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Preparation method of ternary terbium complex monomer and ternary terbium complex monomer-mma copolymer luminescent material
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The technology of terbium complex and luminescent material is applied in the field of preparation of ternary terbium complex monomer and terbium complex monomer-MMA copolymer luminescent material, which can solve the problem of weak rare earth ion fluorescence and limit rare earth luminescence Wide application of materials, unstable luminescence and other problems, to achieve the effects of excellent thermal stability, easy to popularize and use, and low cost
Inactive Publication Date: 2017-03-22
CHONGQING UNIV OF TECH
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However, the fluorescence of rare earth ions is extremely weak and the luminescence is extremely unstable, which seriously limits the wide application of rare earth luminescent materials.
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Embodiment 1
[0052] Embodiment 1: the preparation method of ternary terbium complex monomer:
[0053] Weigh 0.5603g TbCl 3 .6H 2 O was added to a three-necked flask, and 50ml of absolute ethanol was used as a solvent, and it was fully dissolved by vibration of an ultrasonic cleaner. In the three-necked flask, add ammonia water that can just neutralize the carboxyl groups in the reaction system.
[0054] Weigh 0.632g of p-hydroxybenzoic acid and dissolve it in 25ml of THF.
[0055] Weigh 0.304 g of methylvinylimidazole benzoic acid and dissolve it in 50 ml of DMF.
[0056] Fix the dropping funnel in the three-necked flask, coat the interface with vacuum silicone grease, pour the p-hydroxybenzoic acid fully dissolved in THF into the dropping funnel, turn on the switch, and control the dropping speed of 5-15 seconds / drop, so that p-Hydroxybenzoic acid coordinates with terbium ions.
[0057] After p-hydroxybenzoic acid is fully coordinated with terbium ions, pour methylvinylimidazole benz...
Embodiment 2
[0060] Example 2: The preparation method of ternary terbium complex monomer-MMA copolymer luminescent material:
[0061] Free radical polymerization should be carried out under strict anhydrous and oxygen-free conditions. Before polymerization, the solvent DMF should be dried to remove water and the initiator AIBN should be recrystallized.
[0062] The mass of fixed MMA is 1g, according to the molar ratio of ternary terbium complex monomer: MMA=10:100, weigh 0.0804g of ternary terbium complex monomer. Use 3-10ml of DMF (N,N-dimethylformamide) to dissolve the ternary terbium complex monomer and the initiator AIBN0.0095g.
[0063] Through the three-way pipe, the air in the polymerization tube is extracted, and the inert gas argon is passed into the tube to seal the polymerization tube tightly.
[0064] Using simethicone as the heating medium, place the polymerization tube in a collector heating agitator, and seal the tube for 24-48 hours of polymerization at 65°C.
[0065] Slo...
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Abstract
The invention relates to a preparation method of a ternary terbium complex monomer and a copolymer luminescent material of the ternary terbium complex monomer and MMA. The method comprises the steps that firstly, the ternary terbium complex monomer is prepared, and recrystallization is conducted on an initiating agent AIBN (azodiisobutyronitrile) through methyl alcohol; then the ternary terbium complex monomer is dissolved by utilizing DMF (N,N-dimethylformamide) and DMSO (dimethyl sulfoxide) or a toluene solvent respectively, wherein the molar ratio of the ternary terbium complex monomer to the MMA is 1-10 to 100, and the initiating agent AIBN accounts for 0.5%-1% of the total mass of an initiating system; after reaction is conducted for 20-60 h under the conditions that inert gas argon exists, water and oxygen do not exist, and the temperature ranges from 50 DEG C to 85 DEG C, copolymer powder is obtained through methyl alcohol reprecipitation. The copolymer can be used for electronic terminals such as computers, televisions and mobile phones and mainly serves as the luminescent material of the panel display field. In addition, due to the fact that a pendant group -N-H- of the copolymer contains a reactive hydrogen atom, the copolymer can be used for ion recognition and fluorescent probes.
Description
technical field [0001] The invention relates to a ternary terbium complex monomer and a preparation method of a ternary terbium complex monomer-MMA copolymer luminescent material. Background technique [0002] The outer electron structure of rare earth ions is basically the same, and the unique structure of the 4f layer electron energy level is similar, which makes rare earth luminescent materials have the advantages of high quantum yield, narrow emission band, long fluorescence lifetime, and high purity of luminescent color. In recent years, rare earth luminescent materials have developed rapidly and are increasingly used in solid-state sensors, fluorescent probes, anion and cation detectors, agricultural films, electroluminescent components and other fields. However, the fluorescence of rare earth ions is extremely weak and the luminescence is extremely unstable, which seriously limits the wide application of rare earth luminescent materials. Contents of the invention ...
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