JPH0394028A - Separation of rare-earth element - Google Patents
Separation of rare-earth elementInfo
- Publication number
- JPH0394028A JPH0394028A JP2138776A JP13877690A JPH0394028A JP H0394028 A JPH0394028 A JP H0394028A JP 2138776 A JP2138776 A JP 2138776A JP 13877690 A JP13877690 A JP 13877690A JP H0394028 A JPH0394028 A JP H0394028A
- Authority
- JP
- Japan
- Prior art keywords
- extraction
- earth elements
- rare
- extracted
- extractant
- 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
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 40
- 238000000926 separation method Methods 0.000 title description 4
- 238000000605 extraction Methods 0.000 claims abstract description 48
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 7
- 238000000638 solvent extraction Methods 0.000 claims abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 26
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 4
- 239000003350 kerosene Substances 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 3
- 239000011707 mineral Substances 0.000 abstract description 3
- KRTSDMXIXPKRQR-UHFFFAOYSA-N dimethyl [4-(methylamino)-4-oxobut-2-en-2-yl] phosphate Chemical compound CNC(=O)C=C(C)OP(=O)(OC)OC KRTSDMXIXPKRQR-UHFFFAOYSA-N 0.000 abstract 2
- 229940085991 phosphate ion Drugs 0.000 abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 2
- LJKDOMVGKKPJBH-UHFFFAOYSA-N 2-ethylhexyl dihydrogen phosphate Chemical compound CCCCC(CC)COP(O)(O)=O LJKDOMVGKKPJBH-UHFFFAOYSA-N 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 12
- 239000012071 phase Substances 0.000 description 9
- -1 (1.1,3.3-tetramethylbutyl)phenyl-2-ethyl Chemical group 0.000 description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 7
- 235000011007 phosphoric acid Nutrition 0.000 description 7
- 239000008346 aqueous phase Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 150000003014 phosphoric acid esters Chemical class 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- LPFAQQYUKORPFJ-UHFFFAOYSA-N (2-ethyl-1,1-diphenylhexyl) dihydrogen phosphate Chemical compound C=1C=CC=CC=1C(OP(O)(O)=O)(C(CC)CCCC)C1=CC=CC=C1 LPFAQQYUKORPFJ-UHFFFAOYSA-N 0.000 description 1
- QIVUCLWGARAQIO-OLIXTKCUSA-N (3s)-n-[(3s,5s,6r)-6-methyl-2-oxo-1-(2,2,2-trifluoroethyl)-5-(2,3,6-trifluorophenyl)piperidin-3-yl]-2-oxospiro[1h-pyrrolo[2,3-b]pyridine-3,6'-5,7-dihydrocyclopenta[b]pyridine]-3'-carboxamide Chemical compound C1([C@H]2[C@H](N(C(=O)[C@@H](NC(=O)C=3C=C4C[C@]5(CC4=NC=3)C3=CC=CN=C3NC5=O)C2)CC(F)(F)F)C)=C(F)C=CC(F)=C1F QIVUCLWGARAQIO-OLIXTKCUSA-N 0.000 description 1
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-O azanium;hydrofluoride Chemical compound [NH4+].F LDDQLRUQCUTJBB-UHFFFAOYSA-O 0.000 description 1
- 150000001733 carboxylic acid esters Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 description 1
- ZJIPHXXDPROMEF-UHFFFAOYSA-N dihydroxyphosphanyl dihydrogen phosphite Chemical class OP(O)OP(O)O ZJIPHXXDPROMEF-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- NMCWERWDCXNTLB-UHFFFAOYSA-N ethyl phenyl hydrogen phosphate Chemical compound CCOP(O)(=O)OC1=CC=CC=C1 NMCWERWDCXNTLB-UHFFFAOYSA-N 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、希土類元素、アルミニウムおよび燐酸イオン
を含有する水溶液から希土類元素を効率よく分離する溶
媒抽出法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a solvent extraction method for efficiently separating rare earth elements from an aqueous solution containing rare earth elements, aluminum and phosphate ions.
