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Lithium cluster complex based on aromatic tetracarboxylic acid and preparation method thereof

An aromatic tetracarboxylic acid, complex technology, applied in lithium organic compounds, 1/11 group organic compounds without C-metal bonds, organic chemical methods, etc., can solve high charge density, difficulty in Li-MOFs synthesis, Li problems such as low atomic mass, to achieve the effect of a simple preparation method

Inactive Publication Date: 2019-02-22
山西师范大学
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, due to the low atomic mass and high charge density of the metal element Li, it is an ideal metal center element for light coordination compounds, but the synthesis of Li-MOFs is relatively difficult due to the strong hydrophilicity of lithium. difficulty

Method used

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  • Lithium cluster complex based on aromatic tetracarboxylic acid and preparation method thereof
  • Lithium cluster complex based on aromatic tetracarboxylic acid and preparation method thereof
  • Lithium cluster complex based on aromatic tetracarboxylic acid and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 0.012g (0.30mmol) lithium hydroxide hydrate, 0.041g (0.12mmol) 3,3′,5,5′-diphenyltetracarboxylic acid to a container containing 4mL N,N-dimethylformamide, Put 2mL ethanol and 1mL distilled water in a 20mL glass bottle, stir at room temperature for 20 minutes to mix evenly, then put the glass bottle in an oven at 120°C for 72 hours of constant temperature reaction, cool, wash with absolute ethanol to remove impurity powder, and obtain a colorless and transparent Blocky crystals, that is, lithium cluster-based complexes, whose structural unit is Li 5.5 (L) 4 (DMF)(H2 O)·(H 2 O), L represents 3,3′,5,5′-diphenyltetracarboxylic acid, DMF represents N,N-dimethylformamide, and its yield is 40% based on lithium calculation.

[0033] Such as figure 1 As shown, the prepared lithium cluster complex belongs to the monoclinic C222 1 Space group, unit cell parameter a is 28.3992(15) b is 33.4487(14) c is 22.6224(7) α is 90°, β is 90°, γ is 90°, and the unit cell volume ...

Embodiment 2

[0036] Dissolve 0.023g (0.56mmol) lithium hydroxide hydrate in 1mL distilled water, dissolve 0.018g (0.04mmol) 5-(2-((3,5-dihydroxy)oxy)oxyethyl) m-dibenzoic acid In a mixed solvent of 4mL N,N-dimethylformamide and 2mL ethanol, stir at room temperature for 20 minutes to make the mixture uniform, then react at a constant temperature at 120°C for 5 hours, cool, rinse with absolute ethanol, and filter to obtain Colorless transparent needle-like crystals, that is, lithium cluster complexes, whose structural unit is Li 3 (L)(DMF)(H 2 O)·(H 2 O), L represents 5-(2-((3,5-dihydroxy)oxy)oxyethyl) m-dibenzoic acid, DMF represents N,N-dimethylformamide, and its yield is 20 based on lithium %.

[0037] Such as Figure 5 As shown, the prepared lithium cluster-based complex belongs to the monoclinic crystal system, P2 1 / n space group, unit cell parameter a is 12.9535(7) b is 10.4429(4) c is 21.4382(13) α is 90°, β is 90°, γ is 91.676(5)°, and the unit cell volume is 2898.8(3) ...

Embodiment 3

[0039] Add 0.014g (0.3mmol) lithium hydroxide hydrate, 0.021g (0.05mmol) 5-(5'-(1,4-benzenebicyclo(methylene)dioxy)) m-dibenzoic acid to a 5mL N,N-Dimethylformamide, 1mL ethanol and 1mL distilled water in a glass bottle, stir at room temperature until the solution is clear, then put the glass bottle in an oven at 120°C for 72 hours at a constant temperature, take out the glass bottle to cool down naturally, and use anhydrous Wash with ethanol to remove impurity powder, and obtain colorless and transparent massive crystals, that is, lithium cluster-based complexes, whose structural unit is Li 4 (L)(DMF) 2 , L represents 5-(5'-(1,4-benzenebicyclo(methylene) dioxy)) m-dibenzoic acid, DMF represents N,N-dimethylformamide, and its yield is 40 based on lithium %.

[0040] Such as Figure 8 As shown, the prepared lithium cluster-based complex belongs to the triclinic crystal system, the P-1 space group, and the unit cell parameter a is 8.6413 (15) b is 9.3155(16) c is 10.0801(...

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Abstract

The invention discloses a lithium cluster based complex based on aromatic tetracarboxylic acid and a preparation method of the lithium cluster based complex. The structural unit of the complex is Lia(L)b(DMF)c(H2O)d.(H2O)e, wherein L represents ligands 3, 3', 5, 5'-biphenyl tetracarboxylic acid, 5-(2-((3, 5-dyhydroxyl)oxygen)yloxyethyl)iso-phthalic acid, 5-(5'-(1, 4-benzene bicyclic(methylene) dioxo))iso-phthalic acid or 1, 3-di(3', 5'-dibenzoic acid)benzene; and DMF represents N, N-dimethyl formamide. The complex and the method have the advantages that lithium hydroxide monohydrate and the four ligands are taken as precursors, 4 lithium cluster based complexes are prepared through a solvothermal method, the preparation method is simple, and the obtained complexes have a fluorescence property and a semiconductor property, and can serve as fluorescence materials and semiconductor materials.

Description

technical field [0001] The invention belongs to the technical field of synthesizing metal-organic framework materials, and in particular relates to a lithium cluster complex based on aromatic tetracarboxylic acid and a preparation method of the complex. Background technique [0002] Metal-organic frameworks (Metal-Organic Framework, referred to as MOFs) are inorganic-organic composites with a three-dimensional network structure formed by hybridization and self-assembly of metal ions or metal clusters and nitrogen or oxygen polydentate organic ligands of aromatic carboxylic acids or bases. Microporous crystals are therefore also called porous complexes. Due to the advantages of large specific surface area and rich pore structure, MOFs have applications in many scientific fields such as gas adsorption and separation, drug sustained release, and optical devices. [0003] At present, due to the low atomic mass and high charge density of the metal element Li, it is an ideal meta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F1/02C09K11/06
CPCC07B2200/13C07F1/005C09K11/06C09K2211/181
Inventor 籍文娟冯琳郝瑞卿裴微微
Owner 山西师范大学