Patent GB-976112-A (GB)
Title: Carbonaceous bodies useful for thermal insulation and processes for preparing same
IPC: C04B38/08
Filed: 1962-06-15
Abstract: Carbonaceous bodies are produced by mixing expanded carbonaceous particles, of bulk density less than 25 lb./cu. ft., particles size 5-1000 microns and volatile content less than 15%, with a binder and compressing and baking the mixture.  Suitable particles containing a large number of enclosed voids may be prepared by rapidly heating or flash-roasting a finely-divided carbonaceous material, which is normally solid but expands and becomes plastic on heating. The starting material should contain 95-100% mesh particles and should have a volatile content of 10-45%. Specified materials are low, medium and high volatile bituminous coals, impsonite, albertite, high volatile petroleum coke, raw coal tar pitch coke and coal tar pitch fortified with thermal blacks or carbon blacks. The material is suspended in a gas containing free oxygen and lead to the top of a vertical reactor maintained at 1150-2000 DEG  F. by gas heating.  The temperature is dependent on the oxygen flow and this is kept within limits of 2-4 cu. ft./lb. of carbonaceous material, if unheated air is used, in order that at least 10% of the evolved, volatile, combustible matter remains unburned. After roasting, the particles are separated from the other products in a cyclone separator, at such a temperature that the volatile products do not condense, and optionally milled and passed into a second reactor, in which volatile matter adhering to the surfaces is removed.  The binder should facilitate even mixing and be suitable for graphitizing, e.g. coal tar, coal tar pitch, diluted pitch, emulsified or dehydrated coal tar, furfuryl alcohol and acetone-furfural co-polymer. A two-stage binder may be used, one compound, e.g. maize, potato, rice wheat or barley starch, sugar or dextrin, facilitating low temperature setting and the other, a powder bituminous material, m.p. 250-350 DEG  F., e.g. coal tar, asphalt, "Gilsonite" (Registered Trade Mark) or vegetable oil pitch, acting as a permanent binder.  10-60 parts by weight of the binder should be mixed with 100 parts of the expanded carbonaceous particles at temperatures up to 200 DEG  C. Activated carbon may also be added.  The mixture should have an apparent density of 0.2-0.9 g./c.c. before forming and this may be achieved by vibrating the mixture or extruding, forming or compressing it as a slurry.  Forming may be carried out at temperatures up to 200 DEG  C. and pressures of 100-1500 lb./sq. in. Before baking, the bodies may be cured by heating to 100 DEG  C. for 18 hours and to 200 DEG  C. for 2.5 hours.  Baking is at 800-2000 DEG  C. in an inert atmosphere or using a packing compound, the temperature being reached over 3 or 4 days.  The baked bodies may be graphitized by heating to 2000-3000 DEG  C. in a graphite tube resistance furnace containing nitrogen the temperature being reached in steps of 100-400 DEG  C./hr. The products have apparent densities of 0.4-0.9 g./c.c., thermal conductivities at 375 DEG  F. of 2-115 (B.t.u. inches)/(hr. ft.2  DEG F.) and a permeability of 0.05-3.0 Darcys.ALSO:Expanded carbonaceous particles containing a large number of enclosed voids are produced by rapidly heating or flash roasting a finely divided carbonaceous material, which is normally solid but becomes plastic on heating. The starting material should contain 95%-100 mesh particles and should have a volatile content of 10-45%.  Specified materials are low, medium and high volatile bituminous coals, impsonite, albertite, high volatile petroleum coke, raw coal tar pitch coke and coal tar pitch fortified with thermal blacks and carbon blacks.  The material is suspended in a gas containing free oxygen and led to the top of a vertical reactor maintained at 1150-200 DEG  F.  The temperature is dependent on the oxygen flow and this is kept at 2-4cu. feet/lb. of carbonaceous material, if unheated air is used, in order that at least 10% of the evolved, volatile, combustible matter remains unburnt.  After roasting, the particles are separated in a cyclone separator at such a temperature that the volatile products do not condense, and optionally milled and passed into a second reactor in which volatile matter adhering to the surfaces is removed.