CN109517992A - A kind of separation method of trivalent actinium series and lanthanide series - Google Patents
A kind of separation method of trivalent actinium series and lanthanide series Download PDFInfo
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- CN109517992A CN109517992A CN201811620325.4A CN201811620325A CN109517992A CN 109517992 A CN109517992 A CN 109517992A CN 201811620325 A CN201811620325 A CN 201811620325A CN 109517992 A CN109517992 A CN 109517992A
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- trivalent
- series
- separation method
- extraction
- lanthanide series
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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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- 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
- C22B3/40—Mixtures
- C22B3/409—Mixtures at least one compound being an organo-metallic compound
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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
- C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
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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
Abstract
The invention belongs to extraction and separation technology fields, are related to the separation method of a kind of trivalent actinium series and lanthanide series.The separation method is [1 be added after being adjusted with acid acidity in load trivalent actinium series and the organic phase of trivalent lanthanide series, 2,3- triazine -4- base] aqueous solution of pyridine is stripped, trivalent actinides back extraction is taken into water phase, to realize the separation of trivalent actinium series and lanthanide series.Using the separation method of trivalent actinium series and lanthanide series of the invention, back extraction trivalent actinides that can be selective more effectively from the load organic phases of trivalent actinium lanthanum, to realize the separation of trivalent actinium lanthanum.
Description
Technical field
The invention belongs to extraction and separation technology fields, are related to the separation method of a kind of trivalent actinium series and lanthanide series.
Background technique
Nowadays, the development of nuclear energy is one of the important channel for solving energy problem in China, especially to those shortages
The area of power resource.But nuclear energy also produces a large amount of radioactive waste while making huge contribution for the mankind, it
Human development and environment are caused it is direct or potentially hazardous.Therefore, the disposition of dealing carefully with of radioactive waste has become respectively
The problem that state's government and street levels are especially paid attention to, and influence one of the key factor of nuclear energy sustainable development.High activity liquid waste
The safe handling disposition of (High Level radioactive Liquid Waste, HLLW) is Radwastes treatment disposition
Key.
1970s, researcher successively propose " separation-transmuting (partitioning and
Transmutation, P&T) " technical thought of high activity liquid waste is handled, and cause international research concern.P&T is exactly first by secondary actinium
Series elements (Minor Actinide, MA) and long-lived fission product are separated from high activity liquid waste, then are converted by transmuting method
At short life or stable nuclide.After P&T, Minor actinides are converted into the substance of hypotoxicity by high toxicity, to mitigate to ring
The harm in border；Meanwhile Deal with Time can be shortened, simplify the design of disposition library, increases disposition storage capacity, reduce high-level waste body
Product.But containing a large amount of lanthanide series (Lanthanide) simultaneously in high activity liquid waste, majority is that neutron poison is transmuted without can enter
Become treatment process.Therefore, no matter select accelerator or reactor to provide environment for transmuting, require An (III) and Ln first
(III) it is separated.
But due to An (III) (Am in aqueous solution3+, Cm3+) very much like with the chemical characteristic of Ln (III), and be
Hard acid, so that this two is that separation between ion is extremely difficult.Nowadays mature high-level liquid waste partitioning process generally first with
The general character of the two extracts An (III) and Ln (III) jointly, so that the two enters same logistics, recycles both it later
Between fine distinction, realize efficiently separating for An (III) and Ln (III).An (III) is separated with Ln (III) and is mostly used with nitrogenous
Heterocyclic compound is the N corrdination type extractant of representative or the S corrdination type extraction by representative of dithiophosphlic acid class compound
Agent.Another method is the first selectivity back extraction An from the load organic phases for completing An (III) and Ln (III) coextraction process
(III), then the back extraction of Ln (III) is carried out, the process of the program is relatively easy.Representative such mature process is i-
SANEX process and TLSPEAK process: where SO is selected in i-SANEX3The back extraction An (III) of-Ph-BTBP selectivity；
The mixed solution of TLSPEAK process selecting DTPA and lactic acid is as stripping agent.Above-mentioned two process can be from load organic phases
It is directly realized by the separation of An (III) Yu Ln (III), but ineffective.
