Abstract: There is disclosed a method for the preparation of difluoromethane wherein methylene chloride is reacted with. hydrogen fluoride in liquid phase, at a temperature of about 70.degree. to 90.degree. C. under a pressure of about 11 to 12 kg/cm.sup.2.g in the presence of antimony pentachloride. It is important that the concentration of quinquevalent antimony is maintained at a level of 85% or more with the feed mole ratio of hydrogen fluoride to methylene chloride ranging from about 2.0 to 2.3.Applicable to industrial scale, the method is operated in a batch system or in a continuous system. In addition, it exhibits superior conversion rate of the materials and production yield.