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190 Chapter 7 7.4.2 Hydrogenation of PNP to PAP The catalytic aqueous-phase in-situ hydrogenation of PNP to PAP using NaBH4 as a hydrogen source was carried out in a 100 cm 3 batch reactor at room temperature (298K), ambient pressure and 1300 min -1 stirring speed. Figure 7.28 depicts the catalytic experimental setup. In the typical catalytic experiment, 5.0 cm 3 of an aqueous solution of NaBH4 (0.60 mmol dm −3 ) were added to 45.0 cm 3 of an aqueous solution of PNP (0.18 mmol dm −3 ). The reaction was started by introducing 5.0 mg of the catalyst. PNP concentration changes were monitored via online UV-vis spectroscopy (AvaSpec-3648, optical path length: 5 mm) at a wavelength of 400 nm (see Figure 7.29). The initial reaction rate (r0) was calculated by assuming a zero order reaction from the linear decrease of PNP concentration after the addition of the catalyst. Figure 7.28. Experimental setup for aqueous-phase in-situ hydrogenation of PNP to PAP with NaBH 4 as hydrogen source using an online UV-vis spectrometer. Figure is provided by M. Al-Naji.
Absorbance, a. u. Chapter 7 191 O 2 N OH NaBH 4 catalyst H 2 N t reaction OH 250 300 350 400 450 500 Wavelength, nm Figure 7.29. UV-vis spectra for increasing reaction time in the aqueous-phase in-situ hydrogenation of PNP with NaBH 4 to PAP. Figure is provided by M. Al-Naji.
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Controlled Modification of Metal-Or
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This thesis is based on the work pe
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Bochum) for the study of XPS and UH
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Zhang, for their continuous support
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II 3.2.1 Synthesis and characteriza
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IV 7.3.4 Synthesis of Cu-DEMOF samp
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VI DMSO dobdc e.g. EA EDX EtOH EXAF
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VIII TOF UHV UiO UMCM vs WCA XANES
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2 Chapter 1 limitations of the (non
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4 Chapter 2 For the synthesis of CP
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6 Chapter 2 cavities is able to rev
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8 Chapter 2 2.2.2 MOF features Adva
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10 Chapter 2 Figure 2.5. A series o
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12 Chapter 2 the material is retain
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14 Chapter 2 2.3 Synthetic approach
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16 Chapter 2 Expansion of this stru
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18 Chapter 2 (H2BPDC) [75] or other
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20 Chapter 2 Cr III CUSs of MIL-101
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22 Chapter 2 Figure 2.14. Schematic
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24 Chapter 2 adsorbate-surface inte
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3 Controlled secondary building uni
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28 Chapter 3 3.1 Preparation and in
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30 Chapter 3 formula of [Ru3 II,III
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Intensity, a. u. 32 Chapter 3 quali
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34 Chapter 3 After activating the R
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36 Chapter 3 presence of the residu
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Intensity, a. u. 38 Chapter 3 the a
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40 Chapter 3 extent than acetic aci
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42 Chapter 3 Ru-nodes. Therefore, r
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44 Chapter 3 decomposition of [BF4]
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deriv. normalized E) 46 Chapter 3 F
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48 Chapter 3 3.1.6 Summary Applying
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50 Chapter 3 3.2 Elaboration of Ru
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52 Chapter 3 with that of the Ru II
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54 Chapter 3 Figure 3.20. (a) XANES
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4 Linker-based MOF solid solutions:
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58 Chapter 4 4.1 Introduction 4.1.1
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60 Chapter 4 framework [Cu2(ndc)2(d
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62 Chapter 4 partial replacing of B
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64 Chapter 4 in the case of ip intr
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66 Chapter 4 4.2.1.1 Crystallinity