近年、希土類元素の分離、精製の目的にリン酸エステル
系、ジ亜リン酸エステル系、カルボン酸系等の抽出剤を
用いる事は知られている。中でも酸性有機リン酸エステ
ル類が好適に用いられ、具体的にはジ（２−エチルヘキ
シル）リン酸（以下ｒＤ２ＥＨＰＡＪと記載する）は抽
出能力が比較的大きく、希土の分離、精製上において優
れた抽出剤としてよく知られている。また、Ｄ２ＥＨＰ
Ａが有効に機能する水溶液の酸性度はｐＨＯ以上である
のに対し、ｐＨＯ以下でも機能する更に抽出能力の強い
抽剤として（１．１，３．３−テトラメチルブチル）フ
ェニル２−エチルへキシルリン酸（以下ｒＯＰＥＨＰＡ
」と記載する）が開発されている（特開昭６３−２０６
３１２）。In recent years, it has been known to use extractants such as phosphate esters, diphosphite esters, and carboxylic acid esters for the purpose of separating and purifying rare earth elements. Among them, acidic organic phosphoric acid esters are preferably used. Specifically, di(2-ethylhexyl) phosphoric acid (hereinafter referred to as rD2EHPAJ) has a relatively large extraction ability and is excellent in the separation and purification of rare earths. It is well known as an extractant. Also, D2EHP
The acidity of the aqueous solution in which A functions effectively is above pHHO, whereas (1.1,3.3-tetramethylbutyl)phenyl-2-ethyl is an extractant with even stronger extraction ability that functions even below pHHO. xyl phosphoric acid (rOPEHPA)
”) has been developed (Japanese Patent Application Laid-Open No. 63-206
312).
しかしながら、Ｄ ２ Ｅ Ｈ Ｐ ＡやＯＰＥＨＰＡ
等のリン酸エステル系の抽出剤を用い、希土類元素の他
にアル旦ニウムとリン酸を含む水溶液から希土類元素を
抽出する場合、アルミニウムが多量に抽出されるため希
土類元素の抽出率が低くなる現象が見られる。このため
大量の抽出剤を要するだけでなく抽出されたアルミニウ
ムを水相へ逆抽出するためにはフッ酸やフフ化水素アン
モニウムといった高価でかつ腐食性の強い薬品を用いな
ければならないという問題点を有している。However, D2EHPA and OPEHPA
When extracting rare earth elements from an aqueous solution containing aluminum and phosphoric acid in addition to rare earth elements using a phosphate ester extractant such as, a large amount of aluminum is extracted, resulting in a low extraction rate of rare earth elements. A phenomenon can be seen. This not only requires a large amount of extractant, but also requires the use of expensive and highly corrosive chemicals such as hydrofluoric acid and ammonium hydrogen fluoride in order to back-extract the extracted aluminum into the aqueous phase. have.
本発明者らは、従来技術のかかる問題点を解消すべく鋭
意検討した結果、アルミニウムに比べ希土類元素の抽出
速度が速く、しかも一旦抽出剤に抽出された希土類元素
が、後から抽出されてくるアルミニウムによって置換さ
れ、再び水相側へ戻り、最終的にそれぞれの元素の抽出
平衡に達する事を見い出した。The inventors of the present invention have conducted intensive studies to solve these problems with the conventional technology, and have found that the extraction speed of rare earth elements is faster than that of aluminum, and that the rare earth elements once extracted into the extractant can be extracted later. It was discovered that the aluminum is substituted by aluminum, returns to the aqueous phase side, and finally reaches the extraction equilibrium of each element.
したがって、アルミニウムの抽出率が低い状態、すなわ
ち、系が抽出平衡に達する前に抽出操作を停止させる事
により、希土類元素とアルミニウムの分離を良くする事
ができる事を見い出し本発明に到達した。Therefore, the present inventors have discovered that the separation of rare earth elements and aluminum can be improved by stopping the extraction operation when the extraction rate of aluminum is low, that is, before the system reaches extraction equilibrium.
