Inorganic Microporous Membranes for Gas Separation in Fossil Fuel ...

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4 Results and discussion He Permeance (mol/s m 2 Pa) 2.5E-08 2.5�10 8 2.0E-08 2.0·10 8 1.5E-08 1.5·10 8 1.0·10 8 1.0E-08 0.5·10 8 5.0E-09 0.0·10 8 Helium Nitrogen 0.0E+00 0.0E+00 -250 0 250 500 750 1000 1250 Time after Steam (h) 109 5.0E-09 5�10 -9 4.0E-09 4·10 -9 3.0E-09 3·10 -9 2·10 -9 2.0E-09 1·10 -9 1.0E-09 0·10 -9 Figure 76: He (♦) and N2 (■) permeance of a Ti0.5Zr0.5O2 membrane (#205) calcined at 600ºC before and after exposure to 3 bar of steam at 200ºC. N 2 Permeance (mol/s m 2 Pa)
5 Conclusions and recommendations 5 Conclusions and recommendations First, this chapter includes the conclusions of the studied zeolite materials. The basic aim was to prepare zeolite material that could separate gasses by molecular sieving. Recommendations on the zeolite materials are discussed to achieve this goal. Second, the results on sol-gel derived TiO2-ZrO2 sols, bulk materials, layers and membranes are summarised and related to the preparation of the TiO2-ZrO2 gas separation membrane goal. Additionally, suggestions for further research are outlined to achieve industrial goals. 8-ring Deca-dodecasil 3R and 6-ring Dodecasil 1H zeolite materials Deca-dodecasil 3R (DDR) hydrothermal synthesis is complex and formed zeolite mixtures of DDR with DOH or SGT (Dodecasil 1H or Sigma 2). The synthesis of DDR as a potential CO2/N2 separation membrane material was unsuccessful. Further syntheses with varying gel compositions of nutrients from several suppliers and reaction conditions should be performed in order to understand how to prepare single phase DDR. Dodecasil 1H (DOH) crystal synthesis, structure directing agent (SDA) free synthesis and SDA-free DOH by means of post synthesis treatments were performed to prepare allsilica zeolite material with pores inaccessible to gasses with the exception of gasses with a kinetic diameter of H2 or smaller. DOH can be synthesised under standard conditions (Teflon lined autoclave heated under static conditions, 200°C, gel composition: 100SiO2:9-11ADA:70-270EN:3000- 7400H2O forming crystals >100 µm). Changing the synthesis conditions from static to dynamic by means of autoclave rotation or stirring the gel in situ to obtain a more homogeneous gel mixture reduces the DOH crystallisation time from 21 days to 4 days coupled with a decrease in crystal size. The DOH crystal size can also be reduced by aging the gel at 80ºC for several hours before hydrothermal crystallisation at 200ºC. The DOH nucleation and growth can be decoupled. The DOH crystal size can be reduced to thin hexagonal plates with sizes in the order of 10 µm being too large for membrane formation or to act as seeds for the layer formation by means of the secondary growth of DOH nuclei. The DOH crystal size might be synthesised smaller by means of further crystallisation optimisation. This might be accomplished by changing the gel composition, aging of the gel and reaction condition such as the heating ramp and stirring/rotating conditions. Secondary growth of DOH crystals in gel composition with the absence of SDA was unsuccessful. Low DOH yield was obtained using a small amount of SDA in the gel composition. These synthesised DOH crystals have a ~75% SDA cage occupancy. SDAfree DOH synthesis by means of seeded synthesis was not obtained. This proposed 110
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Mitglied der Helmholtz-Gemeinschaft
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Forschungszentrum Jülich GmbH Inst
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List of Abbreviations Ac Acetyl Ace
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Summary CO2 capture and storage mig
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Zusammenfassung Die Abtrennung und
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Content Content CONTENT............
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1 Introduction and aims 1 Introduct
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1 Introduction and aims Candidate m
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2 Theoretical background 2 Theoreti
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2 Theoretical background Despite th
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2 Theoretical background Table 2 Ox
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2 Theoretical background 2.1.2 Micr
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2 Theoretical background Poly-cryst
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2 Theoretical background membranes
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2 Theoretical background Dry or wet
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2 Theoretical background the materi
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2 Theoretical background Figure 9 D
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2 Theoretical background Figure 11
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2 Theoretical background due to its
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2 Theoretical background 2.3.3.2 Mi
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2 Theoretical background 2.4 Microp
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2 Theoretical background Figure 15
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2 Theoretical background wall inter
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3 Experimental 3 Experimental The m
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3 Experimental vacuum sample holder
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3 Experimental o of as-made DOH cry
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3 Experimental Another solution was
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3 Experimental 3.4 Characterisation
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3 Experimental Element analysis The
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3 Experimental Additionally, the hy
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4 Results and discussion Abundance
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4 Results and discussion 4.2 Zeolit
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4 Results and discussion Table 14 D
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4 Results and discussion hours usin
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Page 72 and 73: 4 Results and discussion The carbon
Page 74 and 75: 4 Results and discussion DOH crysta
Page 76 and 77: 4 Results and discussion 900 [ºC]
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Page 80 and 81: 4 Results and discussion without a
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Page 84 and 85: 4 Results and discussion Solid Cont
Page 86 and 87: 4 Results and discussion difference
Page 88 and 89: 4 Results and discussion V [cm ads
Page 90 and 91: 4 Results and discussion The averag
Page 92 and 93: 4 Results and discussion DTA µV/mg
Page 94 and 95: 4 Results and discussion Vads / cm
Page 96 and 97: 4 Results and discussion The increa
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Page 100 and 101: 4 Results and discussion V micro /V
Page 102 and 103: 4 Results and discussion In pure Ti
Page 104 and 105: 4 Results and discussion In summary
Page 106 and 107: 4 Results and discussion Intensity
Page 108 and 109: 4 Results and discussion nanonic YS
Page 110 and 111: 4 Results and discussion ~50nm TiO2
Page 112 and 113: 4 Results and discussion Raman Inte
Page 114 and 115: 4 Results and discussion Tungsten 5
Page 116 and 117: 4 Results and discussion Mol% Carbo
Page 118 and 119: 4 Results and discussion Permeance
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Page 126 and 127: 6 References 22. Shao, Z., Dong, H.
Page 128 and 129: 6 References 65. Van den Berg, A. W
Page 130 and 131: 6 References 108. Wen, T. L., Heber
Page 132 and 133: Curriculum Vitae - George van der D
Page 134: Last but not least, I would like to
Page 137: Band | Volume 8 ISBN 978-3-89336-52
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