JPS605655B2 - Separation method of yztrium - Google Patents
Separation method of yztriumInfo
- Publication number
- JPS605655B2 JPS605655B2 JP5804877A JP5804877A JPS605655B2 JP S605655 B2 JPS605655 B2 JP S605655B2 JP 5804877 A JP5804877 A JP 5804877A JP 5804877 A JP5804877 A JP 5804877A JP S605655 B2 JPS605655 B2 JP S605655B2
- Authority
- JP
- Japan
- Prior art keywords
- extraction
- extraction rate
- curve
- rate
- hpa
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 238000000926 separation method Methods 0.000 title description 8
- 238000000034 method Methods 0.000 claims description 12
- 229910052727 yttrium Inorganic materials 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims description 7
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 claims description 6
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 claims description 5
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 5
- -1 ethylhexyl Chemical group 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- 150000002910 rare earth metals Chemical class 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims 1
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 claims 1
- 229960003330 pentetic acid Drugs 0.000 claims 1
- 238000000605 extraction Methods 0.000 description 48
- 239000002904 solvent Substances 0.000 description 12
- 238000007796 conventional method Methods 0.000 description 5
- 238000007865 diluting Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 229910052691 Erbium Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000003350 kerosene Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Description
【発明の詳細な説明】 本発明は、イットリウムの分離法に関する。[Detailed description of the invention] The present invention relates to a method for separating yttrium.
イットリウム（Ｙ）（原子番号３９）は、カラーテレビ
用赤色ケィ光体原料をはじめ、光学レンズ素材「エレク
トロニクス材料として、その需要が広まりつつある。Ｙ
と他の希±との分離法としては、従来酸性リン酸ェステ
ルを抽出溶媒として用いる抽出分離法、及びイオン交換
樹脂塔に、Ｙ及び希土の混合水溶液を流通して分離する
イオン交換法が一般的な方法として知られている。Yttrium (Y) (atomic number 39) is in increasing demand as a raw material for red phosphors for color televisions, optical lens materials, and electronics materials.
Conventional methods for separating Y and other rare earths include an extraction separation method using acidic phosphate ester as an extraction solvent, and an ion exchange method in which a mixed aqueous solution of Y and rare earth is passed through an ion exchange resin tower. This is known as a general method.
しかしながら、これらの方法は、いずれもＹの分離法と
して、充分に満足できるものとは言い難い。However, none of these methods can be said to be fully satisfactory as a method for separating Y.
即ち、前者の場合、Ｙと軽希士（ＬａからＥｕまで）と
の分離は良好に行なわれるが、蚤希士例えば原子番号６
４〜７１の希士の分離に関しては、満足すべき結果が得
られない。That is, in the former case, separation of Y and light rare metals (from La to Eu) is performed well;
Regarding the separation of numbers 4 to 71, satisfactory results were not obtained.
又、後者のイオン交換法の場合、得られる精製Ｙ水溶液
の濃度が小さく、濃縮にぼう大な設備と熱源が必要であ
るうえ、イオン交モ剣樹脂塔を流れる溶離液の流速が小
さいため生産性が低い。In addition, in the case of the latter ion exchange method, the concentration of the purified Y aqueous solution obtained is small, large-scale equipment and heat sources are required for concentration, and the flow rate of the eluent flowing through the ion exchange resin tower is low, making production difficult. low gender.
本発明者らは、Ｙと原子番号が６４〜７１の童希±の新
しい分離法について研究を行なった結果、従来法に比べ
極めて簡単にＹと原子番号６４〜７１の希士を分離しう
る方法を見し、出し、先に特許出願を行なった（特願昭
５１−６８３３２）。待顔昭５１−６８３３２の方法の
特徴は、ジェチレントリアミン五酢酸（以下「ＤＴＰＡ
」という）を含みかつ、Ｙと原子番号６４一７１の希±
を含有する混合水溶液をジー（２ーェチルヘキシル）リ
ン酸（以下「Ｄ班ＨＰＡｉという）のような酸性リン酸
ェステルと接触させることにより、Ｙと原子番号６４〜
７１の希土とを効果的に分離する点にある。The present inventors conducted research on a new separation method for Y and atomic numbers 64 to 71, and found that it is possible to separate Y and atomic numbers 64 to 71 more easily than conventional methods. He found a method, published it, and filed a patent application (Japanese Patent Application No. 68332/1983). The characteristics of the method of Machigao 1976-68332 are that jetylenetriaminepentaacetic acid (hereinafter referred to as "DTPA")
''), and Y and rare ± of atomic number 64-71.
By contacting the mixed aqueous solution containing
The point is that it effectively separates the 71 rare earths.