Therefore, the back extraction trivalent actinium series for selecting suitable water phase complexing agent selective from the load organic phases of trivalent actinium lanthanum
Element realizes that efficiently separating for trivalent actinium lanthanum has great significance.
Summary of the invention
The object of the present invention is to provide the separation method of a kind of trivalent actinium series and lanthanide series, with can be more effectively from three
Selective back extraction trivalent actinides in the load organic phases of valence actinium lanthanum, to realize the separation of trivalent actinium lanthanum.
In order to achieve this, the present invention provides point of a kind of trivalent actinium series and lanthanide series in the embodiment on basis
From method, the separation method is to be added to be adjusted with acid acidity in load trivalent actinium series and the organic phase of trivalent lanthanide series
The aqueous solution of [1,2,3- triazine -4- base] pyridine afterwards is stripped, and trivalent actinides back extraction is taken into water phase, thus real
The separation of existing trivalent actinium series and lanthanide series.
The present invention provides one kind to separate An based on the extractant of water solubility containing N [1,2,3- triazine -4- base] pyridine (PTD)
(III) with the method for Ln (III), the specific technical proposal is: select PTD as stripping agent (its structural formula is as follows),
Its concentration is 5-100mmol/L；The HNO of certain volume is added3, so that HNO in water phase3Concentration is 0.1-3mol/L；
Temperature when extraction controls between 20-25 DEG C.The object that this method is directed to is that TODGA loads the organic of An (III) and Ln (III)
Phase studies 0.2-0.5M TODGA+0.5-1.0M TBP/ kerosene, 0.2-0.5M TODGA+ octanol/kerosene (5%/95%, v/
When v) being used as extraction system, back extraction behavior of the PTD to Am and Eu.Extraction procedure is as shown in Figure 1:
(1) extraction tank 1A is used to be stripped An (III), including stripping section (6-10 grades), for selectivity An (III) is anti-
Extract to water phase.The composition of 1AF is as it was noted above, set its flow as 0.8-1.21mL/min；1AX is the water for being stripped An (III)
Phase system, group become 0.1-3.0mol/L HNO3+ 5-100mol/L PTD solution sets its flow as 0.8-1.0mL/min；
Extraction section (6-8 grades) is mended, a small amount of Ln (III) for that will be stripped into water phase mends extraction and arrives organic phase.1AS group becomes 0.15-
0.2mol/L TODGA+0.4-0.6mol/L TBP sets its flow as 0.3-0.5mL/min.The feed liquid residence time in 1A slot
For 2-5min.
(2) extraction tank 1B is stripped series 8-12 grades for being stripped Ln (III).2BX is the aqueous phase system for being stripped Ln (III),
Group becomes 0.01-0.02mol/L HNO3, its flow is set as 0.8-1.1mL/min.The feed liquid residence time is 2- in 1B slot
5min。
In a preferred embodiment, the present invention provides the separation method of a kind of trivalent actinium series and lanthanide series,
Described in load trivalent actinium series and lanthanide series organic phase in organic solvent be containing TODGA (tetra- octyl of N, N, N`, N`--
3- oxygen glutaramide) organic solvent.
In a kind of more preferred embodiment, the present invention provides the separation side of a kind of trivalent actinium series and lanthanide series
Method, wherein the organic solvent in the organic phase of the load trivalent actinium series and lanthanide series is 0.2-0.5mol/L TODGA+
0.5-1.0mol/L TBP/ kerosene or 0.2-0.5mol/L TODGA+ volume ratio 5% octanol/kerosene.
In a preferred embodiment, the present invention provides the separation method of a kind of trivalent actinium series and lanthanide series,
Described in acid be nitric acid, with nitric acid adjust acidity after, nitric acid in the aqueous solution of described [1,2, the 3- triazine -4- base] pyridine
Concentration is 0.1-3mol/L.
In a preferred embodiment, the present invention provides the separation method of a kind of trivalent actinium series and lanthanide series,
In be adjusted with acid the concentration of [1,2,3- triazine -4- base] pyridine in the aqueous solution of [1,2,3- triazine -4- base] pyridine after acidity
For 5-100mmol/L.
