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    • 52. 发明授权
    • Process for making alkali metal phosphate solutions containing little
fluorine
    • 制造含少量氟的碱金属磷酸盐溶液的方法
    • US4640824A
    • 1987-02-03
    • US682053
    • 1984-12-14
    • Gunther SchimmelReinhard Gradl
    • Gunther SchimmelReinhard Gradl
    • C01B25/237C01B25/30C01B25/46C01B25/16
    • C01B25/46C01B25/308
    • The disclosure relates to a process for making alkali metal phosphate solutions containing little fluorine from pre-purified alkali metal phosphate solutions obtained from crude phosphoric acid by extracting the acid with an organic solvent being immiscible or only partially miscible with water, scrubbing the crude extract with water or an alkali metal solution, re-extracting the phosphoric acid from the scrubbed extract with the use of an aqueous alkali metal solution while establishing an alkali metal/P-molar ratio equal to or larger than 1:1, and separating the resulting organic phase from the pre-purified alkali metal phosphate solution obtained.To this end, the disclosure provides:(a) for the pre-purified alkali metal phosphate solution to be stirred at 60.degree.-120.degree. C. into a compound of an alkaline earth metal Me.sup.2+ with a solubility in water at 20.degree. C. of more than 0.01 mol Me.sup.2+ /1, alkaline earth metal compounds with a solubility in water of less than 5 g/l being used in the form of particles of which more than 50% have a size of less than 8 .mu.m, for the whole to be reacted over a period of 0.5 to 4 hours, and for the resulting precipitate to be separated from the alkali metal phosphate solution so purified, and(b) for the alkaline earth metal compound necessary for effecting the defluorination to be suspended or dissolved in the alkali metal phosphate solution needed for effecting the re-extraction, and for the reaction between the alkali metal phosphate solution and alkaline earth metal compound to be effected in the mixing zone of the re-extraction unit.
    • 本公开涉及通过用与水不混溶或仅与水部分混溶的有机溶剂萃取酸来从粗磷酸获得的预纯化碱金属磷酸盐溶液中制备含少量氟的碱金属磷酸盐溶液的方法,用 水或碱金属溶液,使用碱金属水溶液从洗涤的提取物中再次提取磷酸,同时确定等于或大于1:1的碱金属/ P摩尔比,并分离所得的有机物 从预纯化的碱金属磷酸盐溶液获得。 为此,本公开内容提供:(a)将预纯化的在60-120℃下搅拌的碱金属磷酸盐溶液转变成在20℃在水中溶解度的碱土金属Me2 +的化合物。 大于0.01mol Me2 + / 1,在水中的溶解度小于5g / l的碱土金属化合物以超过50%的尺寸小于8μm的颗粒的形式使用,对于 整个反应0.5至4小时,并将所得沉淀物从纯化的碱金属磷酸盐溶液中分离出来,(b)对于实现脱氟所必需的碱土金属化合物悬浮或溶解 在进行再提取所需的碱金属磷酸盐溶液中,以及在再提取单元的混合区域中进行的碱金属磷酸盐溶液和碱土金属化合物之间的反应。
    • 56. 发明授权
    • Decolorization and purification of crude wet-process phosphoric acid
    • 粗制湿法磷酸的脱色和纯化
    • US4330516A
    • 1982-05-18
    • US203490
    • 1980-11-03
    • Louis Winand
    • Louis Winand
    • C01B25/234C01B25/235C01B25/46E01B25/16
    • C01B25/461C01B25/235C01B25/462
    • Crude wet-process phosphoric acid prepared by mineral acid acidulation of uncalcined phosphate rock and containing contaminating amounts of organic impurities is purified and decolorized into an essentially colorless food-grade phosphoric acid, by (i) preliminarily decolorizing such crude acid, (ii) liquid-liquid extracting said predecolorized acid with an essentially water-insoluble organic extractant, (iii) back-extracting the extracted phosphoric acid with an aqueous phase, (iv) concentrating the back-extracted aqueous phosphoric acid solution at elevated, coloration-developing temperatures, and (v) then subjecting the concentrated solution which results to a final decolorization, to afford a purified, essentially colorless phosphoric acid solution.
