EP0109327B1 - Procédé de récupération globale de l'uranium, de l'yttrium, du thorium et des terres rares contenus dans un minerai phosphate au cours de la préparation d'acide phosphorique par voie humide - Google Patents

Procédé de récupération globale de l'uranium, de l'yttrium, du thorium et des terres rares contenus dans un minerai phosphate au cours de la préparation d'acide phosphorique par voie humide Download PDF

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Publication number
EP0109327B1
EP0109327B1 EP83402114A EP83402114A EP0109327B1 EP 0109327 B1 EP0109327 B1 EP 0109327B1 EP 83402114 A EP83402114 A EP 83402114A EP 83402114 A EP83402114 A EP 83402114A EP 0109327 B1 EP0109327 B1 EP 0109327B1
Authority
EP
European Patent Office
Prior art keywords
attack
yttrium
phosphoric acid
silica
uranium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP83402114A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0109327A1 (fr
Inventor
Jean Fava
André Lambert
Jean-Paul Tognet
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Rhodia Chimie SAS
Original Assignee
Rhone Poulenc Chimie SA
Rhone Poulenc Chimie de Base SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Rhone Poulenc Chimie SA, Rhone Poulenc Chimie de Base SA filed Critical Rhone Poulenc Chimie SA
Publication of EP0109327A1 publication Critical patent/EP0109327A1/fr
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Publication of EP0109327B1 publication Critical patent/EP0109327B1/fr
Expired legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02Obtaining thorium, uranium, or other actinides
    • C22B60/0204Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0217Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
    • C22B60/0252Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
    • C22B60/0278Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries by chemical methods
    • C22B60/0282Solutions containing P ions, e.g. treatment of solutions resulting from the leaching of phosphate ores or recovery of uranium from wet-process phosphoric acid
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02Obtaining thorium, uranium, or other actinides
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00Obtaining rare earth metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02Obtaining thorium, uranium, or other actinides
    • C22B60/0291Obtaining thorium, uranium, or other actinides obtaining thorium

