CN114582541A - Method for removing rare earth elements in spent fuel by chlorination process - Google Patents

Method for removing rare earth elements in spent fuel by chlorination process Download PDF

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Publication number
CN114582541A
CN114582541A CN202011371376.5A CN202011371376A CN114582541A CN 114582541 A CN114582541 A CN 114582541A CN 202011371376 A CN202011371376 A CN 202011371376A CN 114582541 A CN114582541 A CN 114582541A
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China
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rare earth
spent fuel
mixture
chlorination
earth elements
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CN202011371376.5A
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杜占
朱庆山
范川林
潘锋
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Institute of Process Engineering of CAS
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Institute of Process Engineering of CAS
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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/28—Treating solids
    • G21F9/30—Processing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • C22B1/2406—Binding; Briquetting ; Granulating pelletizing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00—Obtaining rare earth metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02—Obtaining thorium, uranium, or other actinides
    • C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0208—Obtaining thorium, uranium, or other actinides obtaining uranium preliminary treatment of ores or scrap
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02—Obtaining thorium, uranium, or other actinides
    • C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0213—Obtaining thorium, uranium, or other actinides obtaining uranium by dry processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/001—Dry processes
    • C22B7/002—Dry processes by treating with halogens, sulfur or compounds thereof; by carburising, by treating with hydrogen (hydriding)
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies

Abstract

The invention belongs to the technical field of chemical separation and spent fuel post-treatment, and discloses a method for removing rare earth elements in spent fuel by a chlorination process. The method comprises the steps of pretreating spent fuel to obtain a mixture of triuranium octoxide and rare earth oxide, then fully mixing the mixture with uranium tetrachloride to press the mixture into a ball, carrying out chlorination reaction to convert the rare earth oxide in the spent fuel into rare earth chloride, then volatilizing and separating the rare earth chloride by adopting a vacuum separation method to obtain the triuranium octoxide and uranium dioxide mixture without rare earth elements, and simultaneously condensing and collecting volatile matters to obtain the rare earth-containing chloride. The method has the advantages of high safety, simple process flow, capability of efficiently removing rare earth elements in the spent fuel, no impurity introduction, no waste liquid and waste gas generation and the like, and has good industrial application prospect.

Description

Method for removing rare earth elements in spent fuel by chlorination process
Technical Field
The invention belongs to the technical field of chemical separation and spent fuel post-treatment, and relates to a method for removing rare earth elements in spent fuel by a chlorination process.
Background
The nuclear fission energy is clean energy with mature technology, has the advantages of high efficiency, low carbon, large-scale utilization and the like, and is one of effective ways for solving the problem of continuous supply of energy in the future. However, the current situation that uranium resources are poor, the utilization rate of uranium resources of a nuclear reactor is low, and a large amount of high-level spent fuel is accumulated becomes a bottleneck for restricting the development of nuclear power. In order to improve the utilization rate of uranium resources and reduce the emission of high-radioactivity fission products and long-life radionuclides, scientific researchers in China innovatively put forward a brand-new concept and research scheme of an Accelerator Driven Advanced Nuclear Energy System (ADANES). The ADANES system is an advanced nuclear fuel closed cycle technology, integrates nuclear fuel proliferation, long-life nuclide transmutation and nuclear energy power generation, can improve the utilization rate of uranium resources to about 95%, reduces emission of long-life nuclear waste by more than 95%, and is expected to enable fission nuclear energy to become safe, reliable and clean strategic energy.
