公开(公告)号：US4554144A

公开(公告)日：1985-11-19

申请号：US568707

申请日：1984-01-06

Applicant: Fernando Ore'

Inventor： Fernando Ore'

IPC: C01B25/238 ,  C01B25/16

CPC classification number: C01B25/238

Abstract: Magnesium and aluminum impurities are removed from aqueous phosphoric acid by treatment with a fluorine material and an alkali metal containing material in such a manner that the atomic ratio of fluorine to aluminum is adjusted so that it is greater than about 2 and the alkali metal plus magnesium to aluminum atomic ratio to a value no greater than about 2. In one embodiment the fluorine to aluminum ratio is below about 11, preferably between about 4 and about 8. By controlling such atomic ratios in the limits prescribed, a more purified aqueous phosphoric acid can be produced having a substantial reduction in the magnesium and aluminum content thereof. The process is useful for wet-process phosphoric acids. The process is also particularly useful for acids having low P.sub.2 O.sub.5 content and/or high aluminum concentration. The purification process does not require evaporation for the removal of impurities, as for example fluorine as silicon tetrafluoride.

Abstract translation: 通过用含氟材料和含碱金属的材料处理氟磷与铝的原子比使其大于约2，碱金属加镁，从磷酸水溶液中除去镁和铝杂质 铝原子比为不大于约2.在一个实施方案中，氟与铝的比率低于约11，优选约4至约8.通过将所述原子比控制在规定的限度内，将更纯化的磷酸水溶液 可以制造其镁含量和铝含量显着降低。 该方法可用于湿法磷酸。 该方法对于具有低的P2O5含量和/或高的铝浓度的酸也是特别有用的。 净化过程不需要蒸发去除杂质，例如氟作为四氟化硅。

公开(公告)号：US4260584A

公开(公告)日：1981-04-07

申请号：US910163

申请日：1978-05-26

Applicant: Fernando Ore ,  John D. Ellis ,  James H. Moore

Inventor： Fernando Ore ,  John D. Ellis ,  James H. Moore

IPC: B01D9/00 ,  B01D19/02 ,  B01J16/00 ,  B01J19/18 ,  C01B25/22 ,  C01B25/223 ,  C01B25/225 ,  C01B25/226 ,  C01B25/222

CPC classification number: C01B25/226 ,  B01D19/02 ,  B01D9/0018 ,  B01J16/00 ,  B01J19/1868 ,  C01B25/2204 ,  C01B25/2235 ,  C01B25/225

Abstract: The invention comprises a multi-vessel reaction apparatus useful for reacting phosphate rock and sulfuric acid in which the reaction slurry undergoes intra- and inter- vessel circulation (preferably through a draft tube). The solution portion of the slurry in a first vessel or set of vessels (the "dissolver") is preferably maintained at at lower sulfate ion concentration and the solution portion of the slurry in the second vessel or system of vessels (the "crystallizer") is preferably maintained at a positive sulfate ion concentration. Also preferred are means for maintaining the second vessel or set of vessels at a reduced pressure. Most preferred is that means be included in at least one said vessel for incorporating a crystal modifier (e.g. a sulfonic acid, a sulfonic acid salt, tall oil fatty acids or alkoxylated or esterified tall oil fatty acids) in the crystallizer. The system can be used in the anhydrite, hemihydrate or gypsum types of processes.

Abstract translation: 本发明包括用于使磷酸盐岩和硫酸反应的多容器反应装置，其中反应浆料经受血管内和血管间循环（优选通过引流管）。 第一容器或一组容器（“溶解器”）中的浆液的溶液部分优选保持在较低的硫酸根离子浓度，并且浆液在第二容器或容器系统（“结晶器”）中的溶液部分 优选维持在正硫酸根离子浓度。 还优选的是用于在减压下维持第二容器或容器组的装置。 最优选的是，该方法包括在至少一个所述容器中，用于在结晶器中引入结晶改性剂（例如磺酸，磺酸盐，妥尔油脂肪酸或烷氧基化或酯化的妥尔油脂肪酸）。 该系统可用于无水石膏，半水合物或石膏类型的工艺。

公开(公告)号：US4853201A

公开(公告)日：1989-08-01

申请号：US217186

申请日：1988-07-11

Applicant: Fernando Ore ,  Thomas E. Richards

Inventor： Fernando Ore ,  Thomas E. Richards

IPC: C01B25/229

CPC classification number: C01B25/2295

Abstract: P.sub.2 O.sub.5 values occluded in the crystals which are precipitated during the hemihydrate process for manufacturing phosphoric acid are recovered by dissolving and recrystallizing the hemihydrate crystals as dihydrate crystals in an acidic environment having a P.sub.2 O.sub.5 concentration of from about 0.1% to about 10% and a free sulfate concentration in the range of about 0.1% to about 10%. Water is used to wash the dihydrate filter cake, and the filtrate from this wash is used to redissolve the hemihydrate crystals. The free sulfate values are preferably supplied to the dihydrate crystallizer as sulfuric acid.

