JPH0785772B2 - Lithium isotope separation agent - Google Patents
Lithium isotope separation agentInfo
- Publication number
- JPH0785772B2 JPH0785772B2 JP14712493A JP14712493A JPH0785772B2 JP H0785772 B2 JPH0785772 B2 JP H0785772B2 JP 14712493 A JP14712493 A JP 14712493A JP 14712493 A JP14712493 A JP 14712493A JP H0785772 B2 JPH0785772 B2 JP H0785772B2
- Authority
- JP
- Japan
- Prior art keywords
- lithium
- separation
- isotope
- isotopes
- agent
- 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 - Lifetime
Links
- 229910052744 lithium Inorganic materials 0.000 title claims description 37
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims description 36
- 238000005372 isotope separation Methods 0.000 title claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 19
- AQTIRDJOWSATJB-UHFFFAOYSA-K antimonic acid Chemical compound O[Sb](O)(O)=O AQTIRDJOWSATJB-UHFFFAOYSA-K 0.000 claims description 12
- 238000000034 method Methods 0.000 description 21
- 238000000926 separation method Methods 0.000 description 18
- 238000001179 sorption measurement Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910000497 Amalgam Inorganic materials 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 239000003456 ion exchange resin Substances 0.000 description 3
- 229920003303 ion-exchange polymer Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000010457 zeolite Substances 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
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 150000002642 lithium compounds Chemical class 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- YBJHBAHKTGYVGT-ZKWXMUAHSA-N (+)-Biotin Chemical compound N1C(=O)N[C@@H]2[C@H](CCCCC(=O)O)SC[C@@H]21 YBJHBAHKTGYVGT-ZKWXMUAHSA-N 0.000 description 1
- NLMDJJTUQPXZFG-UHFFFAOYSA-N 1,4,10,13-tetraoxa-7,16-diazacyclooctadecane Chemical compound C1COCCOCCNCCOCCOCCN1 NLMDJJTUQPXZFG-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- VMPVEPPRYRXYNP-UHFFFAOYSA-I antimony(5+);pentachloride Chemical compound Cl[Sb](Cl)(Cl)(Cl)Cl VMPVEPPRYRXYNP-UHFFFAOYSA-I 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000002739 cryptand Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- FEPMHVLSLDOMQC-UHFFFAOYSA-N virginiamycin-S1 Natural products CC1OC(=O)C(C=2C=CC=CC=2)NC(=O)C2CC(=O)CCN2C(=O)C(CC=2C=CC=CC=2)N(C)C(=O)C2CCCN2C(=O)C(CC)NC(=O)C1NC(=O)C1=NC=CC=C1O FEPMHVLSLDOMQC-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は新規なリチウム同位体分
離剤に関するものである。更に詳しく言えば本発明はリ
チウム同位体の分離性能に優れた立方晶系のアンチモン
酸からなるリチウム同位体分離剤に関するものである。FIELD OF THE INVENTION The present invention relates to a novel lithium isotope separation agent. More specifically, the present invention relates to a lithium isotope separating agent comprising cubic antimonic acid, which is excellent in lithium isotope separation performance.
【０００２】[0002]
【従来の技術】近年、リチウムは、例えばセラミック
ス、グリース、空調用冷媒、医薬品、電池等の原料とし
て使用されており、また将来は、アルミニウム合金材料
などに用いられる重要な物質として注目されている。こ
れらはいずれも原子量６及び７のリチウム同位体の混合
物がその原料として用いられているが、それぞれ単一の
原子量のものに分離されたリチウムは原子力分野におい
て有用であり、例えば原子量６のリチウムは核融合炉用
の原料として、原子量７のリチウムは、原子力発電にお
ける中性子捕捉剤として注目されている。このため、混
合溶液からのリチウム同位体の相互分離技術の確立が強
く要望されている。2. Description of the Related Art In recent years, lithium has been used as a raw material for ceramics, grease, air-conditioning refrigerants, pharmaceuticals, batteries, etc., and in the future, it has been attracting attention as an important substance used for aluminum alloy materials and the like. . A mixture of lithium isotopes having an atomic weight of 6 and 7 is used as a raw material for each of these, and lithium separated into a single atomic weight is useful in the field of nuclear energy. For example, lithium having an atomic weight of 6 is As a raw material for a nuclear fusion reactor, lithium with an atomic weight of 7 has been attracting attention as a neutron capture agent in nuclear power generation. Therefore, there is a strong demand for establishment of mutual separation technology for lithium isotopes from the mixed solution.