本発明者らは、Ｙの生産性を向上させる目的で、Ｙと原
子番号６４〜７１の希±との分離効率は低下させること
なく、Ｙの抽出速度を速める抽出溶媒系について鋭意検
討を行なった結果、従来法よりも抽出速度の遠い溶媒系
を見い出し「以下の発明に到達した。In order to improve the productivity of Y, the present inventors have conducted intensive studies on an extraction solvent system that accelerates the extraction rate of Y without reducing the separation efficiency between Y and dilute compounds with atomic numbers of 64 to 71. As a result, they discovered a solvent system with a faster extraction rate than conventional methods and achieved the following invention.
本発明はＤＴＰＡを含みかつＹと原子番号６４〜７１の
希士を含有する混合水溶液をＤ班ＨＰＡの溶液と接触さ
せることにより、Ｙと希±の分離を行なう点では、特願
昭５１−６８３３２と同じであるが、その特徴は、Ｄが
ＨＰＡの希釈溶媒として、■炭素数１０〜１４の脂肪族
炭化水素、■炭素数６〜１０の脂肪族アルコールより選
ばれる少くとも１種の有機溶媒を用いることにあり、上
記希釈溶媒を使用することによりＹの抽出速度が向上し
、生産性を高めることができる。The present invention is characterized in that Y and diluted substances are separated by contacting a mixed aqueous solution containing DTPA and Y and diluted elements with atomic numbers 64 to 71 with a solution of Group D HPA. It is the same as 68332, but its characteristics are that D is a diluent for HPA, and at least one kind of organic compound selected from ■ aliphatic hydrocarbons having 10 to 14 carbon atoms, and ■ aliphatic alcohols having 6 to 10 carbon atoms. By using the above diluent solvent, the extraction rate of Y can be improved and productivity can be increased.
以下本発明を詳細に説明する。The present invention will be explained in detail below.
本発明方法の対象は、Ｙと原子番号６４〜７１の希土の
少くとも一種を含む混合物であればよいが、とくに本発
明は、ＹとＤｙ（原子番号６６）乃至Ｌｕ（原子番号７
１）の重希土との分離に好適である。The object of the method of the present invention may be any mixture containing Y and at least one of rare earths having an atomic number of 64 to 71, but the present invention is particularly applicable to Y and Dy (atomic number 66) to Lu (atomic number 7).
Suitable for separation from heavy rare earth (1).
本発明の方法に適用されるＹ及び重希土を含有する水溶
液は通常０．００５〜２Ｍ′ぞと〈に０．０５〜０．５
Ｍ／そ程度の濃度のものが用いられる。本発明方法にお
いてＤ班ＨＰＡの希釈溶媒としては以下の有機溶媒の少
くとも１種が使用される。The aqueous solution containing Y and heavy rare earth applied to the method of the present invention is usually 0.005 to 2 M' and 0.05 to 0.5
A concentration of about M/M is used. In the method of the present invention, at least one of the following organic solvents is used as a diluting solvent for Group D HPA.
■ 炭素数１０〜１４の脂肪族炭化水素。■ Aliphatic hydrocarbons having 10 to 14 carbon atoms.
■ 炭素数６〜１０の脂肪族アルコール。■ Aliphatic alcohol with 6 to 10 carbon atoms.
炭素数９以下の脂肪族炭化水素を用いた場合には従釆法
で使用されているケロシンを希釈溶媒とした場合に比べ
、Ｙの抽出速度は同程度又はそれ以下となり効果がなく
、逆に炭素数１５以上の脂肪族炭化水素では融点が高く
（ｍｐｌｏ。When an aliphatic hydrocarbon with carbon number 9 or less is used, the extraction rate of Y is the same or lower than when kerosene, which is used in the conventional method, is used as a diluting solvent, making it ineffective. Aliphatic hydrocarbons with 15 or more carbon atoms have a high melting point (mplo.
０）かつ粘度も高くなるため扱いにくい。0) and the viscosity increases, making it difficult to handle.
また、炭素数５以下のアルコールでは、水に対する溶解
度がかなり大きいため使用中溶媒組成の変化が生じ不便
であり、逆に炭素数１１以上のアルコールでは融点が高
く（ｍｐ１６．９０）取り扱いに難がある。有機溶媒中
のＤ班ＨＰＡ濃度は０．０２〜１．５Ｍ′〆程度に選ぶ
のが抽出操作上好ましいが、Ｙの抽出速度はＤ斑ＨＰＡ
濃度が高いほど大きくなる。一方、本発明方法において
水溶液中に溶解させて使用されるＤＴＰＡは分離すべき
原子番号６４〜７１の車希±に対し、通常当量以上の量
で、かつ、Ｙ及び上記重希±の総量の０．４〜１．５倍
当量程度で使用される。ＤＴＰＡを含有し、かつ、Ｙ及
び原子番号６４〜７１の希±を含有する水溶液はｐＨＩ
．５以上９以下に調整するのが好ましく、ｐＨ１．５以
下では充分な分離効果を期待しえない。In addition, alcohols with carbon numbers of 5 or less have a considerably high solubility in water, which causes changes in the solvent composition during use, which is inconvenient, while alcohols with carbon numbers of 11 or more have a high melting point (mp 16.90) and are difficult to handle. be. It is preferable for the extraction operation to select the concentration of group D HPA in the organic solvent to be about 0.02 to 1.5 M', but the extraction rate of Y is lower than that of group D HPA.
