The invention discloses a preparation method of high-purity nitric acid, which uses industrial-grade nitric acid as a raw material, adds metal nitrate salt for reaction, performs membrane filtration through a microfiltration membrane to remove impurity anions in nitric acid, and passes through melamine-formaldehyde-thiourea resin / The polyacrylic resin composite material membrane is used for membrane filtration to remove impurity cations in nitric acid, and the filtrate is rectified, prepared with high-purity water, blown white, and filtered with a microfiltration membrane to obtain the target product. The content of the high-purity nitric acid obtained by the method of the present invention is 69-70wt%, the impurity metal ion is lower than 1ppb, and the dust particles greater than 0.5 micron are lower than 5 / ml, which meets the standard of SEMI C8, and the microfiltration membrane is used for membrane filtration, and the melamine -Formaldehyde-thiourea resin / polyacrylic acid resin composite membrane is used for membrane filtration, which can effectively remove impurity anions and cations in industrial-grade nitric acid, and the raw materials for making composite membranes can be reused, and the product has good purity, which is suitable for industrial production.