A new type of non-soluble copper aluminophosphate(denoted as CuAlPO) was synthesized by(static) hydrothermal crystallization and characterized by using several physicochemical techniques.XRD analysis reveals that CuAlPO can be obtained from a reactive gel of molar composition: iso-Pr2NH∶0.3CuO∶(0.7Al2O3∶)P2O5∶80H2O in a Teflon-lined stainless steel autoclave at 180 ℃ for 72 h and has the same crystal structure as that of hexagonal SiO2(JCPDS No.83-2299).The sources of CuO,Al2O3 and P2O5 were copper sulfate pentahydrate,aluminum isopropoxide and o-phosphoric acid(mass fraction: 85%),respectively.SEM shows a characteristic hexagonal morphology and a crystallite size of about 2 μm for both the as-synthesized CuAlPO and the calcined CuAlPO(550 ℃,6h).Low specific surace area(2.0 m2/g) and pore volume(0.004 mL/g) of CuAlPO were observed by N2-adsorption measurement.Catalytic evaluation tests demonstrate that an excellent transformation of phenol into catechol and hydroquinone over the material was achieved in water under the benign reaction conditions with a phenol conversion of 29.5% being observed at room temperature(30 ℃).