The higher the concentration, the larger it becomes. On the other hand, in the method of the present invention, DTPA used dissolved in an aqueous solution is usually used in an amount equivalent to or more than the total amount of Y and the heavy diluted metal having an atomic number of 64 to 71 to be separated. It is used in an amount of about 0.4 to 1.5 times equivalent. An aqueous solution containing DTPA and containing Y and a dilute compound with an atomic number of 64 to 71 has a pH of
．． It is preferable to adjust the pH to 5 or more and 9 or less, and if the pH is 1.5 or less, a sufficient separation effect cannot be expected.
以上の如く本発明に従ってＹの精製を行なえば重希士と
Ｙの分離を一種類の抽出溶媒（Ｄ餌ＨＰＡ）を用いるこ
とによって、高純度Ｙをうろことができ、また、従来法
に比べ、Ｙの抽出速度が速いため、Ｙの生産性を高める
ことができる。As described above, if Y is purified according to the present invention, high-purity Y can be extracted by using one type of extraction solvent (D-bait HPA) to separate heavy oxidants and Y, and compared to conventional methods, , Y can be extracted at a high speed, so that the productivity of Y can be increased.
以下に本発明を実施例により更に具体的に説明する。The present invention will be explained in more detail below using examples.
実施例 １
０．０５Ｍ／そのＹＣ１３、０．０５Ｍ／そのＥｒＣ１
３、０．１１Ｍ／そのＤＴＰＡを含み、かつ溶液のｐＨ
を調整するためにＨＣＩ−ＣＨ３ＣＯＯＮＨ４緩衝液（
ＣＨ３ＣＯＯＮＨ４濃度０．９Ｍ′夕）を用いて舟３．
３に調整したフィード液１００の上を０．９Ｍ／そのＤ
班ＨＰＡを含むデカン溶液１００泌を用いて抽出を行な
った。Example 1 0.05M/YC13, 0.05M/ErC1
3, containing 0.11 M/its DTPA and the pH of the solution
HCI-CH3COONH4 buffer (
Boat 3.
0.9M/that D on the feed liquid 100 adjusted to 3.
Extraction was performed using a 100% decane solution containing HPA.
抽出時間は５分及び１５分とした。各抽出時間における
全抽出率及びＹ、Ｅｒそれぞれの抽出率を第１図に示す
。第１図において、曲線１はＹの抽出率を、曲線５は全
抽出率を、曲線８はＥｄ抽出率を表わす。比較例 １実
施例１と同じ組成のフィード液１００の‘を、０．５Ｍ
′そのＤ餌ＨＰＡを含む下記３種の溶媒■ノナン、■オ
クタン、■ケロシン１００の‘を用い実施例１と同じ抽
出条件下で抽出を行なった。Extraction times were 5 and 15 minutes. FIG. 1 shows the total extraction rate and the extraction rates of Y and Er at each extraction time. In FIG. 1, curve 1 represents the extraction rate of Y, curve 5 represents the total extraction rate, and curve 8 represents the extraction rate of Ed. Comparative Example 1 Feed liquid 100' with the same composition as Example 1 was added to 0.5M
Extraction was carried out under the same extraction conditions as in Example 1 using the following three solvents containing HPA: nonane, octane, and kerosene 100.
抽出時間はいずれも５分及び１８分とした。各抽出時間
に対する全抽出率及び、Ｙ、Ｅｒそれぞれの抽出率を第
１図に示す。第１図において「曲線２、曲線６及び曲線
１０がそれぞれノナンを希釈溶媒として用いた場合のＹ
の抽出率、全抽出率及びＥｒの抽出率を表わし、曲線４
、曲線７及び曲線１１がそれぞれオクタンを希釈溶媒と
して用いた場合のＹの抽出率、全抽出率及びＥｒの抽出
率を表わし、曲線３、曲線６及び曲線９がそれぞれケロ
シンを希釈溶媒として用いた場合のＹの抽出率、全抽出
率及びＥｒの抽出率を表わす。The extraction time was 5 minutes and 18 minutes in both cases. FIG. 1 shows the total extraction rate and the extraction rates of Y and Er for each extraction time. In Figure 1, "Curve 2, Curve 6 and Curve 10 are the Y when nonane is used as a diluting solvent."
