JPS58501994A - Refining of uranium-containing concentrates - Google Patents

Refining of uranium-containing concentrates

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JPS58501994A
JPS58501994A JP82503397A JP50339782A JPS58501994A JP S58501994 A JPS58501994 A JP S58501994A JP 82503397 A JP82503397 A JP 82503397A JP 50339782 A JP50339782 A JP 50339782A JP S58501994 A JPS58501994 A JP S58501994A
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uranium
liquid
refining
suspension
temperature
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ジユ−ベ−ル・フイリツプ
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ウラニウム・ペシネ・ユジンヌ・キユルマン
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Priority claimed from FR8121637A external-priority patent/FR2516498A1/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B15/00Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
    • C01B15/04Metal peroxides or peroxyhydrates thereof; Metal superoxides; Metal ozonides; Peroxyhydrates thereof
    • C01B15/047Metal peroxides or peroxyhydrates thereof; Metal superoxides; Metal ozonides; Peroxyhydrates thereof of heavy metals
    • C01B15/0475Metal peroxides or peroxyhydrates thereof; Metal superoxides; Metal ozonides; Peroxyhydrates thereof of heavy metals of 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
    • 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

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  • Organic Chemistry (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • Manufacturing & Machinery (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

(57)【要約】本公報は電子出願前の出願データであるため要約のデータは記録されません。 (57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

【発明の詳細な説明】 ウラン含有精鉱の精製処理 不発明は不簡物特にジルコニウム及び/又は・・フニウムを含有するウラン含有 精鉱の精製方法に係る。本発明方法は、先ず厳腎な調整量で導入される酸性剤に よってウラン含有精鉱を処理し次に過酸化水素で処理して不純な過酸化ウランン 形仮イしめる第1段階と第1段階で得らfた不納なウラン@有面相を酸性剤で処 理して精製さnたウラン含有゛柩を得ること全確保する第2段階とを新規な風合 ぜとして含む。[Detailed description of the invention] Refining of uranium-containing concentrates Non-inventive materials include uranium-containing materials, especially those containing zirconium and/or... Concerning the method for refining concentrate. The method of the present invention first involves introducing an acidic agent in a strictly controlled amount. Therefore, the uranium-containing concentrate is treated and then treated with hydrogen peroxide to remove impure uranium peroxide. The first step is to fix the shape, and the non-conforming uranium phase obtained in the first step is treated with an acidic agent. The second step is to ensure that the refined uranium-containing coffin is obtained through processing and a new texture. Included as

ウラン含有精鉱がウランの最終面目製の際ンこ明ら刀・7c好ましくない存在で ある多数の不両物全言有すること又は含有する可能位がるることは丁でに以前ρ 1ら矧られている。Uranium-containing concentrate is an undesirable presence when making the final face of uranium. To have or to have the possibility of containing a number of different words 1 is limited.

前記のヌロさウラン含有精鉱の処理て於いては通常、先ず二弁1.ジン二云1− ・昌)下−≧ぞ 慟伴暑ウラニル塩の形状のウランを投出ゼしめ、次に過敏化水素全使用して退散 化物O状態でウラン?沈殿でくるっ専門薔は、前記の如き処理について記載し、 不納物が存在するため十分に魂粋なウラン化合物を得るのは雌しいと解説してい る。In the treatment of the above-mentioned slimy uranium-containing concentrate, usually two valves 1. Jin Niyun 1- ・Masashi) lower −≧zo Inject uranium in the form of uranyl salt, then use all sensitizing hydrogen to escape. Uranium in the chemical O state? For specialized roses that are produced by precipitation, the above-mentioned treatment is described, He explains that it is unwise to obtain a sufficiently refined uranium compound because there are undeliverables. Ru.

フラン含有精鉱の処理に最もよく使用さnり万云二、R−正aLT’rの” ’ l’he extractive rvletallurgy of Ura: 1ix” 1971手数 。Most commonly used in the treatment of furan-containing concentrates. l'he extractive rvletallurgy of Ura: 1ix” 1971 moves.

コロラド・スクール・オブ・マイン・リサーチ・インステイテユート。Colorado School of Mine Research Institute.

247 − 248ページ、及び、” Proceeding of the  Intsrna−tional Conference on the Paa ceftxl uses of 、Atomic ErLergy”英国、14 巻、141−143ページ (1955年)に収載のE、 L、Z I#Ib1 ER(D ” 粗ウラン含有生成物の化学的精製に於けるIR階としての過5化 ウランの製造分離”に記載されている。Pages 247-248, and “Proceeding of the Intsrna-tional Conference on the Paa ceftxl uses of, Atomic ErLergy” UK, 14 Volume, pages 141-143 (1955) E, L, Z I#Ib1 ER(D'' Per5ation as an IR phase in the chemical purification of crude uranium-containing products Uranium Production Separation”.

これらの論文によれば、ウランを含有する不純溶液〒のウランを沈殿させるとき 存在する不罰吻全俗解状態に維持することに1脇的には可能であるが、得られる ウラン含有沈殿物は前記沈殿物の分離が行なわれる際に無視し得ない量の不純物 全保持しておシこの事実は長時間の後洗浄を行なっても変わらない。According to these papers, when precipitating uranium in an impure solution containing uranium Although it is possible to maintain the existing state of non-punishment and general understanding, it is possible to obtain The uranium-containing precipitate contains a non-negligible amount of impurities when the precipitate is separated. This fact remains true even after a long period of post-washing.

90ち、過酸化ウランの沈殿及び洗浄によれば、銀、ヒ素、アルンガン、モリブ デン、バナジウム、ナトリウム、ニッケル、アンチモン、スズ、亜鉛の如き不N ’aH十分に除去され得るが、鉄、リン、ケイ素については別の精製処理を予め 実施しない限9十分に妥当な除去は確保さ!1.ない。90. According to the precipitation and washing of uranium peroxide, silver, arsenic, arungan, molyb Non-N such as den, vanadium, sodium, nickel, antimony, tin, zinc ’aH can be sufficiently removed, but iron, phosphorus, and silicon require separate purification treatment in advance. Unless implemented 9 sufficiently reasonable removal is ensured! 1. do not have.

ウラン含有精鉱が更にジルコニウム及び/′又は/・フニワムの如き別の不純物 を含有する場合、これらの不純物は通常、それらを含む水溶液が過酸化水素で処 理でれる際ウランと同時に沈殿する。そのため、得られた過款化ウランから杉エ ネルギ利用のだめの十分に純粋なウランを得ることができない。The uranium-containing concentrate may also contain other impurities such as zirconium and/' or/. These impurities are usually removed when aqueous solutions containing them are treated with hydrogen peroxide. It precipitates at the same time as uranium when it is extracted. Therefore, from the obtained superstructured uranium, cedar It is not possible to obtain sufficiently pure uranium for energy use.

ウラン含有精鉱の前記の如き常用の処理方法に基いた改良方法もまた専門書に記 載されている。これらの方法は、浸出不徘物全同時に含むウラン含有駿水浴液〃 )ら過酸化ウランを沈殿せしむべく過識化X素を使用するまでは等しく、L種以 上の特定不純物を除去するための方法が互いに異なる。Improvements to the above-mentioned conventional treatment methods for uranium-containing concentrates are also described in specialized texts. It is listed. These methods require a uranium-containing water bath solution containing all leached impurities at the same time. ) until the use of superimposed X element to precipitate uranium peroxide; The methods for removing the above specific impurities are different from each other.

例えば、まνf、5HABBIR及びに、E−TA:viE による’ Rep ort of InvestigatiOns 7931 of US Bur eau of :!viines1974”に収載の“過酸化水素によるウラン の沈殿”に於いては、モリブデン質不純物とバナジウム質不純物と1外〈金偏1 づウランの酸性水溶液を室温にて過酸化不素を用い溶液のpdを3乃至6の範囲 の種々の値に調整しつつ4時間に亘って処理する過酸化ウランの生成方法が記載 さnている。著者等はこの論文中で、十分にN製された過酸化ウラン沈殿物を得 るには該浴液のpH’i 3.5乃至5に維持する必要があると明言している。For example, νf, 5HABBIR and 'Rep' by E-TA:viE ort of InvestigationOns 7931 of US Bur eau of:! "Uranium produced by hydrogen peroxide" listed in "Viines 1974" In the "precipitation", molybdenum impurities, vanadium impurities, An acidic aqueous solution of uranium is heated at room temperature using hydrogen peroxide to bring the pd of the solution to a range of 3 to 6. Describes a method for producing uranium peroxide, which is processed over a period of 4 hours while adjusting to various values of I'm here. In this paper, the authors obtained a fully N-made uranium peroxide precipitate. It clearly states that it is necessary to maintain the pH'i of the bath solution between 3.5 and 5.

前記の如き方法がジルコニウム及び/又はハフニウムのスロさ特殊な不純物を含 有する不純なウラン含有精鉱に使用さnた場合、これらの特殊不純物は適職化7 に素導入の際にウランと共に沈殿するので結果的には不純な退散化2ランしか生 成され得な存在不純物に関していっそう進歩した別の方法が米国特許第2,77 0,521号に記載されていS、、この方法は、硫識ウラニル溶液を処理するた めて先ず炭酸カルシウムを用いて溶液のpHを3乃至4に調整して鉄、@、クロ ム、コバルト、ニッケル。The method described above may contain special impurities such as zirconium and/or hafnium. When used in impure uranium-containing concentrates, these special impurities are When the element is introduced, it precipitates with uranium, so in the end only 2 impure degenerates are produced. Another method that is more advanced with respect to impurities present is disclosed in U.S. Pat. No. 2,777. No. 0,521, this method is used to treat sulfuric uranyl solutions. First, adjust the pH of the solution to 3 to 4 using calcium carbonate to remove iron, @, and chlorine. cobalt, nickel.

マンガン、モリブデンの如き不別物を沈殿さぞ、次に不純物沈殿物を分離してか ら不純物が少なくなったウラン含有浴液に過酸化水素全導入し沈殿媒体9温度を 65°C以下pH金2.5乃至3.5に維得して溶液刀工ら過酸化ウランを沈殿 ぜしめる。Precipitate the impurities such as manganese and molybdenum, then separate the impurity precipitate. Hydrogen peroxide was completely introduced into the uranium-containing bath liquid with reduced impurities, and the temperature of the precipitation medium was raised to 9. Precipitate uranium peroxide from solution by maintaining pH 2.5 to 3.5 below 65°C Forbidden.

処理すべき硫酸ウラニル浴液が普通の不、副物のみでなく、ジルコニウム及び/ 又はハフニウムから成る不純物をも含有する場合、前記方法は余シ有利でないと 考えられる。筒改なら、炭撃カルシウムに用いて不利物、の選択的沈入を行なう この方法は、ウラン含有溶液中の5O2−イオンの濃度を低下させその結果とし てウラン、ジルコニウム及び/又はノ・フニワムの一部と除去すべき不純物との 共沈を生起し易く、このときに無視し得ないウランの損失が生じるからでるる。The uranyl sulfate bath solution to be treated contains not only ordinary waste and by-products, but also zirconium and/or or also contains impurities consisting of hafnium, the method may be less advantageous. Conceivable. With Tsutsukai, it is used for charcoal calcium to selectively deposit disadvantageous materials. This method reduces the concentration of 5O2- ions in uranium-containing solutions and as a result a part of uranium, zirconium and/or nitride and impurities to be removed. This is because coprecipitation is likely to occur, resulting in a non-negligible loss of uranium.

更に、ジルコニウム及び/又はハフニウムは一部分し刀工不別物と共に沈殿しな いのでウラン含有液に浴屏したでまの残9の部分な過酸化ウランと共に沈殿する でhろう。Additionally, zirconium and/or hafnium may not partially precipitate with the swordsmiths. Inode is precipitated with the remaining 9 parts of uranium peroxide after bathing in the uranium-containing liquid. Let's go.

従って轟業者に提案された公知技術の方法は、ウラン含有液が醗性剤による精鉱 浸出によシ得られたものでるる場合存在不純・物中にジルコニウム及び/又はハ フニウムが含でれるので十分に満足な解決方法とはなり得ないっ例数なら前記の 処理によれば前記の如き特殊不純物のあるものとウランとの同時沈殿が生起され るので核エネルギオり用に必要な稠度テ得るためには後に過酸化ウランの精製処 理を行なう必要かめるからでめる。Therefore, the method of the prior art proposed to Todoroki is that the uranium-containing liquid is mixed with a concentrate using a solubilizing agent. If the product is obtained by leaching, there may be impurities such as zirconium and/or halide present in the product. It cannot be a fully satisfactory solution because it contains funium.If the number of cases is During processing, uranium and special impurities such as those mentioned above will co-precipitate. Therefore, in order to obtain the consistency necessary for nuclear energy use, uranium peroxide must be purified later. You need to do it, so you can do it.

このように、提案された処理がユーザーの要求を充足さくることができないため 出願人は研究の結果、前記の欠点が無く純度が極めて同上したウラン含有液を得 ることが可能なウラン含有精鉱の精製方法全発見しその構成に成功した。In this way, the proposed process cannot satisfy the user's request. As a result of research, the applicant has obtained a uranium-containing liquid that does not have the above-mentioned drawbacks and is extremely pure. We have successfully discovered and constructed a method for refining uranium-containing concentrate.

