US3718493A - Process for the production of carbon filaments from coal tar pitch - Google Patents
Process for the production of carbon filaments from coal tar pitch Download PDFInfo
- Publication number
- US3718493A US3718493A US00084896A US3718493DA US3718493A US 3718493 A US3718493 A US 3718493A US 00084896 A US00084896 A US 00084896A US 3718493D A US3718493D A US 3718493DA US 3718493 A US3718493 A US 3718493A
- Authority
- US
- United States
- Prior art keywords
- pitch
- coal tar
- temperature
- filament
- filaments
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 17
- 229910052799 carbon Inorganic materials 0.000 title abstract description 14
- 239000011294 coal tar pitch Substances 0.000 title abstract description 13
- 238000000034 method Methods 0.000 title description 17
- 238000004519 manufacturing process Methods 0.000 title description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000011295 pitch Substances 0.000 description 39
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 230000001590 oxidative effect Effects 0.000 description 10
- 230000003647 oxidation Effects 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 229920000049 Carbon (fiber) Polymers 0.000 description 8
- 239000004917 carbon fiber Substances 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 238000009987 spinning Methods 0.000 description 8
- 239000011280 coal tar Substances 0.000 description 7
- 239000012298 atmosphere Substances 0.000 description 5
- 238000003763 carbonization Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000011282 treatment Methods 0.000 description 5
- 239000000835 fiber Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- RJKGJBPXVHTNJL-UHFFFAOYSA-N 1-nitronaphthalene Chemical compound C1=CC=C2C([N+](=O)[O-])=CC=CC2=C1 RJKGJBPXVHTNJL-UHFFFAOYSA-N 0.000 description 2
- WHRZCXAVMTUTDD-UHFFFAOYSA-N 1h-furo[2,3-d]pyrimidin-2-one Chemical compound N1C(=O)N=C2OC=CC2=C1 WHRZCXAVMTUTDD-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 235000006173 Larrea tridentata Nutrition 0.000 description 2
- 244000073231 Larrea tridentata Species 0.000 description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229960002126 creosote Drugs 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011316 heat-treated pitch Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000000379 polymerizing effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- BFCFYVKQTRLZHA-UHFFFAOYSA-N 1-chloro-2-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1Cl BFCFYVKQTRLZHA-UHFFFAOYSA-N 0.000 description 1
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 description 1
- 238000012935 Averaging Methods 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- VYZAHLCBVHPDDF-UHFFFAOYSA-N Dinitrochlorobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C([N+]([O-])=O)=C1 VYZAHLCBVHPDDF-UHFFFAOYSA-N 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- VLZLOWPYUQHHCG-UHFFFAOYSA-N nitromethylbenzene Chemical compound [O-][N+](=O)CC1=CC=CC=C1 VLZLOWPYUQHHCG-UHFFFAOYSA-N 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011301 petroleum pitch Substances 0.000 description 1
- 239000011312 pitch solution Substances 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
- D01F9/15—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from coal pitch
Definitions
- Satisfactory carbon fibers have also been made from molten decomposition products of synthetic polymeric materials such as polyvinylchloride, polyvinyl acetate, and from fusible carbon-yielding materials like blown asphalt and petroleum pitch.
- the fusible material is spun into fibers, oxidized and carbonized to yield carbon fibers possessing strengths of over 100,000 p.s.i.
- coal tar pitch however, these measures have failed and the art does not provide any successful method for the satisfactory spinning of pitches of coal tar origin and for their subsequent conversion into useful carbon fibers having properties comparable to those possessed by carbon fibers from other raw materials.
- the pitch filament is oxidized in one or more stages in an oxidizing medium and then carbonized at a temperature in the vicinity of 1000 C. in an inert atmosphere. If desired, the resulting carbon filament may be graphitized by heating in an inert atmosphere at elevated temperatures.
- a critical operation in the transformation process of the invention is the removal of the quinoline insolubles from the coal tar pitch selected.
- Quinoline insolubles represent material which is not soluble in the pitch at spinning temperature or, in other words, Which forms an undesirable second phase. This removal is generally done before heat treating and distilling the pitch. This sequence of operations however is not binding, especially when a pitch of low quinoline insoluble content is employed.
- the pitch may be diluted in an appropriate solvent, filtered or centrifuged and recovered.
- the solvents usable for this purpose are generally speaking any aromatic liquid having a boiling point or range between about 200 and 400 C., provided that the major liquifiable portion of the coal tar pitch is soluble in it.
