CN111394741B - Fluorinated U3O8Or UO3Method for dissolving in chloride molten salt - Google Patents

Fluorinated U3O8Or UO3Method for dissolving in chloride molten salt Download PDF

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CN111394741B
CN111394741B CN202010218739.5A CN202010218739A CN111394741B CN 111394741 B CN111394741 B CN 111394741B CN 202010218739 A CN202010218739 A CN 202010218739A CN 111394741 B CN111394741 B CN 111394741B
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韩伟
纪文静
李梅
孟洋洋
王伟
汪文娟
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Harbin Engineering University
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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Abstract

The invention provides a fluorinated U3O8Or UO3Dissolving in molten chloride salt, mixing uranium oxide with NH4HF2Mixing thoroughly, grinding, and placing into crucible, wherein U is3O8And NH4HF2The mass ratio of (A) to (B) is 1: 1-1: 12.3; UO3And NH4HF2The mass ratio of the components is 1: 1-1: 12.0, and then the mixture is placed at the temperature of 350-600 ℃ for full reaction for 2-6 h. After the reaction is finished, the product is characterized by an X-ray diffraction instrument to be UO2F2And calculating to obtain a fluorination rate as high as 97.5%, and then calculating to obtain a UO of about 0.7-2% (mass ratio to molten salt)2F2Adding into molten chloride molten salt, wherein the temperature range of the chloride molten salt is as follows: at 400-700 ℃ and UO2F2After dissolution, the molten salt is changed from colorless transparency to yellow transparency; the invention provides a fluorinated U3O8Or UO3The method for dissolving the uranium oxide in the chloride molten salt has the advantages that the fluorination rate is high, the problem of dissolving the uranium oxide in the chloride molten salt can be solved, the process is carried out in the air, and the whole process is simple to operate.

