JPH0810274B2 - Method for regenerating organic solvent containing tributyl phosphite - Google Patents
Method for regenerating organic solvent containing tributyl phosphiteInfo
- Publication number
- JPH0810274B2 JPH0810274B2 JP8363786A JP8363786A JPH0810274B2 JP H0810274 B2 JPH0810274 B2 JP H0810274B2 JP 8363786 A JP8363786 A JP 8363786A JP 8363786 A JP8363786 A JP 8363786A JP H0810274 B2 JPH0810274 B2 JP H0810274B2
- Authority
- JP
- Japan
- Prior art keywords
- organic solvent
- tbp
- uranium
- ion exchange
- solvent
- 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 - Fee Related
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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、ウランの再転換工程やウランスクラツプ回
収工程に用いられるトリブチルフオスフエート含有有機
溶媒の再生処理方法に関するものである。TECHNICAL FIELD The present invention relates to a method for regenerating a tributylphosphate-containing organic solvent used in a uranium reconversion step and a uranium scrap recovery step.
六弗化ウラン（UF6）から二酸化ウラン（UO2）を得る
（これをウランの再転換という）ため種々の方法が行な
われている。その中の一つに、UF6ガスを硝酸アルミニ
ウム水溶液に吹き込んで硝酸ウラニル（UO2（NO3）２）
を生成せしめ、該UO2（NO3）２をトリブチルフオスフエ
ート（TBPと略記する）含有有機溶媒で抽出精製し、精
製UO2（NO3）２をアンモニアと反応させて重ウラン酸ア
ンモニウムとして沈殿させ、該沈殿物を仮焼してU3O8と
し、これを水素で還元してUO2粉末とする方法がある。
この方法は上記のように溶媒抽出による精製工程がある
ため、弗素混入の少ないUO2粉末が得られる点で優れて
いる。このようなTBP溶媒抽出は、ウランスクラツプか
らウランを回収する場合にも適用されている。Various methods are used to obtain uranium dioxide (UO 2 ) from uranium hexafluoride (UF 6 ) (this is called reconversion of uranium). Uranyl nitrate (UO 2 (NO 3 ) 2 ) was produced by blowing UF 6 gas into an aqueous solution of aluminum nitrate.
UO 2 (NO 3 ) 2 is extracted and purified with an organic solvent containing tributylphosphate (abbreviated as TBP), and the purified UO 2 (NO 3 ) 2 is reacted with ammonia to give ammonium diuranate. There is a method of precipitating and calcining the precipitate to U 3 O 8 and reducing this with hydrogen to obtain UO 2 powder.
Since this method has a purification step by solvent extraction as described above, it is excellent in that UO 2 powder containing less fluorine can be obtained. Such TBP solvent extraction is also applied when recovering uranium from a uranium scrap.
上記TBPはケロシン、ドデカン等の炭化水素油で希釈
して用いられ、TBPの含有率は通常30〜40容量％とされ
ている。ところでこのTBP含有有機溶媒は上記の工程に
おいて絶えずウランや硝酸と接触するため、放射線によ
る損傷、化学的な損傷を受け、次第に逆抽出性能が低下
してくる。この逆抽出性能の低下現象はおよそ次のよう
に考えられている。即ち、TBPが分解すると、ジブチル
フオスフエート（DBP）、モノブチルフオスフエート（M
BP）、ブタノール、リン酸等を生成し、炭化水素油が硝
酸によつて酸化され、又分解してカルボン酸、ニトロ化
合物、ヒドロキサム酸等を生成し、これらの分解生成物
のいくつかがウランと強固に結合して逆抽出を妨げるこ
とになる。このように逆抽出性能が低下すると有機溶媒
中に残留するウラン濃度が増大し、ウランの損失が大き
くなると共に抽出能力も低下するので、劣化がある程度
まで達すればこの溶媒を新しい溶媒と交換しなければな
らない。The TBP is used by diluting it with a hydrocarbon oil such as kerosene or dodecane, and the content of TBP is usually 30 to 40% by volume. By the way, this TBP-containing organic solvent constantly contacts with uranium and nitric acid in the above-mentioned step, so that the TBP-containing organic solvent is damaged by radiation and chemically damaged, and the back-extraction performance is gradually lowered. It is considered that the deterioration phenomenon of the back extraction performance is as follows. That is, when TBP is decomposed, dibutylphosphonate (DBP), monobutylphosphate (M
BP), butanol, phosphoric acid, etc., hydrocarbon oil is oxidized by nitric acid, and decomposes to form carboxylic acid, nitro compound, hydroxamic acid, etc. Some of these decomposition products are uranium. Binds tightly with and prevents back extraction. When the back extraction performance is decreased in this way, the concentration of uranium remaining in the organic solvent increases, the loss of uranium increases, and the extraction capacity also decreases, so if the deterioration reaches to a certain extent, this solvent must be replaced with a new solvent. I have to.
