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Covalent organic framework with triphenylphosphine as skeleton, preparation method and application thereof

A covalent organic framework, triphenylphosphine technology, applied in the preparation of organic compounds, carbon-based compound preparation, organic chemistry and other directions, can solve the problems of the reusability and stability of small molecule catalysts need to be improved, and achieve improved Catalytic activity and reusability, cheap and easy availability of raw materials and solvents, enhanced interaction effect

Active Publication Date: 2021-01-22
YUNNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The triphenylphosphine ligand unit is widely used in organometallic catalysts, such as commercially available tetrakis (triphenylphosphine) palladium, bis(triphenylphosphine) palladium dichloride and other catalysts in the Suzuki-Miyaura coupling reaction have Excellent catalytic performance, but the reusability and stability of these small molecule catalysts need to be improved

Method used

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  • Covalent organic framework with triphenylphosphine as skeleton, preparation method and application thereof
  • Covalent organic framework with triphenylphosphine as skeleton, preparation method and application thereof
  • Covalent organic framework with triphenylphosphine as skeleton, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: A method for preparing a covalent organic framework with triphenylphosphine as a skeleton, the steps are as follows:

[0033] S1: Take 0.17mmol of triphenylphosphinetrialdehyde 60mg, 0.25mmol of p-phenylenediamine 28mg, add 10ml into a glass tube with a body length of 18cm and a neck length of 9cm, add 0.14ml of mesitylene and 0.42ml of 1,4-dioxine For six rings, after ultrasonically dispersing the raw materials evenly, add 0.35ml of 6mol / L acetic acid, and continue ultrasonically dispersing to form suspension A.

[0034] S2: The suspension A was frozen in liquid nitrogen, vacuumized, and degassed three times in sequence. Under the vacuum state, the glass tube was baked and sealed with a flame gun, and placed in a 120°C oven for 3 days. After cooling, the crude product was obtained.

[0035] S3: Roughly washed with N,N-dimethylformamide, then Soxhlet extracted with tetrahydrofuran and chloroform for 12 hours, and vacuum-dried at 65°C for 12 hours to obtain 6...

Embodiment 2

[0037] Example 2: A method for preparing a covalent organic framework with triphenylphosphine as a skeleton, the steps are as follows:

[0038] S1: Take 0.17mmol of triphenylphosphinetrialdehyde 60mg, 0.25mmol of p-phenylenediamine 28mg, add 10ml into a glass tube with a body length of 18cm and a neck length of 9cm, add 0.28ml of tert-butanol and 0.28ml of o-dichlorobenzene, and ultrasonically After the raw materials are evenly dispersed, add 0.35ml of 6mol / L acetic acid, and continue ultrasonic dispersion to form suspension A.

[0039] S2: The suspension A was frozen in liquid nitrogen, vacuumized, and degassed three times in sequence. Under the vacuum state, the glass tube was baked and sealed with a flame gun, and placed in a 120°C oven for 3 days. After cooling, the crude product was obtained.

[0040] S3: Suction filtration and washing with N,N-dimethylformamide, Soxhlet extraction with tetrahydrofuran and chloroform for 12 hours, and vacuum drying at 65°C for 12 hours t...

Embodiment 3

[0042] Example 3: The application of a covalent organic framework with triphenylphosphine as a skeleton (hereinafter referred to as Phos-COF) in the controllable preparation of metal nanoparticles, the specific preparation steps are as follows:

[0043] S1: Take 40mg of Phos-COF and 4mg of potassium tetrachloropalladate (K 2 PdCl 4 ), added to a 20ml reaction flask, added 4.8ml of methanol, and stirred at room temperature for 24 hours to form a suspension A.

[0044] S2: Vacuum the suspension A into a paste, then add 3.8ml of methanol to disperse, add 15mg of sodium borohydride (NaBH 4) in 1ml of methanol, stirred for 30 minutes to obtain a crude product.

[0045] S3: The crude product was centrifuged three times with methanol and dichloromethane at 10,000 rpm respectively, and the insoluble matter was collected and vacuum-dried at 65° C. for 12 hours to obtain 39 mg of a brown powder solid, with a yield of 94%.

[0046] Transmission electron microscope of the Pd nanopartic...

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Abstract

The invention discloses a covalent organic framework with triphenylphosphine as a framework as well as a preparation method and application of the covalent organic framework and relates to the field of covalent organic framework materials. The compound is formed by polycondensation of a triphenylphosphine-containing trialdehyde monomer and diamine monomer. The preparation method comprises the following steps: adding monomer triphenylphosphine trialdehyde and diamine into a solvent; carrying out ultrasonic dispersion and adding an acetic acid solution for continuous ultrasonic operation to forma suspension turbid liquid; carrying out liquid nitrogen refrigeration-vacuumizing-degassing treatment, sealing and standing on the suspension to obtain a crude product; carrying out suction filtration washing on the crude product by using N,N-dimethylformamide, and then carrying out Soxhlet extraction and vacuum drying by using tetrahydrofuran and chloroform in sequence to obtain the covalent organic framework with the triphenylphosphine as the framework. The covalent organic framework related in the invention introduces a triphenylphosphine structural unit with high coordination capabilityinto a material framework for the first time, and has a broad application prospect in the fields of gas adsorption and separation, photoelectricity, in particular to catalysis.

Description

technical field [0001] The invention relates to the field of covalent organic framework materials, in particular to a novel covalent organic framework material with triphenylphosphine as a skeleton, a preparation method and application thereof. Background technique [0002] The triphenylphosphine ligand unit is widely used in organometallic catalysts, such as commercially available tetrakis (triphenylphosphine) palladium, bis(triphenylphosphine) palladium dichloride and other catalysts in the Suzuki-Miyaura coupling reaction. Excellent catalytic performance, but the reusability and stability of these small molecule catalysts need to be improved. The introduction of triphenylphosphine ligand units into organic porous materials can effectively improve the catalytic activity, reusability and stability of triphenylphosphine metal nanoparticles or triphenylphosphine metal complex catalysts. [0003] Covalent Organic Frameworks (COFs) is a kind of two-dimensional or three-dimensi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00C07C201/14C07C45/68C07C41/30C07C1/32B22F9/24B01J31/24B01J31/06C07C15/14C07C43/205C07C47/546C07C205/06C07B37/04
Inventor 邱立陶娆张伟
Owner YUNNAN UNIV
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