The invention discloses a preparation method of 3-cyanopyridine oxynitride. The preparation method is characterized by comprising the following steps of: melting 500kg of 3-cyanopyridine, adding the molten 3-cyanopyridine into an enamel reaction kettle, adding 10kg of concentrated 
sulfuric acid and 8kg of 
molybdenum oxide into the reaction kettle, stirring the mixture, slowly heating to 65 DEG C, beginning to dropwise add 
hydrogen peroxide, controlling the dropping speed at about 200kg / h, after the dropwise adding operation is ended, continuing to react at the temperature of 65-68 DEG C for 7-8h, sampling, detecting the sample by using 
gas chromatography, and ending the heat preservation when the content of the 3-cyanopyridine is lower than or equal to 1.0%; and adjusting the pH value of the reaction liquid to 9.5-10.5 by using 
potassium carbonate, crystallizing, cooling the 
crystal to be below 5 DEG C, centrifuging, and 
drying the 
crystal at the temperature of 80-90 DEG C to obtain the 3-cyanopyridine oxynitride, wherein the 
water content of the 3-cyanopyridine oxynitride is smaller than or equal to 1.0%. Compared with the prior art, the preparation method has the 
advantage that the production cost is greatly reduced, so that the economic benefit and market competitiveness of an enterprise are increased.