Activation and Micropore Structure Determination of Carbon-Fiber Composite Molecular Sieves
The progress of research in the development of novel, rigid, monolithic adsorbent carbon fiber composites is described. Carbon fiber composites am produced at ORNL and activated at the CAER using steam or CO{sub 2} under different conditions, with the aims of producing a uniform degree of activation through the material, and of closely controlling pore structure and adsorptive properties. The principal focus of the work to date has been to produce materials with narrow porosity far use in gas separations. Carbon fiber composites are prepared at ORNL, usually in plate or tubular form, by vacuum molding from water slurries containing phenolic resin and chopped isotropic petroleum pitch fibers. The composites are activated at the CAER in steam or CO{sub 2} using samples of dimensions up to 1.5 x 4 x 12 cm that are cut from the original plates. One of the objectives is to produce uniformly activated composites, which is especially critical when attempting to active large monoliths. It has been found that there are appreciable variations in the density and permeability of the as-formed composites that must relate to the forming technique. These variations are expected to exert some influence on the rate and extent of reaction and surface area development. In attempting to uniformly activate the composites, two reactor configurations have been investigated. In the more successful arrangement, steam ''is introduced at several points along the length of the composite. A reduction in steam partial pressure from 95vol% to 44vol% significantly improved the uniformity of surface area distribution. Activation with CO{sub 2} was still better, which is attributed to the much slower reaction rate than with steam. Measurements of composite dimensions have shown that there is an overall shrinkage during activation. A direct correlation is found between dimensional shrinkage and burnoff, and is similar for a and steam activation. The causes of the shrinkage are not yet clear. At levels of burnoff above about 40%, the extent of contraction is sufficient to produce stresses that result in fracture. Activated composites have been evaluated for the separation of CH{sub 4}-CO{sub 2} mixtures, and an apparatus has been constructed specifically for this purpose. Samples activated to low burn-off (5-7% wt loss) with low surface areas (from 300-500m{sup 2}/g) give much better separation of CO{sub 2} and CH{sub 4}, than samples produced at higher burnoff, and there appears to be no benefit in producing composites at burnoffs higher than 10%. The greater separation efficiency obtained at low burnoff means that the most effective CFCMS can be produced at relatively low cost. Continuing work will attempt to define the parameters that influence this gas separation, and whether these are applicable to other gas mixtures. Five samples of CFCMS have been recently prepared for shipment to British Oxygen Corporation (BOC) for testing as molecular sieves. The samples were machined to specific dimensions at ORNL (approx. 2.5 cm diameter x 1.25 cm thick) and activated at CAER. The samples were produced to different burn-off, but all have relatively narrow pore size distributions with average pore diameters around 6A.
- Research Organization:
- Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
- Sponsoring Organization:
- US Department of Energy (US)
- DOE Contract Number:
- AC05-00OR22725
- OSTI ID:
- 814103
- Report Number(s):
- ORNL/SUB/94-SN719/01; TRN: US200316%%450
- Resource Relation:
- Other Information: PBD: 1 Jan 1995
- Country of Publication:
- United States
- Language:
- English
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