CN116835655A - U (U) 3 O 8 Preparation of UO 2 Is a method of (2) - Google Patents

U (U) 3 O 8 Preparation of UO 2 Is a method of (2) Download PDF

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Publication number
CN116835655A
CN116835655A CN202310268266.3A CN202310268266A CN116835655A CN 116835655 A CN116835655 A CN 116835655A CN 202310268266 A CN202310268266 A CN 202310268266A CN 116835655 A CN116835655 A CN 116835655A
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vacuum
temperature
preparation
sintering
active carbon
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CN202310268266.3A
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CN116835655B (en
Inventor
许恒斌
杨明帅
宋文臣
沈振芳
李斌
王长水
何辉
晏太红
叶国安
李保乐
姚本林
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China Institute of Atomic of Energy
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China Institute of Atomic of Energy
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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
    • C01G43/01—Oxides; Hydroxides
    • C01G43/025—Uranium dioxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • 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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  • 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 discloses a U 3 O 8 Preparation of UO 2 Is prepared through reduction of U by active carbon 3 O 8 Active carbon and U are shortened by tabletting and forming 3 O 8 The inter-molecular distance of the gas to prevent the powder from being entrained in the reaction process; and the porous structure of the activated carbon greatly increases the U 3 O 8 Contact area, improved reduction efficiency, and activated carbon in final product UO 2 Has been removed, ensure UO 2 Is of a purity of (3); the method is simple, short in period and high in safety; suitable for large-scale reduction U 3 O 8 Preparation of UO 2 。

