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公开(公告)号：US4479923A
公开(公告)日：1984-10-30
申请号：US511386
申请日：1983-07-06
IPC分类号： C01B25/225 , C01B25/32 , C01B25/16 , C01B15/16 , C01B25/26
CPC分类号： C01B25/225 , C01B25/322
摘要： Phosphate rock, including low grade phosphate ore, is treated to recover phosphoric acid and other valuable products by a series of steps including contacting phosphate ore with a weak phosphoric acid to form a suspension of at least a portion of the slimes contained in the ore so that the slimes can be separated from the ore, and separating the slimes to provide a deslimed phosphate ore. Deslimed phosphate rock is solubilized with phosphoric acid to convert at least a portion of the calcium contained in the rock and form a solution of monocalcium phosphate and phosphoric acid. After removal of solids, this solution can be treated with sulfuric acid in a gypsum crystallizer to form gypsum and the phosphoric acid product wherein filterable gypsum crystals are obtained by maintaining a total SO.sub.3 content of 1.5-4 wt. % in a first crystallizer and neutralizing the SO.sub.3 in a second crystallizer. In other aspects of the invention, at least a portion of the phosphoric acid produced may be recycled to convert additional ore and the slime suspension may be treated to recover the weak acid recovered from the suspension. Further, wash water from the gypsum filter may be recycled to the desliming stage, the filtrate from the deslimer may be cycled to the acidulation reactor and monocalcium phosphate may be recovered as a separate product from phosphoric acid and connected to other useful products.
摘要翻译： 包括低品位磷矿石在内的磷酸盐岩通过一系列步骤处理磷酸和其他有价值的产品，包括使磷矿与弱磷酸接触，形成矿石中至少一部分泥浆的悬浮液 泥浆可以与矿石分离，并分离泥浆以提供去矿磷酸盐矿石。 用磷酸溶解去离子磷酸盐岩以转化岩石中所含的钙的至少一部分，形成磷酸一钙和磷酸的溶液。 去除固体后，该溶液可以在石膏结晶器中用硫酸处理以形成石膏和磷酸产物，其中通过保持总SO 3含量为1.5-4wt。获得可过滤的石膏晶体。 在第一结晶器中的％，并在第二结晶器中中和SO 3。 在本发明的其它方面，所生产的磷酸的至少一部分可以再循环以转化另外的矿石，并且可以处理粘泥悬浮液以回收从悬浮液中回收的弱酸。 此外，来自石膏过滤器的洗涤水可以再循环到脱盐阶段，来自去淤泥的滤液可以循环到酸化反应器，并且磷酸一钙可作为与磷酸分离的产物回收并连接到其它有用的产物。
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公开(公告)号：US4393032A
公开(公告)日：1983-07-12
申请号：US338999
申请日：1982-01-12
IPC分类号： C01B25/225 , C01B25/32 , C01B25/16 , C01B15/16 , C01B25/26
CPC分类号： C01B25/322 , C01B25/225
摘要： Phosphate rock, including low grade phosphate ore, is treated to recover phosphoric acid and other valuable products by a series of steps including contacting phosphate ore with a weak phosphoric acid to form a suspension of at least a portion of the slimes contained in the ore so that the slimes can be separated from the ore, and separating the slimes to provide a deslimed phosphate ore. Deslimed phosphate rock is solubilized with phosphoric acid to convert at least a portion of the calcium contained in the rock and form a solution of monocalcium phosphate and phosphoric acid. After removal of solids, this solution can be treated with sulfuric acid in a gypsum crystallizer to form gypsum and the phosphoric acid product wherein filterable gypsum crystals are obtained by maintaining a total SO.sub.3 content of 1.5-4 wt. % in a first crystallizer and neutralizing the SO.sub.3 in a second crystallizer. In other aspects of the invention, at least a portion of the phosphoric acid produced may be recycled to convert additional ore and the slime suspension may be treated to recover the weak acid recovered from the suspension. Further, wash water from the gypsum filter may be recycled to the desliming stage, the filtrate from the deslimer may be cycled to the acidulation reactor and monocalcium phosphate may be recovered as a separate product from phosphoric acid and connected to other useful products.
