Method for preparing micro-capsule containing high light-effect rare earth compounding matter

Abstract

A process for preparing the RE match microcapsules with high optical effect includes such steps as choosing a main luminous body from Eu(III) beta-biketone matches Eu(acac)3Phen, Eu(TFA)3Phen, Eu(HFA)3Phen, Eu(TTA)3Phen, Eu(DBM)3Phen and Eu(PTA)3Phen, preparing the solid microcapsule whose shell layer contains said RE matches, and preparing the hollow microcapsules whose shell contains RE matches by dissolving the central core.

Description

technical field

[0001] The invention relates to a method for preparing microcapsules containing rare earth complexes with high light efficiency, in particular to a method for preparing solid microcapsules and hollow microcapsules containing rare earth complexes with high light efficiency with a stable core-shell structure by using assembly technology at the molecular level new technology. Background technique

[0002] The luminescence of rare earth complexes has the characteristics of high luminescence intensity of organic dyes and good monochromaticity of luminescence of rare earth ions. It has a large absorption coefficient for ultraviolet light and can efficiently transfer energy to rare earth ions. The dye molecules have luminescence peaks spanning tens of nanometers or even hundreds of nanometers. Therefore, rare earth complexes have an absolute advantage in luminescent monochromaticity over dyes, and are ideal luminescent substances for observing clear images of red,...

Examples

Embodiment 1

[0050] Embodiment 1. The preparation method of rare earth complex microcapsules containing high light efficiency, the steps are as follows:

[0051] (1) Select Europium(III) β-diketone complex Eu(DBM) 3 Phen;

[0052] (2) join the sodium chloride aqueous solution that concentration is 30mg / ml;

[0053] (3) With step (2) solution as solvent, select the anionic polyelectrolyte polystyrene sulfonate (PSS) that molecular weight is 70,000, mix its concentration and be the solution of 2.0mg / ml;

[0054] (4) select the cationic polyelectrolyte polyallyl ammonium chloride (PAH) that molecular weight is 70,000, take step (2) solution as solvent, mix its concentration and be the solution of 2.0mg / ml;

[0055] (5) by Eu(DBM) 3 Phen and PSS mass ratio are 1: 2 mixing the solution that step (1) obtains and the solution that step (3) obtains;

[0056] (6) by Eu(DBM) 3 Phen and PAH mass ratio are 1: 2 mixing the solution that step (1) obtains and the solution that step (4) obtains;

[...

Embodiment 2

[0066] Embodiment 2. The preparation method of rare earth complex microcapsules containing high light efficiency, the steps are as follows:

[0067] (1) Selection of rare earth complexes Eu(DBM) 3 Phen; with reference to embodiment 1 step (1)-(9) method, use MnCO 3 As template microspheres, make each milliliter solution contain 2.0×10 8 Microcapsules were deposited for 600 seconds, centrifuged at 3000rps for 600 seconds, and washed 3 times in ultrapure water to prepare Eu(DBM) 3 Solid Microcapsules of Phen {MnCO 3 [(Eu(DBM) 3 Phen / PAH)(Eu(DBM) 3 Phen / PSS)] 4} and hollow microcapsules [(Eu(DBM) 3 Phen / PAH)(Eu(DBM) 3 Phen / PSS)] 4 ;

[0068] (2) Containing Eu(DBM) 3 The microcapsule film of Phen is complete and the structure is intact; the fluorescence performance of the microcapsule is excellent, and only one layer of Eu(DBM) is deposited in the shell 3 When Phen, the microcapsules emit light visible to the naked eye under the excitation of ultraviolet light; hollow E...

Embodiment 3

[0069] Example 3. The preparation method of microcapsules containing rare earth complexes with high light efficiency, the steps are as follows:

[0070] (1) Select the rare earth complex Eu(TTA) 3 Phen; with reference to embodiment 1 step (1)-(9) method, make every milliliter solution contain 5.0 * 10 7 Microcapsules were deposited for 600 seconds, centrifuged at 3000rps for 600 seconds, washed 3 times in ultrapure water, and prepared containing Eu(TTA) 3 Phen Solid Microcapsules {MF[(Eu(TTA) 3 Phen / PSS)(Eu(TTA) 3 Phen / PAH)] 4} and hollow microcapsules [(Eu(TTA) 3 Phen / PSS)(Eu(TTA) 3 Phen / PAH)] 4 ;