Description

U (U) 3 O 8 Preparation of UO 2 Is a method of (2)
Technical Field
The invention belongs to the technical field of spent fuel aftertreatment, and particularly relates to a U 3 O 8 Preparation of UO 2 Is a method of (2).
Background
Uranium dioxide is an important component of fast reactor MOX fuel, and has important application prospect in fast neutron breeder reactor (FBR). The most stable oxide form of uranium is triuranium octoxide, and uranium dioxide can be spontaneously converted into triuranium octoxide at room temperature, so that the physical and chemical properties of the uranium octoxide are changed.
A common uranium dioxide production process is the Ammonium Diuranate (ADU) method: using UF6 as raw material, hydrolyzing and precipitating to obtain Ammonium Diuranate (ADU), and then adding H 2 Decomposing and reducing the uranium dioxide powder under the atmosphere. However, the process for preparing uranium dioxide has long production period, complex working procedures and unstable O/U ratio of the obtained uranium dioxide powder.
Disclosure of Invention
Aiming at the technical problems existing in the prior art, the invention aims to provide a U with stable O/U ratio, safe, simple, convenient and efficient operation process 3 O 8 Preparation of UO 2 Is a method of (2).
In order to achieve the above purpose, the invention adopts the following technical scheme: u (U) 3 O 8 Preparation of UO 2 Comprising the steps of:
(1) Uniformly mixing activated carbon and triuranium octoxide in a proper proportion, and tabletting for molding;
(2) Carrying out low-temperature vacuum sintering on the pressed active carbon and triuranium octoxide;
(3) High-temperature vacuum heating to remove active carbon;
(4) Vacuum cooling to below 50deg.C, and cooling to obtain UO 2 And (5) a core block.
Further, in the step (1), the amount of the activated carbon is more than 2.9% of the mass of the triuranium octoxide.
Further, in the step (2), the temperature of the low-temperature vacuum sintering is 500-1300 ℃, the vacuum degree is less than 100Pa, and the sintering time is 0-8 h.
Further, in the step (3), the high-temperature vacuum heating temperature is more than 1300 ℃, the vacuum degree is less than 100Pa, and the heating time is 0-8 h.
Further, in the step (4), the vacuum cooling temperature is 20-30 ℃.
The technical scheme of the invention has the beneficial effects that the U is as follows 3 O 8 Preparation of UO 2 Is prepared through reduction of U by active carbon 3 O 8 The intermolecular distance of reactants is shortened through tabletting and forming, so that entrainment of gas to powder in the reaction process is prevented; and the porous structure of the activated carbon greatly increases the U 3 O 8 Improves the reduction efficiency, and the active carbon is arranged in the final product UO 2 Has been removed, ensure UO 2 Is of a purity of (3); the method is simple, short in period and high in safety; suitable for large-scale reduction U 3 O 8 Preparation of UO 2 。
Drawings
FIG. 1 is a UO prepared by the method of example two of the present invention 2 An XRD pattern of (a);
FIG. 2 is a UO prepared by the method of example III of the present invention 2 An XRD pattern of (a);
FIG. 3 is a UO prepared by the method of example IV of the invention 2 Is a XRD pattern of (C).
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Example 1
The embodiment of the invention provides a U 3 O 8 Preparation of UO 2 Comprising the steps of:
(1) Mixing proper amount of active carbon and triuranium octooxide uniformly, tabletting and forming; the dosage of the activated carbon is 2.9% of the mass of the triuranium octoxide, so that the excessive amount of the activated carbon is ensured; the reduction rate of the triuranium octoxide is ensured; the intermolecular distance of reactants is shortened by tabletting and forming, so that the reaction is easier to occur, and the entrainment of gas to powder in the reaction process can be prevented;
(2) Carrying out low-temperature vacuum sintering on the pressed active carbon and triuranium octoxide; the low-temperature vacuum sintering temperature is 500-1300 ℃, the vacuum degree is below 100Pa, and the sintering time is 0-8 h
(3) High-temperature vacuum heating to remove active carbon; the high-temperature vacuum heating temperature is more than 1300 ℃, the vacuum degree is less than 100Pa, and the heating time is 0-8 h;
(4) Vacuum cooling to below 50deg.C, and cooling to obtain UO 2 And (5) a core block. Preventing UO caused by contact with air during cooling 2 The pellets are oxidized again, maintaining a stable O/U ratio.
Preferably, in the step (1), the pressure range of the tabletting molding is 56-226 Mpa; under the pressure range, the formed activated carbon and the lump of triuranium octoxide are not loose and are not easy to break.
Preferably, in the step (2), the vacuum temperature is 900 ℃, the vacuum degree is 0.1Pa, and the sintering time is 4 hours.
Preferably, in the step (3), the high-temperature sintering temperature is 1500 ℃, the vacuum degree is 0.1Pa, and the sintering time is 4 hours.
Preferably, in the step (4), the temperature is reduced to 20 ℃ to 30 ℃ in vacuum.
Example two
Method U adopting embodiment one of the invention 3 O 8 Preparation of UO 2 Comprising the steps of:
(1) Weighing active carbon with the mass ratio of 0.12:1, uniformly mixing the active carbon with triuranium octoxide, and uniaxially pressing the mixture in a steel mould (8 mm) for 3min under the pressure of 113MPa for molding;
(2) Placing the sample into a vacuum furnace, and vacuum sintering for 4 hours under the condition of 900-0.1 Pa;
(3) Cooling to room temperature under vacuum of 0.1Pa, and taking out the sample.
Weighing the sample, wherein the mass of the sample after reaction is 1.053g, and the mass loss of the sample is 0.067g; the sample was completely and fully burnt in an air atmosphere at 600 c, giving a powder mass of 0.99g.
Referring to FIG. 1, a sample prepared by the method of the present invention is shown with excess activated carbon doped therein
The rest is the same as the first embodiment.
Example III
Method U adopting embodiment one of the invention 3 O 8 Preparation of UO 2 Comprising the steps of:
(1) Weighing active carbon with the mass ratio of 0.12:1, uniformly mixing the active carbon with triuranium octoxide, and uniaxially pressing the mixture in an 8mm steel mould for 3min under the pressure of 113MPa for molding;
(2) Placing the sample into a vacuum furnace, and vacuum sintering for 4 hours under the condition of 900-0.1 Pa;
(3) Vacuum sintering for 4h under the condition of 1500-0.1 Pa;
(4) Cooling to room temperature under vacuum of 0.1Pa, and taking out the sample.
Referring to FIG. 2, the method of the embodiment of the invention will U 3 O 8 Complete conversion to UO 2 The sample was weighed, the sample mass lost 0.159g, and the excess activated carbon was substantially removed.
The rest is the same as the first embodiment.
Example IV
Method U adopting embodiment one of the invention 3 O 8 Preparation of UO 2 Comprising the steps of:
(1) Weighing active carbon with the mass ratio of 0.12:1, uniformly mixing the active carbon with triuranium octoxide, and uniaxially pressing the mixture in an 8mm steel mould for 3min under the pressure of 113MPa for molding;
(2) Placing the sample into a vacuum furnace, and vacuum sintering for 4 hours at 900 ℃ and 0.1 Pa;
(3) Continuously sintering for 4 hours under the conditions of 1500 ℃ and 0.1 Pa;
(4) Cooling to 300 ℃ under the vacuum condition of 0.1Pa, and opening the furnace cover.
The columnar sample in the furnace burns rapidly in the process of uncovering, turns into powder in 1min, and is weighed after collection, and the mass is 0.98g.
Referring to FIG. 3, a restored U is shown 3 O 8 Re-oxidized again during uncapping; a mass loss of 0.02g is an operational error during powder transfer.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.

