Rare-earth ligand intercalated hydrotalcite with fluorescent property and its preparing method

A technology of rare earth complexes and fluorescence characteristics is applied in the field of rare earth complex intercalation hydrotalcite and its preparation, and can solve the problems of high rare earth ion content, poor light and thermal stability of rare earth complexes, poor dispersibility of rare earth complexes, etc.

Inactive Publication Date: 2006-01-04
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

However, the rare earth complexes prepared by this method have inherent defects of poor light and thermal stability; and the rare ear...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Step A: take by weighing 71.3g Zn(NO 3 )·6(H 2 O) and 45.02g Al(NO 3 )·9(H 2 O) Dissolve in 300ml to remove CO 2 Mixed salt solution was prepared with water, another 25.92g NaOH was dissolved in 300ml to remove CO 2 In water, alkali solution and mixed salt solution are quickly nucleated in a rotating liquid film reactor at room temperature, and the resulting slurry N 2 Crystallized at 100°C for 6h under protection, and the product was centrifuged and washed until neutral; a small amount of sample was taken out and dried at 65°C for 24h for characterization, and Zn 2 Al-NO 3 LDHs, whose Zn 2+ / Al 3+ =2.

[0021] Step B: 7.01g ethylenediaminetetraacetic acid (H 4 C 10 h 12 N 2 o 8 , 0.024mol) solid powder into a three-necked flask multiplied by 200ml of deionized water, heated and boiled for 15min, then added 4.49g (0.006mol) Tb 4 o 7 Solid, continue heating to reflux, add a small amount of NaOH particles into the reactor every 0.5h, until the pH value of t...

Embodiment 2

[0025] Step A: Take the step A method in Example 1 to obtain Mg 2 Al-NO 3 LDHs precursor.

[0026] Step B: According to the method of Step B in Example 1, NaTbEDTA complex was prepared.

[0027] Step C: Take a method similar to step C in Example 1, weigh 8.29g (0.016mol) NaTbEDTA complex and add it to the reactor, and add hot Mg after all the solids are dissolved 2 Al-NO 3 LDHs precursor (5.50g, 0.004mol); After finishing, the pH value of adjusting solution is 8, N 2 Under the protection of 65 ℃ constant temperature 24h. The product uses CO 2 After washing with water and drying at 65° C. for 24 hours, a layered material containing rare earth ions between layers can be obtained.

[0028]According to the X-ray diffraction pattern, Mg 2 The interlayer spacing of Al-TbEDTA LDHs increases from 0.874nm of the precursor to 1.457nm, and the unit cell parameters a corresponding to the characteristic absorption peaks of the two LDHs near 61° at 2θ are both approximately 0.304nm...

Embodiment 3

[0030] Step A: Obtain Zn by step A method in embodiment 1 2 Al-NO 3 LDHs precursor.

[0031] Step B: Take the method similar to Step B in Example 1, 7.76g amine triacetic acid (N(CH 2 -COOH) 3 , referred to as NTA, 0.004mol) solid powder into a three-necked bottle filled with 200ml of water, heated and boiled for 15min, then added 3.52g (0.001mol) Eu 2 o 3 Solid, continue heating to reflux, add a small amount of NaOH particles into the reactor every 0.5h, until the pH value of the reaction solution is 6, and the liquid becomes clear. Filter the solution, heat and concentrate it, then evaporate at room temperature to obtain powdered Na 3 Eu(NTA) 3 ·(H 2 O) Crystals.

[0032] Step C: Weigh 6.43g (0.008mol) Na 3 Eu(NTA) 3 Complex was added to stirring and N 2 In the protected reactor, after all the solids are dissolved, add hot Zn 2 Al-NO 3 LDHs precursor (5.72g, 0.004mol); after the completion, adjust the pH value of the solution to 6, keep the temperature at 65°C...

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Abstract

The present invention provides a kind of RE complex anion intercalated hydrotalcite with fluorescent property and its preparation process. Through ion exchange, the RE complex anion enters to interlamination of the hydrotalcite to constitute laminated material with RE complex anion accounting 40-100 % of the total interlamination anion mole number; and after the RE complex intercalation enter the interlamination of the hydrotalcite, the fluorescent performance may be maintained. The present invention utilizes the intercalating and assembling performance and the laminate controlling and locating effect of laminated hydrotalcite material to assemble RE ion with excellent optical performance into interlamination of the hydrotalcite and to realize the molecule level hybridization of RE ion in interlamination of the hydrotalcite. Through regulating the laminate metal, the present invention prepares organic and inorganic hybridized luminous material with homogeneously distributed RE element and adjustable material grain size.

Description

[0001] Field [0002] The invention belongs to the technical field of rare earth luminescent materials, and in particular provides a rare earth complex intercalation hydrotalcite with fluorescence characteristics and a preparation method thereof. Background technique [0003] Rare earth elements have unique 4f electronic structure, large atomic magnetic moment and strong spin-orbit coupling. Their rich optical, electrical and magnetic properties are widely used in today's industrial production and scientific research. One of the most striking is the luminescent properties of rare earth materials, which have strong absorption capacity and high conversion rate, and can emit spectra from ultraviolet to infrared. [0004] The preparation of rare earth luminescent materials can be divided into two types, one is inorganic functional materials, which have good light, heat and chemical stability (Luo Xixian, Yu Jingjie, Lin Guangxu, Xiao Zhiqiang, Duan Jinxia, ​​Xiao Zhiguo, Luminesce...

Claims

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Application Information

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IPC IPC(8): C09K11/77
Inventor 段雪王连英李仓
Owner BEIJING UNIV OF CHEM TECH
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