CN107177744A - A kind of method of extract and separate group of the lanthanides and actinides - Google Patents
A kind of method of extract and separate group of the lanthanides and actinides Download PDFInfo
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- CN107177744A CN107177744A CN201710354665.6A CN201710354665A CN107177744A CN 107177744 A CN107177744 A CN 107177744A CN 201710354665 A CN201710354665 A CN 201710354665A CN 107177744 A CN107177744 A CN 107177744A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/32—Carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention belongs to group of the lanthanides and actinides separation technology field, it is related to a kind of extract and separate group of the lanthanides and the method for actinides.Described method is to adjust the concentration of inorganic acid in the solution containing group of the lanthanides and actinides for 0.1 5mol/L, then adds and contains N, and the organic solvent of the sweet acid amic acid of N dialkyl group two carries out extract and separate.Utilize the method for the extract and separate group of the lanthanides and actinides of the present invention, good extracting power, loading capacity and extraction selectivity can be had concurrently in extract and separate group of the lanthanides from radioactivity spentnuclear fuel lysate, high activity liquid waste or in the acid leaching solution containing lanthanide series and actinides.
Description
Technical field
The invention belongs to group of the lanthanides and actinides separation technology field, it is related to a kind of extract and separate group of the lanthanides and actinides
Method.
Background technology
Solvent extraction is that separation and recovery group of the lanthanides and actinides in separation of rare earth elements, nuclear industry are extracted in metallurgical industry
The most frequently used separation method.Due to lanthanide series and actinides metal ion in the neutral or meta-alkalescence aqueous solution easy water
Solution, therefore extract and separate flow is carried out all in acid solution system accordingly, this requires extractant has to acid preferable
Stability, and there is stronger extracting power to lanthanide series and actinides in an acidic solution.Furthermore, it is contemplated that waste is most
Smallization, extractant is preferably made up of carbon, hydrogen, oxygen, several elements of nitrogen；Extractant with later can burning disposal completely, subtracted with trying one's best
The generation of few secondary waste.
In view of the foregoing, lanthanide series and actinides the extractant overwhelming majority developed in the past are all fat-soluble neutrality
Organic molecule, and it is most of all using oxygen atom as coordination atom.This most representative kind of extractants is tributyl phosphate
(TBP), it has good extracting power and selectivity to tetravalence plutonium and hexavalent uranium.The uranium of this performance research and development based on TBP
Plutonium coextraction separation process (PUREX flows) is occupied an leading position in spentnuclear fuel post processing field always in the past few decades.But due to
Develop the requirement of Clear nuclear energy, the originally indissociable trivalent of PUREX flows and pentavalent actinides ion, be also required to now from
Separated in high activity liquid waste.In order to meet these demands, people design the extraction that several extracting powers of study on the synthesis are better than TBP
Take agent, main strategy is to improve its extraction ability by increasing the coordination site of extractant.
Although when extractant coordination site from TBP, one of trialkylphosphine oxide (TRPO), increase to malonic acid bisamide,
Two of N, N- dialkyl amide substituent methyl-dialkyl group phosphine oxide (CMPO), then to the sweet acid bisamide (TRDGA) of tetraalkyl two
At three, the extracting power to trivalent lanthanide series and actinides ion is stepped up, still, due to extractant coordination site
Increase, the Coordination Space of the metal ion occupied is also in increase, and the Coordination Space for leaving anion (such as nitrate anion) for is reduced.Work as extraction
When taking agent for tridentate ligand TRDGA, the inner sphere complexation space of lanthanide series and actinides is extracted agent and occupied completely, all companions
Anion in ion pair form can only be extracted into organic phase in peripheral space.So, although extracting power may improve a lot,
But because solubility of the ion pair in non-polar organic solvent is relatively low, cause loading capacity relatively small.
The content of the invention
It is an object of the invention to provide a kind of extract and separate group of the lanthanides and the method for actinides, with can be weary from radioactivity
Extract and separate group of the lanthanides and during actinides in fuel dissolution liquid, high activity liquid waste or acid leaching solution containing lanthanide series, has concurrently good
Good extracting power, loading capacity and extraction selectivity.
In order to achieve this, in the embodiment on basis, the present invention provides a kind of extract and separate lanthanide series, actinium series member
The method of element, described method is to adjust the concentration of inorganic acid in the solution containing group of the lanthanides and actinides for 0.1-5mol/L, so
Add afterwards and contain N, the organic solvent of the sweet acid amic acid of N- dialkyl group two carries out extract and separate.
