The present application relates to the field of nonferrous
metallurgy, and provides a method for preparing high-quality
sodium pyroantimonate by pre-oxidation and double
decomposition, comprising the following steps: under the assistance of ultrasonic
waves, adding
antimony oxide and
hydrogen peroxide into a dilute
nitric acid solution at 50-80 DEG C to react, carrying out liquid-
solid separation, washing, and
drying to obtain a powdered
antimony pentoxide product; slurryzing the
antimony pentoxide product with a
potassium hydroxide solution, then adding the obtained
slurry into a high-pressure reaction kettle, stirring and reacting under high temperature and
high pressure, carrying out liquid-
solid separation after cooling to obtain a
potassium pyroantimonate solution; adding
sodium hydroxide into the
potassium pyroantimonate solution after heating to 70-90 DEG C, carrying out a double
decomposition reaction, carrying out liquid-
solid separation, and
drying to obtain a
sodium pyroantimonate product. The essence of the present application is to achieve the purpose of deeply removing impurities through the two processes of acidic oxidation and pressure
dissolution, and to prepare a high-quality sodium pyroantimonate product by using a double
decomposition reaction. The present application has the advantages of good quality of the sodium pyroantimonate product, good
filtration performance, and stable technical indexes.