. Thompson
  • Patent number: 5133781
    Abstract: A method of compatibilization asphaltenes containing bituminous liquids which process comprises:a) reacting an asphaltene with phosphorous trichloride in the presence of a liquid to form a phosphochlorinated asphaltene containing from about 0.01 wt % to about 20 wt. % phosphorous;b) reacting the phosphochlorinated asphaltene with an equimolar amount of aliphatic or aromatic alcohols and phenols selected from the group consisting of:i) an aliphatic alcohol;ii) a naphthyl alcohol;iii) an alkyl quinizarin;iv) an oligomeric mixed polyether aliphatic terminal diol; andv) an oligomeric polyalkene terminal diol to produce a compatibilized asphaltene; andc) recovering the compatibilized asphaltene product.
    Type: Grant
    Filed: December 21, 1990
    Date of Patent: July 28, 1992
    Assignee: Texaco Inc.
    Inventors: Thomas F. DeRosa, Rodney L. Sung, Benjamin J. Kaufman, Eugene M. Jao
  • Patent number: 5132005
    Abstract: A method of compatibilization asphaltenes containing bituminous liquids which process comprises:a) reacting an asphaltene with phosphorous trichloride to form a phosphochlorinated asphaltene containing from about 0.01 wt % to about 20 wt % phosphorous;b) reacting the phosphochlorinated asphaltene with an equimolar amount of aliphatic or aromatic amines and polyamines selected from the group consisting of:(i) a piperzine;(ii) an aliphatic amine;(iii) an alkyl piperdize;(iv) an aligomeric mixed polyether aliphatic terminal diamine;(v) an oligomeric polyether aliphatic terminal amine;(vi) an oligermic polyether aliphatic terminal triamine;(vii) a substituted aromatic polyether terminal amine; and(viii) an oligomeric or polymeric amine to produce a capatibilized asphaltene; and(c) recovering the asphaltene product.
    Type: Grant
    Filed: December 21, 1990
    Date of Patent: July 21, 1992
    Assignee: Texaco Inc.
    Inventors: Thomas F. Derosa, Rodney L. Sung, Benjamin J. Kaufman, Eugene M. Jao
  • Patent number: 5128021
    Abstract: A novel pitch material made from coal tar pitch has:a) mesophase content of .ltoreq.2%,b) content of toluene-insolubles (.beta.-resin) between 58 and 75%,c) content of quinoline-insolubles of <2%,d) softening point in the 200.degree. to 300.degree. C. range, according to the Kramer-Sarnow (KS) measurement,e) content of volatile matter .ltoreq.20% andf) ash content of .ltoreq.0.06%.The pitch material of high coke yield (80 to beyond 90%) is suitable for the manufacture of molded carbonaceous shapes of high quality and of pitch coke. A further application would be as impregnation agent or bind. The method of making new pitch uses hot filtration in the presence of a filtration and followed by thin-film evaporation.
    Type: Grant
    Filed: August 3, 1989
    Date of Patent: July 7, 1992
    Assignees: Bergwerksverband GmbH, Didier Engineering GmbH
    Inventors: Ingo Romey, Rudolf Geier, Rolf H. Joest, Wilhelm Wullscheidt
  • Patent number: 5120424
    Abstract: The disclosed bonding pitch for electrodes, having a softening point C.I.A. comprised between 80.degree. C. and 150.degree. C., a concentration of quinoline-insoluble substances higher or equal to 4% by weight, a concentration of .alpha.+.beta. resins comprised between 28 and 40% by weight, and a fixed carbon content determined according to the standard ISO 6998, at least equal to 51% by weight, is characterized by a vitreous transition domain .DELTA.Tg, determined by differential calorimetric analysis, at the most equal to 50.degree. C. In order to produce such a pitch, a pitch having a content of quinoline-insoluble substances lower than 4% by weight is subjected to a treatment by waves having a frequency between 0.9 and 300 GHz. Such treatment makes possible the increase of the carbon content of the pitch while preserving a good affinity to the coke and significantly decreasing its vitreous transitional domain.
