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Preparation method of fluorescent rare earth complex modified nanometer silicon-aluminum emulsion

A rare earth complex and nano-silicon technology, which is applied in chemical instruments and methods, dyed organic silicon compound treatment, dyed low-molecular-weight organic compound treatment, etc. , the effect of strong fluorescence intensity and uniform particle size

Active Publication Date: 2015-05-27
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above publications all mention nano fluorescent materials, they do not involve modified nano silicon-aluminum emulsions.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0033] 1.1.2 Nano Al 2 o 3 Preparation of emulsion:

[0034] Mix 27g-40.5g of double distilled water (adjusted between 0.1-1.5 moles of aluminum isopropoxide), 0.003g-0.3g of acetic anhydride (0.2%-2% of the mass of isopropanol), 0.075g-0.15g of carbonic acid Diethyl ester (5%-10% of the mass of isopropanol) is ultrasonically mixed in 10mL of ethyl acetate (or toluene), ready for use; the mass is not more than 1.5 grams of aluminum isopropoxide and it is made by adding 10 grams of isopropanol solution, and then added dropwise to the above solution (the concentration of aluminum isopropoxide is not more than 15%). The reaction temperature is 180°C-220°C to obtain modified nano-Al 2 o 3 Lotion;

[0035] 1.1.3 Nano-Al prepared in step 2 2 o 3 The emulsion was added to the modified nano-SiO prepared in step 1 2 Emulsion, ratio range: partially hydrolyzed silicon emulsion: modified nano-Al 2 o 3 Emulsion=4:1-20:1 (mass ratio), add isopropanol 0.8-1.2 times the mass of par...

specific Embodiment approach

[0040] 1) Preparation of modified silicon partial hydrolyzate

[0041] Put 40 grams of ethyl orthosilicate, 18 grams of tetra-n-butyl zirconium (or 40 grams of ethyl orthosilicate and 18 grams of tetra-n-butyl zirconium and 18 grams of tributyl phosphate) in ethyl acetate (or toluene) Mix well, add 0.8 g of formic acid, add 100 mL of double distilled water dropwise, add dropwise for 120 minutes, stir ultrasonically for 6 hours, and react at a temperature of 150°C-240°C to obtain a partially hydrolyzed nano-silica emulsion, which is ready for use;

[0042] 2) Nano Al 2 o 3 Preparation of emulsion:

[0043] Mix 27 grams of twice-distilled water, 0.3 grams of acetic anhydride, and 18 grams of diethyl carbonate in 10 mL of ethyl acetate (or toluene) by ultrasonic mixing, and set aside; add 1.5 grams of aluminum isopropoxide to 10 grams of isopropanol to prepare into a solution, and then added dropwise to the ethyl acetate solution of acetic anhydride and diethyl carbonate. The...

specific Embodiment approach 2

[0049] 1. Preparation of modified nano silicon-aluminum emulsion:

[0050] Step 1: Preparation of modified silicon partial hydrolyzate

[0051] Put 35 grams of ethyl orthosilicate, 12 grams of tetra-n-butyl zirconium (or 35 grams of ethyl orthosilicate and 12 grams of tetra-n-butyl zirconium and 12 grams of tributyl phosphate) in ethyl acetate (or toluene) Mix well, add 0.06 g of formic acid, add 100 mL of double distilled water dropwise, add dropwise for 120 minutes, stir ultrasonically for 6 hours, and react at a temperature of 150°C-240°C to obtain a partially hydrolyzed nano-silica emulsion, which is ready for use;

[0052] 2) Nano Al 2 o 3 Preparation of emulsion:

[0053] Mix 38 grams of double-distilled water, 0.076 grams of acetic anhydride, and 14 grams of diethyl carbonate in 10 mL of ethyl acetate (or toluene) by ultrasonic mixing, and set aside; add 1.0 grams of aluminum isopropoxide to 10 grams of isopropanol to prepare into a solution, and then added dropwise...

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Abstract

The invention provides a preparation method of a fluorescent rare earth complex modified nanometer silicon-aluminum emulsion. The method comprises the following steps: 1) preparing a modified nanometer silicon-aluminum emulsion: (1) ultrasonically and uniformly mixing ethyl orthosilicate with a modifying agent, a solvent and a catalyst, dropwise adding distilled water to prepare a modified partially-hydrolyzed nanometer silicon emulsion; (2) dissolving aluminum isopropoxide in calculated quantity into isopropanol, and then dropwise adding the mixture into the ultrasonically and sufficiently mixed solution of water, catalyst, modifying agent and solvent in calculated quantity to obtain a modified nanometer Al2O3 emulsion; (3) adding the modified nanometer Al2O3 emulsion prepared in the step (2) into the modified nanometer silicon-aluminum emulsion obtained by distilling to remove the solvent in the step (1); 2) performing surface modification on the modified nanometer silicon-aluminum emulsion, namely modifying the modified nanometer silicon-aluminum by using an organosilicon coupling agent; 3) preparing the fluorescent rare earth complex modified nanometer silicon-aluminum emulsion. The preparation process is simple and easy to operate, the exciting light wavelength of the prepared fluorescent rare earth complex modified nanometer silicon-aluminum emulsion is 330nm, the light emitting wavelength is 612nm, and the light-emitting strength is 98a.u.

Description

technical field [0001] The invention relates to a preparation method of a rare earth complex modified fluorescent material, in particular to a preparation method of a fluorescent rare earth complex modified nano-silicon-aluminum emulsion used for rapid detection test paper. Background technique [0002] Using fluorescent rare earth complexes and modified silica-alumina composite nanoparticles through unique assembly technology to prepare fluorescent rare earth complexes modified with high luminous efficiency, good hydrophilicity and emulsion stability, and high luminous intensity Nano-silicon-aluminum emulsion, test paper and on-site tester for rapid testing. [0003] There have been many research reports on rare earth ions or rare earth complexes and silica-doped luminescent materials. In the patent document with the application number 201010225072.8, a novel core-shell fluorescent material is disclosed, which relates to an optoelectronic luminescent material. Includes: C...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/02C09K11/64C09K11/06C09C1/40C09C1/28C09C3/12C09C3/08
Inventor 郭艳宏邹明强房世宇张帆
Owner HARBIN ENG UNIV
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