すなわち本発明の要旨は、希土類元素とアルごニウム及
びリン酸のイオンを含む水溶液から溶媒抽出法によって
希土類元素を分離するにあたりアルミニウムの抽出率が
一定となった時のアルくニウム抽出量（すなわちアルミ
ニウムの平衡抽出量）に対し、１０〜５０％のアルミニ
ウムが抽出された時点（すなわちアルＳニウムの平衡到
達率が１０〜５０％の時点）で抽出操作を停止させる事
によりアルミニウムと希土類元素間の分離を向上させる
事を特徴とする希土類元素の分離方法に存する。In other words, the gist of the present invention is to calculate the amount of aluminum extracted (i.e., By stopping the extraction operation when 10 to 50% of aluminum has been extracted (i.e., when the equilibrium attainment rate of aluminum is 10 to 50%), the relationship between aluminum and rare earth elements can be reduced. The present invention relates to a method for separating rare earth elements, which is characterized by improving the separation of rare earth elements.
以下本発明を詳細に説明する。The present invention will be explained in detail below.
先ず本発明の適用対象である希土類元素とアルミニウム
及びリン酸のイオンを含む水溶液とは、例えばリン酸希
土類及びリン酸アルミニウムを含む鉱石からＨＣＩ等の
鉱酸で希土類元素を浸出させた時に得られる液、等を挙
げることができるが、一般には実質量のアルミニウムと
リン酸イオンが共存する希土類元素含有水溶液である。First, the aqueous solution containing rare earth elements and aluminum and phosphoric acid ions, to which the present invention is applied, is obtained, for example, by leaching rare earth elements from ores containing rare earth phosphates and aluminum phosphate with a mineral acid such as HCI. Generally, it is an aqueous solution containing a rare earth element in which substantial amounts of aluminum and phosphate ions coexist.
より具体的には、抽出操作の設計に際してアルミニウム
イオンとリン酸イオンが無視し得ない程度の量で共存す
る希土類元素含有水溶液であって、例えば典型的には希
土類元素の原子に対するアルミニウムの原子比及びリン
酸イオンのモル比がそれぞれ０．１〜２０，０．１〜２
０程度の量で存在する水溶液に適用される。More specifically, when designing the extraction operation, a rare earth element-containing aqueous solution in which aluminum ions and phosphate ions coexist in non-negligible amounts, for example, typically the atomic ratio of aluminum to rare earth element atoms. and the molar ratio of phosphate ions is 0.1 to 20 and 0.1 to 2, respectively.
Applicable to aqueous solutions present in amounts of around 0.
また、本発明において即ちアルくニウムの平衡３
４
抽出量とは、アルミニウムの抽出率が一定となった時具
体的には一定の抽出操作を行なう間、抽剤または水相を
適当な時間間隔でサンプリングし、アルミニウムの抽出
率が一定となった時の抽剤中の＾ｆｆｉｉｌを示す。こ
こで抽出率一定とは、同じ抽出操作を３０分以上続けて
も、抽出率の変動が±５％以内となる事を示す。そして
、そのＡＩ！．平衡抽出量に対し、１０〜５０％のＡｎ
が抽出された時点で抽出操作を停止させる事により、希
土類元素の抽出率を高い状態に保ち、アルミニウムの抽
出率を低く抑える事ができる。In addition, in the present invention, the equilibrium 3 4 extraction amount of aluminum refers to when the extraction rate of aluminum becomes constant, specifically, during a certain extraction operation, the extraction agent or aqueous phase is removed at appropriate time intervals. The figure shows the amount of ^ffiil in the extractant when the extraction rate of aluminum becomes constant. Here, the constant extraction rate means that even if the same extraction operation is continued for 30 minutes or more, the variation in the extraction rate is within ±5%. And that AI! ．． 10 to 50% of An
By stopping the extraction operation when is extracted, the extraction rate of rare earth elements can be kept high and the extraction rate of aluminum can be kept low.
