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Aqueous-phase preparation method of anhydrous uranyl chloride

A technology for the preparation of uranyl chloride and aqueous phase, which is applied in the field of uranyl chloride, can solve the problems of harsh reaction conditions and low synthesis efficiency, and achieve the effects of low requirements for equipment and process conditions, fast reaction and good economy

Active Publication Date: 2021-12-10
SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of harsh reaction conditions or low synthesis efficiency in the above-mentioned prior art, the present invention provides an aqueous phase preparation method of anhydrous uranyl chloride

Method used

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  • Aqueous-phase preparation method of anhydrous uranyl chloride
  • Aqueous-phase preparation method of anhydrous uranyl chloride
  • Aqueous-phase preparation method of anhydrous uranyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Add 7.00ml of pure water and 3.00ml of concentrated hydrochloric acid into a round bottom flask, place in a water bath and heat to 90°C; keep magnetic stirring, and add 2g of U3O8 powder.

[0032] Add 2.00ml of hydrogen peroxide dropwise at a rate of 0.18ml / min, and time the reaction for 1h from the dropwise addition. The ultraviolet absorption spectrum of the obtained uranyl solution is as follows: figure 1 As shown, there is only one strong absorption peak at 414nm, indicating that only hexavalent uranyl ions exist in the solution, proving that U 3 o 8 Has been completely converted to uranyl.

[0033] After the reaction, the solution in the flask was transferred to a tetrafluoroethylene tube and placed on a constant temperature heating plate, and evaporated and crystallized at 80°C for 24 hours. The XRD spectrogram of the obtained uranyl chloride crystal containing water of crystallization is as follows figure 2 As shown, in which, in addition to the background s...

Embodiment 2

[0038] Add 7.60ml of pure water and 2.40ml of concentrated hydrochloric acid into a round bottom flask, place in a water bath and heat to 60°C; keep magnetic stirring, and add 2g of U3O8 powder.

[0039] Add 1.50ml of hydrogen peroxide dropwise at a rate of 0.15ml / min, and time the reaction for 30min from the beginning of the dropwise addition.

[0040] After the reaction, the solution was transferred to a tetrafluoroethylene tube and placed on a heating plate, and evaporated and crystallized at 60°C for 48h.

[0041] Subsequently, the tetrafluoroethylene tube was quickly transferred to a vacuum drying oven, and dried at 150°C and -0.1MPa for 48h.

[0042] The dried powder was transferred into a corundum crucible, placed in a high-temperature furnace with an argon atmosphere, and dried at 235 °C for 6 h.

[0043] After being dried and dehydrated, the uranyl chloride product is sealed and stored after cooling to avoid moisture absorption.

Embodiment 3

[0045] Add 10ml of concentrated hydrochloric acid into the round bottom flask, place it in a water bath and heat it to 70°C; keep magnetic stirring, and add 2g of U3O8 powder.

[0046] Add 3.00ml of hydrogen peroxide dropwise at a rate of 0.2ml / min, and time the reaction for 90min from the beginning of the dropwise addition.

[0047] After the reaction, the solution was transferred to a tetrafluoroethylene tube and placed on a heating plate, and evaporated and crystallized at 110° C. for 12 hours.

[0048] Subsequently, the tetrafluoroethylene tube was quickly transferred to a vacuum drying oven, and dried at 220°C and -0.1MPa for 12h.

[0049] The dried powder was transferred into a corundum crucible, placed in a high-temperature furnace with an argon atmosphere, and dried at 260 °C for 1 h.

[0050] After being dried and dehydrated, the uranyl chloride product is sealed and stored after cooling to avoid moisture absorption.

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Abstract

The invention relates to an aqueous-phase preparation method of anhydrous uranyl chloride. The method comprises the following steps of: by taking triuranium octaoxide powder as a raw material and a hydrochloric acid aqueous solution as a solvent, slowly and continuously dropwise adding hydrogen peroxide under a heating condition to obtain a uranyl solution; preforming evaporative crystallization on the uranyl solution, so as to obtain uranyl chloride crystals containing crystal water; placing the uranyl chloride crystals containing the crystal water in a vacuum drying oven to dry the uranyl chloride crystals containing the crystal water to obtain a uranyl chloride monohydrate crystal; and drying the uranyl chloride monohydrate crystal in an inert atmosphere high-temperature furnace to obtain the anhydrous uranyl chloride. The preparation method is an aqueous-solution system, a hydrogen peroxide oxidation method is adopted, the triuranium octaoxide is dissolved in the hydrochloric acid aqueous solution in an auxiliary mode through the hydrogen peroxide, the dissolution rate and solubility of the triuranium octaoxide in the hydrochloric acid aqueous solution are greatly increased, the conditions are milder, and the reaction is rapid; uranium ions obtained after dissolution are all oxidized into uranyl ions, the synthesis efficiency is higher; and the decomposition of the uranyl chloride is effectively avoided by controlling the drying temperature in different stages.

Description

technical field [0001] The invention relates to uranyl chloride, and more particularly to an aqueous phase preparation method of anhydrous uranyl chloride. Background technique [0002] At present, in the research on uranyl compounds in anhydrous systems, such as the uranyl electrolysis process in the molten salt system, the direct oxidation method of the molten salt phase is mainly used, and the uranium The oxide is oxidized to uranyl and thus dissolved in the molten salt. Although the molten salt phase direct oxidation method realizes the in-situ reduction of uranyl and avoids the introduction of water into the system, its conversion efficiency is low, the operating temperature is high, and chlorine gas severely corrodes the equipment. The synthesis of anhydrous uranyl chloride in a non-molten salt system is usually prepared by the gas phase reaction of uranium tetrachloride and oxygen under anhydrous conditions, but uranium tetrachloride itself is unstable and difficult ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G43/00
CPCC01G43/00C01P2002/72C01P2002/84Y02E30/30
Inventor 李玉禾黄卫窦强李晴暖
Owner SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI