Intercalation compound LixVOPO4.2H2O (x = 0.4-1.0) was prepared by redox intercalation of VOPO4.2H2O with lithium iodide in acetone solution. Kinetics of the reaction at 20 and 40-degrees-C, X-ray diffraction and ac conductivity of prepared compounds were studied. Four stages denoted as 3, 2, 3/2, 1 were found in LixVOPO4.2H2O. The conductivity decreases with increasing content of lithium in LixVOPO4.2H2O. This phenomenon is discussed regarding protons as charge carriers.