Maruzen Petrochemical Company, Limited

Other

Agency of Industrial Science and Technology

Sakae Naito

Masatoshi Tsuchitani

Ryoichi Nakajima

Kiyotaka Suzuki

Makoto Tamura

Kensuke Iuchi

Shintaro Hasebe

Hiroshi Morijiri

Shuji Okada

Sjuji Okada

When preparing carbon artefacts from heavy oils of petroleum or coal origin, removal of undesirable components or recovery of desirable components from raw materials or intermediates is usually required so as to improve the quality of the final products. Such removal or recovery operation is conventionally done by filtration. In the past, regeneration of filters clogged with solid carbonaceous materials inevitably formed by the filtration operations is difficult and troublesome procedures. Herein disclosed is a simple and effective process for regenerating filters clogged with solid carboneceous materials, characterized by treating the filter medium in an aqueous solution of hydrogen peroxide with heating and then optionally conducting ultrasonic washing in water or a solvent. By this simple process, clogged filters can be regenerated completely to show the same filtration performance as new filters.

Process for regenerating clogged filters

Commercially attractive continuous processes for the preparation of mesophase pitches for manufacturing high-performance carbon fibers are disclosed. One feature resides in that conversion of a pitch into a mesophase pitch is conducted continuously by using a unique continuous dispersion-heat-treating apparatus. The other feature resides in that the raw material for hydrogenation treatment which is a pretreatment preceeding to the final heat treatment for the production of a mesophase pitch, is prepared by using a heavy oil or pitch having substantially no BTX-insoluble material as the starting raw material, subjecting the raw material to a simple four-step treatment of (1) a continuous heat treatment in a tubular heater, (2) a distillation operation, (3) a BTX-solvent extraction and (4) a distillation operation; while recycling a soluble component obtained in the step (4) to the heat treatment of step (1) and recovering a BTX-solvent insoluble component formed in step (3) as the material for the hydrogenation treatment. This feature can provide a significant increase in the yield of a mesophase pitch. Furthermore, unexpectedly, the recycle of the soluble component into the heat treatment of step (1) is helpful to improve the characteristics of the ultimate products, i.e., carbon fibers or graphite fibers. Combination of the first and the second features, of course, can provide a better commercial success. In fact, the process of the present invention can provide a carbon fiber having a tensile strength of more than 300 kg/mm.sup.2 and a graphite fiber having a tensile strength of more than 400 kg/mm.sup.2 and a modulus of elasticity of more than 60 ton/mm.sup.2. Processes with minor modifications to the above are also disclosed.

Process for preparing pitches

Commercially attractive continuous processes for the preparation of mesophase pitches for manufacturing high-performance carbon fibers are disclosed. One feature resides in that conversion of a pitch into a mesophase pitch is conducted continuously by using a unique continuous dispersion-heat-treating apparatus. The other feature resides in that the raw material for hydrogenation treatment which is a pretreatment preceeding to the final heat treatment for the production of a mesophase pitch, is prepared by using a heavy oil or pitch having substantially no BTX-insoluble material as the starting raw material, subjecting the raw material to a simple four-step treatment of (1) a continuous heat treatment in a tubular heater, (2) a distillation operation, (3) a BTX-solvent extraction and (4) a distillation operation; while recycling a soluble component obtained in the step (4) to the heat treatment of step (1) and recovering a BTX-solvent insoluble component formed in step (3) as the material for the hydrogenation treatment. This feature can provide a significant increase in the yield of a mesophase pitch. Furthermore, unexpectedly, the recycle of the soluble component into the heat treatment of step (1) is helpful to improve the characteristics of the ultimate products, i.e., carbon fibers or graphite fibers. Combination of the first and the second features, of course, can provide a better commercial success. In fact, the process of the present invention can provide a carbon fiber having a tensile strength of more than 300 kg/mm.sup.2 and a graphite fiber having a tensile strength of more than 400 kg/mm.sup.2 and a modulus of elasticity of no more than 60 ton/mm.sup.2. Processes with minor modifications to the above are also disclosed.

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. One important merit of the process is that the production ratio of ultra HP carbon fibers and GP carbon fibers can easily be changed to accommodate to market's demand. Accordingly, the process has wide flexibility in operation. Of course, the effective utilization of valueless spent fraction can reduce the production costs of not only ultra HP carbon fibers but also GP carbon fibers.

Process for producing pitch for the manufacture of high-performance

The unwanted components from coal tars should be removed at a certain stage of the process for producing homogeneous spinning pitches which are suitable for use in the production of high-performance carbon fibers from coal tars. The unwanted components can be eliminated from coal tars in a very efficient manner by the following procedures: subjecting the coal tars to distillation or flash distillation so as to separate a heavy component having a boiling point higher than a predetermined temperature, dissolving the heavy component in a monocyclic aromatic hydrocarbon solvent, and subjecting the solution to filtration or centrifugation.

Method of purifying coal tars for use in the production of carbon

A process for the preparation of an excellent mesophase pitch suitable for use as a spinning pitch for the production of high performance carbon fibers is disclosed. The mesophase pitch can satisfy the four remarkable characteristics at the same time, i.e., a softening point of below 320.degree. C. as determined by Mettler method, a mesophase content of above 90% as examined on a polarized microscope, a quinoline insoluble content of less than 20%, and a xylene soluble content of less than 20%. The mesophase pitch is particularly homogeneous and is easily spinnable. The process can be characterized by a preliminary extraction step, a continuous heat treatment step, and an extraction step. In some cases, the preliminary extraction step can be omitted. Graphite fibers having a tensile strength of about 400 Kg/mm.sup.2 and a modulus of elasticity of above 60 ton/mm.sup.2 can be obtained from the mesophase pitch. Further, even carbon fibers prepared at a carbonization temperature of 1000.degree. C. have a tensile strength of about 300 Kg/mm.sup.2.

Process for the preparation of mesophase pitches

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

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Chiba, Japan

Sakae Naito