摘要翻译： 包括低品位磷矿石在内的磷酸盐岩通过一系列步骤处理磷酸和其他有价值的产品，包括使磷矿与弱磷酸接触，形成矿石中至少一部分泥浆的悬浮液 泥浆可以与矿石分离，并分离泥浆以提供去矿磷酸盐矿石。 用磷酸溶解去离子磷酸盐岩以转化岩石中所含的钙的至少一部分，形成磷酸一钙和磷酸的溶液。 去除固体后，该溶液可以在石膏结晶器中用硫酸处理以形成石膏和磷酸产物，其中通过保持总SO 3含量为1.5-4wt。获得可过滤的石膏晶体。 在第一结晶器中的％，并在第二结晶器中中和SO 3。 在本发明的其它方面，所生产的磷酸的至少一部分可以再循环以转化另外的矿石，并且可以处理粘泥悬浮液以回收从悬浮液中回收的弱酸。 此外，来自石膏过滤器的洗涤水可以再循环到脱盐阶段，来自去淤泥的滤液可以循环到酸化反应器，并且磷酸一钙可作为与磷酸分离的产物回收并连接到其它有用的产物。
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3.发明授权Preparation of monocalcium phosphate and/or phosphoric acid from phosphate rock 失效从磷酸盐岩中制备磷酸一钙和/或磷酸
公开(公告)号：US4435370A
公开(公告)日：1984-03-06
申请号：US306856
申请日：1981-09-29
CPC分类号： C01B25/30 , C01B25/225 , C01B25/328 , C01F11/22 , C05B7/00
摘要： Monocalcium phosphate, phosphoric acid and/or potassium phosphate, calcium fluoride and gypsum are produced in a process involving acidulation of phosphate rock with phosphoric acid, and wherein monocalcium phosphate dissolved in phosphoric acid is formed during acidulation. In important features, insolubles and impurities are removed and a portion of the monocalcium phosphate may be separated and recovered. Alkali metal ion is added to the solution to form alkali metal fluosilicate, such as K.sub.2 SiF.sub.6, is separated and hydrolyzed with calcium ion to form CaF.sub.2 and the solution is recycled as RH.sub.2 PO.sub.4 /H.sub.3 PO.sub.4 for further reaction with fluorides, where R is alkali metal. A portion of the MCP/H.sub.3 PO.sub.4 solution and/or crystallized monocalcium phosphate can then be reacted with potassium sulfate, potassium bisulfate, or mixtures thereof, to form KH.sub.2 PO.sub.4 or KH.sub.2 PO.sub.4 /H.sub.3 PO.sub.4 solutions, and gypsum or with H.sub.2 SO.sub.4 to produce phosphoric acid. The remaining monocalcium phosphate/phosphoric acid solution can be reacted with sulfuric acid to produce phosphoric acid product and the recycle phosphoric acid required in the phosphate rock acidulation step.
摘要翻译： 磷酸磷酸钙，磷酸和/或磷酸钾，氟化钙和石膏是在磷酸盐酸化磷酸盐岩的过程中生产的，其中在酸化过程中形成溶解在磷酸中的磷酸一钙。 在重要特征中，去除了不溶物和杂质，并且可以分离和回收一部分磷酸一钙。 将碱金属离子加入到溶液中以形成碱金属氟硅酸盐如K 2 SiF 6，用钙离子分离并水解形成CaF 2，并将溶液作为RH 2 PO 4 / H 3 PO 4再循环，以进一步与氟化物反应，其中R为碱金属。 然后可以将一部分MCP / H 3 PO 4溶液和/或结晶的一磷酸钙与硫酸钾，硫酸氢钾或其混合物反应，以形成KH 2 PO 4或KH 2 PO 4 / H 3 PO 4溶液，石膏或与H 2 SO 4反应生成磷酸。 剩余的磷酸一磷酸盐/磷酸溶液可以与硫酸反应生成磷酸产物和磷酸盐酸化步骤中需要的再循环磷酸。
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公开(公告)号：US3956464A
公开(公告)日：1976-05-11
申请号：US135297
申请日：1971-04-19
CPC分类号： C01B25/46 , C01B25/301 , C05B7/00
摘要： Potassium phosphates useful as fertilizer materials, are produced by the reaction of phosphate rock or a solubilized form thereof, concentrated sulfuric acid and potassium hydrogen sulfate wherein the potassium hydrogen sulfate is added in a controlled manner and preferably in admixture with at least a portion of the sulfuric acid, the precipitated calcium sulfate precipitate is removed and the filtrate processed for recovery of the potassium phosphates. In further embodiments, high-sulfate containing filtrates are treated to lower the sulfate ion content of the products and effect partial neutralization by any of several methods such as by treatment thereof with fresh phosphate rock or source of calcium ion such as calcium oxide, alternatively or successively, and the resulting solution is used as a fertilizer, or liquids are removed and the solids are dried and/or dehydrated for recovery of the potassium phosphate compounds. Also methods are provided for the addition of nitrogen values.
