Abstract:

The dataset shows details of the optical micrographs and cryo-scanning electron micrographs of oil droplets stabilized by carbonized halloysite nanotubes. Scanning electron microscopy is used to show images of native halloysite clay nanotubules (HNT) and carbonized HNT (CHNT) that is carbonized using chitosan as carbon source. Additional data reported include the mass of carbon coating on the HNT, particle partitioning and varying droplet diameters obtained using HNT with different levels of carbonization. This data supports the paper "Tuning the Wettability of Halloysite Clay Nanotubes by Surface Carbonization for Optimal Emulsion Stabilization" published in LANGMUIR doi: 10.1021/acs.langmuir.5b03878

Suggested Citation:

Vijay T. John, Olasehinde Owoseni. 2016. Dataset for: Tuning the Wettability of Halloysite Clay Nanotubes by Surface Carbonization for Optimal Emulsion Stabilization. Distributed by: GRIIDC, Harte Research Institute, Texas A&M University–Corpus Christi. doi:10.7266/N7QZ27ZS

Publications:

Owoseni, O., Zhang, Y., Su, Y., He, J., McPherson, G. L., Bose, A., & John, V. T. (2015). Tuning the Wettability of Halloysite Clay Nanotubes by Surface Carbonization for Optimal Emulsion Stabilization. Langmuir, 31(51), 13700–13707. doi:10.1021/acs.langmuir.5b03878

Purpose:

The dataset was developed to demonstrate how the optimal partitioning of halloysite nanotubes to the oil-water interface can be achieved by a selective, surface carbonization technique. This effort is significant in effective oil spill remediation.

Data Parameters and Units:

