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High-strength water-dispersible rare earth fluoride up-conversion luminescent material and preparation method thereof

A rare earth fluoride and luminescent material technology, applied in luminescent materials, chemical instruments and methods, applications, etc., can solve the problems that have not yet been discovered, and achieve the effects of good water dispersibility, high crystallinity and good compatibility

Active Publication Date: 2018-07-31
HUNAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report on the preparation of rare earth fluoride up-conversion luminescent materials by one-step hydrothermal method using WPU prepolymer as a ligand.

Method used

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  • High-strength water-dispersible rare earth fluoride up-conversion luminescent material and preparation method thereof
  • High-strength water-dispersible rare earth fluoride up-conversion luminescent material and preparation method thereof
  • High-strength water-dispersible rare earth fluoride up-conversion luminescent material and preparation method thereof

Examples

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Embodiment 1

[0037] This embodiment provides a method for preparing a high-strength water-dispersible rare earth fluoride up-conversion luminescent material, which includes the following steps:

[0038] S1. Raw material treatment: dry diisocyanate, polycarbonate diol, carboxylic acid type hydrophilic chain extender, acetone and other raw materials to remove water;

[0039] S2. Preparation of WPU prepolymer: Take the raw materials in step S1, adjust the mass fractions of the diisocyanate, polycarbonate diol, and carboxylic acid type hydrophilic chain extender to 40%, 47%, and 13% respectively , add dibutyltin dilaurate and acetone, raise the temperature to 40~70℃ and react for 7 hours to obtain WPU prepolymer;

[0040] Wherein, the volume fraction of the acetone is 22%, and the add-on of the dibutyltin dilaurate is 0.15% of the total solid content;

[0041] S3. Hydrothermal synthesis: Add 4 g of the WPU prepolymer in step S2 to 1 mmol of the aqueous solution of rare earth chloride salt, ad...

Embodiment 2

[0046] Refer to Example 1 for the preparation method of the high-strength water-dispersible rare earth fluoride up-conversion luminescent material provided in this example. The difference from Example 1 is that in step S2, the diisocyanate and polycarbonate binary The mass fractions of alcohol and carboxylic acid-type hydrophilic chain extenders are 40%, 51%, and 9% respectively; in step S3, the rare earths are yttrium, ytterbium, and erbium, and the molar ratio of Y3+, Yb3+, and Er3+ is 78:20 : 2, the mol ratio of carboxyl group and rare earth salt in the WPU prepolymer is 2:1, and the addition of the ammonia water is 0.5 mL.

Embodiment 3

[0048] Refer to Example 1 for the preparation method of the high-strength water-dispersible rare earth fluoride up-conversion luminescent material provided in this example. The difference from Example 1 is that in step S2, the diisocyanate and polycarbonate binary The mass fractions of alcohol and carboxylic acid type hydrophilic chain extenders are 40%, 49%, and 11% respectively; in step S3, the rare earths are yttrium, ytterbium, and thulium, and the molar ratio of Y3+, Yb3+, and Tm3+ is 78:20 : 2, the mol ratio of carboxyl group and rare earth salt in the WPU prepolymer is 2.5:1, and the addition of the ammonia water is 0.625 mL.

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Abstract

The invention relates to the technical field of anti-counterfeiting materials, and discloses a preparation method of a high-strength water-dispersible rare earth fluoride up-conversion luminescent material. The method comprises the steps of preparing a water-based polyurethane (WPU) prepolymer by a nucleophilic addition prepolymerization reaction; and then in an aqueous solution of a rare earth salt, using the WPU prepolymer as a ligand, performing a hydrothermal reaction, performing centrifugation, performing washing, and performing drying to obtain the rare earth fluoride up-conversion luminescent material. The up-conversion luminescent material prepared by the method provided by the invention is a bifurcate rod-liked micron crystal, has the characteristics of high crystallinity, strongluminescence, good water dispersibility and the like, and is very suitable to be added into a water-based ink system to be used for counterfeiting prevention.

Description

technical field [0001] The invention relates to the technical field of anti-counterfeiting materials, more specifically, to a high-strength water-dispersible rare earth fluoride up-conversion luminescent material and a preparation method thereof. Background technique [0002] With the rapid development of market economy and information technology, counterfeiting methods are becoming more and more sophisticated, and the raging of counterfeit and shoddy products seriously endangers people's health and safety. Some traditional anti-counterfeiting methods are constantly being cracked by criminals, and emerging anti-counterfeiting technologies are constantly becoming green, intelligent and popular. Radio frequency (RFID) tags, microlens array anti-counterfeiting, biometric identification such as DNA, voiceprint, and human iris, and materials or technologies such as stimulus responses (optical / electrical / magnetic responses, physical / chemical stimuli) have emerged as the times requ...

Claims

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Application Information

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IPC IPC(8): C08G18/66C08G18/44C08G18/34C08K3/16C09K11/06C09K11/02C09K11/85
CPCC08G18/34C08G18/44C08G18/6659C08K3/16C09D11/102C09K11/025C09K11/06C09K11/7772C09K2211/182
Inventor 刘跃军杨玲王正祥钟云飞
Owner HUNAN UNIV OF TECH
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