Clinoptilolite　(CP)　was　successfully　synthesized　via　a　hydrothermal　route　in　the　presence　of　polyethylene　glycol　(PEG),　and　it　was　then　delaminated　by　washing　using　Zn2+　containing　acid.　HKUST-1,　as　one　kind　of　the　Cu-based　MOFs,　showed　a　high　CO2　adsorption　capacity　owing　to　its　large　pore　volume　and　specific　surface　area.　In　the　present　work,　we　selected　one　of　the　most　efficient　ways　for　preparing　the　HKUST-1@CP　compounds　via　coordination　between　exchanged　Cu2+　and　ligand　(trimesic　acid).　Their　structural　and　textural　properties　were　characterized　by　XRD,　SAXS,　N-2　sorption　isotherms,　SEM,　and　TG-DSC　profiles.　Particularly,　the　effect　of　the　additive　PEG　(average　molecular　weight　of　600)　on　the　induction　(nucleation)　periods　and　growth　behaviors　were　detailed　and　investigated　in　the　hydrothermal　crystallization　procedures　of　synthetic　CPs.　The　corresponding　activation　energies　of　induction　(E-n)　and　growth　(E-g)　periods　during　crystallization　intervals　were　calculated.　Meanwhile,　the　pore　size　of　the　inter-particles　of　HKUST-1@CP　was　14.16　nm,　and　the　BET　specific　area　and　pore　volume　were　55.2　m(2)/g　and　0.20　cm(3)/g,　respectively.　Their　CO2　and　CH4　adsorption　capacities　and　selectivity　were　preliminarily　explored,　showing　0.93　mmol/g　for　HKUST-1@CP　at　298　K　with　the　highest　selective　factor　of　5.87　for　CO2/CH4,　and　the　dynamic　separation　performance　was　evaluated　in　column　breakthrough　experiments.　These　results　suggested　an　efficient　way　of　preparing　zeolites　and　MOFs　composites　that　is　conducive　to　being　a　promising　adsorbent　for　applications　in　gas　separation.