摘要翻译： 可用作肥料材料的磷酸钾通过磷酸盐岩或其溶解形式，浓硫酸和硫酸氢钾的反应产生，其中硫酸氢钾以受控的方式加入，优选与至少一部分 硫酸，除去沉淀的硫酸钙沉淀物，处理滤液以回收磷酸钾。 在另外的实施方案中，处理含高硫酸盐的滤液以降低产物的硫酸根离子含量并通过几种方法中的任何一种方法进行部分中和，例如通过用新鲜的磷酸盐岩或钙离子源如氧化钙处理，或者或 将所得溶液用作肥料，或者除去液体，并将固体干燥和/或脱水以回收磷酸钾化合物。 还提供了用于添加氮值的方法。
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公开(公告)号：US4268492A
公开(公告)日：1981-05-19
申请号：US64182
申请日：1979-08-06
摘要： Alkali metal fluosilicate is used as an intermediate reactant in a process for the production of hydrochloric acid and an alkali metal sulfate from sulfuric acid and an alkali metal chloride. The process includes the reaction of alkali metal fluosilicate with sulfuric acid to produce alkali metal sulfate and H.sub.2 SiF.sub.6, the latter being reacted with alkali metal chloride to produce HCl and alkali metal fluosilicate. The resulting hydrochloric acid may be converted to anhydrous hydrogen chloride. A continuous process for the production of hydrochloric acid and of alkali metal sulfate such as potassium sulfate from an alkali metal fluosilicate material is also disclosed.
摘要翻译： 在从硫酸和碱金属氯化物制备盐酸和碱金属硫酸盐的方法中使用碱金属氟硅酸盐作为中间体反应物。 该方法包括碱金属氟硅酸盐与硫酸反应生成碱金属硫酸盐和H 2 SiF 6，后者与碱金属氯化物反应产生HCl和碱金属氟硅酸盐。 所得盐酸可以转化为无水氯化氢。 还公开了从碱金属氟硅酸盐材料生产盐酸和碱金属硫酸盐如硫酸钾的连续方法。
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公开(公告)号：US4328196A
公开(公告)日：1982-05-04
申请号：US190850
申请日：1980-09-25
CPC分类号： C01D5/00 , C01B25/301 , C01B33/186 , C01D9/00 , C01F11/22 , C01P2006/80
摘要： Alkali metal-containing salt products selected from the group consisting of alkali metal dihydrogen phosphate, alkali metal sulfate, alkali metal nitrate, and mixtures thereof, together with alkaline earth metal fluoride, are produced from alkali metal fluosilicate by the steps of:(a) reacting alkali metal fluosilicate with alkaline earth metal ion in an aqueous solution to form alkali metal hydroxide and solid alkaline earth metal fluoride with SiO.sub.2 ;(b) separating the solid alkaline earth metal fluoride and SiO.sub.2 and recovering as useful products;(c) reacting the remaining alkali metal hydroxide solution with a mineral acid selected from the group consisting of phosphoric acid, sulfuric acid, nitric acid, and mixtures thereof, at a temperature in the range of about 30.degree.-100.degree. C. until the reaction is complete; and(d) recovering the alkali metal-containing product.Also provided by this invention is a continuous system for conducting this reaction whereby mother liquors may be recycled and the acid reused in the process, and wherein mineral acid is recovered from which anhydrous HCl can be produced.
摘要翻译： 由碱金属氟硅酸盐由碱金属氟硅酸盐制备选自碱金属磷酸二氢盐，碱金属硫酸盐，碱金属硝酸盐及其混合物的碱金属盐产物，其步骤为：（a） 使碱金属氟硅酸盐与碱土金属离子在水溶液中反应，形成碱金属氢氧化物和固体碱土金属氟化物与SiO2; （b）分离固体碱土金属氟化物和SiO 2并作为有用产物回收; （c）将剩余的碱金属氢氧化物溶液与选自磷酸，硫酸，硝酸及其混合物的无机酸在约30℃-100℃的温度下反应，直到 反应完成 和（d）回收含碱金属的产物。 本发明还提供了一种用于进行该反应的连续系统，由此母液可以再循环并且酸在该方法中重复使用，并且其中回收无机酸可从其中产生无水HCl。
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公开(公告)号：USRE29458E
公开(公告)日：1977-10-25
申请号：US597180
申请日：1975-07-18
CPC分类号： C01B25/301 , C05B7/00
摘要： Fertilizer materials, especially potassium dihydrogen phosphate, are produced by the reaction of phosphate rock or a solubilized form thereof, such as mono calcium phosphate, dicalcium phosphate, etc., concentrated sulfuric acid, potassium hydrogen sulfate and, optionally fresh or recycle phosphoric acid, the resulting mixture is filtered to remove the calcium sulfate precipitate and the potassium dihydrogen phosphate is recovered from the filtrate, either by concentration and filtration or by extraction with an organic solvent.