【０００３】従来、リチウム同位体の分離方法として
は、例えばアマルガム法、溶融塩法、蒸留法、吸着法な
どが知られている。アマルガム法は、リチウムを水銀ア
マルガムとして電解することによって同位体を分離する
方法であるが、水銀を用いることから環境衛生上、大き
な問題がある。溶融塩法はリチウム化合物を加熱して溶
融状態にし、電気泳動を行って同位体を分離する方法で
あるが、加熱に高いエネルギーを要し、また装置が複雑
であるため分離コストが高くつくのを免れないという欠
点がある。蒸留法はリチウム金属やリチウム化合物を蒸
発させ同位体を分離する方法であるが、原材料が高価で
あることや高温にする必要があることから、やはり分離
コストが高くなるという欠点がある。Conventionally, as a method for separating lithium isotopes, for example, an amalgam method, a molten salt method, a distillation method, an adsorption method and the like are known. The amalgam method is a method for separating isotopes by electrolyzing lithium as mercury amalgam. However, since it uses mercury, it has a big problem in environmental hygiene. The molten salt method is a method in which a lithium compound is heated to a molten state and electrophoresed to separate isotopes, but it requires high energy for heating and the apparatus is complicated, so the separation cost is high. There is a drawback that you cannot escape. The distillation method is a method of separating isotopes by evaporating lithium metal or a lithium compound, but it also has a drawback that the separation cost is high because the raw materials are expensive and it is necessary to raise the temperature.
【０００４】これらの方法に対し、吸着法はイオン交換
反応など溶液から固相への吸着反応を利用して同位体を
分離する方法であり、常温で操作でき、かつ、装置が簡
単であるため、分離方法として適当な方法であるが、同
位体分離を行うためには、分離性能の高い吸着剤を使用
しなければならない。リチウム同位体の分離剤として
は、従来強酸性イオン交換樹脂やゼオライトが知られて
いる。しかしながら、強酸性イオン交換樹脂は６Ｌｉと
７Ｌｉとの分離係数が１．００２と低いため、リチウム
同位体の完全な分離を行うためには、大量の樹脂を用
い、かつ分離処理を精密に行う必要があるなどの問題を
有しており、一方、ゼオライトは該分離係数が１．００
４〜１．００６と比較的高いものの、水溶液中で不安定
であるという欠点を有している。In contrast to these methods, the adsorption method is a method for separating isotopes by utilizing an adsorption reaction from a solution to a solid phase such as an ion exchange reaction, and can be operated at room temperature and has a simple apparatus. Although it is a suitable separation method, an adsorbent having high separation performance must be used in order to perform isotope separation. As a lithium isotope separating agent, a strongly acidic ion exchange resin and zeolite have been conventionally known. However, the strong acid ion exchange resin is 6 Li
7 Since the separation coefficient from Li is as low as 1.002, in order to completely separate lithium isotopes, there is a problem that a large amount of resin must be used and the separation treatment must be performed precisely. On the other hand, zeolite has a separation factor of 1.00.
Although it is relatively high at 4 to 1.006, it has the drawback of being unstable in an aqueous solution.
【０００５】また、有機クリプタンド樹脂を用いるリチ
ウム同位体の分離方法についても報告されているが、こ
の方法においては、樹脂の製造コストが高くつく上、分
離効率が重分ではないという欠点がある。Further, a method for separating a lithium isotope using an organic cryptand resin has been reported, but this method has drawbacks that the production cost of the resin is high and the separation efficiency is not serious.
【０００６】[0006]
【発明が解決しようとする課題】化学交換法によるリチ
ウム同位体の分離においては、分離効率が高く、かつ水
溶液中で安定な分離剤が必要である。この問題が解決で
きれば効率的かつ経済的なリチウム同位体分離プロセス
を構築することができる。In the separation of lithium isotopes by the chemical exchange method, a separation agent having high separation efficiency and stable in an aqueous solution is required. If this problem can be solved, an efficient and economical lithium isotope separation process can be constructed.
【０００７】本発明は、このような要件を満足しうるリ
チウム同位体分離剤を提供することを目的としてなされ
たものである。The present invention has been made for the purpose of providing a lithium isotope separation agent which can satisfy such requirements.
【０００８】[0008]
【課題を解決するための手段】本発明者らは、前記目的
を達成するために鋭意研究を重ねた結果、立方晶系アン
チモン酸がリチウム同位体に対して高い分離効率を示す
ことを見いだし、この知見に基づいて本発明を完成する
に至った。すなわち、本発明は効率的かつ経済的にリチ
ウム同位体を分離するための分離剤を提供するものであ
る。Means for Solving the Problems As a result of intensive studies for achieving the above-mentioned object, the present inventors have found that cubic antimonic acid exhibits high separation efficiency for lithium isotopes, The present invention has been completed based on this finding. That is, the present invention provides a separating agent for separating lithium isotopes efficiently and economically.