    • 通过无矿酸酸化未煅烧的磷酸盐岩并含有污染量的有机杂质制备的粗制湿法磷酸被纯化并脱色成基本上无色的食品级磷酸,通过(i)预先使这种粗酸脱色,(ii)液体 - 用基本上不溶于水的有机萃取剂提取所述预脱色酸,(iii)用水相反萃取萃取的磷酸,(iv)在升高的着色显影温度下浓缩反萃取的磷酸水溶液, 和(v)然后使得到最终脱色的浓缩溶液得到纯化的基本无色的磷酸溶液。
    • 60. 发明授权
    • Purification and conversion of phosphoric acid to ammonium phosphates
    • 磷酸与磷酸铵的纯化和转化
    • US4236911A
    • 1980-12-02
    • US92771
    • 1979-11-08
    • John F. McCullough
    • John F. McCullough
    • C01B25/46C05B7/00C22B60/02C01B15/16
    • C22B60/0282C01B25/463C05B7/00Y02P10/212
    • A method of purifying filter-grade wet-process phosphoric acid, then converting the purified phosphoric acid directly to ammonium phosphate without first concentrating the phosphoric acid. The wet-process phosphoric acid is treated with a mixture of ammonia or an ammonium salt and acetone near or at the boiling point of the mixture. Solids are separated from the phosphoric acid liquid phase. The solids are a mixture of metal phosphates, gypsum, and fluosilicates. Adhering phosphoric acid is washed free of the solids with fresh acetone. Wash liquor is combined with purified phosphoric acid. Gaseous ammonia is added to the phosphoric acid-acetone extract in the ratio necessary to produce either monoammonium phosphate (MAP) or diammonium phosphate (DAP). Ammonium phosphate is filtered from the acetone-water mother liquor, then, depending on the level of ammonium phosphate left in the mother liquor and the type of ammonium phosphate produced (MAP or DAP), the mother liquor is treated in one of several ways. If DAP is produced and the amount of DAP left dissolved in the mother liquor is sufficiently low, the acetone is distilled from the mother liquor and recycled and the aqueous waste either discarded or used for filter cake wash water in the phosphoric acid plant. If necessary, the amount of ammonium phosphate left with the aqueous waste can be reduced to nil by adding lime to the mother liquor. This converts ammonium phosphate to dicalcium phosphate and ammonia. The precipitated calcium phosphate is separated and returned to the phosphoric acid plant. Ammonia and acetone are co-distilled and return to the process.
    • 一种净化过滤级湿法磷酸的方法,然后将纯化的磷酸直接转化成磷酸铵,而无需首先浓缩磷酸。 湿法磷酸在混合物的沸点附近或沸点下用氨或铵盐和丙酮的混合物处理。 固体与磷酸液相分离。 固体是金属磷酸盐,石膏和氟硅酸盐的混合物。 用新鲜的丙酮洗涤不含固体的粘附磷酸。 洗涤液与纯化的磷酸结合。 按照制备磷酸二氢铵(MAP)或磷酸二氢铵(DAP)所需的比例,向磷酸 - 丙酮提取液中加入气态氨。 从丙酮 - 水母液中过滤磷酸铵,然后根据母液中残留的磷酸铵水平和产生的磷酸铵(MAP或DAP)的类型,母液以几种方式之一进行处理。 如果产生DAP并且残留在母液中的DAP的量足够低,则从母液中蒸馏丙酮并再循环,并将废水丢弃或用于磷酸设备中的滤饼洗涤水。 如有必要,通过向母液中加入石灰,残留在废水中的磷酸铵的量可以减少到零。 这将磷酸铵转化为磷酸二钙和氨。 将沉淀的磷酸钙分离并返回到磷酸装置。 将氨和丙酮共同蒸馏并返回该过程。