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Preparation method of high-purity tubular conjugated microporous polymer carbonized high-purity carbon nanotube

A technology of conjugated micropores and carbon nanotubes, which is applied in the directions of carbon nanotubes, chemical instruments and methods, nanocarbons, etc., can solve the problems of clogging, uneven distribution of thickness, defects on the surface of the tube wall, etc.

Inactive Publication Date: 2016-07-06
LANZHOU UNIVERSITY OF TECHNOLOGY
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Problems solved by technology

But its synthesized polymer nanotubes were stuck in the middle, and the hollow tubes showed signs of clogging
Non-patent literature 2-MicroporousMesoporousMater.2014,196,335–340. and literature 3-J.Mater.Chem.A,2015,3,87–91 disclose a template-free method through one-step Sonogashira–Hagihara coupling to obtain conjugated Microporous polymer nanotubes, but in Non-Patent Document 2, the prepared conjugated microporous polymer nanotubes have adhesions and the thickness distribution of the tubes is relatively uneven. In Non-Patent Document 3, the prepared conjugated microporous polymer nanotubes Microporous polymer nanotubes are composed of nanotube bundles or have defects on the surface of the tube wall

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  • Preparation method of high-purity tubular conjugated microporous polymer carbonized high-purity carbon nanotube
  • Preparation method of high-purity tubular conjugated microporous polymer carbonized high-purity carbon nanotube
  • Preparation method of high-purity tubular conjugated microporous polymer carbonized high-purity carbon nanotube

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preparation example Construction

[0010] According to the preparation method described above, its preparation steps are:

[0011] (1) Preparation of high-purity conjugated microporous polymer nanotubes: 1,3,5-triethynylbenzene and 2-amino-3,5 -Dibromopyridine is used as a monomer, with toluene and triethylamine as the solvent Pd(0) and CuI as the catalyst, the ratio of ethynyl and bromine in the monomer is adjusted to 5:1, and it is prepared by polymerizing at 80°C for 72h High-purity conjugated microporous polymer nanotubes;

[0012] (2) Preparation of high-purity carbon nanotubes by carbonizing high-purity conjugated microporous polymer nanotubes: heating the precursor of high-purity conjugated microporous polymer nanotubes to 600 °C at a heating rate of 5 °C / min in an argon atmosphere ℃, or 700°C, or 1000°C, let it carbonize, keep warm for 3h after the temperature rise, after the temperature drops to room temperature, wash the carbonized sample with ethanol and distilled water, and dry at 80°C for 24h to o...

Embodiment 1

[0014] Example 1: Weigh 750.9mg 1,3,5-triethynylbenzene, 377.87mg 2-amino-3,5-dibromopyridine, 150mg tetrakis(triphenylphosphine) palladium and 50mg cuprous iodide, add to containing In a flask containing 7.5ml of toluene and 7.5ml of triethylamine, degas with nitrogen for 30min, then raise the temperature to 80°C and stir for 72h to obtain a yellow polymer. The polymer was filtered and washed several times successively with chloroform, acetone, water and methanol to remove unreacted monomers and catalyst residues; then using methanol as a solvent, the obtained polymer was extracted by Soxhlet for 72 hours to obtain a high-purity conjugated microporous polymer nanotubes. The prepared high-purity conjugated microporous polymer nanotubes were raised to different temperatures (600°C, 700°C, 1000°C) at a heating rate of 5°C / min for 3 hours to carbonize the conjugated microporous polymer nanotubes. Then cool to room temperature, wash and dry several times with absolute ethanol and...

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Abstract

The invention discloses a preparation method of a high-purity tubular conjugated microporous polymer carbonized high-purity carbon nanotube. The method comprises the following steps: by using 1, 3, 5-triethynylbenzene and 2-amino-3, 5-dibromopyridine as monomers, using toluene and trimethylamine as solvents, and Pd(0) and CuI as catalysts, and regulating proportion of acetenyl and bromine in the monomers as 5: 1, polymerizing for 72 hours at 80 DEG C to prepare the high-purity organic polymer nanotube, and then carbonizing under the carbonization temperature by using the organic polymer nanotube as the precursor to obtain the high-purity carbon nanotube.

Description

technical field [0001] The invention relates to a preparation method of high-purity conjugated microporous polymer nanotubes. Background technique [0002] Since Lijima's research group first reported carbon nanotubes in 1991, carbon nanotubes have been used as a new type of carbon material such as: gas storage, composite materials, medicine, electronics, power generation, energy storage, catalysts, fuel cells, etc. field. Traditional carbon nanotube preparation methods mainly include arc method, laser evaporation method and chemical vapor deposition method. In contrast, carbon nanotubes prepared by graphite arc method and laser evaporation method have higher crystallization degree, but the yield is lower. The chemical vapor deposition method can realize the industrial mass production of carbon nanotubes, but the carbon nanotubes prepared by this method have many structural defects and are accompanied by impurities. High-purity carbon nanotubes can be prepared by high-tem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82Y30/00B82Y40/00
CPCC01B2202/32C01P2004/03
Inventor 李安孙寒雪朱照琪梁卫东弁鹏
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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