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Preparation method and application of organic phosphine grafted hollow metal organic framework material

A metal-organic framework and organophosphine technology, which is applied in the field of preparation of organophosphine-grafted hollow metal-organic framework materials, can solve problems such as poor smoke suppression performance, achieve good mechanical properties, novel and simple method, and improve compatibility Effect

Active Publication Date: 2020-05-05
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most polymer materials are extremely flammable and produce a large amount of toxic and harmful gases. MOFs materials have excellent catalytic performance, but poor smoke suppression performance, while hollow materials can store gas well, and phosphorus can be in both gas phase and condensed phase. It plays a flame-retardant role, so the preparation of an organophosphine-grafted hollow MOFs material is an effective way to improve the flame-retardant properties of polymer materials.

Method used

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  • Preparation method and application of organic phosphine grafted hollow metal organic framework material
  • Preparation method and application of organic phosphine grafted hollow metal organic framework material
  • Preparation method and application of organic phosphine grafted hollow metal organic framework material

Examples

Experimental program
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Effect test

Embodiment 1

[0039] 1. Preparation of organophosphine-grafted hollow zirconium metal-organic framework materials:

[0040] Such as figure 1 As shown, the specific steps of the preparation method of organophosphine grafted hollow metal organic framework materials include:

[0041] (1) Add 0.384g 2-aminoterephthalic acid, 0.54g zirconium tetrachloride, 120mL dimethylformamide (DMF) and 10mL acetic acid to the reaction vessel, stir at room temperature for 20min, pour the reaction solution into four In a vinyl fluoride reactor, react at 120°C for 24h, wash with DMF and methanol for 3 times, and vacuum dry at 60°C to obtain the zirconium metal organic framework (Zr-MOF-NH 2 ).

[0042] (2) Add 8.25g of sodium tungstate and 25mL of water into the reaction vessel, stir at room temperature for 30min, and use 2mol L -1 HCl to adjust the pH of the solution to 2.0, then add water to obtain a 250 mL solution, and add oxalic acid to adjust the pH of the solution to 2.3. Take 70mL solution and add i...

Embodiment 2

[0050] 1. Preparation of organophosphine-grafted hollow zirconium metal-organic framework materials:

[0051] Such as figure 1 As shown, the specific steps of the preparation method of organophosphine grafted hollow metal organic framework materials include:

[0052] (1) Add 0.384g 2-aminoterephthalic acid, 0.54g zirconium tetrachloride, 120mL dimethylformamide (DMF) and 10mL acetic acid to the reaction vessel, stir at room temperature for 20min, pour the reaction solution into four In a vinyl fluoride reactor, react at 120°C for 24h, wash with DMF and methanol for 3 times, and vacuum dry at 60°C to obtain the zirconium metal organic framework (Zr-MOF-NH 2 ).

[0053] (2) Add 8.25g of sodium tungstate and 25mL of water into the reaction vessel, stir at room temperature for 30min, and use 2mol L -1 HCl to adjust the pH of the solution to 2.0, then add water to obtain a 250 mL solution, and add oxalic acid to adjust the pH of the solution to 2.3. Take 70mL solution and add i...

Embodiment 3

[0063] 1. Preparation of organophosphine-grafted hollow zirconium metal-organic framework materials:

[0064] Such as figure 1 As shown, the specific steps of the preparation method of organophosphine grafted hollow metal organic framework materials include:

[0065] (1) Add 0.384g 2-aminoterephthalic acid, 0.54g zirconium tetrachloride, 120mL dimethylformamide (DMF) and 15mL acetic acid to the reaction vessel, stir at room temperature for 20min, pour the reaction solution into four In a vinyl fluoride reactor, react at 120°C for 24h, wash with DMF and methanol for 3 times, and vacuum dry at 60°C to obtain the zirconium metal organic framework (Zr-MOF-NH 2 ).

[0066] (2) Add 8.25g of sodium tungstate and 25mL of water into the reaction vessel, stir at room temperature for 30min, and use 2mol L -1 HCl to adjust the pH of the solution to 2.0, then add water to obtain a 250 mL solution, and add oxalic acid to adjust the pH of the solution to 2.3. Take 70mL solution and add i...

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Abstract

The invention discloses a preparation method and application of an organic phosphine grafted hollow metal organic framework material. The preparation method comprises the following steps: firstly, letting 2-aminoterephthalic acid react with zirconium tetrachloride to obtain a zirconium organic framework material with amino, then obtaining a hollow zirconium organic framework material through a metal-acid assisted etching method, and finally grafting organic phosphine DOPO through a Kabachnik-Fiels reaction. The synergistic effect among metal, hollow and organic phosphine in the organic phosphine grafted hollow zirconium metal organic framework material greatly enhances the flame retardancy and smoke suppression performance of the high polymer material; due to the existence of the organic ligand, the compatibility of a flame retardant and a polymer matrix is improved, and compared with other metal-based flame retardants, the flame-retardant polymer composite material has excellent flameretardancy and good mechanical properties.

Description

technical field [0001] The invention belongs to the technical field of metal organic framework materials, and in particular relates to a preparation method and application of organic phosphine grafted hollow metal organic framework materials. Background technique [0002] Metal-organic framework materials, or MOFs for short, are organic-inorganic hybrid materials with intramolecular pores formed by the self-assembly of organic ligands and metal ions or clusters through coordination bonds. The material has excellent catalytic performance, and the existence of organic ligands can well solve the compatibility problem between inorganic particles and polymer matrix, so MOFs materials can be applied in the field of polymer flame retardancy. Most polymer materials are extremely flammable and produce a large amount of toxic and harmful gases. MOFs materials have excellent catalytic performance, but poor smoke suppression performance, while hollow materials can store gas well, and ph...

Claims

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Application Information

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IPC IPC(8): C08G83/00C08L63/02C08L87/00C08L77/00
CPCC08G83/008C08L63/00C08L77/00C08L2201/02C08L87/00
Inventor 戴李宗王秀陈婷何凯斌洪静鹿振武陈国荣曾碧榕
Owner XIAMEN UNIV
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