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公开(公告)号：US3998935A
公开(公告)日：1976-12-21
申请号：US545554
申请日：1975-01-30
摘要： Potassium sulfate (K.sub.2 SO.sub.4) is prepared by contacting potassium chloride with an aqueous solution containing potassium bisulfate at a temperature of about 65.degree.-110.degree. C., cooling the solution and permitting the potassium sulfate to crystallize from solution.
摘要翻译： 通过在约65-110℃的温度下使氯化钾与含有硫酸氢钾的水溶液接触来制备硫酸钾（K 2 SO 4），冷却溶液并允许硫酸钾从溶液中结晶。
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公开(公告)号：US4371512A
公开(公告)日：1983-02-01
申请号：US231361
申请日：1981-02-03
摘要： Alkali metal sulfates are produced from an aqueous solution containing alkali metal hydrogen sulfate which comprises contacting the aqueous solution of alkali metal hydrogen sulfate with a hydrophilic solvent, the hydrophilic solvent being effective to extract at least a portion of the sulfuric acid formed as the alkali metal hydrogen sulfate is converted to alkali metal sulfate in the solution, together with at least a portion of the water present; permitting the alkali metal sulfate solid to crystallize; and recovering the solid alkali metal sulfate product. The hydrophilic solvent may then be extracted and separated from the sulfuric acid with a hydrophobic solvent and both solvents can be recovered and recycled.
摘要翻译： 碱金属硫酸盐由含有碱金属硫酸氢盐的水溶液制备，其包括使碱金属硫酸氢盐的水溶液与亲水性溶剂接触，所述亲水溶剂有效提取至少一部分形成为碱金属的硫酸 硫酸氢盐与溶液中的至少一部分水一起转化为溶液中的碱金属硫酸盐; 允许碱金属硫酸盐固体结晶; 并回收固体碱金属硫酸盐产物。 然后可以用疏水性溶剂将亲水性溶剂萃取并与硫酸分离，并且可以回收和再循环两种溶剂。
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公开(公告)号：US4191734A
公开(公告)日：1980-03-04
申请号：US888038
申请日：1978-03-20
IPC分类号： C01B25/225 , C01B25/237 , C01B25/30 , C05B11/08 , C01B25/22
CPC分类号： C01B25/303 , C01B25/225 , C01B25/2375 , C05B11/08
摘要： Substantially fluoride-free phosphoric acid is produced by the acidulation of phosphate rock with sulfuric acid wherein the acidulation reaction is conducted in the presence of added potassium as K.sub.2 O bearing compounds, e.g. KHSO.sub.4, K.sub.2 SO.sub.4, KH.sub.2 PO.sub.4 or KOH, and additional silica, to precipitate fluorides and silica as potassium silicofluoride and then removed on separation of the gypsum formed. Optionally, additional silica may be added to the phosphoric acid solution recovered after precipitation and removal of the gypsum, to precipitate additional fluoride as potassium silicofluoride to further purify the phosphoric acid. In a further embodiment sufficient potassium may be added along with additional silica in the acidulation step to produce potassium dihydrogen phosphate and phosphoric acid as additional products. The phosphoric acid and potassium dihydrogen phosphate are recovered substantially free from fluoride contamination and the reaction is carried out in the substantial absence of fluorine evolution into the atmosphere. Also disclosed is a process for conducting a conventional phosphoric acid facility to produce phosphoric acid and gypsum wherein defluorination of the phosphoric acid recovered is achieved by silicon dioxide and K.sub.2 O addition and the fluorides are removed from the system, the process including steps for production of pure phosphoric acid and potassium dihydrogen phosphate.
摘要翻译： 通过用硫酸酸化磷酸盐岩产生基本上不含氟化物的磷酸，其中酸化反应在加入的K 2存在下作为带有K2O的化合物，例如， KHSO 4，K 2 SO 4，KH 2 PO 4或KOH和另外的二氧化硅，以氟硅酸钠和二氧化硅的形式沉淀，然后在形成的石膏分离后除去。 任选地，可以在沉淀和除去石膏之后回收的磷酸溶液中加入另外的二氧化硅，以沉淀另外的氟化硅作为氟硅酸钾以进一步纯化磷酸。 在进一步的实施方案中，在酸化步骤中可以连同另外的二氧化硅一起加入足量的钾，以产生磷酸二氢钾和磷酸作为附加产物。 基本上没有氟化物污染物回收磷酸和磷酸二氢钾，并且基本上没有氟进入大气中进行反应。 还公开了一种用于进行常规磷酸设备来生产磷酸和石膏的方法，其中通过二氧化硅和K 2 O添加实现回收的磷酸的脱氟，并且从体系中除去氟化物，该方法包括生产纯的 磷酸和磷酸二氢钾。
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