JPH0212095A - Method for cleaning solvent - Google Patents

Method for cleaning solvent

Info

Publication number
JPH0212095A
JPH0212095A JP63163252A JP16325288A JPH0212095A JP H0212095 A JPH0212095 A JP H0212095A JP 63163252 A JP63163252 A JP 63163252A JP 16325288 A JP16325288 A JP 16325288A JP H0212095 A JPH0212095 A JP H0212095A
Authority
JP
Japan
Prior art keywords
nitric acid
condensate
tbp
solvent
butyl phosphate
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
Application number
JP63163252A
Other languages
Japanese (ja)
Inventor
Katsuyuki Otsuka
大塚 勝幸
Isao Kondo
勲 近藤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Power Reactor and Nuclear Fuel Development Corp
Original Assignee
Power Reactor and Nuclear Fuel Development Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Power Reactor and Nuclear Fuel Development Corp filed Critical Power Reactor and Nuclear Fuel Development Corp
Priority to JP63163252A priority Critical patent/JPH0212095A/en
Publication of JPH0212095A publication Critical patent/JPH0212095A/en
Pending legal-status Critical Current

Links

Classifications

    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00Energy generation of nuclear origin
    • Y02E30/30Nuclear fission reactors
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies

Landscapes

  • Heat Treatment Of Water, Waste Water Or Sewage (AREA)

Abstract

PURPOSE:To reduce the quantity of produced waste water so that the burden of waste water disposal can be reduced and safety against corrosion, fire, and explosion can be improved by separating the waste water into a condensate and residues of TBP (tri-n-butyl phosphate), etc., by using a freeze vacuum drying method. CONSTITUTION:A coolant 3 and heating medium 4 are supplied to and discharged from a freeze dryer 1 and the dryer 1 freezes and dries a solvent 2 by cooling and sublimation. The material sublimated at the dryer 1 is supplied to a condenser 5. A coolant 7 is supplied to and discharged from the condenser 5 and, at the same time, the condenser 5 is evacuated by a vacuum pump 6. A condensate is reserved in a condensate receiving tank 8 where the condensate is separated into an organic phase 9 and aqueous phase 10 by a difference in specific gravity and n-dodecane, etc., 11 and water, nitric acid, etc., 12 are respectively extracted for circulation from the phases 9 and 10. A waste nitric acid solution 14 containing non-evaporating TBP 13 and nuclear fuel materials and fission products is taken out at the dryer 1 and the TBP 13 is separated for reutilization. The waste nitric acid solution 14 is led to a disposing system.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は再処理工場、燃料製造工場等で用いる溶媒抽出
における溶媒洗浄工程の代替として利用する溶媒洗浄方
法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a solvent cleaning method used as an alternative to the solvent cleaning step in solvent extraction used in reprocessing plants, fuel manufacturing plants, etc.

〔従来の技術〕[Conventional technology]

一般に、再処理工場や燃料製造工場等の溶媒抽出工程に
用いて劣化した溶媒は、炭酸ナトリウム、水酸化ナトリ
ウムによる溶媒洗浄工程に送られて炭酸ソーダ液、苛性
ソーダ液で洗浄し、不純物を除去して再生溶媒として再
利用している。
Generally, degraded solvents used in solvent extraction processes at reprocessing plants and fuel manufacturing plants are sent to a solvent cleaning process using sodium carbonate and sodium hydroxide, where they are washed with soda carbonate and caustic soda solutions to remove impurities. and reused as recycled solvent.

〔発明が解決すべき課題〕[Problem to be solved by the invention]

しかしながらこのような方法によると、溶媒劣化が進ん
だものは、溶媒洗浄しても容易に再生できず炭酸ソーダ
液、苛性ソーダ液を含む洗浄廃液の発生量が多くなる欠
点がある。また、これらナトリウムを含む廃液は、硝酸
と結合して硝酸ナトリウムとなり、硝酸すトリウムを含
む廃液は蒸発缶等で濃縮しても硝酸ナトリウム含有量に
より一定程度以上には減容できない。
However, this method has the disadvantage that if the solvent has deteriorated, it cannot be easily regenerated even by solvent washing, and a large amount of washing waste liquid containing soda carbonate solution and caustic soda solution is generated. In addition, these sodium-containing waste liquids combine with nitric acid to become sodium nitrate, and even if waste liquids containing thorium nitrate are concentrated in an evaporator or the like, the volume cannot be reduced beyond a certain level due to the sodium nitrate content.

