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190 Chapter 7<br />

7.4.2 Hydrogenation of PNP to PAP<br />

The catalytic aqueous-phase in-situ hydrogenation of PNP to PAP using NaBH4 as a<br />

hydrogen source was carried out in a 100 cm 3 batch reactor at room temperature (298K),<br />

ambient pressure and 1300 min -1 stirring speed. Figure 7.28 depicts the catalytic<br />

experimental setup. In the typical catalytic experiment, 5.0 cm 3 of an aqueous solution of<br />

NaBH4 (0.60 mmol dm −3 ) were added to 45.0 cm 3 of an aqueous solution of PNP (0.18<br />

mmol dm −3 ). The reaction was started by introducing 5.0 mg of the catalyst. PNP<br />

concentration changes were monitored via online UV-vis spectroscopy (AvaSpec-3648,<br />

optical path length: 5 mm) at a wavelength of 400 nm (see Figure 7.29). The initial<br />

reaction rate (r0) was calculated by assuming a zero order reaction from the linear<br />

decrease of PNP concentration after the addition of the catalyst.<br />

Figure 7.28. Experimental setup for aqueous-phase in-situ hydrogenation of PNP to PAP with<br />

NaBH 4 as hydrogen source using an online UV-vis spectrometer. Figure is provided by M. Al-Naji.

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