CN109234534B - A kind of technique of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste - Google Patents
A kind of technique of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste Download PDFInfo
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- CN109234534B CN109234534B CN201810896690.1A CN201810896690A CN109234534B CN 109234534 B CN109234534 B CN 109234534B CN 201810896690 A CN201810896690 A CN 201810896690A CN 109234534 B CN109234534 B CN 109234534B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The disclosure belongs to spentnuclear fuel post-processing technology field, and in particular to a kind of technique of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste.The technique is that trivalent actinium series and trivalent group of the lanthanides are extracted into organic phase in 1A slot using extraction system, washing system and wash Zr, Pd and other fission products；Back extraction system is recycled to be stripped trivalent actinium series and trivalent group of the lanthanides.The technique is good with effect of extracting, back extraction series is few and can reduce the beneficial effect of the radioactive liquid waste volume of subsequent generation to the greatest extent.
Description
Technical field
The disclosure belongs to spentnuclear fuel post-processing technology field, and in particular to one kind coextraction trivalent actinium series from high activity liquid waste
With the technique of trivalent lanthanide series.
Background technique
Include 60 multiple elements in spentnuclear fuel, U, Pu therein can extract by Purex flow, remaining element is then main
Into high activity liquid waste (HLLW).HLLW has long-term irradiation hazard, extracts the α cores such as trivalent actinides therein (Am, Cm)
Element carries out transmuting, and the long-term hazards of HLLW can be greatly shortened, meanwhile, trivalent actinides have important application value.For
This, develops multiple HLLW separation process both at home and abroad, such as the TRPO process of China, the DIMAMEX process of France, the U.S.
TRUEX process and the amido podand process of some country's research and development, these processes can extract the trivalent actinium series member in HLLW
Element.In fact, the chemical property and trivalent actinides due to lanthanide series are close, in these processes, lanthanide series will be into
Enter trivalent actinides logistics, that is, realizes the co-extraction of trivalent actinium series and lanthanide series.
In high-level liquid waste partitioning process, amido podand process is to study more a kind of process recently, and Germany, India, China are all
Correlative study has been carried out, and has developed corresponding amido podand process.Currently, the amido podand process developed both at home and abroad is all made of N,
N, N ',-four octyl -3- oxa- of N '-glutaramide (TODGA) is extractant, structural formula are as follows:
The extracting power of the extractant is strong, so that the back extraction of trivalent actinium series and group of the lanthanides and the decontamination of fission element are difficult, so as to cause anti-
Extract liquid and cleaning solution relative volume is larger, corresponding back extraction sum of series washing series is more, and the waste liquid of generation also increases.Therefore,
At present need to seek a kind of effect of extracting it is good and can reduce to the greatest extent radioactive liquid waste generate coextraction trivalent actinium series and trivalent lanthanum
The technique of series elements.
Summary of the invention
(1) goal of the invention
According to the problems of prior art, that present disclose provides a kind of effect of extracting is good, back extraction series is few and can use up
Amount reduces the work of coextraction trivalent actinium series and trivalent lanthanide series in the slave high activity liquid waste of the radioactive liquid waste volume of subsequent generation
Skill.
(2) technical solution
In order to solve the problems of prior art, technical solution provided by the invention is as follows:
A kind of technique of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste, the technique are to utilize extractor body
Trivalent actinium series and trivalent group of the lanthanides are extracted into organic phase in 1A slot and wash Zr, Pd and other fission products by system, washing system；
Back extraction system is recycled to be stripped trivalent actinium series and trivalent group of the lanthanides, specific steps include:
1) concentrated nitric acid is added, by the acidity adjustment of high activity liquid waste to be processed (HLLW) to 4~4.5mol/L, and sets height and puts
The flow of waste liquid is 1；Oxalic acid and HEDTA is added into the high activity liquid waste after tune acid, and makes the concentration of oxalic acid in high activity liquid waste
For 0.15~0.20mol/L, HEDTA concentration is 0.05~0.08mol/L in high activity liquid waste；
2) extraction system is added to the extraction section of 1A slot；Extraction system includes extractant 1AX and phase modifying agent TBP,
Middle extractant is N, N, N ',-four octyl -2- methyl -3- oxa- of N '-glutaryl, structural formula are as follows:
The extracting power of the extractant is weaker than TODGA, but the back extraction series of rear end stripping section can be effectively reduced using the extractant,
Spent Radioactive liquid measure can be greatly reduced simultaneously.
