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A kind of three-dimensional rare earth coordination polymer green fluorescent material containing mixed carboxylic acid and its preparation method

A coordination polymer, green fluorescence technology, applied in the direction of luminescent materials, compounds containing elements of Group 3/13 of the periodic table, potassium organic compounds, etc., to achieve novel crystal structure, easy large-scale industrial production, low cost. Effect

Inactive Publication Date: 2016-04-20
NINGXIA UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, at present, there are very few reports on rare earth coordination polymer fluorescent materials constructed by mixing flexible carboxylic acid ligands, and rare earth coordination polymer green light materials with high chromaticity and good stability still need to be further developed

Method used

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  • A kind of three-dimensional rare earth coordination polymer green fluorescent material containing mixed carboxylic acid and its preparation method
  • A kind of three-dimensional rare earth coordination polymer green fluorescent material containing mixed carboxylic acid and its preparation method
  • A kind of three-dimensional rare earth coordination polymer green fluorescent material containing mixed carboxylic acid and its preparation method

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preparation example Construction

[0035] The preparation method comprises the following steps:

[0036] 1) mixing and stirring: Tb(NO 3 ) 3 ·6H 2 O, aminotriacetic acid, oxalic acid and water are mixed with a certain ratio of substances, and then stirred at room temperature for about three hours;

[0037] 2) adjust the pH value: adjust the pH value between 2-6 with the mixture obtained in step 1) with acid and alkali solution;

[0038] 3) Heating: put the mixture obtained in step 2) into a 25ml stainless steel reaction kettle with a polytetrafluoroethylene liner, the filling degree is 80%, seal it, put it into an oven at 120-180°C, under autogenous pressure Under the action, heat and crystallize for 3-6 days. Turn off the power of the oven, gradually cool to room temperature, and open the reaction kettle to obtain colorless and transparent block crystals;

[0039] 4) Washing and drying: the colorless and transparent block crystals obtained in step 3) are washed with distilled water for 1-3 times, and then...

Embodiment 1

[0045] Preparation method 1 of [KTb2(NTA)(ox)2(H2O)5]n:

[0046] Tb(NO 3 ) 3 ·6H 2 O (0.33g, 0.76mmol), aminotriacetic acid (0.20g, 1mmol), oxalic acid (0.13g, 1mmol) and water (15mL) were mixed in a ratio of 0.76:1:1:833, with 1mol / 1 L of dilute hydrochloric acid and 1 mol / L potassium hydroxide solution to adjust the pH value to 2, then stirred at room temperature for three hours.

[0047] The obtained mixture was put into a 25mL stainless steel reaction kettle lined with polytetrafluoroethylene, with a filling degree of 80%, sealed, placed in an oven at 170°C, and heated for crystallization under autogenous pressure for three days. Turn off the power of the oven, cool down to room temperature gradually, open the reaction kettle to obtain colorless and transparent massive crystals; wash the obtained crystals with distilled water for 3 times, and then dry them for 4 hours at a temperature of 40°C to obtain aminotriacetic acid Three-dimensional terbium coordination polymer...

Embodiment 2

[0054] Preparation method two of [KTb2(NTA)(ox)2(H2O)5]n:

[0055] Tb(NO 3 ) 3 ·6H 2 O (0.33g, 0.76mmol), aminotriacetic acid (0.20g, 1mmol), oxalic acid (0.13g, 1mmol) and water (15mL) were mixed in a ratio of 0.76:1:1:833, with 2mol / 1 L of dilute hydrochloric acid and 2 mol / L potassium hydroxide solution to adjust the pH value to 4, then stirred at room temperature for three hours.

[0056] The obtained mixture was put into a 25mL stainless steel reaction kettle lined with polytetrafluoroethylene, with a filling degree of 80%, sealed, placed in an oven at 160°C, and heated for crystallization under autogenous pressure for 5 days. Turn off the power of the oven, cool down to room temperature gradually, and open the reaction kettle to obtain colorless and transparent massive crystals; wash the obtained crystals with distilled water for 3 times, and then dry them at 70°C for 3 hours to obtain aminotriacetic acid Three-dimensional terbium coordination polymer green fluoresc...

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Abstract

The invention relates to a green rare-earth organic luminescent material, particularly a three-dimensional rare-earth coordination polymer green fluorescent material containing mixed carboxylic acids and a preparation method thereof. The fluorescent material is characterized in that the molecular formula is C10H16Tb2KNO19. The fluorescent material has the following structural features: 1) by using KTb2(NTA)(ox)2(H2O)5 as a structural unit, aminotriacetic acid and oxalic acid are mixed with the ligand to form a three-dimensional network structure by bridging; and 2) the fluorescent material belongs to a monoclinic system, the space group is P2(1) / m, and the cell parameters are as follows: a=6.3008(3)A, b=10.0210(6)A, c=16.0417(9)A, alpha=gamma=90 degrees, and beta=100.682(3) degrees. The rare-earth coordination polymer green fluorescent material has the advantages of bright color and high stability, can not deteriorate after being placed in air for a long time, and has favorable water stability.

Description

technical field [0001] The invention relates to a green rare earth organic luminescent material, in particular to a three-dimensional rare earth coordination polymer green fluorescent material containing mixed carboxylic acid and a preparation method thereof. Background technique [0002] Since Tang et al. of the United States made a breakthrough in the research of organic electroluminescence (OEL) in 1987, OEL has been hailed as the flat panel display technology of the 21st century and has become one of the hot spots of international research. In recent years, the research on organic light-emitting materials has attracted more and more people's interest. Compared with inorganic light-emitting materials, organic light-emitting materials have higher luminous efficiency and a wider selection range of light-emitting colors, and have the advantage of being easy to form large-area films. In recent years, the research on high-performance organic green light-emitting devices is re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F19/00C07F5/00C07F1/06C09K11/06
Inventor 杨庆凤薛屏王晓中李鹏姜红梅胡明昕
Owner NINGXIA UNIVERSITY
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