不縄物?含有しており特に該不別物がシ゛ルコニウム及び/′又はハフニウムか ら成るグループ上構成する元素の少くとも1遣金含むようなウラン含MN鉱を精 製する之めの不発明の万云、・;、過酸化ウランの形成を生起すべく高温哉性水 性探体中での鐘筬化不素による前記精鉱の処理を苫ひ。An unnatural thing? Contains silconium and/or hafnium. Refining uranium-containing MN ore containing at least one of the elements constituting the group consisting of The inventive method of producing... The treatment of the concentrate by fertilization in a sex probe is recommended.

不発明方法の特徴は、第1段階に於いてウランを定1FFJに沈殿イしめ不純物 の全部又は一部を浸出ぜしめる目的で、ワラン言有精鉱全水性媒体yc憑凋させ 、次に戚洗剤全用いて前記、E1孜を發っくりと調整的に酸性化し、得られた叔 住化水性煤不全送散化水素で処理して主としてウランとジルコニウム及び/又は ハフニウムのほぼ全1とを含む沈殿物全形成させ、該沈設物全不純物を含む液相 から分離すること、次に第2段階に於いて、第1段階で得られた沈殿物を酸性剤 で処理してウランを可溶ウラニルイオンに変化させて溶出せしめ、ウラニルイオ ンを含有する液相全ジルコニウム及び/又はハフニウムを含む化合物から形成さ れた同相りjら分離することでるるっ本発明方法で処理される固体状ウラン含有 8砿′r1当菜者が十分に公知のウラン含有鉱石の湿式冶金処理によジ得られた ものである。こ几らの謂繁は通常、大部分がフランから成り多部分が不純物、例 えば銀、ヒ素、アルミニウム、ビスマス、カルシウム、マグぷシウム、マンガン 、モリブデン、バナノウム、ナトリウム、ニッグル、アンチtン−,スズと特に ジルコニウム及び/又はハフニウムから形成されるグループを、構成する金属の 少くとも1棟とから成る固体混合物の状態を石する。 ゛不発明方法で処理され る液体状ウラン含有吉鉱12:固体状ウラン宮有謂鉱中に存在する不純物と同じ 不純物を含有して29、特K、ジルコニウムとハフニウムとから形成さnるグル ープを構成する金属チクくとも1徨含有している。The feature of the uninvented method is that in the first step, uranium is precipitated to a constant concentration of 1 FFJ to eliminate impurities. For the purpose of leaching all or part of the Waran Kogou concentrate, it is impregnated with an entirely aqueous medium Next, E1 was carefully and selectively acidified using all the detergents mentioned above, and the obtained alcoholic acid was Primarily uranium, zirconium and/or A precipitate containing almost all of hafnium is formed, and a liquid phase containing all impurities of the precipitate Then, in the second step, the precipitate obtained in the first step is treated with an acidic agent. treatment to convert uranium into soluble uranyl ions and elute them. liquid phase containing all zirconium and/or hafnium-containing compounds. The solid uranium-containing material treated by the method of the present invention can be 8 翿'r1 was obtained by the well-known hydrometallurgical treatment of uranium-containing ores. It is something. These products usually consist mostly of furan with a large proportion of impurities, e.g. For example, silver, arsenic, aluminum, bismuth, calcium, magpsium, manganese , molybdenum, vananium, sodium, niggle, anti-tin, tin and especially The group formed from zirconium and/or hafnium is the metal that constitutes it. Stone the state of a solid mixture consisting of at least one building.゛Processed by an uninvented method Liquid uranium-containing Yoshimine 12: Same impurities as those present in solid uranium Miya ore. Glue formed from 29, special K, zirconium and hafnium containing impurities It contains at least one amount of metal that makes up the group.

処理の第1段階に於いては、稍製すべさウラン含有精鉱が固体の場合、該精鉱7 を攪拌下に維持された水性媒体中に分散させ、酸性剤で処理される懸濁液を得る 。次に酸性剤を該含浸液中に緩つくりと導入してウランと存在不純物の大部分と を双方とも浸出ぞしめる。酸性剤の暖徐な導入時間lrJ、通常5乃至200分 間であるが、特に10乃至120分間に選択さnる。不純物のH+轟1として決 定される。In the first stage of processing, if the uranium-containing concentrate is solid, the concentrate 7 is dispersed in an aqueous medium maintained under stirring to obtain a suspension that is treated with an acidic agent. . An acidic agent is then slowly introduced into the impregnating solution to remove most of the uranium and impurities present. Both of them are exuded. Gradual introduction time of acidic agent lrJ, usually 5 to 200 minutes time, but in particular 10 to 120 minutes. Determined as impurity H + Todoroki 1 determined.

芙際には導入すべき酸性剤の1はアル刀り性カチ万ン及び/又は同等のカチ万ン に対して決定されるっ不発明方法の第1段:階で導入すべき酸性剤の量は少くと も前記カチ万ンの化学量論的量τ−・10;ノ/) Oil’−’l L子厘珊 ばυIす1.1ノ7工Z−5活Jフ範囲の量が使用される。実際には、導入すべ き酸性剤の量は酸性化後の遊離Hの濃度が少くとも0.01N暑手与+ζ少4堵 魂−0−,−1讃・ 好ましくは少くとも0.INになるように選択さnる。ウ ラン含有精鉱の水性懸濁液に導入される酸性剤の量洸従って、得らnた酸性化媒 体は水性懸濁液の状態に維持さnたり又は場合によっては軽度に混濁した液の状 悪全呈する。後者の場合液は、ウラン含有精鉱中に最初に存在してい友不純吻の 大部分とウランの全1とを溶′S状悪で@有している。One of the acidic agents to be introduced at the time of preparation is an alkaline acid and/or an equivalent acid. The amount of acidic agent to be introduced in the first step of the non-inventive method is determined for The stoichiometric amount of the above-mentioned kachiman τ-・10;ノ/) Oil'-'l An amount in the range 1.1 to 7 is used. Actually, it is necessary to introduce The amount of acidic agent used should be such that the concentration of free H after acidification is at least 0.01N Soul -0-, -1 praise, preferably at least 0. Selected to be IN. cormorant The amount of acidifying agent introduced into the aqueous suspension of orchid-containing concentrate is therefore The body is maintained in an aqueous suspension or, in some cases, in the form of a slightly turbid liquid. exhibit evil. In the latter case, the liquid is initially present in the uranium-containing concentrate and It has most of the uranium and all of the uranium in a molten state.

得られた酸性化媒体が懸濁液であるか溶液であるかに関ゎシ無く、該媒体の温度 は70℃以下に維持されるべく調整される。Regardless of whether the acidified medium obtained is a suspension or a solution, the temperature of the medium is adjusted to be maintained at 70°C or below.

好ましくは該温度は30℃乃至40℃の範囲に維持される。Preferably the temperature is maintained in the range of 30°C to 40°C.

ウラン含有精鉱が溶液の状態である場合、該溶液に固体精鉱と同様の酸性化処理 を行なう。When the uranium-containing concentrate is in a solution state, the solution is subjected to the same acidification treatment as solid concentrate. Do this.

酸性化処理後所望の温度に維持された酸性化水性媒体を次に過酸化水素で処理す る。過酸化水素は過酸化ウランのみを沈殿させるに必要な化学量論的量の少くと も2倍に等しい量で前記媒体中に導入される。The acidified aqueous medium, maintained at the desired temperature after the acidification process, is then treated with hydrogen peroxide. Ru. Hydrogen peroxide has a low stoichiometric amount required to precipitate only uranium peroxide. is also introduced into the medium in an amount equal to twice as much.

過酸化水素の量は過酸化ウランの沈殿に必要な化学量論的量の少くとも1.4倍 に等しく、特に化学量論的量の2倍乃至3倍である。これによシララン含有精鉱 中に最初に存在しておりジルコニウムとハフニウムとから形成されるグループに 属する元素少くとも1種から成る不純物とウランとが同体状に変えられて維持さ れる。The amount of hydrogen peroxide is at least 1.4 times the stoichiometric amount required for precipitation of uranium peroxide. , in particular 2 to 3 times the stoichiometric amount. This is a concentrate containing silarane. A group formed from zirconium and hafnium that was first present in An impurity consisting of at least one element belonging to uranium is changed into a constitutive state and maintained. It will be done.

ウランと少くとも1種のジルコニウム元素及びハフニウム元素とを同体状に変え て維持する処理は当業者が熟知する如く通常はλ5乃至4,5のpHにて行なわ れる。Converting uranium and at least one kind of zirconium element and hafnium element into isoforms As is well known to those skilled in the art, the maintenance treatment is usually carried out at a pH of λ5 to 4.5. It will be done.

pHは水酸化ナトリウム、水酸化カリウム又は水飄化アンモニウムの如きアルカ リ性剤の導入によって調整される。pH is an alkali such as sodium hydroxide, potassium hydroxide or ammonium hydroxide. regulated by the introduction of softening agents.

温度とpHとが選択値に維持されている酸性化媒体に過酸化水素を導入後、この 処理で得られた懸濁液を熟成処理する。熟成処理では懸濁液を最初に選択された 温度範囲で6時間以下好ましくは2乃至4時間攪拌下に維持する。After introducing hydrogen peroxide into the acidifying medium where the temperature and pH are maintained at selected values, this The suspension obtained in the treatment is subjected to an aging treatment. In the aging process, suspension was first selected The temperature is maintained under stirring for up to 6 hours, preferably from 2 to 4 hours.

この最終熟成処理後の懸濁液に対して固液分離処理を行なう。The suspension after this final aging treatment is subjected to solid-liquid separation treatment.

この処理は必要ならば濾過助剤例えばKi≦se1gure即ちケイソウ土を存 在させ当業者に公知の手段例えば濾過、傾瀉、遠心等によって行なわれ得る。分 離後に得られた固相は固相の含浸液を導出すべく十分な量の水又は0.2%過酸 化水素水溶液で洗浄される。This treatment may include filter aids such as Ki≦se1gure, diatomaceous earth, if necessary. This can be done by means known to those skilled in the art, such as filtration, decantation, centrifugation, etc. minutes The solid phase obtained after separation is treated with a sufficient amount of water or 0.2% peracid to derive the solid phase impregnating solution. Washed with an aqueous solution of hydrogen chloride.

第1段階に適用可能な髪形例としては、使用ウラン含有精鉱に関わり無くはるか に再現性の良い純度のウラン含有液を得るために錯生成剤の機能を果すフン化物 イ万ン源を用いて酸性化水性媒体を処理する。この変形例の場合、得られた媒体 が懸濁液の状態でろるか溶液の状態であるかに関わり無く媒体の温度は少くとも 70℃に維持されるべく調整され、好ましくは90に維持された酸性化水性媒体 は次に、フッ化物イオン源により処理される。こCイオン源は例えば存在不純物 のほぼ全部を溶出させ得る化合物i(F 、 NaF 、KF 、 NH4F  、 Na25t F6a>ら成り単独で又は混合物として開用される。錯生成剤 はモル比F/(Zr十Hf)が少くとも1に等しく好ましくは4乃至10になる 量で酸性化水性媒体に導入される。As an example of a hairstyle that can be applied to the first stage, regardless of the uranium-containing concentrate used, Haruka Fluoride acts as a complexing agent to obtain a uranium-containing liquid with good reproducible purity. The acidified aqueous medium is treated using an ion source. For this variant, the resulting medium Regardless of whether the medium is in suspension, solid or solution, the temperature of the medium is at least acidified aqueous medium adjusted to be maintained at 70°C, preferably maintained at 90°C; is then treated with a fluoride ion source. This C ion source, for example, Compound i (F, NaF, KF, NH4F) that can elute almost all of , Na25t, F6a> and can be used alone or as a mixture. complexing agent is such that the molar ratio F/(Zr + Hf) is at least equal to 1 and preferably from 4 to 10. amount is introduced into the acidified aqueous medium.

錯生成剤が導入される量水性媒体の温度は少くとも70℃好ましくは90℃乃至 100℃に維持される。温度が選択匝に維持された酸性化媒体への錯生成剤の導 入後、この処理によシ得られた溶液を熟成処理する。熟成処理では該浴数を最初 に選択さnた温度範囲内で6時間以下好ましくは1乃至4時間攪拌下に維持する 。熟成処理仮し性化浸り牝・地を叱た水溶液を次に60℃未満好ましくは30℃ 乃至40℃の温度に冷却し、次いで過通酸化水素で処理する。過酸化水素は過波 化ウランのみを沈殿させるのに必要な化学童論的量に少くとも等しい1で前記媒 体に導入さnる。特に化学量論的量の2乃至10倍の量が使用される。冷却され た媒体に過収化本素全導入後、この処理風より得られた懸濁液に水酸化ナトリウ ム、本機化カリウム又は水酸化アンモニウムの如きアルカリ性剤を導入してpH を緩つくジと2.5乃至4.5の範囲の選択値に調車する。pH調整後の懸濁液 を次に、60℃未満の温度で6時間以下好ヱしくに2乃至4時間攪拌下に維持し て熟成処理する。The temperature of the aqueous medium in which the complexing agent is introduced is at least 70°C, preferably 90°C to Maintained at 100°C. Introduction of the complexing agent into the acidified medium where the temperature is maintained at a selected temperature. After the addition, the solution obtained by this treatment is subjected to an aging treatment. In the aging process, the number of baths is maintained under stirring for no more than 6 hours, preferably from 1 to 4 hours, within a temperature range selected for . Aging treatment Temporarily immersed in an aqueous solution of the female body at a temperature lower than 60°C, preferably 30°C Cool to a temperature between 40° C. and then treat with hydrogen peroxide. Hydrogen peroxide is too much The amount of said medium is at least equal to the amount necessary to precipitate only uranium chloride. introduced into the body. In particular, amounts of 2 to 10 times the stoichiometric amount are used. cooled After introducing all the super-yielded element into the medium, sodium hydroxide was added to the suspension obtained from this treated air. pH is adjusted by introducing an alkaline agent such as electrolyzed potassium or ammonium hydroxide. The wheel is pulled loosely to a selected value in the range of 2.5 to 4.5. Suspension after pH adjustment is then kept under stirring at a temperature below 60° C. for up to 6 hours, preferably from 2 to 4 hours. and ripening process.

