CN106629807A - Method for preparing nuclear-pure thorium tetrafluoride from thorium oxalate through purification - Google Patents
Method for preparing nuclear-pure thorium tetrafluoride from thorium oxalate through purification Download PDFInfo
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- CN106629807A CN106629807A CN201611048130.8A CN201611048130A CN106629807A CN 106629807 A CN106629807 A CN 106629807A CN 201611048130 A CN201611048130 A CN 201611048130A CN 106629807 A CN106629807 A CN 106629807A
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- thorium
- tetrafluoride
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- purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F15/00—Compounds of thorium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Abstract
The invention provides a method for preparing nuclear-pure thorium tetrafluoride from thorium oxalate slag through purification. The method comprises the following steps: (1) dissolving thorium oxalate in nitric acid after alkali conversion; (2) reducing tetravalent cerium with hydrogen peroxide, extracting uranium with low concentration TBP and extracting thorium with high concentration TBP; (3) precipitating and dehydrating thorium tetrafluoride. The thorium tetrafluoride prepared and obtained by a set of technological method from conversion of thorium oxalate slag to extraction and preparation of thorium tetrafluoride in the invention meets standards of raw materials for a molten salt reactor, has the experimental transformation ability reaching the kilogram level, and has the production capacity easy to expand.
Description
Technical field
The invention belongs to nuclear fuel material prepared technology field, and in particular to it is a kind of with Extraction of rare eart when produce it is impure
High thhorium oxalate slag is method of the raw material through converting, purifying, preparing the pure thorium tetrafluoride of core.
Background technology
Thorium has naturally radioactive, and thorium tetrafluoride can produce metal thorium, also may be used by carrying out thermal reduction with calcium metal or magnesium
The powder of metal thorium is obtained in fused salt electrolysis process, with LiF, BeF2、UF4Fusedsalt reactor is may together for Deng salt-mixture.232Th is captureed
Obtain fissible generation after conversion after a neutron233U,233U be with235U and239Pu equally can be used for reactor by fission chain
Formula reaction produces substantial amounts of nuclear energy.In China's thorium resources the thorium anhydride total amount verified is enriched about at 28.6335 ten thousand tons.
What at present bulk concentrate was commonly used in Rare Earth Production is water logging separating technology after sulfuric acid high-temperature process, and high temperature is roasted
Burn heating response when rare earth element generate can rare earth sulfate soluble in water be dissolved in solution, thorium formed thorium pyrophosphate or
The water insoluble and sour aggregation in slag of thorium phosphate, because the thorium in waste residue has radioactivity, substantial amounts of thorium resources are finally with waste residue
Form storage is pending, causes secondary environment pollution problem.In order to extract thorium in Rare Earth Production, there is document report to roast
Burn thorium when temperature is reduced and generate water-soluble sulfate with rare earth, then extraction precipitation obtains the higher thhorium oxalate of purity
Prepare for subsequent combustion and raw material is provided.Thus the thorium compound purity relatively low (main component is as shown in table 1) of Process production, difficult
To reach the purity requirement of nuclear energy fuel property, to prepare and meet the core pure compound impurity content of nuclear fuel requirement especially
It is to cover the big chemical element in section to thermal neutron prisoner to separate again, required purity is made by further purification
Compound.
The thhorium oxalate of table 1 calcines the composition content of rear oxidation thing
The content of the invention
It is an object of the invention to provide purification prepares the preparation method of the pure level thorium tetrafluoride of core in a kind of slag from thhorium oxalate,
The method prepares the pure level thorium tetrafluoride of core by purifying conversion to thhorium oxalate slag, and to obtain thorium base MSR raw material is used for.