- Said liquid should also be removed from the filtered pitch solution at temperatures preferably not exceeding 300 C., either at atmospheric pressure or under reduced pressure.
- examples of usable liquids which fit these specifications are light creosote oil, anthracene oil, phenanthrene, quinoline, highly aromatic petroleum fractions and the like.
- the dilution of the pitch and the subsequent filtration can be carried out at any temperature within a range g0- ing from the softening point of the pitch to about 300 C. Proportions of solvent to pitch vary with the viscosity of the substance at the temperatures selected. In general, a dilution of 1:1 at a temperature of about 200 C. has been found convenient.
- the diluted pitch is then filtered to remove the undissolved material. This may be accomplished in a number of manners with known equipment, provided of course that the foraminous member of this equipment can withstand the filtration conditions. Fritted glass and porous stainless steel septums having openings of about 10 microns in average diameter are satisfactory.
- the filtration process may be facilitated and improved in a conventional manner by additions of known filter aids to the pitch liquid.
- the number of actual filtrations and their timing may vary according to several factors such as viscosity of the pitch liquid, amount and nature of undissolved solids, temperature, pressure and the like.
- at least one filtration is required for the purpose of this invention and that it may be carried out on a liquid solvent diluted or undiluted pitch at any stage before the actual passage of the pitch through the filament-forming spinneret.
- the solvent is removed by evaporation preferably under reduced pressure at about 150 C., in any event, at a temperature not exceeding 300 C.
- the separation of the undesirable second phase may be accomplished by centrifugation rather than filtration, although the latter technique is preferred in most instances.
- the coal tar pitch to be used for spinning filaments is heat treated and distilled to improve its molecular weight range. Either or both of these treatments may be carried out, as indicated earlier, before, after or between filtrations.
- the pitch is distilled at a temperature within the range of about 280 to 305 C. to remove its lower molecular weight components. This may be accomplished by any conventional method including distillation under reumbled pressure, steam distillation and so on, using any conventional equipment such as a molecular still and the like, provided the temperature limits are respected.
- the pitch is heat soaked at similar temperatures for a period of about 10 to 100 hours or more under pressures which may range from less than one atmosphere to more than one atmosphere.
- the heat treated coal tar pitch prepared in the manner described is then spun into a continuous filament through a nozzle or spinneret with an internal diameter appropriate for the thickness of filament required.
- the pitch is melted at a temperature between its melting point and about 300 C. and the melt is extruded through the spinnerets orifice by sufiicient nitrogen pressure to achieve a satisfactory rate or by other conventional means such as a metering pump, a piston and the like.
- the actual pressure and temperature used depend on the properties of the heat treated pitch used as well as upon each other. In this respect, it has been found that a pitch of the type prescribed by this invention can be spun satisfactorily under a driving N pressure of about 80 p.s.i.
- Extrusion of the filament at high temperature initiates an oxidation process which may be intensified by passing the filament through an oxidizing atmosphere for a length of time sufficient to create the infusibility required by the subsequent carbonization treatment.
- Suitable oxidizing media for this purpose include air; ozone in air; oxygen blended with air, flue gases or inert gases; vapors or mists of nitroaromatic compounds such as nitrobenzene, nitrophenol, alpha-nitronaphthalene, nitrotoluene, nitrochlorobenzene and the like; oxidizing gases such as sulfur dioxide, sulfur trioxide, nitric oxide and the like.
- the filament may be cooled to a temperature below its fusing point and then passed through liquid oxi dizing baths of the above mentioned nitroaromatics or of other oxidizing liquids such as nitric acid, sulfuric acid, chromic acid, permanganate solutions and the like.
- the temperature at any time during the oxidation treatment should preferably be not higher than 10 C. below the softening point of the pitch at the given time.
- This batch type oxidation is best carried out in a circulating oven through which passes a constant flow of air or oxygen containing gas, both fresh and recycled, pre-heated at the desired temperature.
- the oxidized filament may then be cooled to room temperature or subjected immediately to carbonization. If cooling is elected, it should be gradual, the to 100 C. step being accomplished at about the same rate as the reverse step previously carried out, with the last 100 to room temperature adjustment taking about three hours.
- the 100 to 500 C. temperature range is the most critical in the carbonization process, special care need be exerted in controlling the heating rate through that range.