ここで、抽出操作を停止するＡｊ２の抽出量が低い程抽
出される希土の純度は上がるが、抽出時間が短かくなり
すぎると実際の抽出操作が行なえない問題があるので実
際の抽出時間はこれらの要因を配慮して場合に応じた好
適値を選択すれば良い。Here, the purity of the extracted rare earth increases as the extraction amount of Aj2, which stops the extraction operation, is lower, but if the extraction time becomes too short, there is a problem that the actual extraction operation cannot be performed, so the actual extraction time is A suitable value may be selected depending on the situation, taking these factors into account.
従って、その具体値は一概に特定できないが、Ａｆｆｉ
の抽出量が平衡抽出量の１０〜５０％、好ましくは１５
〜４０％となる範囲であって一般には３分以内、通常１
分以内、好ましくはｌＯ〜３０秒の範囲から選択される
。Therefore, although the specific value cannot be determined unconditionally, Affi
The extraction amount is 10 to 50% of the equilibrium extraction amount, preferably 15
~40%, generally within 3 minutes, usually 1
It is selected within minutes, preferably from the range of 10 to 30 seconds.
ここで、「抽出操作」とは、攪拌装置を備えた容器中で
抽剤相と水相を攪拌混合する操作を示し、「抽出操作を
停止する」とは攪拌を止める事を示す。Here, the "extraction operation" refers to an operation of stirring and mixing the extractant phase and the aqueous phase in a container equipped with a stirring device, and "stopping the extraction operation" refers to stopping the stirring.
以上の様な操作に適用される抽出剤としては、Ｄ２ＥＨ
ＰＡ，○ＰＥＨＰＡの他に（１，１，３．３−テトラメ
チルブチル）フェニルｎブチルリン酸、（１，１，３．
３−テトラメチルブチル）フェニルエチルリン酸（ｔｅ
ｒｔ７’チル）フェニルｎプチルリンＬ （ｔｅｒｔ
フチル）フェニル２−エチルへキシルリン酸などの酸性
有機リン酸エステル系が挙げられる。The extractant that can be applied to the above operations is D2EH.
In addition to PA, ○PEHPA, (1,1,3.3-tetramethylbutyl)phenyl n-butyl phosphate, (1,1,3.
3-tetramethylbutyl) phenylethyl phosphate (te
rt7'chill) phenyl nbutylphosphorus L (tert
Examples include acidic organic phosphoric acid esters such as phenyl (phenyl) 2-ethylhexyl phosphoric acid.
これらの抽出剤は粘度が高いので通常有機溶媒により希
釈し、０．００１〜３モル／１、好ましくは０．０５〜
１．５モル／１程度の溶液として用いるのが良い。有機
溶媒としては、ケロセンのような石油留分、ヘキサン、
オクタン、デカン等の脂肪族炭化水素、ジブチルエーテ
ル、ジイソプロビルエーテル等のエーテル類、ベンゼン
、トルエン等の芳香族炭化水素等が挙げられる。Since these extractants have a high viscosity, they are usually diluted with an organic solvent to give a concentration of 0.001 to 3 mol/1, preferably 0.05 to 3 mol/1.
It is preferable to use it as a solution of about 1.5 mol/1. Organic solvents include petroleum distillates such as kerosene, hexane,
Examples include aliphatic hydrocarbons such as octane and decane, ethers such as dibutyl ether and diisopropyl ether, and aromatic hydrocarbons such as benzene and toluene.
