The invention relates to a preparation method of solid carbon dot fluorescent powder with high quantum yield. The preparation method comprises the following steps: weighing raw materials according tothe following constituents in parts by weight: 0.25 to 1 part of potassium hydrogen phthalate, 0.5 part of sodium azide and 0.25 to 1 part of boric acid; mixing the raw materials, then dissolving themixture in a formaldehyde solution ultrasonically, putting the mixed solution in a microwave oven for heating at the power of 225 to 750 W for 4 to 10 min, and completely evaporating the liquid at theend of reaction to obtain white powder which is nitrogen and boron-doped carbon dots (NBCDs). The preparation method is low in cost, high in preparation speed and easy to operate; the quantum yield (QY) of the prepared solid luminous NBCSs is extremely high, and the absolute solid luminous QY of the NBCSs is 67.7 percent.