第1段階後の分離洗浄された固相は過酸化ウランと少くと51種のジルコニウム 化合物及び/又はノ・フニウム化合物を含有する沈殿物から形成されておシ、液 相ζ他の不純物の実質的に全部を港解状態で含有している。The separated and washed solid phase after the first stage is uranium peroxide and at least 51 types of zirconium. A liquid formed from a precipitate containing compounds and/or non-funium compounds. Phase ζ contains substantially all of the other impurities in the dissolved state.

処理の第2段階に於いては、第1段階で得られた主としてウランを含む同相をa ′#処理し次に、該面相本来のペースト状のまま、又は、水もしくは再利用液か ら取る水性媒体に念澗芒ぜてから酸性剤で処理する。In the second stage of processing, the homophase containing mainly uranium obtained in the first stage is ’# Treated and then applied with the original paste form or with water or recycled liquid. After soaking it in an aqueous medium, it is treated with an acidic agent.

第2段階に於いて本来の状態又は水性懸濁液の状態のウラン含有固相中に導入さ れる酸性剤の量μ該相中に存在するウランの溶出のみを生起する量に相当する。In the second step, the uranium is introduced into the solid phase in situ or in aqueous suspension. The amount μ of acidic agent used corresponds to the amount that causes only the elution of the uranium present in the phase.

本来の状態又は7に性懸濁゛液形厄後のウラン含有同相が酸性剤の作用を受ける 前に60乃至100’C升ましくは85乃至95℃の温度にフロ熱さnてもよい 。し刀・し乍ら酸性剤の導入後7C7:u熱さnる方が好ましい。後者の場合は ウランの溶解による気体発生を論節し得べく温度上昇が景保lこ行なわr−る。The uranium-containing phase in its original state or in liquid suspension is subjected to the action of acidic agents. It may be heated to a temperature of 60 to 100°C or 85 to 95°C before heating. . It is preferable to heat the solution after introducing the acidic agent. In the latter case In order to prevent gas generation from dissolving uranium, the temperature is increased.

ウランの溶解処理ぼ前記範囲の選択’JAW Vこてよ注化課体七熟成処理する ことにより完了する。この処理には通常は少くとも1時間が必要でるり、好zL <に3乃至5時間が必要でめる。Selection of the scope of uranium dissolution treatment This completes the process. This process usually requires at least an hour or <3 to 5 hours are required.

浴屏及び熟成処理後に狩られた懸濁液に通常、水相中のジルコニウム及び/又は ハフニウム化合物の・磐解度を低下さぞる目おで40℃以下の温度に冷却される 。次に、前記懸濁液を分層処理してウランに富む精製液を収集しジルコニウム化 合物及び/又はハフニウム化合物から成る不倒物を含有する同相を車離し得る。The suspension obtained after bathing and aging usually contains zirconium and/or Hafnium compounds are cooled to a temperature of 40℃ or less, which reduces the degree of oxidation. . Next, the suspension is subjected to layer separation treatment, and the purified liquid rich in uranium is collected and converted into zirconium. The same phase containing a compound and/or a compound consisting of a hafnium compound can be removed.

本発明方法の第1段階及び第2段階の各々で使用される酸性剤は硝駿、硫諷、塩 酸及びフッ化水素酸から成るグループから選択され得る。2つの段階で同じ酸性 剤が使用さnてもよいが好ましくは異なる酸性剤が吏用されしかも2種以上の酸 の混合物から成るのが望ましい。The acidic agent used in each of the first and second stages of the method of the present invention is sulfur, sulfur, and salt. It may be selected from the group consisting of acids and hydrofluoric acids. Same acidity in two stages Although different acidic agents may be used, preferably different acidic agents are used and more than one acidic agent may be used. Preferably, it consists of a mixture of.

このように従来技術pら際立った本発明方法の特徴は第1段階に於いて不純物の 主要部分が溶出除去されることであり、また第2段階の特徴は第1段階で得られ た不純ウランのみが溶解され最終不利物が固体状で味去されることにめる。As described above, the feature of the method of the present invention that stands out from the prior art is that impurities are removed in the first step. The main part is eluted and removed, and the characteristics of the second stage are those obtained in the first stage. Only the impure uranium is dissolved and the final undesirables are removed in solid form.

実際には、本発明によるウラン含有稍鉱の謂製方法は以下の処理を含んで2カ、 これらの処理は遵、読的でめっでもよく不連続的でらってもよい。In fact, the so-called method for producing uranium-containing pyrite according to the present invention includes the following treatments: These processes may be continuous, and may be performed discontinuously.

a)攪拌状態に維持された水性媒体に稍裏すべきウラン含有稍鉱を懸濁させるか 又は処理すべきウラン含有液km入する、b)攪拌された媒体を適温に維持しつ つ調整量の酸性剤を發つく9と導入する、 C)段階b)で得られた水性媒体のpHを2.5乃至4.5の範囲に雄待し過酸 化フランの沈殿のみに必長な化学量論1つ量の少くとも2倍に等しい量の過酸化 水素を該水性媒体に導入する、 d)段階b)及びC)で選択された温度条件及びpH条件下で6時間以下の攪拌 維持によp段階C)で得らfた懸濁液を熟成する、 e)溶出不純物を含有する液と主としてウランを池数化物の形状で含有する面相 とを分離する、 f)段階e)で得らnた同相を洗浄する、g)水又は再利用液から既る水性扉体 にウラン含有同相を、懸濁させる、 ′rL)段階g)で得らnたウランせM付濁液甲で存在フランに河する化学童論 的量以下の酸性剤:/こよシワラン全洛解さぞ、酸性化以前又は散性化中に加熱 する、 l)選択温度下で少くとも1時間攪井軸秀して段階n)で侍られた怠濁液全熟成 する、 J)段階l)で得られた懸濁液全40”C以下の温度に冷却する、k)F4芙ウ ランに冨む液とジルコニウム化合物及び/又はノ・フニウム化合物で・ら成る不 純吻チクくとも1極言Mする面相とを分離する。a) Suspending the uranium-containing ore in an aqueous medium maintained in an agitated state; or km of the uranium-containing liquid to be treated; b) maintaining the stirred medium at a suitable temperature; 9. Introducing an adjusted amount of acidic agent; C) Adjust the pH of the aqueous medium obtained in step b) to a range of 2.5 to 4.5 and add peracid. an amount of peroxide equal to at least twice the stoichiometric amount required only for the precipitation of chlorinated furan; introducing hydrogen into the aqueous medium; d) Stirring for up to 6 hours under the temperature and pH conditions selected in steps b) and C). Aging the suspension obtained in step C) by maintaining e) A liquid containing eluted impurities and a phase containing mainly uranium in the form of chloride. to separate the f) washing the same phase obtained in step e); g) aqueous door body made from water or recycled liquid; suspending the uranium-containing homophase in 'rL) The uranium obtained in step g) is a chemical theory that flows into the uranium present in the suspension liquid A. Acidic agent below the required amount: / Koyo Shiwaran Zenrakukaizo, heat before acidification or during dispersion. do, l) Full ripening of the slurry served in step n) by stirring for at least 1 hour at the selected temperature. do, J) Cooling the suspension obtained in step l) to a temperature below 40"C; k) F4 A compound consisting of a liquid contained in orchid and a zirconium compound and/or a zirconium compound and/or a zirconium compound. Separate the pure-hearted prick from the monotonous face.

変形例によれば段階す、c、dが以下の即く行なわれる。According to a variant, steps c and d are carried out immediately below.

b)攪拌さ′n−た媒体を適温に維持し眉整量の酸性剤を厩つくりと導入する bl )媒体を適温に俄持しフッ化物イ万ン源がら成る錯生成剤を調ヤ量で緩っ く)と導入して不、創動を電化する、 ’1)2)段階b1で得られた媒体を段階 a)及びb)で週択ぢfた温度条沖 下で6時間以下侃拌姫待して該原本を熟成する、 b3 )段階b2で得られた媒体を60”C未満の温度に冷却する、 C)段1階b3で得らr−た水性媒体に過酸化ウランの沈殿のみに必要な化学量 論お量に少くとも等しい量の過酸fヒポ素全導入する、 C1)段階C)で侍られた媒体のpt(を2.5乃至4.5の亘になるまで援つ 〈pと調整する、 d)段階 clで得られた懸濁液を段階b3及びclで選択てnた温度条件及び 旭条件下で6埒間以下ズ芹組片して該懸濁液を熟成する。b) Maintain the stirred medium at an appropriate temperature and introduce a suitable amount of acidic agent. bl) Keep the medium at an appropriate temperature and loosen the complexing agent consisting of a fluoride ion source in a controlled amount. electrification of non-creative power by introducing '1) 2) The medium obtained in step b1 was heated to a temperature range of 100 to 100 ml in steps a) and b). The original is matured by stirring for less than 6 hours under the b3) cooling the medium obtained in step b2 to a temperature below 60”C; C) The chemical amount required for precipitation of uranium peroxide only in the aqueous medium obtained in step 1 b3. introducing at least an amount of hypohyperoxide peroxide, C1) Support the pt of the medium served in step C) until it reaches a range of 2.5 to 4.5. <adjust with p, d) The suspension obtained in step cl is subjected to the selected temperature conditions and in steps b3 and cl. The suspension is matured by cutting it into pieces of not more than 6 square meters under the same conditions.

不発明方法及びその変形例の2つの段階を示ア慨絡図VC遍く符号を伴なった以 下の記載より本発明が更て十分て理解されよう。A schematic diagram VC showing the two stages of the non-inventive method and its variants is shown below with accompanying symbols throughout. The present invention will be more fully understood from the description below.

第1図によればウラン含有精鉱Slは囚に於いて水性媒体に懸濁さnる。水性媒 体は再利用液L□3とL工、との混合物から成り攪拌下に維持されている。According to FIG. 1, uranium-containing concentrate Sl is suspended in an aqueous medium in a container. aqueous medium The body consists of a mixture of recycled liquid L□3 and L□3 and is maintained under stirring.

前記の如く得られた懸濁液L1は次に、ウラン含有樗繁中に最初から存在する不 純物の全部又は一部全浸出イしむべく(B)に於いて緩つくりと尋人される酸性 剤L20により処理6iる。The suspension L1 obtained as described above is then freed from the impurities originally present in the uranium-containing Toshige. Acidic acid which is said to be mild in (B) in order to completely leached out all or part of the pure substance. Treatment 6i with agent L20.

この間、媒体の温度は80°以下に調整されている。During this time, the temperature of the medium is adjusted to 80° or less.

攪拌下で前記温度に維秀された敵性化で・濁放り。は’C)7こ於いて温度とp Hとを調整され過酸化水素水溶液により処理でれる。When the temperature is maintained under stirring, it becomes hostile and becomes cloudy. is 'C) 7. Temperature and p H and can be treated with an aqueous hydrogen peroxide solution.

過酸化水素の活性量は過酸化ウランの形成に必要な化学量甥的量の少くとも1. 4倍に等しい。The active amount of hydrogen peroxide is at least 1.0% of the stoichiometric amount required for the formation of uranium peroxide. Equal to 4 times.

FC)で得られた過酸化ウランの懸濁液L3全■)で熟成処理する。The suspension L3 of uranium peroxide obtained in FC) is subjected to aging treatment.

熟成処理は、初選沢温度範囲で亡澗液全6侍1司以下撹拌下に棄持して成る。The aging process consists of discarding the remaining liquid under stirring at a temperature range of 6 to 1 liter.

熟成処理後に侍らnた懸濁液L4に固液分配処理を笑施して、不、創動含有液L 5とウラン言有稍鉱申に最初に存在していたウランのVXぼ全ftジルコニウム 及び/又はハフニウム不列物と某に含むケーキS、と金得る。After the aging treatment, solid-liquid distribution treatment is performed on the suspension L4 containing the liquid, resulting in a liquid containing liquid L4. 5 and uranium VX, which was originally present in the uranium minerals, almost all ft zirconium and/or a cake S containing hafnium irregularity and a certain amount.

次に(F)Yこ於いてケーそS、る水溶fLLi23で洗浄しケーキs5が含浸 していた不純?Jt導出する液LI3とケーキs6とを得る。Next, in (F)Y, the cake S is washed with water-soluble fLLi23 and the cake s5 is impregnated. Was it impure? A liquid LI3 for deriving Jt and a cake s6 are obtained.

