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A kind of rare earth lanthanum complex and its synthesis method

A synthesis method and complex technology, applied in the field of rare earth lanthanum complexes and their synthesis, to achieve the effects of simple synthesis method, mild reaction conditions, and high purity

Inactive Publication Date: 2016-05-04
BEIJING NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, in the prior art, there is no report on the synthesis of complexes using carboxylic acid-substituted tetraaza-18-crown-6 and rare earth lanthanum ions

Method used

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  • A kind of rare earth lanthanum complex and its synthesis method
  • A kind of rare earth lanthanum complex and its synthesis method
  • A kind of rare earth lanthanum complex and its synthesis method

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preparation example Construction

[0040] The preparation method of the above-mentioned rare earth lanthanum complex may include:

[0041]1) Synthesis of 4,7,13,16-tetracarboxymethyl-1,10-dioxo-4,7,13,16-tetraazacycloctadecane, referred to as L, the synthesis route is as follows:

[0042]

[0043] The synthesis method is: dissolving 1,10-dioxo-4,7,13,16-tetraaza-18-crown-6 in CH 2 Cl 2 Finally, add anhydrous potassium carbonate, heat to reflux for 0.5-3h, add ethyl bromoacetate and then heat to reflux for 18-24 hours, filter and evaporate to obtain an oily substance; among them, ethyl bromoacetate and 1,10-dioxo- The molar ratio of 4,7,13,16-tetraza-18-crown-6 is preferably 4-7; CH 2 Cl 2 The ratio of volume to 1,10-dioxo-4,7,13,16-tetraza-18-crown-6 moles is preferably 10L / mol-20L / mol; anhydrous potassium carbonate and 1,10-di The molar ratio of oxygen-4,7,13,16-tetraaza-18-crown-6 is preferably 4-8.

[0044] Mix the above oil with hydrochloric acid aqueous solution to obtain a mixed solution, heat the...

Embodiment 1

[0070] Weigh 0.52g (2mmol) of 1,10-dioxo-4,7,13,16-tetraza-18-crown-6 in a 50mL round bottom flask,

[0071] Add 20mL CH 2 Cl 2 As a solvent, add 1.2g (8.8mmol) of anhydrous potassium carbonate, reflux for 3h, then add 0.92mL (8.4mmol) of ethyl bromoacetate, reflux for 24h under normal pressure, filter, and rotate the filtrate to obtain 1.0 g of oil.

[0072] by HCl:H 2 The volume ratio of O=1.5:1 prepares hydrochloric acid aqueous solution, the obtained oil is mixed with hydrochloric acid aqueous solution (20mL) to obtain a mixed solution, which is refluxed at normal pressure for 24 hours and then filtered to obtain a filtrate. The filtrate was evaporated to about 10ml, and the hydrochloride crystals of Ligand L precipitated out. The crystals were collected by filtration and dried at room temperature to obtain 0.9gL, whose M.p.>300°C.

[0073] Weigh 0.128g (0.2mmol) of Ligand L into a 50mL beaker, add 20mL of absolute ethanol, and stir to form a suspension of Ligand L. W...

Embodiment 2

[0075] Weigh 0.78g (3mmol) of 1,10-dioxo-4,7,13,16-tetraza-18-crown-6 in a 50mL round bottom flask,

[0076] Add 45mLCH 2 Cl 2 As a solvent, add 2.5g (18mmol) of anhydrous potassium carbonate, reflux for 1.5h, then add 1.96mL (18mmol) of ethyl bromoacetate, reflux for 20h, filter, and rotate the filtrate to obtain 1.4g of oil .

[0077] by HCl:H 2 Aqueous hydrochloric acid was prepared at a volume ratio of O=2:1, and the resulting oil was mixed with aqueous hydrochloric acid (25mL) to obtain a mixed solution, which was refluxed at normal pressure for 18 hours and then filtered to obtain a filtrate, which was evaporated To about 12ml, the hydrochloride crystals of Ligand L were precipitated, and the crystals were collected by filtration and dried in air at room temperature to obtain 1.4gL, whose M.p.>300°C.

[0078] Weigh 0.192g (0.3mmol) of Ligand L into a 50mL beaker, add 25mL of absolute ethanol, and stir to form a suspension of Ligand L. Weigh 0.096g (2.4mmol) of NaOH,...

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Abstract

The embodiment of the invention discloses a rare earth lanthanum complex and a synthetic method thereof. The method comprises the following steps: dispersing ligands L in ethyl alcohol to form a suspension liquid of the ligands L; adding NaOH into the suspension liquid of the ligands L, and adding water to the suspension liquid of the ligands L with NaOH until the turbid suspension liquid becomes transparent to generate a solution of L, wherein the mole ratio of NaOH to the compound L is 7-9; dissolving La(NO3)3.6H2O into ethyl alcohol to form an ethyl alcohol solution of the La(NO3)3.6H2O, and adding the ethyl alcohol solution of the La(NO3)3.6H2O into the solution of the ligands L to generate a mixed solution of the rare earth lanthanum complex, wherein the ratio of the mole number of the La(NO3)3.6H2O to the volume of ethyl alcohol is 0.025-0.030 mol / L; performing evaporative crystallization on the mixed solution of the rare earth lanthanum complex, then filtering and drying to obtain single crystals of the rare earth lanthanum complex. The synthetic method of the rare earth lanthanum complex provided by the invention is simple and easy, the reaction condition is mild, and the synthetic rare earth lanthanum complex is high in purity.

Description

technical field [0001] The invention relates to the field of compound synthesis, in particular to a rare earth lanthanum complex and a synthesis method thereof. Background technique [0002] The research on rare earth lanthanum complexes has always attracted people's attention. Due to the unique 4f electronic structure of lanthanum and the interaction with organic ligands, further modification can improve its characteristics, so rare earth lanthanum compounds can be widely used in rare earth separation, medicine and other fields. Among the many ligands of rare earth lanthanum complexes, crown ether compounds are very important. Rare earth lanthanum and crown ether compounds form complexes, which are widely used, for example, as selective reagents for lanthanide ions and antidotes for heavy metals. [0003] Nitrogen lariat crown ether, also known as arm crown ether, is formed by introducing a side chain group into aza crown ether. [0004] The hydrogen on the nitrogen atom...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F19/00
Inventor 马淑兰苏飞飞潘军军韦燕鹏
Owner BEIJING NORMAL UNIVERSITY