Production of carbon by eliminating hydrogen halide from polymerized halohydrocarbons

• US 3,960,768 A
• Filed: 07/05/1974
• Issued: 06/01/1976
• Est. Priority Date: 01/28/1972
• Status: Expired due to Term

• Current Assignee: Sirmac Limited
• Original Assignee: Sirmac Limited
• Inventors: Pfitzner, Klaus, Ripperger, Willi, Kaiser, Rudolf, Palm, Richard Adolf, Oettinger, Willi
• Primary Examiner(s): Douglas, Winston A.
• Assistant Examiner(s): Konopka, P. E.
• Application Number:
  US05/486,059
• Time in Patent Office: 697 Days
• Field of Search: 252/421, 252/445, 252/444, 423/449, 423/445, 423/447, 201/25, 201/2.5, 55/67, 55/386, 264/24
• US Class Current: 502/8
• CPC Class Codes: B01J 20/20 comprising free carbon; comprising carbon obtained by carbonising processes
• CPC Class Codes: B01J 20/28011 Other properties, e.g. density, crush strength
• CPC Class Codes: B01J 20/28057 Surface area, e.g. B.E.T specific surface area
• CPC Class Codes: B01J 20/281 Sorbents specially adapted for preparative, analytical or investigative chromatography
• CPC Class Codes: B01J 20/282 Porous sorbents ion exchange B01J39/00 - B01J41/00
• CPC Class Codes: B01J 20/3078 Thermal treatment, e.g. calcining or pyrolizing
• CPC Class Codes: B01J 2220/54 Sorbents specially adapted for analytical or investigative chromatography
• CPC Class Codes: C01B 32/306 with molecular sieve properties

Abstract

Hard abrasion-resistant carbon is obtained from polymerized halohydrocarbons by elimination of hydrogen halide in a two-stage process carried out so that in the first decomposition stage, which is carried out at temperatures within the range from 140° to 250°C, a definite amount (not less than 5% by weight and not more than 50% by weight) of the total amount of hydrogen halide capable of being split off is removed. Appropriately shaped end products can be obtained by using raw materials having a globular, cylindrical or other shape. The carbon obtained is suitable as the stationary phase for chromatographic separation and analysis of mixtures.

Claims

1. A process for producing hard, abrasion-resistant spherical carbon from beads of polyvinylidene chloride produced directly by bead polymerization consisting essentially of heating said beads of polyvinylidene chloride to a temperature of from about 140°

to about 250°

C in a first stage under flowing nitrogen for from about 1 hour to about 10 hours whereby from 30 to 45% of the hydrogen chloride that is capable of being removed is eliminated and thereafter raising the treatment temperature very slowly from about 250°

to about 350°

C in the transition stage between the first and a second stage, and further heating said beads in said second stage to a temperature within the range of about 600°

to about 950°

C in the presence of an inert or reducing gas, wherein carbon-containing compounds selected from the group consisting of methane, homologs of methane, acetylene, benzene and carbon tetrachloride are mixed with the inert or reducing gas of said second stage in concentrations of from about 0.05 to about 20% by volume to decompose and deposit pyrocarbon on the surface and in the pores of said beads, said heating being continued until the residual chlorine content of the beads has been reduced to less than 250 ppm, said beads undergoing linear shrinkage during said heating stages of up to 50%.

2. A process as set forth in claim 1 wherein the temperature in the first stage is maintained at from 170°

-200°

C and wherein the residual chlorine content of the beads is reduced to less than 50ppm in the second stage.

3. The product obtained according to the process set forth in claim 2.

4. A process as set forth in claim 2 wherein the second stage of the process is followed by an aftertreatment stage in which the carbon is heated to more than about 1800°

C in an inert or reducing atmosphere.

5. A process as set forth in claim 1 wherein said inert gas is nitrogen.

6. A process as set forth in claim 1 wherein said reducing gas is hydrogen.