液L5とL6とが混合されて液L□4を構成する。L□4の一部分し□5は(3 )で再利用され、残りの部分L□6は処理サイクル〃1ら卿敷される。Liquids L5 and L6 are mixed to form liquid L□4. A part of L□4 and □5 is (3 ), and the remaining portion L□6 is subjected to processing cycles 〃1 and so on.

ケーキS6は旬に於いて水性再利用液L□8に、@濁され、得られた懸濁液L7 は次に卸ンこ於いて設性液L24によって敵性化される。液L24の酸量はウラ ンの溶出のみに対応する。次に該懸濁液は最高100℃までの温度に加熱される 。Cake S6 was suspended in aqueous reuse liquid L□8 during the season, and the resulting suspension L7 is then turned into an enemy by the setting fluid L24 in the tank. The amount of acid in liquid L24 is Compatible with elution only. The suspension is then heated to a temperature of up to 100°C. .

得られた懸濁液L8は(I)に於いて、■での使用温度と等しい温度で少くとも 1時間熟成処理される。The obtained suspension L8 is heated in (I) at a temperature equal to the temperature used in (■) at least Aged for 1 hour.

熟成処理後に得られた。@濁液L9を分離処理してウランに冨′UNR液L□。Obtained after aging treatment. @Turn the turbid liquid L9 into uranium by separating it and convert it into UNR liquid L□.

と主としてジルコニウ°ム化合物及び/又はハフニウム化合動刃・ら形成δれた 沈殿物Sloとを得る。and mainly formed from zirconium compound and/or hafnium compound moving blade. A precipitate Slo is obtained.

沈殿物S1oを次VtC■に於いて水性液L25で洗浄し、?itL、□と実質 的にウランを含まないケーキS□1とを得る。The precipitate S1o was then washed with aqueous liquid L25 at VtC■, and ? itL, □ and real A cake S□1 containing no uranium is obtained.

ウラン含有液L1oとL□□とを混合して液L□7を得る。αL□7の一部分し □8は(G)で再利用される。残りの部分L□9がウランの改造液に札当する。Uranium-containing liquid L1o and L□□ are mixed to obtain liquid L□7. Part of αL□7 □8 is reused in (G). The remaining portion L□9 is used as a bill for uranium modification fluid.

ケーキS□□ばへjに於いて水εiL、6による再パルプ化(repuipag e)処理を受け懸濁、夜し工2を生じるっ液L12はh)K於いて固1分箱処理 を受ける。Repulping with water εiL, 6 in Cake S□□Bahej e) The treated solution L12, which is suspended and produces a night-time process 2, is h) treated in a solid box for 1 minute at K. receive.

実質的にジルコニウム不純物及び/又はハフニウム不、純物のみから構成さnた 固体S□3は処理サイクル刃ムら除去さn液し□3は囚に於いて再利用さnる。Consisting essentially only of zirconium impurities and/or hafnium impurities. The solid S□3 is removed from the processing cycle and the liquid S□3 is reused in the prison.

髪形方法を示す第2図によnば、ウラン含有清風S□は囚に於いて水性媒体に懸 濁される。水性媒不は再利用液L□3とL□。According to Figure 2, which shows the hairstyle method, uranium-containing Seifu S□ is suspended in an aqueous medium in prison. It becomes cloudy. The aqueous medium is recycled liquid L□3 and L□.

との混合物から構成されて2ρ撹拌下に矩狩さnている。It is composed of a mixture of 2ρn and 2ρn while stirring.

前記の如く得られた。萄濁液L1Σ次にIBIに於いて、ウラン含再精鉱甲に最 初に存在していた不純物の全部又汀一部を浸出イしL・べく酸性剤L20を緩つ くりと導入して処理する。この間媒体の温度は少くとも70°Cに調整される。Obtained as described above. Suspension liquid L1ΣNext, in IBI, the uranium-containing reconcentrate A Loosen the acidic agent L20 by leaching out all or some of the impurities that were initially present. Introduce and process. During this time the temperature of the medium is adjusted to at least 70°C.

前記温度で攪拌下に矩脣さnた敵性化懸濁液L2を(BA) ンこ於いてフッ化 物イオン源刀)ら成る錯生成剤金用いて処理する。The hostile suspension L2 was stirred at the above temperature (BA) and then fluorinated. It is treated using a complexing agent consisting of gold (ion source).

錯生成剤ばL45として調長量で餞つくρと導入さr3る。A complexing agent L45 is introduced as ρ, which thickens in a controlled amount.

錯化により得らnた水性媒体L4□は仄に(bB)に於いて、媒体を初選択温度 範囲で6時間以下攪拌下lこ雄荷する熟双処理業受ける。The aqueous medium L4□ obtained by the complexation is at (bB) at the initial selected temperature of the medium. The product is subjected to a processing operation in which it is unloaded under stirring for less than 6 hours.

熟成処理後の懸濁液L42全CBC)にでいて608禾調り温度1で冷却する。After the aging treatment, the suspension L42 (all CBC) is discharged and cooled at a temperature of 1.

前記温度で攪拌下に維持された懸濁液L43をCC)に於いて調整温度で過酸化 水素導入後L2□で処理する。過酸化水素の活性量は過酸化ウランの形成に必要 な化学X論的士に少くとも等しい。Suspension L43, maintained under stirring at said temperature, is peroxidized in CC) at a controlled temperature. After introducing hydrogen, process with L2□. The active amount of hydrogen peroxide is necessary for the formation of uranium peroxide At least equivalent to a chemist.

(C)で得られた過酸化ウラン懸濁液L3を(CA)に於いて溶液L22を導入 してpMを2.5乃至4.5の値に調整する。Solution L22 was introduced into the uranium peroxide suspension L3 obtained in (C) in (CA). Adjust the pM to a value between 2.5 and 4.5.

(CA)で得らnた適宜化ウラン懸濁液L44ζ次に(2)に於いて、最初に選 択されたph及び温度の範囲で6時間以下攪拌下に維得される熟成処理ケ受ける 。The optimized uranium suspension L44ζ obtained in (CA) is then first selected in (2). subjected to an aging treatment maintained under stirring at a selected pH and temperature range for up to 6 hours; .

熟成処理後に得らnた懸濁液L4を、固液分離に有利な薬品846を任意に存在 さゼて固液分離処理し、不純物を含む液L5とウラン含M楕誠に最初に存在して いたウランのほぼ全量をジルコニウム不純物及び/又は−・フニウム不純物と共 に含むケーキS、とを得る。The suspension L4 obtained after the aging treatment is optionally treated with a chemical 846 that is advantageous for solid-liquid separation. After solid-liquid separation treatment, the impurity-containing liquid L5 and the uranium-containing liquid L5 were initially present. Almost the entire amount of uranium was mixed with zirconium impurities and/or -fnium impurities. We obtain cake S, which contains .

ケーキS5f:次に町に焚いて水溶液L23により況浄しケーキS5の不純含浸 液を導出する液L6とケーキS6とを得る。Cake S5f: Next, burn it in the town and clean it with aqueous solution L23 to impregnate cake S5. A liquid L6 and a cake S6 are obtained.

液り、とL6とが混合され1L14t−構成する。液L工、の一部分は(3)に 戻いて再利用され、別の部分L□6は処理サイクル刀Xらネトへされる。The liquid and L6 are mixed to form 1L14t. Part of the liquid L engineering is in (3) It is returned and reused, and another portion L□6 is sent to the processing cycle.

ケーキS6にG)に於いて再利用X性液L□8に懸濁てれ、得られた懸濁液L7 は次に0に於いて酸性液L24によシ酸性化される。酸の量はウランの溶出のみ に対応する。次に該懸濁液は最高100″Cまでの温度に加熱される。Cake S6 is suspended in reused X liquid L□8 in G), and the resulting suspension L7 is then acidified by acidic liquid L24 at 0 . The amount of acid is only for uranium elution corresponds to The suspension is then heated to a temperature of up to 100''C.

得られた。ε温液L8は(I)K於いて面の使用温度と等しい温度で少くとも1 時間の熟成処理を受ける。Obtained. ε hot liquid L8 is at least 1 at a temperature equal to the working temperature of the surface at (I)K. Subjected to the aging process of time.

熟成処理後に得られた懸濁液り、を、1壜分離に有利な薬品S4□を任意に存在 させて部分離しウランに富む精製液L1oと主としてジルコニウム化合物及び/ 又はノ〜フニウム化合物から形成される沈殿物S1oとを得る。Optionally, a chemical S4□, which is advantageous for separation, is added to the suspension obtained after the aging process. The partially dissociated uranium-rich purified liquid L1o and mainly zirconium compounds and/or Alternatively, a precipitate S1o formed from a no-phnium compound is obtained.

沈殿物SIOを次に卸に於いて水性液L25で洗浄し液LL1とウランを実質的 に含まないケーキSよ□とを得る。The precipitate SIO is then washed with aqueous liquid L25 in a wholesaler to remove substantially all of the uranium from liquid LL1. We get a cake S that does not contain □.

ウラン含有液L とL とを混合して液りよ7を得る。液L工。Mix uranium-containing liquids L and L to obtain liquid 7. Liquid L engineering.

011 の一部分L はC)に於いて再利用され、残りの部分L工、はウラ8 ン友造液に相当する。011 Part L is reused in C), and the remaining part L is back 8 It corresponds to Yuzo liquid.

ケーキS を軸に於いてriC性液L26を用いて再パルプ化処理して慧濁液L 12を得、液L1−南に於いて固液分離処理する。Cake S is repulped using riC liquid L26 as the axis to obtain a slurry liquid L. 12 was obtained and subjected to solid-liquid separation treatment in liquid L1-south.

実質的にジルコニウム不純物及び/又は・・フニウム不純物のみから成る固体S □3は処理サイクルから除去され、液L□3は(A)に於いて再利用される。Solid S consisting essentially only of zirconium impurities and/or hunium impurities □3 is removed from the processing cycle and liquid L□3 is recycled in (A).

不発明の範囲を示す実施例よシネ発明が更に十分に理屏されよう。The invention will be more fully understood through examples showing the scope of the invention.

実施例 1 この実施例は、第1段階に於いて過酸化水素導入後にCD)に於いて行な君實督 量H11へ、過酸化物の形状でのウランの沈殿効率に与える重要性を示すために 行なったものである。Example 1 This example is based on the actual instructions carried out in CD) after the introduction of hydrogen peroxide in the first stage. to the quantity H11, in order to show the importance it has on the precipitation efficiency of uranium in peroxide form. It was done.

このために、200Iのウラン酸アンモニウム精鉱を200Jの水に懸濁させた 。ウラン酸アンモニウム精鉱は以下の重量%組成を有していた。For this, 200 I of ammonium uranate concentrate was suspended in 200 J of water. . The ammonium uranate concentrate had the following weight percent composition:

U :61.16% Mo : 0.39係 Zr : 133% NH4” : 4,7g% その他:32.34% 前記の如く形成された懸濁液に3.OIの100%HNo=及び57gの100 JH,O,を20分間で順次添加した。媒体のpH値は3に調整されておシ懸濁 液の温度は35Cに維持されていた=熟成時間の影響は以下の表Iに示す結果の 考察によって確認され得る。表Iは、ケーキの分離洗浄後台無毒辛、本来の熟成 処理に充てられた時間の関数として示す。U: 61.16% Mo: 0.39 person Zr: 133% NH4”: 4.7g% Others: 32.34% 3. To the suspension formed as above. 100% HNo of OI = and 57g of 100 JH, O, were added sequentially over 20 minutes. The pH value of the medium was adjusted to 3 and the suspension was The temperature of the liquid was maintained at 35C = the effect of aging time was on the results shown in Table I below. This can be confirmed by consideration. Table I shows that after the cake is separated and cleaned, it is not poisonous and the original ripening It is shown as a function of the time devoted to processing.

酸性懸濁液への過酸化水素導入後、O乃至4時間までを30分ずづ区切った種々 の時間に対応する6つのテストを行なった。After the introduction of hydrogen peroxide into the acidic suspension, various treatments separated by 30 minutes from O to 4 hours. Six tests were conducted corresponding to the times of .

表 1 表は、浸出ウランが完全に沈殿するためには少くとも1時間に等しい熟成時間が 必要であることを示す。Table 1 The table shows that an aging time equal to at least 1 hour is required for the leached uranium to completely precipitate. Indicate that it is necessary.

実施例2 この実施例は、第1段階で得られた過酸化ウランに含1れるウランを完全に溶解 させるために第2段階で導入される酸性剤の量の影響を示し得る。Example 2 In this example, the uranium contained in the uranium peroxide obtained in the first step was completely dissolved. The effect of the amount of acidic agent introduced in the second stage to achieve this effect can be shown.

酸性剤の導入量を変更して2つのテストを実施した。酸性剤の導入量の影響は表 ■に示す結果から明らかである。Two tests were conducted by changing the amount of acidic agent introduced. The effect of the amount of acidic agent introduced is shown in the table. This is clear from the results shown in (2).

このために、実施例1で定義されたウラン含有精鉱を使用して方法の第1段階を 実施してウェットケーキS6を形成し、該ケ−キを本発明方法の第2段階で処理 した。To this end, the first stage of the process is carried out using the uranium-containing concentrate defined in Example 1. to form a wet cake S6, which is then treated in the second stage of the method of the invention. did.