Definitions

  • the present invention relates to a process for the overall recovery of uranium, yttrium, thorium and rare earths contained in a phosphate ore during the preparation of phosphoric acid by wet process.
  • phosphate ores used for the manufacture of phosphoric acid contain significant amounts of uranium, yttrium, thorium and rare earths.
  • yttrium represents in quantity approximately half of the whole.
  • silica hinders the filtration of the attack slurry during the separation of the gypsum and the phosphoric acid.
  • silica can prove to be a nuisance in the subsequent stages of a process for manufacturing phosphoric acid, in particular during liquid-liquid extractions.
  • the object of the invention is to further improve the solubilization of rare earths, of yttrium and of thorium on attack without harming the subsequent progress of the process for the manufacture of phosphoric acid.
  • the process according to the invention for the overall recovery of uranium, yttrium, thorium and rare earths contained in a phosphate ore, during the preparation of phosphoric acid by wet process, is characterized in that during the acid attack of the ore, optionally carried out in the presence of silica, aluminum is added to the attack medium in trivalent form and / or a ferric compound in such a way that the amount of aluminum and / or iron present in this attack medium varies between 0.8% and 1.5% by weight expressed as A1 2 0 3 and / or Fe 2 O 3 relative to the ore subjected to attack.
  • the process of the invention makes it possible to reach percentages of solubilization of the above-mentioned elements greater than those of silica while keeping a shorter filtration time.
  • the attack on the phosphate ore which can be carried out more particularly with sulfuric acid takes place under known and usual conditions of temperature and concentration of acids.
  • Aluminum or iron can be introduced either with the attack acid or in the attack slurry.
  • Aluminum is added in the form of a salt of this element, for example in the form of a sulfate, a phosphate, an alumina or any other precursor capable of releasing the aluminum ion under the conditions of 'attack. It is the same for iron which can in particular be added in the form of sulfate, of oxide, such as ferric oxide.
  • aluminum and iron can be added in the form of aluminum-calcium phosphates containing iron such as Thies phosphates and Ta ⁇ ba fines, so that the proportions of aluminum and iron in the attack medium are within the limits indicated in claim 1.
  • the amounts of aluminum, iron and silica used depend on the type of ore processed, the attack conditions that one wishes to observe and the type of acid that one wishes to obtain.
  • the resulting porridge is filtered.
  • a residue or primary gypsum is obtained in the case of a sulfuric attack and a phosphoric acid solution.
  • the whole solid obtained after this filtration is called gypsum here.
  • the phosphoric acid solution notably includes uranium in almost the entire quantity present in the starting ore and a significant proportion of yttrium, thorium and rare earths.
  • the acid is brought into contact with an organic phase comprising a di (alkylphenyl) phosphoric acid, dissolved in an inert organic solvent and in the presence of a trialkylphosphine oxide.
  • organic phase is reextracted using a solution containing hydrofluoric acid and phosphoric acid.
  • a Kouribga phosphate ore of the following composition 31.07% P 2 0 5 ; 344 ppm yttrium; 140 ppm uranium; Ce0 2 : 42 ppm; LaC0 3 : 132 ppm; Tb 4 O 7 : 9 ppm; Yb 2 O 3 : 21 ppm.
  • This mineral is attacked with sulfuric acid without any additives, then in another series of tests in the presence of precipitated silica in variable quantity and in a third series of tests in the presence of aluminum sulphate and d '' a mixture of aluminum sulphate and silica in variable quantity.
  • the amount of aluminum is calculated as AI z 0 3 .
  • the filtration times given were obtained by measuring the filtration time on buchner of the attack slurry and the filtration time of the cake after addition of a representative quantity of washing water. of the quantity of washing water used industrially. The sum of these two times for each test corresponds to the time indicated in Table 1.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Geology (AREA)
  • Materials Engineering (AREA)
  • Environmental & Geological Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
EP83402114A 1982-11-10 1983-10-28 Procédé de récupération globale de l'uranium, de l'yttrium, du thorium et des terres rares contenus dans un minerai phosphate au cours de la préparation d'acide phosphorique par voie humide Expired EP0109327B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8218910A FR2535702B1 (fr) 1982-11-10 1982-11-10 Procede de recuperation globale de l'uranium, de l'yttrium, du thorium et des terres rares contenus dans un minerai phosphate au cours de la preparation d'acide phosphorique par voie humide
FR8218910 1982-11-10

Publications (2)

Publication Number Publication Date
EP0109327A1 EP0109327A1 (fr) 1984-05-23
EP0109327B1 true EP0109327B1 (fr) 1986-12-30

Family

ID=9279094

Family Applications (1)

Application Number Title Priority Date Filing Date
EP83402114A Expired EP0109327B1 (fr) 1982-11-10 1983-10-28 Procédé de récupération globale de l'uranium, de l'yttrium, du thorium et des terres rares contenus dans un minerai phosphate au cours de la préparation d'acide phosphorique par voie humide

Country Status (15)

Country Link
US (1) US4636369A (fi)
EP (1) EP0109327B1 (fi)
JP (1) JPS6058175B2 (fi)
KR (1) KR890004520B1 (fi)
AU (1) AU559423B2 (fi)
BR (1) BR8306163A (fi)
CA (1) CA1222376A (fi)
DE (1) DE3368689D1 (fi)
ES (1) ES8406374A1 (fi)
FI (1) FI74491C (fi)
FR (1) FR2535702B1 (fi)
GR (1) GR78756B (fi)
IL (1) IL70180A (fi)
MA (1) MA19949A1 (fi)
ZA (1) ZA838268B (fi)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BR8707200A (pt) * 1987-12-23 1989-08-15 Pirelli Brasil Sintese de supercondutores a partir da xenotima
JP3731786B2 (ja) * 1998-02-19 2006-01-05 三菱電機株式会社 ワイヤ放電加工装置
CN100439239C (zh) * 2006-10-12 2008-12-03 贵州宏福实业开发有限总公司 降低磷酸中稀土含量的方法
CN101451200B (zh) * 2007-11-29 2011-04-20 北京有色金属研究总院 一种从磷矿中富集回收稀土的方法
CN103184356B (zh) * 2011-12-28 2014-12-17 有研稀土新材料股份有限公司 一种稀土磷矿的处理方法和富集稀土的方法
CN113332957A (zh) * 2021-06-09 2021-09-03 江西理工大学 改性磁性掺杂材的制备方法及其从稀土矿废水中回收稀土元素的方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0031793A2 (de) * 1979-12-03 1981-07-08 Schweizerische Aluminium AG Verfahren zur Herstellung von Phosphorsäure, bei dem Uran in einer gewinnbaren Form erhalten wird

