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Bispyrazole extractant derived from o-phenanthroline and its preparation method and use

A technology of phenanthroline and extraction agent, which is applied in the fields of nuclear fuel cycle and nuclear waste treatment, and can solve the problems of slow extraction kinetics and difficult stripping.

Active Publication Date: 2021-04-02
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the problems of slow extraction kinetics and difficult stripping in nitrogen-containing extractants currently used for Lns / Ans separation, the invention provides a bispyrazole extractant derived from o-phenanthroline

Method used

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  • Bispyrazole extractant derived from o-phenanthroline and its preparation method and use
  • Bispyrazole extractant derived from o-phenanthroline and its preparation method and use
  • Bispyrazole extractant derived from o-phenanthroline and its preparation method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] This example prepares 2,9-bis(5-n-octyl-1-hydrogen-pyrazole)-1,10-phenanthroline (nOct-BPPhen) with structural formula (13), and its synthetic route is as follows Shown:

[0049]

[0050] The preparation process of above-mentioned nOct-BPPhen comprises the following steps:

[0051] (1) Under stirring conditions, add selenium dioxide (5.3g, 48mmol) into a complex solvent composed of 150mL 1,4-dioxane and 10mL water, heat up to reflux, and then dropwise add 2,9- Dimethyl-1,10-phenanthroline in 1,4-dioxane solution [from 2,9-dimethyl-1,10-phenanthroline (5.0g, 24mmol) dissolved in 100mL 1,4-dioxane to obtain], after the dropwise addition, react for 3.0h, then filter while hot, place the obtained filtrate to cool until solid precipitates, and then filter the filtrate to obtain a reddish-brown flocculent solid, namely 2, 9-dicarbaldehyde-1,10-phenanthroline (4.8g, yield 85%);

[0052] (2) Under stirring conditions, add 4.8 g of 2,9-dicarbaldehyde-1,10-phenanthroline ob...

Embodiment 2

[0062] This example prepares 2,9-bis(5-n-butyl-1-hydrogen-pyrazole)-1,10-phenanthroline (nBu-BPPhen) with structural formula (14), and its synthetic route is as follows Shown:

[0063]

[0064] The preparation process of above-mentioned nBu-BPPhen comprises the following steps:

[0065] (1) Under stirring conditions, KMnO 4 (7.6g, 48mmol) was added to 120mL of dichloromethane, heated to reflux, and then a dichloromethane solution of 2,9-dimethyl-1,10-phenanthroline was added dropwise [from 2,9-di Methyl-1,10-phenanthroline (5.0g, 24mmol) was dissolved in 100mL of dichloromethane to obtain], after the dropwise addition was completed, reacted for 4.0h, then filtered while it was hot, and the obtained filtrate was left to cool until solids were precipitated. Then the filtrate was filtered to obtain a reddish-brown flocculent solid, namely 2,9-dicarbaldehyde-1,10-phenanthroline (3.5 g, yield 62%);

[0066] (2) Under stirring conditions, add 3.5 g of 2,9-dicarbaldehyde-1,10-p...

Embodiment 3

[0071] This embodiment prepares 2,9-bis(5-isobutyl-1-hydrogen-pyrazole)-1,10-phenanthroline (iBu-BPPhen) with structural formula (15), and its synthetic route is as follows Shown:

[0072]

[0073] The preparation process of above-mentioned iBu-BPPhen comprises the following steps:

[0074] (1) Under stirring conditions, K 2 Cr 2 o 7 (14g, 48mmol) was added to 150mL tetrahydrofuran, heated to reflux, and then dropwise added a solution of 2,9-dimethyl-1,10-phenanthroline in tetrahydrofuran [from 2,9-dimethyl-1, 10-Phenanthroline (5.0g, 24mmol) was dissolved in 100mL tetrahydrofuran to obtain], after the dropwise addition was completed, reacted for 5.0h, then filtered while it was hot, and the obtained filtrate was left to cool until solids were precipitated, and then filtered the filtrate to obtain red Brown flocculent solid, namely 2,9-dicarbaldehyde-1,10-phenanthroline (4.5 g, yield 80%);

[0075] (2) Under stirring conditions, add 4.5 g of 2,9-dicarbaldehyde-1,10-phena...

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Abstract

The invention discloses a double-pyrazole extracting agent derived from o-phenanthroline with the following structural general formula, and a preparation method and application of the double-pyrazoleextracting agent. In the formula, R is any one selected from n-octyl, n-butyl, isobutyl, ethyl, pyridyl and phenyl. The double-pyrazole extracting agent derived from the o-phenanthroline provided by the invention has a unique rigid structure and an alkyl chain for improving the solubility, and simultaneously only four elements of C, H, O and N are contained, so that the extraction kinetics of a separation extraction system can be greatly increased, the extraction capacity of an organic phase can be increased, secondary pollutants cannot be produced, and thus the environmental protection is facilitated. The extraction agent can be used to separate Ans (actinide elements) / Lns (lanthanide elements), and can not only form a separation extraction system of the Ans / Lns, but also can be used to form a separation reverse extraction system of the Ans / Lns.

Description

technical field [0001] The invention belongs to the technical field of nuclear fuel cycle and nuclear waste treatment, relates to an extraction system for separation of lanthanides / actinides, in particular to a kind of bispyrazole extractant derived from o-phenanthroline, the preparation method of the extractant and its use in Use in lanthanide / actinide separations. Background technique [0002] Spent fuel is spent nuclear fuel that has been exposed to radiation, usually from nuclear reactors in nuclear power plants. The nuclear fuel undergoes fission reaction through neutron bombardment in the reactor, and is discharged from the reactor after a certain period of time. The discharged spent fuel is cooled and processed through the Purex process to recover uranium and plutonium. However, the treated high-level liquid waste (HLLW) still contains long-lived radionuclides, such as 99 Tc, 129 I. Actinides (Ans) and lanthanides (Lns), etc., will pose long-term harm to the ecolo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/04G21F9/12
CPCC07D471/04G21F9/125
Inventor 丁颂东宋莲君刘莹张利荣王志鹏陈志力王学羽杨秀英
Owner SICHUAN UNIV
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