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Rare earth-N, N'-(2-hydroxy-3-methoxybenzene methyl) ethylene diamine complex single crystal and preparation thereof

A technology of methoxybenzyl and complexes, which is applied in the field of single crystal compounds and their preparation, can solve the problems of inaccurately judging the real structure of powder complexes, achieve clear composition and molecular structure, and require low experimental equipment , The effect of simple process

Inactive Publication Date: 2012-05-09
HUAIHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For solid powder rare earth complexes, the structure is often characterized by means of elemental analysis, nuclear magnetic resonance, mass spectrometry, infrared spectroscopy, etc., but these means cannot accurately determine the real structure of the powder complexes. For crystals, X-single crystal Diffractometer measurement and analysis to obtain the real structure of the complex, thus truly reflecting the weak interaction between the complex molecules and the two-dimensional or three-dimensional supramolecular structure, which is of great significance for the study of the properties and mechanism of the complex

Method used

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  • Rare earth-N, N'-(2-hydroxy-3-methoxybenzene methyl) ethylene diamine complex single crystal and preparation thereof
  • Rare earth-N, N'-(2-hydroxy-3-methoxybenzene methyl) ethylene diamine complex single crystal and preparation thereof
  • Rare earth-N, N'-(2-hydroxy-3-methoxybenzene methyl) ethylene diamine complex single crystal and preparation thereof

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Experimental program
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Effect test

Embodiment 1

[0023] Example 1. Rare earth-N, N'-(2-hydroxy-3-methoxybenzyl) ethylenediamine complex single crystal is characterized in that its crystal structure is as follows figure 1 shown. Among them: Ln represents the rare earth ion Tb 3+ , Pr 3+ , Er 3+ . When Ln is rare earth ion Pr 3+ , the unit cell parameters of the complex are: orthorhombic crystal system, space group Iba2, α=β=γ=90°, the space is packed into a three-dimensional network; when Ln is a rare earth ion Tb 3+ When , the unit cell parameters of the single crystal of the complex are: orthorhombic crystal system, space group Iba2, α=β=γ=90°, the space is packed into a three-dimensional network; when Ln is a rare earth ion Er 3+ , the unit cell parameters of the single crystal of the complex are: orthorhombic system, space group Iba2, α=β=γ=90°, the space is packed into a three-dimensional network.

Embodiment 2

[0024] Example 2. A kind of rare earth-N as described in embodiment 1, the preparation method of N '-(2-hydroxyl-3-methoxybenzyl) ethylenediamine complex single crystal, first rare earth ion Tb 3+ or Pr 3+ or Er 3+ Soluble in ethanol, then add N,N'-(2-hydroxy-3-methoxybenzyl)ethylenediamine to react, and the rare earth ion and N,N'-(2-hydroxy-3-form The ratio of the amount of oxybenzyl) ethylenediamine substance is 2:1.

Embodiment 3

[0025] Example 3. refer to figure 1 , 2 . N,N'-(2-hydroxy-3-methoxybenzyl)ethylenediamine praseodymium (III) complexes. Its preparation method steps are as follows:

[0026] 0.355g (1mmol) PrCl 3 ·6H 2 Dissolve O in 10ml of ethanol, weigh 0.48g (2mmol) of N,N'-(2-hydroxy-3-methoxybenzyl)ethylenediamine and dissolve in 10ml of ethanol, mix and react for 2h, filter , The brown-red crystals precipitated out after the solution was left for a few weeks. IR (KBr, cm -1 ): 3258, 2946, 2858, 1572, 1477, 1385, 1292, 1234, 1076, 947, 845, 733, 533. Elemental Analysis, C 36 h 45 N 4 o 8 Pr: Calculated for C53.75; H5.65; N6.98. The measured values ​​are C53.61; H5.54; N6.88. X-diffraction single crystal structure picture figure 1 shown. The crystallographic data are listed in Table 1.

[0027] Table 1 Crystallographic data of the complexes

[0028]

[0029]

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Abstract

The invention discloses a rare earth-N,N'-(2-hydroxyl-3-methoxyl benzyl)ethylenediamine complex single crystal. The invention also discloses a method for preparing the rare earth-N,N'-(2-hydroxyl-3-methoxyl benzyl)ethylenediamine complex single crystal, which is characterized in that rare earth ions, namely Tb<3+> or Pr<3+> or Er<3+>, are dissolved in ethanol first, and N,N'-(2-hydroxyl-3-methoxyl benzyl)ethylenediamine is added into the mixture for reaction, wherein the mass ratio of the rare earth ions to the N,N'-(2-hydroxyl-3-methoxyl benzyl)ethylenediamine is 2:1. The method for preparing the complex single crystal has simple technique and low requirements on experimental equipment, and a prepared complex has definite compositions and molecular structure.

Description

technical field [0001] The invention relates to a single crystal compound and a preparation method thereof, in particular to a preparation method and structure of a rare earth-N,N'-(2-hydroxyl-3-methoxybenzyl)ethylenediamine complex single crystal. Background technique [0002] Rare earth elements are abundant elements in my country. The electronic layer structure of rare earth elements differs from other elements in the periodic table in that except for the rare earth elements ytterbium, lutetium, nulium, and rhodium, the number of electrons in the 4f electron layer of other rare earth elements is less than 14. Filled state, this special electron arrangement structure makes rare earth have a series of special physical and chemical characteristics, especially when rare earth is combined with other substances, it shows excellent characteristics and functions that people did not expect. In recent years, it has been found that rare earth complexes not only have unique fluorescen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/58C07C213/08C07F5/00
Inventor 刘玉芬夏海涛
Owner HUAIHAI INST OF TECH
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