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    • 1. 发明授权
    • Method of defluorinating phosphates
    • 氟化磷酸盐的方法
    • US4405575A
    • 1983-09-20
    • US371333
    • 1982-04-23
    • Albert E. Henderson
    • Albert E. Henderson
    • A23K1/175C01B25/32C05B1/00C01F1/00C01B25/16C01F5/00C05B11/04
    • C01B25/328A23K20/26C05B1/00Y10S71/03
    • This invention comprises a method for removing fluorine from natural phosphates, superphosphate materials and wet process phosphoric acids starting materials comprising(a) admixing rock phosphate having a fluorine content above that desired with an acid mixture within the range of rock:acid mixture of about 0.8 to 1 and 1:1.4 by weight;(b) said acid mixture being substantially concentrated phosphoric acid and concentrated sulfuric acid in a range of phosphoric:sulfuric of about 1:1 to 5:1 by weight;(c) said admixing being at a temperature in the range of 215.degree. to 265.degree. F. while adding water in an amount of up to about 12% by weight of the total mixture and then subjecting the above charge;(d) in a first heating stage adding (1) recycle in an amount substantially of recycle to charge of 1:1 to 10:1 by weight (2) and water while heating to a temperature in the range of 300.degree. F. to 400.degree. F. for a period of time up to about 6 minutes;(e) and in a second heating stage, maintaining the temperature in the range of 400.degree. to 600.degree. F. for a period of time of up to about 6 mimutes, and then;(f) quickly cooling the resulting product above to a temperature range below about 300.degree. F. to 200.degree. F. while neutralizing to about 1 to 6% free acid and with addition of at least sufficient amount of water to have water of hydration of substantially 2 to 9% by weight in the final product;(g) and, crushing the above resulting product to a desired granular size and separating and returning smaller fine particles as recycle.
    • 本发明包括从天然磷酸盐,过磷酸盐材料和湿法磷酸起始材料中除去氟的方法,其包括(a)将具有高于所需值的氟含量的磷酸盐与酸混合物混合在约0.8的岩石:酸混合物的范围内 至1和1:1.4; (b)所述酸混合物是基本浓缩的磷酸和浓硫酸的重量比为约1:1至5:1的磷酸:硫酸; (c)所述混合物在215-265°F的温度范围内,同时加入最多达总混合物重量的约12%的水,然后对上述电荷进行处理; (d)在第一加热阶段中,加入(1)基本上循环量为1:1至10:1(重量)和水的循环量,同时加热到300°F的温度至 400°F,时间长达约6分钟; (e),在第二加热阶段,将温度保持在400〜600°F的范围内,时间可达6乇左右。 (f)将所得产物快速冷却至低于约300°F至200°F的温度范围,同时中和至约1至6%游离酸,并加入至少足够量的水以使水合水 在最终产品中基本上为2至9重量% (g),并将上述所得产物粉碎成所需的颗粒尺寸,并分离和返回较小的微粒作为再循环。