Clinoptilolite　was　synthesized　via　hydrothermal　method　using　aluminum　hydroxide　as　aluminum　source　and　silica　sol　(Ludox)　as　silicon　source.　The　influences　of　synthesized　parameters　(i.e.,　molar　ratio　of　n(OH-)/n(Si),　crystallization　time　and　crystallization　temperature,　etc.)　on　the　structure　of　prepared　clinoptilolite　and　its　CH4/N2　separation　performance　were　investigated　by　various　characterization　techniques,　including　XRD,　TEM,　BET,　FT-IR,　TG,　29Si-NMR.　Particularly,　the　kinetic　behaviors　of　crystallization　rate　were　evaluated,　and　the　apparent　activation　energies　for　induction　and　growth　period　according　to　Arrhenius　equation　are　91.5　and　7.2　kJ/mol,　respectively.　Meanwhile,　Ca2+　and　K+　clinoptilolites　were　prepared　through　water　solution　ion　exchange　method.　Moreover,　the　CH4/N2　separation　performance　was　also　evaluated　for　clinoptilolites　with/without　ion　exchange.　Experimental　results　suggest　that　equilibrium　selectivity　of　CH4/N2　is　strongly　depended　on　the　type　of　exchanged　cationic　charge,　its　quantity　and　distribution　in　the　skeleton.　K-clinoptilolite　exhibited　a　good　separation　performance,　and　could　be　a　promising　absorbent　for　coal　bed　methane　recovery.　©　2019,　Editorial　Office　of　Acta　Petrolei　Sinica(Petroleum　Processing　Section).　All　right　reserved.