各テストでは不純過酸化ウランから形成されたケーキS6を20011ずつ使用 した。Each test used 20,011 pieces of cake S6 formed from impure uranium peroxide. did.

この表によれば遊離酸度が0.INから2NK変わると不純物Zrの誕度が約4 0倍になる。このことは、81段階で得られたウラン含有沈殿物を溶解でぜるた めに導入される酸の量の厳密な調節が必要であることを示す。According to this table, the free acidity is 0. When 2NK changes from IN, the degree of birth of impurity Zr is about 4 It becomes 0 times. This means that the uranium-containing precipitate obtained in step 81 can be completely dissolved by dissolving it. This indicates the need for tight control of the amount of acid introduced.

実施例3 この実施例は、第1段階で得られた沈殿物からウランを溶解婆せる処理に続く第 2段階での熟成処理(I)の継続時間が重要視される理由を明らかにする。Example 3 This example describes the process of dissolving uranium from the precipitate obtained in the first stage. The reason why the duration of the two-stage aging process (I) is important will be clarified.

このために、実施例2のテス) (G)と同量の被処理物質(200I)及び処 理物質(39,65,!i’の100 % HNO3)を使用し5つの連続テス トを実施した。各テストでは、酸性懸濁g、を攪拌下で90Cに維持し、テスト 毎に維持時間を変えた。テスト結呆は熟成分離後に収集された水相中のZr濃度 として表1に表は少くとも2時間、特に約4時間の熟成を行なうのが必要である ことを示す。このような熟成時間を用いると不純物Zr及びMoの態度が計容範 囲に維持される。For this purpose, the same amount of the substance to be treated (200I) as in Example 2 (Test) (G) and the Five consecutive tests using physical substances (100% HNO3 of 39,65,!i’) We conducted a test. In each test, the acidic suspension g, was maintained at 90C under stirring and the test The maintenance time was changed each time. The test result is the Zr concentration in the aqueous phase collected after aging separation. As shown in Table 1, it is necessary to ripen for at least 2 hours, especially about 4 hours. Show that. When such aging time is used, the behavior of impurities Zr and Mo is within the measurement range. maintained within the surroundings.

実施例4(第1図に基く) この実施例では、2段階処理を含む本発明方法を説明する。Example 4 (based on Figure 1) This example describes a method of the invention that includes a two-step process.

本発明方法によれば処理の第1段階に於いて、乾燥状態で以下の重量%組成を有 するウラン含有精鉱200M量部を懸濁化Mo 0.39 % ての他+HzO: 32.34% 該ゾーン(A)に200重量部の水を導入し次に均質な懸濁液を得るために必要 な時間攪拌した。この懸濁液に30部の100%HNO3相当量を20分間で添 刀日した(ゾーンB)。前記の如く得られた懸濁液に次に、57.0 j9のH 2O,(100%) (L21 )を20分間で添加しくゾーンC)、水散化ナ トリウム(L22)を添加してpH3に調整した。ゾーン(C)から出た懸濁液 りうに大し、該懸濁液を温度35Cで攪拌下に2時間30分間維持する熟成処理 を(D)に於いて実施した。(D)で得られた懸濁液L4を次に(E)に於いて 分離処理し液L5と同相S6とを傅た。According to the method of the present invention, in the first stage of the treatment, the dry state has the following weight percent composition: Suspended 200M parts of uranium-containing concentrate with Mo 0.39% Other than that +HzO: 32.34% 200 parts by weight of water are introduced into said zone (A) and then necessary to obtain a homogeneous suspension. The mixture was stirred for a period of time. To this suspension was added an amount equivalent to 30 parts of 100% HNO3 over 20 minutes. It was a long day (Zone B). The suspension obtained above was then treated with 57.0j9 H Add 2O, (100%) (L21) in 20 minutes to zone C), aqueous dispersion na The pH was adjusted to 3 by adding thorium (L22). Suspension coming out of zone (C) A ripening treatment in which the suspension is kept under stirring at a temperature of 35C for 2 hours and 30 minutes. was carried out in (D). The suspension L4 obtained in (D) is then processed in (E). After separation treatment, liquid L5 and the same phase S6 were obtained.

面相S5を次に(F)に於いて200重量部の水を用いて処理し、洗浄後の液L 6と固相S6とを得た。* LsとL6とを混合して液L14を得た。液L+4 の一部分LI5はい)に於いてウラン含刊精鉱を懸濁させるために再利用され、 残シの部分Llflは第1段階での不純物の蓄積を避けるためにサイクルから取 出された。The surface phase S5 was then treated with 200 parts by weight of water in (F), and the liquid L after washing was 6 and solid phase S6 were obtained. *Liquid L14 was obtained by mixing Ls and L6. Liquid L+4 A part of LI5 is reused to suspend uranium-containing concentrate in LI5, The residual portion Llfl is removed from the cycle to avoid the accumulation of impurities in the first stage. Served.

液L14は323重量部であシ以下の重量組成を有していた。Liquid L14 had a weight composition of 323 parts by weight or less.

NH4NO3: 12.9 % N a NO3: 1.7 % H20+その他:80.05% 従って、ウラン含有精鉱中に最初に存在していたモリブデンの90.0%が液L 14によって除去された。NH4NO3: 12.9% N a NO3: 1.7% H20+Other: 80.05% Therefore, 90.0% of the molybdenum initially present in the uranium-containing concentrate is Removed by 14.

洗浄(F)後のケー48.は349重量部のウェットケーキであった。60iC で乾燥後に該ケーキは以下の重量%組成を有してその他+H20: 32.81 係 本発明による処理の第2段階に於いて、第1処理段階で得られたケーキS6が( H)に於いて65部の100%HNO!で処理された。この酸は20分間で緩つ くシと導入され、これによシ得られた懸濁液り、は(I)に於いて90Cに加熱 されこの温度で4時間維持された。K48 after cleaning (F). was 349 parts by weight wet cake. 60iC After drying at Person in charge In the second stage of the treatment according to the invention, the cake S6 obtained in the first treatment stage is ( 65 copies of 100% HNO in H)! Processed with. This acid will loosen in 20 minutes The resulting suspension was heated to 90C in (I). and maintained at this temperature for 4 hours.

ゾーンCI)から出た懸濁液L9を(J)に於いて分離し液LtoとケーキSt Oとを得た。ケーキStOを(K)に於いて22重量部の水(Lzs)で洗浄し 、ケーキS□1と液Luとを得た。液L1oとLllとを混合して液LITを構 成した。液L17は450重量部であった。The suspension L9 coming out of zone CI) is separated in (J) to form liquid Lto and cake St. I got O. Cake StO was washed with 22 parts by weight of water (Lzs) in (K). , cake S□1 and liquid Lu were obtained. Construct liquid LIT by mixing liquids L1o and Lll. accomplished. Liquid L17 was 450 parts by weight.

この液L17は以下の組成を有していた。This liquid L17 had the following composition.

U :27.2 % Mo : 0.016% Zr : 0.005% &O十NO3+その他ニア2.779%精製された液L17の一部分はCG)に 於いて、第1段階で得られたケーキS6を懸濁させるために再利用され、残シの 部分Lt。U: 27.2% Mo: 0.016% Zr: 0.005% &O 1 NO3 + other 2.779% purified liquid L17 is part of CG) The cake S6 obtained in the first stage is reused to suspend it, and the remaining cake is Part Lt.

がウランの製造液を構成した。60Uで乾燥後のケーキS11は、5.6重量部 の重さであった。constituted the uranium production liquid. Cake S11 after drying at 60U is 5.6 parts by weight The weight was .

該ケーキはウラン含有精鉱中に最初に存在していたジルコニウムの実質的に99 .1%を含有してお9、ウラン濃度は精鉱中に最初に存在していたウランの0. 4%の損失を示す量であった。The cake contains substantially 99% of the zirconium originally present in the uranium-containing concentrate. .. The uranium concentration is 0.1% of the uranium originally present in the concentrate. The amount represented a loss of 4%.

この損失分は連続方法の場合にはCM)に於いて弱酸性液L−に再度懸濁された 。液L26は(N)での濾過後に液L13として(A)に於いて再利用される。In the case of a continuous process, this loss was resuspended in weakly acidic liquid L- in CM). . After filtration with (N), liquid L26 is reused as liquid L13 in (A).

実施例 5 この実施料では本発明方法の変形例を使用する方法と使用しない方法とを比較し た。Example 5 In this license, a method using a modified example of the method of the present invention and a method not using it are compared. Ta.

テストNは変形例を使用しない第1図の方法を示す。Test N shows the method of FIG. 1 without using the variant.

テスト0は第2図に示す本発明方法の変形例を示す。Test 0 represents a variation of the method of the invention shown in FIG.

テス)Nによれば、処理の第1段階に於いて懸濁化ゾーンい)に、乾燥状態で以 下の重量%ffi成を有するニジニジrP匝販つラン含有稍鉱を150重量部導 入した。According to Tess) N, in the first stage of the process, in the suspension zone, the following Introducing 150 parts by weight of orchid-containing ore having a weight percent ffi composition of I entered.

U :68.2 % Mo : O,13% zr : 2.44部 平 :9.0 % その他+H20: 20.23% 同じゾーン(A)に123重量部の水を導入し、次に均質懸濁液の形成に必要な 時間攪拌した。この懸濁液に39仏の100%HNO3相当量を20分間で添加 した(ゾーンB)。前記め如く得られた懸濁液に次に(シーyC)、29.01 1 (7)H2O2(100%)(Lzt)を20分間で添加し、水酸化ナトリ ウム(L22)を添加してpHk 3.4に調整した。ゾーン(C)から出た懸 濁液L3に対しくD)に於いて該懸濁液を温度30Cで攪拌下に2時間維持する 熟成処理を実施した。U: 68.2% Mo: O, 13% zr: 2.44 copies Flat: 9.0% Others + H20: 20.23% Into the same zone (A) 123 parts by weight of water are introduced and then the amount of water required to form a homogeneous suspension is Stir for hours. Add an amount equivalent to 39 grams of 100% HNO3 to this suspension over 20 minutes. (Zone B). Next, to the suspension obtained as above (CyC), 29.01 1 (7) Add H2O2 (100%) (Lzt) for 20 minutes and add sodium hydroxide. (L22) was added to adjust the pH to 3.4. Hanging out of zone (C) In D) for suspension L3, maintain the suspension at a temperature of 30C for 2 hours under stirring. A ripening treatment was carried out.

CD)で得られた懸濁液L4に次に(E)に於いて分離処理し液L5と固相S5 とを得た。固相85を次K (F)に於いて200重量部の水で処理し洗浄後の 液L6と固相S6とを得た。The suspension L4 obtained in CD) is then separated in step (E) to form a liquid L5 and a solid phase S5. I got this. The solid phase 85 was treated with 200 parts by weight of water in the next K (F), and after washing A liquid L6 and a solid phase S6 were obtained.

液L5とL6とを混合し液L14を得た。液L14の一部分L15は(A)に於 いてウラン含有精鉱を懸濁させるために再利用された。残シの部分L16は第1 段階に不純物が蓄積するのを避けるためにサイクルから除去された。Liquids L5 and L6 were mixed to obtain liquid L14. A portion L15 of the liquid L14 is in (A). It was then reused to suspend uranium-containing concentrate. The remaining part L16 is the first removed from the cycle to avoid impurities accumulating in the stage.

液L14は300重量部であシウ°ラン含有精鉱中に最初に存在していたモリブ デンの97.5%を含有していた。即ち該モリブデンが液L14によって除去さ れた。Liquid L14 contains 300 parts by weight of molyb originally present in the concentrate containing uranium. It contained 97.5% of Den. That is, the molybdenum is removed by liquid L14. It was.

洗浄(F)後のケーキS6は260重量部のウェットケーキであった。60Cで 乾燥後、該ケーキは以下の重量%組成を有していた。Cake S6 after washing (F) was a wet cake of 260 parts by weight. At 60C After drying, the cake had the following weight percent composition:

U :68.0 係 Mo : 0,02% Zr : 2.44% Na : 0.28チ その他十H20: 29.26% 処理の第2段階に於いて第1処理段階で得られたケーキS6はCG)に於いて2 60部の再利用液Ll11で処理された。次に、懸濁液L7は(H)に於いて9 3.6部の100%HNO,により処理された。U:68.0 Person in charge Mo: 0.02% Zr: 2.44% Na: 0.28chi Other 10 H20: 29.26% In the second stage of processing, the cake S6 obtained in the first stage of processing is It was treated with 60 parts of recycle liquid Ll11. Next, suspension L7 is 9 in (H) Treated with 3.6 parts of 100% HNO.

この酸は20分間で緩つくシと導入された。得られた懸濁液L8はCI)に於い て90Cにされこの温度で2時間維持された。The acid was introduced slowly over a period of 20 minutes. The suspension L8 obtained was in CI) The temperature was brought to 90C and maintained at this temperature for 2 hours.

ゾーン(I)から出た懸濁液L9を(J)に於いて分離し液LIOとケーキS1 ゜と金得た、ケーキ81Gを(K)に於いて17重量部の水(L25)で洗浄し 、ケーキ811と液Lllとを得た。液L1oとLllとを混合して液L17を 構成した。液L17は500重量部であった。この液L17は以下の組成を有し ていた。Suspension L9 coming out of zone (I) is separated in (J) to form liquid LIO and cake S1. Cake 81G obtained with ゜ was washed with 17 parts by weight of water (L25) in (K). , cake 811 and liquid Lll were obtained. Mix liquid L1o and Lll to make liquid L17. Configured. Liquid L17 was 500 parts by weight. This liquid L17 has the following composition. was.