本発明は上記問題点を解決するためのもので、廃棄物処
理、処分の観点からは可能な限り炭酸ソーダ、苛性ソー
ダのようなナトリウムを含む物質の利用をなくすため、
洗浄液の利用をやめ、廃液発生壇を減らして廃液処理の
負荷を軽くし、しかも装置の腐蝕・火災・爆発が起きな
い低温を利用して安全性の高い溶媒洗浄方法を提供する
。ことを目的とする。
The present invention is intended to solve the above problems, and from the viewpoint of waste treatment and disposal, to eliminate the use of sodium-containing substances such as soda carbonate and caustic soda as much as possible.
To provide a highly safe solvent cleaning method that eliminates the use of cleaning liquid, reduces the waste liquid generation stage, reduces the load of waste liquid treatment, and uses low temperature that does not cause corrosion, fire, or explosion of equipment. The purpose is to

〔課題を解決するための手段〕[Means to solve the problem]

そのために本発明の溶媒洗浄方法は、再処理工場、燃料
製造工場等の溶媒抽出から発生する溶媒の再生のための
溶媒洗浄工程において、凍結真空乾燥法により水、硝酸
、昇華する核種、n−ドデカン等よりなる凝11液と、
リン酸トリ−n−ブチル(以下TBPと言う)、フタル
酸ジブチル(以下DBPと言う)、リン酸ブチル(以下
MBPと言う)および昇華しない核燃料物質、核分裂生
成物よりなるTBP等残留物とに分離し、前記凝縮液は
、水、硝酸等よりなる水相とn−ドデカン等よりなる有
機相とに分離し、前記TBP等残留物は、硝酸溶液によ
り洗浄し、TBPに同伴している核燃料物質、核分裂生
成物を分離し、TBPを再利用することを再利用する。
For this purpose, the solvent cleaning method of the present invention uses a freeze-vacuum drying method to remove water, nitric acid, sublimated nuclides, n- A coagulated liquid 11 consisting of dodecane etc.,
To residues such as tri-n-butyl phosphate (hereinafter referred to as TBP), dibutyl phthalate (hereinafter referred to as DBP), butyl phosphate (hereinafter referred to as MBP), and TBP made of non-sublimed nuclear fuel materials and fission products. The condensate is separated into an aqueous phase consisting of water, nitric acid, etc. and an organic phase consisting of n-dodecane, etc. The TBP and other residues are washed with a nitric acid solution and the nuclear fuel accompanying the TBP is separated. Recycle the material, separate the fission products and reuse the TBP.

〔作用] 本発明は再処理工場、燃料製造工場等で利用している溶
媒抽出の溶媒洗浄工程において、ナトリウムを含む物質
(炭酸ソーダ、苛性ソーダ)の利用する溶媒洗浄工程の
代替法として、凍結真空乾燥法を用い、凝縮液とTBP
等残留物に分離し、凝縮液は、さらに比重差によりn−
ドデカン等の可燃性有機溶媒と水、硝酸等に分離し、T
BP等残留物は硝酸溶液で洗浄することによりTBPを
再生させることができる。
[Function] The present invention is an alternative method to the solvent cleaning process of solvent extraction used in reprocessing plants, fuel manufacturing plants, etc., which uses sodium-containing substances (soda carbonate, caustic soda). Using the drying method, condensate and TBP
The condensate is further divided into n-
Separate into flammable organic solvent such as dodecane, water, nitric acid, etc.
TBP can be regenerated by washing residual BP etc. with a nitric acid solution.

(実施例) 以下、実施例を図面を参照して説明する。(Example) Examples will be described below with reference to the drawings.

第1図は本発明の廃溶媒処理の全体構成を示す図である
。lは凍結乾燥器、2は溶媒、3は冷媒、4は加熱媒体
、5は凝縮器、6は真空ポンプ、7は冷媒、8は凝縮液
受槽、9は有機相、10は水相、11はn−ドデカン等
、12は水・硝酸等、13はTBP・核燃料物質・核分
裂生成物、14は廃硝酸溶液である。
FIG. 1 is a diagram showing the overall configuration of waste solvent treatment according to the present invention. 1 is a freeze dryer, 2 is a solvent, 3 is a refrigerant, 4 is a heating medium, 5 is a condenser, 6 is a vacuum pump, 7 is a refrigerant, 8 is a condensate receiver, 9 is an organic phase, 10 is an aqueous phase, 11 12 is water, nitric acid, etc., 13 is TBP, nuclear fuel material, nuclear fission product, and 14 is waste nitric acid solution.