[0071] (2) Containing Eu(TTA) 3 The microcapsule film of Phen is complete and the structure is intact; the fluorescence performance of the microcapsule is excellent, and only one layer of Eu(TTA) is deposited in the shell 3 When Phen, the microcapsules emit light visible to the naked eye under the excitation of ultraviolet light; the hollow Eu(TTA) 3 The fluorescent emis...

technical field

[0001] The invention relates to a method for preparing microcapsules containing rare earth complexes with high light efficiency, in particular to a method for preparing solid microcapsules and hollow microcapsules containing rare earth complexes with high light efficiency with a stable core-shell structure by using assembly technology at the molecular level new technology. Background technique

[0002] The luminescence of rare earth complexes has the characteristics of high luminescence intensity of organic dyes and good monochromaticity of luminescence of rare earth ions. It has a large absorption coefficient for ultraviolet light and can efficiently transfer energy to rare earth ions. The dye molecules have luminescence peaks spanning tens of nanometers or even hundreds of nanometers. Therefore, rare earth complexes have an absolute advantage in luminescent monochromaticity over dyes, and are ideal luminescent substances for observing clear images of red,...

Examples

Embodiment 1

[0050] Embodiment 1. The preparation method of rare earth complex microcapsules containing high light efficiency, the steps are as follows:

[0051] (1) Select Europium(III) β-diketone complex Eu(DBM) 3 Phen;

[0052] (2) join the sodium chloride aqueous solution that concentration is 30mg / ml;

[0053] (3) With step (2) solution as solvent, select the anionic polyelectrolyte polystyrene sulfonate (PSS) that molecular weight is 70,000, mix its concentration and be the solution of 2.0mg / ml;

[0054] (4) select the cationic polyelectrolyte polyallyl ammonium chloride (PAH) that molecular weight is 70,000, take step (2) solution as solvent, mix its concentration and be the solution of 2.0mg / ml;

[0055] (5) by Eu(DBM) 3 Phen and PSS mass ratio are 1: 2 mixing the solution that step (1) obtains and the solution that step (3) obtains;

[0056] (6) by Eu(DBM) 3 Phen and PAH mass ratio are 1: 2 mixing the solution that step (1) obtains and the solution that step (4) obtains;

[...

Embodiment 2

[0066] Embodiment 2. The preparation method of rare earth complex microcapsules containing high light efficiency, the steps are as follows:

[0067] (1) Selection of rare earth complexes Eu(DBM) 3 Phen; with reference to embodiment 1 step (1)-(9) method, use MnCO 3 As template microspheres, make each milliliter solution contain 2.0×10 8 Microcapsules were deposited for 600 seconds, centrifuged at 3000rps for 600 seconds, and washed 3 times in ultrapure water to prepare Eu(DBM) 3 Solid Microcapsules of Phen {MnCO 3 [(Eu(DBM) 3 Phen / PAH)(Eu(DBM) 3 Phen / PSS)] 4} and hollow microcapsules [(Eu(DBM) 3 Phen / PAH)(Eu(DBM) 3 Phen / PSS)] 4 ;

[0068] (2) Containing Eu(DBM) 3 The microcapsule film of Phen is complete and the structure is intact; the fluorescence performance of the microcapsule is excellent, and only one layer of Eu(DBM) is deposited in the shell 3 When Phen, the microcapsules emit light visible to the naked eye under the excitation of ultraviolet light; hollow E...

Embodiment 3

[0069] Example 3. The preparation method of microcapsules containing rare earth complexes with high light efficiency, the steps are as follows:

[0070] (1) Select the rare earth complex Eu(TTA) 3 Phen; with reference to embodiment 1 step (1)-(9) method, make every milliliter solution contain 5.0 * 10 7 Microcapsules were deposited for 600 seconds, centrifuged at 3000rps for 600 seconds, washed 3 times in ultrapure water, and prepared containing Eu(TTA) 3 Phen Solid Microcapsules {MF[(Eu(TTA) 3 Phen / PSS)(Eu(TTA) 3 Phen / PAH)] 4} and hollow microcapsules [(Eu(TTA) 3 Phen / PSS)(Eu(TTA) 3 Phen / PAH)] 4 ;

[0071] (2) Containing Eu(TTA) 3 The microcapsule film of Phen is complete and the structure is intact; the fluorescence performance of the microcapsule is excellent, and only one layer of Eu(TTA) is deposited in the shell 3 When Phen, the microcapsules emit light visible to the naked eye under the excitation of ultraviolet light; the hollow Eu(TTA) 3 The fluorescent emis...

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