**2.4. Catalytic activity measurements**

Partial hydrogenation of sunflower and soybean oil over prepared catalysts was carried out under laboratory and pilot plant conditions. Schematics of the lab- and pilot-experimental setup are shown in **Figures 3** and **4**.

**Figure 3.** Schematic representation of the experimental setup—laboratory reactor system.

Supported Nickel-Based Catalysts for Partial Hydrogenation of Edible Oils http://dx.doi.org/10.5772/66967 141

**Figure 4.** Schematic representation of the experimental setup—pilot plant reactor system.

extrapolation of the isotherms to zero pressure. Further details about the expressions used to

*Experimental setup—pulse chemisorb TPDRO 1100. In situ* reduction of catalyst precursors at

the precursors were degassed by temperature programmed desorption at 425°C (carrier gas

*X-ray photoelectron spectroscopy (XPS)*. The quantitative chemical composition of surfaces of catalyst precursors and the valence state of studied ions were obtained by X-ray photoelectron spectroscopy. XPS measurements were performed using a VG Scientific Escalab Mk II spectrometer interfaced with the necessary data handling software Lab Cal 2. Spectra were recorded under ultrahigh vacuum conditions (10−8 Torr), using Al Kα primary radiation (1486.6 eV). Data were collected in the sequence of a survey scan (to determine the C 1s reference), followed by scans of

Partial hydrogenation of sunflower and soybean oil over prepared catalysts was carried out under laboratory and pilot plant conditions. Schematics of the lab- and pilot-experimental

the O 1s, S 2p, Ni 2p3/2 and Ag 3d regions to minimize the time of exposure to X-rays.

**Figure 3.** Schematic representation of the experimental setup—laboratory reactor system.

min−1 H2

/Ar (4.9 vol% of H<sup>2</sup>

) of pure H2

. Finally, the catalyst precursors were

at 45°C.

). After reduction,

calculate nickel crystallite sizes can be found in our previous paper (see [29]).

430°C (2°C min−1) for 1 h, under a flow of 20 cm3

**2.4. Catalytic activity measurements**

setup are shown in **Figures 3** and **4**.

Ar) and cooled at 45°C, to carry out chemisorption of H<sup>2</sup>

140 New Advances in Hydrogenation Processes - Fundamentals and Applications

subjected to a known number of calibrated pulses (0.353 cm3

*Experimental setup—laboratory reactor system*. The hydrogenation tests were carried out in a Parr 5100 glass 1 L jacketed reactor operated in a semibatch mode. The laboratory system comprises a catalytic reactor interfaced with a mass flow controller—Bronkhorst EL-FLOW model F-201C and a digital electronic pressure meter—Bronkhorst EL-PRESS model P-502C and a minicomputer. The reactor was connected to a hydrogen source, maintained at a constant pressure. The reduced catalyst was added to the oil when the reaction temperature was reached using a new type of catalyst feeder constructed in our laboratories (IChTM-DCCE). The catalytic tests were performed at 160°C and 0.2 MPa, using 900 g of sunflower oil. The catalyst weight was adjusted in order to keep constant oil to Ni mass ratio (0.06 wt% Ni with respect to the amount of oil). The stirring rate was 1200 rpm. An experimental procedure of hydrogenation test under laboratory conditions was described in detail in our previous paper [30].

*Experimental setup—pilot plant reactor system*. The catalytic experiments were carried out in a 7.5-L batch-stirred PPV (Pilot Plant Vital) reaction vessel. The PPV and its ancillaries were available at the research facilities of Oils and Vegetable Fats Factory Vital-Vrbas. **Figure 4** shows a schematic representation of the experimental setup.

Each experiment was performed at a constant liquid volume and constant oil/catalyst mass ratio (see [29]). Before the reactor was heated, the headspace was purged with nitrogen to remove oxygen. The catalyst sample was precisely weighed and added to the liquid soybean oil at working temperature (160°C), under a mixing speed set at 750 rpm. The reactor was then pressurized with pure hydrogen to the operating pressure (0.16 MPa). During the experiments, the heat flow, hydrogen uptake and reactor temperature and pressure were monitored by instruments interfaced to the reactor PPV system. For each run, the soybean oil batch was partially hydrogenated to a final IV of 90. The composition of fatty acids in the original soybean oil and hydrogenated products was analyzed by the capillary gas chromatographic method. Experiments were performed on a Schimadzu GC-9A equipped with flame ionization detector (FID). Chromatographic conditions were as follows: HP-88 capillary column (100 m × 0.25 mm, 0.20 μm film thickness, Agilent), oven temperature of 180°C, detector and injector temperature of 240°C. Injection was carried out in the splite mode at a splite ratio of 1:4. The injection volume was 2 μL. Helium was used as the carrier gas at a constant flow rate of 1.2 cm3 min−1. The IUPAC method II.D.19 [70] for preparation and CG analysis of fatty acids methyl esters was used to convert fatty acids, taken out at predetermined time intervals from the catalytic reactor, into their corresponding methyl esters.