図において、凍結乾燥器1へは溶媒供給系から溶媒2が
供給されるようになっている。凍結乾燥器lへは冷媒3
、加熱媒体4が供給排出され、溶媒2を冷却凍結、昇華
乾燥するようになっている。
In the figure, a solvent 2 is supplied to a freeze dryer 1 from a solvent supply system. Refrigerant 3 to freeze dryer 1
, a heating medium 4 is supplied and discharged, and the solvent 2 is cooled, frozen, and sublimated to dry.

凍結乾燥器1で昇華した物質は凝縮器5に供給される。The substance sublimed in the freeze dryer 1 is supplied to the condenser 5.

凝縮器5には冷媒7が供給排出されると共に、真空ポン
プ6で排気されており、4i縮液は凝縮液受槽゛8へ貯
留し、比重差により有機相9と水相10とに分離し、そ
れぞれ有機相からはn−ドデカン等11が抽出され、水
相10からは水・硝酸等12が抽出され再利用される。
A refrigerant 7 is supplied to and discharged from the condenser 5, and is also exhausted by a vacuum pump 6, and the 4i condensate is stored in a condensate receiving tank 8 and separated into an organic phase 9 and an aqueous phase 10 due to the difference in specific gravity. , n-dodecane etc. 11 are extracted from the organic phase, and water, nitric acid etc. 12 are extracted from the aqueous phase 10 and reused.

また凍結乾燥器lで蒸発しないTBP13と核燃料物質
・核分裂生成物を含む廃硝酸溶液14は残留物として取
り出され、TBP13は分離されて再利用され、廃硝酸
溶液14は廃棄系へ導かれることになる。
In addition, the TBP 13 that does not evaporate in the freeze dryer 1 and the waste nitric acid solution 14 containing nuclear fuel materials and fission products are taken out as residue, the TBP 13 is separated and reused, and the waste nitric acid solution 14 is led to the disposal system. Become.

こうして、TBP等、n−ドデカン等、核燃料物質、核
分裂生成物、硝酸、水等が再処理工場9、燃料製造工場
等の溶媒抽出工程から排出され、再生もしくは廃棄され
る。
In this way, nuclear fuel materials such as TBP, n-dodecane, nuclear fission products, nitric acid, water, etc. are discharged from the solvent extraction process of the reprocessing plant 9, fuel manufacturing plant, etc., and are recycled or disposed of.

第2図は第1図のプロセスフローを示す図で、■は溶媒
、■は凍結工程、■は昇華工程、■はTBP等残留物、
■は洗浄工程、■はTBP、■は廃硝酸溶液、■は調整
槽、■は廃液処理系、[相]は凝縮器、■は凝縮液、@
はn−ドデカン等、■は水・硝酸等である。
Figure 2 is a diagram showing the process flow of Figure 1, where ■ is the solvent, ■ is the freezing process, ■ is the sublimation process, ■ is the residue such as TBP, etc.
■ is the cleaning process, ■ is TBP, ■ is the waste nitric acid solution, ■ is the adjustment tank, ■ is the waste liquid treatment system, [phase] is the condenser, ■ is the condensate, @
is n-dodecane, etc., and ■ is water, nitric acid, etc.

TBP等、n−ドデカン等、核燃料物質、核分裂生成物
、水、硝酸等を含む再処理工場、燃料製造工場等の溶媒
抽出工程から発生する溶媒■は、凍結工程■において冷
却凍結される。凍結された溶媒凍結体は、昇華工程■に
おいて加熱、減圧、真空状態に置かれ、凍結体より溶媒
中に含まれている硝酸、水、n−ドデカン等と昇華する
核種が昇華され、それらは凝縮器により凝縮され凝縮液
■になる。
Solvent (1) generated from the solvent extraction process at a reprocessing factory, fuel manufacturing factory, etc., containing nuclear fuel materials such as TBP, n-dodecane, etc., nuclear fission products, water, nitric acid, etc., is cooled and frozen in the freezing process (2). The frozen solvent frozen body is heated, depressurized, and placed in a vacuum state in the sublimation process (2), and the nuclides that sublimate with nitric acid, water, n-dodecane, etc. contained in the solvent are sublimated from the frozen body, and they are It is condensed by the condenser and becomes condensate liquid■.

