Preparation method for in-situ grafting carbon nano tube containing benzoxazole ring polymer

A technology of benzoxazole rings and carbon nanotubes, applied in the field of materials, can solve problems such as the limitation of the range of applicable monomers, achieve uniform properties, wide application prospects, and maintain integrity

Active Publication Date: 2012-06-27

EAST CHINA UNIV OF SCI & TECH

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Among these methods, although the polymers prepared by reversible addition-cleavage chain transfer polymerization, anionic polymerization, ring-opening polymerization, ring-opening metathesis polymerization and ring-opening catalyst coordination polymeri...

Abstract

The invention belongs to the technical field of materials, and particularly relates to a preparation method for an in-situ grafting carbon nano tube containing benzoxazole ring polymer. According to the method, 4-halogenate carboxylic ester benzocyclobutene is grafted to a multi-wall carbon nano tube by Diels-Alder reaction, atom transfer radical polymerization initiates the polymerization of N-(o-hydroxyphenyl) acrylamide monomer, and a product is subjected to thermal cyclization so as to obtain the in-situ grafting carbon nano tube containing the benzoxazole ring polymer. The method has theadvantages that: the damage and cutting of the carbon nano tube, which are caused by acid treatment, can be avoided; the structural integrity of the carbon nano tube is kept; the in-situ grafting carbon nano tube containing benzoxazole ring polymer, which is obtained by the atom transfer radical polymerization, is uniform in performance; grafting polymers are connected with each other through delocalized pi bonds of the carbon nano tube so as to form a unique conjugated system; and the in-situ grafting carbon nano tube containing the benzoxazole ring polymer has wide application prospect in the aspects of semiconductors, antistatic materials, anode materials, electromagnetic shielding and structure stealth materials and the like.

Technology Topic

Antistatic MaterialsCarbon nanotube +12

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[0033] Example 1

[0034] A preparation method of in-situ grafted carbon nanotubes containing benzoxazole ring polymers. Using multi-walled carbon nanotubes as the initial raw material, ethyl 4-bromoisobutyrate is obtained through Diels-Alder reaction. Benzocyclobutene is grafted onto the surface of carbon nanotubes as a monomer polymerization initiator; atom transfer radical polymerization is used to initiate polymerization of N-(o-hydroxyphenyl)acrylamide monomer on the surface of carbon nanotubes, and finally passed The heat treatment makes the polymer ring closed to obtain in-situ grafted carbon nanotubes containing the benzoxazole ring polymer; the specific steps are:

[0035] (1) Preparation of carbon nanotube initiator

[0036] Multi-walled carbon nanotubes (produced by Shenzhen Nanoport Co., Ltd., diameter <10nm, purity> 97%) Disperse 50mg in 10g tetradecane, sonicate for 30min, stir and heat to 235℃ and continue for 25min; then add 1g 4-bromoisobutyrate ethyl benzocyclobutene dropwise, react for 30min and cool to At room temperature, it was filtered through a 0.4μm pore size polytetrafluoroethylene membrane and washed repeatedly with 1000 mL of tetrahydrofuran until the thin layer chromatography no longer showed ethyl 4-bromoisobutyrate benzocyclobutene; vacuum dried at room temperature, The carbon nanotube initiator is obtained.

[0037] (2) Preparation of polyacrylamide functionalized carbon nanotubes

[0038] Dissolve 20 mg of the carbon nanotube initiator obtained in step (1) and 3.26 g of N-(o-hydroxyphenyl)acrylamide monomer in 20 mL of o-xylene, add 1.23 mg of cuprous bromide and 2.7 mg of bipyridine, After sealing, it was filled with nitrogen three times and stirred at 100°C for 24 hours under a nitrogen atmosphere. After the viscosity increased significantly, the nitrogen atmosphere was removed, and the reaction was stopped in the air and precipitated in methanol. After passing through a 0.4μm pore size polytetrafluoroethylene After filtering with ethylene membrane, the obtained precipitate is re-dissolved in the high boiling point solvent, filtered, washed with suction, and dried in vacuum at 60° C. to obtain polyacrylamide functionalized carbon nanotubes.

[0039] (3) Preparation of carbon nanotubes grafted with benzoxazole ring polymer in situ

[0040] The polyacrylamide-functionalized carbon nanotubes obtained in step (2) are treated under vacuum at 250°C for 12 hours, and the product obtained after thermal ring closure is the in-situ grafted carbon nanotubes containing benzoxazole ring polymers tube.

Example Embodiment

[0041] Example 2

[0042] A preparation method of in-situ grafted carbon nanotubes containing benzoxazole ring polymers. Single-walled carbon nanotubes are used as the initial raw material, and ethyl 4-bromopropionate benzene is converted through Diels-Alder reaction. And cyclobutene is grafted to the surface of carbon nanotubes as a monomer polymerization initiator; atom transfer radical polymerization is used to initiate the polymerization of N-(o-hydroxyphenyl) methacrylamide monomer on the surface of carbon nanotubes. Finally, the polymer is ring-closed by heat treatment to obtain in-situ grafted carbon nanotubes containing the benzoxazole ring polymer; the specific steps are:

[0043] (1) Preparation of carbon nanotube initiator

[0044] The single-walled carbon nanotubes (manufactured by Shenzhen Nanoport Co., Ltd., pipe diameter) calcined in air at 300°C for 20 hours in an argon atmosphere <2nm, purity> 90%) 50 mg dispersed in 20 mg dodecane, sonicated for 30 minutes and then heated to 200°C with stirring for 60 minutes; then 1 g ethyl 4-bromopropionate benzocyclobutene was added dropwise, reacted for 60 minutes and then cooled to Filter through a 0.4μm pore size polytetrafluoroethylene membrane at room temperature and repeatedly wash with 1000mL tetrahydrofuran until TLC shows that it no longer contains ethyl 4-bromoisobutyrate benzocyclobutene. Dry at room temperature under vacuum , Get the carbon nanotube initiator.

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Preparation method for in-situ grafting carbon nano tube containing benzoxazole ring polymer

A technology of benzoxazole rings and carbon nanotubes, applied in the field of materials, can solve problems such as the limitation of the range of applicable monomers, achieve uniform properties, wide application prospects, and maintain integrity

AI-Extracted Technical Summary

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Abstract

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Description & Claims & Application Information

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