CN112390290A - High-purity UF for thorium-based molten salt reactor4Preparation method - Google Patents
High-purity UF for thorium-based molten salt reactor4Preparation method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 150000003839 salts Chemical class 0.000 title claims abstract description 30
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 title claims abstract description 27
- 229910052776 Thorium Inorganic materials 0.000 title claims abstract description 27
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000001035 drying Methods 0.000 claims abstract description 23
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- SANRKQGLYCLAFE-UHFFFAOYSA-H uranium hexafluoride Chemical compound F[U](F)(F)(F)(F)F SANRKQGLYCLAFE-UHFFFAOYSA-H 0.000 claims abstract description 14
- 229910052770 Uranium Inorganic materials 0.000 claims abstract description 12
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims abstract description 12
- MZFRHHGRNOIMLW-UHFFFAOYSA-J uranium(4+);tetrafluoride Chemical compound F[U](F)(F)F MZFRHHGRNOIMLW-UHFFFAOYSA-J 0.000 claims abstract description 12
- 238000003682 fluorination reaction Methods 0.000 claims abstract description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 8
- 230000007062 hydrolysis Effects 0.000 claims abstract description 7
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 16
- 239000003054 catalyst Substances 0.000 claims description 12
- 239000012065 filter cake Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 8
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 7
- 239000000413 hydrolysate Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000012716 precipitator Substances 0.000 claims description 7
- 238000002309 gasification Methods 0.000 claims description 6
- 108010009736 Protein Hydrolysates Proteins 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- KCKICANVXIVOLK-UHFFFAOYSA-L dioxouranium(2+);difluoride Chemical compound [F-].[F-].O=[U+2]=O KCKICANVXIVOLK-UHFFFAOYSA-L 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000010531 catalytic reduction reaction Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000003758 nuclear fuel Substances 0.000 abstract description 9
- 239000000843 powder Substances 0.000 abstract description 5
- 238000011160 research Methods 0.000 abstract description 5
- 238000002474 experimental method Methods 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000009834 vaporization Methods 0.000 abstract description 2
- 230000008016 vaporization Effects 0.000 abstract description 2
- 238000012795 verification Methods 0.000 abstract description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N sulfur dioxide Inorganic materials O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 229910020323 ClF3 Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G43/00—Compounds of uranium
- C01G43/04—Halides of uranium
- C01G43/06—Fluorides
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21C—NUCLEAR REACTORS
- G21C3/00—Reactor fuel elements and their assemblies; Selection of substances for use as reactor fuel elements
- G21C3/42—Selection of substances for use as reactor fuel
- G21C3/44—Fluid or fluent reactor fuel
- G21C3/54—Fused salt, oxide or hydroxide compositions
-
- 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
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Plasma & Fusion (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The invention belongs to the technical field of nuclear fuel circulation, and particularly relates to high-purity UF for a thorium-based molten salt reactor4The preparation method provides qualified high-purity (UF) for the thorium-based molten salt reactor4UF with content not less than 99 percent)4The powder lays a foundation for successfully completing scientific research verification of the thorium-based molten salt reactor in the fourth generation experiment, makes technical reserve for technical popularization of the thorium-based molten salt reactor and closed loop of an industrial chain in the future, and provides technical support for high-purity uranium of nuclear fuel of other projects. The invention develops and develops a process for directly preparing UF by adopting uranium hexafluoride vaporization hydrolysis, catalytic precipitation, drying and calcination and introducing hydrogen fluoride for secondary fluorination4The high-purity uranium tetrafluoride product with the content of more than or equal to 99 percent has the impurity content meeting the special quality requirement of the thorium-based molten salt reactor fuel molten salt, has stable process, simple equipment, easy operation and higher product direct yield, and can completely meet the subsequent thorium-based molten salt reactor fuel supply requirement.
Description
Technical Field
The invention belongs to the technical field of nuclear fuel circulation, and particularly relates to high-purity UF for a thorium-based molten salt reactor4A preparation method.
Background
UF4Preparation technique research originated in the United states of the 30 s in the 20 th century, and the main purpose is to prepare UF6And nuclear pure dense metal uranium, UF4Or can form fused salt with other fluorides and be directly used as fuel of a homogeneous power reactor. UF4The preparation can be generally divided into dry and wet processes.