U :26.180% Mo : 0.007% Zr : 0.050% HzO+ NOx+その他ニア3.763%精製された液L17の一部分はCG )に於いて、第1段階で得られたケーキS6を懸濁させるために再利用され、残 υの部分L19がウランの製造液を構成した。60Cで乾燥後のケーキSllは 9.5重量部の重さであった。該ケーキはウラン含有精鉱中に最初に存在してい たジルコニウムの実質的に94.7%を含有しておシ、ウラン濃度は精鉱中に最 初に存在していたウランの0.4チの損失を示す量でめった。この損失分は連続 方法の場合にはCM)に於いて弱酸性液L2sに再度懸濁された。液I4は(N )で濾過後に液L13として(A)に於いて再利用される。U: 26.180% Mo: 0.007% Zr: 0.050% HzO + NOx + Other Near 3.763% A part of the purified liquid L17 is CG ), the cake S6 obtained in the first stage is reused to suspend it, and the remaining Part L19 of υ constituted the uranium production liquid. The cake Sll after drying at 60C is It weighed 9.5 parts by weight. The cake is initially present in the uranium-containing concentrate. It contains essentially 94.7% of zirconium, and the uranium concentration is the lowest in the concentrate. The amount was a loss of 0.4 t of the originally existing uranium. This loss is continuous In the case of the method (CM), it was resuspended in a weakly acidic solution L2s. Liquid I4 is (N ) and then reused as liquid L13 in (A).

変形方法を示すテストOによれば、第1段階に於いて懸濁化ゾーン(A)にテス )Nと同じ市販のウラン含有精鉱を500重量部導入した。同じゾーン(A)に 500重量部の水を導入し均質懸濁液を得るために必要な時間攪拌した。該懸濁 液に423部の100%HNO3相当量を20分間で添加した(ゾーンB)。According to test O, which shows the deformation method, in the first stage the suspension zone (A) is tested. ) 500 parts by weight of the same commercially available uranium-containing concentrate as N was introduced. in the same zone (A) 500 parts by weight of water were introduced and stirred for the time necessary to obtain a homogeneous suspension. the suspension An amount equivalent to 423 parts of 100% HNO3 was added to the solution over 20 minutes (Zone B).

次に懸濁液L2を(BA)に導入し57.6重量部のKFによシ90Cで錯化処 理を行なった。Next, suspension L2 was introduced into (BA) and complexed with 57.6 parts by weight of KF and 90C. I did the right thing.

得られた水性媒体L41に対しくBB)に於いて、該懸濁液を温度90Cで攪拌 下に1時間維持する熟成処理を実施した。In the obtained aqueous medium L41 (BB), the suspension was stirred at a temperature of 90C. A ripening treatment was carried out in which the temperature was maintained for 1 hour.

ゾーン(BB)から出た水性媒体り、を(BC)に於いて温度30Cまで冷却し た。The aqueous medium coming out of zone (BB) is cooled to a temperature of 30C in (BC). Ta.

冷却された水性媒体り、に(ゾーンCで)330.8部の(100%) HzO x (L21 )を25分間で添加した。In the cooled aqueous medium (in zone C) 330.8 parts (100%) HzO x (L21) was added over 25 minutes.

ゾーン(C)から出た懸濁液L3に対しくCA)に於いて水酸化カリウム液しヤ を導入してpHの緩除な調整処理を行ない、pH値を3.5にした−。In CA), potassium hydroxide solution is added to the suspension L3 coming out of zone (C). was introduced to slowly adjust the pH, and the pH value was brought to 3.5.

ゾーン(CA)から出た懸濁液L44に対しくD)に於いて、該懸濁液を温度3 6Cで攪拌下に45分間維持する熟成処理を行なった。In D) for the suspension L44 coming out of zone (CA), the suspension was heated to a temperature of 3. A ripening treatment was carried out at 6C and maintained for 45 minutes under stirring.

(D)で得られた懸濁液L4を次に(E)に於いて公理処理して液L5と同相S sとを得た。The suspension L4 obtained in (D) is then subjected to axiomatic treatment in (E) to obtain a liquid S in the same phase as the liquid L5. I got s.

同相S5を次に(F)に於いて200重量部の水で洗浄処理して洗浄後の液L6 と固相S6とを得た。The same phase S5 is then washed with 200 parts by weight of water in (F), and the washed liquid L6 and solid phase S6 were obtained.

数L5とL6とを混合して液L14とした。液L14の一部分Ltsは(A)に 於いてウラン含有精鉱を懸濁させるために再利用され、残りの部分Li6は不純 物の蓄積を避(r′fるためにサイクルから取出された。Liquid L5 and L6 were mixed to form liquid L14. Part Lts of liquid L14 is (A) The remaining Li6 is recycled to suspend the uranium-containing concentrate. removed from the cycle to avoid accumulation of material.

fiL14は4700部でありウラン含有精鉱中に最初に存在していたモリブデ ンの97.6%を含有していた。該モリブデンはこの液L14によって除去され た。fiL14 is 4,700 parts, which is the molybdenum originally present in the uranium-containing concentrate. It contained 97.6% of the total amount. The molybdenum is removed by this liquid L14. Ta.

洗浄CF)後のケーキS6は1900重量部のウェットケーキであった。Cake S6 after washing CF) was a wet cake of 1900 parts by weight.

60Cで乾燥後の該ケーキは以下の重量係組成ヲ有していた。After drying at 60C, the cake had the following composition by weight:

U :65.17 係 Mo : 0.003% Zr : 2.52 % その他十HzO: 32.307% 処理の第2段階に於いて、第1処理段階後に得られたケーキS6は(G)に於い て578部の再利用液L18によシ処理された。U: 65.17 Section Mo: 0.003% Zr: 2.52% Other 10HzO: 32.307% In the second stage of processing, the cake S6 obtained after the first stage of processing is in (G) It was then treated with 578 parts of recycled liquid L18.

次に懸濁液L7は(H)に於いて172部の100%HNO3によυ処理された 。この酸は85Cで120分間で緩つく9と導入された。前記の如く得られた懸 濁液L8はCI)に於いて85tll’に2時間維持された。Suspension L7 was then treated with 172 parts of 100% HNO3 in (H) . The acid was introduced at 85C for 120 minutes. The concerns obtained as above Suspension L8 was maintained at 85 tll' in CI) for 2 hours.

ゾーンCI)から出た懸濁液L9を(J)に於いて分離し液LIOとケーキSI Oとを得た。ケーキSho k (K) VC於t+Zljoo重量部の水(L 25 )で洗浄し、ケーキSllとiLuとを得た。1LxoとLllとを混合 して液L17を構成した。液L17は2850重量部でめった。この液L17は 以下の組成余有していた。The suspension L9 coming out of zone CI) is separated in (J) to form liquid LIO and cake SI. I got O. Cake Sho k (K) VC+Zljoo parts by weight of water (L 25) to obtain cake Sll and iLu. 1 Mixing Lxo and Lll A liquid L17 was prepared. Liquid L17 was mixed at 2,850 parts by weight. This liquid L17 is The following composition remained.

U :2L5 % Mo : 0.001% Zr : 0.010% H20+ NO3+その他ニア8.489%精製されだ液L17の一部分はCG )に於いて、第1段階で得られたケーキ86を懸濁させるために再利用され、残 夛の部分L19がウランの製造液を構成した。60Cで乾燥後のケーキstiは 32.0重量部の重さであった。該ケーキはウラン含有精鉱中に最初に存在して いたジルコニウムの実質的に98.7%を含有してお9、ウラン濃度は精鉱中に 最初に存在していたウランの0.4%の損失を示す量であった。この損失分は連 続方法の場合には(M)に於いて弱酸性液L2IIに再度懸濁された。液Luは (N)での濾過後に液L13として(A)に於いて再利用される。U:2L5% Mo: 0.001% Zr: 0.010% H20 + NO3 + other near 8.489% purified saliva L17 is partially CG ), the cake 86 obtained in the first stage is reused to suspend and the remaining Part L19 constituted the uranium production liquid. The cake sti after drying at 60C is It weighed 32.0 parts by weight. The cake is initially present in the uranium-containing concentrate. The concentration of uranium in the concentrate is This amount represented a loss of 0.4% of the uranium originally present. This loss is In the case of the subsequent method (M), it was resuspended in weakly acidic liquid L2II. Liquid Lu is After filtration with (N), it is reused as liquid L13 in (A).

前記の如く、テストNと0との比較によシ、本発明方法の変形によって得られる ウラン含有液L19の純度が極めて顕著に上昇することが明らかである。As mentioned above, by comparing test N and 0, we can obtain by a modification of the method of the invention It is clear that the purity of the uranium-containing liquid L19 increases very significantly.

実施例 に の実施例に於いて出願人は、本発明方法の変形を3つの異なる工業的方法で得ら れた3種の市販ウラン精鉱に適用した。Example In the example, the applicant obtained variations of the process according to the invention in three different industrial processes. The method was applied to three types of commercially available uranium concentrates.

そのうちの1つたるテストOについてはすでに実施例5に記載した。One of them, Test O, has already been described in Example 5.

テストPでは不純ウラン醒72オシ′)ムの形状の市販のウラン含有精鉱が処理 される。In Test P, a commercially available uranium-containing concentrate in the form of impure uranium 72 oscim was processed. be done.

テストQでは不純ウラン醒ナトリウムの形状の市販のウラン含有精鉱が処理され る。In test Q, a commercially available uranium-containing concentrate in the form of impure uranium-based sodium was processed. Ru.

変形方法を示すテストPによれば、第1段階に於いて、以下のN量チ組成を有す る市販のウラン含有精鉱469部を懸濁化ゾーン(A)に導入した。According to test P showing the deformation method, in the first stage, the following N content and composition were obtained. 469 parts of commercially available uranium-containing concentrate were introduced into the suspension zone (A).

U ニア0.6 % MO: Q、19% Zr : 0.32% PO4: 0.28% 804 : 5.32% NH4+: 1.4 % Na : 1.05% Mg : 0.3 % フに+その他:20.54/。U near 0.6% MO: Q, 19% Zr: 0.32% PO4: 0.28% 804: 5.32% NH4+: 1.4% Na: 1.05% Mg: 0.3% Funi + Others: 20.54/.

(以下余白) 同じゾーン囚に500重量部の水を導入し均質懸濁液を得るために必要な時間攪 拌した。該懸濁液に423部の工ooチHNO3相当量を20分間で添加した( ゾーンB)。次に懸濁液L2を(BA)に導入し7.84重量部のKFによfi 90℃で錯化処理を行なった。(Margin below) 500 parts by weight of water was introduced into the same zone and stirred for the time necessary to obtain a homogeneous suspension. Stirred. An amount equivalent to 423 parts of HNO3 was added to the suspension over a period of 20 minutes ( Zone B). Next, suspension L2 was introduced into (BA) and added to 7.84 parts by weight of KF. Complexation treatment was carried out at 90°C.

得られた水性媒体L41に対しくBB)に於いて、該懸濁液を温度90℃で攪拌 下に1時間維持する熟成処理を実施した。In the obtained aqueous medium L41 (BB), the suspension was stirred at a temperature of 90°C. A ripening treatment was carried out in which the temperature was maintained for 1 hour.

ゾーン(BB)から出た水性媒体L42 k (BC)に於いて温度30℃まで 冷却した。Temperature up to 30℃ in aqueous medium L42k (BC) coming out of zone (BB) Cooled.

冷却された水性媒体L43に(ゾーンCで)321部の(100チ)H2O2( L21 )を25分間で添加した。In the cooled aqueous medium L43 (in zone C) 321 parts (100 g) of H2O2 ( L21) was added over 25 minutes.

ゾーン(C)から出た懸濁液L3に対しくCA)に於いて水酸化カリウム液L2 2 i導入してpHの緩除な調整処理を行ない、pH値′fr:3.5にした。In CA), potassium hydroxide solution L2 is added to the suspension L3 coming out of zone (C). 2i was introduced and the pH was slowly adjusted to a pH value of 3.5.

ゾーン(CA )から出た懸濁液L44に対しくD)に於いて、該懸濁液を温度 36℃で攪拌下に45分間維持する熟成処理を行なった。In D) for suspension L44 coming out of zone (CA), the suspension is heated to A ripening treatment was carried out at 36° C. and maintained for 45 minutes under stirring.

(D)で得られた懸濁液L4を次に(E)に於いて分離処理して液L5と固相S 5とを得た。The suspension L4 obtained in (D) is then separated in (E) to form a liquid L5 and a solid phase S. I got 5.

固相S5を次に(F)に於いて200重量部の水で洗浄処理して洗浄後の液L6 と固相S6とを得た。The solid phase S5 is then washed with 200 parts by weight of water in (F) to obtain a washed liquid L6. and solid phase S6 were obtained.

液L5とL6とを混合して液L+4とした。液L14の一部分L15は(A)に 於いてウラン含有精鉱を懸濁させるために再利用され、残少の部分L16は第1 段階での不純物の蓄積を避けるためにサイクルから取出された。Liquids L5 and L6 were mixed to form liquid L+4. Part L15 of liquid L14 is converted to (A) The remaining portion L16 is reused to suspend the uranium-containing concentrate in the first removed from the cycle to avoid impurity build-up at the stage.

