The invention relates to a high-purity arsenic preparation method. The high-purity arsenic preparation method adopts an arsenic crude product as a raw material and orderly comprises 1, an oxidation reaction, 2, an esterification reaction, 3, solid-liquid separation, 4, adsorption purification, 5, solid-liquid separation, 6, rectification purification, 7, hydrolysis-crystallization, 8, solid-liquid separation, 9, water washing, 10, dehydration, 11, drying, and 12, a reduction reaction. The high-purity arsenic preparation method has the advantages of short process, simple separation purification processes, high product purity, stable quality, safe and reliable processes, low energy consumption and less three wastes and is a clean production method satisfying green chemical development requirements.