CN112939085A - Method for preparing uranium tetrafluoride through dry fluorination - Google Patents
Method for preparing uranium tetrafluoride through dry fluorination Download PDFInfo
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- CN112939085A CN112939085A CN201911260357.2A CN201911260357A CN112939085A CN 112939085 A CN112939085 A CN 112939085A CN 201911260357 A CN201911260357 A CN 201911260357A CN 112939085 A CN112939085 A CN 112939085A
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- uranium
- tetrafluoride
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- uranium tetrafluoride
- calcining
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- MZFRHHGRNOIMLW-UHFFFAOYSA-J uranium(4+);tetrafluoride Chemical compound F[U](F)(F)F MZFRHHGRNOIMLW-UHFFFAOYSA-J 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000003682 fluorination reaction Methods 0.000 title claims abstract description 27
- 238000001354 calcination Methods 0.000 claims abstract description 31
- 239000012025 fluorinating agent Substances 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 229910052770 Uranium Inorganic materials 0.000 claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 16
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 150000003671 uranium compounds Chemical class 0.000 claims abstract description 15
- FSVQVLHGIXXZGC-UHFFFAOYSA-N [Si].[U] Chemical compound [Si].[U] FSVQVLHGIXXZGC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011261 inert gas Substances 0.000 claims abstract description 10
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 5
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims abstract 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 229910000442 triuranium octoxide Inorganic materials 0.000 claims description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 9
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 235000012239 silicon dioxide Nutrition 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- -1 uranium peroxide Chemical class 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 230000036632 reaction speed Effects 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- JCMLRUNDSXARRW-UHFFFAOYSA-N trioxouranium Chemical compound O=[U](=O)=O JCMLRUNDSXARRW-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 5
- WZECUPJJEIXUKY-UHFFFAOYSA-N [O-2].[O-2].[O-2].[U+6] Chemical compound [O-2].[O-2].[O-2].[U+6] WZECUPJJEIXUKY-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- DSAWYFXJVXQFIV-UHFFFAOYSA-N aminoazanium;fluoride Chemical compound [F-].[NH3+]N DSAWYFXJVXQFIV-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 3
- ZAASRHQPRFFWCS-UHFFFAOYSA-P diazanium;oxygen(2-);uranium Chemical compound [NH4+].[NH4+].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[U].[U] ZAASRHQPRFFWCS-UHFFFAOYSA-P 0.000 claims description 3
- 238000004093 laser heating Methods 0.000 claims description 3
- OOAWCECZEHPMBX-UHFFFAOYSA-N oxygen(2-);uranium(4+) Chemical compound [O-2].[O-2].[U+4] OOAWCECZEHPMBX-UHFFFAOYSA-N 0.000 claims description 3
- FCTBKIHDJGHPPO-UHFFFAOYSA-N uranium dioxide Inorganic materials O=[U]=O FCTBKIHDJGHPPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910000439 uranium oxide Inorganic materials 0.000 claims description 3
- 229910002007 uranyl nitrate Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000000446 fuel Substances 0.000 abstract description 4
- 239000002351 wastewater Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000007983 Tris buffer Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to a treatment method, and particularly relates to a method for preparing uranium tetrafluoride through dry fluorination. It comprises the following steps: firstly, calcining metallic uranium, uranium compound, uranium-silicon mixture and the like into oxides at high temperature; secondly, uniformly mixing the calcined oxide with fluorinating agents such as ammonium fluoride and ammonium bifluoride according to a certain proportion; and thirdly, putting the mixed material into a muffle furnace or a converter with a heating function, introducing inert gases or reducing gases such as nitrogen, hydrogen, ammonia and the like, electrifying and heating until oxides are completely converted into uranium tetrafluoride powder. The invention has the following remarkable effects: avoids the generation of uranium-containing wastewater and reduces the cost. The method can be applied to the fields of nuclear chemical industry and fuel element manufacturing, and the recovery processing of unqualified uranium silicon mixtures in the manufacturing process of fuel elements and the preparation of uranium tetrafluoride from raw materials of uranium, uranium compounds, uranium silicon mixtures and the like.
Description
Technical Field
The invention belongs to a treatment method, and particularly relates to a method for preparing uranium tetrafluoride through dry fluorination.