液L14は4700重量部であシララン含有精鉱中に最初に存在していたモリブ デンの98.9 %を含有していた。該モリブデンはこの液L14によって除去 された。Liquid L14 was 4,700 parts by weight and contained molyb which was initially present in the silalane-containing concentrate. It contained 98.9% of Den. The molybdenum is removed by this liquid L14. It was done.

洗浄(F)後のケーキS6は約1900重量部のウェットケーキであった。60 ℃で乾燥後の該ケーキは以下の重量%組成を有しMO: 0.003% Zr : 0.39 % その他士水: 33.307% 処理の第2段階に於いて、第1処理段階後に得られたケーキS6は(G)に於い て578部の再利用液LIDにょシ処理された。次に懸濁液L7は(H)に於い て172部の100 To HNO3により処理された。この酸は85℃で12 0分間で緩っくシと導入された。前記の如く得られた懸濁液L8は(I)に於い て85℃に2時間維持された。Cake S6 after washing (F) was a wet cake of about 1900 parts by weight. 60 The cake after drying at °C has the following weight % composition: MO: 0.003% Zr: 0.39% Other Shimizu: 33.307% In the second stage of processing, the cake S6 obtained after the first stage of processing is in (G) 578 parts of recycled liquid LID was used. Next, suspension L7 is in (H) and treated with 172 parts of 100 To HNO3. This acid has 12 It was introduced slowly in 0 minutes. Suspension L8 obtained as above was in (I) and maintained at 85°C for 2 hours.

ゾーン(I)から出た懸濁液L9を(J)に於いて分離し液L1゜とケーキSi nとを得た。ケーキ810を(K)に於いて1100重量部の水(L25 )で 洗浄し、ケーキS11と液Lllとを得た。液LIOとLllとを混合して液L 17を構成した。液L+7は2850重量部であった。この液T−tt’rは以 下の組成を有していた。The suspension L9 coming out of zone (I) is separated in (J) to form liquid L1° and cake Si. I got n. Cake 810 in (K) with 1100 parts by weight of water (L25) After washing, cake S11 and liquid Lll were obtained. Mix liquid LIO and Lll to make liquid L. 17 were constructed. Liquid L+7 was 2850 parts by weight. This liquid T-tt'r is as follows. It had the following composition.

U二21,6% Mo : 0.001% Zr : 0.010% H20+NO,十その他: 78.389%精製された液L17の一部分は(G )に於いて、第1段階で得られたケーキS6を懸濁させるために再利用され、残 りの部分L 1gがウランの製造液を構成した。U2 21.6% Mo: 0.001% Zr: 0.010% H20 + NO, ten others: A part of the liquid L17 purified by 78.389% is (G ), the cake S6 obtained in the first stage is reused to suspend it, and the remaining 1 g of portion L constituted the uranium production liquid.

60℃で乾燥後のケーキ811は5重量部の重さであった。該ケーキはウラン含 有精鉱中に最初に存在していたジルコニウムの実質的に96.9チを含Mしてお シ、ウラン濃度は精鉱中に最初に存在していたウランの04%の損失を示す量で あった。この損失分は連続方法の場合には(M)に於いて弱酸性液L26に再度 懸濁された。液L26は(N)でのt過後に液L+3として(A)に於いて再利 用される。Cake 811 after drying at 60°C weighed 5 parts by weight. The cake contains uranium. Contains substantially 96.9% of the zirconium originally present in the concentrate. The uranium concentration represents the loss of 0.4% of the uranium originally present in the concentrate. there were. In the case of a continuous method, this loss is re-added to the weakly acidic liquid L26 in (M). suspended. Liquid L26 is reused in (A) as liquid L+3 after t in (N). used.

同じく本発明の変形を示すテス)QKよれば、第1段階に於いて以下の重量%組 成を有するテス)Nと同種の市販のウラン含有精鉱255重量部を懸濁化ゾーン (A)に導入した。According to Tess) QK, which also shows a modification of the present invention, in the first stage, the following weight percentage set is 255 parts by weight of a commercially available uranium-containing concentrate of the same type as (Tess) N was added to the suspension zone. (A) was introduced.

U : 64.9チ Zr : 1.1チ Na : g、0チ 8i0z : 2.7チ 804 : 2,8% F : 0.1チ 水土その他: 22.2チ 同じゾーン(A)に255重量部の水を導入し均質懸濁液を得るために必要な時 間攪拌した。該懸濁液に423部のiQQ%HNo3相当量を15分間で添加し た(ゾーンB)。次に懸濁液L2を(BA)に導入し14.3重量部のKFによ シフ5℃で錯化処理を行なった。U: 64.9ch Zr: 1.1 chi Na: g, 0 chi 8i0z: 2.7chi 804: 2.8% F: 0.1 chi Water, soil and others: 22.2ch Introducing 255 parts by weight of water into the same zone (A) as needed to obtain a homogeneous suspension. Stir for a while. An amount equivalent to 423 parts of iQQ%HNo3 was added to the suspension over 15 minutes. (Zone B). Next, suspension L2 was introduced into (BA) and 14.3 parts by weight of KF was added. The complexation treatment was carried out at a Schiff temperature of 5°C.

得られた水性媒体L41に対しくBB)に於いて、該懸濁液をゾーン(BB)か ら出た水性媒体L42を(BC)に於いて温度30℃まで冷却した。In the obtained aqueous medium L41 (BB), the suspension was transferred to zone (BB). The aqueous medium L42 that came out was cooled to a temperature of 30° C. in (BC).

冷却された水性媒体L43に(ゾーンCで)160部の(100%)H2O2( L21 )を25分間で添加した。In the cooled aqueous medium L43 (in zone C) 160 parts (100%) H2O2 ( L21) was added over 25 minutes.

ゾーン(C)から出た懸濁液L3に対しくCA)に於いて水酸化カリウム液L2 2を導入してpHの緩除な調整処理を行ない、pH値を3.5にした。In CA), potassium hydroxide solution L2 is added to the suspension L3 coming out of zone (C). 2 was introduced to slowly adjust the pH, and the pH value was brought to 3.5.

ゾーン(CA)から出た懸濁液L44に対しくD)に於いて、該懸濁液を温度3 6℃で攪拌下に45分間維持する熟成処理を行なった。In D) for the suspension L44 coming out of zone (CA), the suspension was heated to a temperature of 3. A ripening treatment was carried out at 6° C. and maintained for 45 minutes under stirring.

(D)で得られた懸濁液L4を次に(E)に於いて分離処理して液L5と固相S sとを得た。The suspension L4 obtained in (D) is then separated in (E) to form a liquid L5 and a solid phase S. I got s.

固相8sk次に(F)に於いて200重量部の水で洗浄処理して洗浄後の液L6 と固相S6とを得た。Solid phase 8sk Next, in (F), wash with 200 parts by weight of water to obtain liquid L6 after washing. and solid phase S6 were obtained.

液L5とL6とを混合して液L+4とした。液L14の一部分L15は(A)に 於いてウラン含有精鉱を懸濁させるために再利用され、残シの部分L1gは第1 段階での不純物の蓄積を避けるためにサイクルから取出された。Liquids L5 and L6 were mixed to form liquid L+4. Part L15 of liquid L14 is converted to (A) The remaining part L1g is reused to suspend the uranium-containing concentrate in the first removed from the cycle to avoid impurity build-up at the stage.

液L!4は2500重量部であった。Liquid L! 4 was 2500 parts by weight.

洗浄(F)後のケーキS6は658重量部のウェットケーキであった。60℃で 乾燥後の該ケーキは以下の重量%組成を有していた。Cake S6 after washing (F) was a wet cake of 658 parts by weight. at 60℃ After drying, the cake had the following weight percent composition:

U : 64.4 チ その他+H20: 34.51% 処理の第2段階に於いて、第1処理段階後に得られたケーキS6は(G)に於い て1050部の再利用液L1gにょ夛処理された。U: 64.4 Others + H20: 34.51% In the second stage of processing, the cake S6 obtained after the first stage of processing is in (G) Then, 1050 parts of 1 g of recycled liquid was added.

次に懸濁液L7は(H)に於1/−,て87部O100%HNO3K ヨ’)  処理された。この酸は85℃で120分間で緩っくりと導入された。Next, suspension L7 was added to (H) by 1/-, and 87 parts O100% HNO3K yo') It has been processed. The acid was introduced slowly over 120 minutes at 85°C.

前記の如く得られた懸濁液L8は(I)に於いて85℃に2時間維持された。Suspension L8 obtained as above was maintained at 85° C. in (I) for 2 hours.

ゾーン(I)から出た懸濁液り、t(J)に於いて分離し液LIOとケーキ81 0 (!:を得た。ケーキ81Gを(K)に於いて500重量部の水(L25) で洗浄し、ケーキ811と液Lllとを得た。液LIOとLl+とを混合して液 L1?全構成した。液L17は2540重量部であった。この液L17は以下の 組成を有していた。The suspension coming out of zone (I) is separated at t (J) into liquid LIO and cake 81 0 (!: obtained. Cake 81G in (K) 500 parts by weight of water (L25) Cake 811 and liquid Lll were obtained. Mix liquid LIO and Ll+ to make liquid L1? Completely configured. Liquid L17 was 2540 parts by weight. This liquid L17 is as follows. It had a composition.

U : 24.9 % Zr : 0.005% H20+N03+その他: 70.595%精製されだ液L+7の一部分は(G )に於いて、第1段階で得られたケーキS6を懸濁させるために再利用され、残 りの部分L19がウランの製造液全構成した。60℃で乾燥後のケーキ811は 9.3重量部の重さであった。該ケーキはウラン含有精鉱中に最初に存在してい たジルコニウムの実質的に98.9 %を含有しておシ、ウラン濃度は精鉱中に 最初に存在していたウランの2%の損失を示す量であった。この損失分は連続方 法の場合には(M)に於いて弱酸性液L26に再度懸濁された。液L26は(N )でのf通抜に液L13として(A)に於いて再利用される。U: 24.9% Zr: 0.005% H20+N03+Others: A portion of 70.595% purified saliva L+7 is (G ), the cake S6 obtained in the first stage is reused to suspend it, and the remaining Part L19 comprised the entire uranium production solution. Cake 811 after drying at 60℃ is It weighed 9.3 parts by weight. The cake is initially present in the uranium-containing concentrate. It contains substantially 98.9% of zirconium, and the concentration of uranium in the concentrate is This amount represented a loss of 2% of the uranium originally present. This loss is continuous In the case of method (M), it was resuspended in weakly acidic liquid L26. Liquid L26 is (N ) is reused as liquid L13 in (A).

前記の如きテスト0.P、Qとテス)Nとの比較より、本発明方法の変形方法が 出発ウラン含有精鉱の種類の違いに関わり無く得られるウラン含有液LI9の純 度を向上させることが立証され得る。Test 0 as above. From the comparison with P, Q and Tess) N, it is clear that the modified method of the present invention is Purity of uranium-containing liquid LI9 obtained regardless of the type of starting uranium-containing concentrate It can be proven to improve the degree of

¥=杯扁 FIG、1 利段階 第1M7′旨 j 茅2P’iF旨 FIG、2¥= Cup FIG, 1 profit stage 1st M7' effect j Kaya 2P'iF effect FIG.2

Claims (1)

