JPH073471B2 - Solvent purification method - Google Patents

Solvent purification method

Info

Publication number
JPH073471B2
JPH073471B2 JP19004288A JP19004288A JPH073471B2 JP H073471 B2 JPH073471 B2 JP H073471B2 JP 19004288 A JP19004288 A JP 19004288A JP 19004288 A JP19004288 A JP 19004288A JP H073471 B2 JPH073471 B2 JP H073471B2
Authority
JP
Japan
Prior art keywords
solvent
tri
butyl phosphate
phosphate
butyl
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
Application number
JP19004288A
Other languages
Japanese (ja)
Other versions
JPH0238998A (en
Inventor
勝幸 大塚
仁 大内
勲 近藤
Original Assignee
動力炉・核燃料開発事業団
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 動力炉・核燃料開発事業団 filed Critical 動力炉・核燃料開発事業団
Priority to JP19004288A priority Critical patent/JPH073471B2/en
Publication of JPH0238998A publication Critical patent/JPH0238998A/en
Publication of JPH073471B2 publication Critical patent/JPH073471B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related 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

  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

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
における溶媒精製工程、劣化溶媒の精製工程に利用でき
る溶媒精製方法に関するものである。
TECHNICAL FIELD The present invention relates to a solvent refining method that can be used in a solvent refining step in solvent extraction used in a reprocessing factory, a fuel manufacturing factory, etc., and a degrading solvent refining step.

〔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
用いて劣化したリン酸トリ−n−ブチル(以下TBPと言
う)、n−ドデカン等の溶媒は、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。
In general, solvents such as tri-n-butyl phosphate (hereinafter referred to as TBP) and n-dodecane that have deteriorated in the solvent extraction process of a reprocessing plant or a fuel manufacturing plant are washed with sodium carbonate or sodium hydroxide. It is sent to the process and washed with a sodium carbonate solution and a caustic soda solution to remove impurities and reused as a regenerated solvent.

〔発明が解決すべき課題〕[Problems 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
と結合して酢酸ナトリウムとなり、硝酸ナトリウムを含
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ため、炭酸ソーダ、
苛性ソーダのようなナトリウムを含む物質を利用を少な
くすることが望まれていた。
However, according to such a method, a solvent that has deteriorated due to deterioration in solvent cannot be easily regenerated even if it is washed with a solvent, and a large amount of cleaning waste liquid containing a sodium carbonate solution and a caustic soda solution is generated. Further, the waste liquid containing these sodium is combined with nitric acid to become sodium acetate, and the waste liquid containing sodium nitrate cannot be reduced to a certain degree or more due to the sodium nitrate content even if it is concentrated in an evaporator or the like, soda carbonate,
It has been desired to reduce the utilization of sodium-containing substances such as caustic soda.

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、処分の観点から可能な限り炭酸ソーダ、苛性ソーダ
のような溶媒洗浄液に使用しているナトリウムを含む物
質の利用をやめ、低温真空蒸留法で溶媒中のTBPとリン
酸ジブチル(以下DBPと言う)、リン酸ブチル(以下MBP
と言う)等を分離し、ナトリウムを含む廃液発生量を減
らして廃液処理の負荷を軽減する溶媒精製方法を提供す
ることを目的とする。
The present invention is to solve the above-mentioned problems. From the viewpoint of waste treatment and disposal, the use of substances containing sodium used in solvent cleaning solutions such as sodium carbonate and caustic soda is stopped as much as possible at low temperature vacuum. TBP and dibutyl phosphate (hereinafter referred to as DBP) in the solvent by distillation method, butyl phosphate (hereinafter referred to as MBP)
It is an object of the present invention to provide a solvent purification method in which the amount of waste liquid containing sodium is reduced to reduce the load of waste liquid treatment.

〔課題を解決するための手段〕[Means for Solving the Problems]

そのために本発明の溶媒精製法は、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精
製工程において、低温真空蒸留法により水、硝酸、n−
ドデカン、及びこれらと同伴する核種よりなる凝縮液
と、リン酸トリ−n−ブチル及びリン酸ジブチル、リン
酸ブチル、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第1の分離工程、
リン酸トリ−n−ブチル等残留物を酢酸溶液で洗浄し、
リン酸トリ−n−ブチル、リン酸ジブチル、リン酸ブチ
ルを核燃料物質、核分裂生成物等を含む精製廃液から分
離する精製工程、分離されたリン酸トリ−n−ブチル、
リン酸ジブチル、リン酸ブチルから低温真空蒸留法によ
りリン酸トリ−n−ブチルを分離する第2の分離工程か
らなることを特徴とする。
Therefore, the solvent refining method of the present invention is a refining process for regenerating a solvent generated from solvent extraction in a reprocessing factory, a fuel manufacturing factory, etc., by water, nitric acid, n-
Condensed liquid consisting of dodecane and nuclides accompanied with these, and residuals such as tri-n-butyl phosphate and dibutyl phosphate, butyl phosphate, nuclear fuel material, tri-n-butyl phosphate consisting of fission products A first separation step of separating,
The residue such as tri-n-butyl phosphate was washed with an acetic acid solution,
A purification step of separating tri-n-butyl phosphate, dibutyl phosphate, and butyl phosphate from a refinery waste liquid containing nuclear fuel materials, fission products, etc., the separated tri-n-butyl phosphate,
It is characterized by comprising a second separation step of separating tri-n-butyl phosphate from dibutyl phosphate and butyl phosphate by a low temperature vacuum distillation method.

