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Polymerization confined to the pore was first adapted for the nanoscale structure adjustment of adsorption resin. The self-cross-linked polymer (P-1) formed in the pore of hyper-cross-linked resin (HR) by the Friedel–Crafts reaction of p-dichloroxylene (p-DCX), occupying the macropore of the HR resin and bringing about an external micropore. Compared with the raw HR resin, the volume of the micropore of HR@P-1 in 0.4 < D < 1 nm increased but the volume of the macropore has obviously decreased. After the loading of P-1 in the nanopore of HR, HR@P-1 has better gas adsorption performance. At 298 and 100 KPa, the adsorption capacity of CO2is almost 30% higher than that of HR, reaching 35.7 cm3/g, due to the increase in the smaller micropore volume. Moreover, HR@P-1 has also been found to be the first C2H6-selective adsorption resin. The uptake of C2H6is up to 56 cm3/g, and the IAST selectivity of C2H6/CH4reaches 15.3. HR@P-1 can also separate syngas efficiently at ambient temperature and be regenerated by simple vacuum operation.

The morphology and regeneration ability of adsorbents are important for gas pressure swing adsorption and separation. Herein, HCP-1 (a hyper-crosslinked polymer) and HCP@MAO(Fe) (a hyper-crosslinked polymer modified by ferrocene) with a spherical morphology are synthesized by a post-crosslinking reaction of chloromethylated styrene-divinylbenzene (Cl-St-DVB) beads for the separation of CO2/CO and CO2/CH4. Both static adsorption and dynamic separation tests verified that HCP@MAO(Fe) has the best gas adsorption and separation performance. The highest adsorption capacity of CO2reached 1.24 mmol/g. The IAST selectivity of CO2/CO is up to 20.6. Moreover, HCP@MAO(Fe) can be regenerated by simple vacuum operation, contributing to the low value of adsorption enthalpy (24.5 KJ/mol). The adsorption mechanism between CO2and the resin framework was also studied by experiments and electrostatic potential map analysis. A stronger interaction can be found between CO2and HCP@MAO(Fe) as a result of the higher Mulliken charge of the cyclopentadiene structure.