    Type: Grant
    Filed: January 16, 1991
    Date of Patent: June 9, 1992
    Assignee: Norsolor
    Inventors: Denis Cottinet, Serge Buche, Pierre Couderc, Jean L. Saint Romain
  • Patent number: 5104518
    Abstract: Carbonates, oxides, carbides or fluorides of alkaline earth metals are added to coal tar pitches before coking. After the coking, which is preferably carried out by the delayed coking process, this produces coal tar pitch cokes or coal tar pitch needle cokes which have no irreversible expansion or a strongly reduced irreversible expansion upon heating in the temperature range of 1400.degree. to 2000.degree. C.
    Type: Grant
    Filed: March 6, 1990
    Date of Patent: April 14, 1992
    Assignee: Sigri GmbH
    Inventor: Hubert Jager
  • Patent number: 5098480
    Abstract: Disclosed is a method of producing an industrial asphalt from a bituminous material. One preferred embodiment comprises mixing together without air-blowing:a. a feed material comprising a bituminous material having a viscosity of at least 50 centistokes at 350.degree. F. and wherein said feed material forms a single phase when mixed with 5 percent of 85 percent phosphoric acid; andb. from about 0.1 to 20.0 percent by weight of phosphoric acid, said mixing being done at a temperature in the range of 351.degree. to 600.degree. F., whereby the softening point of the feed is substantially increased and the penetration is significantly decreased.A second preferred embodiment comprises heating at an elevated temperature a mixture comprising:1. from about 0.1 to 20.0 percent by weight green phosphoric acid, and2. a bituminous material to make up 100 percent by weight, said bituminous material comprising asphalt.
    Type: Grant
    Filed: May 23, 1990
    Date of Patent: March 24, 1992
    Assignee: Chevron Research and Technology Company
    Inventors: Edgar L. McGinnis, Judson E. Goodrich
  • Patent number: 5059300
    Abstract: Disclosed is a method for modifying the physical properties of a bituminous material which comprises heating at an elevated temperature a mixture comprising:(a) 0.1 to 20.0 percent by weight phosphoric acid;(b) 1 to 15 percent by weight solvent deasphalted bottoms; and(c) a bituminous material to make up 100 percent by weight, said bituminous material comprising vacuum distilled asphalt.
    Type: Grant
    Filed: September 19, 1988
    Date of Patent: October 22, 1991
    Assignee: Chevron Research and Technology Company
    Inventor: Edgar L. McGinnis
  • Patent number: 5057297
    Abstract: A method for producing graphite structures which are of light weight and excel in elasticity from a carbonaceous material comprises in succession the steps of: (a) treating said carbonaceous material with nitric acid or a nitric-sulfuric acid mixture, (b) bringing the acid-treating carbonaceous material into contact with a basic aqueous solution to make it soluble, (c) adding an acidic aqueous solution to the obtained soluble matter to regulate the pH of said soluble matter to 3 or less, thereby precipitating a carbonaceous component therefrom, and (d) graphitizing the thus precipitated carbonaceous component at 2,400.degree. C. or higher temperature.
    Type: Grant
    Filed: October 27, 1989
    Date of Patent: October 15, 1991
    Assignee: Koa Oil Company, Limited
    Inventors: Masaki Fujii, Masanori Minohata
  • Patent number: 5032250
    Abstract: Isotropic pitch containing mesogens is combined with a solvent and subjected to dense phase or supercritical conditions and the mesogens are phase separated. In one aspect the isotropic pitch containing mesogens is fluxed with a solvent to solubilize the mesogens, the flux mixture is filtered to remove nonsolubles and the mesogens are phase separated by use of the same solvent under dense phase or supercritical conditions of temperature and pressure. The phase separation conditions are such that the mesogens are recovered as mesophase.
    Type: Grant
    Filed: December 22, 1988
    Date of Patent: July 16, 1991
    Assignee: Conoco Inc.
    Inventors: Hugh E. Romine, James R. McConaghy, Jr.