本発明方法においては抽出装置は、抽剤相と希土類元素
を含む水溶液が十分に混合する装置であれば特に限定し
ないが、工業的にはごキサーセトラーが好ましく、抽出
操作時間が特に短い（数秒）場合は、遠心抽出器を用い
る事もできる。また、抽剤相と水相の容量比については
特に限定しないが、通常は水相／抽剤相比１０以下、好
ましくは３ないしｌである。In the method of the present invention, the extraction device is not particularly limited as long as the extractant phase and the aqueous solution containing the rare earth element are sufficiently mixed, but industrially, an extractor settler is preferable, and if the extraction operation time is particularly short (several seconds). A centrifugal extractor can also be used. Further, the volume ratio of the extractant phase to the aqueous phase is not particularly limited, but the aqueous phase/extractant phase ratio is usually 10 or less, preferably 3 to 1.
温度については、特に限定しないが、常温で十分操作可
能である。The temperature is not particularly limited, but it can be operated at room temperature.
また本発明は回分式、連続式のい・ずれにも適用できる
。連続式の場合、一般に、効率的に抽出を行なうため、
向流多段方式の抽出操作が行なわれるが、この場合、あ
らかじめ向流多段抽出に供する原料水溶液と抽剤を用い
て回分弐抽出を行ない、本発明の条件番こ当てはまる滞
留時間を決定し、そして、その滞留時間で、多段抽出の
各段を操作する事により、希土類元素の高抽出率を保ち
つつ、アルミニウムの抽出を抑える事ができる。Further, the present invention can be applied to either batch type or continuous type. In the case of continuous type, generally, in order to extract efficiently,
A countercurrent multistage extraction operation is performed. In this case, batch extraction is performed in advance using the raw material aqueous solution and extractant to be subjected to the countercurrent multistage extraction, and the residence time that meets the conditions of the present invention is determined. By operating each stage of the multi-stage extraction at that residence time, it is possible to suppress the extraction of aluminum while maintaining a high extraction rate of rare earth elements.
希土類元素およびアルミニウムを抽出した抽剤は、まず
Ｉｌ１あるいはｌｌＮＯ３等の鉱酸と接触さセて希土類
元素を逆抽出した後、抽剤中に残存しているアルミニウ
ムを、ＩＰあるいはＮＨａＦＨＦ等で逆抽、除去し、抽
剤を再生する事ができる。The extractant from which rare earth elements and aluminum have been extracted is first contacted with a mineral acid such as Il1 or llNO3 to back-extract the rare earth elements, and then the aluminum remaining in the extractant is back-extracted with IP or NHaFHF. , can be removed and the extractant can be regenerated.
以下、本発明を実施例により更に詳細に説明するが本発
明は以下の実施例に限定されるものではない。EXAMPLES Hereinafter, the present invention will be explained in more detail with reference to examples, but the present invention is not limited to the following examples.
実施例−１および比較例−１．２．３
表−１に示す組威の塩酸酸性水溶液（ｐＨ０．４に調整
）３０ｍｊｌ！とＤ２ＥＨＰＡの１ｍｏｊ２／１ケロセ
ン溶液１５ｌＩＩ！！．を１００ｍＩ！．分液ロート（
スキーブ型）に仕込み、垂直振とう型振とう器（ＩＷＡ
ＫＩ ＫＭ−ＳＨＡＫＥＲ ＭＯＤＥＬ ＶＬＤ
Ｎ）を用いて、３００回／分の振とう数で０．５分間攪
拌した（実施例−１）。攪拌停止後、静置分液し、抽剤
相の１０ｍ！！．をとり、塩リン酸混液（ Ｉ Ｃ１
５ｍｏｆ ／ １ ， Ｈ３ＰＯ４ ３ｍｏｊ２／ １
を含む水溶液）１０ｍｌで２回逆抽出し、塩リン酸逆抽
液中の希土類元素およびＡｆ濃度をＩＣＰで分析する事
により、抽剤相中の抽出威分濃度を測定した。Example-1 and Comparative Example-1.2.3 30 mjl of aqueous hydrochloric acid solution (adjusted to pH 0.4) shown in Table-1! and D2EHPA in 1 moj2/1 kerosene solution 15lII! ! ．． 100mI! ．． Separating funnel (
A vertical shaking shaker (IWA) was prepared.
