4-sulfophthalic acid rare-earth metal complex, preparation method therefor and application thereof

Abstract

The invention relates to a 4-sulfophthalic acid rare earth metal complex, a preparation method therefor and an application thereof. A general chemical formula of the 4-sulfophthalic acid rare earth metal complex is [Ln( H2O )2( SP )], wherein the Ln are plus trivalent lanthanide-series rare-earth ions Dy (III), Tb (III) and Er (III), and SP is a negative trivalent anion of the 4-sulfophthalic acid. The 4-sulfophthalic acid rare-earth metal complex is prepared by a solvent-thermal method which has a high yield, good reproducibility and high thermal stability. Under ultraviolet excitation, the solid-state complex can emit feature red light, green light or blue light, and has a high application value in the field of material science while being used as a photoluminescent material.

Description

[0001] Statement Regarding Funding Research or Development

[0002] The application for this invention has been supported by the National Natural Science Foundation of China (fund numbers: 21171129 and 21173157) and the Tianjin Higher Education Science and Technology Development Fund Project (fund number: 2012ZD02). technical field

[0003] The invention relates to the technical field of metal-organic coordination polymers and photoluminescent materials thereof, in particular to the preparation method and the Its optical properties make it applicable as a photoluminescent material in the field of material science. Background technique

[0004] Rare earth organic luminescent materials have important applications in the fields of luminescence, hydrogen storage materials, and biomedicine due to their characteristics of good monochromaticity, low excitation energy, high luminous intensity, and high energy transfer efficiency. One of the active fields in the development and appl...

Examples

Embodiment 1

[0027] 4-sulfophthalic acid rare earth metal complex A Synthesis:

[0028] Dissolve 4-sulfophthalic acid (0.65 mmol, 160.2 mg) and dysprosium chloride hexahydrate (0.3 mmol, 113.1 mg) in a mixed solvent of double distilled water (8.0 mL) and methanol (2.0 mL) . The pH of the reaction system was adjusted to 6 with triethylamine, and after stirring for several minutes, the reaction mixture was sealed into a 23.0 ml hydrothermal kettle. The sealed reaction kettle was transferred to a temperature-controlled oven, and kept at 170 °C for four days, then heated at 3.0 °C h –1 rate program to cool down to room temperature. After opening the reaction kettle, colorless needle-like crystals were obtained directly, washed with methanol, and dried in air to obtain the complex A .

Embodiment 2

[0030] 4-sulfophthalic acid rare earth metal complex B Synthesis:

[0031] Dissolve 4-sulfophthalic acid (0.65 mmol, 160.2 mg) and terbium chloride hexahydrate (0.3 mmol, 112.0 mg) in a mixed solvent of double distilled water (6.0 mL) and ethanol (4.0 mL) . The pH of the reaction system was adjusted to 6 with triethylamine, and after stirring for several minutes, the reaction mixture was sealed into a 23.0 ml hydrothermal kettle. The sealed reaction kettle was transferred to a temperature-controlled oven, and kept at 170 °C for four days, then heated at 3.0 °C h –1 rate program to cool down to room temperature. After opening the reaction kettle, colorless needle-like crystals were obtained directly, washed with methanol, and dried in air to obtain the complex B .

Embodiment 3

[0033] 4-sulfophthalic acid rare earth metal complex C Synthesis:

[0034] 4-Sulphophthalic acid (0.65 mmol, 160.2 mg) and erbium oxide (0.3 mmol, 114.8 mg) were dissolved in a mixed solvent of double distilled water (8.0 mL) and ethanol (2.0 mL). The pH of the reaction system was adjusted to 5 with triethylamine, and after stirring for several minutes, the reaction mixture was sealed into a 23.0 ml hydrothermal kettle. The sealed reaction kettle was transferred to a temperature-controlled oven, and kept at 200 °C for four days, then heated at 3.0 °C h –1 rate program to cool down to room temperature. After opening the reaction kettle, light pink needle-like crystals were obtained directly, washed with methanol, and dried in air to obtain the complex C .

[0035] 4-sulfophthalic acid rare earth metal complex prepared by the present invention (embodiment 1-3, A - C ) is characterized by the following structure:

[0036] (1) Determination of the crystal structure of the c...

[0001] Statement Regarding Funding Research or Development

[0002] The application for this invention has been supported by the National Natural Science Foundation of China (fund numbers: 21171129 and 21173157) and the Tianjin Higher Education Science and Technology Development Fund Project (fund number: 2012ZD02). technical field

[0003] The invention relates to the technical field of metal-organic coordination polymers and photoluminescent materials thereof, in particular to the preparation method and the Its optical properties make it applicable as a photoluminescent material in the field of material science. Background technique

[0004] Rare earth organic luminescent materials have important applications in the fields of luminescence, hydrogen storage materials, and biomedicine due to their characteristics of good monochromaticity, low excitation energy, high luminous intensity, and high energy transfer efficiency. One of the active fields in the development and appl...

Examples

Embodiment 1

[0027] 4-sulfophthalic acid rare earth metal complex A Synthesis:

[0028] Dissolve 4-sulfophthalic acid (0.65 mmol, 160.2 mg) and dysprosium chloride hexahydrate (0.3 mmol, 113.1 mg) in a mixed solvent of double distilled water (8.0 mL) and methanol (2.0 mL) . The pH of the reaction system was adjusted to 6 with triethylamine, and after stirring for several minutes, the reaction mixture was sealed into a 23.0 ml hydrothermal kettle. The sealed reaction kettle was transferred to a temperature-controlled oven, and kept at 170 °C for four days, then heated at 3.0 °C h –1 rate program to cool down to room temperature. After opening the reaction kettle, colorless needle-like crystals were obtained directly, washed with methanol, and dried in air to obtain the complex A .

Embodiment 2

[0030] 4-sulfophthalic acid rare earth metal complex B Synthesis:

[0031] Dissolve 4-sulfophthalic acid (0.65 mmol, 160.2 mg) and terbium chloride hexahydrate (0.3 mmol, 112.0 mg) in a mixed solvent of double distilled water (6.0 mL) and ethanol (4.0 mL) . The pH of the reaction system was adjusted to 6 with triethylamine, and after stirring for several minutes, the reaction mixture was sealed into a 23.0 ml hydrothermal kettle. The sealed reaction kettle was transferred to a temperature-controlled oven, and kept at 170 °C for four days, then heated at 3.0 °C h –1 rate program to cool down to room temperature. After opening the reaction kettle, colorless needle-like crystals were obtained directly, washed with methanol, and dried in air to obtain the complex B .

Embodiment 3

[0033] 4-sulfophthalic acid rare earth metal complex C Synthesis:

[0034] 4-Sulphophthalic acid (0.65 mmol, 160.2 mg) and erbium oxide (0.3 mmol, 114.8 mg) were dissolved in a mixed solvent of double distilled water (8.0 mL) and ethanol (2.0 mL). The pH of the reaction system was adjusted to 5 with triethylamine, and after stirring for several minutes, the reaction mixture was sealed into a 23.0 ml hydrothermal kettle. The sealed reaction kettle was transferred to a temperature-controlled oven, and kept at 200 °C for four days, then heated at 3.0 °C h –1 rate program to cool down to room temperature. After opening the reaction kettle, light pink needle-like crystals were obtained directly, washed with methanol, and dried in air to obtain the complex C .

[0035] 4-sulfophthalic acid rare earth metal complex prepared by the present invention (embodiment 1-3, A - C ) is characterized by the following structure:

[0036] (1) Determination of the crystal structure of the c...

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