【０００９】本発明分離剤である立方晶系アンチモン酸
は、五塩化アンチモンを加水分解して得た無定形アンチ
モン酸の沈澱、あるいはアンチモン酸カリウムを硝酸な
どの酸溶液で処理して得られた無定形アンチモン酸の沈
澱を３０〜７０℃で長時間熟成することによって合成さ
れる。得られた立方晶系アンチモン酸はＦｄ３ｍの空間
群に属し、その格子定数は１０．４±０．１オングスト
ロームである。該アンチモン酸はナトリウム選択吸着性
に優れ、かつ水溶液中で安定であることから、混合塩溶
液からのナトリウム除去、回収用吸着剤として用いられ
ている。The cubic antimonic acid which is the separating agent of the present invention was obtained by precipitating amorphous antimonic acid obtained by hydrolyzing antimony pentachloride or by treating potassium antimonate with an acid solution such as nitric acid. It is synthesized by aging the precipitation of amorphous antimonic acid at 30 to 70 ° C. for a long time. The obtained cubic antimonic acid belongs to the space group of Fd3m, and its lattice constant is 10.4 ± 0.1 angstrom. Since antimonic acid has excellent sodium selective adsorption and is stable in an aqueous solution, it is used as an adsorbent for removing and recovering sodium from a mixed salt solution.
【００１０】従って、該アンチモン酸はリチウム選択吸
着性はないものの、リチウムが吸着する際の脱水和のエ
ネルギーが６Ｌｉと７Ｌｉで異なることを利用して高効
率でリチウム同位体を分離することができる。この立方
晶アンチモン酸は、通常粉末状のものであるが、それを
そのままリチウム同位体分離剤として用いてもよいし、
粉末を造粒し、粒状体として用いてもよく、あるいは繊
維状または膜状に成形してもよい。Therefore, although the antimonic acid does not have a lithium selective adsorption property, it is possible to separate lithium isotopes with high efficiency by utilizing the fact that the energy of dehydration when lithium is adsorbed differs between 6 Li and 7 Li. You can This cubic antimonic acid is usually in powder form, but it may be used as it is as a lithium isotope separation agent,
The powder may be granulated and used as a granular body, or may be formed into a fiber or a film.
【００１１】このような立方晶系アンチモン酸からなる
リチウム同位体分離剤を用いてリチウム同位体を分離す
るには、リチウム同位体を含有する混合溶液中に、該分
離剤を加え、リチウムの吸着処理を行う工程を繰り返し
行えばよい。自然に安定に存在する６Ｌｉと７Ｌｉのう
ち、該分離剤により強く吸着される６Ｌｉは段階的に固
相中に移行し、一方溶液中の７Ｌｉの割合は段階的に高
くなり、相互分離が完成する。In order to separate a lithium isotope using such a lithium isotope separating agent comprising cubic antimonic acid, the separating agent is added to a mixed solution containing a lithium isotope and lithium is adsorbed. The process of performing the treatment may be repeated. Of 6 Li and 7 Li naturally occurring stable, 6 Li is strongly adsorbed by the separating agent stepwise shifts to the solid phase, whereas the ratio of 7 Li in the solution stepwise increases, Mutual separation is completed.
【００１２】一般的には粒状に成形した該分離剤を充填
したクロマトグラフィー用カラムを作成して分離を行う
方法が用いられる。すなわち、該カラム中にリチウム同
位体を含有する混合溶液を一定量流すことによってリチ
ウム吸着帯を形成し、次いで溶離液を該カラムの上部よ
り流し続けることによってリチウム吸着帯を移動させて
同位体の分離を行う。この際、溶離液としては通常、中
性ないし酸性の水溶液が用いられる。この方法により、
該分離剤により強く吸着する６Ｌｉを後端側に、より弱
く吸着する７Ｌｉを前端側に濃縮させることができる。
このような吸着−溶離による同位体の分離処理は、繊維
状あるいは膜状の分離剤を用いて行うこともできる。[0012] Generally, a method is used in which a column for chromatography filled with the separating agent formed in a granular form is prepared and separation is performed. That is, a fixed amount of a mixed solution containing a lithium isotope is flowed in the column to form a lithium adsorption zone, and then the eluent is continuously flowed from the upper part of the column to move the lithium adsorption zone to move the isotope of the isotope. Perform separation. At this time, a neutral or acidic aqueous solution is usually used as the eluent. By this method,
The 6 Li strongly adsorbed by the separating agent can be concentrated on the rear end side, and the weakly adsorbed 7 Li can be concentrated on the front end side.
