Troger's base conjugated microporous polymer photocatalyst, and preparation method and application thereof

A technology towards Geer bases and microporous polymers, applied in the direction of organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of insufficient absorption and utilization of visible light , to achieve excellent CO2 adsorption capacity, large application potential, and large specific surface area

Active Publication Date: 2021-01-01
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN109942570A discloses a conjugated microporous polymer based on phenothiazine, and uses the material for the photocatalytic aerobic selenization of indole, bu

Method used

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  • Troger's base conjugated microporous polymer photocatalyst, and preparation method and application thereof
  • Troger's base conjugated microporous polymer photocatalyst, and preparation method and application thereof
  • Troger's base conjugated microporous polymer photocatalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The reaction equation of the present embodiment is as follows:

[0035]

[0036] Dissolve 2.369g diiodochauger base (5.0mmol) in 40mL anhydrous N,N-dimethylformamide, add 3.344g carbazole (20mmol), 2.764g potassium carbonate (20mmol), 0.095g iodine Cuprous chloride (0.5mmol) and 0.009g 1,10-phenanthroline (0.05mmol) were reacted at 150°C for 24h under nitrogen protection. Cool to room temperature, remove the solvent, and purify the product by column chromatography (ethyl acetate / petroleum ether=1:3) to obtain a light brown carbazole-based conjugated microporous polymer monomer.

[0037]Disperse 0.203g (0.367mmol) of carbazole-based conjugated microporous polymer monomer in 25mL of anhydrous chloroform, then add 0.595g (3.67mmol) of ferric chloride, and react at 60°C for 24h under nitrogen protection. Then 50 mL of methanol was added to the reaction mixture, and the resulting mixture was stirred for another 1 hour, and the precipitate was collected by filtration and ...

Embodiment 2

[0043] The reaction equation of the present embodiment is as follows:

[0044]

[0045] With 20ml of N,N-dimethylformamide and 20ml of triethylamine mixed solution as the reaction medium, add 0.356g of diiodo Chaoger base (0.75mmol), 0.075g of 1,3,5-triethynylbenzene ( 0.5mmol), 0.029g Pd (pph 3 ) 4 (0.025mmol) and 0.005g CuI (0.025mmol), reacted at 80°C for 24h under nitrogen protection. Collect the precipitate after the reaction, stir the precipitate in hydrochloric acid solution for 1 hour, wash with water, stir in a mixed solution of acetone, toluene and methanol for 1 hour, dry, and perform Soxhlet extraction with a mixed solution of methanol and tetrahydrofuran to obtain a yellow Conjugated microporous polymer in powder form.

[0046] Figure 5 It is the infrared spectrogram of the conjugated microporous polymer prepared in Example 2. Among them at 1316cm -1 and 1097cm -1 It is the stretching vibration absorption peak of C-N outside the ring, which is the carbo...

Embodiment 3

[0050] The reaction equation of the present embodiment is as follows:

[0051]

[0052] With 20ml of N,N-dimethylformamide and 20ml of triethylamine mixed solution as the reaction medium, add 0.356g of diiodochauger base (0.75mmol), 0.063g of 1,4-diethynylbenzene (0.5mmol ), 0.029g Pd (pph 3 ) 4 (0.025mmol) and 0.005g CuI (0.025mmol), reacted at 80°C for 24h under nitrogen protection. Collect the precipitate after the reaction, stir the precipitate in hydrochloric acid solution for 1 hour, wash with water, stir in a mixed solution of acetone, toluene and methanol for 1 hour, dry, and perform Soxhlet extraction with a mixed solution of methanol and tetrahydrofuran to obtain a yellow Conjugated microporous polymer in powder form.

[0053] Figure 8 It is the infrared spectrogram of the conjugated microporous polymer prepared in Example 3. Among them at 1316cm -1 and 1097cm -1 It is the stretching vibration absorption peak of C-N outside the ring, which is the carbon-ni...

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Abstract

The invention discloses a Troger's base conjugated microporous polymer and a preparation method thereof. The Troger's base conjugated microporous polymer is prepared by taking diiodo Troger's base andcarbazole or aromatic diyne and triyne compounds as raw materials through an oxidative coupling or Sonogashira coupling copolymerization reaction. The conjugated microporous polymer has a V-shaped rigid skeleton structure, is high in physical and chemical stability, strong in gas adsorption capacity, large in specific surface area and strong in visible light absorption capacity, and can be applied to the fields of photocatalytic pollutant degradation, water decomposition and CO2 reduction.

Description

technical field [0001] The invention belongs to the technical field of photoelectric functional materials, and in particular relates to a Chaoger base conjugated microporous polymer, a preparation method and its photocatalytic application. Background technique [0002] The organic framework of conjugated microporous polymers is completely connected by benzene rings and carbon-carbon triple bonds in the form of π-electron conjugation, which provides a basis for their applications in optoelectronics, energy storage and sensing. Since Cooper reported the first polyaryne-based conjugated microporous polymer in 2007, many conjugated microporous polymers with different structures and properties have been continuously developed. Although this type of material does not have long-term programmability, due to its relatively mild synthetic reaction conditions, it is very suitable for the use of functionalized monomers to construct functionalized new conjugated microporous polymers. Th...

Claims

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Application Information

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IPC IPC(8): C08G61/12B01J31/06B01J35/10
CPCC08G61/124C08G61/122B01J31/063B01J35/1004B01J35/004C08G2261/11C08G2261/12C08G2261/132C08G2261/3241C08G2261/312C08G2261/3328C08G2261/344C08G2261/354C08G2261/43C08G2261/415C08G2261/598Y02W10/37
Inventor 杨勇徐胜宇唐钲熊丽君
Owner NANJING UNIV OF SCI & TECH
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