JPH07292425A - Method for separating and recovering molybdenum and/ or vanadium - Google Patents
Method for separating and recovering molybdenum and/ or vanadiumInfo
- Publication number
- JPH07292425A JPH07292425A JP6107950A JP10795094A JPH07292425A JP H07292425 A JPH07292425 A JP H07292425A JP 6107950 A JP6107950 A JP 6107950A JP 10795094 A JP10795094 A JP 10795094A JP H07292425 A JPH07292425 A JP H07292425A
- Authority
- JP
- Japan
- Prior art keywords
- vanadium
- molybdenum
- separating
- extractant
- extraction
- 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.)
- Pending
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、モリブデンおよび/ま
たはバナジウムとアルミニウムとが共存する水溶液から
溶媒抽出法により、モリブデンおよび/またはバナジウ
ムを分離回収する方法に関する。特に、使用済みの脱硫
触媒を硫酸で浸出処理した液のように、多量のアルミニ
ウムを含有する硫酸水溶液からこれらの金属イオンを効
果的に分離回収する方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for separating and recovering molybdenum and / or vanadium from an aqueous solution in which molybdenum and / or vanadium and aluminum coexist by a solvent extraction method. In particular, it relates to a method for effectively separating and recovering these metal ions from an aqueous sulfuric acid solution containing a large amount of aluminum, such as a solution obtained by leaching a used desulfurization catalyst with sulfuric acid.
【0002】[0002]
【従来の技術】モリブデンやバナジウムを含有する鉱石
の産地は偏在していることもあって、モリブデンやバナ
ジウムは各種の産業廃棄物等の2次資源から回収を行う
ことが望まれている。2. Description of the Related Art Since ores containing molybdenum and vanadium are unevenly distributed, it is desired that molybdenum and vanadium be recovered from secondary resources such as various industrial wastes.
【0003】これらの金属を比較的高濃度で含有する廃
棄物として原油の脱硫用の触媒があげられる。しかしな
がら脱硫廃触媒はこれらの金属の他、これらの5倍以上
のアルミニウムを含有しており、また鉄を含有している
場合もある。従ってバナジウムとモリブデンをアルミニ
ウムや鉄から効率的に分離することが技術上の問題点で
ある。As a waste containing these metals in a relatively high concentration, there is a catalyst for desulfurization of crude oil. However, the desulfurization waste catalyst contains not only these metals but also aluminum which is 5 times or more of these metals, and may also contain iron. Therefore, it is a technical problem to efficiently separate vanadium and molybdenum from aluminum and iron.
【0004】溶媒抽出法で分離・回収する場合、抽出剤
としてD2EHPA〔ジ−(2−エチルヘキシル)リン
酸〕、PC−88A〔2−エチルヘキシルホスフォン酸
モノ2−エチルヘキシルエステルを成分とする大八化学
工業(株)の商品名〕などの酸性燐化合物抽出剤を用い
た場合には、アルミニウムに対するバナジウムへの選択
性が乏しい上に逆抽出に問題がある。すなわち、これら
の抽出溶媒からモリブデンとバナジウムを逆抽出するた
めには後処理も考慮してアンモニア水溶液が用いられる
が、アンモニアの濃度が小さいと水溶液が白濁し、濃度
が高いと有機相が2相に分かれるなどの操業上の困難を
生じる。また抽出剤として高分子量アミンを用いた場合
においても有機相中に抽出された金属濃度が高くなると
有機相が2相に分かれるというトラブルを生ずる。In the case of separation and recovery by a solvent extraction method, D2EHPA [di- (2-ethylhexyl) phosphoric acid] and PC-88A [2-ethylhexylphosphonic acid mono-2-ethylhexyl ester] are used as extractants. In the case of using an acidic phosphorus compound extractant such as the trade name of Chemical Industry Co., Ltd.), the selectivity for vanadium with respect to aluminum is poor and there is a problem in back extraction. That is, in order to back-extract molybdenum and vanadium from these extraction solvents, an aqueous ammonia solution is used in consideration of the post-treatment. However, when the concentration of ammonia is low, the aqueous solution becomes cloudy, and when the concentration is high, the organic phase has two phases. It causes operational difficulties such as being divided into Further, even when a high molecular weight amine is used as the extractant, if the metal concentration extracted in the organic phase becomes high, the organic phase is divided into two phases.
