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.
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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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