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68 Chapter 4 suggesting the absence
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70 Chapter 4 Table 4.1. The molar f
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72 Chapter 4 Figure 4.11. IR spectr
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74 Chapter 4 taking into account th
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76 Chapter 4 As quantitative digest
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78 Chapter 4 (Figure 4.16). Notably
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80 Chapter 4 framework Ru-species (
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82 Chapter 4 Figure 4.20. XANES spe
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84 Chapter 4 It is important to not
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86 Chapter 4 Ru δ+ have been obser
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88 Chapter 4 Figure 4.25. UHV-IR sp
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90 Chapter 4 Table 4.5. Possible de
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CO 2 adsorbed, mmol/g 92 Chapter 4
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H 2 adsorbed, mmol/g 94 Chapter 4 F
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CO 2 adsorbed, mmol/g 96 Chapter 4
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H 2 adsorbed, mmol/g 98 Chapter 4 8
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H 2 adsorbed, mmol/g 100 Chapter 4
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102 Chapter 4 presence of H2. [236]
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104 Chapter 4 reactive metal center
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106 Chapter 4 4.2.6 Conclusions App
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108 Chapter 4 4.3 Defects Engineeri
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Intensity, a. u. 110 Chapter 4 as-s
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weight loss, % 112 Chapter 4 100 Cu
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weight loss, % 114 Chapter 4 record
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116 Chapter 4 4.3.2 Composition and
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V, cm 3 /g 118 Chapter 4 500 400 30
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120 Chapter 4 Figure 4.50. From lef
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5 Simultaneous introduction of vari
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124 Chapter 5 preferred like Cu 2+
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126 Chapter 5 5.2 Preparation and S
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128 Chapter 5 Figure 5.5. Pawley Fi
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130 Chapter 5 5.3 Compositional cha
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132 Chapter 5 Table 5.3. The assign
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134 Chapter 5 framework are dominan
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136 Chapter 5 5.4 Synthesis, compos
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138 Chapter 5 obtained Pd-doped sol
Page 158 and 159: 140 Chapter 5 Figure 5.18. Deconvol
Page 160 and 161: V, cm 3 /g 142 Chapter 5 sorption i
Page 162 and 163: 144 Chapter 5 time as well as the i
Page 164 and 165: 146 Chapter 5 5.6 Conclusions In su
Page 166 and 167: 148 Chapter 6 coordinating anion),
Page 168 and 169: 7 Experimental Section In this Chap
Page 170 and 171: 152 Chapter 7 as water and hydroxyl
Page 172 and 173: 154 Chapter 7 internal standards an
Page 174 and 175: 156 Chapter 7 Uppermost layer is in
Page 176 and 177: 158 Chapter 7 to the more tightly b
Page 178 and 179: 160 Chapter 7 7.2 Experimental data
Page 180 and 181: 162 Chapter 7 [Ru2(OOCC(CH3)3)4(H2O
Page 182 and 183: 164 Chapter 7 Figure 7.7. The PXRD
Page 184 and 185: 166 Chapter 7 [Ru2(OOCCH3)4(H2O)2]B
Page 186 and 187: 168 Chapter 7 [Ru2(OOCCH3)4](THF)2
Page 188 and 189: 170 Chapter 7 [Ru3(BTC)2(OH)1.5]n·
Page 190 and 191: 172 Chapter 7 [Ru3(BTC)2]n∙(AcOH)
Page 192 and 193: 174 Chapter 7 Table 7.3. Feeding mo
Page 194 and 195: 176 Chapter 7 For comparison of the
Page 196 and 197: 178 Chapter 7 7.3.4 Synthesis of Cu
Page 198 and 199: 180 Chapter 7 D3 The mixture of H3B
Page 200 and 201: 182 Chapter 7 D5 This sample was re
Page 202 and 203: 184 Chapter 7 The synthesis of D7 a
Page 204 and 205: 186 Chapter 7 7.4 Experimental data
Page 206 and 207: 188 Chapter 7 Figure 7.26. PXRD pat
Page 210 and 211: 192 Chapter 7 7.5 Supplementary det
Page 212 and 213: 8 Bibliography [1] A. J. Ihde, The
Page 214 and 215: 196 Bibliography [61] S. Ma, D. Sun
Page 216 and 217: 198 Bibliography [121] T. K. Prasad
Page 218 and 219: 200 Bibliography [180] Y. Kobayashi
Page 220 and 221: 202 Bibliography [239] A. L. Harreu
Page 222 and 223: 204 Bibliography [297] A. P. Hammer
Page 224 and 225: 206 Appendix List of Presentations
Page 226: 208 Appendix 05. 2015 Grant from th
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