In a preferred embodiment, the present invention provides a kind of extract and separate group of the lanthanides and the method for actinides, its
The concentration of inorganic acid is 2-5mol/L in middle solution of the regulation containing group of the lanthanides and actinides.
In a preferred embodiment, the present invention provides a kind of extract and separate group of the lanthanides and the method for actinides, its
Described in inorganic acid be nitric acid, hydrochloric acid, phosphoric acid, perchloric acid and/or sulfuric acid.
In a preferred embodiment, the present invention provides a kind of extract and separate group of the lanthanides and the method for actinides, its
Described in N, the sweet acid amic acid of N- dialkyl group two be N, the sweet acid amic acids of N- bis- (2- ethylhexyls) two.
In a preferred embodiment, the present invention provides a kind of extract and separate group of the lanthanides and the method for actinides, its
Described in contain N, the organic solvent of the sweet acid amic acid of N- dialkyl group two is N, and the sweet acid amic acid of N- dialkyl group two has with fat-soluble
The mixture of machine solvent.
In a kind of more preferred embodiment, the present invention provides the side of a kind of extract and separate group of the lanthanides and actinides
Method, wherein one or more of the described fat-soluble organic solvent in kerosene, toluene, dimethylbenzene, diisopropylbenzene (DIPB), n-octyl alcohol
Combination.
In a preferred embodiment, the present invention provides a kind of extract and separate group of the lanthanides and the method for actinides, its
Described in contain N, N, the volume basis of the sweet acid amic acid of N- dialkyl group two in the organic solvent of the sweet acid amic acid of N- dialkyl group two
It is 3.5-40% than content.
In a preferred embodiment, the present invention provides a kind of extract and separate group of the lanthanides and the method for actinides, its
Described in solution containing group of the lanthanides and actinides contain N, the body of the organic solvent of the sweet acid amic acid of N- dialkyl group two with described
Product is than being 1: 10-10: 1.
In a preferred embodiment, the present invention provides a kind of extract and separate group of the lanthanides and the method for actinides, its
Described in extract and separate time be 1-20 minutes.
In a preferred embodiment, the present invention provides a kind of extract and separate group of the lanthanides and the method for actinides, its
Described in extract and separate temperature be 5-50 DEG C.
The beneficial effects of the present invention are utilize the method for the extract and separate group of the lanthanides and actinides of the present invention, Neng Gou
Extract and separate group of the lanthanides and actinides from radioactivity spentnuclear fuel lysate, high activity liquid waste or in the acid leaching solution containing lanthanide series
When, have good extracting power, loading capacity and extraction selectivity concurrently.
The present invention can not be while requirement in terms of meeting extracting power and loading capacity two according to the extractant developed in the past
Defect, designed and synthesized both to meet has good extraction ability under the conditions of highly acidity to lanthanide series and actinides, again
A kind of extractants with larger loading capacity：The sweet acid amic acid (DRDGA) of N, N- dialkyl group two.With N, (the 2- ethyl hexyls of N- bis-
Base) exemplified by two sweet acid amic acids (DEHDGA), its molecular structure is as follows.
The extractant can be used for extract and separate lanthanide series and actinides ion from high acid solution.Due to different price
The lanthanide series of state is different with the extracting power of actinides ion, it can also be used to the separation between different valence state ion.
The extraction separating method of the present invention, is not only suitable for the separation and Extraction rare earth element from metallurgical industry acid solution,
Suitable for separation and Extraction lanthanide series and actinides from nuclear fuel cycle associated acid solution.
Brief description of the drawings
Fig. 1 is the result of study of Eu (III) and U (VI) distribution coefficient in embodiment 1.
Fig. 2 is the result of study of Pu (IV) distribution coefficient in embodiment 2.
Embodiment
The embodiment of the present invention is further illustrated with accompanying drawing with reference to embodiments.