Curve 4 represents the extraction rate of Er, the total extraction rate and the extraction rate of Er.
, curve 7 and curve 11 represent the extraction rate of Y, total extraction rate and extraction rate of Er when octane is used as the diluting solvent, respectively, and curve 3, curve 6 and curve 9 are respectively when kerosene is used as the diluting solvent. The extraction rate of Y, the total extraction rate, and the extraction rate of Er are shown for each case.
実施例 ２
実施例１と同じ組成のフイード液１００の乙を０．５Ｍ
′そのＤ班ＨＰＡを含むｎ−へキサノール溶液１００奴
を用いて抽出した。Example 2 0.5M of feed liquid 100 with the same composition as Example 1
'The D group was extracted using 100 ml of n-hexanol solution containing HPA.
抽出時間は５分、３０分及び９０分とした。各抽出時間
に対する全抽出率及びＹ、Ｅｒそれぞれの抽出率を第２
図に示す。第２図においてＬ曲線１２、曲線１４及び曲
線１５がそれぞれＹ抽出率、全抽出率及びＥｒ抽出率を
表わす。比較例 ２
実施例１と同じ組成のフィード液１００のＺを０．５Ｍ
／そのＤがＨＰＡを含むケロシン溶液１００机‘を用い
て抽出した。The extraction times were 5 minutes, 30 minutes and 90 minutes. The total extraction rate and each extraction rate of Y and Er for each extraction time are
As shown in the figure. In FIG. 2, L curve 12, curve 14, and curve 15 represent the Y extraction rate, the total extraction rate, and the Er extraction rate, respectively. Comparative Example 2 Feed liquid 100 with the same composition as Example 1 with Z of 0.5M
/The D was extracted using 100 volumes of kerosene solution containing HPA.
抽出時間は５分、３び分及び９０分とした。各抽出時間
に対する全抽出率及びＹ、Ｅｒそれぞれの抽出率を第２
図に示す。第２図において、曲線１３がＹ抽出率、曲線
Ｉ６が全抽出率、曲線１７がＥｄ母出率を表わす。The extraction times were 5 minutes, 3 minutes, and 90 minutes. The total extraction rate and each extraction rate of Y and Er for each extraction time are
As shown in the figure. In FIG. 2, curve 13 represents the Y extraction rate, curve I6 represents the total extraction rate, and curve 17 represents the Ed output rate.
第１図は実施例１及び比較例１の結果を、縦軸を抽出率
、機軸を抽出時間として図示したものであり、第２図は
同様に実施例２及び比較例２の結果を図示したものであ
る。
夕／図
汁２図Figure 1 shows the results of Example 1 and Comparative Example 1, with the vertical axis representing the extraction rate and the axis representing the extraction time. Figure 2 similarly shows the results of Example 2 and Comparative Example 2. It is something. Evening/Picture soup 2
Claims (1)
リウム及び原子番号６４〜７１の希土を含有する水溶液
よりジ−（２−エチルヘキシル）リン酸を抽出剤として
、イツトリウムを抽出分離するにあたり、ジ−（２−エ
チルヘキシル）リン酸を炭素数１０〜１４の脂肪族炭化
水素及び炭素数６〜１０の脂肪族アルコールより選ばれ
る少くとも１種の有機溶媒により希釈して用いることを
特徴とするイツトリウムの分離法。1 In extracting and separating yttrium from an aqueous solution containing diethylenetriaminepentaacetic acid and also containing yttrium and a rare earth with an atomic number of 64 to 71 using di-(2-ethylhexyl) phosphoric acid as an extractant, di-(2- A method for separating yttrium, characterized in that phosphoric acid (ethylhexyl) is diluted with at least one organic solvent selected from aliphatic hydrocarbons having 10 to 14 carbon atoms and aliphatic alcohols having 6 to 10 carbon atoms.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5804877A JPS605655B2 (en) | 1977-05-19 | 1977-05-19 | Separation method of yztrium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5804877A JPS605655B2 (en) | 1977-05-19 | 1977-05-19 | Separation method of yztrium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS53142310A JPS53142310A (en) | 1978-12-12 |
| JPS605655B2 true JPS605655B2 (en) | 1985-02-13 |
Family
ID=13073034
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5804877A Expired JPS605655B2 (en) | 1977-05-19 | 1977-05-19 | Separation method of yztrium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS605655B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2562059B1 (en) * | 1984-04-02 | 1989-12-01 | Rhone Poulenc Spec Chim | PROCESS FOR SEPARATING RARE EARTH BY LIQUID-LIQUID EXTRACTION |
-
1977
- 1977-05-19 JP JP5804877A patent/JPS605655B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS53142310A (en) | 1978-12-12 |
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