凝縮液■は、比重差により有機相のn−ドデカン等@と
水相の水、硝酸等@に分離され、可燃性のn−ドデカン
等@は焼却され、水、硝酸等@は再利用される。
The condensate ■ is separated into an organic phase, n-dodecane, etc., and an aqueous phase, water, nitric acid, etc., due to the difference in specific gravity.The flammable n-dodecane, etc., are incinerated, and the water, nitric acid, etc., are recycled. Ru.

昇華工程■において、TBP、DBP、MBPおよび昇
華しない核燃t4物質、核分裂生成物等は、TBP等残
留物■となる。TBP等残留物■は、洗浄工程において
硝酸溶液■で洗浄するとTBP■と核燃料物質、核分裂
生成物を含む廃硝酸溶液■に分けられる。
In the sublimation process (2), TBP, DBP, MBP, nuclear fuel T4 materials, nuclear fission products, etc. that do not sublimate become TBP and other residues (2). When TBP and other residues (2) are washed with nitric acid solution (2) in the cleaning process, they are separated into TBP (2) and waste nitric acid solution (2) containing nuclear fuel materials and fission products.

TBP■は、調整槽■においてn−ドデカン等と混合さ
れて再利用される。廃硝酸溶液■は、廃液処理系■へ送
られる。
TBP (2) is mixed with n-dodecane etc. in the adjustment tank (2) and reused. The waste nitric acid solution (■) is sent to the waste liquid treatment system (■).

なお、以上の説明においてはTBPを例にとって説明し
たが、本発明による溶媒の処理方法は、TBPのみでな
く、溶媒抽出で使用されている他の種類の溶媒の分離再
生にも適用可能であることは明らかである。
Although TBP was used as an example in the above explanation, the solvent processing method according to the present invention is applicable not only to TBP but also to the separation and regeneration of other types of solvents used in solvent extraction. That is clear.

〔発明の効果〕〔Effect of the invention〕

以上のように本発明によれば、再処理工場、燃料製造工
場等で利用している溶媒抽出の溶媒洗浄工程を凍結真空
乾燥法で代替することができ、凝縮液とTBP等残留物
に分離できる。そして凝縮液は、さらに比重差によりn
−ドデカン等の可燃性有a熔媒と水、硝酸等に分離でき
、TBP等残留物は硝酸溶液で洗浄することによりTB
Pを再生させることができる。
As described above, according to the present invention, the solvent cleaning process of solvent extraction used in reprocessing plants, fuel manufacturing plants, etc. can be replaced by the freeze-vacuum drying method, and the condensate and residues such as TBP can be separated. can. The condensate is further divided into n due to the difference in specific gravity.
- Can be separated into flammable atomized solvent such as dodecane, water, nitric acid, etc., and TBP and other residues can be removed by washing with nitric acid solution.
P can be regenerated.

