Preparation method of polyacid rare earth ion complex with slow magnetic relaxation behavior

A technology of rare earth ions and magnetic relaxation, which is applied in organic chemistry and other fields, can solve the problems of slow magnetic relaxation, and achieve the effects of good repeatability, high yield and stable preparation method

Inactive Publication Date: 2013-03-06
NORTHEAST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the influence of symmetry and intermolecular interactions of magnetic memory units, only three types of rare earth single-ion complexes have observed slow magnetic relaxation behavior.

Method used

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  • Preparation method of polyacid rare earth ion complex with slow magnetic relaxation behavior
  • Preparation method of polyacid rare earth ion complex with slow magnetic relaxation behavior
  • Preparation method of polyacid rare earth ion complex with slow magnetic relaxation behavior

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) NdPMo 12 o 40 ·nH 2 The preparation of O: the α-H 3 PMo 12 o 40 14H 2 O (410mg, 0.2mmol) and NdCl 3 ·6H 2 O (80mg, 0.2mmol) was dissolved in a small beaker containing 20mL of water, stirred, heated, and the solvent was evaporated until light yellow crystals were precipitated, then cooled. The yield was 65% (calculated as Mo).

[0024] (2) Preparation of 4,4'-dimethyl-2,2'-bipyridine-N-N'-dioxide (bpyno for short): 4,4-dimethyl-2,2-bipyridine (5.4 g, 25mmol), glacial acetic acid (10mL) and 35% aqueous hydrogen peroxide (10mL) were placed in a three-necked flask equipped with a reflux condenser, and heated in a water bath at 70-80°C for 3 hours. Thereafter, 35% aqueous hydrogen peroxide (7.5 mL) was added to the reaction system, and heating was continued for 9 hours. After cooling, acetone (75 mL) was added to obtain a pale yellow precipitate, which was filtered with suction and washed twice with acetone. The product was dried in vacuum and the yield was 58...

Embodiment 2

[0027] (1) SmPMo 12 o 40 ·nH 2 The preparation of O: the α-H 3 PMo 12 o 40 14H 2 O (410mg, 0.2mmol) and SmCl 3 ·6H 2 O (80mg, 0.2mmol) was dissolved in a small beaker containing 20mL of water, stirred, heated, and the solvent was evaporated until light yellow crystals were precipitated, then cooled. The yield was 65% (calculated as Mo).

[0028] (2) Preparation of 4,4'-dimethyl-2,2'-bipyridine-N-N'-dioxide (bpyno for short): 4,4-dimethyl-2,2-bipyridine (5.4 g, 25mmol), glacial acetic acid (10mL) and 35% aqueous hydrogen peroxide (10mL) were placed in a three-necked flask equipped with a reflux condenser, and heated in a water bath at 70-80°C for 3 hours. Thereafter, 35% aqueous hydrogen peroxide (7.5 mL) was added to the reaction system, and heating was continued for 9 hours. After cooling, acetone (75 mL) was added to obtain a pale yellow precipitate, which was filtered with suction and washed twice with acetone. The product was dried in vacuum and the yield was 58...

Embodiment 3

[0031] (1) EuPMo 12 o 40 ·nH 2 The preparation of O: the α-H 3 PMo 12 o 40 14H 2 O (410mg, 0.2mmol) and EuCl 3 ·6H 2 O (80mg, 0.2mmol) was dissolved in a small beaker containing 20mL of water, stirred, heated, and the solvent was evaporated until light yellow crystals were precipitated, then cooled. The yield was 65% (calculated as Mo).

[0032] (2) Preparation of 4,4'-dimethyl-2,2'-bipyridine-N-N'-dioxide (bpyno for short): 4,4-dimethyl-2,2-bipyridine (5.4 g, 25mmol), glacial acetic acid (10mL) and 35% aqueous hydrogen peroxide (10mL) were placed in a three-necked flask equipped with a reflux condenser, and heated in a water bath at 70-80°C for 3 hours. Thereafter, 35% aqueous hydrogen peroxide (7.5 mL) was added to the reaction system, and heating was continued for 9 hours. After cooling, acetone (75 mL) was added to obtain a pale yellow precipitate, which was filtered with suction and washed twice with acetone. The product was dried in vacuum and the yield was 58...

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Abstract

The invention discloses a preparation method of polyacid rare earth ion complex with slow magnetic relaxation behavior. The method comprises the steps of: (1) dissolving alpha-H3PMo12O40.14H2O and LnCl3.6H2O in water according to a certain proportion, heating, stirring and volatilizing the solution to obtain a pale yellow crystal LnPMo12O40.nH2O; (2) reacting the aqueous solution mixture of 4,4-dimethyl-2,2-dipyridyl, glacial acetic acid and hydrogen peroxide for 12-24h under hot water bath, cooling and adding acetone to obtain a pale yellow solid 4,4'-dimethyl-2,2'-dipyridyl-N-N'-dioxide; and (3) performing a slow self-assembled reaction on 4,4'-dimethyl-2,2'-dipyridyl-N-N'-dioxide and the LnPMo12O40.nH2O through a slow diffusion method to obtain the final product is [Ln(bpyno)4][PMo12O40].2H2O. The novel polyacid rare earth complex with slow magnetic relaxation behavior is prepared by the induction of polyacid anions with nanometer sizes, high symmetry and high negative charges; and the preparation method disclosed by the invention is stable, high in yield, good in repeatability and is suitable for actual operations.

Description

technical field [0001] The invention relates to the preparation of a single-molecule magnet with slow magnetic relaxation behavior applicable to magnetic storage devices, in particular to a preparation method of a multi-acid-based rare earth ion complex with slow relaxation behavior. Background technique [0002] Since the beginning of the 21st century, people have higher and higher requirements for digital information processing and storage, hoping for faster information processing speed and higher digital information storage density. The usual strategy is to make the size of the existing magnetic memory unit (ie, magnetic nanoparticles) smaller and smaller to meet the above requirements. However, as the particle size continues to decrease, the magnetic memory cell will lose its magnetic energy barrier due to domain wall motion and other reasons, and then lose its storage function. This urgently requires people to discover new materials and new technologies to replace trad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F19/00
Inventor 李阳光周文喆唐金魁王永慧冯小佳王鑫郝秀丽
Owner NORTHEAST NORMAL UNIVERSITY
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