In a preferred embodiment, the present invention provides the separation method of a kind of trivalent actinium series and lanthanide series,
Described in back extraction temperature be 20-25 DEG C.
In a preferred embodiment, the present invention provides the separation method of a kind of trivalent actinium series and lanthanide series,
Described in separation method carried out in extraction tank, the extraction tank includes extraction tank 1A and extraction tank 1B,
The extraction tank 1A includes stripping section and benefit extraction section, and the stripping section is for the first by trivalent actinium series of selectivity
Element, which is stripped, is taken into water phase, and a small amount of trivalent lanthanide series that the benefit extraction section is used to be stripped into water phase, which is mended, to be extracted to organic
Phase；
The extraction tank 1B is for being stripped trivalent lanthanide series.
In a kind of more preferred embodiment, the present invention provides the separation side of a kind of trivalent actinium series and lanthanide series
Method, wherein the stripping section is 6-10 grades, the benefit extraction section is 6-8 grades.
In a kind of more preferred embodiment, the present invention provides the separation side of a kind of trivalent actinium series and lanthanide series
Method, wherein the back extraction series of the extraction tank 1B is 8-12 grades.
In a kind of more preferred embodiment, the present invention provides the separation side of a kind of trivalent actinium series and lanthanide series
Method, wherein the residence time of feed liquid is 2-5min in extraction tank 1A and extraction tank 1B.
The beneficial effects of the present invention are utilize the separation method of trivalent actinium series and lanthanide series of the invention, Neng Gougeng
Effectively back extraction trivalent actinides selective from the load organic phases of trivalent actinium lanthanum, to realize point of trivalent actinium lanthanum
From.
Beneficial effects of the present invention are embodied in:
(1) PTD, can complete burning disposal containing only tetra- kinds of elements of C, H, O, N；
(2) An (III) and Ln (III) are stripped as stripping agent directly from load organic phases using PTD step by step, separated
Effect is good, and the content of lanthanide series is less than 0.3% in An (III) logistics, and the content of actinides is lower than in Ln (III) logistics
0.1%；
(3) it avoids and is first stripped An (III) and Ln (III) into water phase jointly, then the step of carrying out the two separation, simplify
Separation process；
(4) strip kinetics of PTD are fast, and retention time of the logistics in extraction tank is no more than 5min, and can be compared with peracid
(0.5mol/L) is used under degree.
Detailed description of the invention
Fig. 1 is the flow chart of the trivalent actinium lanthanum extraction and separation of embodiment 1.
Specific embodiment
A specific embodiment of the invention is further illustrated with attached drawing with reference to embodiments.
Embodiment 1: the extraction and separation of trivalent actinium series and lanthanide series
1AF is load organic phases, is 0.2mol/L TODGA+0.5mol/L TBP/ kerosin, wherein metal ion
Concentration is as shown in table 1.
The composition of 1 load organic phases 1AF of table
Using mixer-settler as extraction equipment, 1AF feed liquid is separated using process shown in FIG. 1, wherein the benefit of 1A slot extracts
6 grades of section, since the strip kinetics of PTD are fast, sets organic phase in the retention time of 1A slot as 2 minutes by 10 grades of stripping section；1B slot
16 grades of back extraction series, retention time be 2 minutes.The composition and stream of each logistics are than as shown in table 2.
The composition and stream ratio of 2 each bursts of logistics of table
After balance, using the activity of Am and Cm in alpha energy spectrum measurement An (III) and Ln (III) logistics, measured using ICP-MS
Thus concentration of the Ln (III) in two streams calculates An (III) and the content of Ln (III) in two streams, such as 3 institute of table
Show.As can be seen that the yield of all elements shows that mass balance is good all between 99%-106%, and pass through the stream
Journey, 99.9% or more An (III) enter the logistics of An (III), only less than 0.1% entrance Ln (III)；And Ln (III),
99.7% or more entrance purification Ln (III) logistics, only less than 0.3% entrance An (III) logistics.