【0005】一方、ヒドロキシオキシム化合物は、19
60年代初めに開発され、多くの金属についてその抽出
特性が研究され、いくつかの特許も出願されてきた。例
えば、米国特許4,026,988(1977年)にお
いてはこの抽出剤がモリブデンの他、銅、砒素、ビスマ
ス、アンチモン、錫等を含む水溶液中からモリブデンを
選択的に抽出することが述べられている。また米国特許
3,415,616(1968年)においてはこの抽出
剤によるバナジウムの抽出が述べられている。しかしな
がらこれまで出願された特許、またはこれまで発表され
ている論文等にはモリブデンとバナジウムのアルミニウ
ムに対する選択性は述べられておらず、かつまたこの抽
出剤を用いてモリブデンとバナジウムをアルミニウムか
ら選択的に抽出分離した後、両者をさらに分離するとい
う方法も述べられていない。On the other hand, the hydroxyoxime compound is 19
Developed in the early sixties, many metals have been investigated for their extraction properties and several patents have been filed. For example, U.S. Pat. No. 4,026,988 (1977) describes that this extractant selectively extracts molybdenum from an aqueous solution containing molybdenum, copper, arsenic, bismuth, antimony, tin and the like. There is. Also, U.S. Pat. No. 3,415,616 (1968) describes the extraction of vanadium with this extractant. However, the patents filed so far, the papers published so far, etc. do not mention the selectivity of molybdenum and vanadium for aluminum, and this extractant is also used to selectively separate molybdenum and vanadium from aluminum. There is also no description of a method of further separating the two after the extraction and separation.
【0006】[0006]
【発明が解決しようとする課題】本発明の目的は、前述
のように従来円滑な操業が困難であった大量のアルミニ
ウムを含む水溶液からモリブデンとバナジウムを選択的
に分離回収する方法を提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide a method for selectively separating and recovering molybdenum and vanadium from an aqueous solution containing a large amount of aluminum, which has been difficult to operate smoothly as described above. It is in.
【0007】[0007]
【課題を解決するための手段】本発明は、モリブデンお
よび/またはバナジウムと、アルミニウムが共存する水
溶液からモリブデンおよび/またはバナジウムを分離回
収する方法において、下記一般式〔I〕The present invention provides a method for separating and recovering molybdenum and / or vanadium from an aqueous solution in which molybdenum and / or vanadium and aluminum coexist.
【化2】 (但し、R1およびR3は炭素数6〜20、好ましくは6
〜14の直鎖または側鎖を有するアルキル基、R2は水
素または炭素数1〜6の直鎖または側鎖を有するアルキ
ル基。)で示されるヒドロキシオキシム化合物を抽出剤
として含有する抽出溶媒と前記水溶液とをpH2以下で
接触させてモリブデンおよび/またはバナジウムを選択
的に抽出することを特徴とするモリブデンおよび/また
はバナジウムの分離回収方法に関する。[Chemical 2] (However, R 1 and R 3 have 6 to 20 carbon atoms, preferably 6 carbon atoms.
~ 14 alkyl group having a straight chain or a side chain, R 2 is hydrogen or an alkyl group having a straight chain or a side chain of 1 to 6 carbon atoms. ) The extraction solvent containing the hydroxyoxime compound as an extractant is brought into contact with the aqueous solution at a pH of 2 or less to selectively extract molybdenum and / or vanadium, thereby separating and recovering molybdenum and / or vanadium. Regarding the method.
【0008】この抽出剤の代表的なものとしては、5,
8−ジエチル−7−ヒドロキシドデカン−6−オキシ
ム、5,10−ジエチル−8−ヒドロキシテトラデカン
−7−オキシムなどが挙げられる。Typical examples of this extractant include 5,
8-diethyl-7-hydroxydodecane-6-oxime, 5,10-diethyl-8-hydroxytetradecane-7-oxime and the like can be mentioned.
