Inorganics 2014, 2(3), 455-467; doi:10.3390/inorganics2030455
Article

Design of Experiments: Optimizing the Polycarboxylation/Functionalization of Tungsten Disulfide Nanotubes

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Received: 12 May 2014; in revised form: 16 July 2014 / Accepted: 17 July 2014 / Published: 11 August 2014
(This article belongs to the Special Issue Inorganic Fullerene-like Nanoparticles and Inorganic Nanotubes)
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.
Abstract: Design of experiments (DOE) methodology was used to identify and optimize factors that influence the degree of functionalization (polycarboxylation) of WS2 INTs via a modified acidic Vilsmeier–Haack reagent. The six factors investigated were reaction time, temperature and the concentrations of 2-bromoacetic acid, WS2 INTs, silver acetate and DMF. The significance of each factor and the associated interactive effects were evaluated using a two-level factorial statistical design in conjunction with statistical software (MiniTab® 16) based on quadratic programming. Although statistical analysis indicated that no factors were statistically significant, time, temperature and concentration of silver acetate were found to be the most important contributors to obtaining maximum functionalization/carboxylation. By examining contour plots and interaction plots, it was determined that optimal functionalization is obtained in a temperature range of 115–120 °C with a reaction time of 54 h using a mixture of 6 mL DMF, 200 mg INTs, 800 mg 2-bromoacetic acid and 60 mg silver acetate.
Keywords: DOE; design of experiments; optimization; tungsten disulfide; nanotubes; WS2 INTs; Vilsmeier–Haack reagents
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MDPI and ACS Style

Raichman, D.; Strawser, D.; Lellouche, J.-P. Design of Experiments: Optimizing the Polycarboxylation/Functionalization of Tungsten Disulfide Nanotubes. Inorganics 2014, 2, 455-467.

AMA Style

Raichman D, Strawser D, Lellouche J-P. Design of Experiments: Optimizing the Polycarboxylation/Functionalization of Tungsten Disulfide Nanotubes. Inorganics. 2014; 2(3):455-467.

Chicago/Turabian Style

Raichman, Daniel; Strawser, David; Lellouche, Jean-Paul. 2014. "Design of Experiments: Optimizing the Polycarboxylation/Functionalization of Tungsten Disulfide Nanotubes." Inorganics 2, no. 3: 455-467.

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