しかしながらこのように劣化したTBP含有有機溶媒は
上記のようにウランを含有しており、これは永久に保管
しなければならず、この保管のためのスペース及び費用
が必要である。又、TBPは高価であり、新しいTBPを逐次
購入することも経済的に負担である。劣化したTBP含有
有機溶媒を何らかの手段で再生できれば繰返し使用が可
能となり、保管スペース及び費用の減少と新しい溶媒の
購入量の圧縮を図ることができ、極めて好都合である。
このため劣化溶媒の再生処理技術の確立が強く要請され
ていた。However, the TBP-containing organic solvent thus deteriorated contains uranium as described above, and it must be stored permanently, and space and cost for this storage are required. In addition, TBP is expensive, and purchasing new TBP one after another is economically burdensome. If the deteriorated TBP-containing organic solvent can be regenerated by some means, it can be used repeatedly, which can reduce the storage space and cost and reduce the purchase amount of new solvent, which is extremely convenient.
Therefore, there has been a strong demand for establishment of a regeneration treatment technology for the deteriorated solvent.
本発明は、上記事情に鑑みて為されたもので、劣化し
たTBP含有有機溶媒を効果的に再生処理する方法を提供
するものである。The present invention has been made in view of the above circumstances, and provides a method for effectively regenerating a deteriorated TBP-containing organic solvent.
この目的を達成するため本発明の方法は、劣化したTB
P含有有機溶媒をアルカリ水溶液で洗浄処理して有機相
と水相とに分離した後、該水相をアンモニアで処理して
ウランを回収する一方、該有機相を粗大網状イオン交換
樹脂によりイオン交換処理してトリブチルフオスフエー
ト含有有機溶媒を再生する点に特徴がある。To achieve this goal, the method of the present invention uses degraded TB
After the P-containing organic solvent is washed with an alkaline aqueous solution to separate it into an organic phase and an aqueous phase, the aqueous phase is treated with ammonia to recover uranium, while the organic phase is subjected to ion exchange with a coarse reticulated ion exchange resin. It is characterized in that the organic solvent containing tributylphosphate is regenerated by treatment.
本発明において劣化溶媒を先ずアルカリ洗浄するの
は、次工程におけるイオン交換樹脂への負荷を軽減して
樹脂寿命（この場合の寿命はイオン交換能が消耗する時
間を云う）を延長すると共に、ウランの回収を容易にす
るためである。In the present invention, the deteriorated solvent is first washed with an alkali in order to reduce the load on the ion exchange resin in the next step and extend the resin life (the life in this case means the time when the ion exchange capacity is consumed), and This is to facilitate the collection of
本発明に用いるアルカリ水溶液にはナトリウム、カリ
ウム、カルシウムの炭酸塩、水酸化物のほか炭酸アンモ
ニウム、アンモニア水等が使用できる。これらは複数種
併用しても良い。該溶液の濃度は５〜15重量％程度が適
当である。洗浄処理は、TBP含有有機溶媒10容に対して
アルカリ水溶液１〜５容程度の割合で接触せしめれば良
い。この接触方式は混合が良く行なわれるものであれば
どのような方式でも良く、撹拌法、パルスカラム法等適
当な手段を選択して良い。このアルカリ洗浄によれば劣
化物の主たる成分であるTBP分解生成物の殆どを水相に
移して有機相から除去することができる。しかしながら
このアルカリ洗浄では希釈剤である炭化水素油の劣化物
質、特にニトロ化合物は効果的に除去することができな
い。このニトロ化合物の除去は次工程の粗大網状イオン
交換樹脂を用いるイオン交換処理によつて殆んど完全に
行なうことができる。As the alkaline aqueous solution used in the present invention, sodium carbonate, potassium carbonate, calcium carbonate, hydroxide, ammonium carbonate, aqueous ammonia and the like can be used. These may be used in combination. The concentration of the solution is preferably about 5 to 15% by weight. The washing treatment may be performed by contacting the TBP-containing organic solvent with 10 volumes of an alkaline aqueous solution in a ratio of about 1 to 5 volumes. This contact method may be any method as long as mixing is performed well, and an appropriate means such as a stirring method or a pulse column method may be selected. By this alkali cleaning, most of the TBP decomposition products, which are the main components of the deteriorated products, can be transferred to the aqueous phase and removed from the organic phase. However, this alkaline cleaning cannot effectively remove the deteriorated substances of the hydrocarbon oil as a diluent, especially the nitro compounds. The removal of the nitro compound can be almost completely performed by the ion exchange treatment using the coarse reticulated ion exchange resin in the next step.