  • Patent number: 4999099
    Abstract: An improved process for producing an anisotropic pitch product suitable for carbon fiber manufacture. A carbonaceous feedstock is heated at elevated temperature while passing a reactive sparging gas through the feedstock. The sparging gas is an oxidative gas such as a gaseous mixture containing a major proportion of inert gas and from about 0.1 to 2% by volume of oxygen. The process produces an anisotropic pitch having from 50 to 100% by volume mesophase which is suitable for producing good quality carbon fibers.
    Type: Grant
    Filed: January 30, 1986
    Date of Patent: March 12, 1991
    Assignee: Conoco Inc.
    Inventors: Ta-Wei Fu, Manfred Katz
  • Patent number: 4997542
    Abstract: An impregnation pitch having a Kraemer-Sarnow softening point ranging from about 60.degree. C. to 80.degree. C., a content of quinoline-insoluble substances less than or equal to 7% by weight, and a filterability index greater than or equal to 4.5. A process for the manufacture thereof, wherein a tar or a pitch having a Kraemer-Sarnow softening point not exceeding 60.degree. C. and a content of quinoline-insoluble substances below or equal to 7% by weight is subjected to a thermal treatment capable of removing constituents with a molecular mass of below 1,200.
    Type: Grant
    Filed: March 18, 1988
    Date of Patent: March 5, 1991
    Assignee: Norsolor
    Inventors: Pierre Couderc, Serge Buche, Jean-Louis Saint Romain
  • Patent number: 4996037
    Abstract: There are provided improved processes for the manufacture of enriched pitches, carbon fiber precursors, carbon fibers, and graphite fibers. The improvement comprises employing an elevated wiped-film evaporator in a wiped-film evaporator system comprising the wiped-film evaporator and a means for recovering enriched pitch, such as a positive displacement pump, to form an enriched pitch from catalytic pitch and regulating the operating conditions of the wiped-film evaporator system to provide the desired enriched pitch. The wiped-film evaporator is located a specific distance above the means for recovering enriched pitch. The vertical distance between the outlet of the wiped-film evaporator and the inlet of the means for recovering enriched pitch is within the range of about 10 feet to about 40 feet, preferably about 20 feet to about 40 feet.
    Type: Grant
    Filed: March 12, 1986
    Date of Patent: February 26, 1991
    Inventors: Donald C. Berkebile, Donald M. Lee, Larry D. Veneziano, Joseph J. Lauer, Roy E. Booth, William P. Hettinger
  • Patent number: 4986895
    Abstract: Pitch substantially free from primary and secondary QI components and solids comprising secondary QI components are prepared by centrifuging coal tar or coal tar pitch at a high temperature, heat-treating the separated supernatant liquid and centrifuging again the liquid at a high temperature.
    Type: Grant
    Filed: September 5, 1989
    Date of Patent: January 22, 1991
    Assignee: Osaka Gas Company Limited
    Inventors: Makihiko Mori, Katsumi Fujita, Yoshiteru Nakagawa, Yasunori Goda, Toyohiro Maeda
  • Patent number: 4986893
    Abstract: Disclosed herein is a process for producing a substantially quinoline-soluble and optically anisotropic pitch for carbon materials, which process comprises the steps of (1) polymerizing naphthalene by heating at a temperature of not higher than 330.degree. C. for 0.5 to 100 hours in the presence of Lewis acid catalyst, (2) removing said catalyst from the reaction mixture, (3) subjecting said reaction mixture to thermal treatment at a temperature of 390.degree. to 450.degree. C. for 1 to 5 hours under a pressure of not less than an atmospheric pressure so as to produce neither a quinoline-insoluble pitch nor optically anisotropic pitch, thereby carrying out aromatization of the polymerizate of naphthalene, and (4) heating the thus treated material at a temperature of 350.degree. to 380.degree. C. for 3 to 10 hours under a reduced pressure while flowing an inert gas, thereby removing the volatile components for said material, and the pitch produced by the process.