Such isotope separation treatment by adsorption-elution can also be performed using a fibrous or membrane-like separating agent.
【００１３】[0013]
【発明の効果】本発明のリチウム同位体分離剤を用いる
ことによって、リチウム同位体を含有する混合溶液から
６Ｌｉと７Ｌｉの分離を高効率にかつ経済的に行うこと
ができる。EFFECTS OF THE INVENTION By using the lithium isotope separation agent of the present invention, a lithium isotope-containing mixed solution can be obtained.
Separation of 6 Li and 7 Li can be performed with high efficiency and economically.
【００１４】[0014]
【実施例】次に、実施例により本発明を更に詳細に説明
するが、本発明はこれらの例によってなんら限定される
ものではない。EXAMPLES Next, the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.
【００１５】実施例 立方晶系アンチモン酸０．１ｇを０．１Ｍの水酸化リチ
ウム１０ｍＬ中に浸漬し、２５℃で１週間振とうした。
振とう後のリチウム吸着量は４１．５ｍｇ／ｇであり、
溶液中のリチウムの５９％が吸着した。原液及び吸着後
の上澄み液中の７Ｌｉ／６Ｌｉ同位体モル比を表面電離
型質量分析装置で測定したところ、それぞれ１２．５６
４１及び１２．７３６１であった。分離係数Ｓを式Example 0.1 g of cubic antimonic acid was immersed in 10 mL of 0.1 M lithium hydroxide and shaken at 25 ° C. for 1 week.
The lithium adsorption amount after shaking was 41.5 mg / g,
59% of the lithium in the solution was adsorbed. The molar ratios of 7 Li / 6 Li isotopes in the stock solution and the supernatant after adsorption were measured by a surface ionization mass spectrometer, and each was 12.56.
41 and 12.7361. Separation factor S
【数１】 ［ただし、（７Ｌｉ／６Ｌｉ）ｓｏｌｎ．は溶液中の同
位体比、（７Ｌｉ／６Ｌｉ）ａｄ．は分離剤中の同位体
比であるに従って計算したところ１．０２６であった。[Equation 1] [However, ( 7 Li / 6 Li) soln. Is the isotope ratio in the solution, ( 7 Li / 6 Li) ad. Was calculated to be 1.026 according to the isotope ratio in the separating agent.
【００１６】このことから、本発明の分離剤はイオン交
換樹脂やゼオライトに比べて、高い同位体分離性能を有
することは明らかである。From this, it is clear that the separating agent of the present invention has higher isotope separation performance than ion-exchange resins and zeolites.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 加納 博文 香川県高松市花ノ宮町二丁目３番３号 工 業技術院四国工業技術試験所内 (72)発明者 馮 旗 香川県高松市花ノ宮町二丁目３番３号 工 業技術院四国工業技術試験所内 (56)参考文献 特開 昭61−33220（ＪＰ，Ａ) 特公 平３−25760（ＪＰ，Ｂ２) 特公 平５−9374（ＪＰ，Ｂ２) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Hirofumi Kano Inventor Hirofumi Kano 2-3-3 Hananomiya-cho, Takamatsu-shi, Kagawa Inside Shikoku Institute of Industrial Technology, Industrial Technology Institute (72) Inventor Feng Flag 2-chome, Hananomiya-cho, Takamatsu, Kagawa No. 3-3 Inside Shikoku Industrial Technology Laboratory, Institute of Industrial Technology (56) Reference Japanese Patent Laid-Open No. 61-33220 (JP, A) Japanese Patent Publication 3-25760 (JP, B2) Japanese Patent Publication 5-9374 (JP, B2) )
Claims (1)
同位体分離剤1. A lithium isotope separation agent comprising cubic antimonic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14712493A JPH0785772B2 (en) | 1993-05-13 | 1993-05-13 | Lithium isotope separation agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14712493A JPH0785772B2 (en) | 1993-05-13 | 1993-05-13 | Lithium isotope separation agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06319956A JPH06319956A (en) | 1994-11-22 |
| JPH0785772B2 true JPH0785772B2 (en) | 1995-09-20 |
Family
ID=15423091
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14712493A Expired - Lifetime JPH0785772B2 (en) | 1993-05-13 | 1993-05-13 | Lithium isotope separation agent |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0785772B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4936442B2 (en) * | 2006-11-14 | 2012-05-23 | 独立行政法人産業技術総合研究所 | Lithium isotope separation agent and method for producing lithium isotope concentrate using the same |
-
1993
- 1993-05-13 JP JP14712493A patent/JPH0785772B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH06319956A (en) | 1994-11-22 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |