A kind of terbium complex green fluorescent luminescent material and preparation method thereof

Abstract

The invention discloses a terbium complex green fluorescent luminous material. The complex luminous material is a three-dimensional coordination polymer containing two kinds of organic polycarboxylicacid anion ligands, and the general formula of the material is [Tb(1,4-bdc)0.5(1,2-bdc)(H2O)2]n, wherein 1,4-bdc represents terephthalic acid radical divalent anions, 1,2-bdc represents phthalic acidradical divalent anions, and n is a natural number greater than 100. According to the terbium complex green fluorescent luminous material, two kinds of benzene-ring containing organic dicarboxylic acid including terephthalic acid and phthalic acid are adopted as the ligands and react with terbium perchlorate under hydrothermal conditions, a terbium complex containing the two kinds of ligands is prepared and emits green fluorescence under the excitation of 250-350nm ultraviolet light, the luminescence belongs to the characteristic fluorescence of trivalent terbium ions, and under the excitation of 300nm ultraviolet light, the luminescence quantum efficiency reaches 56%, which indicates that the complex has good photoluminescence properties. Meanwhile, the complex does not decompose at thetemperature of 300 DEG C or below, which indicates that the complex has good thermal stability.

Description

technical field

[0001] The invention relates to a preparation method for synthesizing a three-dimensional coordination polymer by reacting terbium perchlorate, terephthalic acid and phthalic acid under hydrothermal conditions. Background technique

[0002] The synthesis and properties of rare earth complexes are one of the important contents of rare earth chemistry research, especially in the fields of luminescence, magnetism, catalysis, and gas adsorption of complexes. Among rare earth elements, the complexes of four elements, samarium, europium, terbium and dysprosium, have good photoluminescence properties in the visible region, especially the two elements, europium and terbium, can generate good luminescence properties when the organic ligand is properly selected The complexes have potential broad application prospects in photoluminescence and electroluminescence materials. Among them, the terbium complexes emit green characteristic fluorescence of trivalent terbium ion...

Examples

preparation example Construction

[0023] A method for preparing a terbium complex green fluorescent light-emitting material, comprising weighing terephthalic acid and phthalic acid, adding an aqueous solution of terbium perchlorate for reaction, wherein terbium perchlorate: terephthalic acid: phthalic acid The ratio of the amount of the substance is 1:0.4~0.6:0.8~1.2, adjust the pH value to 4.5~6.5, heat to 150℃~210℃, react for 24~96 hours, and then cool down at 1~5℃ per hour, A colorless crystal of the complex is obtained, washed with ethanol, dried and collected to obtain a green fluorescent light-emitting material of the terbium complex.

[0024] In the present invention, the preferred solution is: the ratio of the amount of terbium perchlorate: terephthalic acid: phthalic acid is 1:0.5:1; the pH value is 5.5, heated to 180 ° C, reacted for 72 hours, and then Cool down at 2°C per hour.

[0025] In the present invention, the reaction is carried out in a reaction kettle, and the solvent for adjusting the pH ...

Embodiment 1

[0027] Accurately weigh 0.0166 g terephthalic acid and 0.0332 g phthalic acid with an analytical balance in the reaction kettle, and add 5.00 mL of terbium (Tb) perchlorate (0.04 mol L -1 ) in the reactor. Add 5 mL of deionized water to the reaction kettle, and use 1 mol L -1 The pH was adjusted to 6 with sodium hydroxide. Then, put it into an oven, set the temperature to 180°C, react in the oven for 72 hours, and then lower the temperature at 2°C per hour to obtain colorless crystals with complexes, which are washed with absolute ethanol, air-dried, and collected.

Embodiment 2

[0029] Accurately weigh 0.0133 g of terephthalic acid and 0.0299 g of phthalic acid with an analytical balance in the reaction kettle, and add 4.00 mL of terbium (Tb) perchlorate (0.05 mol L -1 ) in the reactor. Add 5mL of deionized water to the reaction kettle, and use 1mol·L -1 Potassium hydroxide adjusts the pH to 4.5. Then, put it into an oven, set the temperature to 160°C, react in the oven for 25 hours, and then lower the temperature at 1°C per hour to obtain colorless crystals with complexes, washed with absolute ethanol, air-dried, and collected.

technical field

[0001] The invention relates to a preparation method for synthesizing a three-dimensional coordination polymer by reacting terbium perchlorate, terephthalic acid and phthalic acid under hydrothermal conditions. Background technique

[0002] The synthesis and properties of rare earth complexes are one of the important contents of rare earth chemistry research, especially in the fields of luminescence, magnetism, catalysis, and gas adsorption of complexes. Among rare earth elements, the complexes of four elements, samarium, europium, terbium and dysprosium, have good photoluminescence properties in the visible region, especially the two elements, europium and terbium, can generate good luminescence properties when the organic ligand is properly selected The complexes have potential broad application prospects in photoluminescence and electroluminescence materials. Among them, the terbium complexes emit green characteristic fluorescence of trivalent terbium ion...

Examples

preparation example Construction

[0023] A method for preparing a terbium complex green fluorescent light-emitting material, comprising weighing terephthalic acid and phthalic acid, adding an aqueous solution of terbium perchlorate for reaction, wherein terbium perchlorate: terephthalic acid: phthalic acid The ratio of the amount of the substance is 1:0.4~0.6:0.8~1.2, adjust the pH value to 4.5~6.5, heat to 150℃~210℃, react for 24~96 hours, and then cool down at 1~5℃ per hour, A colorless crystal of the complex is obtained, washed with ethanol, dried and collected to obtain a green fluorescent light-emitting material of the terbium complex.

[0024] In the present invention, the preferred solution is: the ratio of the amount of terbium perchlorate: terephthalic acid: phthalic acid is 1:0.5:1; the pH value is 5.5, heated to 180 ° C, reacted for 72 hours, and then Cool down at 2°C per hour.

[0025] In the present invention, the reaction is carried out in a reaction kettle, and the solvent for adjusting the pH ...

Embodiment 1

[0027] Accurately weigh 0.0166 g terephthalic acid and 0.0332 g phthalic acid with an analytical balance in the reaction kettle, and add 5.00 mL of terbium (Tb) perchlorate (0.04 mol L -1 ) in the reactor. Add 5 mL of deionized water to the reaction kettle, and use 1 mol L -1 The pH was adjusted to 6 with sodium hydroxide. Then, put it into an oven, set the temperature to 180°C, react in the oven for 72 hours, and then lower the temperature at 2°C per hour to obtain colorless crystals with complexes, which are washed with absolute ethanol, air-dried, and collected.

Embodiment 2

[0029] Accurately weigh 0.0133 g of terephthalic acid and 0.0299 g of phthalic acid with an analytical balance in the reaction kettle, and add 4.00 mL of terbium (Tb) perchlorate (0.05 mol L -1 ) in the reactor. Add 5mL of deionized water to the reaction kettle, and use 1mol·L -1 Potassium hydroxide adjusts the pH to 4.5. Then, put it into an oven, set the temperature to 160°C, react in the oven for 25 hours, and then lower the temperature at 1°C per hour to obtain colorless crystals with complexes, washed with absolute ethanol, air-dried, and collected.

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