Figure 1 Energy Particle Detachment.xlsx - contact angle, free energy of detachment sphere(ΔG/kT), free energy of detachment cylinder (Aspect Ratio, 5)(ΔG/kT), free energy of detachment cylinder (aspect ratio, 10) (ΔG/kT). Figure 2a.jpg: Schematic for the synthesis of carbonized halloysite. Figure 2 FTIR Analysis.xlsx - carbonization mechanism (Halloysite, Carbon/Halloysite, Chitosan/Halloysite, Chitosan), Transmittance (a.u), wavenumber (1/cm). Table 2 TGA of CHNT.xlsx: Sample name, mass percent of Carbon coating on halloysite nanotube (%). Table 2 Zeta Potential of Chitosan HNT mixtures.xlsx: Mass ratio of Chitosan to halloysite, zeta potential (mV). Figure 3a TGA Analysis.xlsx: Temperature (degrees Celsius), Mass loss (%), HNT = halloysite aluminosilicate nanotube, CHNT1 = mass ratio used in particle synthesis chitosan to hallyosite = 0.002, CHNT3 = mass ratio used in particle synthesis chitosan to halloysite 0.02, CHNT5 = mass ratio used in particle synthesis chitosan to halloysite 0.05, CHNT7 = mass ratio used in particle synthesis chitosan to halloysite 0.5, CHNT8 = mass ratio used in particle synthesis chitosan to halloysite 1. Figure 3b.jpg: Photograph of carbonized halloysite (CHNT) samples with increasing levels of carbonization from left to right. Figure 4a SEM of HNT.jpg - SEM image of native HNT (magnification 5000x). Figure 4b SEM of HNT.jpg - SEM image of native HNT (magnification 150000X). Figure 4c SEM of CHNT5 - SEM image of carbonized nanotubes mass ratio used in particle synthesis chitosan to halloysite 0.05 (magnification 9000x). Figure 4d SEM of CHNT5.jpg - SEM image of carbonized nanotubes mass ratio used in particle synthesis chitosan to halloysite 0.05 (magnification 70000x). Figure 4e SEM of CHNT7.jpg - SEM image of carbonized nanotubes mass ratio used in particle synthesis chitosan to halloysite 0.5 (magnification 100000x). Figure 4f TEM of CHNT7.jpg - TEM image of carbonized halloysite (CHNT5) mass ratio used in particle synthesis chitosan to halloysite 0.05. Figure 4g SEM EDS of CHNT7.jpg - Energy dispersive X-ray spectroscopy (EDS) spectrum of CHNT. Figure 5a Partition Experiment.jpg - photograph of (from left to right) native HNT, intermediate carbonization CHNT4 (mass ratio used in particle synthesis chitosan to halloysite 0.025, high carbonization CHNT7 (mass ratio used in particle synthesis chitosan to halloysite = 0.5) immediately after gentle mixing. Figure 5b Partition Experiment.jpg - photograph of (from left to right) native HNT, intermediate carbonization CHNT4 (mass ratio used in particle synthesis chitosan to halloysite 0.025, high carbonization CHNT7 (mass ratio used in particle synthesis chitosan to halloysite = 0.5) after 1 hour. Figure 6a Optical Microscope CHNT1.jpg - optical microscopy image of emulsion stabilized by halloysite (HNT) mass ratio used in particle synthesis chitosan to halloysite = 0.002. Figure 6a Optical Microscope CHNT2 - optical microscopy image of emulsion stabilized by halloysite (HNT) mass ratio used in particle synthesis chitosan to halloysite = 0.01. Figure 6a Optical Microscope CHNT4.jpg - optical microscopy image of emulsion stabilized by halloysite (HNT) mass ratio used in particle synthesis chitosan to halloysite 0.025. Figure 6a Optical Microscope CHNT6.jpg - optical microscopy image of emulsion stabilized by halloysite (HNT) mass ratio used in particle synthesis chitosan to halloysite 0.2. Figure 6a Optical Microscope CHNT7.jpg - optical microscopy image of emulsion stabilized by halloysite (HNT) mass ratio used in particle synthesis chitosan to halloysite 0.5 Figure 6 a HNT.jpg - optical microscopy image of emulsion stabilized by halloysite (HNT). Figure 6b1 Interfacial Tension.xlsx - Sample (HNT = halloysite aluminosilicate nanotube, CHNT1 = mass ratio used in particle synthesis chitosan to halloysite = 0.002, CHNT2 = mass ratio used in particle synthesis 0.01, CHNT3 = mass ratio used in particle synthesis chitosan to halloysite 0.02, CHNT4 = mass ratio used in particle synthesis chitosan to halloysite 0.025, CHNT5 = mass ratio used in particle synthesis chitosan to halloysite 0.05, CHNT6 = mass ratio used in particle synthesis chitosan to halloysite 0.2, CHNT7 = mass ratio used in particle synthesis chitosan to halloysite 0.5), interfacial tension (mN/m). Figure 6b2 Droplet Sizes.xlsx - Sample (HNT = halloysite aluminosilicate nanotube, CHNT1 = mass ratio used in particle synthesis chitosan to halloysite = 0.002, CHNT2 = mass ratio used in particle synthesis 0.01, CHNT3 = mass ratio used in particle synthesis chitosan to halloysite 0.02, CHNT4 = mass ratio used in particle synthesis chitosan to halloysite 0.025, CHNT5 = mass ratio used in particle synthesis chitosan to halloysite 0.05, CHNT6 = mass ratio used in particle synthesis chitosan to halloysite 0.2, CHNT7 = mass ratio used in particle synthesis chitosan to halloysite 0.5), Droplet number, Droplet sizes (micron). Figure 7a Carbon Coating and Contact Angle.xlsx - sample (HNT = halloysite aluminosilicate nanotube, CHNT1 = mass ratio used in particle synthesis chitosan to halloysite = 0.002, CHNT2 = mass ratio used in particle synthesis 0.01, CHNT3 = mass ratio used in particle synthesis chitosan to halloysite 0.02, CHNT4 = mass ratio used in particle synthesis chitosan to halloysite 0.025, CHNT5 = mass ratio used in particle synthesis chitosan to halloysite 0.05, CHNT6 = mass ratio used in particle synthesis chitosan to halloysite 0.2, CHNT7 = mass ratio used in particle synthesis chitosan to halloysite 0.5, CHNT8 = mass ratio used in particle synthesis chitosan to halloysite 1), replicates, contact angle (degrees), mass percentage of carbon on halloysite (wt%). Figure 7b contact angle CHNT2.jpg - photograph of contact angle mass ratio used in particle synthesis chitosan to halloysite 0.01. Figure 7b contact angle CHNT4.jpg- photograph of contact angle mass ratio used in particle synthesis chitosan to halloysite 0.025. Figure 7b contact angle CHNT8.jpg - photograph of contact angle mass ratio used in particle synthesis chitosan to halloysite 1. Figure 7b contact angle HNT.jpg - photograph of contact angle halloysite aluminosilicate nanotube. Figure 8a Photograph.jpg - cryo-scanning electron microscopy image of dodecane-in-water stabilized by CHNT2 (mass ratio used in particle synthesis 0.01) (magnification 70x). Figure 8b Photograph.jpg - cryo-scanning electron microscopy image of dodecane-in-water stabilized by CHNT2 (mass ratio used in particle synthesis 0.01)(magnification 900x). Figure 8c Photograph.jpg - cryo-scanning electron microscopy image of dodecane-in-water stabilized by CHNT2 (mass ratio used in particle synthesis 0.01)(magnification 11000x). Figure 8d Photograph.jpg - cryo-scanning electron microscopy image of dodecane-in-water stabilized by CHNT2 (mass ratio used in particle synthesis 0.01)(magnification 60000x). Figure 8e Photograph.jpg - cryo-scanning electron microscopy image of dodecane-in-water stabilized by CHNT6 (mass ratio used in particle synthesis 0.2) (magnification 60x). Figure 8f Photograph.jpg - cryo-scanning electron microscopy image of dodecane-in-water stabilized by CHNT6 (mass ratio used in particle synthesis 0.2) (magnification 600x). Figure 8g Photograph.jpg - cryo-scanning electron microscopy image of dodecane-in-water stabilized by CHNT6 (mass ratio used in particle synthesis 0.2) (magnification 13000x). Figure 8h Photograph.jpg - cryo-scanning electron microscopy image of dodecane-in-water stabilized by CHNT6 (mass ratio used in particle synthesis 0.2) (magnification 80000x)

Methods:

Interfacial Tension: Goniometer (Ramé-Hart Model 250) and the analysis was carried out using the DROPimage Advanced Software. Contact Angle Measurements: Particle compression (in Specac) at 30 MPa (Riken high pressure hydraulic equipment). Water was added using 21 gauge needle (Ramé-Hart), angle was measured at dodecane-water-particle interface. Fourier Transform InfraRed Spectroscopy (FTIR): Thermo Nicolet Nexus 670 FT-IR spectrophotometer.Cryo-Scanning Electron Microscopy (SEM) Hitachi S-4800 Field Emission SEM operated at a voltage of 3 kV and a working distance of 9 mm. Scanning Electron Microscopy (SEM) Hitachi S-4700 Field Emission SEM, Transmission Electron Microscopy (TEM) JEOL 2010, operated at 200 kV. Energy Dispersive X-ray Spectroscopy (EDS) Hitachi S-4700 Field Emission SEM operated at a voltage of 20 kV and a working distance of 15 mm. Thermogravimetric Analysis: TA Instruments SDT 2960. Zeta Potential Measurement Phase analysis light scattering (PALS) (Nanobrook ZetaPALS, Brookhaven Instrument. Magnification used for optical microscopy in images labeled Figure 6a was 10x/0.30 on a Nikon Eclipse LV100 Microscope.

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