Embodiment 1：Eu (III) and U (VI) distribution coefficient (extracting power) research
Temperature is 25 degree, and extraction time is 5 minutes, is in a ratio of 1: 1,0.5M DEHDGA- kerosene systems extraction trace quantity Eu
(III) and U (VI) result it is as shown in Figure 1.Fig. 1 results illustrate that, as aqueous phase acidity increases, distribution coefficient is first reduced and risen afterwards
Height, distribution ratio is minimum near 1M acidity.Acid concentration be 0.2,0.5,1.0,1.5,2.0,2.5,3M nitric acid when, Eu (III)
Distribution ratio be respectively 510,25,11,13,25,37,45；U (VI) distribution ratio is respectively 15,0.7,0.4,0.88,1.49,
2.2、3.1。
Embodiment 2：The research of Pu (IV) distribution coefficient (extracting power)
Temperature is 25 degree, and extraction time is 5 minutes, is in a ratio of 1: 1,0.05M DEHDGA- kerosene systems extraction trace quantity
Pu (IV) result is as shown in Figure 2.Fig. 2 results illustrate that, as aqueous phase acidity increases, distribution coefficient is first reduced and raised afterwards,
Nearby distribution ratio is minimum for 1M acidity.Acid concentration be 0.2,0.5,1.0,1.5,2.0,2.5,3M nitric acid when, Pu (IV) distribution
Than being respectively 150,15,10,14,25,45,85.
Embodiment 3：Th (IV) loading capacity is studied
Temperature is 25 degree, and extraction time is 5 minutes, is in a ratio of 1: 1,0.5M DEHDGA- kerosene systems from 3M HNO3It is molten
0.15M Th (IV) are extracted in liquid, the Th (IV) more than 99% is extracted in organic phase.
Embodiment 4：DEHDGA is studied the extraction selectivity of group of the lanthanides in high activity liquid waste and actinides
Temperature is 25 degree, and extraction time is 5 minutes, is in a ratio of 1: 1,0.1M DEHDGA- kerosene systems from 1M HNO3It is molten
0.01M Pu (IV) are extracted in liquid and 0.01M Eu (III), the Pu (IV) more than 90% and the Eu (III) less than 10% are extracted
Into organic phase.
Embodiment 5：DEHDGA is studied the extraction selectivity of lanthanide series
Temperature is 25 degree, and extraction time is 5 minutes, is in a ratio of 1: 1,0.2M DEHDGA- kerosene systems dense from lanthanide series
Degree respectively 0.01g/L, and HNO containing 0.3M3Solution in 14 kinds of lanthanide series of extraction (La, Ce, Pr, Nd, Sm, Eu, Gd,
Tb, Dy, Ho, Er, Tm, Yb, Lu), gained distribution ratio is respectively 0.03,0.18,0.40,0.82,4.8,8.2,
9.4,18.7,26.4,33.4,34.3,34.2,33.1,32.5.
Obviously, those skilled in the art can carry out the essence of various changes and modification without departing from the present invention to the present invention
God and scope.So, if these modifications and variations to the present invention belong to the model of the claims in the present invention and its equivalent technology
Within enclosing, then the present invention is also intended to comprising including these changes and modification.Above-described embodiment or embodiment are simply to the present invention
For example, the present invention can also be implemented with other ad hoc fashions or other particular form, without departing from the present invention's
Main idea or substantive characteristics.Therefore, it is regarded as from the point of view of the embodiment of description is in terms of any illustrative and non-limiting.This
The scope of invention should be illustrated that any change equivalent with the intention and scope of claim should also be included by appended claims
Within the scope of the invention.
Claims (10)
1. a kind of method of extract and separate group of the lanthanides and actinides, it is characterised in that described method is that regulation contains group of the lanthanides and actinium
In the solution of series elements the concentration of inorganic acid be 0.1-5mol/L, then add contain N, the sweet acid amic acid of N- dialkyl group two it is organic
Solvent carries out extract and separate.
2. according to the method described in claim 1, it is characterised in that：Adjust inorganic acid in the solution containing group of the lanthanides and actinides
Concentration is 2-5mol/L.
3. according to the method described in claim 1, it is characterised in that：Described inorganic acid is nitric acid, hydrochloric acid, phosphoric acid, perchloric acid
And/or sulfuric acid.
4. according to the method described in claim 1, it is characterised in that：The sweet acid amic acid of described N, N- dialkyl group two is N, N- bis-
(2- ethylhexyls) sweet acid amic acid.
5. according to the method described in claim 1, it is characterised in that：It is described to contain N, the sweet acid amic acid of N- dialkyl group two it is organic
Solvent is N, the mixture of the sweet acid amic acid of N- dialkyl group two and fat-soluble organic solvent.