3) washing system is added to the washing section of 1A slot, wherein washing section is divided into the first washing section and the second washing section,
Washing system includes first washing system 1AS corresponding with washing section1With the second washing system 1AS2；Wherein the first washing system
1AS1It is made of 2.5~3mol/L nitric acid, 0.3~0.4mol/L oxalic acid and 0.08~0.1mol/L HEDTA, is put relative to height
The flow-rate ratio of waste liquid is 0.4~0.6；Second washing system 1AS2Stream for 1.5~1.8mol/L nitric acid, relative to high activity liquid waste
Amount is than being 0.4~0.6；
4) the feed liquid 1AP that 1A slot obtains is introduced in 2B slot；Stripping agent 2BX is added to the stripping section of 2B slot, wherein
2BX is 0.05~0.10mol/L nitric acid, the flow-rate ratio 0.5~0.6 relative to high activity liquid waste；
Preferably, the N, N, N ',-four octyl -2- methyl -3- oxa- of N '-glutaryl concentration be 0.15~
0.25mol/L。
Preferably, the series of extraction section is 5~7 grades.
Preferably, the concentration of the phase modifying agent TBP is 0.3~0.6mol/L.
Preferably, the N, N, N ',-four octyl -2- methyl -3- oxa- of N '-glutaryl concentration is 0.2mol/L.
Preferably, the concentration of the modifying agent TBP is 0.5mol/L.
Preferably, it is 1~1.2 that the stream of extraction system and high activity liquid waste, which compares,.
Preferably, the washing series of first washing section is 5~7 grades, and the washing series of the second washing section is 4~5 grades.
Preferably, the back extraction series of stripping section is 8~12 grades.
Preferably, the extraction series of the extraction section is 6 grades, and the washing series of the first washing section is 6 grades, the second washing section
Washing series be 4 grades.
(3) beneficial effect
The disclosure uses N, N, N ',-four octyl -2- methyl -3- oxa- of N '-glutaryl is as extractant from high activity liquid waste
Trivalent actinium series and trivalent lanthanide series are extracted, traditional method using TODGA as extractant is changed, due to the extractant
Extracting power be weaker than TODGA, the extraction of the fission products such as Zr, Pd, Sr can be effectively reduced, to reduce cleaning solution volume；
Meanwhile the single-stage distribution ratio of (concentration of nitric acid is less than 0.1mol/L) extraction trivalent actinium series and trivalent group of the lanthanides is much smaller than under low acid
TODGA, is conducive to the back extraction of trivalent actinium series and trivalent group of the lanthanides, to reduce back extraction sum of series strip liquor volume.Generally speaking
The waste liquid amount that the technique provided using the disclosure is generated is about the half of TODGA process.The disclosure also defines extraction, washes simultaneously
The design parameter and process washed and be stripped ensure that the effect of extracting of coextraction trivalent group of the lanthanides and trivalent actinium series, specific effect are as follows:
1. by the acidity adjustment of high activity liquid waste HLLW to be processed to 4~4.5mol/L, N, N, N under the acidity ', N '-four is pungent
Base -2- methyl -3- oxa--glutaryl is relatively strong to the extracting power of trivalent actinium series and group of the lanthanides (single-stage distribution ratio is greater than 100), can protect
Demonstrate,prove effective extraction of trivalent actinium series and trivalent group of the lanthanides；0.15~0.20mol/L oxalic acid and 0.05~0.08mol/L is added
HEDTA can be greatly reduced the fission products such as Zr, Pd and be extracted into organic phase.