Claims (8)

1. U (U) 3 O 8 Preparation of UO 2 Is characterized by comprising the steps of:
(1) Uniformly mixing activated carbon and triuranium octoxide in a proper proportion, and tabletting for molding;
(2) Carrying out low-temperature vacuum sintering on the pressed active carbon and triuranium octoxide;
(3) High-temperature vacuum heating to remove active carbon;
(4) Vacuum cooling to below 50deg.C, and cooling to obtain UO 2 And (5) a core block.
2. A U according to claim 1 3 O 8 Preparation of UO 2 Is characterized in that in the step (1), the amount of the activated carbon is more than 2.9 percent of the mass of the triuranium octoxide.
3. A U according to claim 1 3 O 8 Preparation of UO 2 The method is characterized in that in the step (2), the temperature of low-temperature vacuum sintering is 500-1300 ℃, the vacuum degree is less than 100Pa, and the sintering time is 0-8 h.
4. According to claimA U as defined in claim 1 3 O 8 Preparation of UO 2 In the step (3), the high-temperature vacuum heating temperature is more than 1300 ℃, the vacuum degree is less than 100Pa, and the heating time is 0-8 h.
5. A U according to claim 1 3 O 8 Preparation of UO 2 The method of (2) is characterized in that in the step (4), the vacuum cooling temperature is 20-30 ℃.
6. A U according to claim 1 3 O 8 Preparation of UO 2 In the step (2), the vacuum temperature is 900 ℃, the vacuum degree is 0.1Pa, and the sintering time is 4 hours.
7. A U according to claim 1 3 O 8 Preparation of UO 2 The method is characterized in that in the step (3), the high-temperature sintering temperature is 1500 ℃, the vacuum degree is 0.1Pa, and the sintering time is 4 hours.
8. A U according to claim 1 3 O 8 Preparation of UO 2 The method is characterized in that in the step (4), the temperature is reduced to 20-30 ℃ in vacuum.
CN202310268266.3A 2023-03-15 2023-03-15 A method for preparing UO2 from U3O8 Active CN116835655B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3953556A (en) * 1973-01-12 1976-04-27 The United States Of America As Represented By The United States Energy Research And Development Administration Method of preparing uranium nitride or uranium carbonitride bodies
JPH0545484A (en) * 1991-08-12 1993-02-23 Nuclear Fuel Ind Ltd Uranium dioxide powder for atomic fuel and manufacture thereof
JPH0572384A (en) * 1991-03-29 1993-03-26 Nuclear Fuel Ind Ltd Method for producing nuclear fuel sintered body
CN1319848A (en) * 2001-03-30 2001-10-31 中国核动力研究设计院 Method for preparing Gd2O3-UO2 flammable poison fuel core block by using U3O8 powder
US20130148774A1 (en) * 2011-12-13 2013-06-13 Korea Hydro And Nuclear Power Co., Ltd. Porous uo2 sintered pellets and method for fabricating porous uo2 sintered pellets and electrolytic reduction using same
CN106297904A (en) * 2016-08-25 2017-01-04 中广核研究院有限公司 Preparation method of UO2–SiC fuel pellets and UO2–SiC fuel pellets made by the preparation method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3953556A (en) * 1973-01-12 1976-04-27 The United States Of America As Represented By The United States Energy Research And Development Administration Method of preparing uranium nitride or uranium carbonitride bodies
JPH0572384A (en) * 1991-03-29 1993-03-26 Nuclear Fuel Ind Ltd Method for producing nuclear fuel sintered body
JPH0545484A (en) * 1991-08-12 1993-02-23 Nuclear Fuel Ind Ltd Uranium dioxide powder for atomic fuel and manufacture thereof
CN1319848A (en) * 2001-03-30 2001-10-31 中国核动力研究设计院 Method for preparing Gd2O3-UO2 flammable poison fuel core block by using U3O8 powder
US20130148774A1 (en) * 2011-12-13 2013-06-13 Korea Hydro And Nuclear Power Co., Ltd. Porous uo2 sintered pellets and method for fabricating porous uo2 sintered pellets and electrolytic reduction using same
CN106297904A (en) * 2016-08-25 2017-01-04 中广核研究院有限公司 Preparation method of UO2–SiC fuel pellets and UO2–SiC fuel pellets made by the preparation method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
李红霞等编: "《耐火材料手册 第2版》", 31 January 2021, 冶金工业出版社, pages: 202 - 203 *

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