The invention discloses a preparation method of ammonium bifluoride. The preparation method comprises the following steps of: with unsaturated ammonium fluoride solution with the mass percent concentration of 10-50% adopted, adding hydrofluoric acid with the mass percent concentration of 15-50%, and controlling reaction temperature to be 40-80 DEG C; after the reaction is finished, adding ammoniasolution with the mass percent concentration of 12-25% into a reaction system, reacting with excessive hydrofluoric acid, controlling reaction temperature to be below 30 DEG C, reacting for 40-90 minutes, concentrating ammonium bifluoride solution obtained in a three-opening bottle, then cooling and crystallizing, so as to obtain ammonium bifluoride crystals; and drying the ammonium bifluoride crystals, thus an ammonium bifluoride product is obtained. The invention has the beneficial effects that: compared with the prior art, process route is simple, conditions and requirements are unharsh, and realization is easy; the prepared ammonium bifluoride product has low moisture content and high purity, the product does not cake, energy consumption problem is noticed in a production process of ammonium bifluoride, and excessive consumption of energy source is avoided. By adopting the preparation method disclosed by the invention, fluorine resource is efficiently utilized, and the fluorine resource which enters into a system is finally converted into the ammonium bifluoride product. The preparation method disclosed by the invention has obvious economic benefit and is applicable to being popularized in fluorine chemical enterprises.