粗大網状イオン交換樹脂はスチレン−ジビニルベンゼ
ンコポリマー類であつて、４級アンモニウム性官能基を
有するものを強塩基性陰イオン交換樹脂、アミノ性官能
基を有するものを弱塩基性陰イオン交換樹脂、スルフオ
ン酸官能基を有するものを陽イオン交換樹脂と云い、こ
の形式の樹脂は、例えば米国ローム−アンド−ハース社
（Rohm＆Haas Company）からアンバーリスト（Amberlys
t）の商品名で市販されている。上記ニトロ化合物の除
去にはこのうちの強塩基性粗大網状陰イオン交換樹脂が
最も適している。しかしニトロ化合物以外のものを除去
するためには他のものを使用すると良い。イオン交換処
理はこのような樹脂の充填層（ベツド）に前記アルカリ
洗浄済のTBP含有有機溶媒（有機相）を通過せしめるこ
とによつて行なわれる。Coarse reticulated ion exchange resins are styrene-divinylbenzene copolymers, those having a quaternary ammonium functional group are strongly basic anion exchange resins, those having amino functional groups are weak basic anion exchange resins, Those having sulfonate functional groups are referred to as cation exchange resins, and resins of this type are available from Amberlys, such as those available from Rohm & Haas Company, USA.
It is marketed under the trade name of t). Of these, the strongly basic coarse reticulated anion exchange resin is most suitable for removing the nitro compound. However, in order to remove other than the nitro compound, another one should be used. The ion exchange treatment is carried out by passing the alkali-cleaned TBP-containing organic solvent (organic phase) through a packed bed (bed) of such a resin.
通液量は１時間当り充填樹脂量の４〜６倍（即ち、４
〜６ベツドボリユーム/hr）が適当な範囲である。粗大
網状イオン交換樹脂はTBP分解生成物を除去する能力も
あるが、これらは前工程のアルカリ洗浄で除去されるの
でその分だけ負荷が軽減され、樹脂寿命が延長される。The flow rate is 4 to 6 times the volume of the filled resin per hour (ie
~ 6 beds volume / hr) is a suitable range. The coarse reticulated ion exchange resin has the ability to remove TBP decomposition products, but since these are removed by the alkali washing in the previous step, the load is reduced correspondingly and the resin life is extended.
本発明においてアルカリ洗浄とイオン交換処理は必ず
しも連続して行なう必要はなく、通常劣化したTBP含有
有機溶媒に含有される分解生成物はTBP分解生成物が大
部分であるので、アルカリ洗浄再生のみで再使用するこ
とを複数回（例えば10〜15回）行なつた後にイオン交換
処理を１回行なうという割合で再生処理すれば充分であ
る。このような場合TBP含有有機溶媒中にはニトロ化合
物が濃縮しているので、イオン交換における溶媒の処理
量は充填樹脂量の約80〜90倍量となる。In the present invention, the alkali cleaning and the ion exchange treatment do not necessarily have to be continuously performed, and since the decomposition products usually contained in the deteriorated TBP-containing organic solvent are mostly TBP decomposition products, only alkali cleaning regeneration is necessary. It is sufficient to perform the regeneration treatment at a rate of performing the ion exchange treatment once after the reuse is performed plural times (for example, 10 to 15 times). In such a case, since the nitro compound is concentrated in the TBP-containing organic solvent, the treatment amount of the solvent in the ion exchange is about 80 to 90 times the filling resin amount.