〔作用〕[Action]

本発明は再処理工場、燃料製造工場等で利用している溶
媒抽出の溶媒精製工程において、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、低温真空蒸留法を用い、凝縮液とTBP等
残留物に分離し、凝縮液は、さらに比重差等によりn−
ドデカン等の可燃性有機溶媒と水、硝酸等に分離し、TB
P等残留物は硝酸溶液で洗浄したのち、再度低温真空蒸
留法でTBPとDBP、MBPを分離することによりTBPを再生さ
せることができる。
INDUSTRIAL APPLICABILITY The present invention uses a low temperature vacuum distillation method as an alternative method to a solvent washing step using a substance containing sodium (sodium carbonate, caustic soda) in a solvent purification step of solvent extraction used in a reprocessing factory, a fuel manufacturing factory, etc. Used to separate the condensate and the residue such as TBP.
Separated into flammable organic solvents such as dodecane and water, nitric acid, etc.
After the residue such as P is washed with a nitric acid solution, TBP can be regenerated by separating TBP from DBP and MBP by the low temperature vacuum distillation method again.

〔実施例〕〔Example〕

以下、実施例を図面を参照して説明する。 Hereinafter, embodiments will be described with reference to the drawings.

第1図は本発明の溶媒処理フローの全体構成を示す図で
ある。図中、は劣化溶媒、は低温真空蒸留工程、
は凝縮器、は凝縮液、は分離槽、はn−ドデカン
等、は水、硝酸等、は精製工程、は酸回収工程、
はn−ドデカン、はTBP等残留物、は精製工程、
はTBP、DBP、MBP、は精製廃液、は低温真空蒸留
工程、は廃液処理系、はTBP、はDBP、MBP、は
溶媒調整槽、は凝縮器である。
FIG. 1 is a diagram showing an overall configuration of a solvent treatment flow of the present invention. In the figure, is a deteriorated solvent, is a low temperature vacuum distillation step,
Is a condenser, is a condensate, is a separation tank, is n-dodecane, etc., is water, nitric acid, etc. is a purification step, is an acid recovery step,
Is n-dodecane, is a residue such as TBP, is a purification step,
Is TBP, DBP, MBP, purified waste liquid, low temperature vacuum distillation step, waste liquid treatment system, TBP, DBP, MBP, solvent adjusting tank, and condenser.

図において、TBP、n−ドデカン、核燃料物質、核分裂
物質、水、硝酸等を含む再処理工場、燃料工場等の溶媒
抽出工程から発生する劣化溶媒は、低温真空蒸留工程
において蒸留される。このとき、劣化溶媒中に含まれ
るn−ドデカン、水、硝酸、及びそれらに同伴する核種
は、蒸発して凝縮器へ送られる。凝縮器へは冷媒が
循環供給されると共に、真空ポンプにより減圧排気され
て凝縮が行われ、凝縮液となる。凝縮液は、分離槽
において比重差等により可燃性の有機相と水相とに分
離され、それぞれ有機相としてn−ドデカン等が抽出
され、水相として水・硝酸等が抽出される。nドデカ
ン等は精製工程へ送られ、n−ドデカンは精製後
再利用される。また水・硝酸等は酸回収工程へ送ら
れて硝酸が回収される。
In the figure, a deteriorated solvent generated from a solvent extraction process such as a reprocessing plant or a fuel plant containing TBP, n-dodecane, a nuclear fuel material, a fission material, water, nitric acid, etc. is distilled in a low temperature vacuum distillation step. At this time, n-dodecane, water, nitric acid, and nuclides accompanying them contained in the deteriorated solvent are evaporated and sent to the condenser. Refrigerant is circulated and supplied to the condenser, and is vacuum-exhausted by a vacuum pump to condense and become a condensed liquid. The condensate is separated into a combustible organic phase and an aqueous phase due to a difference in specific gravity in the separation tank, and n-dodecane and the like are extracted as the organic phase and water and nitric acid and the like are extracted as the aqueous phase. N-dodecane and the like are sent to the purification step, and n-dodecane is reused after purification. Also, water, nitric acid, etc. are sent to the acid recovery process to recover nitric acid.