To reach above-mentioned purpose, the technical solution used in the present invention is：One kind purification from thhorium oxalate prepares core pure four
The method of thorium fluoride, it comprises the steps：
(1) nitric acid dissolving after the conversion of thhorium oxalate alkali
Weigh thhorium oxalate raw material to add water pulping, add NaOH, the addition mole of thhorium oxalate raw material and NaOH
Than for 1：(4～12), 60～110 DEG C of temperature, temperature retention time 0.5～5 hour, slurry filtration obtains thorium dioxide solid, then
Nitric acid dissolving is added to the solid after filtration, concentration of nitric acid exists in gained lysate after dissolving reaction for the addition control of nitric acid
0.5～5mol/L；Then filter and obtain thorium nitrate solution, thorium nitrate concentration is 80～150g/L in solution；
(2) hydrogen peroxide reduction quadrivalent cerium, low concentration TBP extraction uranium and high concentration TBP extraction thorium：
Hydrogen peroxide, every liter of Th (NO are added in step (1) gained thorium nitrate solution3)4The H added in solution2O2Measure as 10
～200ml, obtains Th (NO3)4Material liquid；
Then to adopt volume ratio be 2%～10%TBP- kerosene to Th (NO3)4Material liquid carries out putting forward uranium extraction, water phase and an oil phase
Than for 1：(0.9～1.1)；
Then volume ratio is mutually used for 25%～40%TBP- sulfonated kerosene counter-current extractions to extraction gained water, water phase and an oil phase ratio
For 1：(0.9～1.1), is then washed to saturated organic phase with 3.5～5mol/L nitric acid, afterwards with 50～60 DEG C of deionizations
Water carries out back extraction, obtains pure thorium nitrate solution；
(3) thorium tetrafluoride precipitation and dehydration：
Add hydrofluoric acid in step (2) thorium nitrate solution after purification under agitation, reaction temperature is 50～95 DEG C, hydrogen
Fluoric acid adds mole for 4～5 times of thorium nitrate mole, filters after 15～30min of ageing；After filtering obtain aqueous four
Thorium fluoride filter cake；
Aqueous thorium tetrafluoride filter cake sloughs suction under inert gas shielding in the drying 1.5～4 hours of 150～250 DEG C of temperature
Attached water, in 440～650 DEG C of calcining 10～60min removing crystallizations water of temperature water content is obtained<0.05% thorium tetrafluoride finished product.
The method that a kind of purification from thhorium oxalate as above prepares the pure thorium tetrafluoride of core, the title described in its step (1)
Take thhorium oxalate raw material to add water pulping, add NaOH, alkali addition to be the 105%～300% of theoretical amount.
The method that a kind of purification from thhorium oxalate as above prepares the pure thorium tetrafluoride of core, adopting described in its step (2)
With 2%～10% TBP- kerosene to Th (NO3)4Material liquid carries out carrying uranium extraction, and extraction series is 5 grades.
The method that a kind of purification from thhorium oxalate as above prepares the pure thorium tetrafluoride of core, adopting described in its step (2)
With 25%～40%TBP- sulfonated kerosene counter-current extractions, using 10 grades of mixer-settlers as extraction section, 5 grades of washing sections, with 10 grades
Mixer-settler is used as back extraction section.
The method that a kind of purification from thhorium oxalate as above prepares the pure thorium tetrafluoride of core, described in its step (3)
Stirring is lower plus hydrofluoric acid is to excessive 2%～15%, filters after ageing, and reaction temperature is 50～95 DEG C.
Having the beneficial effect that acquired by the present invention：(1) thorium tetrafluoride prepared by the present invention can be by entering with calcium metal or magnesium
Row thermal reduction produces metal thorium, and the powder of metal thorium also can be prepared in fused salt electrolysis process, also serves as thorium base fusedsalt reactor raw material.
(2) present invention can carry out extracting conversion processing to radiation to the thhorium oxalate slag for producing uranium-bearing, cerium and other impurities during Extraction of rare eart
Property element carry out effective recycling, reduce the radioactive pollution to environment.(3) present invention adds nitre after converting with thhorium oxalate and alkali
Acid dissolving, solute effect is easy to industrialized production well after conversion.(4) present invention separates pre- using hydrogen peroxide to uranium, cerium with thorium
Again high concentration TBP extracts the mode of thorium first to reduce quadrivalent cerium joint low concentration TBP extraction uranium, and extractant is inexpensive to be easy to industrial metaplasia
Produce, purification effect well meets the purity needs of thorium tetrafluoride.
The present invention converts, extracts, preparing a whole set of process of thorium tetrafluoride, the tetrafluoro for preparing from thhorium oxalate slag
Change thorium and meet MSR raw material standard, experiment conversion capability reaches feather weight level, and production capacity is easily enlarged, to later
Thorium base MSR raw material is studied and practical application is significant.
Description of the drawings
Fig. 1 is that the present invention converts the flow chart that purification prepares thorium tetrafluoride from thhorium oxalate slag.