    Type: Grant
    Filed: January 4, 1990
    Date of Patent: January 22, 1991
    Assignee: Kureha Kagaku Kogyo Kabushiki Kaisha
    Inventors: Ikuo Seo, Saburou Takahashi, Tooru Ohono
  • Patent number: 4976845
    Abstract: A process for increasing the content of mesophase in a pitch includes using a high molecular aromatic fraction based on a material selected from the group consisting of coal tar, crude oil and their mixture in molten form, thermally treating the fraction in form of a thin, continously moving film, and removing volatile components by degassing during the thermal treatment. The process distinguishes in using a high molecular aromatic fraction which may contain mesophase, shaping the fraction continuously mechanically to a thin film with a layer of thickness of between substantially 0.
    Type: Grant
    Filed: September 1, 1989
    Date of Patent: December 11, 1990
    Inventors: Peter Oerlemans, Rolf Marrett, Armin Eckert, Klaus Altfeld
  • Patent number: 4959139
    Abstract: Binder pitch is prepared by combining a petroleum aromatic mineral oil thermal tar and super finely subdivided calcined premium coke particles. The petroleum aromatic mineral oil thermal tar is obtained by hydrotreating, thermally cracking and vacuum distilling an aromatic mineral oil. Additionally, the aromatic mineral oil thermal tar may be subjected to heat soaking.
    Type: Grant
    Filed: January 9, 1989
    Date of Patent: September 25, 1990
    Assignee: Conoco Inc.
    Inventors: Dave L. Blakeburn, II, Ta-Wei Fu, Keith M. Roussel
  • Patent number: 4943365
    Abstract: Contrary to known alkylation of pitches, it is disclosed that pitches are modified with particular aromatically substituted and activated C.sub.1 to C.sub.4 alkyl groups. The resulting modified pitches are easily polycondensed and give high coking residues and good mesophase formation. This is achieved on the one hand by dispensing with catalysts, which can be only incompletely removed from the pitch and, on the other hand, by employing reactive short chain alkyl aromatic compounds.
    Type: Grant
    Filed: March 9, 1987
    Date of Patent: July 24, 1990
    Assignee: Rutgerswerke AG
    Inventors: Winfried Boenigk, Maximilian Zander, Jurgen Stadelhofer
  • Patent number: 4931163
    Abstract: A carbon fluoride comprising carbon atoms and fluorine atoms and having a structure in which layers containing fluorinated condensed cyclohexane rings are stacked to form a packing structure, the atomic ratio of fluorine to carbon atoms being 0.5 to 1.8, the carbon fluoride exhibiting a powder X-ray diffraction pattern in which there are peaks respectively at about 13.degree. (2.theta.) and at about 40.degree. (2.theta.) and no peak on the low side of diffraction angle relative to 13.degree. (2.theta.) and exhibiting a spectrum of electron spectroscopy for chemical analysis in which there are peaks respectively due to a monofluorocarbon group and due to a difluorocarbon group, the intensity ratio of the peak due to the difluorocarbon group to the peak due to the monofluorocarbon group being 0.15 to 1.5. The carbon fluoride has a unique property that it is capable of forming a film by vacuum deposition. The carbon fluoride may be produced by the direct fluorination of a pitch or meso-carbon microbeads.
    Type: Grant
    Filed: May 25, 1988
    Date of Patent: June 5, 1990
    Assignee: Osaka Gas Co, Ltd.
    Inventors: Nobuatsu Watanabe, Hidekazu Tohara, Yuji Matsumura, Hiroyuki Fujimoto
  • Patent number: 4929404
    Abstract: A graphitic or carbonaceous molding comprising graphite powder and a mesophase-containing pitch is obtained by suspending graphite powder in a tar, heating the suspension while blowing an inert gas therein to form the mesophase-containing pitch on the graphite particles to obtain carbonaceous precursors and molding/carbonizing or graphitizing the carbonaceous precursors.
    Type: Grant
    Filed: May 17, 1988
    Date of Patent: May 29, 1990
    Assignee: Mitsubishi Petrochemical Company Limited
    Inventors: Kunimasa Takahashi, Takashi Kameda, Haruo Shibatani
  • Patent number: 4925547
    Abstract: 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.