Description

Fluorinated U3O8Or UO3Method for dissolving in chloride molten salt
Technical Field
Invention of the inventionRelates to a fluorinated U3O8Or UO3And the method of dissolving in chloride fused salt can be applied to the technical field of spent fuel dry post-treatment.
Background
In order to cope with the shortage of fossil fuels and ensure energy safety, nuclear power is favored due to cleanliness and high energy density in the 20 th century and the 60-70 th era. In the power generation process of a nuclear power plant, when the fission of nuclear fuel cannot maintain a certain power, the replaced unburnt nuclear fuel is called spent fuel (also called irradiated nuclear fuel). The spent fuel contains a large amount of about 95% U, 1% Pu, 0.1% minor actinides MA (Np, Am and Cm) and 3% long-life fission products (LLFP), which constitute a great potential hazard to the earth's biological and human environment. Therefore, the problem of processing and disposing of spent fuel has become a key problem affecting the sustainable development of nuclear power.
The spent fuel dry method post-treatment has the advantages of radiation resistance, low critical risk, less radioactive waste and the like, is suitable for treating spent fuel with high fuel consumption and short cooling period, and hopefully meets the separation requirement of the spent fuel or transmutation target in the advanced nuclear fuel circulation. The Korean Atomic Energy Research Institute (KAERI) proposed a dry-process spent fuel reprocessing process, also known as the ER process, at the end of the 90 s of the 20 th century. The specific process is to carry out oxidation calcination on a spent fuel element which is cut into 3-10 cm long in oxygen or air atmosphere at the temperature of about 500 ℃ to realize separation of pellets and cladding, and to separate UO2Is converted into U3O8And UO3Powder particles.
In order to enable the uranium oxide to be dissolved in molten salt for electrolytic purification. Patent CN108364703A discloses passing NH4Cl chlorination UO2Make UO2Dissolved in LiCl-KCl molten salt. Patent CN108034965A discloses the treatment of cancer by AlCl3Chlorinated UO2Make UO2Dissolved in LiCl-KCl molten salt. Patent CN109913901A discloses a method for introducing CCl under the protection of argon4Gas chlorination U3O8Reaction product UCl4Dissolved in LiCl-KCl molten salt.
Disclosure of Invention
The invention provides a fluorinated U3O8Or UO3And dissolving in chloride molten salt by dissolving uranium oxide (U)3O8And UO3One of) and NH4HF2After reaction at elevated temperature, the reaction product UO is reacted2F2Dissolving in chloride molten salt.
The invention is realized by the following steps:
fluorinated U3O8Or UO3The method for dissolving the fused salt in chloride is characterized by comprising the following steps:
will U3O8Or UO3Fully mixing with fluorinating agent powder, grinding, placing into a crucible for fluorination reaction, and obtaining a product UO after the reaction is finished2F2And UO2F2Added to molten chloride molten salt and found to be completely dissolved, the molten salt changed from colorless to yellow and transparent.
The fluorinating agent is NH4HF2；
The U is3O8And NH4HF2The mass ratio of (A) to (B) is 1: 1-1: 12.3; UO3And NH4HF2The mass ratio of (A) to (B) is 1: 1-1: 12.0;
the temperature of the fluorination reaction is 350-600 ℃;
the fluorination reaction time is 2-6 hours;
the chloride molten salt is as follows: one or more molten salts of LiCl-KCl, LiCl-CsCl and NaCl-CsCl are mixed;
the mol ratio of LiCl to KCl in the chloride fused salt LiCl-KCl is 74:51, the mol ratio of LiCl to CsCl in the chloride fused salt LiCl-CsCl is 29:21, and the mol ratio of NaCl to CsCl in the chloride fused salt NaCl-CsCl is 7: 13;
heating chloride fused salt LiCl-KCl to 400-600 ℃, heating chloride fused salt LiCl-CsCl to 400-600 ℃, and heating chloride fused salt NaCl-CsCl to 550-700 ℃;
the UO2F2Quality of fused salt with chlorideThe ratio is 0.7 to 2%.
The principle is as follows:
U3O8+6NH4HF2+1/2O2(g)＝3UO2F2+6NH4F+3H2O(g) (1)
U3O8+6NH4HF2+1/2O2(g)＝3UO2F2+6NH3(g)+6HF(g)+3H2O(g) (2)
3UO3+6NH4HF2＝3UO2F2+6NH4F+3H2O(g) (3)
3UO3+6NH4HF2＝3UO2F2+6NH3(g)+6HF(g)+3H2O(g) (4)
the invention has the beneficial effects that:
the invention provides a fluorinated U3O8Or UO3The whole operation can be carried out under the atmospheric condition without adopting strong corrosive gas. The selected fluorination reagent is excellent, the fluorination rate is high, and the problem that uranium oxide is difficult to dissolve in molten salt is solved.
Drawings
FIG. 1 shows that UO with the mass ratio of 0.7% is added into LiCl-KCl eutectic molten salt with the temperature of 500 DEG C2F2Color of molten salt;
FIG. 2 shows uranium oxide and NH at different temperatures4HF2Gibbs free energy diagram of the reaction;
FIG. 3 is U at 773K3O8And NH4HF2(wherein U is3O8And NH4HF2In a mass ratio of 1:8.12) XRD of the product after reaction;
FIG. 4 is a UO at 773K3And NH4HF2(wherein UO3And NH4HF2In a mass ratio of 1:7.13) XRD of the product after reaction.
Detailed Description
The invention is described in detail below with reference to the accompanying drawings and specific embodiments.
The technical scheme adopted by the invention for realizing the purpose is as follows:
(1) the fluorination method comprises the following steps: uranium oxide (U)3O8And UO3One of) and NH4HF2Mixing well, grinding, and filling into crucible (wherein U is3O8And NH4HF2The mass ratio of (A) to (B) is 1: 1-1: 12.3; UO3And NH4HF2The mass ratio of (1: 1) - (1: 12.0), and then fully reacting for 2-6 h at the temperature of 350-600 ℃.
