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

Inorganics

Daniel Raichman¹  David Strawser¹ 

[1] Department of Chemistry, Nanomaterials Research Center, Institute of Nanotechnology & Advanced Materials, Bar-Ilan University, Ramat-Gan 52900, Israel;

关键词: DOE;    design of experiments;    optimization;    tungsten disulfide;    nanotubes;    WS₂ INTs;    Vilsmeier–Haack reagents;   

DOI  :  10.3390/inorganics2030455

来源: mdpi

【 摘 要 】

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.

【 授权许可】

CC BY   
© 2014 by the authors; licensee MDPI, Basel, Switzerland.