The post-processing of the spent fuel is an important step in the ADANES system, the post-processing flow of the spent fuel comprises separation of the spent fuel from cladding, separation of volatile fission elements, separation of rare earth elements and the like, wherein the pre-processing technologies of separation of the spent fuel from cladding, separation of volatile products and the like are mature, the device equipment is simple, the industrial application is easy, and the separation of the rare earth elements in the spent fuel is difficult, so that the method is an important difficult problem which needs to be solved urgently and efficiently in safe and utilization of the spent fuel. The rare earth elements have larger neutron absorption cross sections, and can seriously affect the proliferation of nuclear fuel and the transmutation of nuclear waste. The Chinese patent application CN1186564A discloses a method for removing rare earth elements from waste nuclear fuel, which comprises the steps of firstly oxidizing uranium dioxide in the waste nuclear fuel into triuranium octoxide at the temperature of 200-. The triuranium octoxide (about 10 mu m) and the rare earth oxide (about 1 mu m) after phase separation are both fine and tightly combined, and the method of filtering and separating by adopting ultrasonic dispersion-superfine filter cloth is only suitable for laboratory operation and is difficult to realize in practical large-scale application. Chinese patent CN105195328B discloses a method for removing rare earth elements in spent fuel by using a double organic phase flotation separation system containing ionic liquid, which takes P507 (2-ethylhexyl phosphonic acid-2-ethylhexyl monoester) as a rare earth separation extractant, ionic liquid as a synergistic enhanced extractant and oleic acid/kerosene as a diluent, and removes the rare earth elements by a multi-stage series differential flotation process. The method has the advantages that the single-process rare earth removal rate is low, multiple times of circulating separation are needed, the operation process is complex, the types of used liquid phase solvents are more, the use amount is larger, and the large-scale application is difficult. Chinese patent CN108538417B discloses a method for directly dissolving and removing rare earth elements in spent fuel by using ionic liquid, and the method adopts specific functionalized ionic liquid to selectively dissolve and remove the rare earth elements according to the solubility difference of uranium dioxide and rare earth oxide in the ionic liquid. Although the invention can directly remove the rare earth elements, the using amount of the ionic liquid is large, and the dissolved radioactive rare earth elements are difficult to recover, so that the risk of nuclear diffusion exists.
Therefore, the method safely and efficiently removes the rare earth elements in the spent fuel through technological and technical innovation, and is the key point for realizing the recycling of the spent fuel in China.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for removing rare earth elements in spent fuel, which is safe, reliable, green and environment-friendly and has a simple process. The method can realize the efficient removal of the rare earth elements in the spent fuel, has high safety, no impurity introduction, no waste liquid and waste gas generation, simple process flow and simple and convenient operation, and is suitable for large-scale treatment.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for removing rare earth elements in spent fuel by a chlorination method comprises the working procedures of pretreatment, chlorination, vacuum separation, condensation and the like, and specifically comprises the following steps:
(1) shearing, oxidizing and pretreating spent fuel at high temperature to obtain a pretreated product;
(2) mixing and briquetting the pretreatment product obtained in the step (1) and uranium tetrachloride to obtain a lump mixture;
(3) performing chlorination reaction on the block mass mixture obtained in the step (2) to obtain a chlorination product;
(4) and (4) carrying out vacuum separation on the chlorination product obtained in the step (3) to obtain a mixture of triuranium octoxide and uranium dioxide from which the rare earth elements are removed, and simultaneously condensing and collecting volatile matters to obtain rare earth-containing chloride.
In the step (1), the spent fuel contains more than 94% of uranium dioxide, 0.1-5% of rare earth elements and 0.1-1% of volatile fissile elements. The rare earth element refers to one or more of La, Pr, Nd, Sm, Yb and Gd. The volatile fission element is one or more of H, I, Xe, Kr, C, Cs, Te and Mo.
In the step (1), the pretreatment product is a mixture of triuranium octoxide and rare earth oxide.
In the step (2), the ratio of the added molar quantity of the uranium tetrachloride to the molar quantity of the rare earth elements in the spent fuel is (0.75-0.825): 1.
in the step (3), the chlorination temperature is 400-.
In the step (4), the vacuum separation temperature is 600-1600 ℃, the vacuum separation time is 1-10h, and the vacuum degree is 0.00001-9000 Pa.
Compared with the prior art, the invention has the following outstanding advantages:
(1) the method takes the uranium tetrachloride as the chlorinating agent, can efficiently remove the rare earth elements in the spent fuel through chlorination-vacuum separation, has simple process flow and equipment structure, is simple and convenient to operate, is convenient for large-scale treatment, and has good industrial application prospect.