(2) Characterization of the product after fluorination: XRD test analysis of the collected product proves that the fluorinated product is UO2F2。
(3) Calculation of fluorination rate: weighing the collected product and calculating the fluorination rate (η), wherein the fluorination rate (η) is defined as:
Figure BDA0002425322790000031
wherein m is1Is a practically obtained UO2F2Mass of (c), m2For theoretically obtained UO2F2The quality of (c).
(4)UO2F2Dissolving: loading chloride molten salt into a crucible, then melting at 350-700 ℃, and adding UO after the molten salt is completely melted2F2And after 2-3 minutes, the molten salt is dissolved, and the molten salt is changed from colorless transparency to yellow transparency.
All of the above steps can be carried out under atmospheric conditions.
Example 1:
fluorination: weighing U3O8Mass of (3) is 1.00g, NH4HF2Has a mass of 8.12g, is3O8And NH4HF2Fully mixing, grinding, filling into a crucible, covering the crucible with a cover, placing into a 500 ℃ well type furnace, and reacting for 3 h. After the reaction was completed, the product was collected and weighed to obtain 1.01gUO2F2Theoretically calculate UO2F2The mass of (2) was 1.10g, and the fluorination rate (. eta.) was calculated to be 92.1%.
Dissolving: KCl and LiCl were weighed to 22.50g and 19.00g, mixed well and uniformly in a crucible, placed in a 500 ℃ shaft furnace, and after the salt had melted, 0.30gUO was added2F2. After 2 minutes, UO2F2The molten salt is dissolved, and the molten salt is changed from colorless transparency to yellow transparency.
Example 2:
fluorination: weighing U3O8Mass of (3) is 1.00g, NH4HF2Has a mass of 8.12g, is3O8And NH4HF2Fully mixing, grinding, filling into a crucible, covering the crucible with a cover, placing into a 400 ℃ well type furnace, and reacting for 3 h. After the reaction was completed, the product was collected and weighed to obtain 1.07gUO2F2Theoretically calculate UO2F2The mass of (2) was 1.10g, and the fluorination rate (. eta.) was found to be 97.5% by calculation.
Dissolving: KCl and LiCl were weighed to 22.50g and 19.00g, mixed well and uniformly in a crucible, placed in a 500 ℃ shaft furnace, and after the salt had melted, 0.30gUO was added2F2. After 2 minutes, UO2F2The molten salt is dissolved, and the molten salt is changed from colorless transparency to yellow transparency.
Example 3:
fluorination: weighing NH4HF2Has a mass of 8.12g, U3O8Has a mass of 1.00g, is3O8And NH4HF2Fully mixing, grinding, filling into a crucible, covering the crucible with a cover, placing into a 350 ℃ well type furnace, and reacting for 3 hours. After the reaction was complete, the product was collected and weighed to give 1.05gUO2F2Theoretically calculate UO2F2The mass of (2) was 1.10g, and the fluorination rate (. eta.) was calculated to be 95.7%.
Dissolving: KCl and LiCl were weighed to 22.50g and 19.00g, mixed well and uniformly in a crucible, placed in a 500 ℃ shaft furnace, and after the salt had melted, 0.30gUO was added2F2. To be treatedAfter 2 minutes, UO2F2The molten salt is dissolved, and the molten salt is changed from colorless transparency to yellow transparency.
Example 4:
fluorination: weighing NH4HF2Has a mass of 7.13g, UO3Has a mass of 1.00g, and is obtained by mixing UO3And NH4HF2Fully mixing, grinding, filling into a crucible, covering the crucible with a cover, placing into a 400 ℃ well type furnace, and reacting for 3 h. After the reaction was complete, the product was collected and weighed to give 0.97gUO2F2Theoretically calculate UO2F2The mass of (2) was 1.08g, and the fluorination rate (. eta.) was found to be 90.1% by calculation.
Dissolving: KCl and LiCl were weighed to 22.50g and 19.00g, mixed well and uniformly in a crucible, placed in a 500 ℃ shaft furnace, and after the salt had melted, 0.30gUO was added2F2. After 2 minutes, UO2F2The molten salt is dissolved, and the molten salt is changed from colorless transparency to yellow transparency.
Wherein FIG. 2 shows the oxide and NH of uranium at different temperatures4HF2The Gibbs free energy diagram of the reactions in which the fluorination reactions (1), (2), (3) and (4) correspond to the following, respectively, the Gibbs free energies of these reactions are all less than zero by calculation, and these reactions can proceed spontaneously as judged by thermodynamics:
U3O8+6NH4HF2+1/2O2(g)＝3UO2F2+6NH4F+3H2O(g) (1)
U3O8+6NH4HF2+1/2O2(g)＝3UO2F2+6NH3(g)+6HF(g)+3H2O(g) (2)
3UO3+6NH4HF2＝3UO2F2+6NH4F+3H2O(g) (3)
3UO3+6NH4HF2＝3UO2F2+6NH3(g)+6HF(g)+3H2O(g) (4)
in summary, the following steps: the invention provides a fluorinated U3O8Or UO3And dissolving in chloride molten salt. First uranium oxide (U)3O8Or UO3) And NH4HF2Mixing well, grinding, and filling into crucible (wherein U is3O8And NH4HF2The mass ratio of (A) to (B) is 1: 1-1: 12.3; UO3And NH4HF2The mass ratio of (1: 1) - (1: 12.0), and then fully reacting for 2-6 h at the temperature of 350-600 ℃. After the reaction is finished, the product is characterized by an X-ray diffractometer (XRD) to prove that the product is UO2F2And the fluorination rate can be up to 97.5 percent by calculation. Then, about 0.7-2% (mass ratio with molten salt) of UO is added2F2Adding into molten chloride molten salt, wherein the temperature range of the chloride molten salt is as follows: at 400-700 ℃ and UO2F2After dissolution, the molten salt changed from colorless to transparent to yellow. The invention provides a fluorinated U3O8Or UO3The method for dissolving the uranium oxide in the chloride molten salt has high fluorination rate on one hand and can solve the problem of dissolving the uranium oxide in the chloride molten salt on the other hand. Meanwhile, the process is carried out in the air, and the whole process is simple to operate.