Background
The method is characterized in that the uranium tetrafluoride powder is an important intermediate product in the manufacturing process of nuclear fuel elements, a wet production process is mostly adopted when the uranium tetrafluoride powder is prepared by taking metal uranium, uranium compounds, uranium-silicon mixtures and the like as raw materials, the traditional wet preparation process comprises the working procedures of dissolution (hydrolysis), extraction, catalytic precipitation, drying and calcination, wastewater treatment and the like, and the wet preparation process has the defects of long process flow, large reagent dosage, large production amount of wastewater and waste residues, high conversion cost and the like.
Disclosure of Invention
Compared with the traditional wet reaction, the method can shorten the preparation process of uranium tetrafluoride, avoid the generation of a large amount of uranium-containing wastewater in the preparation process, can convert various raw materials to prepare uranium tetrafluoride, can reduce the extraction and purification processes for preparing uranium tetrafluoride from silicon-containing raw materials, greatly shorten the process flow, reduce the cost, and can be used for recycling silicon-containing waste materials in the component manufacturing process, so the method has important significance for preparing uranium tetrafluoride and recycling the uranium-containing waste materials.
The invention is realized by the following steps: a method for preparing uranium tetrafluoride by dry fluorination comprises the following steps:
firstly, calcining metallic uranium, uranium compound, uranium-silicon mixture and the like into oxides at high temperature;
secondly, uniformly mixing the calcined oxide with fluorinating agents such as ammonium fluoride and ammonium bifluoride according to a certain proportion;
and thirdly, putting the mixed material into a muffle furnace or a converter with a heating function, introducing inert gases or reducing gases such as nitrogen, hydrogen, ammonia and the like, electrifying and heating until oxides are completely converted into uranium tetrafluoride powder.
The method for preparing uranium tetrafluoride through dry fluorination as described above, wherein the raw materials of uranium, uranium compounds, uranium-silicon mixtures and the like are calcined and oxidized to obtain oxides; the uranium compound can be triuranium octoxide, uranium dioxide, uranium trioxide, ammonium diuranate, uranium peroxide, uranyl tricarbonate, uranyl nitrate, and other compounds which can be decomposed into oxides.
According to the method for preparing uranium tetrafluoride through dry fluorination, the oxide obtained by calcining and oxidizing the raw material and the fluorinating agent are uniformly mixed according to a certain proportion, and then the mixture is calcined at a high temperature under the protection of inert gas or reducing gas to produce uranium tetrafluoride powder.
The method for preparing uranium tetrafluoride through dry fluorination as described above, wherein the fluorinating agent comprises one or more components which can be decomposed into reducing gas and hydrogen fluoride at high temperature, such as ammonium fluoride, ammonium bifluoride, hydrazine fluoride and the like.
The method for preparing uranium tetrafluoride through dry fluorination is characterized in that the amount of the fluorinating agent is more than 1.2 times of the sum of the theoretical amounts of oxides completely converted into uranium tetrafluoride and silicon dioxide completely converted into fluosilicic acid.
The method for preparing uranium tetrafluoride through dry fluorination as described above, wherein the inert gas may be nitrogen, argon, or other gas that does not react with uranium oxide, uranium tetrafluoride, or silicon dioxide, and the reducing gas includes ammonia, hydrogen fluoride gas, or other gases.
The method for preparing uranium tetrafluoride through dry fluorination as described above, wherein the calcination mode is heat conduction heating, microwave heating, laser heating, etc.; the selection equipment can be a muffle furnace, a converter and the like; the material of the device should be the material which is resistant to hydrogen fluoride corrosion and high temperature such as NS331, NCu30, etc.
The method for preparing uranium tetrafluoride through dry fluorination as described above, wherein the calcining oxidation reaction temperature T1 of the raw material is within the range of 400 ℃ to T1 to 1000 ℃, and the reaction time is until the raw material is completely oxidized into triuranium octoxide powder.
The method for preparing uranium tetrafluoride through dry fluorination is characterized in that the reaction temperature T2 when the oxide and the fluorinating agent are calcined is within the range of 400-1000 ℃ and T2-1000 ℃, and the reaction time T is more than 1 h.
The method for preparing uranium tetrafluoride through dry fluorination is described above, wherein the reaction speed is slower when the oxide and the fluorinating agent are calcined with larger particle size, and the reaction speed is faster when the particle size is smaller, so that the particle size of the raw material can be properly reduced in the preparation process.