Abstract translation: 在用于制造磷酸的半水合物过程中沉淀的晶体中吸收的P2O5值通过在半胱氨酸晶体作为二水合物晶体在P2O5浓度为约0.1％至约10％的酸性环境中溶解并重结晶而回收，并且将游离硫酸盐 浓度在约0.1％至约10％的范围内。 水用于洗涤二水合物滤饼，并使用该洗涤液的滤液再溶解半水合物晶体。 游离硫酸值优选作为硫酸供应至二水合物结晶器。

公开(公告)号：US4377560A

公开(公告)日：1983-03-22

申请号：US282466

申请日：1981-07-13

Applicant: Fernando Ore'

Inventor： Fernando Ore'

IPC: C01B7/19 ,  C01B25/223 ,  C01B25/235 ,  C01B25/16

CPC classification number: C01B25/235 ,  C01B25/223 ,  C01B7/191

Abstract: A process for producing low aluminum content phosphoric acid from high aluminum matrix comprises digesting the matrix in phosphoric acid; adding a flocculant to consolidate gelatinous or fine undigested solids; separating the flocculated solids from the mother liquid comprising monocalcium phosphate; acidifying the monocalcium phosphate with sulfuric acid to precipitate solid calcium sulfate and simultaneously adding at least one sodium or potassium compound or both to co-precipitate some of the soluble fluoride with the gypsum; separating the product phosphoric acid from the precipitated solids; recycling part of the lower fluoride content phosphoric acid back to the digestion step; and, aging the remainder of the product phosphoric acid until a precipitate of aluminum fluorophosphate forms and separating the precipitate to produce a low aluminum content phosphoric acid. Additional fluorine (e.g., a fluoride compound) can be added to accellerate formation of the aluminum fluorophosphate.

Abstract translation: 从高铝基质生产低含铝磷酸的方法包括在磷酸中消化基质; 加入絮凝剂以固化凝胶状或细小的未消化的固体; 从含有单磷酸钙的母液中分离出絮凝固体; 用硫酸酸化磷酸一钙以沉淀固体硫酸钙，同时加入至少一种钠或钾化合物或两者以使一些可溶性氟化物与石膏共沉淀; 将产物磷酸与沉淀的固体分离; 将部分氟化物含量较低的磷酸回收回消化步骤; 并且将剩余的产物磷酸老化直到形成氟磷酸铝的沉淀物并分离沉淀物以产生低含铝磷酸。 可以加入额外的氟（例如氟化合物）以氟化磷酸铝的形成。

公开(公告)号：US4284614A

公开(公告)日：1981-08-18

申请号：US145641

申请日：1980-05-01

Applicant: Fernando Ore

Inventor： Fernando Ore

IPC: C01B25/225 ,  C01B25/226 ,  C01B25/238 ,  C01B25/46 ,  C01B25/22

CPC classification number: C01B25/225 ,  C01B25/226 ,  C01B25/238

Abstract: High quality phosphoric acid is produced from phosphate rock and high alumina pebble which is a byproduct of phosphate rock mining operations. The rock or pebble with or without comminution is digested in phosphoric and sulfuric acid and the resultant phosphoric acid contains the metallic ions normally present in the treated rock and pebble. The metallic ions are then extracted from the acid by ion exchange with a water-immiscible organic sulphonic acid compound (preferably in the presence of an organophosphate or phosphonate). After phase separation the organic phase containing the extracted metallic ions can be regenerated. The process is especially useful when the digestion is done at a P.sub.2 O.sub.5 concentration and temperature which produces calcium sulfate hemihydrate.

Abstract translation: 高品质的磷酸由磷酸盐岩和高铝石卵石生产，这是磷酸盐岩开采作业的副产品。 有或没有粉碎的岩石或卵石在磷酸和硫酸中消化，所得磷酸含有通常存在于处理过的岩石和卵石中的金属离子。 然后通过与水不混溶的有机磺酸化合物（优选在有机磷酸盐或膦酸盐存在下）离子交换，从酸中提取金属离​​子。 相分离后，可以再生含有提取的金属离子的有机相。 当P2O5浓度和产生硫酸钙半水合物的温度进行消化时，该方法特别有用。

公开(公告)号：USRE31629E

公开(公告)日：1984-07-10

申请号：US083890

申请日：1979-10-11

Applicant: James L. Bradford ,  Fernando Ore

Inventor： James L. Bradford ,  Fernando Ore

IPC: C01B25/234 ,  C01B25/238 ,  C22B3/40

CPC classification number: C22B3/0095 ,  C01B25/234 ,  C01B25/238 ,  Y02P10/234

Abstract: Water immiscible organic acid phosphates used in conjunction with water immiscible organic sulfonic acids results in an improved process for the purification of phosphoric acid. An increase in the extraction of ionic metallic impurities and a decrease in the extraction of P.sub.2 O.sub.5 values from the aqueous phosphoric acid phase .[.is.]. .Iadd.are .Iaddend.observed in the improved solvent extraction process.