Family Cites Families (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2425573A (en) * 1940-11-28 1947-08-12 Soddy Frederick Separation of thorium and the rareearth group from minerals
US2761758A (en) * 1950-08-04 1956-09-04 Ray S Long Process for recovery of uranium
US2789879A (en) * 1950-11-15 1957-04-23 Kaufman David Recovery of uranium from phosphoric acid
US2819145A (en) * 1952-10-15 1958-01-07 Robert F Mccullough Metal value recovery from leached zone material
US2859092A (en) * 1953-02-05 1958-11-04 Richard H Bailes Solvent extraction process for the recovery of metals from phosphoric acid
FR1104263A (fr) * 1954-05-07 1955-11-17 Comptoir Des Phosphates De L A Procédé pour la séparation, par précipitation, de l'uranium à partir d'une liqueur fortement acide
US2743156A (en) * 1954-08-06 1956-04-24 Max C Metziger Uranium recovery process
US2841467A (en) * 1955-01-18 1958-07-01 Robert F Mccullough Method for recovery of mineral values from leached zone material
US2990244A (en) * 1957-12-24 1961-06-27 Keith B Brown Extraction of thorium and uranium values from acid leach liquors
FR1585270A (fi) * 1968-09-11 1970-01-16
US3937783A (en) * 1974-02-21 1976-02-10 Allied Chemical Corporation Recovery of fluorine, uranium and rare earth metal values from phosphoric acid by-product brine raffinate
DE2652766A1 (de) * 1976-03-09 1977-09-22 Robert Dr Michel Verfahren zur herstellung von phosphorsaeure aus phosphatgestein
US4284614A (en) * 1976-04-13 1981-08-18 Occidental Petroleum Corp. Process for production of high purity phosphoric acid from high alumina phosphate pebble rock
FR2423545A1 (fr) * 1977-08-25 1979-11-16 Minemet Rech Sa Procede pour la recuperation de l'uranium contenu dans des solutions phosphatees
JPS5855086B2 (ja) * 1978-04-18 1983-12-08 三菱マテリアル株式会社 リン酸液中に溶存するウランの回収方法
US4374805A (en) * 1978-05-26 1983-02-22 Uranium Recovery Corporation Reductants for reducing metals in acid media
FR2515630B1 (fr) * 1981-10-30 1985-10-04 Rhone Poulenc Spec Chim Procede d'extraction et de separation de l'uranium, du thorium et des terres rares par traitement de solutions aqueuses de chlorures de ces elements

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0031793A2 (de) * 1979-12-03 1981-07-08 Schweizerische Aluminium AG Verfahren zur Herstellung von Phosphorsäure, bei dem Uran in einer gewinnbaren Form erhalten wird

Also Published As

Publication number Publication date
US4636369A (en) 1987-01-13
FR2535702A1 (fr) 1984-05-11
FI834107A0 (fi) 1983-11-09
IL70180A0 (en) 1984-02-29
DE3368689D1 (en) 1987-02-05
FI74491C (fi) 1988-02-08
FI834107A (fi) 1984-05-11
KR890004520B1 (ko) 1989-11-10
KR840006508A (ko) 1984-11-30
FI74491B (fi) 1987-10-30
CA1222376A (fr) 1987-06-02
ZA838268B (en) 1984-09-26
JPS6058175B2 (ja) 1985-12-18
MA19949A1 (fr) 1984-07-01
AU559423B2 (en) 1987-03-12
EP0109327A1 (fr) 1984-05-23
IL70180A (en) 1987-10-30
ES527101A0 (es) 1984-07-01
FR2535702B1 (fr) 1986-09-12
ES8406374A1 (es) 1984-07-01
JPS59116126A (ja) 1984-07-04
AU2111383A (en) 1984-05-17
GR78756B (fi) 1984-10-02
BR8306163A (pt) 1984-06-12

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