一方、TBP、DBPとMBPとこれに同伴している核燃料物質
・核分裂生成物等は、TBP等残留物として取り出さ
れ、精製工程において硝酸溶液で洗浄され、TBP、DB
P、MBPと、核燃料物質、核分裂生成物等を含む精製廃
液となる。TBP、DBP、MBPは低温真空蒸留工程で
蒸発される。この時、TBPは蒸発して凝縮器へ送られ
る。TBPは、溶液調整槽においてn−ドデカン等と
混合され、再利用される。そして、精製廃液は廃液処
理系へ送られる。
On the other hand, TBP, DBP, MBP, and nuclear fuel materials and fission products accompanying them are taken out as TBP residue and washed with nitric acid solution in the refining process.
It becomes a refined waste liquid containing P, MBP, nuclear fuel materials, fission products, etc. TBP, DBP and MBP are evaporated in the low temperature vacuum distillation process. At this time, TBP is evaporated and sent to the condenser. TBP is reused after being mixed with n-dodecane or the like in the solution adjusting tank. Then, the refined waste liquid 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。
In the above description, TBP was described as an example, but the method for treating a solvent according to the present invention is not limited to TBP,
Clearly, it is also applicable to the separation and regeneration of other types of solvents used in solvent extraction.

〔発明の効果〕〔The invention's effect〕

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低温真空
蒸留法で行うことにより、凝縮液とTBP等残留物に分離
できる。そして凝縮液は、さらに比重差等によりn−ド
デカン等の可燃性有機相と水、硝酸等の水相に分離で
き、TBP等残留物は硝酸溶液で洗浄し、更に低温真空蒸
留で行うことによりDBP、MBPに分離ができる。そして、
TBPを再生させることができる。
As described above, according to the present invention, the condensate and the residue such as TBP can be separated by performing the solvent washing step of the solvent extraction used in the reprocessing factory, the fuel manufacturing factory, etc. by the low temperature vacuum distillation method. The condensate can be further separated into a flammable organic phase such as n-dodecane and an aqueous phase such as water and nitric acid due to the difference in specific gravity, etc., and the residue such as TBP is washed with nitric acid solution and further subjected to low temperature vacuum distillation. Can be separated into DBP and MBP. And
TBP 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、ナトリウムを使用
しなくなったため、アスファルト固化、ガラス固化へ送
られる硝酸ソーダ量を大幅に減らすことが可能となる。
As a result, solvent washing with a substance containing sodium (sodium carbonate, caustic soda) becomes unnecessary, and since sodium is not used, it is possible to significantly reduce the amount of sodium nitrate sent to asphalt solidification and vitrification.

【図面の簡単な説明】[Brief description of drawings]

第1図は本発明の溶媒精製の全体構成を説明する図であ
る。 ……劣化溶媒、……低温真空蒸留工程、……凝縮
器、……凝縮液、……分離槽、……n−ドデカン
等、……水、硝酸等、……精製工程、……酸回収
工程、……n−ドデカン、……TBP等残留物、…
…精製工程、……TBP、DBP、MBP、……精製廃液、
……低温真空蒸留工程、……廃液処理系、,……
TBP、……DBP、MBP、……溶媒調整槽、……凝縮
器。
FIG. 1 is a diagram for explaining the overall structure of solvent purification according to the present invention. …… Degraded solvent …… Low temperature vacuum distillation process …… Condenser …… Condensate …… Separation tank …… n-dodecane etc. …… Water, nitric acid etc. …… Purification process …… Acid recovery Process, n-dodecane, TBP residue, etc.
… Refining process ………… TBP, DBP, MBP,… Refining waste liquid,
...... Low temperature vacuum distillation process ...... Waste liquid treatment system ......
TBP, ... DBP, MBP, ... solvent adjustment tank, ... condenser.

