Abstract: Nafion solution has been widely applied in many fields, for example, the fuel cell, the modifying electrode, the electrochemistry analysis, and the electrochemistry catalyze. The technique of preparation of special Nafion solution by using high boiling-point dissolvent is reported. Comparing the IR spectrum of the casting Nafion membrane with the original Nafion membrane, it is know that the preparation method of special Nafion solution could not change the chemical composition and the molecule structure of the Nafion membrane, and that the molecule arrangement of the casting Nafion membrane is more orderliness than the original Nafion membrane. This solution obtained in the technique has more superiority property than the Nafion solution of water-alcohols (low boiling-point) system when it is used in the PEMFC.