アルカリ洗浄工程では、TBP分解生成物のほか、炭化
水素油の劣化物質であるカルボン酸、ヒドロキサム酸等
が除去され、これらに結合しているウランも一緒にアル
カリ洗浄液（水相）に入る。この洗浄廃液に炭酸塩が含
有される場合は一旦酸性にして脱炭酸した後、又炭酸塩
を含有しない場合はそのまゝアンモニアを添加すればウ
ランを重ウラン酸アンモニウムとして沈殿回収すること
ができる。又、洗浄液中にアンモニアが存在すればウラ
ンは直ちに重ウラン酸アンモニウムを生成して沈殿する
ので、そのまゝ固液分離すれば良い。母液は低レベル放
射性廃液となり、これは他の雑廃水と共に別途処理され
る。In the alkaline washing step, in addition to the TBP decomposition products, carboxylic acids, hydroxamic acids, etc., which are deterioration substances of hydrocarbon oil, are removed, and uranium bound to these is also introduced into the alkaline washing liquid (aqueous phase). When carbonate is contained in this washing waste liquid, it is possible to precipitate and recover uranium as ammonium diuranate by acidifying and decarboxylating it once, and adding carbonate if it does not contain carbonate. . Further, if ammonia is present in the cleaning liquid, uranium immediately forms ammonium diuranate and precipitates, so that solid-liquid separation may be performed. The mother liquor becomes a low level radioactive effluent, which is treated separately with other miscellaneous wastewater.
一方使用済の粗大網状イオン交換樹脂は、HNU3−HFと
NaOHで再生することも可能であるが、この再生液の処理
は比較的難しく、むしろ廃棄するのが得策である。この
場合樹脂をそのまゝ保管しても良いが、灰化して減容す
るのが好ましく、又灰化すればウランの抽出も容易とな
り、これからウランを回収することも可能となる。On the other hand, the used coarse reticulated ion exchange resin is HNU 3 -HF.
Although it is possible to regenerate with NaOH, it is relatively difficult to process this regenerant and it is better to discard it. In this case, the resin may be stored as it is, but it is preferable to reduce the volume by ashing, and if the ashing is performed, the extraction of uranium becomes easy and the uranium can be recovered from this.
ウランの再転換工程に用い、逆抽出後のウラン濃度が
約100mg/となつたTBP含有有機溶媒（TBP35容量％、ｎ
−ドデカン65容量％）3000と５重量％のNa2CO3水溶液
300を槽中で撹拌混合した後静置して有機相と水相を
分離した。この洗浄を２回行なつた後、アルカリ洗浄済
の有機相の一部を、アンバーリストＡ−26（米国ローム
・アンド・ハース社製の強塩基製粗大網状陰イオン交換
樹脂の商品名）10を充填したカラム中に、流速４ベツ
ドボリユーム/hrで通液し、イオン交換処理した。Used in the uranium reconversion process, the TBP-containing organic solvent (TBP 35% by volume, n
-Dodecane 65% by volume) 3000 and 5% by weight Na 2 CO 3 aqueous solution
300 was stirred and mixed in a tank and then left to stand to separate an organic phase and an aqueous phase. After this washing was carried out twice, a part of the alkali-washed organic phase was amberlist A-26 (trade name of a coarse base reticulated anion exchange resin manufactured by Rohm and Haas Company, USA). The solution was passed through the column filled with the solution at a flow rate of 4 bed volumes / hr to carry out ion exchange treatment.