【特許請求の範囲】 1.不純物を含有しており前記不純物中に勢に夕くEも1種Oジルコニウム元素 及び/又はハフニウム元素が含まれているウラン含有精鉱を精製するために、過 酸化ウランの形成を生起すべく高温酸性水性媒体中での過酸化水素による前記精 鉱の処理を含む方法でろり、第1段階に於いて、ウランを定量的に沈殿せしめ不 純物の全部又は一部子浸出せしめる目的で、ウラン含有稍焦を水性媒体に懸濁さ せ、次に酸性剤を用いて前記懸濁液fI:緩つくりと調車的に酸性化し、得られ た酸性化水性媒体を過騒化水素で処理して主としてウランとジルコニウム及び/ 又はハフニウムのほぼ全量とを含む沈殿物を形成させ、該沈殿物を不純物を含む 液相がら分離すること、次に第2段階に於いて、第1段階で得られた沈殿物を酸 性剤で処理してウランを可溶ウラニルイオンに変化させて溶出せしめ、ウラニル イオンを含有する液相?ジルコニウム及び、/又はノ・フニウムを含む化合物か ら形成された同相から分離すること全特徴とするウラン含有精鉱の精製方法。 2、第1段階に於ける酸性剤の導入時間が5乃至200分間であρ好ましくは1 0乃至120分間であること全特徴とする請求の範囲IK記載のウラン含有M誠 の冷製方法。 3、第1段階に於ける酸性剤の導入量が、酸性化後の遊理H′の濃度が少くとも 0.01N好ましくは少くとも0.INになる量であることを特徴とする請求の 範囲1及び2に記載のウラン含有精鉱の精製方法。 4、酸性化さnた水性媒体が懸濁液又は溶液であることを特徴とする請求の範囲 1乃至3のいずnかに記載のウラン含有精鉱の精製方法。 5、酸性化された水性媒体のA散化水素による処理が、80℃以下好7しくば3 0℃乃至40℃の範囲で調整さr、た温度にて行なわnることを@黴とする請求 の範囲1乃至4のいずれかに記載のウラン含M稍りの精製方法。 6、重性化さnた水性媒体への過≧fヒ水索の導入量71)過酸化ウランの沈殿 に必要な化学量論的量に少くとも等しく籍に前記化学量論的量の2乃至10倍で あることを特徴とする請求の範囲1乃至5のいずれ〃)に記載のウラン含有精鉱 の精製方法っ7、酸性化された水性媒体がフッ化物イ万ン源によって処理さnる ことを特徴とする請求の範囲1乃至4のいずれかに記載のウラン含有精鉱の精製 方法。 8、酸性化さ扛た媒体の温度が少くとも70℃に等しく好ましくは90℃乃至1 00℃の範囲で選択さnることを特徴とする請求の範囲7に記載のウラン含有精 鉱の精製方法。 9. フッ化物イオン源が単独又は混合物として使用される化合物HF 、 N aF 、 KF 、 NH4F 、 Na2S iF6から構成されることを特 徴とする請求の範囲7に記載のウラン含有精鉱の精製方法。 10 モル比F/(Zr十Hf)が少くとも1に等しく特に4乃至IQの範囲で あることを特徴とする請求の範囲7乃至9のいずnかに記載のウラン含有精鉱の 精製方法。 11、錯生成剤導入子の水性媒体の温度が少くとも70℃好1しく¥′X、90 ℃乃至100℃に維泣されていることを特徴とする請求の範囲7乃至10のいず f′Lかに記載のウラン含有精鉱の精製方法。 12、銘生成剤を含有する兼臼化された水性媒体が6時間以下好ましくば1乃至 4時間攪拌下に維持されることを特徴とする請求の範囲7乃至11のいずれかた 記載のウラン含有精鉱の精製方法。 13、錯生成剤を含有する酸性化された水性媒体が少くとも70℃好ましくIr 190℃乃至100℃の温度に維持されることを特徴とする請求の範囲12に記 載のウラン含有精鉱の精製方法。 14、錯化された酸性媒体が60℃禾満好ましくは30℃乃至40Lの温度に冷 却さnることを特徴とする請求の範囲7乃至13のいずれかに記載のウラン含有 精鉱の精製方法。 15、過酸化後の懸濁液がアルカリ性剤の導入によシ2.5乃至45の範囲から 選択されたpHK暖つくりと調霊されることを特徴とする請求の範囲7乃至14 のいずnか知記載のウラン含有精鉱の精製方法。 16、過酸化水素による処理後に得られた懸濁液が6時間以下好ましくは2乃至 4時間攪拌下に維持をnること全特徴とする請求の範囲1乃至15のいずれかに 記載のウラン含iH鉱の精製方法。 17、過酸化水素舖よる処理後に得らnた懸濁液が80℃以下好ましくは30℃ 乃至40℃の温度¥C維持さ几ること全特徴とする請求の範囲1乃至16のいず れかに記載Dノラン含有酋鉱の精製方法。 18、第1段階後に得られた沈殿物がそのまぽの状態で酸性剤てより処理される ことを特徴とする請求の範囲1乃至17のいずれかに記載のウラン含有精鉱の精 製方法。 19、第1段階により得らnた沈殿物が、酸性化された水又は哉性再利用液に懸 濁させられることを特徴とする請求の範囲1乃至18のいずれ′D)に記載のウ ラン含有脩鉱の精製方法。 20 第1段階で得ら九た沈殿物の処理に必要な該洗剤り童が存在ウランに対応 する化学量論的1以下であることを特徴とする請求の範囲1乃至19のいずnか に記載のウラン含有5指鉱の精製方法。 21、第1段階により得られた沈殿物の酸性剤てよる処理が60℃乃至100℃ 00℃好785℃乃至95Cの温度で行なわfることを特徴とする請求の範囲1 乃至20のいずnかに記載のウラン含有精鉱の精製方法。 22、第1段階により得らfた沈殿物の酸性剤による処理が少くとも1時間好ま しくは3乃至5時間で行なわれることを特徴とする請求の範囲1乃至21のいず nかに記載のウラン含有精鉱の精製方法。 23、第1段階により得らfた沈殿物を酸性剤で処理して得らnる:混濁液が4 0℃以下の温度に冷却さr−ることを特徴とする請求の範囲l乃至22のいずn 炉に記載のウラン含有祠鉱の精製方法。 24 第1段階及び第2段階に於いて尋人される酸性剤が、硝酸、値数、塩酸及 び2種以上の前記酸の混合物刀\ら成るグ)v−プに属することを特徴とする請 求の範囲1乃至23のいずT、r+−に記載のウラン含有稍謳の精製方法。[Claims] 1. Contains impurities, and E, which appears in the impurities, is also a type O zirconium element. and/or to refine uranium-containing concentrates containing the element hafnium. said purification with hydrogen peroxide in a hot acidic aqueous medium to cause the formation of uranium oxide. In the first step, uranium is precipitated quantitatively and A slag containing uranium is suspended in an aqueous medium for the purpose of leaching all or part of the pure substance. Then, the suspension fI was acidified using an acidic agent in a loose manner and the obtained The acidified aqueous medium obtained is treated with supernoisy hydrogen to produce mainly uranium and zirconium and/or or forming a precipitate containing almost the entire amount of hafnium, and converting the precipitate into a precipitate containing impurities. The liquid phase is separated, and then in the second step, the precipitate obtained in the first step is acidified. The uranium is treated with a chemical agent to change it into soluble uranyl ions and elute them, producing uranyl. Liquid phase containing ions? Compounds containing zirconium and/or zirconium A method for refining a uranium-containing concentrate, characterized in that it is separated from the same phase formed by the uranium concentrate. 2. The introduction time of the acidic agent in the first stage is 5 to 200 minutes, and ρ is preferably 1. The uranium-containing M-mass according to claim IK, which is characterized in that the duration is 0 to 120 minutes. cold manufacturing method. 3. The amount of acidic agent introduced in the first stage is such that the concentration of free H' after acidification is at least 0.01N preferably at least 0.01N. of a claim characterized in that the amount is IN. A method for refining uranium-containing concentrate according to scopes 1 and 2. 4. Claims characterized in that the acidified aqueous medium is a suspension or a solution. 4. A method for refining a uranium-containing concentrate according to any one of 1 to 3. 5. The treatment of the acidified aqueous medium with A-dispersed hydrogen is preferably 80°C or lower. A claim that @mold is carried out at a temperature adjusted in the range of 0°C to 40°C. The method for purifying uranium-containing M-like substances according to any one of 1 to 4 above. 6. Amount of uranium peroxide introduced into the polymerized aqueous medium 71) Precipitation of uranium peroxide 2 to 10 times the stoichiometric amount at least equal to the stoichiometric amount required for The uranium-containing concentrate according to any one of claims 1 to 5), characterized in that Purification method 7, in which the acidified aqueous medium is treated with a fluoride source. Refining of uranium-containing concentrate according to any one of claims 1 to 4, characterized in that Method. 8. The temperature of the acidified medium is at least equal to 70°C, preferably 90°C to 1 The uranium-containing mineral according to claim 7, characterized in that Method of refining ore. 9. Compound HF, N in which a fluoride ion source is used alone or as a mixture It is specially composed of aF, KF, NH4F, Na2S iF6. 8. The method for refining a uranium-containing concentrate according to claim 7. 10 The molar ratio F/(Zr + Hf) is at least equal to 1, especially in the range of 4 to IQ The uranium-containing concentrate according to any one of claims 7 to 9, characterized in that Purification method. 11. The temperature of the aqueous medium of the complexing agent introducer is preferably at least 70°C, ¥'X, 90 Any of claims 7 to 10, characterized in that the temperature is maintained between 100°C and 100°C. A method for refining the uranium-containing concentrate described in f'L. 12. The combined aqueous medium containing the name-forming agent is heated for up to 6 hours, preferably from 1 to Any one of claims 7 to 11, characterized in that the method is maintained under stirring for 4 hours. Method for refining the described uranium-containing concentrate. 13. The acidified aqueous medium containing the complexing agent is heated to at least 70°C, preferably Ir. Claim 12, characterized in that the temperature is maintained at 190°C to 100°C. Method for refining uranium-containing concentrate. 14. The complexed acidic medium is cooled to a temperature of 60°C, preferably 30°C to 40L. The uranium-containing material according to any one of claims 7 to 13, characterized in that the uranium-containing material is Method of refining concentrate. 15. The suspension after peroxidation is reduced by the introduction of an alkaline agent from a range of 2.5 to 45. Claims 7 to 14 characterized in that selected pHK warming and spirit toning are performed. A method for refining a uranium-containing concentrate as described in the above. 16. The suspension obtained after treatment with hydrogen peroxide is maintained for up to 6 hours, preferably from 2 to Any one of claims 1 to 15, characterized in that it is maintained under stirring for 4 hours. The method for refining the uranium-containing iH ore. 17. The temperature of the suspension obtained after treatment with hydrogen peroxide is 80°C or lower, preferably 30°C. Any of claims 1 to 16, characterized in that the temperature is maintained at a temperature of 40°C to 40°C. D. A method for refining nolan-containing axillary ore. 18. The precipitate obtained after the first stage is treated with an acidic agent in its original state. The uranium-containing concentrate according to any one of claims 1 to 17, characterized in that Manufacturing method. 19. The precipitate obtained from the first step is suspended in acidified water or a recycle liquid. The utensil according to any one of claims 1 to 18 'D), characterized in that A method for refining orchid-containing ore. 20 The detergent needed to treat the precipitate obtained in the first stage corresponds to the presence of uranium. Any one of claims 1 to 19 characterized in that the stoichiometric value is 1 or less. The method for refining the five uranium-containing ores described in . 21. Treatment of the precipitate obtained in the first step with an acidic agent at 60°C to 100°C Claim 1 characterized in that the process is carried out at a temperature of 785°C to 95°C. 20. The method for refining a uranium-containing concentrate according to any one of 20 to 20. 22. Treatment of the precipitate obtained from the first step with an acidic agent is preferably carried out for at least 1 hour. or 3 to 5 hours. A method for refining a uranium-containing concentrate according to item (n). 23. The precipitate obtained in the first step is treated with an acidic agent to obtain a turbid liquid. Any one of claims 1 to 22, characterized in that it is cooled to a temperature of 0°C or less. A method for refining uranium-containing ore described in the furnace. 24 The acidic agents used in the first and second stages are nitric acid, nitric acid, hydrochloric acid and and a mixture of two or more of the aforementioned acids. A method for purifying uranium-containing pyrotechnic materials as described in Items 1 to 23 above.
JP82503397A 1981-11-17 1982-11-15 Refining of uranium-containing concentrates Pending JPS58501994A (en)

Applications Claiming Priority (5)

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FR8121637A FR2516498A1 (en) 1981-11-17 1981-11-17 Purifying uranium concentrate contg. zirconium and/or hafnium - by uranium peroxide pptn. followed by uranium leaching
FR8214488A FR2531698A2 (en) 1981-11-17 1982-08-16 Purification treatment of a uranium-bearing concentrate
FR82/14488EFR 1982-08-16
FR81/21637EFR 1982-08-16
PCT/FR1982/000189 WO1983001793A1 (en) 1981-11-17 1982-11-15 Treatment for the purification of a uranium-bearing concentrate

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Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2770521A (en) * 1944-10-20 1956-11-13 Spiegler Louis Separation of uranium from mixtures
DE1005944B (en) * 1955-12-09 1957-04-11 Degussa Process for the extraction of uranium peroxide in its pure form
US3238014A (en) * 1964-07-06 1966-03-01 Theodore A Gens Recovery of uranium and plutonium values from aqueous solutions of ammonium fluoride
US4024215A (en) * 1975-04-24 1977-05-17 Fmc Corporation Production of uranium peroxide
US4247522A (en) * 1978-06-27 1981-01-27 Gardinier, Inc. Method of purifying uranium tetrafluoride hydrate and preparing uranium (VI) peroxide hydrate using a fluoride precipitating agent
DE3065736D1 (en) * 1979-01-25 1984-01-05 Stamicarbon Process for recovering a uranium-containing concentrate and purified phosphoric acid from wet-process phosphoric acid, and products thus obtained
US4312839A (en) * 1979-04-18 1982-01-26 Mobil Oil Corporation Process for controlling calcium in a leach operation
DE3012367A1 (en) * 1980-03-29 1981-10-08 Nukem Gmbh, 6450 Hanau METHOD FOR PREPELLING THE PEROXIDES OF NUCLEAR FUELS WITH HYDROGEN PEROXIDE FROM ACID SOLUTIONS
NL8006571A (en) * 1980-12-03 1982-07-01 Stamicarbon METHOD FOR EXTRACTING A URANIUM-CONTAINING CONTAINER AND PHOSPHORIC ACID, AND URANIUM-CONTAINING CONTAINER AND PHOSPHORIC ACID OBTAINED BY THIS METHOD

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BR8207981A (en) 1983-11-08
CA1184389A (en) 1985-03-26
GB8319269D0 (en) 1983-08-17
GB2119781B (en) 1985-05-01
FR2531698A2 (en) 1984-02-17
WO1983001793A1 (en) 1983-05-26
GB2119781A (en) 1983-11-23
FR2531698B2 (en) 1985-02-15

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