Content of 3 each element of table in product and extraction raffinate
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.If in this way, belonging to the model of the claims in the present invention and its equivalent technology to these modifications and changes of the present invention
Within enclosing, then the present invention is also intended to include these modifications and variations.Above-described embodiment or embodiment are only 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 of the invention
Main idea or substantive characteristics.Therefore, the embodiment of description is regarded as illustrative and non-limiting in any way.This
The range of invention should be illustrated that any variation equivalent with the intention and range of claim also should include by appended claims
Within the scope of the invention.
Claims (10)
1. a kind of separation method of trivalent actinium series and lanthanide series, it is characterised in that: the separation method is in load trivalent
The aqueous solution for being adjusted with acid [1,2,3- triazine -4- base] pyridine after acidity is added in actinium series and the organic phase of trivalent lanthanide series
It is stripped, trivalent actinides back extraction is taken into water phase, to realize the separation of trivalent actinium series and lanthanide series.
2. separation method according to claim 1, it is characterised in that: the load trivalent actinium series and lanthanide series has
Organic solvent in machine phase is the organic solvent containing TODGA.
3. separation method according to claim 2, it is characterised in that: the load trivalent actinium series and lanthanide series has
Organic solvent in machine phase is 0.2-0.5mol/L TODGA+0.5-1.0mol/L TBP/ kerosene or 0.2-0.5mol/L
5% octanol of TODGA+ volume ratio/kerosene.
4. separation method according to claim 1, it is characterised in that: the acid is nitric acid, after adjusting acidity with nitric acid,
The concentration of nitric acid is 0.1-3mol/L in the aqueous solution of described [1,2, the 3- triazine -4- base] pyridine.
5. separation method according to claim 1, it is characterised in that: [1,2, the 3- triazine -4- after being adjusted with acid acidity
Base] pyridine aqueous solution in [1,2,3- triazine -4- base] pyridine concentration be 5-100mmol/L.
6. separation method according to claim 1, it is characterised in that: the temperature of the back extraction is 20-25 DEG C.
7. separation method described in one of -6 according to claim 1, it is characterised in that: the separation method in extraction tank into
Row, the extraction tank include extraction tank 1A and extraction tank 1B,
The extraction tank 1A includes stripping section and mends extraction section, and the stripping section is anti-by trivalent actinides for selectivity
It is extracted into water phase, a small amount of trivalent lanthanide series that the benefit extraction section is used to be stripped into water phase mends extraction to organic phase；
The extraction tank 1B is for being stripped trivalent lanthanide series.
8. separation method according to claim 7, it is characterised in that: the stripping section is 6-10 grades, the benefit extraction
Section is 6-8 grades.
9. separation method according to claim 7, it is characterised in that: the back extraction series of the extraction tank 1B is 8-12
Grade.
10. separation method according to claim 7, it is characterised in that: the stop of feed liquid in extraction tank 1A and extraction tank 1B
Time is 2-5min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111896573A (en) * | 2020-08-07 | 2020-11-06 | 东华理工大学 | Distributed lanthanum extraction online detection system and detection method based on gamma energy spectrum method |
| CN115572841A (en) * | 2022-09-21 | 2023-01-06 | 中国原子能科学研究院 | Extraction method for extracting Sr (II) from Sr (II) -containing solution |
| 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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| DE102009003783A1 (en) * | 2009-04-15 | 2010-10-21 | Karlsruher Institut für Technologie | Agent, useful for extracting or re-extracting actinide (trivalent form) from a mixture of actinide and lanthanide, comprises 2,6-bis-(5-alkyl-1H-pyrazol-3-yl)-pyridine compounds, lipophilic anion source and an organic or inorganic solvent |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111896573A (en) * | 2020-08-07 | 2020-11-06 | 东华理工大学 | Distributed lanthanum extraction online detection system and detection method based on gamma energy spectrum method |
| CN111896573B (en) * | 2020-08-07 | 2023-09-19 | 东华理工大学 | Online detection system and detection method for distributed lanthanum extraction based on gamma-spectroscopy |
| 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 |
| CN115572841A (en) * | 2022-09-21 | 2023-01-06 | 中国原子能科学研究院 | Extraction method for extracting Sr (II) from Sr (II) -containing solution |
| CN115572841B (en) * | 2022-09-21 | 2023-12-12 | 中国原子能科学研究院 | Extraction method for extracting Sr (II) from solution containing Sr (II) |
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