The invention discloses a separation method used for preparing isopropanol via hydrogenation of acetone. According to the separation method, an acetone hydrogenation product is subjected to azeotropic distillation and extractive distillation so as to obtain high-purity isopropanol. The separation method comprises following steps: (1) the acetone hydrogenation product is delivered into a rectifying tower for azeotropic distillation, an azeotrope is collected from the top of the rectifying tower, a heavier component is collected from a tower kettle of the rectifying tower, and an isopropanol product is collected from side lines of a tower body of the rectifying tower; (2) the azeotrope collected from the top of the rectifying tower is delivered into a recovery tower, and is subjected to extractive distillation using an extraction agent, a material flow containing acetone and isopropanol is collected from the top of the recovery tower, and is delivered back to a reactor for recycling, and an aqueous solution rich in the extraction agent is collected from a tower kettle of the recovery tower; and (3) the aqueous solution rich in the extraction agent is delivered into a dehydrating tower, and the extraction is collected from a tower kettle of the dehydrating tower, and is delivered back to the recovery tower. According to the separation method, azeotropic distillation and extractive distillation are adopted, high-purity isopropanol is prepared, raw material consumption is less, extraction agent loss is low, technical processes are simple, and operation is convenient.