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Eu(III)-Fe(II) luminous nano-tube and its preparation method and use

A technology of nanotubes and luminescent materials, applied in the application field of biomolecular recognition, can solve the problems of scarcity of three-dimensional structures, difficulty in selecting ligands, and difficulty in predicting and controlling products.

Inactive Publication Date: 2008-01-09
NANKAI UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, so far, there are few reports about rare earth-transition mixed metal coordination polymers in the literature, and the three-dimensional structure is particularly rare [P.Cheng et al., Angew.Chem.Int.Ed., 934, 42, 2003 ; P. Cheng et al., J. Am. Chem. Soc., 126, 3012, 2004]
The reason why there are few reports on the structures of rare earth-transition mixed metal coordination polymers is that the following challenges are faced in the synthesis of such compounds: a) The high coordination number of rare earth ions makes it difficult to predict and control the products
In addition, it is also easy to make the formed lattice interpenetrate with each other, so it is difficult to observe the effective pore structure in the product; b) the competition reaction between rare earth and transition metal ions and the same ligand often leads to the product containing only one kind of metal instead of The designed mixed metal; c) It is difficult to choose a ligand with a good match in rigidity and coordination ability, because the rigidity and coordination ability of the ligand are also crucial to the topology of the polymer
[0003] On the other hand, the 4f orbital of rare earth ions belongs to the inner orbital, affected by the shielding effect, the impact of this change on the chemical properties of rare earth elements is very small, resulting in the similarity of the chemical properties of rare earth elements, but this The similarity in chemical properties cannot conceal the spectroscopic and applied individuality of these elements

Method used

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  • Eu(III)-Fe(II) luminous nano-tube and its preparation method and use
  • Eu(III)-Fe(II) luminous nano-tube and its preparation method and use
  • Eu(III)-Fe(II) luminous nano-tube and its preparation method and use

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preparation example Construction

[0024] The preparation method of the present invention comprises the following steps:

[0025] 1) Eu 2 o 3 , FeSO 4 ·7H 2 O and PDA are mixed in a molar ratio of 1:3~4:5.5~6, put into the polytetrafluoroethylene liner of the hydrothermal reaction kettle, and first add 4-6mL CH 3 CN, followed by the rapid addition of 7-9 mL H 2 O, without stirring, in case Fe 2+ It is oxidized and sealed tightly with a stainless steel sleeve.

[0026] 2) Rapidly raise the temperature to a high temperature of 145-155° C., and keep the temperature constant for 70-72 hours.

[0027] 3) Cool down to room temperature at a rate of 0.5-1° C. / hour, filter, and wash twice with deionized water to obtain dark red polyhedral prism crystals suitable for single crystal diffraction.

Embodiment 1

[0028] Embodiment 1 [Eu(PDA) 3 Fe 1.5 (H 2 O) 3 ]·1.5H 2 Synthesis of O:

[0029] 0.2mmol Eu 2 o 3 (0.070g), 0.6mmol FeSO 4 ·7H 2 O (0.167g), 1.2mmol PDA (0.200g) mixture, put into the polytetrafluoroethylene liner of 20mL hydrothermal reaction kettle, add 4mLCH first 3 CN, followed by the rapid addition of 8mL H 2 O, without stirring, in case Fe 2+ After being oxidized and sealed tightly with a stainless steel sleeve, the temperature was quickly raised to a high temperature of 150°C, and after a constant temperature of 72 hours, the temperature was programmed to cool down to room temperature. The obtained product was washed twice with 5mL water, and finally a deep red polyhedral prism suitable for single crystal diffraction was selected. shaped crystals. The calculated yield based on metal Eu was 65%.

Embodiment 2

[0030] Embodiment 2 [Eu(PDA) 3 Fe 1. 5(H 2 O) 3 ]·1.5H 2 Characterization of O:

[0031] (1) [Eu(PDA) 3 Fe 1.5 (H 2 O) 3 ]·1.5H 2 Structure determination of O

[0032] The crystal structure was determined using BRUKER SMART 1000 X-ray diffractometer, using graphite monochromatized Mokα rays (λ=0.71073 Ȧ) as the incident radiation, collecting diffraction points by ω-φ scanning, and correcting the unit cell by least square method Parameters, the crystal structure was obtained from the difference Fourier electron density map using the SHELXL-97 direct method, and was corrected by Lorentz and polarization effects. All H atoms were synthesized by difference Fourier and determined by ideal position calculation. The detailed crystal determination data are shown in Table 1. The structure is shown in Figure 1 and Figure 2.

[0033] Table 1 [Eu(PDA) 3 Fe 1.5 (H 2 O) 3 ]·1.5H 2 Crystallographic data for O

[0034] Empirical formula

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Abstract

An Eu(III)-Fe(II) luminescent nanometer tube, its production and use are disclosed. The structural formula is (Eu(PDA)3Fe1.5(H2O)3).1.5H2O, PDA=2, 6-pyridine diacid ligand. MgC12 is added into N,N'-dimethyl-methane amide solution, transmitting-peak strength is increased with Mg2+ ion concentration increasing. It has stable three-dimensional nanometer tubular structure; it can be used as Mg2+ ion fluorescent mark and used for biological molecular discrimination.

Description

【Technical field】 [0001] The present invention relates to the preparation method of nano-luminescent material, especially a kind of Eu(III)-Fe(II) luminescent nano-tube with stable three-dimensional nano-tubular structure, and can be used as fluorescent label of magnesium ion and its preparation method and biomolecule recognition applications. 【Background technique】 [0002] In recent years, the research on rare earth-transition mixed metal coordination polymers has opened up a new field for exploring new multifunctional materials such as catalysis, adsorption, fluorescent labeling, and magnetic storage. However, so far, there are few reports on rare earth-transition mixed metal coordination polymers in the literature, and the three-dimensional structure is particularly rare [P.Cheng et al., Angew.Chem.Int.Ed., 934, 42, 2003 ; P. Cheng et al., J. Am. Chem. Soc., 126, 3012, 2004]. The reason why the structures of rare earth-transition mixed metal coordination polymers are r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06G01N33/52
Inventor 程鹏赵斌
Owner NANKAI UNIV
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