【0009】この抽出剤は、適当な希釈剤に溶解させて
抽出溶媒として用いることができる。工業的に使用可能
な希釈剤としては、ケロシン等の脂肪族系希釈剤、ベン
ゼン、トルエン等の芳香族系希釈剤がある。上記抽出剤
と希釈剤との混合比は、1:99〜99:1が好まし
く、特に好ましくは5:95〜50:50である。This extractant can be dissolved in an appropriate diluent and used as an extraction solvent. Examples of industrially usable diluents include aliphatic diluents such as kerosene and aromatic diluents such as benzene and toluene. The mixing ratio of the extractant and the diluent is preferably 1:99 to 99: 1, and particularly preferably 5:95 to 50:50.
【0010】本発明の方法を用いて、モリブデンとバナ
ジウムを分離回収するには、先ず前記の抽出溶媒とこれ
らの金属イオンを含有する水溶液とをpH2以下、好ま
しくは1.2〜1.5の比較的低いpHで液−液接触さ
せる。液−液接触の方法は、溶媒抽出法において用いら
れる周知の方法のいずれもが使用されうる。抽出の際の
抽出溶媒と水溶液との容積比は特に限定されるものでは
ないが、通常、1:10〜10:1である。この容積比
は、抽出溶媒中の抽出剤の濃度、水溶液中の使用液中の
モリブデンとバナジウムの濃度、液−液接触の方法等を
考慮して決定される。In order to separate and recover molybdenum and vanadium using the method of the present invention, first, the above extraction solvent and an aqueous solution containing these metal ions are adjusted to pH 2 or less, preferably 1.2 to 1.5. Make liquid-liquid contact at a relatively low pH. As the liquid-liquid contact method, any of the well-known methods used in the solvent extraction method can be used. The volume ratio of the extraction solvent and the aqueous solution at the time of extraction is not particularly limited, but is usually 1:10 to 10: 1. This volume ratio is determined in consideration of the concentration of the extractant in the extraction solvent, the concentrations of molybdenum and vanadium in the liquid used in the aqueous solution, the liquid-liquid contact method, and the like.
【0011】次いで、上記抽出工程でモリブデンとバジ
ウムを含有する抽出溶媒を、硫酸水溶液特に、2mol
/dm3以上の濃度の硫酸水溶液でスクラップすること
によりバナジウムを選択的に水溶液中に取り出してモリ
ブデン/バナジウムの分離を行う。しかる後にアンモニ
ア水、好ましくは5vol.%以上、特に好ましくは1
0vol.%以上の濃度のアンモニア水と接触させるこ
とによりモリブデンが有機相から剥離される。この場
合、前記ジ−(2−エチルヘキシル)リン酸〔D2EH
PA〕や2−エチルヘキシルホスフォン酸モノ2−エチ
ルヘキシルエステル〔PC−88A・商品名〕からのア
ンモニア水による剥離と異なり、相分離は非常に良好で
ある。スクラッビングおよび逆抽出の際の抽出溶媒とス
クラップ液または逆抽出液との容積比は特に限定される
ものではないが、通常、10:1〜1:10である。こ
のように、逆抽出工程によって、抽出溶媒を再生するこ
とが可能であり、抽出溶媒をくり返し使用することがで
き、しかも相分離が良好なので溶媒のロスも極めて小さ
くできる。Next, in the above extraction step, the extraction solvent containing molybdenum and badium was added to an aqueous sulfuric acid solution, especially 2 mol.
