Preparation method of nano antimony thioantimonate
A technology of antimony thioantimonate and sodium thioantimonate, applied in antimonate/antimonite, nanotechnology, nanotechnology and other directions, can solve the problem of easy hydrolysis of sodium thioantimonate and easy hydrolysis of antimony trihalide. , waste of environmental water and other problems, to achieve the effect of improving the utilization rate of raw materials, improving the stability and purity, and improving the leaching rate
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Embodiment 1
[0033] The preparation method of nano antimony thioantimonate of the present invention comprises the following steps:
[0034] (1) Add 6.15 mol of sodium sulfide to purified water at a temperature of 50°C under stirring conditions, then add 2.02 mol of elemental sulfur and 1 mol of antimony trioxide, maintain the reaction system at 55°C and stir for 28 minutes, then pump Filter, obtain filtrate, the liquid-solid ratio of described reaction system is 10mL / g;
[0035] (2) cooling and crystallizing the filtrate of step (1) in a low-temperature tank at 0° C. for 20 minutes, separating the crystals and crystallization mother liquor, and obtaining crude crystals of sodium thioantimonate;
[0036] (3) adding the crude crystals of sodium thioantimonate in step (2) into purified water at a temperature of 45° C., stirring for 3 minutes and filtering to obtain a saturated sodium thioantimonate solution;
[0037] (4) recrystallize the saturated sodium thioantimonate solution in step (3) ...
Embodiment 2
[0043] The preparation method of nano antimony thioantimonate of the present invention comprises the following steps:
[0044] (1) Add 6.17 mol of sodium sulfide to purified water at a temperature of 54°C under stirring conditions, then add 2.04 mol of elemental sulfur and 1 mol of antimony trioxide, maintain the reaction system at 60°C and stir for 27 minutes, then pump Filter, obtain filtrate, the liquid-solid ratio of described reaction system is 9mL / g;
[0045] (2) cooling and crystallizing the filtrate of step (1) in a low-temperature tank at 1° C. for 21 minutes, separating the crystals and crystallization mother liquor, and obtaining crude crystals of sodium thioantimonate;
[0046] (3) Add the crude crystals of sodium thioantimonate in step (2) into purified water at a temperature of 42° C., stir for 3.3 minutes and filter to obtain a saturated sodium thioantimonate solution;
[0047] (4) recrystallize the saturated sodium thioantimonate solution in step (3) at 1° C., o...
Embodiment 3
[0053] The preparation method of nano antimony thioantimonate of the present invention comprises the following steps:
[0054] (1) Add 6.19 mol of sodium sulfide to purified water at a temperature of 57°C under stirring conditions, then add 2.07 mol of elemental sulfur and 1 mol of antimony trioxide, maintain the reaction system at 66°C and stir for 26 minutes, then pump Filter, obtain filtrate, the liquid-solid ratio of described reaction system is 8mL / g;
[0055] (2) cooling and crystallizing the filtrate of step (1) in a low-temperature tank at 2° C. for 22 minutes, separating crystals and crystallization mother liquor, and obtaining crude crystals of sodium thioantimonate;
[0056] (3) Add the crude crystals of sodium thioantimonate in step (2) into purified water at a temperature of 39° C., stir for 3.7 minutes and filter to obtain a saturated sodium thioantimonate solution;
[0057] (4) recrystallize the saturated sodium thioantimonate solution in step (3) at 2° C., obt...
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