A kind of preparation method of superfine ferric boride
A technology of iron boride and boric acid solution, applied in the direction of boron/boride, metal boride, etc., can solve the problems of large particle size, low activity and small BET of iron boride
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Embodiment 1
[0036] A kind of preparation method of superfine ferric boride, it is the following steps:
[0037] (1) after ferrous gluconate solution and boric acid solution are mixed, spray drying, obtain spray-dried material, the mol ratio of ferrous gluconate solution and boric acid is 1:1.01;
[0038] (2) Sintering the spray-dried material in a methane atmosphere, the sintering time is 10h, and the sintering temperature is 1200°C to react to obtain the reduced material;
[0039] (3) continue to feed carbon dioxide into the reducing material, and react at a temperature of 700°C for 4 hours to obtain a sintered material;
[0040] (4) The sintered material is subjected to jet crushing, screening and vacuum packaging to obtain superfine iron boride.
[0041] The concentration of described step (1) ferrous gluconate solution is 1.5mol / L, and the concentration of boric acid solution is 1mol / L, and spray drying adopts centrifugal spray drier, and the rotating speed of centrifugal atomizing w...
Embodiment 2
[0049] A kind of preparation method of superfine ferric boride, it is the following steps:
[0050](1) after ferrous gluconate solution and boric acid solution are mixed, spray drying, obtain spray-dried material, the mol ratio of ferrous gluconate solution and boric acid is 1:1.02;
[0051] (2) Sintering the spray-dried material in a methane atmosphere, the sintering time is 10h, and the sintering temperature is 1200°C to react to obtain the reduced material;
[0052] (3) Continue to feed carbon dioxide into the reducing material, and react at a temperature of 850° C. for 2 hours to obtain a sintered material;
[0053] (4) The sintered material is subjected to jet crushing, screening and vacuum packaging to obtain superfine iron boride.
[0054] The concentration of described step (1) ferrous gluconate solution is 3mol / L, and the concentration of boric acid solution is 2mol / L, and spray drying adopts centrifugal spray drier, and the rotating speed of centrifugal atomization ...
Embodiment 3
[0062] A kind of preparation method of superfine ferric boride, it is the following steps:
[0063] (1) after ferrous gluconate solution and boric acid solution are mixed, spray drying, obtain spray-dried material, the mol ratio of ferrous gluconate solution and boric acid is 1:1.015;
[0064] (2) Sintering the spray-dried material in a methane atmosphere, the sintering time is 8h, and the sintering temperature is 1000°C to react to obtain the reduced material;
[0065] (3) Continue to feed carbon dioxide into the reducing material, and react at a temperature of 780° C. for 3 hours to obtain a sintered material;
[0066] (4) The sintered material is subjected to jet crushing, screening and vacuum packaging to obtain superfine iron boride.
[0067] The concentration of described step (1) ferrous gluconate solution is 2mol / L, and the concentration of boric acid solution is 1.2mol / L, and spray drying adopts centrifugal spray drier, and the rotating speed of centrifugal atomizati...
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