6. method according to claim 5, it is characterised in that：Described fat-soluble organic solvent is selected from kerosene, toluene, two
One or more of combinations in toluene, diisopropylbenzene (DIPB), n-octyl alcohol.
7. according to the method described in claim 1, it is characterised in that：It is described to contain N, the sweet acid amic acid of N- dialkyl group two it is organic
The volume percent content of the sweet acid amic acid of N in solvent, N- dialkyl group two is 3.5-40%.
8. according to the method described in claim 1, it is characterised in that：The described solution containing group of the lanthanides and actinides with it is described
Containing N, the volume ratio of the organic solvent of the sweet acid amic acid of N- dialkyl group two is 1: 10-10: 1.
9. according to the method described in claim 1, it is characterised in that：The time of described extract and separate is 1-20 minutes.
10. according to the method described in claim 1, it is characterised in that：The temperature of described extract and separate is 5-50 DEG C.
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Cited By (8)
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| CN108017632A (en) * | 2017-11-07 | 2018-05-11 | 四川大学 | Double pyrazole extractant and preparation method thereof and purposes derived from Phen |
| CN109234534A (en) * | 2018-08-08 | 2019-01-18 | 中国原子能科学研究院 | A kind of technique of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste |
| CN109825703A (en) * | 2019-03-15 | 2019-05-31 | 重庆工商大学 | Application of the oligomerization virtue amide compound extractant containing three central hydrogen bonds in separation Ln/An |
| CN110312702A (en) * | 2017-01-26 | 2019-10-08 | 原子能和替代能源委员会 | Particularly for the asymmetric N of SEPARATION OF URANIUM (VI) and plutonium (IV), N- dialkyl amide, synthesis and purposes |
| CN111074083A (en) * | 2020-01-07 | 2020-04-28 | 青岛农业大学 | Method for extracting lanthanide from lanthanum-actinium mixture and application |
| CN111101004A (en) * | 2019-12-16 | 2020-05-05 | 清华大学 | Method for extracting and separating trivalent lanthanide series and trivalent actinide series ions |
| CN113795894A (en) * | 2020-10-14 | 2021-12-14 | 中广核研究院有限公司 | Spent fuel dry post-treatment method based on plasma |
| WO2023131068A1 (en) * | 2022-01-04 | 2023-07-13 | 中国原子能科学研究院 | Trivalent actinides and lanthanides, and trivalent actinide integrated extraction and separation method and system |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110312702A (en) * | 2017-01-26 | 2019-10-08 | 原子能和替代能源委员会 | Particularly for the asymmetric N of SEPARATION OF URANIUM (VI) and plutonium (IV), N- dialkyl amide, synthesis and purposes |
| CN110312702B (en) * | 2017-01-26 | 2022-10-14 | 原子能和替代能源委员会 | Asymmetric N, N-dialkylamides, in particular for separating uranium (VI) and plutonium (IV), their synthesis and use |
| CN108017632A (en) * | 2017-11-07 | 2018-05-11 | 四川大学 | Double pyrazole extractant and preparation method thereof and purposes derived from Phen |
| CN109234534A (en) * | 2018-08-08 | 2019-01-18 | 中国原子能科学研究院 | A kind of technique of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste |
| CN109825703A (en) * | 2019-03-15 | 2019-05-31 | 重庆工商大学 | Application of the oligomerization virtue amide compound extractant containing three central hydrogen bonds in separation Ln/An |
| CN111101004A (en) * | 2019-12-16 | 2020-05-05 | 清华大学 | Method for extracting and separating trivalent lanthanide series and trivalent actinide series ions |
| CN111074083A (en) * | 2020-01-07 | 2020-04-28 | 青岛农业大学 | Method for extracting lanthanide from lanthanum-actinium mixture and application |
| CN113795894A (en) * | 2020-10-14 | 2021-12-14 | 中广核研究院有限公司 | Spent fuel dry post-treatment method based on plasma |
| WO2022077250A1 (en) * | 2020-10-14 | 2022-04-21 | 中广核研究院有限公司 | Dry aftertreatment method for spent fuel employing plasma |
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| WO2023131068A1 (en) * | 2022-01-04 | 2023-07-13 | 中国原子能科学研究院 | Trivalent actinides and lanthanides, and trivalent actinide integrated extraction and separation method and system |
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