Microporous layered titanium phenylphosphonate, Ti(O3PC6H5)(2) and sulfonated titanium phenylphosphonate, Ti(O3PC6H4SO3H)(0.89) (O3PC6H5)(1.1).1.8H(2)O were prepared in the presence of sodium dodecylsulfate (SDS). Interplanar spacing (d(001)) of titanium phenylphosphonate is 1.43 nm and after sulfonation it increased to 1.64 nm. The surface area of titanium phenylphosphonate is 264 m(2) g(-1).