Molybdenum / vanadium is separated by taking out vanadium selectively into the aqueous solution by scraping with a sulfuric acid aqueous solution having a concentration of / dm 3 or more. After that, ammonia water, preferably 5 vol. % Or more, particularly preferably 1
0 vol. Molybdenum is stripped from the organic phase by contact with aqueous ammonia having a concentration of at least%. In this case, the di- (2-ethylhexyl) phosphoric acid [D2EH
PA] and 2-ethylhexyl phosphonic acid mono 2-ethylhexyl ester [PC-88A, trade name], different from the peeling with ammonia water, the phase separation is very good. The volume ratio of the extraction solvent to the scrap liquid or the back extraction liquid at the time of scrubbing and back extraction is not particularly limited, but is usually 10: 1 to 1:10. As described above, the extraction solvent can be regenerated by the back extraction step, the extraction solvent can be used repeatedly, and the phase separation is good, so that the loss of the solvent can be made extremely small.
【0012】なお、本発明においては、アルミニウムの
他に、鉄、コバルト、ニッケルなどの他の金属が共存し
ている系であっても十分に所期の目的を達成することが
できる。In the present invention, the intended purpose can be sufficiently achieved even in a system in which, in addition to aluminum, other metals such as iron, cobalt and nickel coexist.
【0013】本発明の実施態様を以下に示す。 (1)モリブデンおよび/またはバナジウムと、アルミ
ニウムが共存する水溶液からモリブデンおよび/または
バナジウムを分離回収する方法において、下記一般式
〔I〕Embodiments of the present invention will be described below. (1) In the method of separating and recovering molybdenum and / or vanadium from an aqueous solution in which molybdenum and / or vanadium and aluminum coexist, the following general formula [I]
【化3】 (但し、R1およびR3は炭素数6〜20の直鎖または側
鎖を有するアルキル基、R2は水素または炭素数1〜6
の直鎖または側鎖を有するアルキル基。)で示されるヒ
ドロキシオキシム化合物を抽出剤として含有する抽出溶
媒と前記水溶液とをpH2以下で接触させてモリブデン
および/またはバナジウムを選択的に抽出することを特
徴とするモリブデンおよび/またはバナジウムの分離回
収方法。 (2)前記抽出溶媒と前記水溶液とをpH1.2〜1.
5で接触させる前項(1)記載のモリブデンおよび/ま
たはバナジウムの分離回収方法。 (3)前記ヒドロキシオキシム化合物が5,8−ジエチ
ル−7−ヒドロキシドデカン−6−オキシムである前項
(1)または(2)記載のモリブデンおよび/またはバ
ナジウムの分離回収方法。 (4)モリブデンおよび/またはバナジウムとアルミニ
ウムが共存する水溶液が、使用済の脱硫触媒の浸出液で
ある前項(1),(2)または(3)記載のモリブデン
および/またはバナジウムの分離回収方法。 (5)前項(1),(2),(3)または(4)記載の
方法により得られた抽出液を、硫酸水溶液で処理するこ
とを特徴とするバナジウムの剥離方法。 (6)前項(5)の方法によりバナジウムを除去した残
液にアンモニア水を加えて処理することを特徴とするモ
リブデンの剥離方法。[Chemical 3] (However, R 1 and R 3 are alkyl groups having a straight chain or a side chain having 6 to 20 carbon atoms, and R 2 is hydrogen or 1 to 6 carbon atoms.
An alkyl group having a straight chain or a side chain. ) The extraction solvent containing the hydroxyoxime compound as an extractant is brought into contact with the aqueous solution at a pH of 2 or less to selectively extract molybdenum and / or vanadium, thereby separating and recovering molybdenum and / or vanadium. Method. (2) The extraction solvent and the aqueous solution have a pH of 1.2 to 1.
The method for separating and recovering molybdenum and / or vanadium according to the above (1), wherein the method of contacting with 5 is performed. (3) The method for separating and recovering molybdenum and / or vanadium according to the above (1) or (2), wherein the hydroxyoxime compound is 5,8-diethyl-7-hydroxydodecane-6-oxime. (4) The method for separating and recovering molybdenum and / or vanadium according to the above (1), (2) or (3), wherein the aqueous solution in which molybdenum and / or vanadium and aluminum coexist is a leachate of a used desulfurization catalyst. (5) A method for stripping vanadium, which comprises treating the extract obtained by the method described in (1), (2), (3) or (4) above with an aqueous sulfuric acid solution. (6) A method for removing molybdenum, which comprises treating the residual liquid from which vanadium has been removed by the method described in (5) above with ammonia water.