上記アルカリ洗浄のみ行なつた溶媒とイオン交換まで
行なつた溶媒について、逆抽出性能の比較試験を行なつ
た。この試験は溶媒各50mlを分液漏斗に入れ、これにウ
ランを14g/含有する硝酸濃度１規定の水溶液20mlを加
えてよく振り混ぜてウランを有機溶媒中に抽出し、次い
で該有機溶媒を純水で数回逆抽出操作を行なつて逆抽出
で達成しうる残留ウラン濃度の最低限の値を求めた。そ
の結果、アルカリ洗浄のみ行なつた溶媒の残留ウラン濃
度は約10mg/、イオン交換まで行なつた溶媒は1mg/
以下であつた。この試験の結果からアルカリ洗浄のみで
もかなり逆抽出性能を回復できるが、アルカリ洗浄では
除去し得ない劣化物質があること、この劣化物質は粗大
網状イオン交換樹脂によつて充分除去されていること、
が判る。A comparison test of the back extraction performance was carried out for the solvent which was only subjected to the alkali cleaning and the solvent which was subjected to the ion exchange. In this test, 50 ml of each solvent was placed in a separatory funnel, 20 ml of an aqueous solution containing 14 g of uranium and having a nitric acid concentration of 1 N was added, and the mixture was shaken well to extract uranium into an organic solvent. The minimum residual uranium concentration that can be achieved by back extraction was determined by performing back extraction with water several times. As a result, the residual uranium concentration of the solvent that was only washed with alkali was about 10 mg /, and the solvent that had been subjected to ion exchange was 1 mg /.
It was as follows. From the results of this test, it is possible to recover the back-extracting performance only by alkali washing, but there is a deteriorated substance that cannot be removed by alkali washing, and this deteriorated substance is sufficiently removed by the coarse reticulated ion exchange resin.
I understand.
本発明により、劣化したTBP含有有機溶媒を新品と同
程度の性能に再生回復することができた。これによつて
劣化溶媒の保管の必要がなくなり、又新規購入のTBPは
分解等により消耗する分の補給分だけで済むようにな
り、ランニングコスト節減に大きく寄与することができ
た。According to the present invention, the deteriorated TBP-containing organic solvent can be regenerated and recovered to have the same performance as a new product. As a result, it is no longer necessary to store the deteriorated solvent, and the newly purchased TBP only needs to be replenished by the amount consumed due to decomposition, etc., which can greatly contribute to the running cost reduction.
Claims (1)
機溶媒をアルカリ水溶液で洗浄処理して有機相と水相と
に分離した後、該水相をアンモニアで処理してウランを
回収する一方、該有機相を粗大網状イオン交換樹脂によ
りイオン交換処理してトリブチルフオスフエート含有有
機溶媒を再生することを特徴とする、トリブチルフオス
フエート含有有機溶媒の再生方法。1. A degraded tributylphosphate-containing organic solvent is washed with an alkaline aqueous solution to separate it into an organic phase and an aqueous phase, and then the aqueous phase is treated with ammonia to recover uranium while the organic phase is recovered. A method for regenerating an organic solvent containing tributylphosphonate, comprising subjecting the phase to an ion exchange treatment with a coarse reticulated ion exchange resin to regenerate the organic solvent containing tributylphosphate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8363786A JPH0810274B2 (en) | 1986-04-11 | 1986-04-11 | Method for regenerating organic solvent containing tributyl phosphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8363786A JPH0810274B2 (en) | 1986-04-11 | 1986-04-11 | Method for regenerating organic solvent containing tributyl phosphite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62239099A JPS62239099A (en) | 1987-10-19 |
| JPH0810274B2 true JPH0810274B2 (en) | 1996-01-31 |
Family
ID=13807976
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8363786A Expired - Fee Related JPH0810274B2 (en) | 1986-04-11 | 1986-04-11 | Method for regenerating organic solvent containing tributyl phosphite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0810274B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB9021264D0 (en) * | 1990-09-29 | 1990-11-14 | British Nuclear Fuels Plc | Cleaning of solutions |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5423900A (en) * | 1977-07-25 | 1979-02-22 | Mitsubishi Metal Corp | Recovering regeneration method of radioactive retreating waste organic solvent |
-
1986
- 1986-04-11 JP JP8363786A patent/JPH0810274B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62239099A (en) | 1987-10-19 |
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