Specific embodiment
Below in conjunction with the accompanying drawings prepared by the pure tetrafluoro of core to one kind purification from thhorium oxalate of the present invention with specific embodiment
The method for changing thorium is further described.
Embodiment 1
The method that a kind of purification from thhorium oxalate of the present invention prepares the pure thorium tetrafluoride of core, it comprises the steps：
(1) nitric acid dissolving after the conversion of thhorium oxalate alkali
Weigh thhorium oxalate raw material to add water pulping, add NaOH, the addition mole of thhorium oxalate raw material and NaOH
Than for 1：8,80 DEG C of temperature, temperature retention time 2 hours, slurry filtration obtains thorium dioxide solid, then adds to the solid after filtration
Enter nitric acid dissolving, concentration of nitric acid is in 4mol/L in addition control lysate obtained by after dissolving reaction of nitric acid；Then filter
Thorium nitrate solution is obtained, thorium nitrate concentration is 80g/L in solution；
(2) hydrogen peroxide reduction quadrivalent cerium, low concentration TBP extraction uranium and high concentration TBP extraction thorium：
Hydrogen peroxide, every liter of Th (NO are added in step (1) gained thorium nitrate solution3)4The H added in solution2O2Measure and be
50ml, obtains Th (NO3)4Material liquid；
Then to adopt volume ratio be 5%TBP- kerosene to Th (NO3)4Material liquid carries out carrying uranium extraction, and water phase and an oil phase ratio is 1：
1；Temperature is 40 DEG C, and extraction series is 5 grades.
Then it is 40%TBP- sulfonated kerosene counter-current extractions to extraction gained water volume ratio, water phase and an oil phase ratio is 1：1,
Then saturated organic phase is washed with 4mol/L nitric acid, carries out back extraction with 55 DEG C of deionized waters afterwards, obtain pure
Thorium nitrate solution；The process route of counter-current extraction, using 10 grades of mixer-settlers as extraction section, 5 grades of washing sections, with 10 grades of mixing
Defecator is used as back extraction section.
(3) thorium tetrafluoride precipitation and dehydration：
Add hydrofluoric acid in step (2) thorium nitrate solution after purification under agitation, reaction temperature is 85 DEG C, hydrofluoric acid
Mole is added for 4 times of thorium nitrate mole, is filtered after ageing 30min；After filtering obtain aqueous thorium tetrafluoride filter cake；
Aqueous thorium tetrafluoride filter cake sloughs absorption water under inert gas shielding in the drying 2 hours of 250 DEG C of temperature, in temperature
550 DEG C of calcining 30min removing crystallizations water obtain water content<0.05% thorium tetrafluoride finished product (lily thorium tetrafluoride powder
End).
Chemical analysis is carried out to products obtained therefrom, as a result such as table 2.
The thorium tetrafluoride powder impurities analysis result unit of table 2：μg/g
Embodiment 2
The method that a kind of purification from thhorium oxalate of the present invention prepares the pure thorium tetrafluoride of core, it comprises the steps：
(1) nitric acid dissolving after the conversion of thhorium oxalate alkali
Weigh thhorium oxalate raw material to add water pulping, add NaOH, the addition mole of thhorium oxalate raw material and NaOH
Than for 1：4, temperature 60 C, temperature retention time 5 hours, slurry filtration obtains thorium dioxide solid, then adds to the solid after filtration
Enter nitric acid dissolving, concentration of nitric acid is in 0.5mol/L in addition control lysate obtained by after dissolving reaction of nitric acid；Then cross
Filter obtains thorium nitrate solution, and thorium nitrate concentration is 90g/L in solution；
(2) hydrogen peroxide reduction quadrivalent cerium, low concentration TBP extraction uranium and high concentration TBP extraction thorium：
Hydrogen peroxide, every liter of Th (NO are added in step (1) gained thorium nitrate solution3)4The H added in solution2O2Measure and be
10ml, obtains Th (NO3)4Material liquid；
Then to adopt volume ratio be 2%TBP- kerosene to Th (NO3)4Material liquid carries out carrying uranium extraction, and water phase and an oil phase ratio is 1：
0.9；Temperature is 40 DEG C, and extraction series is 5 grades.
Then it is 40%TBP- sulfonated kerosene counter-current extractions to extraction gained water volume ratio, water phase and an oil phase ratio is 1：
0.9, then saturated organic phase is washed with 4mol/L nitric acid, afterwards back extraction is carried out with 55 DEG C of deionized waters, obtain pure
Net thorium nitrate solution；The process route of counter-current extraction, using 10 grades of mixer-settlers as extraction section, 5 grades of washing sections, with 10 grades
Mixer-settler is used as back extraction section.