- the top carbonization temperature it must be noted that useful carbon fibers may be produced from 700 C. for amorphous carbon filaments to as high as 2800+ C. if graphitic filaments are desired. Heating rates and holding times are no longer critical about 1100 C.
- a graphite filament may be conveniently prepared by heating a carbon filament for about one hour in argon at above 1500 C.
- Carbon filaments (1100 C.) of conventional textile lengths may be produced from coal tar pitch by the method just described, having a tensile strength of 80,000 to 130,000 p.s.i., a modulus of elasticity within the range of 4.5 to 5.2)(10 p.s.i., a volume resistivity in ohm-inch of 1200 to 1600 and an apparent density of about 1.65
- Such filaments are eminently suited as substrate in vapor phase depositions such as manufacture of boron filaments, heat resistant reinforcement in fiber-matrix composites, as well as in other similar applications where filamentary carbon is conventionally and advantageously employed.
- the modified coal tar pitch just described was spun through a spinneret having an orifice of 1.5 mm. in length and a diameter of 0.3 mm.
- the molten pitch at 287 C. was driven through the spinnert by a nitrogen pressure of 110 psi.
- the resulting pitch filament had a final diameter of about 30 microns, when stretched and taken up on a paper cylinder at the rate of 256 meters per minute.
- the wound filament paper packages were then hung on graphite supports in an oven through which fresh and recycled air in a ratio of about 1:1 was constantly circulated while the temperature was raised and lowered in 100 to 40 C. 2.0
- the total residence in the oxidizing oven was thus 178.25 hours.
- the carbon monofilament had an average diameter of 25 microns and, as measured on 0.125 inch long samples, a volume resistivity of 1419 ,uohm-inch with a variation of 15.0%.
Abstract
Description
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US734257A US3595946A (en) | 1968-06-04 | 1968-06-04 | Process for the production of carbon filaments from coal tar pitch |
US8489670A | 1970-10-28 | 1970-10-28 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3718493A true US3718493A (en) | 1973-02-27 |
Family
ID=26771555
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US00084896A Expired - Lifetime US3718493A (en) | 1968-06-04 | 1970-10-28 | Process for the production of carbon filaments from coal tar pitch |
Country Status (1)
Country | Link |
---|---|
US (1) | US3718493A (en) |
Cited By (19)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3919376A (en) * | 1972-12-26 | 1975-11-11 | Union Carbide Corp | Process for producing high mesophase content pitch fibers |
US3919387A (en) * | 1972-12-26 | 1975-11-11 | Union Carbide Corp | Process for producing high mesophase content pitch fibers |
US3995014A (en) * | 1973-12-11 | 1976-11-30 | Union Carbide Corporation | Process for producing carbon fibers from mesophase pitch |
US4026788A (en) * | 1973-12-11 | 1977-05-31 | Union Carbide Corporation | Process for producing mesophase pitch |
US4032430A (en) * | 1973-12-11 | 1977-06-28 | Union Carbide Corporation | Process for producing carbon fibers from mesophase pitch |
US4032607A (en) * | 1974-09-27 | 1977-06-28 | Union Carbide Corporation | Process for producing self-bonded webs of non-woven carbon fibers |
US4066737A (en) * | 1971-05-05 | 1978-01-03 | Koppers Company, Inc. | Method for making isotropic carbon fibers |
US4225416A (en) * | 1975-10-24 | 1980-09-30 | Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler | Process for the production of high quality carbon black forming material |
US4243512A (en) * | 1978-06-28 | 1981-01-06 | Kureha Kagaku Kogyo Kabushiki Kaisha | Process for preparation of pitch for producing carbon fiber |
EP0087749A1 (en) * | 1982-02-23 | 1983-09-07 | Mitsubishi Oil Company, Limited | Pitch as a raw material for making carbon fibers and process for producing the same |
US4517072A (en) * | 1981-05-18 | 1985-05-14 | Domtar Inc. | Process for modifying coal tar materials |
