Process for preparing carbonaceous material carrying ultrafinely dispersed metal

A process for manufacturing a stabilized carbon carbonaceous material carrying ultrafinely dispersed metal thereon, which comprises stabilizing a high-softening-point pitch carrying a metal thereon prepared by the steps of:

• obtaining a starting material comprising one selected from the group consisting of a heavy oil having an H/C atomic ratio in the range of between about 0.8 and 1.2 and substantially free from components insoluble in BTX solvent, and a low-softening-point pitch derived from said heavy oil by distilling off light components therefrom;
• shaping the starting material into a micro-shaped material comprising a form selected from the group consisting of particles, liquid particles, powders, and fibers having a size of 100 μm or less;
• contacting the micro-shaped material with an organic solvent which allows at least 10 wt. % of the micro-shaped material to remain insoluble as insoluble components, and extracting 20 to 90 wt. % of the light components contained in the micro-shaped material thereby obtaining a high-softening-point pitch having a softening point of 150° C. or higher when measured by the temperature gradient method, undergoing a weight loss of 5 wt. % or less when heated up to 300° C., and has mesopores of 100 mm3/g or greater, in terms of minute pore volume calculated by the Dollimore-Heal method from an adsorption isotherm of nitrogen at liquid nitrogen temperature;
• contacting this high-softening-point pitch with an anionic surface active agent to obtain a high-softening-point pitch on which the anionic surface active agent has been absorbed;
• forming an aqueous solution incorporating a metal salt;
• and
• bringing this high-softening-point pitch on which the anionic surface active agent has been adsorbed into contact with the aqueous solution of a metal salt to replace the cation of the surface active agent with the metal ion by heating under an atmosphere containing oxygen.

A process for manufacturing a carbide material carrying ultrafinely dispersed metal thereon, which comprises thermally treating a stabilized carbon material carrying a metal thereon, which is obtained by stabilizing a high-softening-point pitch carrying a metal prepared by the steps of:

• obtaining a starting material comprising one selected from the group consisting of a heavy oil having an H/C atomic ratio in the range of between about 0.8 and 1.2 and substantially free from components insoluble in BTX solvent, and a low-softening-point pitch derived from said heavy oil by distilling off light components therefrom,
• shaping the starting material into a micro-shaped material comprising a form selected from the group consisting of particles, liquid particles, powders, and fibers having a size of 100 μm or less;
• contacting the micro-shaped material with an organic solvent which allows at least 10 wt. % of the micro-shaped material to remain insoluble as insoluble components, and extracting 20 to 90 wt. % of the light components contained in the micro-shaped material thereby obtaining a high-softening-point pitch having a softening point of 150 ° C. or higher when measured by the temperature gradient method, undergoing a weight loss of 5 wt. % or less when heated up to 300° C., and has mesopores of 100 mm3/g or greater, in terms of minute pore volume calculated by the Dollimore-Heal method from an adsorption isotherm of nitrogen at liquid nitrogen temperature;
• contacting this high-softening-point pitch with an anionic surface active agent to obtain a high-softening-point pitch on which the anionic surface active agent has been absorbed;
• forming an aqueous solution incorporating a metal salt;
• and
• bringing this high-softening-point pitch on which the anionic surface active agent has been adsorbed into contact with the aqueous solution of a metal salt to replace the cation of the surface active agent with the metal ion by heating under one condition selected from the group consisting of an atmosphere containing oxygen, an inert atmosphere at a temperature of between about 500° C. and 3,000° C., and an atmosphere containing at least one oxidative gas selected from the group consisting of steam and carbon dioxide at a temperature of between about 500° and 1,500° C.

A process for manufacturing a molded article of a carbonaceous material with ultrafinely dispersed metal carried thereon comprising the steps of:

• molding an article using a stabilized carbonaceous material carrying a metal which is obtained by stabilizing a high-softening-point pitch carrying a metal thereon prepared by the steps of:
• obtaining a starting material comprising one selected from the group consisting of a heavy oil having an H/C atomic ration in the range of between about 0.8 and 1.2 and substantially free from components insoluble in BTX solvent, and a low-softening-point pitch derived from said heavy oil by distilling off light components therefrom,
• shaping the starting material into a micro-shaped material comprising a form selected from the group consisting of particles, liquid particles, powders, and fibers having a size of 100 μm or less;
• contacting the micro-shaped material with an organic solvent which allows at least 10 wt. % of the micro-shaped material to remain insoluble as insoluble components, and extracting 20 to 90 wt. % of the light components contained in the micro-shaped material thereby obtaining a high-softening-point pitch having a softening point of 150° C. or higher when measured by the temperature gradient method, undergoing a weight loss of 5 wt. % or less when heated up to 300° C., and has mesopores of 100 mm3/g or greater, in terms of minute pore volume calculated by the Dollimore-Heat method from an adsorption isotherm of nitrogen at liquid nitrogen temperature;
• contacting this high-softening-point with an anionic surface active agent to obtain a high-softening point pitch on which the anionic surface active agent has been absorbed;
• and
• forming an aqueous solution incorporating a metal ion;
• and
• bringing this high-softening-point pitch on which the anionic surface active agent has been adsorbed into contact with the aqueous solution of a metal salt to replace the cation of the surface active agent with the metal ion by heating under one condition selected form the group consisting of an atmosphere containing oxygen, an inert atmosphere at a temperature of between about 500° C. and 3,000° C., and an atmosphere containing at least one oxidative gas selected form the group consisting of steam and carbon dioxide at a temperature of from 500° C. and 1,500° C. and intermixing therewith at least one selected from the group consisting of a carbide carrying a metal which is obtained by stabilizing a high-softening-point pitch carrying a metal thereon prepared by the steps as above, as a filler, and a high-softening-point pitch carrying a metal obtained by the above steps as a binder,
• and processing said molded article by employing one selected from the group consisting of stabilization, carbonization, and graphitization.