(3) thorium tetrafluoride precipitation and dehydration：
Add hydrofluoric acid in step (2) thorium nitrate solution after purification under agitation, reaction temperature is 50 DEG C, hydrofluoric acid
Mole is added for 4 times of thorium nitrate mole, is filtered after ageing 15min；After filtering obtain aqueous thorium tetrafluoride filter cake；
Aqueous thorium tetrafluoride filter cake sloughs absorption water under inert gas shielding in the drying 1.5 hours of 150 DEG C of temperature, in temperature
440 DEG C of calcining 60min removing crystallizations water of degree obtain water content<0.05% thorium tetrafluoride finished product (lily thorium tetrafluoride powder
End).
Embodiment 3
The method that a kind of purification from thhorium oxalate of the present invention prepares the pure thorium tetrafluoride of core, it comprises the steps：
(1) nitric acid dissolving after the conversion of thhorium oxalate alkali
Weigh thhorium oxalate raw material to add water pulping, add NaOH, the addition mole of thhorium oxalate raw material and NaOH
Than for 1：12,110 DEG C of temperature, temperature retention time 5 hours, slurry filtration obtains thorium dioxide solid, then to the solid after filtration
Addition nitric acid dissolving, concentration of nitric acid is in 5mol/L in addition control lysate obtained by after dissolving reaction of nitric acid；Then cross
Filter obtains thorium nitrate solution, and thorium nitrate concentration is 150g/L in solution；
(2) hydrogen peroxide reduction quadrivalent cerium, low concentration TBP extraction uranium and high concentration TBP extraction thorium：
Hydrogen peroxide, every liter of Th (NO are added in step (1) gained thorium nitrate solution3)4The H added in solution2O2Measure and be
200ml, obtains Th (NO3)4Material liquid；
Then to adopt volume ratio be 5%TBP- kerosene to Th (NO3)4Material liquid carries out carrying uranium extraction, and water phase and an oil phase ratio is 1：
1.1；Temperature is 40 DEG C.
Then it is 40%TBP- sulfonated kerosene counter-current extractions to extraction gained water volume ratio, water phase and an oil phase ratio is 1：
1.1, then saturated organic phase is washed with 5mol/L nitric acid, afterwards back extraction is carried out with 60 DEG C of deionized waters, obtain pure
Net thorium nitrate solution.
(3) thorium tetrafluoride precipitation and dehydration：
Add hydrofluoric acid in step (2) thorium nitrate solution after purification under agitation, reaction temperature is 95 DEG C, hydrofluoric acid
Mole is added for 5 times of thorium nitrate mole, is filtered after ageing 20min；After filtering obtain aqueous thorium tetrafluoride filter cake；
Aqueous thorium tetrafluoride filter cake sloughs absorption water under inert gas shielding in the drying 3 hours of 200 DEG C of temperature, in temperature
650 DEG C of calcining 10min removing crystallizations water obtain water content<0.05% thorium tetrafluoride finished product (lily thorium tetrafluoride powder
End).