For the dry process, UF is used6UF is prepared by gas phase or liquid phase reduction4. U.S. developed hot wall and cold wall hydrogen reduction UF6Preparation of UF4The process of (2) has been applied to industrial production. In addition, CCl4 and ammonia reduction UF were also performed6And (5) researching. In addition, France also invented a new method for using ClF3A hydrogen reduction process as a catalyst. However, the dry preparation processes all have the problems of serious corrosion of equipment, great pollution of reducing agents and the like, and industrial batch application has certain difficulty. Domestic research on UF4 dry process began in the last 50 th century. Tianjin university firstly proposes hydrogen reduction UF6The dry method new process is successful in test and is industrially applied.
Natural UF prepared by foreign wet method according to the report of foreign conference literature in 19984The purity of the product reaches 97.5 percent. While the domestic research is relatively early and the process is mature, the domestic preparation of depleted UF4Technical standards show lean UF6The product purity is 97 percent, and the condition of UF (ultra-fine) of domestic thorium-based molten salt reactor at present cannot be met4Requirement for purity, which requires UF4The purity of the powder is more than 99%.
Disclosure of Invention
Aiming at the defects, the invention aims to provide high-purity UF for thorium-based molten salt reactor4The preparation method provides qualified high-purity (UF) for the thorium-based molten salt reactor4UF with content not less than 99 percent)4The powder lays a foundation for successfully completing scientific research verification of the thorium-based molten salt reactor in the fourth generation experiment, makes technical reserve for technical popularization of the thorium-based molten salt reactor and closed loop of an industrial chain in the future, and provides technical support for high-purity uranium of nuclear fuel of other projects.
The technical scheme of the invention is as follows:
high-purity UF for thorium-based molten salt reactor4The preparation method comprises the steps of firstly, heating and gasifying uranium hexafluoride, and then introducing water for hydrolysis to obtain hydrolysate containing uranyl fluoride and hydrofluoric acid;
step two, adding catalyst hydrochloric acid and copper sulfate and precipitator hydrofluoric acid into the hydrolysate, and introducing SO at high temperature2Carrying out catalytic reduction reaction on the gas to obtain a uranium tetrafluoride filter cake;
step three, UF4Putting the filter cake into a drying fluorination furnace, introducing nitrogen gas for drying and dehydration, then introducing HF for fluorination again at high temperature to prepare high-purity uranium tetrafluoride, and finally discharging the uranium tetrafluoride from the furnace at a reduced temperature under the protection of nitrogen gas;
in the first step, in the uranium hexafluoride gasification process, the gasification temperature is 80-150 ℃;
in the hydrolysis process of uranium hexafluoride, the adding proportion of water is 5-13L/KgU.
And in the first step, the concentration of uranium in the hydrolysate is 80-200 Ug/L.
Adding a catalyst hydrochloric acid in the second step, and controlling the concentration of the hydrochloric acid to be 1.5-3 mol/L;
adding solid copper sulfate serving as a catalyst in the second step, and controlling the concentration of Cu2+ in the solution to be 3.0-8 g/L;
and adding a precipitator hydrofluoric acid in the second step, and controlling the concentration of the hydrofluoric acid in the solution to be 5-15 g/L.
And in the high-temperature precipitation process in the second step, the temperature is increased to 70-95 ℃.
Introducing a reducing agent SO in the step two2Gas, SO2The gas flow is 0.1-1.0 m3The introduction time is 2-6 hours;
detecting that the uranium content in the solution is less than 0.5g/L, determining that the reaction is finished, and filtering to obtain UF4 crystal precipitate and precipitate mother.
Step three is UF4Putting the crystal filter cake into a drying reaction furnace, wherein the purity of the introduced nitrogen is more than or equal to 99.8 percent, and the flow rate of the nitrogen is 0.2-1.0m3/h。
And in the third drying and dehydrating process, the drying and dehydrating temperature is as follows: drying and dehydrating at 250-350 ℃ for 2-4 hours.
Introducing HF gas at high temperature of 500-700 ℃ and introducing hydrogen fluoride gas at flow rate of 0.2-1.0m3And h, introducing HF for 60-120 min.
