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Titanium-doped ternary metal organic framework material and preparation method thereof

An organic framework and ternary metal technology, which is applied in the field of titanium-doped ternary metal-organic framework materials and their preparation, can solve the problems of low catalytic efficiency, poor stability and cannot be reused, and achieves improved catalytic activity and improved hydrothermal energy. Stability, accelerated degradation effect

Active Publication Date: 2019-01-11
苏州安仕泊环保科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at at least one defect or improvement requirement of the prior art, the present invention provides a titanium-doped ternary metal-organic framework material and a preparation method thereof, the purpose of which is to solve the problem of low catalytic efficiency and poor stability of existing photocatalytic materials Problems that cannot be reused

Method used

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  • Titanium-doped ternary metal organic framework material and preparation method thereof
  • Titanium-doped ternary metal organic framework material and preparation method thereof
  • Titanium-doped ternary metal organic framework material and preparation method thereof

Examples

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Effect test

Embodiment 1

[0034] (1) Preparation of 5,5',5"-(((1,3,5-triazine-2,4,6-triyl)tri(benzene-4,1-diyl))tri(acetylene-2 ,1-diyl))triisophthalic acid

[0035] a. Mix 2.3g of 5-iododiethylphthalate and THF / iPr2NH (30mL / 10mL) solution and degas with dry Ar gas for 20min; add 85mg of bis(triphenylphosphine) dichloride and 50mg of CuI, And the mixture was stirred at 25 °C for 15 minutes; then 2,4,6-tris(4-ethynylphenyl)-1,3,5-triazine (1.0 g, 2.6 mmol) in anhydrous THF ( 10 mL) solution, and the mixture was stirred at 50 °C for 10 h. After the reaction was complete, the volatile substances were removed under reduced pressure, and the residue was added to 100 mL of deionized water and washed with CHCl 3 Extraction; the organic phase was washed successively with deionized water, brine, and MgSO 4 dry. Remove CHCl under reduced pressure 3 , and the resulting solid was purified by silica gel column chromatography with CHCl 3 / C 2 h 6 (1:1) elution gave a light yellow solid pentaethyl 5,5',5"-(((...

Embodiment 2

[0049] (1) Preparation of 5,5',5"-(((1,3,5-triazine-2,4,6-triyl)tri(benzene-4,1-diyl))tri(acetylene-2 ,1-diyl))triisophthalic acid

[0050] a. Mix 3.6g of 5-iododiethylphthalate and THF / iPr2NH (30mL / 10mL) solution and degas with dry Ar gas for 20min; add 64mg of bis(triphenylphosphine)palladium dichloride and 37.5mg CuI, and the mixture was stirred at 25°C for 15 minutes; then 2,4,6-tris(4-ethynylphenyl)-1,3,5-triazine (1.0 g, 2.6 mmol) in anhydrous solution in THF (10 mL), and the mixture was stirred at 60 °C for 10 h. After the reaction was complete, the volatile substances were removed under reduced pressure, and the residue was added to 100 mL of deionized water and washed with CHCl 3 Extraction; the organic phase was washed successively with deionized water, brine, and MgSO 4 dry. Remove CHCl under reduced pressure 3 , and the resulting solid was purified by silica gel column chromatography with CHCl 3 / C 2 h 6 (1:1) elution gave a light yellow solid pentaethyl 5,...

Embodiment 3

[0059] (1) Preparation of 5,5',5"-(((1,3,5-triazine-2,4,6-triyl)tri(benzene-4,1-diyl))tri(acetylene-2 ,1-diyl))triisophthalic acid

[0060]a. Mix 2.7g of 5-iododiethylphthalate and THF / iPr2NH (30mL / 10mL) solution and degas with dry Ar gas for 20min; add 106mg of bis(triphenylphosphine)palladium dichloride and 62.5mg CuI, and the mixture was stirred at 25°C for 15 minutes; then 2,4,6-tris(4-ethynylphenyl)-1,3,5-triazine (1.0 g, 2.6 mmol) in anhydrous solution in THF (10 mL), and the mixture was stirred at 65 °C for 12 h. After the reaction was complete, the volatile substances were removed under reduced pressure, and the residue was added to 100 mL of deionized water and washed with CHCl 3 Extraction; the organic phase was washed successively with deionized water, brine, and MgSO 4 dry. Remove CHCl under reduced pressure 3 , and the resulting solid was purified by silica gel column chromatography with CHCl 3 / C 2 h 6 (1:1) elution gave a light yellow solid pentaethyl 5,...

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Abstract

The invention discloses a titanium-doped ternary metal organic framework material and a preparation method thereof. The preparation method comprises the following steps: (S1) preparing 5,5',5''-(((1,3,5-triazine-2,4,6-triyl)tris(phenyl-4,1-diyl))tris(acetylene-2,1-diyl))triisodecanoic acid from 5-diethyl iodophthalate and 2,4,6-tris(4-ethynylphenyl)-1,3,5-triazine; (S2) adding a first metal sourceprecursor, a second metal source precursor and 5,5',5''-(((1,3,5-triazine-2,4,6-triyl)tris(phenyl-4,1-diyl))tris(acetylene-2,1-diyl))triisodecanoic acid into a reactor, and reacting at 25-75 DEG C for 4-90 hours, so as to obtain a binary metal organic framework material mixed solution; and (S3) adding a titanium metal source precursor into the mixed solution prepared in the step (S2) in a molar ratio of (1-10) to (1-10), and carrying out ion exchange, so as to obtain the titanium-doped ternary metal organic framework material. The prepared titanium-doped ternary metal organic framework material is high in catalytic activity and good in hydrothermal stability and can be repeated used.

Description

technical field [0001] The invention belongs to the technical field of metal-organic framework materials, and more specifically relates to a titanium-doped ternary metal-organic framework material and a preparation method thereof. Background technique [0002] Efficient removal of organic pollutants in water is of great ecological and environmental significance, and has become a hot research topic. Some traditional water treatment methods such as adsorption, chemical oxidation and biological treatment often have high operating costs and even produce secondary pollution. And based on TiO 2 , ZnO, Fe 2 o 3 The photocatalytic technology of semiconductor photocatalysts such as CdS, GaP and ZnS can degrade most of the organic pollutants in wastewater into biologically treatable forms or into less toxic organic compounds, and some can even decompose organic matter into CO2 、H 2 O, NO 3 - 、PO 4 3- and small molecules such as halide ions. However, these semiconductor mater...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C08G83/00C02F1/30C02F101/38
CPCC02F1/30C08G83/008B01J31/2243B01J2523/48B01J2523/47B01J2523/67C02F2305/10C02F2101/40C02F2101/38C02F2101/308B01J35/39
Inventor 栾奕齐悦
Owner 苏州安仕泊环保科技有限公司
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