2. extraction system includes extractant N, N, N ',-four octyl -2- methyl -3- oxa- of N '-glutaryl and phase modifying agent
TBP is avoided merely using N, N, N ', when-four octyl -2- methyl -3- oxa- of N '-glutaryl, generates three-phase, to prevent three-phase
Appearance, need to be added TBP as phase modifying agent.
3. washing section is divided into two sections, wherein the first washing section is for washing the fission products such as Zr, Pd in organic phase；The
Two washing sections are for washing the Sr extracted in organic phase, oxalic acid and nitric acid.
4. the stripping agent 2BX of stripping section be 0.05~0.10mol/L nitric acid, relative to high activity liquid waste flow be 0.5~
0.6, when the benefit of the concentration and flow is that back extraction acidity is too low, organic phase and water phase split-phase are more difficult, and back extraction acidity is larger
When, trivalent actinium series and trivalent group of the lanthanides in load organic phases cannot be stripped completely.
5. the extraction system and technique make the rate of recovery of trivalent actinium series and group of the lanthanides be all larger than 99.99%, except 1% or so
Outside Ru, the content of other elements is respectively less than 0.1% in product.
Detailed description of the invention
Fig. 1 is the flow diagram that embodiment 1 provides.
Specific embodiment
The application is further elaborated below in conjunction with specification drawings and specific embodiments.
Embodiment 1
A kind of technique of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste, as schematically shown in Figure 1.The technique
Be trivalent actinium series and trivalent group of the lanthanides are extracted into organic phase in 1A slot using extraction system, washing system and wash Zr, Pd and
Other fission products；Trivalent actinium series and group of the lanthanides are stripped using back extraction system, specific steps include:
1) concentrated nitric acid is added, by the acidity adjustment of high activity liquid waste to be processed (HLLW) to 4mol/L, and sets high activity liquid waste
Flow be 1；Oxalic acid and HEDTA is added to adjusting in the high activity liquid waste after acid, and makes the concentration of oxalic acid in high activity liquid waste to be
0.15mol/L, HEDTA concentration is 0.05mol/L in high activity liquid waste；N, N, N under the acidity ',-four octyl -2- methyl -3- oxygen of N '
Miscellaneous-glutaryl is relatively strong to the extracting power of trivalent actinium series and group of the lanthanides (single-stage distribution ratio is greater than 100), it is ensured that trivalent actinium series and three
Effective extraction of valence group of the lanthanides；0.15mol/L oxalic acid and 0.05mol/L HEDTA is added, the slivers such as Zr, Pd member can be greatly reduced
Element is extracted into organic phase.
2) extraction system is added to the extraction section of 1A slot, the series of extraction section is 6 grades.Extraction system includes extractant
1AX and phase modifying agent TBP, wherein extractant is the N that concentration is 0.15mol/L, N, N ',-four octyl -2- methyl -3- oxa- of N ' -
Glutaryl, structural formula are as follows:The concentration of phase modifying agent TBP is 0.3mol/L, is avoided simple
N, N, N ', there is the phenomenon that three-phase in solution when-four octyl -2- methyl -3- oxa- of N '-glutaryl.The extracting power of the extractant
It is weaker than TODGA, but the back extraction series of rear end stripping section can be effectively reduced using the extractant, while radiation can be greatly reduced
Property waste liquid amount.It is 1 that the stream of extraction system and high activity liquid waste, which compares,.