    Type: Grant
    Filed: August 21, 1989
    Date of Patent: May 15, 1990
    Assignee: Maruzen Petrochemical Co., Ltd.
    Inventors: Masatoshi Tsuchitani, Sakae Naito, Hiroshi Morijiri, Kiyotaka Suzuki
  • Patent number: 4921539
    Abstract: The invention concerns a modified pitch composition specially adapted to bind coal particles with the purpose of transforming it into briquettes; the pitch is modified by reaction with an unsaturated dicarboxylic acid or anhydride thereof, and at least on crosslinking agents selected from hydroxide of a Group I metal, and certain polyamines, polyalcohols and alcoholamines.
    Type: Grant
    Filed: October 12, 1988
    Date of Patent: May 1, 1990
    Assignee: Shell Oil Company
    Inventors: Jean-Pierre Harlin, Jean-Pierre Giorgetti, Bernard Ruquier, Robert Herment
  • Patent number: 4909923
    Abstract: A method for the hydrogenation of coal tar pitch which comprises subjecting said coal tar pitch containing toluene insolubles to slight hydrogenation in the presence of a hydrogenation catalyst having carried on a refractory inorganic oxide carrier at least one member selected from the class consisting of elemental metals, belonging to Groups VI B and VIII in the Periodic Table and oxides and sulfides thereof, under the conditions of 280.degree. to 400.degree. C. of reaction temperature, 20 to 200 kg/cm.sup.2. G of hydrogen pressure, 0.1 to 10 hr.sup.-1 of LHSV, and 500 to 2,000 Nl/liter of hydrogen to liquid ratio, and a catalyst therefor. The "slight" hydrogenation is hydrogenation to a degree such that the difference of hydrogen to carbon atomic ratio between the untreated coal tar pitch and the hydrogenated coal tar pitch falls in the range of 0.03 to 0.5.
    Type: Grant
    Filed: January 15, 1987
    Date of Patent: March 20, 1990
    Assignees: Nippon Steel Chemical Co., Ltd., Chiyoda Chemical Engineering & Construction Co., Ltd.
    Inventors: Hiroshi Okazaki, Tadashi Komoto, Munekazu Nakamura, Osamu Togari, Noriyuki Yoneda, Haruhiko Yoshida, Hideki Hashimoto
  • Patent number: 4908064
    Abstract: Asphalt used for road paving containing catalytic cracking catalyst particles which have been burned to remove hydrocarbons deposited thereon during a petroleum catalytic cracking process. The catalyst particles may be present in the asphalt in amounts of from 0.1% to 5.0% by weight of the asphalt, but more preferably from 0.2% to 2.0% by weight of the asphalt. The particles, which are comprised of crystalline and amorphous silica and alumina and silica-alumina combinations, function to prevent oxidative condensation of the asphalt, thus preventing hardening of the asphalt.
    Type: Grant
    Filed: July 27, 1988
    Date of Patent: March 13, 1990
    Assignee: Marathon Oil Company
    Inventor: Mark A. Plummer
  • Patent number: 4908200
    Abstract: A method for producing graphite structures which are of light weight and excel in elasticity from a carbonaceous material comprises in succession the steps of: (a) treating said carbonaceous material with nitric acid or a nitric-sulfuric acid mixture, (b) bringing the acid-treated carbonaceous material into contact with a basic aqueous solution to make it soluble, (c) adding an acidic aqueous solution to the obtained soluble matter to regulate the pH of said soluble matter to 3 or less, thereby precipitating a carbonaceous component therefrom, and (d) graphitizing the thus precipitated carbonaceous component at 2,400.degree. C. or higher temperature.
    Type: Grant
    Filed: July 1, 1988
    Date of Patent: March 13, 1990
    Assignee: Kao Oil Company, Limited
    Inventors: Masaki Fujii, Masanori Minohata
  • Patent number: 4904371
    Abstract: An improved process for producing an anisotropic pitch product suitable for carbon fiber manufacture. A carbonaceous feedstock substantially free of mesophase pitch is heated for a period of time at an elevated temperature while passing an oxidatively reactive sparging gas such as a mixture of oxygen and nitrogen through the feedstock. The oxidatively treated feedstock is then subjected to a heat soak, for a longer period of time in the absence of a sparging gas. Thereafter the heat soaked feedstock is heated at an elevated temperature in the presence of a non-oxidative sparging gas for a time period equal to or less than the heat soak to produce an anisotropic pitch having from 50 to 100% by volume mesophase which is suitable for producing good quality carbon fibers.