Claims (5)
1. a kind of method that purification from thhorium oxalate prepares the pure thorium tetrafluoride of core, it is characterised in that：The method comprises the steps：
(1) nitric acid dissolving after the conversion of thhorium oxalate alkali
Weigh thhorium oxalate raw material to add water pulping, add the NaOH, thhorium oxalate raw material to be with the addition mol ratio of NaOH
1：(4～12), 60～110 DEG C of temperature, temperature retention time 0.5～5 hour, slurry filtration obtains thorium dioxide solid, then to mistake
Solid addition nitric acid dissolving after filter, concentration of nitric acid is 0.5 in addition control lysate obtained by after dissolving reaction of nitric acid
～5mol/L；Then filter and obtain thorium nitrate solution, thorium nitrate concentration is 80～150g/L in solution；
(2) hydrogen peroxide reduction quadrivalent cerium, low concentration TBP extraction uranium and high concentration TBP extraction thorium：
Hydrogen peroxide, every liter of Th (NO are added in step (1) gained thorium nitrate solution3)4The H added in solution2O2Measure as 10～
200ml, obtains Th (NO3)4Material liquid；
Then to adopt volume ratio be 2%～10%TBP- kerosene to Th (NO3)4Material liquid carries out carrying uranium extraction, and water phase and an oil phase ratio is
1：(0.9～1.1)；
Then it is mutually 25%～40%TBP- sulfonated kerosene counter-current extractions with volume ratio to extraction gained water, water phase and an oil phase ratio is 1：
(0.9～1.1), is then washed to saturated organic phase with 3.5～5mol/L nitric acid, is entered with 50～60 DEG C of deionized waters afterwards
Row back extraction, obtains pure thorium nitrate solution；
(3) thorium tetrafluoride precipitation and dehydration：
Add hydrofluoric acid in step (2) thorium nitrate solution after purification under agitation, reaction temperature is 50～95 DEG C, hydrofluoric acid
Mole is added for 4～5 times of thorium nitrate mole, is filtered after 15～30min of ageing；After filtering obtain aqueous tetrafluoride
Thorium filter cake；
Aqueous thorium tetrafluoride filter cake sloughs absorption water under inert gas shielding in the drying 1.5～4 hours of 150～250 DEG C of temperature,
Water content is obtained in 440～650 DEG C of calcining 10～60min removing crystallizations water of temperature<0.05% thorium tetrafluoride finished product.
2. the method that a kind of purification from thhorium oxalate according to claim 1 prepares the pure thorium tetrafluoride of core, it is characterised in that：
The thhorium oxalate raw material that weighs described in step (1) adds water pulping, adds NaOH, alkali addition for theoretical amount 105%～
300%.
3. the method that a kind of purification from thhorium oxalate according to claim 1 prepares the pure thorium tetrafluoride of core, it is characterised in that：
The TBP- kerosene of the employing 2%～10% described in step (2) is to Th (NO3)4Material liquid carries out carrying uranium extraction, and extraction series is 5
Level.
4. the method that a kind of purification from thhorium oxalate according to claim 1 prepares the pure thorium tetrafluoride of core, it is characterised in that：
Employing 25%～40%TBP- sulfonated kerosene counter-current extractions described in step (2), using 10 grades of mixer-settlers as extraction section, 5
Level washing section, using 10 grades of mixer-settlers as back extraction section.
5. the method that a kind of purification from thhorium oxalate according to claim 1 prepares the pure thorium tetrafluoride of core, it is characterised in that：
Add hydrofluoric acid to excessive 2%～15% under agitation described in step (3), filter after ageing, reaction temperature is 50～95 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111024463A (en) * | 2019-10-16 | 2020-04-17 | 核工业北京化工冶金研究院 | Preparation process of multi-element mixed standard solution for nuclear fuel analysis |
| CN112390290A (en) * | 2020-11-20 | 2021-02-23 | 中核北方核燃料元件有限公司 | High-purity UF for thorium-based molten salt reactor4Preparation method |
| CN112593099A (en) * | 2020-11-20 | 2021-04-02 | 中核北方核燃料元件有限公司 | Method for extracting and preparing nuclear pure ThO from rare earth waste residues2Method for producing powder |
| CN112939085A (en) * | 2019-12-10 | 2021-06-11 | 中核北方核燃料元件有限公司 | Method for preparing uranium tetrafluoride through dry fluorination |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417992A (en) * | 2011-03-25 | 2012-04-18 | 中国科学院长春应用化学研究所 | Purification method of thorium |
-
2016
- 2016-11-25 CN CN201611048130.8A patent/CN106629807B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417992A (en) * | 2011-03-25 | 2012-04-18 | 中国科学院长春应用化学研究所 | Purification method of thorium |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111024463A (en) * | 2019-10-16 | 2020-04-17 | 核工业北京化工冶金研究院 | Preparation process of multi-element mixed standard solution for nuclear fuel analysis |
| CN112939085A (en) * | 2019-12-10 | 2021-06-11 | 中核北方核燃料元件有限公司 | Method for preparing uranium tetrafluoride through dry fluorination |
| CN112390290A (en) * | 2020-11-20 | 2021-02-23 | 中核北方核燃料元件有限公司 | High-purity UF for thorium-based molten salt reactor4Preparation method |
| CN112593099A (en) * | 2020-11-20 | 2021-04-02 | 中核北方核燃料元件有限公司 | Method for extracting and preparing nuclear pure ThO from rare earth waste residues2Method for producing powder |
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