Abstract: A novel crystalline aluminophosphate CFAP-6 was synthesized hydro thermally in a system of di-n-butylamine-(NH₄)₂O-P₂O₅-Al₂O₃-H₂O, the P₂O₅ and Al₂O₃ sources of which were (NH₄)₃PO₄·3H₂Oand Al₂(SO₄)₃ aqueous solutionrespectively.The mole ratio composition of rcactant was: di-n-butylamine/(NH₄)₂O/P₂O₅/Al₂O₃/H₂O = (1~1.2)/(3~3.6)/(l~1.2)/l/67.The reaction is conducted at 200℃. Investigations of DTA, XRD, IRand the adsorption experiment show that transformation of the raw powder (phase a) into more stable crystal form (phase b) with properties of molecular sieve, on heating at 350℃ and giving H₂O and amine(or ampnia) off. Isotherms for the adsorption of H₂O and CH₃OH at 23℃ indicate that the dimension of the adsorption window of CFAP-6 is between 4.3 and 4.9Å and the. capacity about 0.07mL/g.