【0014】[0014]
【実施例】以下に本発明の実施例を述べるが、本発明は
これらの実施例に限定されるものではない。EXAMPLES Examples of the present invention will be described below, but the present invention is not limited to these examples.
【0015】実施例1(モリブデンとバナジウムの抽
出) 脱硫触媒を硫酸水溶液中に溶解させて得られると予想さ
れる、モリブデンとバナジウムの他、大量のアルミニウ
ム、少量のニッケルとコバルトならびに微量の鉄を下記
表1の組成とpHの希硫酸の水溶液NO.1〜NO.3
と5,8−ジエチル−7−ヒドロキシドデカン−6−オ
キシムを成分とするLIX63を脂肪族炭化水素を主成
分とする溶剤であるEXXSOL D80に溶解させた
抽出溶媒とを30℃の温度でO/A(有機相/水相)の
容積比が1で数時間振り混ぜたところ表2に示すように
2以下の低いpHにおいてモリブデンとバナジウムが9
0%以上の割合で選択的に抽出されたのに対して他の金
属は実質的に全く抽出されなかった。Example 1 (Extraction of Molybdenum and Vanadium) In addition to molybdenum and vanadium, which are expected to be obtained by dissolving a desulfurization catalyst in an aqueous sulfuric acid solution, a large amount of aluminum, a small amount of nickel and cobalt, and a small amount of iron are extracted. An aqueous solution of dilute sulfuric acid having the composition and pH shown in Table 1 below. 1-NO. Three
And an extraction solvent prepared by dissolving LIX63 containing 5,8-diethyl-7-hydroxydodecane-6-oxime as a component in EXXSOL D80 which is a solvent containing an aliphatic hydrocarbon as a main component at a temperature of 30 ° C. When the volume ratio of A (organic phase / aqueous phase) was 1 and the mixture was shaken for several hours, as shown in Table 2, molybdenum and vanadium were 9 at a low pH of 2 or less.
It was selectively extracted at a rate of 0% or more, while virtually no other metals were extracted.
【0016】[0016]
【表1】 [Table 1]
【0017】[0017]
【表2】 [Table 2]
【0018】実施例2(バナジウムの選択剥離) 実施例1の方法で抽出して得られた593ppmの濃度
のバナジウムと2940ppmの濃度のモリブデンとを
含むLIX63のEXXSOL D80溶液を様々な濃
度の硫酸水溶液と振り混ぜたところいずれの場合もモリ
ブデンは全く剥離されなかったのに対してバナジウムは
以下の割合で剥離された。Example 2 (Selective stripping of vanadium) EXXSOL D80 solution of LIX63 containing vanadium at a concentration of 593 ppm and molybdenum at a concentration of 2940 ppm obtained by the method of Example 1 was treated with an aqueous sulfuric acid solution of various concentrations. When mixed by shaking, molybdenum was not peeled at all in any case, whereas vanadium was peeled at the following ratio.
【0019】[0019]
【表3】 [Table 3]
【0020】実施例3(モリブデンの剥離) 実施例1の方法で抽出して得られたバナジウムとモリブ
デンとを含むLIX63のEXXSOL D80の溶液
を、2.7mol/dm3の濃度の硫酸でバナジウムを
選択剥離した後の3309ppmの濃度のモリブデンと
11ppmの濃度のバナジウムとを含むLIX63のE
XXSOL D80の有機溶液を様々な濃度のアンモニ
ア水溶液とO/A比が1で30℃の温度で振り混ぜたと
ころ、表4に示すようにモリブデンはほぼ全量剥離され
た。この場合水相/油相間の相界面は極めて明瞭であ
り、相分離は容易であった。Example 3 (Exfoliation of molybdenum) A solution of LIX63 EXXSOL D80 containing vanadium and molybdenum extracted by the method of Example 1 was used to remove vanadium with sulfuric acid having a concentration of 2.7 mol / dm 3. LIX63 E containing 3309 ppm molybdenum and 11 ppm vanadium after selective stripping
When the organic solution of XXSOL D80 was shaken with various concentrations of aqueous ammonia solution at an O / A ratio of 1 and a temperature of 30 ° C., almost all molybdenum was exfoliated as shown in Table 4. In this case, the phase interface between the water phase / oil phase was extremely clear, and phase separation was easy.