(2) According to the invention, no impurities are introduced, no solvent is added or waste liquid or waste gas is generated, the separated rare earth elements and uranium oxide are in a solid phase, the recovery is convenient, the risk of nuclear diffusion is avoided, and the safety is high.
Drawings
Fig. 1 is a flow chart of a method for removing rare earth elements from spent fuel by a chlorination process according to the present invention.
Detailed Description
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. Unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features. The description is only for the purpose of facilitating understanding of the present invention and should not be construed as specifically limiting the present invention.
The invention is described in further detail below with reference to the figures and the detailed description.
It should be noted that, because the spent fuel has strong radioactivity, the example uses a non-radioactive or very low-radioactive simulation material of the same composition instead of the spent fuel.
Example 1
A method for removing rare earth elements in spent fuel by a chlorination method specifically comprises the following steps: (1) shearing, oxidizing and pretreating spent fuel at high temperature to obtain a pretreated product; (2) mixing and briquetting the pretreatment product obtained in the step (1) and uranium tetrachloride to obtain a lump mixture; (3) performing chlorination reaction on the block mass mixture obtained in the step (2) to obtain a chlorination product; (4) and (4) carrying out vacuum separation on the chlorination product obtained in the step (3) to obtain a mixture of triuranium octoxide and uranium dioxide from which the rare earth elements are removed, and simultaneously condensing and collecting volatile matters to obtain rare earth-containing chloride.
Example 2
In this example, the method for removing rare earth elements from spent fuel by chlorination method described in example 1 is adopted, and UO in the used simulation material2Content 98.88% of Nd2O30.12 percent of the content and 1 percent of the I content, wherein the mass fraction of the Nd element is 0.1 percent, and UCl is added4The amount of the material accounts for 0.2 percent of the mass ratio of the simulated material, whereinUCl4The molar ratio of Nd element is 0.75: 1. firstly, shearing, oxidizing and pretreating a simulation material at high temperature to obtain a mixture of triuranium octoxide and a rare earth oxide, then fully mixing and briquetting the mixture with uranium tetrachloride to obtain a briquette-like mixture, then placing the briquette-like mixture in argon gas at 400 ℃ for chlorination for 5 hours with system pressure of 80kPa, then heating a chlorination product at 600 ℃ and a vacuum degree of 0.00001Pa for 10 hours to obtain U with the rare earth element content of less than 0.1 per mill3O8And UO2Mixing the powder and condensing and collecting the collected chloride containing rare earth.
Example 3
In this embodiment, the method for removing rare earth elements from spent fuel by chlorination method described in embodiment 1 is used, and UO in the used simulation material294.07% of Nd2O35.83 percent of the element Nd and 0.1 percent of the element I, wherein the mass fraction of the element Nd is 5 percent, and UCl is added4The amount of the material accounts for 10.86 percent of the mass ratio of the simulated material, wherein UCl4The molar ratio to Nd element was 0.825: 1. firstly, shearing, oxidizing and pretreating a simulation material at high temperature to obtain a mixture of triuranium octoxide and a rare earth oxide, then fully mixing and briquetting the mixture with uranium tetrachloride to obtain a briquette-like mixture, then placing the briquette-like mixture in argon gas at 900 ℃ for chlorination for 0.5h, wherein the system pressure is 150kPa, then heating a chlorination product at 1600 ℃ and a vacuum degree of 9000Pa for 1h to obtain U with the rare earth element content of less than 0.1 thousandth3O8And UO2Mixing the powder and condensing and collecting the collected chloride containing rare earth.
