The process for preparing a carbon molecular sieve adsorbent composition includes starting with activated carbon having a specific effective micropore size. Activated carbon is impregnated into the monomer or partially polymerized polymer to complete the polymerization, after which the impregnating agent is carbonized to reduce the micropores to another specific effective micropore size. Finally, the impregnation / polymerization / carbonization product is annealed at a temperature in the range of 1000 ° C. to 1500 ° C., so that the micropores are finally and expected to a size in the range of 4.0 angstroms to 4.3 angstroms. Reduced to The present invention surprisingly allows for effective fine pore size fine tuning and desirable selectivity, capacity, and adsorption rate, and is particularly suitable for use with, for example, fixed beds in pressure swing or temperature swing processes. A very desirable carbon molecular sieving capacity is obtained to enable propylene / propane separation. [Selection] Figure 2
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