3) washing system is added to the washing section of 1A slot, wherein washing section is divided into the first washing section and the second washing section,
Washing system includes first washing system 1AS corresponding with washing section1With the second washing system 1AS2；Wherein the first washing system
1AS1It is made of 2.5mol/L nitric acid, 0.3mol/L oxalic acid and 0.08mol/L HEDTA, the flow relative to high activity liquid waste is
0.4, for washing the Fission products element such as Zr, Pd in organic phase；Second washing system 1AS2For 1.5mol/L nitric acid, relatively
In high activity liquid waste flow be 0.4, for washing the Sr extracted in organic phase, oxalic acid and nitric acid.
The washing series of first washing section is 6 grades, and the washing series of the second washing section is 4 grades.
4) the feed liquid 1AP that 1A slot obtains is introduced in 2B slot；Stripping agent 2BX is added to the stripping section of 2B slot, wherein
2BX is 0.05~0.10mol/L nitric acid, the flow 0.5~0.6 relative to high activity liquid waste；It is 8 grades that stripping section, which is stripped series,.
When the concentration and the benefit of flow are that back extraction acidity is too low, organic phase and water phase split-phase are more difficult, are stripped acidity
When higher, trivalent actinium series and trivalent group of the lanthanides in load organic phases cannot be stripped completely.
Extraction experiments are carried out using high activity liquid waste of the above method to simulation, high activity liquid waste composition is as shown in table 1,
1 simulated high-level radioactive waste element of table composition and concentration
After balance, content of each element in trivalent actinium series and trivalent group of the lanthanides product liquid, extraction raffinate is as shown in table 2.Institute
There is the yield of element all between 95%~112%.By the process, the rate of recovery of trivalent actinium series and trivalent lanthanide series is big
In 99.99%.The purity is high of trivalent actinium lanthanum product, except 1.1% Ru, the content of other elements is respectively less than 0.1%.
Content of 2 each element of table in product and extraction raffinate
Embodiment 2
Unlike the first embodiment, by the acidity adjustment of high activity liquid waste to be processed (HLLW) to 4mol/L in step 1)；To
Oxalic acid and HEDTA are added in high activity liquid waste after adjusting acid, and the concentration of oxalic acid in high activity liquid waste is made to be 0.20mol/L, Gao Fang
HEDTA concentration is 0.06mol/L in waste liquid；
N described in step 2), N, N ',-four octyl -2- methyl -3- oxa- of N '-glutaryl concentration is 0.2mol/L.Phase
The concentration of modifying agent TBP is 0.4mol/L；It is 1.1 that the stream of extraction system and high activity liquid waste, which compares,.The series of extraction section is 5 grades.
First washing system 1AS in step 3)1By 2.8mol/L nitric acid, 0.35mol/L oxalic acid and 0.09mol/L HEDTA
Composition, the flow relative to high activity liquid waste are 0.5；Second washing system 1AS2For 1.6mol/L nitric acid, relative to high activity liquid waste
Flow be 0.5；2BX is 0.08mol/L nitric acid in step 4), and the flow relative to high activity liquid waste is 0.55；Described first washes
The washing series for washing section is 6 grades, and the washing series of the second washing section is 5 grades.It is 10 grades that stripping section, which is stripped series,.
Embodiment 3
Unlike the first embodiment, by the acidity adjustment of high activity liquid waste to be processed (HLLW) to 4.2mol/L in step 1)；
Oxalic acid and HEDTA is added into the high activity liquid waste after tune acid, and the concentration of oxalic acid in high activity liquid waste is made to be 0.18mol/L, it is high
HEDTA concentration is 0.08mol/L in radioactive waste liquid；
N described in step 2), N, N ',-four octyl -2- methyl -3- oxa- of N '-glutaryl concentration is 0.25mol/L.Phase
The concentration of modifying agent TBP is 0.6mol/L；It is 1.2 that the stream of extraction system and high activity liquid waste, which compares,.The series of extraction section is 7 grades.