【0021】[0021]
【表4】 [Table 4]
【0022】[0022]
【効果】本発明により、アルミニウムを含む水溶液から
モリブデンとバナジウムを選択的に、かつ高抽出率で分
離回収することができた。[Effect] According to the present invention, molybdenum and vanadium can be selectively separated and recovered from an aqueous solution containing aluminum at a high extraction rate.
Claims (1)
と、アルミニウムが共存する水溶液からモリブデンおよ
び/またはバナジウムを分離回収する方法において、下
記一般式〔I〕 【化1】 (但し、R1およびR3は炭素数6〜20の直鎖または側
鎖を有するアルキル基、 R2は水素または炭素数1〜6の直鎖または側鎖を有す
るアルキル基)で示されるヒドロキシオキシム化合物を
抽出剤として含有する抽出溶媒と前記水溶液とをpH2
以下で接触させてモリブデンおよび/またはバナジウム
を選択的に抽出することを特徴とするモリブデンおよび
/またはバナジウムの分離回収方法。1. A method of separating and recovering molybdenum and / or vanadium from an aqueous solution in which molybdenum and / or vanadium and aluminum coexist, in the following general formula [I]: (Provided that R 1 and R 3 are alkyl groups having a straight chain or a side chain having 6 to 20 carbon atoms, R 2 is hydrogen or an alkyl group having a straight chain or a side chain having 1 to 6 carbon atoms) An extraction solvent containing an oxime compound as an extractant and the aqueous solution are adjusted to pH 2
A method for separating and recovering molybdenum and / or vanadium, which comprises contacting the following to selectively extract molybdenum and / or vanadium.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP6107950A JPH07292425A (en) | 1994-04-22 | 1994-04-22 | Method for separating and recovering molybdenum and/ or vanadium |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP6107950A JPH07292425A (en) | 1994-04-22 | 1994-04-22 | Method for separating and recovering molybdenum and/ or vanadium |
Publications (1)
Publication Number | Publication Date |
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JPH07292425A true JPH07292425A (en) | 1995-11-07 |
Family
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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JP6107950A Pending JPH07292425A (en) | 1994-04-22 | 1994-04-22 | Method for separating and recovering molybdenum and/ or vanadium |
Country Status (1)
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JP (1) | JPH07292425A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR101048293B1 (en) * | 2010-03-02 | 2011-07-13 | 전남대학교산학협력단 | Method for removing arsenic to produce high purity molybdenum |
CN102851500A (en) * | 2012-09-19 | 2013-01-02 | 中南大学 | Method for extracting vanadium from vanadium-containing highly concentrated sulfuric acid solution and application of extracting agent |
CN104962743A (en) * | 2015-06-18 | 2015-10-07 | 中南大学 | Method for selectively extracting and recycling gallium, germanium and indium from sulfuric acid leach liquid of zinc displacement residues |
-
1994
- 1994-04-22 JP JP6107950A patent/JPH07292425A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR101048293B1 (en) * | 2010-03-02 | 2011-07-13 | 전남대학교산학협력단 | Method for removing arsenic to produce high purity molybdenum |
CN102851500A (en) * | 2012-09-19 | 2013-01-02 | 中南大学 | Method for extracting vanadium from vanadium-containing highly concentrated sulfuric acid solution and application of extracting agent |
CN104962743A (en) * | 2015-06-18 | 2015-10-07 | 中南大学 | Method for selectively extracting and recycling gallium, germanium and indium from sulfuric acid leach liquid of zinc displacement residues |
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