KI KM-SHAKER MODEL VLD
N) for 0.5 minutes at a shaking rate of 300 times/min (Example-1). After stopping stirring, separate the liquid by standing still, and extract 10 m of extractant phase! ! ．． and a mixture of salt and phosphoric acid (I C1
5mof/1, H3PO4 3moj2/1
The concentration of extracted components in the extractant phase was measured by back-extracting twice with 10 ml of an aqueous solution containing phosphoric acid and analyzing the rare earth element and Af concentrations in the salt-phosphoric acid back-extract by ICP.
その結果を表−２に示す。また、比較として、同様の液
を用い、１０分（比較例−ＩＬ ６０分（比較例−２）
、１２０分（比較例−３）振とう攪拌した場合の抽剤相
中の各戒分濃度を表−２に併せて示す。The results are shown in Table-2. In addition, for comparison, using the same liquid, 10 minutes (Comparative Example-IL 60 minutes (Comparative Example-2)
, 120 minutes (Comparative Example-3) The concentrations of each component in the extraction phase when shaken and stirred are also shown in Table-2.
実施例−２および比較例−４．５．６
表−１に示す組或の塩酸酸性水溶液（ｐＨ０．２に調整
）３０ｍＩ！．とＤＰ８６Ｂのｌｍｏｌ／／！ケロセン
溶液３０ｍｌ！を１００ｍｊ！分液ロ一ト（スキープ型
）に仕込み、実施例−１と同し振とう器、振とう数で０
．５分間攪拌した（実施例−２）。この時の抽剤相中の
各威分濃度を表−３に示す。また比較として、同様の液
を用い、ｌＯ分（比較例４Ｌ ６０分（比較例−５Ｌ
１２０分（比較例６）振とう攪拌した場合の抽剤相中
の各戒分濃度を表−３に併せて示す。Example 2 and Comparative Example 4.5.6 Hydrochloric acid acidic aqueous solution (adjusted to pH 0.2) of the set shown in Table 1 at 30 mI! ．． and DP86B lmol//! Kerosene solution 30ml! 100mj! Pour into a separating funnel (skip type), use the same shaker as in Example-1, and shake at 0.
．． The mixture was stirred for 5 minutes (Example-2). Table 3 shows the concentration of each component in the extraction phase at this time. In addition, for comparison, using the same liquid, 10 minutes (Comparative example 4L 60 minutes (Comparative example - 5L
Table 3 also shows the concentration of each component in the extraction phase when shaking and stirring for 120 minutes (Comparative Example 6).
実施例−１，比較例−１．２．３では、Ａｌの平衡抽出
量は８ ３． ６ｎ＋ ｍｏｂ ／ Ｉｔであるが、そ
れに対し、ＡＩが２ １．３ｍ ｍｏｌ／ｌ． （２
５％）抽出された実施例−１では、比較例−１．２．３
に比べＡｆｆｉ量が小さいのは当然であるが希土量は明
らかに多い。これは、実施例−２，比較例−４，５，６
（平衡Ａｎ １ ０ ０ｍ ｍｏＩ！．／ｊ！）でも同
様である。In Example-1 and Comparative Example-1.2.3, the equilibrium extraction amount of Al was 8.3. 6n+ mob/It, whereas AI is 2 1.3 m mol/l. (2
5%) In extracted Example-1, Comparative Example-1.2.3
Although it is natural that the amount of Affi is small compared to the amount of rare earth, the amount of rare earth is clearly large. This is Example-2, Comparative Example-4, 5, 6
The same is true for (equilibrium An 1 0 0 m moI!./j!).