The invention has the following remarkable effects: the method can realize that the uranium tetrafluoride powder is obtained by taking metal uranium, a uranium compound, a uranium-silicon mixture or a mixture of the metal uranium, the uranium compound and the uranium-silicon as raw materials through raw material oxidation, fluorinating agent mixing and calcination reduction, greatly shortens the preparation flow compared with the traditional wet process, avoids the generation of uranium-containing wastewater, and reduces the cost. The method can be applied to the fields of nuclear chemical industry and fuel element manufacturing, and the recovery processing of unqualified uranium silicon mixtures in the manufacturing process of fuel elements and the preparation of uranium tetrafluoride from raw materials of uranium, uranium compounds, uranium silicon mixtures and the like.
Detailed Description
The invention provides a method for preparing uranium tetrafluoride by dry fluorination. Firstly, calcining metallic uranium, uranium compound, uranium-silicon mixture and the like into oxides at high temperature; secondly, uniformly mixing the calcined oxide with fluorinating agents such as ammonium fluoride and ammonium bifluoride according to a certain proportion; and thirdly, putting the mixed material into a muffle furnace or a converter with a heating function, introducing inert gases or reducing gases such as nitrogen, hydrogen, ammonia and the like, electrifying and heating until oxides are completely converted into uranium tetrafluoride powder.
Calcining and oxidizing the raw materials such as the metal uranium, the uranium compound, the uranium-silicon mixture and the like to obtain an oxide; the uranium compound can be triuranium octoxide, uranium dioxide, uranium trioxide, ammonium diuranate, uranium peroxide, uranyl tricarbonate, uranyl nitrate, and other compounds which can be decomposed into oxides.
The method comprises the steps of uniformly mixing an oxide obtained by calcining and oxidizing raw materials with a fluorinating agent according to a certain proportion, and then calcining at a high temperature under the protection of inert gas or reducing gas to produce uranium tetrafluoride powder.
The fluorinating agent comprises one or more components which can be decomposed into reducing gas and hydrogen fluoride at high temperature such as ammonium fluoride, ammonium bifluoride, hydrazine fluoride and the like;
the amount of the fluorinating agent is more than 1.2 times of the sum of theoretical amounts of oxides completely converted into uranium tetrafluoride and silicon dioxide completely converted into fluosilicic acid.
The inert gas can be nitrogen, argon and other gases which do not react with uranium oxide, uranium tetrafluoride and silicon dioxide, and the reducing gas comprises ammonia gas, hydrogen fluoride gas and the like.
The calcining mode is heat conduction heating, microwave heating, laser heating and the like; the selection equipment can be a muffle furnace, a converter and the like; the material of the device should be the material which is resistant to hydrogen fluoride corrosion and high temperature such as NS331, NCu30, etc.
The calcining oxidation reaction temperature T1 range of the raw materials is between 400 ℃ and T1 and 1000 ℃, and the reaction time is until the raw materials are completely oxidized into triuranium octoxide powder.
The reaction temperature T2 range of the oxide and the fluorinating agent during calcination is between 400 ℃ and T2 and 1000 ℃, and the reaction time T is more than 1 h.
When the oxide and the fluorinating agent are calcined, the reaction speed is slower when the particle size is larger, the reaction speed is higher when the particle size is smaller, and the particle size of the original material can be properly reduced in the preparation process.
Several specific examples are given below
Example 1: preparation of uranium tetrafluoride by dry fluorination of uranium trisilicon powder
300g of uranium trisilicon second powder is weighed, evenly laid in a new first material boat and then put into a muffle furnace for calcination and oxidation, the muffle furnace is made of a new first material, the calcination time is 2 hours, the calcination temperature is 700 ℃, and the compressed air flow is 0.2m3And h, obtaining triuranium octoxide and silicon dioxide powder after the calcination is finished. After the materials are cooled, weighing ammonium fluoride (the theoretical dosage is 150 percent), triuranium octoxide and silicon dioxide, uniformly mixing the ammonium fluoride, the triuranium octoxide and the silicon dioxide in a new material boat, putting the mixture into a muffle furnace for calcination at the calcination temperature of 500 ℃ for 4 hours, introducing a small amount of nitrogen for protection in the calcination process, wherein the nitrogen flow is 0.2m3And h, finally obtaining the uranium tetrafluoride powder.
Example 2: preparation of uranium tetrafluoride by dry fluorination of triuranium octoxide powder
300g of tris octaoxide are weighedUranium octoxide powder and ammonium bifluoride, the ammonium bifluoride quantity is 150% of theoretical quantity, tile in No. one new material boat after mixing triuranium octoxide powder and ammonium bifluoride evenly, put into the muffle furnace and calcine afterwards, the muffle furnace is No. one new material, calcination temperature 500 ℃, calcination time 4h, let in a small amount of hydrogen in the calcination process and protect, the hydrogen flow is 0.2m3And h, finally obtaining the uranium tetrafluoride powder.