───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭62−27697(JP,A) 特開 昭62−49296(JP,A) 特開 昭54−23900(JP,A) ─────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-62-27697 (JP, A) JP-A-62-49296 (JP, A) JP-A-54-23900 (JP, A)

Claims (1)

【特許請求の範囲】[Claims] 【請求項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精製工程において、低温
真空蒸留法により水、硝酸、n−ドデカン、及びこれら
と同伴する核種よりなる凝縮液と、リン酸トリ−n−ブ
チル及びリン酸ジブチル、リン酸ブチル、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
とに分離する第1の分離工程、リン酸トリ−n−ブチル
等残留物を硝酸溶液で洗浄し、リン酸トリ−n−ブチ
ル、リン酸ジブチル、リン酸ブチルを核燃料物質、核分
裂生成物等を含む精製廃液から分離する精製工程、分離
されたリン酸トリ−n−ブチル、リン酸ジブチル、リン
酸ブチルから低温真空蒸留法によりリン酸トリ−n−ブ
チルを分離する第2の分離工程からなることを特徴とす
る溶媒精製法。
1. A refining process for regenerating a solvent generated from solvent extraction in a reprocessing plant, a fuel manufacturing plant, etc., which comprises water, nitric acid, n-dodecane, and a nuclide accompanying these by a low temperature vacuum distillation method. Condensate with tri-n-butyl phosphate and dibutyl phosphate, butyl phosphate, nuclear fuel material,
The first separation step of separating the residue of tri-n-butyl phosphate and the like consisting of fission products, the residue of tri-n-butyl phosphate and the like is washed with a nitric acid solution, and tri-n-butyl phosphate, A purification step for separating dibutyl phosphate and butyl phosphate from a refinery waste liquid containing nuclear fuel substances, fission products, etc., and phosphorus-containing tri-n-butyl phosphate, dibutyl phosphate, and butyl phosphate separated by a low-temperature vacuum distillation method. A solvent purification method comprising a second separation step for separating tri-n-butyl acidate.
JP19004288A 1988-07-29 1988-07-29 Solvent purification method Expired - Fee Related JPH073471B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP19004288A JPH073471B2 (en) 1988-07-29 1988-07-29 Solvent purification method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP19004288A JPH073471B2 (en) 1988-07-29 1988-07-29 Solvent purification method

Publications (2)

Publication Number Publication Date
JPH0238998A JPH0238998A (en) 1990-02-08
JPH073471B2 true JPH073471B2 (en) 1995-01-18

Family

ID=16251389

Family Applications (1)

Application Number Title Priority Date Filing Date
JP19004288A Expired - Fee Related JPH073471B2 (en) 1988-07-29 1988-07-29 Solvent purification method

Country Status (1)

Country Link
JP (1) JPH073471B2 (en)

Family Cites Families (3)

* Cited by examiner, † Cited by third party
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
JPS6227697A (en) * 1985-07-29 1987-02-05 動力炉・核燃料開発事業団 Method and device for processing waste liquor containing radioactive substance
JPS6249296A (en) * 1985-08-28 1987-03-03 株式会社東芝 Evaporating concentrator

Also Published As

Publication number Publication date
JPH0238998A (en) 1990-02-08

Similar Documents

Publication Publication Date Title
CN1269767A (en) Treatment of molten salt reprocessing wastes
KR980701128A (en) Process for Decontaminating Radioactive Materials
JPH073471B2 (en) Solvent purification method
US4981616A (en) Spent fuel treatment method
EP0347255B1 (en) Method of treating high-level radioactive waste liquid
US5180526A (en) Cleaning of solutions of alkylphosphates
US5096624A (en) Process for the treatment of radioactive waste water
US5788935A (en) Process for the regeneration of a spent solution for pickling zirconium alloy elements
US5430226A (en) Method for regenerating spent solvent generated from nuclear fuel cycle
US4394269A (en) Method for cleaning solution used in nuclear fuel reprocessing
JPH036477B2 (en)
CN1121044C (en) Solution pretreating method at beginning end of purex flow process and used silica gel and its preparing process
JPH01316695A (en) Reprocessing of nuclear fuel by using vacuum freeze drying method
US4526658A (en) Method for improving ruthenium decontamination efficiency in nitric acid evaporation treatment
US5110507A (en) Method of separating and purifying spent solvent generated in nuclear fuel cycle
US5252258A (en) Method of recovering and storing radioactive iodine by freeze vacuum drying process
EP0361773B1 (en) Method of recovering radioactive iodine in a spent nuclear fuel retreatment process
US4022708A (en) Method of preparation for storage of liquids used in the reprocessing of spent nuclear fissile and/or fertile materials
JPS61110783A (en) Recovery of zirconium and acid from used etching solution
US5171447A (en) Method of extracting and separating spent solvent generated in nuclear fuel cycle
JPH10213697A (en) Decontamination method for radio active waste
JP3364308B2 (en) Wastewater treatment method and apparatus
JP3438534B2 (en) Treatment method of boron-containing water
JPH0212095A (en) Method for cleaning solvent
JP3197233B2 (en) Method for reducing volume of acidic radioactive waste solution and its treatment system

Legal Events

Date Code Title Description
LAPS Cancellation because of no payment of annual fees