ｌ０
表−１
原料組威
ｐＨＡ：実施例＝１および比較例
ｌ，
２，
３の
場合
ｐＨＢ：実施例
２および比較例−４，
５．
６の
場合
１
１
１２
〈発明の効果〉
本発明により、
効率よく希土類元素、
アルくニ
ウム及びリン酸を含む水溶液より希土類元素を分離する
ことかできる。10 Table-1 Raw material composition pHA: Example = 1 and Comparative Examples 1, 2, 3 pHB: Example 2 and Comparative Examples -4, 5. Case 6 1 1 12 <Effects of the Invention> According to the present invention, rare earth elements can be efficiently separated from an aqueous solution containing rare earth elements, aluminium, and phosphoric acid.
出 願 人 三菱化威株式会社 代 理 人Out wish Man Mitsubishi Kawei Co., Ltd. teenager Reason Man
Claims (1)
含有する水溶液から希土類元素を溶媒抽出するにあたり
、抽出剤相中のアルミニウムの抽出量が平衡抽出量に対
して１０〜５０％の時点で抽出操作を停止することを特
徴とする希土類元素の分離方法。(1) When performing solvent extraction of rare earth elements from an aqueous solution containing rare earth elements, aluminum, and phosphate ions, perform the extraction operation when the amount of aluminum extracted in the extractant phase is 10 to 50% of the equilibrium extraction amount. A method for separating rare earth elements characterized by stopping.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1-151003 | 1989-06-14 | ||
| JP15100389 | 1989-06-14 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0394028A true JPH0394028A (en) | 1991-04-18 |
Family
ID=15509164
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2138776A Pending JPH0394028A (en) | 1989-06-14 | 1990-05-29 | Separation of rare-earth element |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JPH0394028A (en) |
| BR (1) | BR9002803A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003106638A (en) * | 2001-09-28 | 2003-04-09 | Toto Ltd | Indoor heating and ventilating device |
| CN103773955A (en) * | 2013-11-04 | 2014-05-07 | 中铝广西有色金源稀土股份有限公司 | Method for removing aluminium in tombarthite feed liquid |
| CN105229178A (en) * | 2013-03-15 | 2016-01-06 | 埃赫曼公司 | The method of optionally recovering rare earth metal from the acid sulphate aqueous solution being rich in aluminium and phosphate radical |
| CN113088692A (en) * | 2021-04-06 | 2021-07-09 | 鞍山昊旻稀土科技有限公司 | Extractant for extracting naphthenic acid and yttrium extraction process |
| CN115491526A (en) * | 2022-09-29 | 2022-12-20 | 江西理工大学 | Method for extracting and separating rare earth elements by non-aqueous phase solvent extraction system |
-
1990
- 1990-05-29 JP JP2138776A patent/JPH0394028A/en active Pending
- 1990-06-13 BR BR909002803A patent/BR9002803A/en not_active Application Discontinuation
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003106638A (en) * | 2001-09-28 | 2003-04-09 | Toto Ltd | Indoor heating and ventilating device |
| CN105229178A (en) * | 2013-03-15 | 2016-01-06 | 埃赫曼公司 | The method of optionally recovering rare earth metal from the acid sulphate aqueous solution being rich in aluminium and phosphate radical |
| CN103773955A (en) * | 2013-11-04 | 2014-05-07 | 中铝广西有色金源稀土股份有限公司 | Method for removing aluminium in tombarthite feed liquid |
| CN103773955B (en) * | 2013-11-04 | 2016-08-31 | 中铝广西有色金源稀土股份有限公司 | A kind of remove the method for aluminium in rare earth feed liquid |
| CN113088692A (en) * | 2021-04-06 | 2021-07-09 | 鞍山昊旻稀土科技有限公司 | Extractant for extracting naphthenic acid and yttrium extraction process |
| CN115491526A (en) * | 2022-09-29 | 2022-12-20 | 江西理工大学 | Method for extracting and separating rare earth elements by non-aqueous phase solvent extraction system |
Also Published As
| Publication number | Publication date |
|---|---|
| BR9002803A (en) | 1991-08-20 |
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