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C 2017, 3(2), 19; doi:10.3390/c3020019

Apparatus for Scalable Functionalization of Single-Walled Carbon Nanotubes via the Billups-Birch Reduction

1
Smalley-Curl nanoCarbon Center, Rice University, Houston, TX 77005, USA
2
Department of Chemistry, Rice University, Houston, TX 77005, USA
3
Energy Safety Research Institute, Swansea University Bay Campus, Swansea SA1 8EN, UK
4
Department of Materials Science and Nanoengineering, Rice University, Houston, TX 77005, USA
Died 17 March 2016.
*
Author to whom correspondence should be addressed.
Received: 25 May 2017 / Revised: 13 June 2017 / Accepted: 14 June 2017 / Published: 17 June 2017
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Abstract

A prototype design of a reactor for scalable functionalization of SWCNTs by the reaction of alkyl halides with Billups-Birch reduced SWCNTs is described. The Hauge apparatus is designed to allow for the safe handling of all the reagents and products under an inert atmosphere at controlled temperatures. The extent of reaction of Li/NH3 solution with the SWCNTs is measured in-situ by solution conduction, while homogenous mixing is ensured by the use of a homogenizer, and thermocouple are placed at different heights within the reactor flask. Addition of an alkyl halide yield alkyl-functionalized SWCNTs, which may be isolated by solvent extraction leaving a solid sample that is readily purified by hydrocarbon extraction. As an example, reaction of SWCNT/Li/NH3 with 1-iododecane yields dodecane-functionalized SWCNTs (C12-SWCNTs), which have been characterized by TG/DTA, XPS, and Raman spectroscopy. Sample extraction during the reaction allows for probing of the rate of the reaction in order to determine the end point of the reaction, which for C12-SWCNTs (at −78 °C) is 30 min. View Full-Text
Keywords: carbon nanotube; lithium; reduction; functionalization; ammonia carbon nanotube; lithium; reduction; functionalization; ammonia
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. (CC BY 4.0).

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MDPI and ACS Style

Pham, D.; Zhang, K.S.; Lawal, O.; Ghosh, S.; Gangoli, V.S.; Ainscough, T.J.; Kellogg, B.; Hauge, R.H.; Adams, W.W.; Barron, A.R. Apparatus for Scalable Functionalization of Single-Walled Carbon Nanotubes via the Billups-Birch Reduction. C 2017, 3, 19.

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