The invention has the beneficial effects that:
the invention develops and develops a process for directly preparing UF by adopting uranium hexafluoride vaporization hydrolysis, catalytic precipitation, drying and calcination and introducing hydrogen fluoride for secondary fluorination4The high-purity uranium tetrafluoride product with the content of more than or equal to 99 percent has the impurity content meeting the special quality requirement of the thorium-based molten salt reactor fuel molten salt, has stable process, simple equipment, easy operation and higher product direct yield, and can completely meet the subsequent thorium-based molten salt reactor fuel supply requirement.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides high-purity UF for a thorium-based molten salt reactor4The preparation method comprises the following specific steps:
step one, heating and gasifying uranium hexafluoride, introducing water, and hydrolyzing to obtain hydrolysate containing uranyl fluoride and hydrofluoric acid;
step two, adding catalyst hydrochloric acid and copper sulfate and precipitator hydrofluoric acid into the hydrolysate, and introducing SO at high temperature2Carrying out catalytic reduction reaction on the gas to obtain a uranium tetrafluoride filter cake;
step three, UF4Putting the filter cake into a dry fluorination furnace, introducing nitrogen gas for drying and dehydration, then introducing HF for secondary fluorination at high temperature to prepare high-purity tetrafluorideAnd (4) uranium is finally discharged from the furnace under the protection of nitrogen.
In the first step, in the uranium hexafluoride gasification process, the gasification temperature is 80-150 ℃;
in the hydrolysis process of the uranium hexafluoride in the first step, the adding proportion of water is 5-13L/KgU.
In the hydrolysate in the first step, the uranium concentration is 80-200 Ug/L;
adding a catalyst hydrochloric acid in the second step, and controlling the concentration of the hydrochloric acid to be 1.5-3 mol/L;
adding solid copper sulfate serving as a catalyst in the second step, and controlling the concentration of Cu2+ in the solution to be 3.0-8 g/L;
adding a precipitator hydrofluoric acid in the second step, and controlling the concentration of the hydrofluoric acid in the solution to be 5-15 g/L;
in the second step, in the high-temperature precipitation process, the temperature is increased to 70-95 ℃;
introducing a reducing agent SO in the step two2Gas, SO2The gas flow is 0.1-1.0 m3The introduction time is 2-6 hours;
detecting that the uranium content in the solution is less than 0.5g/L, determining that the reaction is finished, and filtering to obtain UF4 crystal precipitate and precipitate mother.
Step three is UF4Putting the crystal filter cake into a drying reaction furnace, wherein the purity of the introduced nitrogen is more than or equal to 99.8 percent, and the flow rate of the nitrogen is 0.2-1.0m3/h；
And in the third drying and dehydrating process, the drying and dehydrating temperature is as follows: drying and dehydrating at 250-350 ℃ for 2-4 hours;
and step three, introducing HF gas at a high temperature of 500-700 ℃, introducing hydrogen fluoride gas flow: 0.2-1.0m3And h, introducing HF for 60-120 min.
Example 1
The treated object is high-purity low-concentration UF of nuclear fuel in thorium-based molten salt experiment reactor of Chinese academy of sciences4In the powder production process, the uranium hexafluoride is vaporized and then undergoes hydrolysis reaction with water to prepare hydrolysate, then hydrochloric acid and copper sulfate are added into the hydrolysate, sulfur dioxide is introduced to prepare a uranium tetrafluoride filter cake, and the uranium tetrafluoride filter cake is put into a dry fluorination furnace to be communicated with the furnaceFirstly, heating and dehydrating, and then introducing HF gas to perform fluorination reaction after dehydration is finished, so as to prepare the high-purity uranium tetrafluoride.
The first step is as follows: and (3) putting the low-concentration uranium hexafluoride container into an autoclave for heating, heating to 110 ℃, and reacting the gasified uranium hexafluoride with deionized water through a guide pipe to produce uranyl fluoride and hydrofluoric acid.
The second step is that: adjusting the uranium concentration of the hydrolysate prepared in the first step to 120 Ug/L; then adding catalyst hydrochloric acid, and controlling the concentration of the hydrochloric acid in the solution at 3 mol/L; adding a precipitator hydrofluoric acid, and controlling the concentration of the hydrofluoric acid in the solution to be 15 g/L; then adding catalyst solid copper sulfate, and controlling the concentration of Cu2+ in the solution to be 4.0 g/L; then evenly stirring the solution, heating to 80 ℃, and introducing a reducing agent SO2Gas, SO2The gas introduction amount is 1.0m3H; and after the reaction is carried out for 5 hours, detecting that the uranium content in the solution is less than 0.5g/L, determining that the reaction is finished, and filtering to obtain UF4 crystal precipitate and a precipitate mother.
