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Application of oligomeric aromatic amide compound extractant containing three-center hydrogen bond in separation of Ln/An

The technology of polyaramide and compound is applied in the field of selective separation and extraction agent of rare earth elements, thorium and uranium, which can solve the problems of slow extraction speed, low extraction capacity, weak selectivity, etc., and achieves high phase separation speed and extraction speed. Fast, chemically stable effect

Inactive Publication Date: 2019-05-31
CHONGQING TECH & BUSINESS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims to solve the problems of large consumption, low extraction capacity, weak selectivity and slow extraction speed when the existing extractant selectively separates thorium and uranium from rare earth elements, and provides an oligomeric extractant containing three-center hydrogen bonds. Polyarylamide compound, the present invention uses pre-organization to assemble carbonyl oxygen with coordination into an inner ring, and utilizes a suitable cavity and a certain chelation effect to achieve selective separation of thorium and uranium ions from rare earth elements , as an extractant, it can efficiently and selectively separate thorium and uranium from rare earth ions under relatively acidic conditions

Method used

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  • Application of oligomeric aromatic amide compound extractant containing three-center hydrogen bond in separation of Ln/An
  • Application of oligomeric aromatic amide compound extractant containing three-center hydrogen bond in separation of Ln/An
  • Application of oligomeric aromatic amide compound extractant containing three-center hydrogen bond in separation of Ln/An

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Synthesis reaction 1:

[0024]

[0025] General procedure for the synthesis of trimer diester 4

[0026] Dissolve (1eq.) monoacid (1) in anhydrous CH 2 Cl 2 Add (1.2eq.) oxalyl chloride and 10 μL of anhydrous DMF, heat to reflux until no bubbles are generated, and distill off the solvent under reduced pressure. Then add 2 mL of anhydrous CH 2 Cl 2 , dissolved, and the solvent was distilled off under reduced pressure, and pumped with an oil pump for 20 minutes. with anhydrous CH 2 Cl 2 Dissolved, drop into containing (0.5eq.) diamine (2) and (1.2eq.) Et 3 N CH 2 Cl 2 solution, stirred overnight. After the diamine reaction is complete, drip water into it to quench the reaction, and use saturated NaHCO 3 (aq) and water three times each, anhydrous Na 2 SO 4 Dry, filter, distill off the solvent under reduced pressure, and separate by column chromatography (silica gel).

[0027] General procedure for the synthesis of trimer diacid 5

[0028] Add (1eq.) trime...

Embodiment 2

[0034] Synthesis reaction 2

[0035]

[0036] General procedure for the synthesis of dimer ester 6

[0037] Dissolve (1eq.) monoacid (1) in anhydrous CH 2 Cl 2 Add (1.2eq.) oxalyl chloride and 10 μL of anhydrous DMF, heat to reflux until no bubbles are generated, and distill off the solvent under reduced pressure. Then add 2 mL of anhydrous CH 2 Cl 2 , dissolved, the solvent was distilled off under reduced pressure, and pumped with an oil pump for 20 minutes. with anhydrous CH 2 Cl 2 Dissolved, drop into containing (1eq.) monoamine (3) and (1.2eq.) Et 3 N CH 2 Cl 2 solution, stirred overnight. After the diamine reaction is complete, drip water into it to quench the reaction, and use saturated NaHCO 3 (aq) and water three times each, anhydrous Na 2 SO 4 Dry, filter, distill off the solvent under reduced pressure, wash with ethyl acetate and heavy CH 2 Cl 2 Precipitate can obtain dimer compound 1H NMR (400M Hz, CDCl 3 )δ=9.81(s,1H),9.26(s,1H),8.79(s,1H),6.50(s...

Embodiment 3

[0045] The application of oligo-arylamide compound containing three-center hydrogen bond as extractant in Ln / An separation, the extraction results are shown in Table 1:

[0046] The molar ratio of extractant to rare earth element is 1:1

[0047] The extractant was diluted with dichloromethane to a concentration of 1×10 -3 mol L -1

[0048] The aqueous phase is Ln(NO 3 ) 3 , Th(NO 3 ) 4 and UO 2 (NO 3 ) 2 : 1×10 -4 mol L -1 ; Nitric acid pH: 3.97

[0049] Temperature: 25°C; Phase: 1 / 1; Shaking: 2 hours

[0050] Table 1

[0051]

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Abstract

The invention relates to an application of an oligomeric aromatic amide compound extractant containing a three-center hydrogen bond in separation of Ln / An. The oligomeric aromatic amide compound containing the three-center hydrogen bond is used for selectively separating thorium and uranium in actinide elements from lanthanide elements, and can realize selective separation of uranium from thoriumamong the actinide elements to a certain extent. The oligomeric aromatic amide compound extractant containing the three-center hydrogen bond is single in composition, good in chemical stability, simple in synthesis and easy to obtain, is suitable for industrial production, is small in extractant dosage, and can be used for selective separation Ln / An elements under specific acidity; moreover, the extractant has the advantages of high extraction speed, high phase separation speed and the like; and therefore, an oligomeric aromatic amide compound containing the three-center hydrogen bond which isused for selectively extracting and separating the actinide elements from the lanthanide elements has good economic benefits and practical application prospects.

Description

technical field [0001] The present invention relates to a class of oligo-arylamide compounds and their applications. Specifically, the present invention relates to a kind of oligo-arylamide compounds and their applications using three-center hydrogen bonds to fix the structural framework, which belongs to rare earth elements and thorium (Th) and The technical field of extraction agent for selective separation of uranium (U). Background technique [0002] The energy issue is one of the most serious challenges facing the world today. Compared with other energy sources, nuclear energy has great advantages such as high efficiency, cleanliness, and high energy. However, as a "double-edged sword", how to deal with the nuclear energy process safely and efficiently The high level liquid waste (HLLW) produced in the environment is related to the sustainable development of energy. The actinides in high-level radioactive waste (HLLW) have a long half-life and high radioactivity. At pr...

Claims

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Application Information

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IPC IPC(8): C22B3/28C22B59/00C22B60/02
Inventor 池哲鑫陈盛明姜春雪闵燕周江林
Owner CHONGQING TECH & BUSINESS UNIV