First washing system 1AS in step 3)1By 3mol/L nitric acid, 0.4mol/L oxalic acid and 0.1mol/L HEDTA group
At the flow relative to high activity liquid waste is 0.6；Second washing system 1AS2For 1.8mol/L nitric acid, relative to high activity liquid waste
Flow is 0.6；2BX is 0.1mol/L nitric acid in step 4), and the flow relative to high activity liquid waste is 0.6；First washing section
Washing series be 5 grades, the washing series of the second washing section is 4 grades.It is 12 grades that stripping section, which is stripped series,.
Claims (10)
1. a kind of technique of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste, which is characterized in that the technique is
Trivalent actinium series and trivalent group of the lanthanides are extracted into organic phase in 1A slot using extraction system, washing system and wash Zr, Pd and its
His fission product；Back extraction system is recycled to be stripped trivalent actinium series and trivalent group of the lanthanides, specific steps include:
(1) concentrated nitric acid is added, by the acidity adjustment of high activity liquid waste to be processed to 4~4.5mol/L, and sets the stream of high activity liquid waste
Amount is 1；Oxalic acid and HEDTA is added to adjusting in the high activity liquid waste after acid, and make the concentration of oxalic acid in high activity liquid waste be 0.15~
0.20mol/L, HEDTA concentration is 0.05~0.08mol/L in high activity liquid waste；
(2) extraction system is added to the extraction section of 1A slot；Extraction system includes extractant 1AX and phase modifying agent TBP, wherein extracting
Taking agent is N, N, N ',-four octyl -2- methyl -3- oxa- of N '-glutaryl, structural formula are as follows:
(3) washing system is added to the washing section of 1A slot, wherein washing section is divided into the first washing section and the second washing section, washing
System includes the first washing system corresponding with washing section and the second washing system；Wherein the first washing system is by 2.5~3mol/
L nitric acid, 0.3~0.4mol/L oxalic acid and 0.08~0.1mol/L HEDTA composition, the flow-rate ratio relative to high activity liquid waste are 0.4
~0.6；Second washing system is 1.5~1.8mol/L nitric acid, and the flow-rate ratio relative to high activity liquid waste is 0.4~0.6；
(4) the feed liquid 1AP that 1A slot obtains is introduced in 2B slot；Stripping agent 2BX is added to the stripping section of 2B slot, wherein 2BX
For 0.05~0.10mol/L nitric acid, the flow-rate ratio relative to high activity liquid waste is 0.5~0.6.
2. the technique of a kind of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste according to claim 1,
It is characterized in that, the concentration of N, N, N described in step (2) ', N '-four octyl -2- methyl -3- oxa-s-glutaryl be 0.15~
0.25mol/L。
3. the technique of a kind of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste according to claim 1,
It is characterized in that, the series of extraction section described in step (2) is 5~7 grades.
4. the technique of a kind of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste according to claim 1,
It is characterized in that, the concentration of phase modifying agent TBP described in step (2) is 0.3~0.6mol/L.
5. the technique of a kind of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste according to claim 1,
It is characterized in that, the concentration of N, N, N described in step (2) ', N '-four octyl -2- methyl -3- oxa-s-glutaryl is 0.2mol/
L。
6. the technique of a kind of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste according to claim 1,
It is characterized in that, the concentration of modifying agent TBP described in step (2) is 0.5mol/L.
7. the technique of a kind of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste according to claim 1,
It is characterized in that, it is 1~1.2 that the stream of extraction system described in step (2) and high activity liquid waste, which compares,.
8. the technique of a kind of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste according to claim 1,
It is characterized in that, the washing series of the first washing section described in step (3) is 5~7 grades, the washing series of the second washing section is 4
~5 grades.
9. the technique of a kind of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste according to claim 1,
It is characterized in that, the back extraction series of step (4) stripping section is 8~12 grades.
10. the technique of a kind of coextraction trivalent actinium series and trivalent lanthanide series from high activity liquid waste according to claim 1,
It is characterized in that, the extraction series of the extraction section is 6 grades, the washing series of the first washing section is 6 grades, and the second washing section is washed
Washing series is 4 grades.
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