公开(公告)号：US4277448A

公开(公告)日：1981-07-07

申请号：US909899

申请日：1978-05-26

Applicant: Fernando Ore ,  John D. Ellis ,  James H. Moore

Inventor： Fernando Ore ,  John D. Ellis ,  James H. Moore

IPC: B01J16/00 ,  C01B25/223 ,  C01B25/225 ,  C01F11/46 ,  C01B25/22

CPC classification number: B01J16/00 ,  C01B25/223 ,  C01B25/225

Abstract: Phosphoric acid is prepared from phosphate rock and sulfuric acid by using a reaction train comprising a dissolving slurry and a crystallization slurry maintained at different sulfate levels. Both inter and intra vessel circulation are used at high rates to minimize reagent concentration gradients and temperature gradients and provide a suitable crystallization environment. Preferably, the intra vessel circulation is substantially in plug flow, as through a draft tube.

Abstract translation: 通过使用包含溶解浆料和维持在不同硫酸盐水平的结晶浆料的反应系，由磷酸盐岩和硫酸制备磷酸。 以高速率使用血管内和血管内循环以最小化试剂浓度梯度和温度梯度，并提供合适的结晶环境。 优选地，血管内循环基本上是流动的，如通过引流管。

公开(公告)号：US4243637A

公开(公告)日：1981-01-06

申请号：US840791

申请日：1977-10-11

Applicant: James L. Bradford ,  Fernando Ore

Inventor： James L. Bradford ,  Fernando Ore

IPC: C01B25/238 ,  C22B60/02 ,  C01G43/00 ,  C01G43/02

CPC classification number: C01B25/238 ,  C22B60/026

Abstract: Impure phosphoric acid containing uranium values is pretreated with a water immiscible organic sulfonic acid, preferably in conjunction with a water immiscible organic acid phosphate compound, for extraction of ionic metallic impurities and organic impurities to produce pretreated phosphoric acid containing uranium values. Pretreated phosphoric acid is contacted with a water immiscible extractant comprising an organic uranium-extracting agent, preferably an organophosphorus compound, dissolved in a water immiscible organic diluent to produce uranium-depleted phosphoric acid and uranium-enriched extractant. Uranium is recovered from the uranium-enriched extractant.

Abstract translation: 含有不纯的含铀价值的磷酸用水不混溶的有机磺酸预处理，优选与水不混溶的有机酸式磷酸盐化合物结合，用于萃取离子金属杂质和有机杂质以产生含有铀值的预处理磷酸盐。 将预处理的磷酸与包含溶解在与水不混溶的有机稀释剂中的有机铀提取剂，优选有机磷化合物的水不混溶的萃取剂接触以产生贫铀磷酸和富铀萃取剂。 从富铀萃取剂中回收铀。

公开(公告)号：US4053564A

公开(公告)日：1977-10-11

申请号：US688265

申请日：1976-05-20

Applicant: James L. Bradford ,  Fernando Ore'

Inventor： James L. Bradford ,  Fernando Ore'

IPC: C01B25/238 ,  C01B25/16

CPC classification number: C01B25/238 ,  Y10S423/14

Abstract: Water immiscible organic acid phosphates used in conjunction with water immiscible organic sulfonic acids results in an improved process for the purification of phosphoric acid. An increase in the extraction of ionic metallic impurities and a decrease in the extraction of P.sub.2 O.sub.5 values from the aqueous phosphoric acid phase is observed in the improved solvent extraction process.

公开(公告)号：US4140748A

公开(公告)日：1979-02-20

申请号：US703139

申请日：1976-07-07

Applicant: Fernando Ore

Inventor： Fernando Ore

IPC: C01B25/22 ,  C01B25/16 ,  C01F1/00 ,  C01F5/00 ,  C22B26/20

CPC classification number: C01B25/22

Abstract: Phosphate rock and sulfuric acid are reacted to produce phosphoric acid and calcium sulfate by means of the hemihydrate wet process. In this improved process, the calcium sulfate hemihydrate is crystallized from solution in the presence of an organic sulfonic acid or a derivative thereof. The organic sulfonic acid or its derivative improves the growth of the calcium sulfate hemihydrate crystals and thus improves the filtration rate of the slurry produced in this improved process.

Abstract translation: 通过半水合物湿法使磷酸盐岩和硫酸反应生成磷酸和硫酸钙。 在该改进方法中，硫酸钙半水合物在有机磺酸或其衍生物存在下从溶液中结晶。 有机磺酸或其衍生物改善了硫酸钙半水合物晶体的生长，因此提高了在该改进方法中产生的浆料的过滤速率。