The synthesis of some novel perylene bisimide derivatives was reported and their linear absorption, emission, and two-photon properties were measured and discussed. Two-photon cross-sections for these compounds were determined to be 8735 GM maximum (nonlinear transmittance, approximate to 7 ns, 10 Hz and 850 nm). The frequency upconversion fluorescence was observed under the excitation of 850-nm-nanoseconds laser pulses with the peaks located around 669 nm.