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Method for extracting and separating trivalent lanthanide and/ or actinide ions by using phenanthroline phosphorus oxide

A technology of o-phenanthroline and phosphorus oxide, which is used in the field of nuclear fuel cycle and waste liquid treatment, can solve the problem that the distribution ratio of trivalent lanthanide and actinide is not high, and it is not suitable for the co-separation process of trivalent lanthanide and actinide. and other problems, to achieve the effect of good application prospect, fast extraction rate and strong extraction ability

Active Publication Date: 2021-03-09
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the distribution ratio of trivalent lanthanides and actinides is not high, so it is not suitable for the co-separation process of trivalent lanthanides and actinides

Method used

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  • Method for extracting and separating trivalent lanthanide and/ or actinide ions by using phenanthroline phosphorus oxide
  • Method for extracting and separating trivalent lanthanide and/ or actinide ions by using phenanthroline phosphorus oxide
  • Method for extracting and separating trivalent lanthanide and/ or actinide ions by using phenanthroline phosphorus oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0062] The preparation of embodiment 1 o-phenanthroline phosphorus oxide BuPh-PhenPO

[0063]

[0064] Using 2,9-dichloro-1,10-phenanthroline (2,9-dichloro-1,10-phenanthroline) as the initial reactant and the intermediate product butylphenylphosphine oxide in anhydrous toluene solvent, Under argon atmosphere, fully dissolve and mix according to the mass ratio of substances (1:2.5~1:3.0), and add K under the catalysis of palladium acetate and dppf 2 CO 3 The reflux reaction was carried out for about 7 hours, and the reaction progress was tracked by TLC thin-layer chromatography until the raw materials were completely reacted. After the reaction mixture was cooled, the solvent was removed by a rotary evaporator to obtain a crude product, and finally the obtained crude product was separated and purified by silica gel column chromatography to obtain the product BuPh-PhenPO.

[0065] like figure 1 As shown, BuPh-PhenPO 1 H NMR spectrum, wherein each peak is attributed to: (5...

Embodiment 2

[0066] Example 2 o-phenanthroline phosphorus oxide Ph 2 - Preparation of PhenPO

[0067]

[0068] With 2,9-dichloro-1,10-phenanthroline (2,9-dichloro-1,10-phenanthroline) as the initial reactant and the intermediate product diphenylphosphine oxide in anhydrous toluene solvent, in Under high-purity argon atmosphere, fully dissolve and mix according to the mass ratio of substances (1:2.5~1:3.0), and add K under the catalysis of palladium acetate and dppf 2 CO 3 The reflux reaction was carried out for about 7 hours, and the reaction progress was tracked by TLC thin-layer chromatography until the raw materials were completely reacted. After the reaction mixture was cooled, it was washed with water to remove water-soluble impurities, dried over anhydrous sodium sulfate to remove water, and then the solvent was removed by a rotary evaporator to obtain a crude product, which was finally purified by silica gel column chromatography using dichloromethane / ethyl acetate Ester / metha...

Embodiment 3

[0071] Preparation of the organic phase: Dissolve the BuPh-PhenPO prepared in Example 1 in 3-nitrobenzotrifluorotoluene solvent to prepare a 0.005 mol / liter BuPh-PhenPO solution as the organic phase of the extraction experiment;

[0072] The preparation of aqueous phase: get containing trace amount (about 10 -9 mol / L) of radioactive elements 241 Am(III) and 152, 154 The aqueous solution of Eu(III) nitric acid is diluted with deionized water and added quantitative concentrated nitric acid to prepare an aqueous solution with a series of nitric acid concentrations as the organic phase of the extraction. The concentration of nitric acid is 0.1, 0.5, 1.0, 2.0, 3.0, 4.0 mol / L;

[0073] First take 0.6mL containing 241 Am(III) and 152,154 Aqueous solutions of nitric acid with different concentrations of the Eu(III) water phase were used as the water phase in the extraction process, and were added to the ground reagent bottles containing magnetrons respectively, and 100 μL contain...

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Abstract

The invention relates to the technical field of nuclear fuel circulation and waste liquid treatment, and particularly relates to a method for extracting and separating trivalent lanthanide and / or actinide ions by using phenanthroline phosphorus oxide. The method comprises the following steps: taking phenanthroline phosphorus oxide shown in a formula (1) as an extracting agent, mixing the phenanthroline phosphorus oxide with an organic solvent to form an organic phase, and extracting the trivalent lanthanide and / or actinide ions from a water phase, wherein the water phase is an acidic solution containing the trivalent lanthanide and / or actinide ions, R1 is phenyl or substituted phenyl, and R2 is phenyl, C1-C10 straight-chain alkyl or branched-chain alkyl. By the method, minor actinide elements and lanthanide elements can be efficiently extracted and separated from a strong nitric acid aqueous solution, the highest extraction rate can reach 99.9%, and the method has good application prospect in the field of co-separation of the trivalent lanthanide and actinide ions in radioactive waste liquid, particularly high-level radioactive waste liquid, in the nuclear industry. Formula (I)sees the description.

Description

technical field [0001] The invention relates to the technical field of nuclear fuel cycle and waste liquid treatment, in particular to a method for o-phenanthroline phosphorus oxide and extraction and separation of trivalent lanthanide and / or actinide ions. Background technique [0002] Vigorously developing nuclear energy has become an important measure for my country to promote energy transformation, respond to climate change, curb global warming, and reduce greenhouse gas emissions. However, with the rapid development of nuclear power, a large amount of spent fuel has also been produced. It is estimated that the cumulative output of spent fuel in my country will be 13,000-14,000 tons in 2030. How to safely and effectively dispose of the spent fuel generated in the process of nuclear power development has become a limit to my country's nuclear power. One of the key bottlenecks for sustainable development. In order to maximize the utilization of nuclear fuel resources, redu...

Claims

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Application Information

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IPC IPC(8): C22B3/38C22B59/00C22B60/02
CPCC22B59/00C22B60/02
Inventor 肖成梁徐雷杨晓
Owner ZHEJIANG UNIV
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