The invention discloses a method for preparing a 
sodium pyroantimonate product from high-
arsenic antimony white and vulcanizing, crystallizing, regenerating and recycling 
mother liquor, and relates to the field of 
antimony fine chemicals. According to the method, the low-cost-value high-
arsenic antimony white is subjected to alkaline oxidation to prepare the 
sodium pyroantimonate product with the high additional value, the 
mother liquor containing impurities such as 
arsenic, lead and 
zinc is subjected to sulfuration 
crystallization to achieve cooling 
crystallization of 
sodium arsenate and sulfuration 
precipitation of lead and 
zinc ions, and the purified and regenerated 
mother liquor is continuously used for preparing the sodium pyroantimonate. The sodium pyroantimonate product meets the second-grade product requirement of the Chinese 
nonferrous metal industry standard (YS / T 22-2010), and the problem of separation of impurities such as antimony, arsenic, lead and 
zinc during preparation of sodium pyroantimonate from high-arsenic antimony white with complex components is solved. Meanwhile, the mother liquor is efficiently regenerated through 
vulcanization and 
crystallization, the problems that arsenic and alkali are difficult to separate and 
energy consumption is high after 
evaporation, concentration and crystallization are carried out are solved, and finally, the regenerated mother liquor is used for preparing sodium pyroantimonate, and efficient preparation of a product and recycling of the mother liquor are achieved; 
technical innovation is provided for high-valued utilization of low-price high-arsenic antimony white and purification and regeneration of mother liquor. The method has the advantages of convenience in operation, stable product components, high mother liquor purification efficiency and the like.