US4604184A (en) * | 1983-11-16 | 1986-08-05 | Domtar Inc. | Modified coal-tar pitch |
EP0201213A2 (en) * | 1985-04-29 | 1986-11-12 | E.I. Du Pont De Nemours And Company | Stabilization of pitch fiber |
DE3703825A1 (en) * | 1987-02-07 | 1988-08-18 | Didier Eng | METHOD AND DEVICE FOR PRODUCING CARBON FIBERS |
US4986893A (en) * | 1987-07-08 | 1991-01-22 | Kureha Kagaku Kogyo Kabushiki Kaisha | Process for producing pitch for carbon materials |
US5238672A (en) * | 1989-06-20 | 1993-08-24 | Ashland Oil, Inc. | Mesophase pitches, carbon fiber precursors, and carbonized fibers |
US5501788A (en) * | 1994-06-27 | 1996-03-26 | Conoco Inc. | Self-stabilizing pitch for carbon fiber manufacture |
CN102732280A (en) * | 2012-07-09 | 2012-10-17 | 遇秉武 | High-softening-point coal-tar pitch production method |
US20140175688A1 (en) * | 2012-12-26 | 2014-06-26 | Honeywell Federal Manufacturing & Technologies, Llc | Methods of making carbon fiber from asphaltenes |
-
1970
- 1970-10-28 US US00084896A patent/US3718493A/en not_active Expired - Lifetime
Cited By (23)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4066737A (en) * | 1971-05-05 | 1978-01-03 | Koppers Company, Inc. | Method for making isotropic carbon fibers |
US3919376A (en) * | 1972-12-26 | 1975-11-11 | Union Carbide Corp | Process for producing high mesophase content pitch fibers |
US3919387A (en) * | 1972-12-26 | 1975-11-11 | Union Carbide Corp | Process for producing high mesophase content pitch fibers |
US3995014A (en) * | 1973-12-11 | 1976-11-30 | Union Carbide Corporation | Process for producing carbon fibers from mesophase pitch |
US4026788A (en) * | 1973-12-11 | 1977-05-31 | Union Carbide Corporation | Process for producing mesophase pitch |
US4032430A (en) * | 1973-12-11 | 1977-06-28 | Union Carbide Corporation | Process for producing carbon fibers from mesophase pitch |
US4032607A (en) * | 1974-09-27 | 1977-06-28 | Union Carbide Corporation | Process for producing self-bonded webs of non-woven carbon fibers |
US4225416A (en) * | 1975-10-24 | 1980-09-30 | Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler | Process for the production of high quality carbon black forming material |
US4243512A (en) * | 1978-06-28 | 1981-01-06 | Kureha Kagaku Kogyo Kabushiki Kaisha | Process for preparation of pitch for producing carbon fiber |
US4517072A (en) * | 1981-05-18 | 1985-05-14 | Domtar Inc. | Process for modifying coal tar materials |
EP0087749A1 (en) * | 1982-02-23 | 1983-09-07 | Mitsubishi Oil Company, Limited | Pitch as a raw material for making carbon fibers and process for producing the same |
US4604184A (en) * | 1983-11-16 | 1986-08-05 | Domtar Inc. | Modified coal-tar pitch |
EP0201213A2 (en) * | 1985-04-29 | 1986-11-12 | E.I. Du Pont De Nemours And Company | Stabilization of pitch fiber |
EP0201213A3 (en) * | 1985-04-29 | 1987-04-22 | E.I. Du Pont De Nemours And Company | Stabilization of pitch fiber |
DE3703825A1 (en) * | 1987-02-07 | 1988-08-18 | Didier Eng | METHOD AND DEVICE FOR PRODUCING CARBON FIBERS |
US4986893A (en) * | 1987-07-08 | 1991-01-22 | Kureha Kagaku Kogyo Kabushiki Kaisha | Process for producing pitch for carbon materials |
US5238672A (en) * | 1989-06-20 | 1993-08-24 | Ashland Oil, Inc. | Mesophase pitches, carbon fiber precursors, and carbonized fibers |
US5614164A (en) * | 1989-06-20 | 1997-03-25 | Ashland Inc. | Production of mesophase pitches, carbon fiber precursors, and carbonized fibers |
US5501788A (en) * | 1994-06-27 | 1996-03-26 | Conoco Inc. | Self-stabilizing pitch for carbon fiber manufacture |
CN102732280A (en) * | 2012-07-09 | 2012-10-17 | 遇秉武 | High-softening-point coal-tar pitch production method |
CN102732280B (en) * | 2012-07-09 | 2014-04-16 | 遇秉武 | High-softening-point coal-tar pitch production method |
US20140175688A1 (en) * | 2012-12-26 | 2014-06-26 | Honeywell Federal Manufacturing & Technologies, Llc | Methods of making carbon fiber from asphaltenes |
US9580839B2 (en) * | 2012-12-26 | 2017-02-28 | Honeywell Federal Manufacturing & Technologies, Llc | Methods of making carbon fiber from asphaltenes |
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