Claims (5)

1. Fluorinated U3O8Or UO3The method for dissolving the fused salt in chloride is characterized by comprising the following steps:
will U3O8Or UO3Fully mixing with fluorinating agent powder, grinding, placing into a crucible for fluorination reaction, and obtaining a product UO after the reaction is finished2F2And UO2F2Adding into molten chloride molten salt, and finding complete dissolution, wherein the molten salt is changed from colorless transparency to yellow transparency, and the fluorinating agent is NH4HF2Said U3O8And NH4HF2The mass ratio of (A) to (B) is 1: 1-1: 12.3; UO3And NH4HF2The mass ratio of (A) to (B) is 1: 1-1: 12.0, the temperature of the fluorination reaction is 350-600 ℃, and the time of the fluorination reaction is 2-6 hours.
2. A fluorinated U according to claim 13O8Or UO3And dissolved in chloride molten salt, characterized in that the chloride molten salt is: one or more of LiCl-KCl, LiCl-CsCl and NaCl-CsCl.
3. A fluorinated U according to claim 23O8Or UO3And dissolved in chloride fused salt, characterized in that, the mol ratio of LiCl and KCl in the chloride fused salt LiCl-KCl is 74:51, the mol ratio of LiCl and CsCl in the chloride fused salt LiCl-CsCl is 29:21, and the mol ratio of NaCl and CsCl in the chloride fused salt NaCl-CsCl is 7: 13.
4. A fluorinated U according to claim 2 or 33O8Or UO3The method for dissolving the chloride fused salt into the chloride fused salt is characterized in that the chloride fused salt LiCl-KCl is heated to 400-600 ℃, the chloride fused salt LiCl-CsCl is heated to 400-600 ℃, and the chloride fused salt NaCl-CsCl is heated to 550-700 ℃.
5. A fluorinated U according to claim 13O8Or UO3And dissolved in a chloride molten salt, characterized in that said UO2F2The mass ratio of the chlorine to the chloride molten salt is 0.7-2%.
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