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4-diphenyl formate/leuh nanometer complex and synthetic method

A technology of nanocomposites and biphenylformic acid, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of fluorescence quenching and fluorescence intensity that cannot meet industrial needs, achieve high stability, improve energy transfer efficiency, and luminescence The effect of performance enhancement

Inactive Publication Date: 2014-06-25
BEIJING NORMAL UNIVERSITY +1
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Layered europium hydroxide LEuH (the rare earth ion at this time is Eu 3+ ) emits characteristic red light at room temperature, but the Eu 3+ with -OH and H 2 O is directly coordinated and has a fluorescence quenching effect, and the fluorescence intensity cannot meet industrial needs

Method used

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  • 4-diphenyl formate/leuh nanometer complex and synthetic method
  • 4-diphenyl formate/leuh nanometer complex and synthetic method
  • 4-diphenyl formate/leuh nanometer complex and synthetic method

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preparation example Construction

[0045] The synthetic method of above-mentioned 4-biphenylcarboxylate / LEuH nanocomposite, comprises the following steps:

[0046] a) Preparation of Eu(OH) by homogeneous precipitation method 2.5 Cl 0.5 ·nH 2 O: EuCl 3 ·6H 2 O, NaCl and HMT (hexamethylenetetramine) are dissolved in water, where EuCl3 ·6H 2 The molar ratio of O, NaCl and HMT is preferably 0.5-1.5: 10-15: 0.5-1.5, preferably dissolved in exhaust water, which refers to the removal of CO 2 The water can be obtained by boiling distilled water for 5 minutes. The amount of exhaust water is preferably 50mL-100mL / 1mmolEuCl 3 ·6H 2 O. N was then introduced into the solution 2 , after 20min to 40min, the hydrothermal reaction is carried out, the preferred reaction temperature is 90°C to 120°C, and the reaction time is 10h to 12h.

[0047] After the reaction is completed, filter, wash the product with distilled water, and finally dry at room temperature to obtain Eu(OH) 2.5 Cl 0.5 ·nH 2 O, also can be abbreviat...

Embodiment 1

[0052] a) 1mmol EuCl 3 ·6H 2 O, 13mmol NaCl, 1mmol HMT dissolved in 80mL exhaust water, pass through N 2 30min, 90°C hydrothermal reaction for 12h. Then suction filtered, washed with distilled water, and dried at room temperature to obtain Cl-LEuH.

[0053] b) Disperse 0.05g of prepared Cl-LEuH in 80mL of 4-biphenylcarboxylic acid sodium salt solution, which contains 3 times of Cl-LEuH molar excess of 4-biphenylcarboxylic acid, and the molar ratio is 1:0.5 4-diphenylformic acid and NaOH mixed in the system, pH = 8.8. Then it was transferred to a 100mL reactor and reacted with water at 70°C for 40h. Finally, it was filtered, washed with distilled water, and dried at room temperature.

[0054] Please refer to figure 1 , figure 1 XRD (X-ray diffraction, X-ray diffraction) patterns of Cl-LEuH and 4-bibenzoate / LEuH prepared in Example 1 of the present invention. Wherein figure a is the XRD figure of Cl-LEuH, can see 0.87nm, 0.43nm, 0.32nm a series of characteristic diffract...

Embodiment 2

[0059] a) 0.8mmol EuCl 3 ·6H 2 O, 14mmol NaCl, 1.2mmol HMT dissolved in 100mL exhaust water, pass N 2 40min, 100°C hydrothermal reaction for 10h, then suction filtration, washing with distilled water, and drying at room temperature to obtain Cl-LEuH.

[0060] b) Disperse 0.05g of prepared Cl-LEuH in 80mL of 4-biphenylcarboxylic acid sodium salt solution, which contains 3 times of Cl-LEuH molar excess of 4-biphenylcarboxylic acid, and the molar ratio is 1:0.75 4-biphenylformic acid and NaOH mixed in the system, pH = 8.6. Transfer to a 100mL reactor and react with water at 120°C for 24h. Finally, it was filtered, washed with distilled water, and dried at room temperature.

[0061] Please refer to Figure 4 , Figure 4 It is the XRD pattern of Cl-LEuH and 4-bibenzoate / LEuH prepared in Example 2 of the present invention. Wherein figure a is the XRD figure of Cl-LEuH, can see 0.87nm, 0.43nm, 0.32nm a series of characteristic diffraction peaks, peak shape is sharp, the Cl obt...

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Abstract

The invention provides 4-diphenyl formate / LEuH nanometer complex and a synthetic method thereof. The synthetic method comprises the following steps of: a) dissolving EuCl3.6H2O, NaCl and hexamethylenetetramine (HMT) in water, and introducing N2 to perform a hydro-thermal reaction, filtering, washing, and drying to synthesize Eu(OH)2.5Cl0.5.nH2O; and b) adding NaOH into 4-diphenic acid to obtain sodium salt solution of the 4-diphenic acid, dispersing the Eu(OH)2.5Cl0.5.nH2O prepared in the step a) in the sodium salt solution of the 4-diphenic acid to perform the hydro-thermal reaction, and washing and drying, wherein the molar number of the 4-diphenic acid is 3 times that of the Eu(OH)2.5Cl0.5.nH2O. In the synthetic method, 4-diphenyl formate is inserted among LEuH layers to improve the efficiency of energy transfer, the stability of the synthesized 4-diphenyl formate / LEuH nanometer complex is high, and the luminous performance of Eu<3+> is enhanced, so the complex is a lamellate composite material with excellent performance.

Description

technical field [0001] The invention relates to the field of luminescent material synthesis, in particular to a 4-biphenylcarboxylate / LEuH nanocomposite and a synthesis method. Background technique [0002] In recent years, the luminescent properties of layered materials have become a research hotspot in the field of luminescence. Due to its unique electronic configuration, rare earth ions are widely used in magnets, catalysts, luminescent materials, etc., Eu 3+ Due to the characteristic red line spectrum of emission, it is often used to prepare luminescent materials. However, Eu 3+ The molar absorptivity coefficient is very small, the fluorescence quantum yield is low, and the luminescence is weak in aqueous solution. In order to enhance the Eu 3+ Fluorescence intensity, an organic sensitizer can be added to absorb energy from an external light source and transfer it to Eu 3+ . The organic ligands of this type of organic sensitization materials require low excitation e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/06
Inventor 马淑兰楚楠凯孙亚红王娟
Owner BEIJING NORMAL UNIVERSITY
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