The third step: mixing UF4Putting the crystal filter cake into a drying reaction furnace, introducing high-purity nitrogen gas, heating to 300 ℃, drying and dehydrating for 3 hours, then heating to 500 ℃, introducing hydrogen fluoride gas, introducing high-purity nitrogen gas in 100min, cooling and discharging, wherein the purity of the prepared UF4 powder is 99.2%.
In the drawings of the disclosed embodiments of the invention, only methods related to the disclosed embodiments are referred to, other methods can refer to common design, and the same embodiment and different embodiments of the invention can be combined with each other without conflict;
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (8)
1. High-purity UF for thorium-based molten salt reactor4The preparation method comprises the steps of firstly, heating and gasifying uranium hexafluoride, and then introducing water for hydrolysis to obtain hydrolysate containing uranyl fluoride and hydrofluoric acid;
step two, adding catalyst hydrochloric acid and copper sulfate and precipitator hydrofluoric acid into the hydrolysate, and introducing SO at high temperature2Carrying out catalytic reduction reaction on the gas to obtain a uranium tetrafluoride filter cake;
step three, UF4Putting the filter cake into a drying fluorination furnace, introducing nitrogen gas for drying and dehydration, then introducing HF for fluorination again at high temperature to prepare high-purity uranium tetrafluoride, and finally discharging the uranium tetrafluoride from the furnace at a reduced temperature under the protection of nitrogen gas;
the method is characterized in that: in the first step, in the uranium hexafluoride gasification process, the gasification temperature is 80-150 ℃;
in the hydrolysis process of uranium hexafluoride, the adding proportion of water is 5-13L/KgU.
2. The high-purity UF for thorium-based molten salt reactor of claim 14The preparation method is characterized by comprising the following steps:
and in the first step, the concentration of uranium in the hydrolysate is 80-200 Ug/L.
3. The high-purity UF for thorium-based molten salt reactor of claim 14The preparation method is characterized by comprising the following steps:
adding a catalyst hydrochloric acid in the second step, and controlling the concentration of the hydrochloric acid to be 1.5-3 mol/L;
adding solid copper sulfate serving as a catalyst in the second step, and controlling the concentration of Cu2+ in the solution to be 3.0-8 g/L;
and adding a precipitator hydrofluoric acid in the second step, and controlling the concentration of the hydrofluoric acid in the solution to be 5-15 g/L.
4. High-purity UF for thorium-based molten salt reactor as claimed in claim 34The preparation method is characterized by comprising the following steps: and in the high-temperature precipitation process in the second step, the temperature is increased to 70-95 ℃.
5. The high-purity UF for thorium-based molten salt reactor of claim 44The preparation method is characterized by comprising the following steps:
introducing a reducing agent SO in the step two2Gas, SO2The gas flow rate is 0.1-1.0m3The introduction time is 2-6 hours;
detecting that the uranium content in the solution is less than 0.5g/L, determining that the reaction is finished, and filtering to obtain UF4 crystal precipitate and precipitate mother.
6. The high-purity UF for thorium-based molten salt reactor of claim 14The preparation method is characterized by comprising the following steps:
step three is UF4Putting the crystal filter cake into a drying reaction furnace, wherein the purity of the introduced nitrogen is more than or equal to 99.8 percent, and the flow rate of the nitrogen is 0.2-1.0m3/h。
7. The high-purity UF for thorium-based molten salt reactor of claim 64The preparation method is characterized by comprising the following steps:
and in the third drying and dehydrating process, the drying and dehydrating temperature is as follows: drying and dehydrating at 250-350 ℃ for 2-4 hours.
8. The high-purity UF for thorium-based molten salt reactor of claim 74The preparation method is characterized by comprising the following steps:
introducing HF gas at high temperature of 500-700 ℃ and introducing hydrogen fluoride gas at flow rate of 0.2-1.0m3And h, introducing HF for 60-120 min.
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2020
- 2020-11-20 CN CN202011314012.3A patent/CN112390290A/en active Pending
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|---|---|---|---|---|
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