Example 4
In this embodiment, the method for removing rare earth elements from spent fuel by chlorination method described in embodiment 1 is used, and UO in the used simulation material2Content of 96% Nd2O33.5 percent of the element I and 3 percent of the element Nd, and adding UCl4The amount of the material accounts for 6.32 percent of the mass ratio of the simulated material, wherein UCl4The molar ratio of Nd element is 0.8: 1. firstly, shearing, oxidizing and pretreating a simulation material at high temperature to obtain a mixture of triuranium octoxide and rare earth oxide, then fully mixing and briquetting the mixture with uranium tetrachloride to obtain a block-shaped mixture,then placing the block-shaped mixture in argon gas at 500 ℃ for chlorination for 4h, wherein the system pressure is 90kPa, and calcining the chlorination product at 1200 ℃ and the vacuum degree of 200Pa for 8h to obtain U with the rare earth element content of less than 0.1 per mill3O8And UO2Mixing the powder and condensing and collecting the collected chloride containing rare earth.
Example 5
In this embodiment, the method for removing rare earth elements from spent fuel by chlorination method described in embodiment 1 is used, and UO in the used simulation material2Content of La 98.13%2O31.17 percent of La element and 0.7 percent of Mo element, wherein the mass fraction of the La element is 1 percent, and UCl is added4The amount of the simulated material is 2.11 percent of the mass ratio of the simulated material, wherein UCl4Molar ratio to La element was 0.77: 1. firstly, shearing, oxidizing and pretreating a simulation material at high temperature to obtain a mixture of triuranium octoxide and a rare earth oxide, then fully mixing and briquetting the mixture with uranium tetrachloride to obtain a briquette-like mixture, then placing the briquette-like mixture in argon gas at 750 ℃ for chlorination for 2.5h, wherein the system pressure is 100kPa, and then calcining a chlorination product at 1000 ℃ and a vacuum degree of 9Pa for 6h to obtain U with the rare earth element content of less than 0.1 thousandth3O8And UO2Mixing the powder and condensing and collecting the rare earth-containing chloride.
Example 6
In this embodiment, the method for removing rare earth elements from spent fuel by chlorination method described in embodiment 1 is used, and UO in the used simulation material295.06 percent of Sm2O34.64 percent of element Sm and 0.3 percent of element Cs, wherein the mass fraction of the element Sm is 4 percent, and UCl is added4The amount of the material accounts for 7.57 percent of the mass ratio of the simulated material, wherein UCl4The molar ratio of Sm to Sm is 0.75: 1. firstly, shearing, oxidizing and pretreating a simulation material at high temperature to obtain a mixture of triuranium octoxide and a rare earth oxide, then fully mixing and briquetting the mixture with uranium tetrachloride to obtain a briquette-like mixture, then placing the briquette-like mixture in argon gas at 650 ℃ for chlorination for 4 hours with the system pressure of 85kPa, and then calcining a chlorination product at 1400 ℃ and the vacuum degree of 1000Pa for 1.5 hours to obtain U with the rare earth element content of less than 0.1 thousandth3O8And UO2MixingPowder and condensed and collected rare earth-containing chloride.
Example 7
In this example, the method for removing rare earth elements from spent fuel by chlorination method described in example 1 is adopted, and UO in the used simulation material294.11% of Yb2O35.69 percent of the element Yb and 0.2 percent of Te, wherein the mass fraction of the element Yb is 5 percent, and UCl is added4The amount of the simulated material accounts for 8.78 percent of the mass ratio of the simulated material, wherein UCl4The molar ratio of Yb element is 0.8: 1. firstly, shearing, oxidizing and pretreating a simulation material at high temperature to obtain a mixture of triuranium octoxide and a rare earth oxide, then fully mixing and briquetting the mixture with uranium tetrachloride to obtain a briquette-like mixture, then placing the briquette-like mixture in argon gas at 680 ℃ for chlorination for 3.5 hours with the system pressure of 120kPa, and then calcining a chlorination product at 900 ℃ and the vacuum degree of 0.1Pa for 2.5 hours to obtain U with the rare earth element content of less than 0.1 thousandth3O8And UO2Mixing the powder and condensing and collecting the collected chloride containing rare earth.
