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Spirobifluorene conjugated microporous polymer/carbon nanotube hybrid material and preparation method thereof

A technology of conjugated micropores and carbon nanotubes, applied in the direction of hybrid capacitor electrodes, etc., can solve the problems of poor conductivity and poor cycle stability, and achieve the effects of simple operation, increased cycle stability, and improved cycle stability.

Active Publication Date: 2019-11-22
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this polymer also has limitations such as poor electrical conductivity and poor cycle life.

Method used

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  • Spirobifluorene conjugated microporous polymer/carbon nanotube hybrid material and preparation method thereof
  • Spirobifluorene conjugated microporous polymer/carbon nanotube hybrid material and preparation method thereof
  • Spirobifluorene conjugated microporous polymer/carbon nanotube hybrid material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] First, 2,2'-7,7'-tetrabromo-9,9'-spirobifluorene (252.8mg, 0.4mmoL), p-phenylenediamine (88.6mg, 0.8mmoL), Pd(dba) 2 (18.4mg, 0.032mmoL), XPhos (23.3mg, 0.048mmoL), sodium tert-butoxide (204.3mg, 2.128mmoL) were placed in a 100mL Schlenk tube, vacuum-backfilled with Ar gas three times, followed by adding 50mL of toluene solvent; Then, the reaction device was reacted at 110°C for 48h. After the end, suction filtration was performed in a sand core funnel, followed by washing with DMF, methanol, and chloroform for 12h each, and finally drying in a vacuum oven at 60°C for 24h. The obtained spirobifluorene conjugated organic polymer powder is denoted as PSPDF.

[0046]The infrared test results of PSPDF obtained in this example and 2,2'-7,7'-tetrabromo-9,9'-spirobifluorene and p-phenylenediamine are as follows figure 1 As shown, it can be seen that the C-Br on the aromatic ring in 2,2'-7,7'-tetrabromo-9,9'-spirobifluorene is at 532cm -1 and 1079cm -1 There is a stretching...

Embodiment 2

[0050] First, 2,2'-7,7'-tetrabromo-9,9'-spirobifluorene (252.8mg, 0.4mmoL), p-phenylenediamine (88.6mg, 0.8mmoL), Pd(dba) 2 (18.4mg, 0.032mmoL), XPhos (23.3mg, 0.048mmoL), sodium tert-butoxide (204.3mg, 2.128mmoL) were placed in a 100mL Schlenk tube, vacuum-backfilled with Ar gas three times, and then aminated poly 0.5% (1mg) wall carbon nanotubes were ultrasonically dispersed in toluene (50mL), and at the same time, the dispersed carbon nanotubes were added into the Schlenk tube, and stirred at room temperature for 0.5h, so that the carbon nanotubes were well dispersed in the polymerization system; then, The reaction device was reacted at 110°C for 48h. After the end, suction filtration was carried out in a sand core funnel, and then washed with DMF, methanol, and chloroform respectively for 12h each, and finally dried in a vacuum oven at 60°C for 24h. The obtained spirobifluorene conjugated microporous polymer / carbon nanotube hybrid material powder is denoted as MWCNT@PSPD-1...

Embodiment 3

[0053] First, 2,2'-7,7'-tetrabromo-9,9'-spirobifluorene (252.8mg, 0.4mmoL), p-phenylenediamine (88.6mg, 0.8mmoL), Pd(dba) 2 (18.4mg, 0.032mmoL), XPhos (23.3mg, 0.048mmoL), sodium tert-butoxide (204.3mg, 2.128mmoL) were placed in a 100mL Schlenk tube, vacuum-backfilled with Ar gas three times, at the same time, aminated poly Wall carbon nanotubes 2% (4mg) were ultrasonically dispersed in toluene (50mL). Secondly, the dispersed carbon nanotubes were added into the Schlenk tube, and stirred at room temperature for 0.5h, so that the carbon nanotubes were well dispersed in the polymerization system; then, The reaction device was reacted at 110°C for 48h. After the end, suction filtration was carried out in a sand core funnel, and then washed with DMF, methanol, and chloroform respectively for 12h each, and finally dried in a vacuum oven at 60°C for 24h. The obtained spirobifluorene conjugated microporous polymer / carbon nanotube hybrid material powder is denoted as MWCNT@PSPD-2.

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Abstract

The invention relates to a spirobifluorene conjugated microporous polymer / carbon nanotube hybrid material and a preparation method thereof. According to the hybrid material, the spirobifluorene conjugated microporous organic polymer grows on the surface of a carbon nanotube in situ through a Buchwald-Hartvelet coupling reaction, and the difference of the multiwalled carbon nanotubes with differentcontents on the performance of the obtained polymer is explored. The method is simple and convenient to operate, and the obtained hybrid material is wide in application range and has the good application prospect at the aspects of energy storage material carriers, supercapacitors and the like.

Description

technical field [0001] The invention belongs to the field of porous organic polymer hybrid materials and preparation thereof, in particular to a spirobifluorene conjugated microporous polymer / carbon nanotube hybrid material and a preparation method thereof. Background technique [0002] With the gradual depletion of traditional fossil fuels, the development of renewable energy and energy storage is imminent. In recent years, as a rising star of energy storage devices, supercapacitors have attracted widespread attention due to their high power, fast charging speed, and long cycle life. The energy stored is mainly based on the adsorption of ions in the electrolyte by the electrode material and the fast reversible redox reaction, so the electrode material is one of the reasons that affect its performance. Therefore, it is very important to prepare electrode materials rich in micropores and extremely high specific surface area. [0003] Conjugated microporous polymers have bee...

Claims

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Application Information

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IPC IPC(8): C08G73/02C08K3/04H01G11/24H01G11/30H01G11/36H01G11/48
CPCC08G73/026C08K3/041H01G11/24H01G11/30H01G11/36H01G11/48Y02E60/13
Inventor 廖耀祖闫春娜王利平
Owner DONGHUA UNIV
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