    Type: Grant
    Filed: October 13, 1988
    Date of Patent: February 27, 1990
    Assignee: Conoco Inc.
    Inventor: Walter M. Kalback
  • Patent number: 4895600
    Abstract: Asphalt compositions are improved by incorporating therein the reaction produce of (a) a phosphorus-containing compound, (b) an amine or polyamine and (c) a carbonyl-containing compound as an anti-stripping agent. These asphalt compositions are useful as a pavement material by blending with an aggregate.
    Type: Grant
    Filed: July 28, 1988
    Date of Patent: January 23, 1990
    Assignee: The Dow Chemical Company
    Inventors: Dane Chang, Druce K. Crump
  • Patent number: 4892641
    Abstract: An improved process for producing an anisotropic pitch product suitable for carbon fiber manufacture. A carbonaceous feedstock substantially free of mesophase pitch is heated at elevated temperature while passing an oxidatively reactive sparging gas such as air through the feedstock. The oxidatively treated feedstock, which remains substantially free of mesophase pitch, is then heated at a higher temperature in the presence of a non-oxidative sparging gas to produce an anisotropic pitch having from 50 to 100% by volume mesophase which is suitable for producing good quality carbon fibers.
    Type: Grant
    Filed: February 8, 1989
    Date of Patent: January 9, 1990
    Assignee: Conoco Inc.
    Inventors: Ta-Wei Fu, Manfred Katz
  • Patent number: 4892642
    Abstract: An improved process for producing an anisotropic pitch product suitable for carbon fiber manufacture. A carbonaceous feedstock substantially free of mesophase pitch is heated at elevated temperature while passing an oxidatively reactive sparging gas such as air through the feedstock. The oxidatively treated feedstock, which contains isotropic pitch, is solvent fractionated to recover a solid pitch which on fusion becomes an anisotropic pitch product having from 50 to 100 percent by volume mesophase. In one aspect of the invention the carbonaceous feedstock is oxidatively treated in a melt phase at a lower temperature and the resulting isotropic pitch is then heated at a higher temperature in a melt phase in the presence or absence of a non-oxidative sparging gas prior to solvent fractionation.
    Type: Grant
    Filed: January 17, 1989
    Date of Patent: January 9, 1990
    Assignee: Conoco Inc.
    Inventors: Hugh E. Romine, Ta-Wei Fu
  • Patent number: 4891126
    Abstract: Pitch that is obtained from a condensed polycyclic aromatic hydrocarbon and the content of an optically anisotropic phase in which is substantially 100% is disclosed. This mesophase pitch has a H/C atomic ratio of 0.5-1.0, contains naphthenic carbon in an amount of at least 7% of the total carbon, and has a softening point of 180.degree.-400.degree. C. Fibers melt-spun from this mesophase pitch can be converted to carbon or graphite fibers having high strength and modulus of elasticity by a heat treatment which consists of heating to a temperature of 250.degree.-300.degree. C. in an air atmosphere, then heating to 1,000.degree. C. or higher in an inert gas atmosphere. Such mesophase pitch is produced by polymerizing a condensed polycyclic aromatic hydrocarbon for 5-300 minutes at a temperature of 180.degree.-400.degree. C. and at a pressure of 5-100 atmospheres in the presence of 0.1-20 moles of HF and 0.05-1 mole of BF.sub.3 per mole of the condensed polycyclic aromatic hydrocarbon.
    Type: Grant
    Filed: November 22, 1988
    Date of Patent: January 2, 1990
    Assignee: Mitsubishi Gas Chemical Company, Inc.
    Inventors: Isao Mochida, Yukio Sakai, Hiroyuki Otsuka