Example 8
In this embodiment, the method for removing rare earth elements from spent fuel by chlorination method described in embodiment 1 is used, and UO in the used simulation material295.69 percent of Pr2O33.51 percent of element Pr and 0.8 percent of Cs, wherein the mass fraction of the element Pr is 3 percent, and UCl is added4The amount of the simulated material is 6.55 percent of the mass ratio of the simulated material, wherein UCl4The molar ratio of the element Pr is 0.81: 1. firstly, shearing, oxidizing and pretreating a simulation material at high temperature to obtain a mixture of triuranium octoxide and a rare earth oxide, then fully mixing and briquetting the mixture with uranium tetrachloride to obtain a briquette-like mixture, then placing the briquette-like mixture in argon gas at 640 ℃ for chlorination for 4.5 hours, wherein the system pressure is 110kPa, and then calcining a chlorination product at 1500 ℃ and a vacuum degree of 5000Pa for 1 hour to obtain U with the rare earth element content of less than 0.1 per mill3O8And UO2Mixing the powder and condensing and collecting the collected chloride containing rare earth.
Example 9
In this example, the method for removing rare earth elements from spent fuel by chlorination method described in example 1, and the simulation used in the methodUO in the material297.59% of Gd2O32.31 percent of Gd element and 0.1 percent of C element, wherein the mass fraction of Gd element is 2 percent, and UCl is added4The amount of the material accounts for 3.96 percent of the mass ratio of the simulated material, wherein UCl4The molar ratio of Gd element to Gd element is 0.82: 1. firstly, shearing, oxidizing and pretreating a simulation material at high temperature to obtain a mixture of triuranium octoxide and a rare earth oxide, then fully mixing and briquetting the mixture with uranium tetrachloride to obtain a briquette-like mixture, then placing the briquette-like mixture in argon gas at 750 ℃ for chlorination for 3 hours with system pressure of 130kPa, and then calcining a chlorination product at 700 ℃ and vacuum degree of 0.0001Pa for 1.5 hours to obtain U with the rare earth element content of less than 0.1 thousandth3O8And UO2Mixing the powder and condensing and collecting the collected chloride containing rare earth.
The method can be realized by upper and lower limit values of intervals of process parameters (such as temperature, time and the like) and interval values, and embodiments are not listed.
Those skilled in the art will recognize that the invention may be practiced without these specific details.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (6)

1. A method for removing rare earth elements from spent fuel by a chlorination method comprises the following steps:
1) shearing, oxidizing and pretreating spent fuel at high temperature to obtain a pretreated product;
2) mixing and briquetting the pretreatment product obtained in the step 1) and uranium tetrachloride to obtain a lump mixture;
3) carrying out chlorination reaction on the block mass mixture obtained in the step 2) to obtain a chlorination product;
4) and (4) carrying out vacuum separation on the chlorination product obtained in the step 3) to obtain a mixture of triuranium octoxide and uranium dioxide from which the rare earth elements are removed, and condensing and collecting volatile matters to obtain rare earth-containing chloride.
2. The method according to claim 1, wherein in the step 1), the uranium dioxide content in the spent fuel is more than 94%, the rare earth element content is 0.1-5%, and the volatile fissile element content is 0.1-1%; the rare earth element refers to one or more of La, Pr, Nd, Sm, Yb and Gd; the volatile fission element is one or more of H, I, Xe, Kr, C, Cs, Te and Mo.
3. The method according to claim 1 or 2, wherein in step 1), the pre-treatment product is a mixture of triuranium octoxide and a rare earth oxide.
4. The method according to any one of claims 1 to 3, wherein in the step 2), the ratio of the molar amount of uranium tetrachloride added to the molar amount of rare earth elements in the spent fuel is (0.75-0.825): 1.
5. the method as claimed in any one of claims 1 to 4, wherein in step 3), the chlorination temperature is 400 ℃ and 900 ℃, the chlorination time is 0.5 to 5h, and the system pressure is 80 to 150 kPa.
6. The method as claimed in any one of claims 1 to 5, wherein the vacuum separation temperature in step 4) is 600-1600 ℃, the vacuum separation time is 1-10h, and the vacuum degree is 0.00001-9000 Pa.
CN202011371376.5A 2020-11-30 2020-11-30 Method for removing rare earth elements in spent fuel by chlorination process Pending CN114582541A (en)

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