Chlorobenzene

Crude jatropha oil was supplied by Biofuel Bionas Sdn Bhd. Formic acid (98%), hydrogen peroxide (30%), sulphuric acid (95%), methanol (99%), and crystal violet (96%) were supplied by R&M Chemicals, Dundee, UK. Magnesium sulphate (97%), hydrogen bromide (33%), 4-methylhexhydrophthalic anhydride (MHPA) (98%), and tetraethyl ammonium bromide (TEAB) (98%) were obtained from ACROS Organic, Carlsbad, CA, USA. Potassium hydrogen phthalate (99%) was obtained from AJAX Chemicals, Taren Point, Australia, and chlorobenzene (99%) was supplied by Merck, Kenilworth, NJ, USA. All chemicals were used as received.

Toluene 2,4-diisocyanate (TDI) (Sigma Aldrich, St. Louis, MO, USA), glycerol (Sigma Aldrich, St. Louis, MO, USA), 1,4-butanediol (Merck, Darmstadt, Germany), 1,6-hexanediol (Merck, Darmstadt, Germany), and chlorobenzene (Merck, Darmstadt, Germany) were used for the preparation of TDI-prepolymers, and cyclohexanone (ABCR, Karlsruhe, Germany) was used as a solvent. For the microcapsule synthesis, isophorone diisocyanate (IPDI) (Sigma Aldrich, St. Louis, MO, USA) was used as a core material, gum arabic (GA) (Sigma Aldrich, St. Louis, MO, USA) was used as a surfactant and cyclohexanone (ABCR, Karlsruhe, Germany), was used as a solvent. For the coating’s preparation, polyol (LUMIFLON LF9716 fluoropolymer consisting of alternating fluoroethylene and vinyl ether segments with an OH value of 170 KOH/g, AGC Chemicals, Exton, PA, USA) and diisocyanate (Desmodur N3900 aliphatic isocyanate resin based on hexamethylene diisocyanate, Convestro, Leverkusen, Germany) were used, and 2,2-dimethoxypropane (Sigma Aldrich, St. Louis, MO, USA) was used as a thinner.

Bentonite clay, PVP-DVB, palladium chloride (PdCl₂), FeCl₂.4H₂O, FeCl₃.6H₂O, ethanol (EtOH), acetic acid, hydrazine hydrate (NH₂NH₂), ammonia, phenylboronic acid, iodobenzene, chlorobenzene, bromobenzene, 4-nitrophenol (4-NP), sodium borohydride (NaBH₄), potassium carbonate (K₂CO₃), and acetonitrile (MeCN), were obtained from Merck and Sigma-Aldrich. The prepared nanocatalyst was characterized by scanning electron microscopy (FE-SEM, TESCAN-MIRA3), transmission electron microscope (TEM, EM10 c–100 kV), and Fourier-transform infrared spectroscopy (FT‐IR, Bruker, Germany, RT-DLATGS detector). Nanocatalyst surface images and EDX-MAP spectra were obtained using the TESCAN MIRA III. Thermogravimetric analysis (TGA) was carried out by a thermal analyzer with a 20 °C/min heating rate in the temperature range of 25 to 1000 °C under compressed nitrogen flow. Also, the chemical composition of the nanocatalyst surface was analyzed using an X-ray photoelectron spectrometer (XPS, SPECS model UHV analysis system). The magnetic property of the prepared nanocatalyst was measured by a vibrating sample magnetometer (VSM) and the percentage of palladium metal immobilized on the substrate was measured using ICP analysis with ARL Model 3410. Finally, the reduction of 4-NP in the presence of the synthesized nanocatalyst was controlled by UV–vis spectroscopy.

Reagents: 2-chloroaniline, 4-chloroaniline, phosphorus trichloride (Acros Organics, Geel, Belgium, for synthesis); salicylic acid, ethyl chloroacetate, methyl chloroacetate, hydrazine monohydrate, β-cyclodextrin (Sigma-Aldrich, St. Louis, MO, USA, for synthesis) and solvents: chlorobenzene, absolute ethanol, dimethylformamide, dimethyl sulfoxide (DMSO), 2-butanone (Merck, Darmstadt, Germany, analytical purity), were used as purchased.

Cyclic olefin polymer, Zeonex ^® 480R (density: 1.01 g/cm³, Melt Flow Index (MFI): 21 g/10 min obtained under a load of 2.16 kg at 280 °C) was supplied by Zeon Europe GmbH (Düsseldorf, Germany). POREFIL^® with a surface tension 16 mN/m was employed as a wetting liquid for the porometry measurements.
Other used chemicals in this study were the solvents chloroform (CF, purity, 99–99.4% (GC)), 1,2,4-trichlorobenzene (TCB, anhydrous, ≥99%), chlorobenzene (CB, Synthesis grade, ≥99%), and toluene (T, purity, ≥99.9 (GC)) obtained from Merck. Some properties of interest for these solvents (e.g., density, boiling point, solubility parameter, dipole moment, and dielectric constant) are summarized in Table 1. N,N-dimethylacetamide (DMAc, Synthesis grade, ≥99%) used in this study as non-solvent was also purchased from Merck.

For the synthesis of the Rb_0.05Cs_0.1FA_0.85PbI₃ perovskite, the following materials were used: lead (II) iodide (Sigma-Aldrich, 99%, St. Louis, MO, USA), formamidinium iodide (FAI) (Sigma-Aldrich, ≥99%, St. Louis, MO, USA), cesium iodide (Sigma-Aldrich, ≥99%, St. Louis, MO, USA), rubidium iodide (Sigma-Aldrich, ≥99%, St. Louis, MO, USA), N,N-dimethylformamide (DMF) (Merck, p.a., Darmstadt, Germany), dimethyl sulfoxide (DMSO) (Merck, p.a., Darmstadt, Germany), chlorobenzene (Merck, p.a., Darmstadt, Germany).
15 × 15 mm indium tin oxide (ITO) coated glass plates (Lumtech, ρ ~15 Ω/sq, CA, USA) were used as substrate and transparent front electrode. For the synthesis of the TiO₂ ETL titanium diisopropoxide (Sigma-Aldrich, 99%, St. Louis, MO, USA), acetylacetonate (Sigma-Aldrich, 99%, St. Louis, MO, USA) and ethanol (Merck, p.a., Darmstadt, Germany) were used. For the preparation of the spiro-OMeTAD HTL, spiro-OMeTAD (Merck, ≥99%, Darmstadt, Germany), 4-tert-butylpyridine (tBP) (Sigma-Aldrich, 99%, St. Louis, MO, USA), FK209 (Sigma-Aldrich, 99%, St. Louis, MO, USA), bis-(trifluoromethane)sulfonimide lithium salt (LiTFSI) (Sigma-Aldrich, 99%, St. Louis, MO, USA) and acetonitrile (Merck, p.a., Darmstadt, Germany) were used.