Claims (10)
1. The method for preparing uranium tetrafluoride through dry fluorination is characterized by comprising the following steps:
firstly, calcining metallic uranium, uranium compound, uranium-silicon mixture and the like into oxides at high temperature;
secondly, uniformly mixing the calcined oxide with fluorinating agents such as ammonium fluoride and ammonium bifluoride according to a certain proportion;
and thirdly, putting the mixed material into a muffle furnace or a converter with a heating function, introducing inert gases or reducing gases such as nitrogen, hydrogen, ammonia and the like, electrifying and heating until oxides are completely converted into uranium tetrafluoride powder.
2. The method for preparing uranium tetrafluoride through dry fluorination according to claim 1, wherein: calcining and oxidizing the raw materials such as the metal uranium, the uranium compound, the uranium-silicon mixture and the like to obtain an oxide; the uranium compound can be triuranium octoxide, uranium dioxide, uranium trioxide, ammonium diuranate, uranium peroxide, uranyl tricarbonate, uranyl nitrate, and other compounds which can be decomposed into oxides.
3. The method for preparing uranium tetrafluoride through dry fluorination according to claim 2, wherein: the method comprises the steps of uniformly mixing an oxide obtained by calcining and oxidizing raw materials with a fluorinating agent according to a certain proportion, and then calcining at a high temperature under the protection of inert gas or reducing gas to produce uranium tetrafluoride powder.
4. The method for preparing uranium tetrafluoride through dry fluorination according to claim 3, wherein: the fluorinating agent comprises one or more components which can be decomposed into reducing gas and hydrogen fluoride at high temperature such as ammonium fluoride, ammonium bifluoride, hydrazine fluoride and the like.
5. The method for preparing uranium tetrafluoride through dry fluorination according to claim 4, wherein: the amount of the fluorinating agent is more than 1.2 times of the sum of theoretical amounts of oxides completely converted into uranium tetrafluoride and silicon dioxide completely converted into fluosilicic acid.
6. The method for preparing uranium tetrafluoride through dry fluorination according to claim 5, wherein: the inert gas can be nitrogen, argon and other gases which do not react with uranium oxide, uranium tetrafluoride and silicon dioxide, and the reducing gas comprises ammonia gas, hydrogen fluoride gas and the like.
7. The method for preparing uranium tetrafluoride through dry fluorination according to claim 6, wherein: the calcining mode is heat conduction heating, microwave heating, laser heating and the like; the selection equipment can be a muffle furnace, a converter and the like; the material of the device should be the material which is resistant to hydrogen fluoride corrosion and high temperature such as NS331, NCu30, etc.
8. The method for preparing uranium tetrafluoride through dry fluorination according to claim 7, wherein: the calcining oxidation reaction temperature T1 range of the raw materials is between 400 ℃ and T1 and 1000 ℃, and the reaction time is until the raw materials are completely oxidized into triuranium octoxide powder.
9. The method for preparing uranium tetrafluoride through dry fluorination according to claim 8, wherein: the reaction temperature T2 range of the oxide and the fluorinating agent during calcination is between 400 ℃ and T2 and 1000 ℃, and the reaction time T is more than 1 h.
10. The method for preparing uranium tetrafluoride through dry fluorination according to claim 9, wherein: when the oxide and the fluorinating agent are calcined, the reaction speed is slower when the particle size is larger, the reaction speed is higher when the particle size is smaller, and the particle size of the original material can be properly reduced in the preparation process.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911260357.2A CN112939085A (en) | 2019-12-10 | 2019-12-10 | Method for preparing uranium tetrafluoride through dry fluorination |
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| CN201911260357.2A CN112939085A (en) | 2019-12-10 | 2019-12-10 | Method for preparing uranium tetrafluoride through dry fluorination |
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Cited By (2)
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| CN111304674A (en) * | 2020-03-25 | 2020-06-19 | 哈尔滨工程大学 | Preparation of UO2Method (2) |
| CN113620346A (en) * | 2021-07-20 | 2021-11-09 | 哈尔滨工程大学 | High-temperature fluorinated U3O8Or UO3Method for preparing uranium tetrafluoride |
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Cited By (2)
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| CN113620346A (en) * | 2021-07-20 | 2021-11-09 | 哈尔滨工程大学 | High-temperature fluorinated U3O8Or UO3Method for preparing uranium tetrafluoride |
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Application publication date: 20210611 |