The invention provides a preparation method of nicarbazin. The preparation method includes the following steps: 1, adding wet paranitroaniline and a solvent into a reaction bottle, and conducting heating, refluxing and water separation; 2, after conducting water distribution, conducting cooling to the room temperature, adding bis(trichloromethyl)carbonate, then conducting heating and stirring to obtain 4, 4'-binitro diphenylcarbamide, and absorbing the generated hydrogen chloride gas with the solvent; 3, adding the liquid absorbing the hydrogen chloride gas as a reaction solvent in another reaction bottle, and adding acetylacetone and urea for a reaction to generate 2-hydroxyl-4,6-dimethyl pyrimidine hydrochloride; 4, regulating the obtained 2-hydroxyl-4,6-dimethyl pyrimidine hydrochloride to be alkaline, then allowing 2-hydroxyl-4,6-dimethyl pyridine hydrochloride to react with 4,4'-binitro diphenylcarbamide in a solution to generate the nicarbazin under the stirring condition, and conducting processing to obtain the finished product of the nicarbazin. The special devices are used and comprise a reaction kettle, a condenser, a gas-liquid separator, a water separator, an anti-inverse-suction one-way valve, an absorption kettle and a second reaction kettle. The raw materials are fully utilized, the product yield is high, the cost is low, and the three wastes are few.