その結果、ナトリウムを含む物質(炭酸ソーダ、苛性ソ
ーダ)による溶媒洗浄が不要となり、アスファルト固化
、ガラス固化へ送られる硝酸ソーダ層を大幅に減らすこ
とが可能となる。
As a result, solvent cleaning with sodium-containing substances (soda carbonate, caustic soda) becomes unnecessary, and the amount of sodium nitrate layer sent to asphalt solidification and vitrification can be significantly reduced.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は本発明の溶媒処理の全体構成を説明する図、第
2図は第1図のプロセスフローを示す図である。 ■・・・凍結乾燥器、2・・・溶媒、3・・・冷媒、4
・・・加熱媒体、5・・・凝縮器、6・・・真空ポンプ
、7・・・冷媒、8・・・凝縮液受槽、9・・・存機相
、10・・・水相、11・・・n−ドデカン等、12・
・・水・硝酸等、13・・・TBP−核燃料物質・核分
裂生成物、14・・・廃硝酸溶液、■・・・溶媒、■・
・・凍結工程、■・・・昇華工程、■・・・TBP等残
留物、■・・・中和洗浄工程、■・・・TB I)、■
・・・廃硝酸溶液、■・・・調整槽、■・・・廃液処理
系、[相]・・・凝縮器、■・・・凝縮液、■・・・n
・ドデカン等、■・・・水・硝酸等。 第1図 出  願 人
FIG. 1 is a diagram explaining the overall configuration of the solvent treatment of the present invention, and FIG. 2 is a diagram showing the process flow of FIG. 1. ■...Freeze dryer, 2...Solvent, 3...Refrigerant, 4
. . . Heating medium, 5. Condenser, 6. Vacuum pump, 7. Refrigerant, 8. Condensate receiver tank, 9. Existing phase, 10. Water phase, 11. ... n-dodecane etc., 12.
...Water, nitric acid, etc., 13...TBP-Nuclear fuel material/fission products, 14...Waste nitric acid solution, ■...Solvent, ■・
・・Freezing process, ■・Sublimation process, ■・Residues such as TBP, ■・Neutralization cleaning process, ■・TB I), ■
...waste nitric acid solution, ■...adjustment tank, ■...waste treatment system, [phase]...condenser, ■...condensate, ■...n
・Dodecane, etc., ■...Water, nitric acid, etc. Figure 1 Applicant

Claims (3)

【特許請求の範囲】[Claims] (1)再処理工場、燃料製造工場等の溶媒抽出から発生
する溶媒の再生のための溶媒洗浄工程において、凍結真
空乾燥法により水、硝酸、昇華する核種、n−ドデカン
等よりなる凝縮液と、リン酸トリ−n−ブチル、フタル
酸ジブチル、リン酸ブチルおよび昇華しない核燃料物質
、核分裂生成物よりなるリン酸トリ−n−ブチル等残留
物とに分離することを特徴とする溶媒洗浄方法。
(1) In the solvent cleaning process for regenerating the solvent generated from solvent extraction at reprocessing plants, fuel manufacturing plants, etc., a condensate consisting of water, nitric acid, sublimated nuclides, n-dodecane, etc. is removed by freeze-vacuum drying. , tri-n-butyl phosphate, dibutyl phthalate, butyl phosphate, and residues such as tri-n-butyl phosphate consisting of non-sublimated nuclear fuel materials and fission products.
(2)前記凝縮液は、水、硝酸等よりなる水相とn−ド
デカン等よりなる有機相とに分離する請求項1記載の溶
媒洗浄方法。
(2) The solvent cleaning method according to claim 1, wherein the condensate is separated into an aqueous phase consisting of water, nitric acid, etc., and an organic phase consisting of n-dodecane, etc.
(3)前記リン酸トリ−n−ブチル等残留物は、硝酸溶
液により洗浄し、リン酸トリ−n−ブチルに同伴してい
るフタル酸ジブチル、リン酸ブチル核燃料物質、核分裂
生成物を分離し、リン酸トリ−n−ブチルを再利用する
請求項1または2記載の溶媒洗浄方法。
(3) The tri-n-butyl phosphate and other residues are washed with a nitric acid solution to separate the dibutyl phthalate, butyl phosphate nuclear fuel material, and fission products that accompany the tri-n-butyl phosphate. 3. The solvent cleaning method according to claim 1 or 2, wherein tri-n-butyl phosphate is reused.
JP63163252A 1988-06-30 1988-06-30 Method for cleaning solvent Pending JPH0212095A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP63163252A JPH0212095A (en) 1988-06-30 1988-06-30 Method for cleaning solvent

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP63163252A JPH0212095A (en) 1988-06-30 1988-06-30 Method for cleaning solvent

Publications (1)

Publication Number Publication Date
JPH0212095A true JPH0212095A (en) 1990-01-17

Family

ID=15770257

Family Applications (1)

Application Number Title Priority Date Filing Date
JP63163252A Pending JPH0212095A (en) 1988-06-30 1988-06-30 Method for cleaning solvent

Country Status (1)

Country Link
JP (1) JPH0212095A (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4980756A (en) * 1972-11-15 1974-08-03
JPS57117U (en) * 1980-06-02 1982-01-05

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4980756A (en) * 1972-11-15 1974-08-03
JPS57117U (en) * 1980-06-02 1982-01-05

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